HomeMy WebLinkAboutContract 26683�►YY SECRETqRY
CONTqACT Np. �p �
Between
C1YY 0F FORT WORTH
and
MATERIALS ANALY�IC�-OL ����/I�ES,
I NC. (MAS)
For
LABORATORY SERVICES RELATING TO PROJECT XL
PHASE I
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DEPARTMENT OF ENVIRONMENTAL MANAGEMENTA
MARCH, 2001
City of Fort Worth, 7'exas
�9�A�ar And aun�;l an�n�un�cAt�an
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DATE REFERENCE NUMBER LOG NAME PAGE
3/27/01 **C-18519 52LAB 1 of 2
sua�ECT APPROPRIATION ORDINANCE AND AWARD OF CONTRACT TO MATERIALS
ANALYTICAL SERVICES, INC. FOR ENVIRONMENTAL LABORATORY SERVICES
FOR PROJECT XL
RECOMMENDATION:
It is recommended that the City Councii:
1. Approve the transfer of $25,000 in undesignated funds in the Environmental Management
Operating Fund to the XL Project in the Environmental Management Project Fund; and
2. Adopt the attached appropriation ordinance increasing estimated receipts and appropriations in the
Environmental Project Fund in the amount of $25,000 from available funds; and
3. Authorize the City Manager to execute a contract with Materials Analytical Services, Inc. for
environmental laboratory services at a total cost not to exceed $25,000 in connection with Project
XL.
DISCUSSION:
Project XL stands for "eXcellence and Leadership", and was created in March 1995 as part of the
Reinventing Environmental Regulation initiatives. XL projects are real world tests of innovative
strategies that achieve cleaner, more cost-effective results than traditional regulatory approaches.
Each project that is accepted into the program involves the granting of regulatory flexibility by the
Environmental Protection Agency (EPA) in exchange for an enforceable commitment by a community to
achieve better environmental results than would have been attained through full compliance with
existing or anticipated future regulations.
In recent years, the City has been waging a stepped up war on urban blight through enforcement of
building maintenance codes and through special emphasis on property redevelopment and sustainable
community issues. The City submitted its Project XL proposal to the EPA in September 1999. The
proposal, entitled "Asbestns Management in the Demolition of Substandard Structures as a Nuisance
Abatement," sought regulatory flexibility from the EPA to proceed with the demolition of substandard
structures that are not in danger of imminent collapse without prior removal of regulated asbestos
containing material.
In January 2000, THE EPA issued a conditional letter of selection. On September 29, 2000, in a
ceremony at City Hall, an agreement was signed by the City of Fort Worth, the Texas Department of
Health, and the Environmental Protection Agency to begin Phase I of the City's XL project. In February
2001, the City received EPA approval to use 2615 Ennis Avenue as the site for Phase I demolition.
Materials Analytical Services, Inc. (MAS) was selected to perform laboratory services because they are
one of the few laboratories in the United States that have relevant experience performing the analyses
needed for this project. In addition, no Texas Department of Health licensed laboratories were found to
have the experience and expertise fdr the required work. MAS has a current National Voluntary
Laboratory Accreditation Program Certification necessary for the project. MAS has experience working
with both the EPA and state governments on similar projects, and has performed satisfactorily on those
projects.
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_ City of Fo�t Worth, Texas
�11�A�ar A11d auncil afrrtm�nac�►tian
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DATE REFERENCE NUMBER LOG NAME PAGE
3/27/01 **C-18519 52LAB 2 ofi 2
suB�ECT APPROPRIATION ORDINANCE AND AW�RD OF CONTRACT TO MATERIALS
ANALYTICAL SERVICES, INC. FOR ENVIRONMENTAL LABORATORY SERVICES
FOR PROJECT XL
The provisions in Chapter 252 of the Texas Local Government Code do not apply because it is a
"procurement necessary to preserve or protect the public health or safety of the municipality's
residents."
FISCAL INFORMATION/CERTIFICATION:
The Finance Director certifies that upon approval of recommendation No. 1 and adoption of the
attached appropriation ordinance, funds will be available in the current capital budget, as appropriated,
of the Environmental Management Project Fund.
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Submitted for City Manager's FUND ACCOUNT CENTER AMOUNT CITY SECRETARY
Office by: (to)
_
2) R101 531060 052200110000 $25,000.00 _ �P�R�vE�
Charles Boswell 8511
Originating Department Head: ' . /'1'�� CO' (A'(���
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Brian Boerner 8079 (from) , MAR 2"� 2���
1) R103 538070 0521100 $25,000.00 /'
Additional Information Contact: 3) R101 531060 052200110000 $25,000.00 (fjp�„L ����
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Brian Boerner gp�g City Sc�crstary of the
City of Foxt �'arth, Tara�
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. Adoptecl Ordinanc� No, ���:
�ON RACT�Np YO7�p � ��
STATE OF TEXAS
KNOW ALL PERSONS BY THESE PRESENTS
COUNTY OF TARRANT
CONTRACT BETWEEN THE CITY OF FORT WORTH, TEXAS, AND
MATERIALS ANALYTICAL SERVICES, INC. (MAS)
FOR LABORATORY SERVICES RELATING TO PROJECT XL PHASE I
This agreement is entered into by and between the City of Fort Worth, Texas, a home-rule
municipal corporation situated in Tarrant and Denton Counties, Texas, hereinafter called "City,"
acting herein through Charles Boswell, its duly authorized Assistant City Manager, and Materials
Analytical Services, Inc. (MAS), hereinafter called "Contracto�;" by and through
�, • , ` , its duly authorized �j���� .r� ���
In consideration of the mutual promises and benefits of this contract, the City and Contractor
agree as follows:
1.
TERM
This contract shall be effective from the date of its execution by both parties, until the
completion of all Contractor services as provided in Section 2, or for a period not to exceed one
(1) year from date of execution, whichever occurs first.
2.
SCOPE OF CONTRACTOR'S SERVICES
A. Contractor shall provide on an as needed basis, all the labor, materials, and equipment
necessary for performing laboratory analysis of air, soil, and water samples taken by or
for City in Phase I of City's Project XL project. Analysis shall be accomplished utilizing
the following methods:
1
2.
�
TEM air analysis in accordance with ISO Method 10312:1995
Water analysis in accordance with EPA Method for the Determination of
Asbestos Fibers in Water
Soil analysis in accordance with EPA Standard Operating Procedure for the .
Screening Analysis of Soil and Sediment Samples for Asbestos Content
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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4. Water (Moisture) content analysis in accordance with ASTM Standard Test
Method D 4959-00 Determination of Water (Moisture) Content of Soil by Direct
Heating
B. Contractor shall forward analytical results to the City within 10 business days of sample
receipt.
C. Contractor shall perform its seivices in a good and professional manner. Contractor shall
adhere to the provisions of the Quality Assurance Project Plan (QAPP) applicable to
laboratory services. A copy of the QAPP is attached hereto as Appendix A, and
incorporated fully into this contract.
D. Contractor shall provide City with all sample containers, preservatives, and returnable
shipping containers necessary for this project, if required by MAS.
E. Contractor's handling instructions and chain-of-custody protocols shall be in accordance
with all Federal and State statutes and regulations for laboratory methods and quality
assurance.
F. Contractor shall be responsible for the disposal of the samples and such disposal shall be
in accordance with all federal and state statutes and regulations.
G. Contractor agrees that it shall maintain during the term of this contract, current and
appropriate federal, state, and local licenses and permits to perfortn the services contained
in this contract.
H. Contractor agrees that it shall not subcontract any of the services to be provided to City,
without first obtaining written permission from City to do so. Subcontractors shall be
held to the same requirements of this contract that pertain to Contractor.
3.
CITY'S RESPONSIBILITIES
A. City shall designate a City representative to provide timely direction to the Contractor
and render City decisions.
B. City shall be responsible for collecting samples or having sample collected, and shipping
them to Contractor.
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COMPENSATION
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Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
Page 2
A. In consideration for the work performed by Contractor under this contract, City shall pay
Contractor a sum not to exceed twenty-five thousand dollars ($25,000.00). Payment shall
be based on the unit price charges as set forth below:
1. TEM air analysis in accordance with ISO Method 10312:1995 =$350 per sample
2. Water analysis in accordance with EPA Method for the Determination of
Asbestos Fibers in Water =$250 per sample.
3. Soil analysis in accordance with EPA Standard Operating Procedure for the
Screening Analysis of Soil and Sediment Samples for Asbestos Content =$250
per sample.
4. Water (Moisture) content analysis in accordance with ASTM Standard Test
Method D 4959-00 Determination of Water (Moisture) Content of Soil by Direct
Heating = $50 per sample.
B. City shall make payment within thirty (30) days of receiving a correct invoice from
Contractor. City is responsible for notifying Contractor of any questions concerning an
invoice. In the event of a disputed or contested billing, only that portion so contested will be
withheld from payment, and the iuldisputed portion will be paid. The City will exercise
reasonableness in contesting any bill or portion thereof. No interest will accrue on any
contested portion of the billing until muhially resolved.
C. Contractor shall receive no compensation for delays or hindrances to the work, except
when direct and unavoidable extra cost to Contractor was caused by City's failure to
provide information, if any, which it is required to do. When extra compensation is
claimed, a written statement thereof shall be presented to the City.
5.
INSURANCE
The Contractor certifies it has, at a minimum, current insurance coverage as detailed
below and will maintain it throughout the terms of this contract. Prior to commencing work, the
Contractor shall deliver to City, certificates documenting this coverage. The City may elect to
have the Contractor submit its entire policy for inspection.
�
:
Commercial General Liabilitv Insurance -$1,000,000.00 per occurrence
Automobile Liabilitv Insurance -$1,000,000.00 per accident
1. This policy shall include pollution coverage; that is, it shall not have the pollution
exclusion. Plus, the policy shall cover loading, unloading and transporting
materials collected under this contract.
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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C. Worker's Compensation Insurance - Statutory limits, plus employer's liability at a
minimum of $ 500,000.00 each accident; $ 500,000.00 disease - policy limit; and $
500,000.00 disease - each employee.
D. Environmental Im�airment Liability�EILI and/or Pollution LiabilitX -$1,000,000.00 per
occurrence. Coverage must be included in policies listed in items A and B above; or,
such insurance shall be provided under separate policy(s). Liability for damage occurring
while loading, unloading and transporting materials collected under the contract project
shall be included under the Automobile Liability insurance or other policy(s).
NOTE: BETWEEN A AND D ABOVE, ANY POLLUTION EXPOSURE, INCLUDING
ENVIRONMENTAL IMPAIRMENT LIABILITY, ASSOCIATED WITH THE
SERVICES AND OPERATIONS PERFORMED UNDER THIS CONTRACT
SHALL BE COVERED; IN ADDITION TO SUDDEN AND ACCIDENTAL
CONTAMINATION OR POLLUTION LIABILITY FOR GRADUAL
EMISSIONS, CLEANUP COSTS SHALL BE COVERED.
E. The following shall pertain to all applicable policies of insurance listed above:
Additional Insured Endorsement: "The City of Fort Worth, its officers, agents,
employees, representatives, and volunteers are added as additional insureds as
respects operations and activities of, or on behalf of the named insured, performed
under contract with the City of Fort Worth." Reasonably equivalent terms may be
acceptable at the sole discretion of the City of Fort Worth.
2. Subcontractors shall be covered under the Contractor's insurance policies or they
shall provide their own insurance coverage; and, in the latter case, documentation
of coverage shall be submitted to the Contractor prior to the commencement of
worlc and the Contractor shall deliver such to the City.
3. Prior to commencing worlc under the contract, the Contractor shall deliver to the
City of Fort Worth insurance certificate(s) documenting the insurance required
and terms and clauses required.
4. Each insurance policy required by this agreement shall contain the following
clauses: "This insurance shall not be canceled, limited in scope or coverage, or
non-renewed until after thirty (30) days prior written notice has been given to the
Director of Environmental Management, City of Fort Worth, 1000 Throckmorton,
Fort Worth, Texas 76102."
5. The insurers for all policies must be approved to do business in the State of Texas
and be currently rated in terms of financial strength and solvency to the
satisfaction of the Director of Risk Management for the City of Fort Worth. The
City's standard is an A. M. Best Key rating A:VII.
c:ontract beriveen the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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5. The insurers for all policies must be approved to do business in the State of Texas
and be currently rated in terms of financial strength and solvency to the
satisfaction of the Director of Risk Management for the City of Fort Worth. The
City's standard is an A. M. Best Key rating A:VII.
6. The deductible or self-insured retention (SIR) affecting the coverage required
shall be acceptable to the Risk Manager of the City of Fort Worth; and, in lieu of
traditional insurance, alternative coverage maintained through insurance pools or
risk relations groups must be also approved." �
6.
INDEMNIFICATION
For purposes of this contract, the phrases "Environmental Damages" and "Environmental
Requirements" shall be defined as stated below:
1. Environmental Damages shall mean all claims, judgments, damages, losses,
penalties, iines, liabilities (including strict liability), encumbrances, liens, costs,
and expenses of investigation and defense of any claim, whether or not such claim
is ultimately defeated, and of any good faith settlement or judgment, of whatever
kind or nature, contingent or otherwise, matured or unmatured, foreseeable or
unforeseeable, including without limitation reasonable attorney's fees and
disbursements and consultant's fees, any of which are incurred as a result of
handling, collection, transportation, storage, disposal, treatment, recovery, and/or
reuse of waste pursuant to this contract, or the existence of a violation of
environmental requirements pertaining to, and including without limitation:
a. Damages for personal injury and death, or injury to properiy or natural
resources;
b. Fees incurred for the services of attorneys, consultants, contractors,
experts, laboratories and all other costs in connection with the
investigation or remediation of such wastes or violation of environmental
requirements including, but not limited to, the preparation of any
feasibility studies or reports of the performance of any cleanup,
remediation, removal, response, abatement, containment, closure,
restoration or monitoring work required by any federal, state or local
governmental agency or political subdivision, or otherwise expended in
connection with the existence of such wastes or violations of
environmental requirements, and including without limitation any
attorney's fees, costs and expenses incurred in enforcing this contract or
collecting any sums due hereunder; and
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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c. Liability to any third person or governmental agency to indemnify such
person or agency for costs expended in connection with this Agreement.
2. Environmental requirements shall mean all applicable present and future statutes,
regulations, rules, ordinances, codes, licenses, pertnits, orders, approvals, plans,
authorizations, concessions, franchises, and similar items, of all governmental
agencies, departments, commissions, boards, bureaus, or instrumentalities of the
United States, states, and political subdivisions thereof and all applicable judicial,
administrative, and regulatory decrees, judgments, and orders relating to the
protection of human health or the environment, including without limitation:
a. All requirements, including, but not limited to, those pertaining to
reporting, licensing, permitting, investigation, and remediation of
emissions, discharges, releases, or threatened releases of hazardous
materials, pollutants, contaminants or hazardous or toxic substances,
materials, or wastes whether solid, liquid, or gaseous in nature, into the
air, surface water, groundwater, storm water, or land, or relating to the
manufacture, processing, distribution, use, treatment, storage, disposal,
transport, or handling of pollutants, contaminants, or hazardous or toxic
substances, materials, or wastes, whether solid, liquid, or gaseous in
nature; and
b. All requirements pertaining to the protection of the health and safety of
employees or the public.
General Indemnification:
CONTRACTOR DOES HEREBY RELEASE, INDEMNIFY, REIMBURSE,
DEFEND, AND HOLD HARMLESS THE CITY, ITS OFFICERS, AGENTS,
EMPLOYEES AND VOLUNTEERS, FROM AND AGAINST ANY AND ALL
LIABILITY, CLAIMS, SUITS, DEMANDS, OR CAUSES OF ACTIONS WHICH
MAY ARISE DUE TO ANY LOSS OR DAMAGE TO PERSONAL PROPERTY,
OR PERSONAL INJURY, AND/OR DEATH OCCURRING AS A
CONSEQUENCE OF THE PERFORMANCE OF THIS CONTRACT, WHEN
SUCH INJURIES, DEATH, OR DAMAGES ARE CAUSED BY THE SOLE
NEGLIGENCE OF CONTRACTOR, ITS OFFICERS, AGENTS, OR
EMPLOYEES, OR THE JOINT NEGLIGENCE OF CONTRACTOR, ITS
OFFICERS, AGENTS, OR EMPLOYEES, AND ANY OTHER PERSON OR
ENTITY.
Environmental Indemnification:
CONTRACTOR DOES HEREBY RELEASE, INDEMNIFY, DEFEND,
REIMBURSE, AND HOLD HARMLESS THE CITY, ITS OFFICERS, AGENTS,
EMPLOYEES AND VOLUNTEERS, AGAINST ANY AND ALL
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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ENVIRONMENTAL DAMAGES AND THE VIOLATION OF ANY AND ALL
ENVIRONMENTAL REQUIREMENTS RESULTING FROM THE HANDLING,
TESTING, STORAGE, DISPOSAL, TREATMENT, RECOVERY, AND/OR
REUSE, BY ANY PERSON, OF SAMPLES, AS A CONSEQUENCE OF THE
PERFORMANCE OF THIS CONTRACT, WHEN SUCH DAMAGES OR
VIOLATIONS ARE CAUSED BY THE SOLE NEGLIGENCE OF
CONTRACTOR, ITS OFFICERS, AGENTS, OR EMPLOYEES, OR THE JOINT
NEGLIGENCE OF CONTRACTOR, ITS OFFICERS, AGENTS, OR
EMPLOYEES, AND ANY OTHER PERSON OR ENTITY.
D. The obligations of the Contractor under this section shall include, but not be limited to,
the burden and expense of defending all claims, suits and administrative proceedings
(with counsel reasonably approved by City), even if such claims, suits or proceedings are
groundless, false, or fraudulent, and conducting all negotiations of any description, and
paying and discharging, when and as the same become due, any and all judgments,
penalties or other sums due against such indemnified persons.
E. Upon learning of a claim, lawsuit, or other liability that Contractor is required hereunder
to indemnify City, City shall provide Contractor with reasonably timely notice of same.
F. The obligations of the Contractor under this section shall survive the expiration of this
Agreement and the discharge of all other obligations owed by the parties to each other
hereunder.
G. In all of its contracts with subcontractors for the performance of any work under this
contract, Contractor shall require the subcontractors to indemnify the City in a manner
consistent with this section.
H. In the event City receives a written claim for damages against the Contractor or its
subcontractors prior to final payment, final payment shall not be made until Contractor
either submits to City satisfactory evidence that the claim has been settled and/or a
release from the claimant involved, or provides City with a letter from Contractor's
liability insurance carrier that the claim has been referred to the insurance carrier.
7.
WARRANTY
Contractor warrants that it understands the currently known hazards and suspected hazards that
are present to persons, property and the environment by providing laboratory services.
Contractor further warrants that it will perform all services under this contract in a safe, efficient
and lawful manner using industry accepted practices, and in full compliance with all applicable
state and federal laws governing its activities. Contractor also warrants that it is under no
restraint or order that would prohibit performance of services under this contract.
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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8.
TERMINATION
A. City may terminate this contract, with or without cause, by giving 30 days written notice
to Contractor, provided that such termination shall be without prejudice to any other
remedy the City may have. In the event of tertnination, any work in progress will
continue to completion unless specified otherwise in the notice of termination.
B. If the City terminates this contract under paragraph A of this section, City shall pay
Contractor for all services performed prior to the termination notice.
C. All completed or partially completed original documents prepared under this contract
shall become the property of the City when the contract is terminated, and may be used
by the City in any manner it desires; provided, however, that the Contractor shall not be
liable for the use of such documents for any purpose other than as described when
requested.
D. In the event either party defaults in the performance of any of its obligations under this
contract, misrepresents to the other a material fact, or fails to notify the other parly of any
material fact which would affect the party's performance of its obligations hereunder, the
non-defaulting party shall have a right to terminate this contract upon giving the
defaulting party written notice describing the breach or omission in reasonable detail.
The defaulting party shall have a thirty (30) day period commencing upon the date of
notice of default in which to effect a cure. If the defaulting party fails to effect a cure
within the aforesaid thirty (30) day period, or if the default cannot be cured, the contract
shall terminate as of the date provided in the notice of default.
9.
DEFAULT
A. Contractor shall not be deemed to be in default because of any failure to perform under
this contract, if the failure arises from causes beyond the control and without the fault or
negligence of Contractor. Such causes shall include acts of God, acts of the public
enemy, acts of Government, in either its sovereign or contractual capacity, fires, flood,
epidemics, quarantine restrictions, strikes, freight embargoes, and unusually severe
weather.
B. If at any time during the term of this contract the work of Contractor fails to meet the
specifications of the contract, City may notify Contractor of the deficiency in writing.
Failure of Contractor to correct such deficiency and complete the work required under
this contract to the satisfaction of City within ten days after written notification shall
result in termination of this contract. Contractor shall pay all costs and attorneys fees
incurred by City in the enforcement of any provision of this contract.
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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C. The remedies provided for herein are in addition to any other remedies available to City
elsewhere in this contract.
10.
RIGHT TO AUDIT
A. Contractor agrees that the City shall, until the expiration of three (3) years after fmal
payment under this contract, have access to and the right to examine and photocopy any
directly pertinent books, documents, papers and records of the Contractor involving
transactions relating to this contract. Contractor agrees that the City shall have access
during normal warking hours to all necessary Contractor facilities and shall be provided
adequate and appropriate workspace in order to conduct audits in compliance with the
provisions of this section. The City shall give Contractor reasonable advance notice of
intended audits.
B. Contractor further agrees to include in all its subcontractor agreements hereunder a
provision to the effect that the subcontractor agrees that the City shall, until the expiration of
three (3) years after final payment under the subcontract, have access to and the right to
examine and photocopy any directly pertinent books, documents, papers a�d records of such
subcontractor, involving transactions to the subcontract, and further, that the City shall have
access during normal working hours to all subcontractor facilities, and shall be provided
adequate and appropriate work space, in order to conduct audits in compliance with the
provisions of this article together with subsection C. hereof. City shall give subcontractor
reasonable advance notice of intended audits.
C. Contractor and subcontractor agree to photocopy such documents as may be requested by
the City. The City agrees to reimburse Contractor and/or subcontractor for the cost of
copies at the rate published in the Texas Administrative Code in effect as of the time
copying is performed
11.
INDEPENDENT CONTRACTOR
It is understood and agreed by the parties hereto that Contractor shall perform all work and
services hereunder as an independent contractor, and not as an officer, agent, servant or
employee of the City. Contractor shall have exclusive control of and the exclusive control of and
the exclusive right to control the details of all the work and services performed hereunder, and all
persons performing same, and shall be solely responsible for the acts and omissions of its
officers, agents, servants, employees, contractors, subcontractors, licensees and invitees. The
doctrine of respondeat superior shall not apply as between City and Contractor, its officers,
agents, employees, contractors and subcontractors, and nothing herein shall be construed as
creating a partnership or joint enterprise between City and Contactor.
Contract between the City Of Fort Worth, Texas, and l'J_,i��'IJ"� ll%`;_�, U�(��l��V'f�'�11J
Materials Analytical Services, Inc. (MAS j,?�jT��i �;�,,i� ("��i���'���rr)'�UI
For laboratory services relating to Project XL Phase I � U U o�. z� 9< <� uir Uu '� Page 9
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12.
NON-DISCRIMINATION
A. During the performance of this contract, Contractor agrees not to discriminate against any
employee or applicant for employment because of race, religion, color, sex or national
origin, except where religion, sex or national origin is a bona fide occupational
qualification reasonably necessary to the normal operation of the Contractor. Contractor
agrees to post in conspicuous places, available to employees and applicants for
employment, notices setting forth the provisions of the non-discrimination clause.
B. Contractor also agrees that in all solicitations or advertisements for employees placed by
or on behalf of this contract, that Contractor is an equal opportunity employer.
C. Notices, advertisements, and solicitations placed in accordance with federal law, rule or
regulation shall be deemed sufficient for the purpose of ineeting the requirements of this
section.
13.
GOVERNING LAW
The City and Contractor agree that the laws of the State of Texas shall govern the validity and
construction of this contract, except where preempted by federal law.
14.
RIGHTS AND REMEDIES NOT WAIVED
In no event shall the making by the City of any payment to Contractor constitute or be construed
as a waiver by the City of any breach of covenant, or any default which may then exist, on the
part of Contractor, and the making of any such payment by the City while any such breach or
default exists shall in no way impair or prejudice any right or remedy available to the City with
respect to such breach or default. Any waiver by either party of any provision or condition of the
contract shall not be construed or decreed to be a waiver of any other provision or condition of
this contract, nor a waiver of a subsequent breach of the same provision or condition, unless such
waiver is expressed in writing and signed by the party to be bound.
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Contract between the City Of Fort Worth, Texas, and � �' Ij� ��"��� 'I ��� � il i�p �� �<<;�q ��
Materials Analytical Services, Inc. (MAS) ! = -•�— - - �---
For laboratory services relating to Project XL Phase I Page 10
15.
ENTIRETY
This contract and any other documents incorporated by reference herein contain all the terms and
conditions agreed to by the City and Contractor, and no other contracts, oral or otherwise,
regarding the subject matter of this contract or any part thereof shall have any validity or bind
any of the parties hereto.
16.
ASSIGNMENT
The City and Contractor bind themselves and any successors and assigns to this contract.
Contractor shall not assign, sublet, or transfer its interest in this contract without written consent
of the City. Nothing herein shall be construed as creating any personal liability on the part of
any officer or agent of the City, nor shall it be construed as giving any rights or benefits
hereunder to anyone other than the City and Contractor.
17.
NOTICE
Notices required to be made under this contract shall be sent to the following persons at the
following addresses; provided, however, that each party reserves the right to change its
designated person for notice, upon written notice to the other party of such change:
If to City:
Written notice shall be sent to:
Brian Boerner, Director
Department of Environmental Management
1000 Throckmorton
Fort Worth, Texas 76102
If to Contractor:
Questions should be directed to:
Michael Gange, Environmental Supervisor
Department of Environmental Management
1000 Throckmorton
Fort Worth, Texas 76102
(817) 871-8504 / Fax (817) 871-6359
�
Name: {� i. ��� v/�'I G� ti�' C�I���:� �,; ��C.Q� c.
Materials Analytical Services, Inc. (MAS) �
3945 Lakefield Court
Suwanee, Georgia 30024
(770) 866-3200 / Fax (770) 866-3259
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
'::!!�(���"�'°'�,�� ��[���R@
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Page 11
18.
VENUE
Should any action, real or asserted, at law or in equity, arise out of the terms and conditions of
this contract, venue for said action shall be in Tarrant County, Texas.
19.
SEVERABILITY
The provisions of this contract are severable; and if for any reason any one or more of the
provisions contained herein are held to be invalid, illegal or unenforceable in any respect, the
invalidity, illegality or unenforceability shall not affect any other provision of this contract, and
this contract shall remain in effect and be construed as if the invalid, illegal or unenforceable
provision had never been contained in the contract.
20.
MODIFICATION
No modification of the contract shall be binding on Contractor or City unless set out in writing
and signed by both parties.
21.
AUTHORIZATION
The undersigned officer and/or agents of the parties hereto are properly authorized officials and
have the necessary authority to execute this contract on behalf of the parties hereto, and each
party hereby certifies to the other that any necessary resolutions extending such authority have
been duly passed and are now in full force and effect.
Contract between the City Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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Page 12
� IN WITNESS WHEREOF, the parties hereto have executed this agreement in triplicate originals
in Fort Worth, Tarrant County, Texas.
�
City of Fort Worth
Materials Analytical Services, Inc.
,� _``
Charles Boswell, Assistant City Manager Name: ir �. Co�. �.e�
Title: �" � � �-.
Date: � % Date: �C-/.> = C% /
--,
Approved as to Form and Legality:
G
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City Attorney
Witness•
. �♦
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Gloria Pearson, City Secretary 7°
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eontract Authorization
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Date
Contract between the Cit}� Of Fort Worth, Texas, and
Materials Analytical Services, Inc. (MAS)
For laboratory services relating to Project XL Phase I
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Page 13
Meeting America's Needs for Experrenced and Comprehensive Environmental Management
Q�p
Section A
August 17, 2000
Revision 1
Page 1 of 30
QUALITY ASSURANCE PROJECT PLAN
AMBIENT AIR MONITORING FOR ASBESTOS
DURING DEMOLITION OF SUBSTANDARD STRUCTURES
IN CTTY OF FORT WORTH, TEXAS (PROJECT XL)
Prepared by:
Environmental Quality Management, Inc.
1310 Kemper Meadow Drive, Suite 100
Cincinnati, Ohio 45240
Prepared for:
City of Fort Worth
Department of Environmental Management
1000 Throckmorton Street
Fort Worth, Texas 76102-6311
Section
�
QAPP
Section A
June 2, 2000
Revision 0
Page 4 of 30
A2 TABLE OF CONTENTS
Pa�e
Project Management . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 30
Al Title and Approval Sheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ,
A2Table of Contents . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A3 Distribution List . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A4 Project Organization . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A.4.1 City of Fort Worth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A4.2 Industrial Hygiene & Safety Technology, Inc . . . . . . . . . . . . . . . .
A4.3 Microscopy Laboratory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A4.4 Demolition Contractor . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
AS Problem Definition/Background . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A5.1 Background ........................................
A5.2 Objectives . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A6 Project Description . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A.6.1 Technical Approach . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A.6.1.1 Demolition of Buildings . . . . . . . . . . . . . . . . . . . . . . .
A.6.1.2 Air Sampling During Demolition of Buildings ......
A.6.1.3 Air Sampling During Landfilling of Demolition Debris
A.6.2 Personnel ..........................................
A.6.3 Project Schedule . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A7 Quality Objectives and Criteria for Measurement Data . . . . . . . . . . . . . .
A7.1 Primary Project Objective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A7.2 Criteria for Acceptance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A7.3 Statistical Power . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A7.4 Precision and Accuracy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A7.5 Completeness .. .. .... . . . . . .. . . . . .. . . . . . .. . . .. . . . .. . .
A7.6 Representativeness ....... ........... ...... ...........
A7.7 Comparability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A7.8 Analytical Sensitivity . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A8 Special Training Requirements/Certification . . . . . . . . . . . . . . . . . . . . . .
A8.1 Field Personnel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A$.2 Laboratory Personnel . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A9 Documentation and Records . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A9.1 Field Operations Records . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
A.9.1.1 Air Sample Documentation . . . . . . . . . . . . . . . . . . . .
A.9.1.2 Meteorological Measurements . . . . . . . . . . . . . . . . . .
A.9.1.3 Photo Documentation . . . . . . . . . . . . . . . . . . . . . . . .
A9.2 Chain-of-Custody Records . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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A2 TABLE OF CONTENTS (continued)
Section
Q�P
Section A
August 17, 2000
Revision 1
Page 5 of 30
Pa�e
A9.3 Laboratory Records . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 of 30
� A.9.3.1 TEM Specimen Examination and Data Recording ... 29 of 30
A.9.3.2 Test Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29 of 30
B Measurement/Data Acquisition . . . . . . . a . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 28
Bl Sampling Design ...........................................
B.l.l Sampling Locations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.1.2 Air Sampling Strategy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.1.3 Particulate Loading Pilot Test . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.1.4 SoilSampling .......................................
B.1.5 Moisture Content of ACM . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.1.6 Water Used for Wetting Structure/Debris . . . . . . . . . . . . . . . . . .
B2 Sampling Methods Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.2.1 Air Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.2.2 Meteorological Monitoring . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.2.3 Soil Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.2.4 Water Sampling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B3 Sample Custody Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.3.1 Field Chain-of-Custody . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.3.2 Laboratory .........................................
B4 Analytical Methods Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.4.1 AirSamples ........................................
B.4.1.1 TEM Specimens Preparation . . . . . . . . . . . . . . . . . . .
B.4.1.2 Measurement Strategy . . . . . . . . . . . . . . . . . . . . . . . .
B.4.2 Soil Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.4.3 Moisture Content of ACM . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.4.4 Water Samples . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
BS Quality Control Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.5.1 Field Quality Control Checks . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.5.2 Analytical Quality Control Checks . . . . . . . . . . . . . . . . . . . . . . . .
B.5.2.1 Quality Control Check of Filter Media . . . . . . . . . . . .
B.5.2.2 Blank Contamination . . . . . . . . . . . . . . . . . . . . . . . . .
B.5.3 Analytical Precision and Accuracy . . . . . . . . . . . . . . . . . . . . . . . .
B.5.3.1 Replicate Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.5.3.2 Duplicate Analysis . . . . . . . . . . . . . . . . . . . . . . . . . . .
B.5.4 Verification Counting . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
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Section
A2 TABLE OF CONTENTS (continued)
QAPP
Section A
August 17, 2000
Revision 1
Page 6 of 30
Pa e
B6 Instrument/Equipment Testing, Inspection, and Maintenance
Requirements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22 of 28
B.6.1 Field Instrumentation/Equipment : . . . . . . . . . . . . . . . . . . . . . . . . 22 of 28
B.6.2 Laboratory Instrumentation/Equipment . . . . . . . . . . . . . . . . . . . . 22 of 28
B7 Instrument Calibration and Frequency . . . . . . . . . . . . . . . . . . . . . . . . . . . 23 of 28
B.7.1 Field Instrument/Equipment Calibration . . . . . . . . . . . . . . . . . . . 23 of 28
B.7.1.1 Air Sampling Pumps . . . . . . . . . . . . . . . . . . . . . . . . . 23 of 28
B.7.1.2 Airflow Calibration Procedure . . . . . . . . . . . . . . . . . . 23 of 28
B.7.2 Calibration of TEM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24 of 28
B8 Inspection/Acceptance Requirements for Supplies and Consumables .... 25 of 28
B.8.1 Air Sampling Filter Media . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25 of 28
B9 Data Acquisition Requirements (Non-direct Measurements) . . . . . . . . . . 26 of 28
B.9.1 Precision . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 of 28
B.9.2 Completeness . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 of 28
B.9.3 Accuracy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26 of 28
B 10 Data Management . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 of 28
B.10.1 Data Assessment . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 of 28
B.10.2 Data Management . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 of 28
B.10.3 Statistical Analysis . . . : . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 of 28
C Assessment/Oversight . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 4
Cl Assessments and Response Actions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 4
C.1.1 Performance and System Audits . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 4
C. l.l.l Field Audits . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 4
C.1.1.2 Laboratory Audit . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 of 4
C.1.2 Corrective Actions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 of 4
C2 Reports to Management . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 of 4
D Data Validation and Usability . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 of 3
D1 Data Review, Validation, and Verification Requirements . . . . . . . . . . . . . . 1 of 3
D2 Validation and Verification Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 of 3
D3 Reconciliation with Data Quality Objectives . . . . . . . . . . . . . . . . . . . . . . . . 3 of 3
EReferences ...................................................... lofl
Appendices
A
I:
C
�
E
Q�P
Section A
August 17, 2000
Revision 1
Page 7 of 30
A2 TABLE OF CONTENT5 (continued)
Comparison of the Asbestos NESHAP and the Fort Worth Method for the
Demolition of Substandard Structures
ISO Method 10312:1995. Ambient Air - Determination of Asbestos Fibres --
Direct-Transfer Transmission Electron Microscopy Method
Standard Operating Procedure for the Screening Analysis of Soil and Sediment
Samples for Asbestos Content
ASTM Standard Test Method D 4959-00. Determination of Water (Moisture)
Content of Soil by Direct Heating
EPA Method 100.1 Analytical Method for the Determination of Asbestos Fibers in
Water
QAPP
Section A
August 17, 2000
Revision 1
Page 8 of 30
FIGURES
Number Pa�e
A-1 Project Organization . . . . : . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 of 30
A-2 Project Schedule . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 19 of 30
A-3 Sampling Data Form . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27 of 30
A-4 Meteorological Measurement Log . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 of 30
B-1 Wind Rose for June, City of Forth Worth . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 of 28
B-2 Analytical Request and Chain-of-Custody Form . . . . . . . . . . . . . . . . . . . . . . . . 13 of 28
C-1 Corrective Action Report . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 of 4
�
QAPP
Section A
August 17, 2000
Revision 1
Page 9 of 30
TABLES
Number Pa�e
A-1 Effect of Number of Days of Demolition or Land Filling and Between-Sample
Variation on Statistical Power Calculations Assuming 5 Samples Upwind and
5 Samples Downwind from the Site . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 of 30
B-1 Air Sampling Strategy . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 3 of 28
B-2 Approximate Number of Grid Openings to Achieve Target Analytical Sensitivity
Based on Air Volume of 3000 Liters (Direct-Transfer Preparation of TEM
Specimens) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14 of 28
Q�p
Section A
June 2, 2000
Revision 0
Page 10 of 30
A3 DISTRIBUTION LIST
Brian Boerner, Environmental Management Division, City of Fort Worth, Texas
Kathryn A. Hansen, Environmental Management Division, City of Fort Worth, Texas
Michael A. Gange, Environmental Management Division, City of Fort Worth, Texas
Shirley Hoover, Environmental Management Division, City of Fort Worth, Texas
Mike Camp, Code Compliance, Department of City Services, City of Fort Worth, Texas
Brian Haggerty, City Manager's Office, City of Fort Worth, Texas
Charles Boswell, Assistant City Manager, City of Fort Worth, Texas
Adele Cardenas, U.S. EPA, Region VI
Todd Wingler, Texas Department of Health
Roger C. Wilmoth, National Risk Management Research Laboratory (NRMRL), U.S. EPA
Tracy K. Bramlett, Industrial Hygiene & Safety Technology, Inc.
Demolition Contractor (To Be Determined)
Microscopy Laboratory (To Be Determined)
QAPP
Section A
August 17, 2000
Revision 1
Page 11 of 30
A4 PROJECT ORGANIZATION
Environmental Quality Management, Inc. (EQ) has been contracted by the City of Fort
Worth, Texas, to design this Quality Assurance Project Plan (QAPP).1 The QAPP was prepared
to meet U.S. Environmental Protection Agency (EPA) requirements applying to projects that
include environmental measurements and is written in the format specified by EPA.�I� The project
organization chart showing the relationships and the lines of communication among project
participants is contained in Figure A-1.
A.4.1 City of Fort Worth
Brian Boerner, CHMIvI, will serve as the Program Manager. He has overall administrative
and technical responsibility for the project.
Kathryn A. Hansen, Esquire, will serve as the Project Manager. She has overall
administrative responsibility for the project. As such, she will resolve any administrative problems
that may occur and serve as the administrative contact with the Texas Department of Health, U.S.
EPA, Industrial Hygiene & Safety Technology, Microscopy Laboratory (To Be Determined),
Demolition Contractor (To Be Determined), and others.
Michael A. Gange will serve as the Technical Project Officer. He has overall technical
responsibility for the project. He will ensure that Industrial Hygiene & Safety Technology, Inc.
Mr. Kominsky (Vice President/Director Industrial Hygiene & Safety, EQ) prepared this QAPP. He has more
than 25 years of experience in the comprehensive practice of industrial hygiene and safety, of which 13 years
were with the National Ins[itute for Occupational Safety and Health (NIOSI�. Since 1988, he has designed,
implemented, and served as Project Manager/Principal Investigator on more than 15 asbestos research projects
for EPA's National Risk Management Research Laboratory (NRMRL). Five studies (4 EPA and 1 commercial
client) involved the determination of ambient concentrations of airborne asbestos in communities during
demolition of buildings containing asbestos-containing materials (AC1Vn and landfill of the resultant asbestos-
containing demolition debris, and other such projects involving fugitive emissions of asbestos. Mr. Kominsky
has a Master's of Science Degree in Industriat Hygiene (University of Pittsburgh, 1973) and Bachelor of
Science Degree in Chemical Engineering (University of Nebraska, 1971). He is a Certified Industrial
Hygienist by the American Boazd of Industrial Hygiene, a Certified Safety Professional by the American Board
of Certified Safety Professionals, and a Certified (Master Level) Hazardous Materials Manager by the Institute
of Hazardous Materials Management. He is an Adjunct Associate Professor in the Department of
Environmental Health at the University of Cincinnati. He has authored or co-authored more than 35 journal
articles (11 articles related to asbestos) regazding occupational, environmental, and pubiic heaith.
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Section A
June 2, 2000
Revision 0
Page 12 of 30
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Section A
August 17, 2000
Revision 1
Page 13 of 30
(IHST) implements the study in strict accordance with the QAPP and that the demolition
contractor (To Se Determined) follows the Fort Worth Method. As such, he will resolve any
technical difficulties with the contractors. He will also be responsible for resolving any technical
difficulties associated with the laboratory analysis of the samples, data analysis and management,
and preparation of the final project report.
A.4.2 Industrial Hygiene & Safety Technology, Inc.
Project Manager/Principal Investigator -- Mr. Tracy K. Bramlett (President, Industrial
Hygiene & Safety Technology, Inc.) will serve as the Project Manager/Principal Investigator and
maintain close communication with Ms. Hansen, Mr. Gange, and the demolition contractor. He
will ensure that all IHST project personnel fully understand and strictly adhere to the QAPP. All
IHST technical team members will be experienced professionals who possess the degree of
specialization and technical competence required to effectively perform the required work.
Mr. Bramlett will coordinate and supervise implementation of the QAPP including site
preparation, sample collection and documentation, data management and analysis, and preparation
of the project report. He will coordinate the sampling staff, ensure all equipment is calibrated
properly and measurements are made in accordance with the QAPP, review and validate field data
(e.g., sampling data logs), review sample custody and traceability records, and coordinate
submission of the samples to the laboratory. He will ensure that any problems or potential
deviations from the QAPP reported by any of the project staff are addressed immediately and
receive corrective and documented action, as necessary. Prior to effecting any deviations from
the approved QAPP, the potential deviation will be discussed with and approval to deviate will be
obtained from Mr. Gange.
A.4.3 Microscopy Laboratory
(To Be Determined) Laboratory will perform the transmission electron microscopy (TEM)
analysis of all samples collected.
A.4.4 Demolition Contractor
(To Be Determined) Demolition contractor will perform the demolition of the facilities.
AS PROBLEM DEFINITION/BACKGROUND
A.5.1 Background
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In order to demolish substandard structures2 that are not in danger of imminent collapse,
the City of Fort Worth currently follows the requirements established by Asbestos National
Emissions Standards for Hazardous Air Pollutants (NESHAP), 40 CFR §61.145. The City of
Fort Worth proposes an alternative method, hereinafter referred to as the Fort Worth Method, for
the demolition of "facilities" in lieu of the current Asbestos NESHAP requirements for the
demolition of substandard structures that are not in imminent danger of collapse. If left standing,
the substandard facilities will within several years become structurally unsound. Instead of
waiting for these buildings to reach such a structural state, the City proposes to be proactive and
demonstrate that facilities with regulated asbestos-containing material (RACM) left in-place is at
least as protective as demolition of buildings with the RACM removed.3 Based on the condition
of the RACM, demolishing facilities while in substandard condition most likely is more protective
of the public and environment than demolishing such facilities in danger of uruivnent danger of
collapse.
Due to the requirements of Asbestos NESHAP, the City has only demolished facilities
with RACM remaining in place when the facility is in unminent danger of collapse. Preliminary
data generated by both phase contrast microscopy (PCM) and transmission electron microscopy
(TEM) indicates that demolition of such structures using the Fort Worth Method does not
generate significant airborne fiber levels.�2�
The Fort Worth Method's one primary difference from the existing Asbestos NESHAP is
handling of the RACM. Prior to and during the course of demolition the facility is thoroughly
wetted and demolition proceeds in a manner that allows the non-asbestos-containing building
In the City of Fort Worth, a structure is considered substandard when it does not meet the
sEandards or specifications established in the City's Minimum Building Standards Code, Ordinance
No. 13743.
The City of Fort Worth proposes to demolish a facility without removal of RACM with certain
exceptions. Spray-applied fireproofing and large quantities of thermal system insulation (>260
linear feet) will be removed using full-containment abatement procedures.
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material (ACBM) to act as a banier between the ACBM and the environment. By proper
handling and wetting of the demolition debris, asbestos fiber release is controlled. A comparison
of the Asbestos NESHAP and the Fort Worth Method is contained in Appendix A.
The Fof-t Worth Method's primary goal is to protect the public and the environment from
the release of asbestos during the demolition of buildings containing in-place RACM. It's
secondary goal is to provide a alternative method for controlling asbestos that creates a cost
savings for municipalities performing demolition of nuisance buildings.
A.5.2 Objectives
The primary objectives of this project are:
2. Determine whether the airborne concentrations of asbestos upwind (comparative
environmental backgroasnd4) during demolition of buildings containing in-place
RACM are statistically significantly different than those concentrations downwind.
3. Determine whether the airborne concentrations of asbestos upwind (comparatzve
environmental backgrounc� during land filling of building demolition contauung
RACM are statistically significantly different than those concentrations downwind.
Environmental background is the airborne concentration of asbestos prevailing in this area that is
upgradient (upwind) from the facilities being demolished or the demolition debris being landfilled.
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August 17, 2000
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A6 PROJECT DESCRIPTION
A.6.1 Technical Approach
The project will be performed in two phases: Phase I and Phase II.
Phase I--Phase I will gather data on the Fort Worth Method's ability to prevent or
minimi�e the release of asbestos fibers during demolition of buildings that are either exempt from
the Asbestos NESHAP requirements (residential buildings that have four or fewer dwelling units)
or not subject to asbestos NESHAP.S The data from Phase I will be analyzed to determine
whether the Fort Worth Method is equivalent to the NESHAP method; i.e., the airborne
concentrations of asbestos upwind (comparative environmental backgroun� during demolition of
the facilities and land filling of the resultant demolition debris are not statistically significantly
different than the respective concentrations downwind. If the Phase I data supports a finding that
the Fort Wor�th Method is equivalent to the Asbestos NESHAP method, the City will proceed
with Phase II. If the methods are not found to be equivalent, the project may end with Phase I.
Phase II--Phase II will gather data on various buildings subject to the Asbestos NESHAP.
These buildings will include single or two-story commercial structures and/or multi-family
residential structures. The ACBM that are likely to be present include, but not limited to resilient
floor tile and mastic, Transite� panels, roofing materials, wallboard joint compound, wall and
ceiling texture, thermal system insulation, and miscellaneous other materials. Prior to demolition
of a structure, a thorough asbestos assessment of the facility will be conducted by a State of
Texas Department of Health licensed Asbestos Inspector. The assessment will identify the type,
quantity, location, and condition of ACBM. Prior to demolition of the.facility, spray-applied
fueproofing or large amounts of thermal system insulation will be removed by a State of Texas
Department of Health licensed Asbestos Abatement Contractor. The type and quantity of ACBM
remaining in the facility will be documented.
Asbestos NESHAP regulations must be followed for demolitions of facilities with at least 260
linear feet of RACM on pipes, 160 square feet of RACM on other facility components, or at least
35 cubic feet off facility components where the amount of RACM previously removed from pipes
and other facility components could not be measured before stripping.
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A.6.1.1 Demolition of Buildings
The buildings will be demolished using heavy equipment only. A typical building
demolition will include the following:
One or more bulldozers for single-story buildings, and a combination of bulldozers,
front-end loader, and track-hoes for multi-story buildings.
Thoroughly and adequately wetting the structure using fire hydrant water applied
with a variable rate 11-G (11 gpm) or 30-G (30 gpm) nozzle prior to, during
demolition, and during debris loading. A water meter (or equivalent device) will
be installed at the water hydrant to measure the volume of water used during
demolition of the structure. The water will be delivered as a mist or concentrated
stream. Direct high-pressure water impact of ACM will be prohibited.6 The
demolition debris will be adequately wet at all times and kept wet during handling
loading into containers for transport to a licensed disposal site.
Collapsing structures inward (majority of the walls and interior components will be
leveled on top of the building foundation) and loading debris prior to removal of
the concrete slab, if present.
• Segregation of demolition debris to the extent feasible to reduce the amount of
contaminated debris that will be treated as asbestos-contaminated waste. Debris
not contaminated by the ACBM will be treated as construction debris, while all
other materials will be treated as asbestos-contaminated waste. The RACM debris
will be transported to a licensed disposal site in lined and covered containers.
Segregation of the waste will be the responsibility of an onsite Asbestos NESHAP
trained individual.
Grading of the site for future use.
A.6.1.2 Air 5ampling During Demolition of Buildings
The first study objective (see Section A.5.2) will be addressed by collecting ambient air
samples at ten locations for three to five consecutive days during demolition of a facility. Five
sampling locations will be located both upwind (comparative environmental background level of
asbestos) and downwind of the demolition area. Meteorological conditions (such as wind
Although experience demonstrates that building demolition projects typically have a minimal to
moderate amount of water runoff depending on the site locations and site conditions, the City will
utilize Best Management Practices to control water runoff and collect storm water on the project
site. Storm drain inlet protection will be used in conjunction with on-site controls (such as natural
and marunade drainage channels), as necessary.
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August 17, 2000
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direction and wind speed) will be determined explicitly to establish and ensure true upwind and
downwind conditions during sampling (see Section B.1.1).
A.61.3 Air Sampling During Land Filling of Demolition Debris
The second study objective (see Section A.5.2) will be addressed by collecting ambient air
samples at ten locations for two to three consecutive days during land filling of the demolition
debris from each facility. The projected monitoring of two to three consecutive days during
landfilling of the demolition debris is based on the amount of time required to landfill the debris
from a given site. Five sampling locations will be located both upwind (comparative
environmental background level of asbestos) and downwind of the land fill. Meteorological
conditions (such as wind direction and wind speed) will be determined explicitly to establish and
ensure true upwind and downwind conditions during sampling (see Section B. L 1).
A.6.2 Personnel
The environmental measurements (field samples and meteorological measurements) will be
made by and at the direction of an ABIH-Certified Industrial Hygienist, Tracy Bramlett. He has
more than 23 years of experience in the comprehensive practice of industrial hygiene with
approxirnately 21 years of asbestos monitoring experience including ambient air monitoring for
asbestos and licensed appropriately by the State of Texas as an air monitoring technician. Other
field personnel will include industrial hygienists experienced in asbestos ambient air monitoring
and related measurements.
A.6.3 Project Schedule
The tentative project schedule is presented in Figure A-2. The major activities are listed
sequentially, and the expected duration of each activity is presented.
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August 17, 2000
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QAPP
Section A
June 2, 2000
Revision 0
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A7 QUALITY OBJECTIVES AND CRITERIA FOR MEASUREMENT DATA
The overall quality assurance objective of this project is to implement procedures for field
sampling, chain-of-custody, laboratory analysis, and reporting that will provide data to satisfy the
Primary Project Objective (i.e., the objective that will lead to the development of scientifically
valid conclusions in the final report). Specific procedures for sampling, chain-of-custody,
laboratory analysis, field and laboratory audits, preventive maintenance of field equipment, and
corrective actions are described in other sections of this QAPP.
A.7.1 Primary Project Objective
The primary project objective is to determine the concentrations of airborne asbestos
upwind (comparative environmental backgrounc� and those concentrations that are present
downwind of the demolition site and the demolition debris land fill.
A.7.3 Criteria for Acceptance
The criteria for acceptance of equivalency of the Fort Worth Method to the e�sting
Asbestos NESHAPS Method will be achieved by meeting either of the following:
There is not a statistically signif'icant difference in the airborne concentrations of
asbestos upwind during demolition of buildings containing in-place RACM or
upwind during land filling of this building demolition debris compared to those
concentrations measured downwind of the respective sites. The statistical
comparisons will be made at the 0.05 level of significance.
2. The downwind sample average is less than 70 asbestos structures per square
milluneter; the AHERA (40 CFR 763) clearance criterion.
A.7.3 Statistical Power
The study is designed to detect a 5-fold difference in average concentration (e.g., a 5-fold
difference between the airborne asbestos concentrations upwind and downwind from the
demolition or land filling sites) with high probability if such a difference actually e�sts. A false-
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August 1'7, 2000
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positive error rate' of 5 percent will be achieved by employing a statistical significance level of
0.05 (i.e., a confidence level of 95%). A false-positive error occurs if we determine that a
significant difference between the upwind and downwind airborne asbestos concentrations exists
when, in fact, it did not. The statistical power of the upwind-downwind comparison will depend
on the number of days required to demolish the building or landfill the demolition debris (Table
A-1). Assuming three days of demolition per facility and ten air samples collected each day (five
locations upwind, five location downwind), a simple parametric comparison (e.g., t-test) between
the upwind and downwind locations will have a false-negative error rate8 of approxirnately 10%
for a 5-fold difference between mean concentrations and approximately 1% for a 10-fold
Table A-1. Effect of Number of Days of Demolition or Land Filling and
Between-Sampte Variation on Statistical Power Calculations Assuming 5 Samples
Upwind and 5 Samples Downwind from the Site
Number of Coefficient of Variation, %
Days Difference 100 150 200 250
2-fold 0.42 0.28 0.16 0.17
2 days
5-fold 0.98 0.85 0.78 0.68
10-fold >0.99 0.99 0.95 0.93
2-fold 0.62 0.41 0.26 0.26
3 days
5-fold 0.99 0.98 0.95 0.89
10-fold >0.99 >0.99 0.99 0.99
2-fold 0.74 0.52 0.41 0.33
4 days
5-fold >0.99 0.99 0.97 0.95
10-fold >0.99 >0.99 >0.99 >0.99
A false-positive error rate is the probability of rejecting the null hypothesis when the null
hypothesis is actually true.
A false-negative error rate is the probability of accepting the null hypothesis when the null
hypothesis is actually false.
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difference (or equivalently, there is a probability of 0.90 of detecting a 5-fold difference and a
probability of approximately 0.99 of detecting a 10-fold difference between mean concentrations
at the upwind and downwind locations). A false-negative error occurs if we determine that no
difference in airborne asbestos concentration e}cists, when in fact the concentrations did differ.
The probability estima.tes assume a between-sample coefficient of variation (CV) of 250
percent, which is environmentally conservative, and were estimated by Monte Carlo simulation
using log-normal random variables. Under more optimistic assumptions regarding the variability
of ineasurements (e.g., a between-sample CV of 150 percent), the probability of detecting a 5-fold
difference between the mean airborne asbestos concentrations upwind and downwind using a
simple comparison (e.g., t-test) would be increased to approximately 98 percent.
A.7.4 Precision and Accuracy
The estimated false-negative error rates assume a between-sample coefficient of variation
of 250 percent. This assumption is reasonable and environmentally conservative, and is based on
measured concentrations of asbestos in ambient air at other locations.�3�5� The between-sample
coefficient of variation is influenced by heterogeneity in the air being measured as well as
sampling and laboratory performance used to collect and analyze the samples, respectively. If the
overall target precision is not achieved, the false-negative error rate will increase. The data will
ultimately be analyzed using analysis of variance (ANOVA) methods, rather than simple t-tests.
The ANOVA methods will provide additional statistical power in detecting differences between
sampling locations and, consequently, the false-negative error rates are expected to be lower than
those stated in Section A.7.2.
In addition, duplicate field samples will be collected during each day of sampling and
compared to results from co-located samples to evaluate the precision as well as serve as a
combined check on the sample collection and analysis procedures.
A.7.5 Completeness
An overall measure of completeness will be given by the percentage of samples specified
in the sampling design that yield usable "valid" data. Although every effort will be made to collect
and analyze all of the samples specified in the sample design, the sample design is robust to
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sample loss. The loss of a small number of samples, provided that they are not concentrated at a
single sampling site, will likely have little effect on the false-negative error rate. The project goal
is to collect at least 95 percent of the samples specified in the sample design.
A.7.6 Representativeness
The sampling locations, sampling periods, and sample durations have been selected to
assure reasonable representativeness. The five upwind sampling locations will be selected as
locations that can be reasonably viewed as representing comparative environmental background
conditions that are unaffected or influenced by activities of the demolition and land filling
operations. The five downwind sampling locations will be selected as representative sites that
would be influenced by potentially significant releases of asbestos from the demolition or
demolition debris land filling operations. Samples will be collected each day (meteorological
conditions permitting) of the demolition or land filling of demolition debris to provide estimates
that are representative of the normal meteorological conditions in the area and to account for the
potential day-to-day variability associated with ambient levels of airborne asbestos.
A.7.7 Comparability
Data collection using standard sampling and analytical methods (e.g., ISO Method
10312:1995, counting structures longer than and shorter than 5�cm in length, and PCM
equivalent fibers9) maximizes fhe comparability of the results with both past sampling results (if
such e�st) and future sampling results.
A.7.8 Analytical Sensitivity
We have selected an analytical sensitivity (i.e., the concentration corresponding to the
finding of one asbestos structure during a sample analysis) that corresponds to asbestos
concentrations representative of general background concentrations in many areas of the United
States. Data presented in Berman and Chatfield�6� indicate that an analytical sensitivity of 0.0005
A PCM (phase contrast microscopy) equivalent fiber is a fiber with an aspect ratio greater than or
equal to 3:1, longer than 5�cm, and which has a diameter between 0.2 ,um and 3.0 �cm.
Q�P
Section A
June 2, 2000
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structure/cubic centimeters of air (s/cm3) is likely sufficient to detect environmental background
concentrations in many areas of the United States. The analytical sensitivity selected for the
ambient air monitoring is 0.0005 s/cm3 for all asbestos structures (ininunum length of 0.5 �cm) and
0.0001 s/cm3 for asbestos structures longer than 5,um (all widths). See Section B.4 "Analytical
Method Requirements." Thus, the number of ineasurements (upwind and downwind) in which
asbestos structures is not observed or detected among the data collected should be minimal.
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A8 SPECIAL TRAINING REQUIl2EMENTS/CERTIFICATION
A.8.1 Field Personnel
The sampling (including equipment calibration, sample collection, and documentation) will
be performed by and/or at the direction of an ABIH-Certified Industrial Hygienist (T. Bramlett).
He has more than 23 years of experience in the comprehensive practice of industrial hygiene with
appro�mately 21 years of asbestos monitoring experience including ambient air monitoring for
asbestos. Other field personnel will include industrial hygienists experienced in asbestos ambient
air monitoring and related measurements.
A.8.2 Laboratory Personnel
(To Be Determined) Laboratory is accredited by the National Institute of Standards and
Technology (1VIST) National Voluntary Laboratory Accreditation Program (NVLAP) to perform
Airborne Asbestos Fiber Analysis. (To Be Determined ) laboratory's NVLAP Laboratory Code
No. is XXX (effective through X��X, 2000).
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June 2, 2000
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A9 DOCUMENTATION AND RECORDS
A.9.1 Field Operations Records
A.9.1.1 Air Sample Documentation
The following information will be recarded on a Sampling Data Form (Figure A-3):
• Names of persons collecting the sample
• Date of record
• S ampling site
• Location of sample
• Type of sample (e.g., high volume, duplicate, field blank)
• Unique sample number (identifies site, sample type, date, and sequence number)
•� Rotameter number and air flow reading (start/stop)
• Linear regression equation and correlation coefficient for the calibrated rotameter
• Sample time (start/stop)
• Relevant notes describing site observations such as, but not limited to site
conditions, demolition method/techniques and equipment, water application nozzle
and hose diameter, water application technique (spray or concentrated stream) and
approxirriate amount of time (e.g., hours) for each will be recorded on the reverse
side of the Sampling Data Form (and on supplemental pages, as necessary).
The upwind and downwind air sampling locations will be identified on a drawing of the
demolition site or land fill area.
At the end of each day, the samples which were collected and the corresponding data
forms/drawings will be submitted to Tracy Bramlett. He will verify the data/information for
completeness; any corrections will be noted and initialed on the form.
A.9.1.2 Meteorological Measurements
Meteorological measurements (wind direction, wind speed, relative humidity, and
temperature) will be recorded on a Meteorologic Data Measurement Log (Figure A-4).
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Section A
June 2, 2000
Revision 0
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Section A
June 2, 2000
Revision 0
Page 28 of 30
�'��TWo�
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Measurement Log
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Investigawr.
TIME �ND WIND BAROME'T2IC TEMPERAT(JRE, REIAT'lyg
SPEED, MPH DIREC!'ION PRFSSURE, In. Hg °F HUMIDTIY, %
Figure A-4. Meteorological Measurement Log.
QAPP
Section A
August 17, 2000
Revision 1
Page 29 of 30
A.9.1.3 Photo Documentation
A 35-mm photograph or digitized image will be taken of every sampling site. This will
include the sampling station, visual debris on or in the soil. A 5-in. by 7-in. index card listing the
sample number will be photographed to identify the sample and location. Other photographs or
digitized images will be taken as necessary to thoroughly document the site conditions (such as
"visible emissions," if such occurs) and activities. In addition, a camcorder will be used to
videotape the demolition and demolition debris land filling operations.
A.9.2 Chain-of-Custody Records
Standard EQ sample traceability procedures described in Section B3 "Sample Custody
Requirements" will be used to ensure sample traceability.
A.9.3 Laboratory Records
A.9.3.1 TEM Specimen Examination and Data Recording
Structure counting data shall be recorded on farms equivalent to the example shown in
ISO 10312:1995 contained in Append� B.
A.9.3.2 Test Report
The test report shall contain items (a) to (p) as specified in Section 11 "Test Report" of
ISO 10312:1995. In addition, the files containing the raw data, in Microsoft Excel format, shall
be submitted. The format of these files shall be as directed by the project manager, but shall
contain the following items:
l. Laboratory Sample Number
2. Project Sampie Number
(4 Blank Lines For Project Manager to Insert Locations and Sampling Details)
3. Date of Analysis
4. Air Volume
5. Active Area of Sample Filter
6. Counting Magnification
7. Mean Grid Opening Dimension in mm
8. Number of Grid Openings Examined
9. Number of Primary Structures Detected
QAPP
Section A
August 17, 2000
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10. One line of data for each structure, containing the following information as
indicated in Figure 7`Bxample of Format for Reporting Structure Counting Data"
of IS O 10312:1995, with the exception that the lengths and widths are to be
reported in millimeters as observed on the screen at the counting magnification:
• Grid Opening Number
• Grid Identification
• Grid Opening Identification/Address
• Structure or Sub-structure Number
• Asbestos Type (Chrysotile or Amphibole)
• Morphological Type of Structure
• Length of Structure in millimeters in 1 mm increments (e.g., 32)
• Width of Structure in miltimeters in 0.2 mm increments (e.g., 3.2)
• Any Other Comments Concerning Structure (e.g., partly obscured by grid
bar)
.�1
B MEASUREMENT/DATA ACQUISITION
B1 SAMPLING DESIGN
B.l.l Sampling Locations
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Section B
A.ugust 17, 2000
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Ambient air samples will be collected at 10 sampling locations each day of the demolition
and each day that the respective demolition debris is placed in the landiill. Five sampling locations
will be located both upwind (comparative environmental background level of asbestos) and
downwind of the land fill. A wind rose for five years (1988 through 1992) of June winds (0000 to
2300 hours) is presented in Figure B-1. When considering a wind fetch of 135 degrees (from the
southeast) through 202.5 degrees (from the south southwest), about 54 percent of the total hours
of wind data over five months of June winds were from this 67.5 degree sector. Should the wind
direction change outside of this 67 degree sector for more than a 60-minute period, the sampling
will be terminated.
B.1.2 Air Sampling Strategy
The air sampling strategy is summarized in Table B-1. Air sampling will be conducted for
3-5 and 2-3 consecutive days during demolition and land filling of the demolition debris,
respectively, if acceptable meteorological conditions e�st. Acceptable meteorologic conditions
include consistent upwind conditions for the environmental comparative background samples and
no rain.
Two sets of air samples will be collected at each sampling locations: a high-volume and a
low-volume sample. A high-volume sample will be collected to achieve the target air volume
(such as 3,000 liters) over the period of the demolition or land filling activities, and a second
sample (low-volume) will be collected to achieve one-half of the target air volume over the same
period. The second sample will be collected in the event that the first sample with the higher air
volume is overloaded with particulate,'° which would preclude transmission electron microscopy
lo The direct transfer analytical method (ISO 10312:1995) should not be used if the general
particulate loading of the sample collection filter exceeds approximately 10 �cg/cm2 of filter
surface, which corresponds to approximately 10 percent coverage of the collection filter by
particulate.
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August 17, 2000
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WIND ROSE PLOT
STATION #03927 - DALLAS/FORT WORTH/REGIONAL AR, TX
. ' NORTH � - ,
' - ` - . • �. 25%
,� ' ' �,20% .
' , . � � i5ib �, �,
• ,� ,� .� � t0io `, , ,
� � � , . 5/ � . � �
� WEST � � -, - • - - , . _ . . , • - , • - • - � - - - • �- - - - - , - - - -�
, , , , � , , EAST�
� 'SOUTH .
Wind Speed (Knols) MODEIER
G.Schewe
>21
DISPIAY
17-21
Wind Speed
it-16
�. �� AVG. WIND SPEED
a - s $•63 Knots
7•3
ORIENTATION
Direction
(blowing from}
DATE
4/8/00
UNIT
Knots
CALM WINDS
6.17%
PLOT YEAR-DATE-TIME
88 89 90 91 92
June 1 - June 30
Midnight -11 PM
COMPANYNAME
EQ
COMMENTS
PROJECT/PLOT NO.
Figure B-l. Wind Rose for June, City of Fort Worth.
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August 17, 2000
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TABLE B-1. AIR SAMPLING STRATEGY
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TABLE B-1(continued)
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TABLE B-1(continued)
(TEM) analysis using the direct transfer method of sample preparation; otherwise, the second
sample will be archived.
Duplicate "Co-Located" Samples -- Two high-volume duplicate air samples (one upwind,
one downwind) will be collected during each day of sampling. Each high-volume duplicate
sample will be analyzed.
Field Blanks -- Two open and two closed field blanks will be collected each day of
sampling. Open field blanks are filter cassettes, that have been transported to the sampling site,
opened for a short-time (< 30 seconds) without any air having passed through the filter, and then
sent to the laboratory. Closed field blanks are filter cassettes that have been transported to the
sampling site and then sent to the laboratory without being opened. The two open field blanks
will be analyzed and the closed field blanks will be archived. The closed field blanks will only be
analyzed if the open field blanks show asbestos contamination.
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Section B
August 17, 2000
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B.1.3 Particulate Loading Pilot Test
One of the biggest difficulties associated with ambient air monitoring is the paramount
requirement to achieve adequate analytical sensitivity with constraints placed on sampling and
analysis. Briefly, analytical sensitivity is a function of the volume of air passed through a filter, the
concentration or dilution attendant to filter preparation, and the area of the filter scanned for
analysis. The volume of air that can be collected is primarily limited by the tolerable loading of
total particulate collected per unit area of filter before the sample is unsuitable for analysis by the
direct-transfer TEM method because of overloading.
A pilot sampling test will be performed to estimate the maximum sample air volume (with
an acceptable particulate loading) to achieve the specified analytical sensitivity by counting the
fewest grid openings. The pilot test will consist of collecting five sets of ambient air samples over
an approxunately 6-hour period to achieve the following total air volumes: 3500, 3000, 2500,
2000, and 1500 liters. The sample will be examined by an experienced electron microscopist to
determine if the particulate loading of the sample exceeds the criterion specified in ISO Method
10312:1995.
B.1.4 Soil Sampling
The Asbestos content of the soil will be determined both before and after demolition of the
structure. Two samples will be collected from each side of the structure yielding a total of eight
samples before and eight samples after demolition of each building. The sampling locations will
be randomly selected from a 5-ft by 5-ft grid system created around the building. The samples
will be collected from the center of each selected grid square. The grid system will be prepared
on a plot plan or similar drawing of the property. If two samples cannot be obtained from each
side of the structure, samples will be obtained from the remaining sides to yield a total of eight
samples.
Before and after samples will be collected from the same approximate locations. The
sampling locations will be marked on the site drawing. In addition, a marker (e.g., fluorescent
orange painted meter pipe) will driven into the ground to mark the location of the soil sample
collected before demolition of the structure.
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B.1.5 Moisture Content of ACM
To determine the effectiveness of the water application process on wetting the asbestos-
containing materials in the structure, 10 representative bulk samples of the asbestos-containing
materials will be collected. The ten bulk samples will be collected of the asbestos-containing
materials after the structure has been demolished. The water (moisture) content of each sample
will be determined. A water meter (or an equivalent device) will be installed at the hydrant to
measure the volume of water used during demolition of the structure.
B.1.6 Water Used for Wetting Structure/Debris
The water used to wet the structure and resultant demolition debris will be sampled to
determine the asbestos content. That is, each sample will be analyzed for asbestos fibers greater
than 0.5 /�m in length; the AHERA (40 CFR 763) definition.
B2 SAMPLING METHODS REQUIREMENTS
B.2.1 Air Sampling
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Section B
August 17, 2000
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The samples will be collected on open-face, 25-mm-diameter 0.45-,um pore size mixed
cellulose ester (MCE) filters with a 5-µm pore size MCE diffusing filter and cellulose support pad
contained in a three-piece cassette with a 50-mm non-conductive cowl. This design of cassette
has a longer cowl than the design specified in ISO 10312:1995, but it has been in general use for
some years for ambient and indoor air sampling. Disposable filter cassettes with shorter
conductive cowls, loaded with the appropriate combination of filter media of known and
consistent origin, do not appear to be generally available. The filter cassettes will be positioned
on tripods approximately 5 feet above the ground or at the elevation best suited to achieve an
unobstructed representative air sample.
The filter assembly will be attached with fle�ble Tygon� tubing (or an equivalent material)
to an electric-powered (110 VAC) 1/6-horsepower vacuum pump operating at an airflow rate of
appro�mately 6.3 liters per minute to achieve the target air volume of 3,000 liters over an eight
hours. Each pump will be equipped with a flow control regulator to maintain the initial flow rate
of within +/- 10% throughout the sampling period. Although the pilot test described in Section
B.1.3 will determine the optimal target air volume, it is anticipated that the air volume for each
sample will be appro�mately 3,000 liters. If 110 VAC line power is not available, portable
gasoline-powered generators will be used to power the sampling pumps.
B.2.2 Meteorological Monitoring
Meteorological data will be collected to support the determination of valid sampling .
periods. Data validity will be based primarily on wind directions which lend themselves to
maintaining the monitors in an upwind and downwind orientation from the demolition site or
landfill.
A combination of nearby National Weather Service (NWS) 12-hour wind direction
forecasts, on-site meteorological data collection using continuous monitoring, and individual
monitoring site qualitative collection data will be used to determine several monitoring objectives.
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These objectives include the following:
l. Forecasting a valid upcoming sampling day.
2. Providing ongoing data collection to support final data validation.
3. Checking ongoing data throughout a sampling period overall and at specific
sampling locations.
The primary specification for objectively deternuning monitored data validity and the
determination of go/no-go on each sample day will be based on two meteorological conditions.
The first is rainfall. If the NWS forecasts greater than a trace (0.1 inch) amount of rainfall for the
upcoming 24-hour sampling period, the sampling day will be canceled. The second criterion for
evaluating data validity and go/no-go situations will be wind direction. For June all winds coming
from the 135 ° through 202.5 ° wind sectors (southeast through south through southwest) will be
selected as valid wind flows. Wind directions prior to each sampling day will be estimated
through NWS forecasts. Sampling will proceed whenever winds are generally forecast for the
southwest through northeast (clockwise through northwest).
Prior to the start of each day's field activities, the NWS at the Dallas-Fort Worth
Inte�national Airport will be contacted to obtain 12-24 hour wind direction and precipitation
forecasts. If the conditions are acceptable, the sampling day will proceed.
For ongoing field activities after the decision has been made to proceed, both continuously
recorded wind speed and direction will be collected as well as predetermined time spot checks at
each monitoring site. A meteorological station will be installed at both the demolition site and
landfill. Each station will consist of a Met One Instruments, Inc. Automet meteorological data
system. It will include continuous wind speed and direction sampling and data logging over the
duration of the sampling period. All data will be collected and archived in the data logger which
can be checked on a routine basis with direct readout as well as downloading to a personal
computer whereby related software will be used to assess hourly, daily, and period archived data.
The wind station will be tripod mounted in an appropriate location away from all obstructions.
The Automet sensors and their associated sensitivity are approved for use in Prevention of
Significant Deterioration Monitoring Projects under U.S. EPA and will provide significant detail
to the wind direction tabulations.
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August 17, 2000
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The meteorological station operator will also collect wind speed data using a hand-held
Dwyer wind speed meter and wind direction data using a dark-colored ribbon attached to the top
of a 6-foot wooden stick. Readings will be taken once every 30 minutes over a duration of about
1 minute using the 1-minute averages to represent the period. A logbook will be kept which notes
these wind directions and wind speeds as well as those noted on the Automet system data logger
for the same time period.
The manual measurement (wind speed and wind direction) ma.de at meteorological station
will also be ma.de at one other upwind and two downwind sampling locations. They will also be
at the same specified 1 minute of each 30-minute time period during sample collection. The wind
speed and wind direction will be noted in a logbook at each sampling location.
Consistency between observations will be promoted through the use of identical hand-held
instruments as well as previous training on proper observation techniques by each site attendant.
If during sampling the wind directions fall outside of the acceptable range at the main
meteorological station for 30 or more concurrent minutes, sampling activities will cease for the
day. The samples will be archived or voided.
B.2.3 Soil Sampling
The soil samples will be collected using a clean metal scooping tool (e.g., a garden
trowel). The samples will be collected from the center of the grid square (see Section B.1.4). To
the extent feasible, each sample will represent the top 1 to 1'h inches of soil from a 4 inch by 4
inch area. The area will be delineated using a metal template with a 1'fi inch vertical flange of
sufficient strength to allow the flange to be pushed into the soil. The template will be constructed
of galvanized sheet metal.
B.2.4 Water Sampling
One water sample will be collected from each water source (i.e., water hydrant) that will
be used to wet the structure and resultant demolition debris. The sample container will be an
unused, precleaned, screw-capped bottle of glass or low density (conventional) polyethylene and
capable of holding at least 1 liter. (Ideally, water samples are best collected in glass bottles.)
Prior to collecting the sample, allow the water from the water source to run to waste for a
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sufficiently long period to ensure that the sample collected is representative of fresh water. As an
additional precaution against contamination, each bottle should be rinsed several times in the
source water being sampled.
Two separate samples of approximately 800 milliliters each will be collected. An air space
will be left in the bottle to allow efficient redispersal of settled material before analysis. The
second bottle will be stored for analysis if confirmation of the results obtained from the analysis of
the first bottle is required.
The samples will be transported to the analytical laboratory and filtered by the laboratory
within 48 hours of each sample collection. No preservatives or acids will be added. At all times
after collection, the samples will be stored in the dark and refrigerated at about 5° C(41 ° F) in
order to minimi�.e bacterial and algal growth. The samples will not be allowed to freeze, since the
effects on asbestos fiber dispersions are not known.
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Section B
August 17, 2000
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B3 SAMPLE CUSTODY REQUIREMENTS
Chain-of-custody procedures emphasize careful documentation of constant secure custody
of samples during field, transport, and analytical stages of environmental measurement projects.
The sample custodian responsible for the proper chain-of-custody during this project is:
Tracy Bramlett, CIH, CSP
Industrial Hygiene & Safety Technology, Inc.
2235 Keller Way
Carrollton, Texas 75006
Phone: 972.478.7415; fax: 972.478.7615
B.3.1 Field Chain-of -Custody
Each sample will have a unique project identification number. This identification number
will be recorded on a Sampling Data Form (Figure A-3) along with the other information
specified on the form. After the labeled sample cassettes are recovered from the sampling trains,
the sample custodian will complete an Analytical Request and Cha.in-of-C�istody Form (Figure B-
2). This form will accompany the samples, and each person having custody of the samples will
note receipt of the same and complete an appropriate section of the form. Samples will be sent to
Laboratory (To Be Determined) via Federal Express Standard Overnight Service.
B3.2 Microscopy Laboratory
The laboratory's sample clerk will examine the shipping container and each filter cassette
to verify sample numbers and check for any evidence of damage or tampering, note any changes
or indication of tampering on the accompanying chain-of-custody form, and then forward the
form to Tracy Bramlett. The sample clerk will log in all samples and assign a unique sample
identification number to each sample and sample set.
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August 17, 2000
Revision 1
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B4 ANALYTICAL METHOD REQUIIZEMENT5
B.4.1 Air Samples
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Section B
August 17, 2000
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The 0.45-�cm pore size m�ed-cellulose ester (MCE) filters will be prepared and analyzed
using International Organization of Standardization (ISO) Method 10312:1995 (15L Ed.),
"Ambient Air - Determination of Asbestos Fibres - Direct-Transfer Transmission Electron
Microscopy Method." A copy of the method is contained in Appendix B.
The principal objective of these analyses is to provide air concentration data of sufficient
quality to support the development of conclusions regarding the effective of the Fort Wor•th
Method to control the release of asbestos fibers during the demolition of substandard structures
containing RACM
B.4.1.1 TEM Specimens Preparation
TEM specimens shall be prepared from the ambient air filters using the dimethylformamide
(DMF) collapsing procedure of ISO 10312:1995, as specified for cellulose ester filters. DMF
shall be used as the solvent for dissolution of the filter in the 7affe washer. For each filter, a
minimum of four TEM specimen grids shall be prepared from a one quarter sector of the filter,
using 200 mesh indexed copper grids. The remaining part of the filter shall be archived until
further notice, in the ,original cassette in clean and legally secure storage, to be possibly selected
for quality assurance analyses.
B.4.1.2 Measurement Strategy
The minimum aspect ratio for the analyses shall be 3:1, as permitted by ISO
10312:1995.
2. The analyses shall be performed by a two-stage examination of the TEM
specimens, as indicated in ISO 10312:1995, in order to provide data of sufficient
precision for each of the structure size ranges of interest. The size ranges of
structures that shall be evaluated, and target analytical sensitivities, for the
anticipated collected air volume of 3000 liters, will be as shown in Table B-2.
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August 17, 2000
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Table B-2. Appro�mate Number of Grid Openings to Achieve
Target Analytical Sensitivity Based on Air Volume of 3000 Liters
(Direct-Transfer Preparation of TEM 5pecimens)
Appro�mate
Number of
Target Appro�mate Appro�mate 0.01 mm2
Analytical Magnification Area Grid
Sensitivity for Examined Openings
Size Range s/cc Examination mm2 Required
All Structures
(Minimum Length of 0.0005 20000 0.256 26
0.5 pm)
Longer than 5 pm, 0.0001 10000 0.256 26
(All Widths)
3. The stopping point in the analysis for each of the examinations defined in 2 shall be
100 primary asbestos structures, or after the completion of the examination of the
grid opening during which the target analytical sensitivity is achieved. A minimum
of 4 grid openings shall be examined, in accordance with the specifications of
ISO 10312:1995.
4. The structure counting data shall be distributed approximately equally among a
minimum of 3 specimen grids, prepared from different parts of the filter sector.
5. The TEM specimen examinations at approximately 20,000 and 10,000 shall be
performed as independent measurements.
6. Measurement of fiber dimensions is extremely important for accurate
determination of aspect ratios. Lengths and widths of fibers shall be recorded in
millimeters as measured on the fluorescent screen. Where the observed width of a
fiber is lower than approximately 5 mm on the screen at either of the two
magnifications used for the 'TEM specimen examinations, the measurement errors
may seriously compromise the accuracy of the calculated aspect ratio.
Accordingly, in this situation, the magnification shall be increased by a factor of
approximately five times to obtain an accurate measurement of the width. For
example, the width of a 1 mm wide fiber cannot be accurately estimated on the
screen. A five-fold increase in the magnification increases the dimension to 5 mm,
which can be estimated with sufficient accuracy for the purpose of this project.
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August 17, 2000
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B.4.2 Soil Samples
The asbestos content of the soil will be determined using a method developed by U.S.
EPA, Region I: Standard Oper•ating Procedur•e for the Screening Analysis of Soil and Sediment
Samples for Asbestos Content (SOP:EIA-INGABED2-SOP, January 11, 1999). To more
accurately quantify the amount of asbestos in the soil samples, the samples will be prepared using
the procedure specified in the addendum to the method. A copy of the method is contained in
Appendix C.
B.4.3 Moisture Content of ACM
The water (moisture) content of the bulk samples of asbestos-containing materials (ACM)
will be determined in accordance with ASTM Standard Test Method D 4959-00 "Determination
of Water (Moisture) Content of Soil by Direct Heating." The method will be modified (as
necessary) to accommodate the ACM bulk samples. A copy of the method is contained in
Append� D.
B.4.4 Water Samples
The asbestos content of the water used to wet the structure and resultant demolition
debris will be determined using EPA Method 100.1 "Analytical Method Determination of
Asbestos in Water." A copy of the method is contained in Appendix E.
Measurement of fiber dimensions is important. Dimension of fibers is recorded as length
and width if greater than 0.5 ,um in length. Reference EPA Method 100.1 for counting and sizing
rules for bundles, fiber aggregates, etc. The analysis may be stopped after 100 fibers have been
counted or 20 grid openings have been examined. The sample grid will be examined in a
transmissions electron microscope (TEM) at a magnification of about 20,000.
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B5 QUALITY CONTROL REQUIREMENTS
The overall quality assurance objective is to provide defensible data of known quality
meeting quality assurance objectives. To that end, procedures are developed and implemented for
field sampling, chain-of-custody, laboratory analysis, reporting, and audits that will provide results
which are scientifically valid and legally defensible in a court of law.
B.5.1 Field Quality Control Checks
Quality control checks for the field sampling aspects of this project will include, but not be
limited to, the following:
• Use of standardized forms (e.g., Figures A-3, A-4, B-2) to ensure completeness,
traceability, and comparability of the data and samples collected.
• Calibration of air sampling equipment including pre- and post-sample calibrations
using a calibrated precision rotameter.
• Proper handling of air sampling filters to prevent cross contamination.
• Collection of field blanks; see Section B.5.2.2.
• Field cross checking of data forms to ensure accuracy and completeness.
B.5.2 Analytical Quality Control Checks
B.5.2.1 Quality Control Check of Filter Media
Before air samples are collected, a minimum of 2 percent of unused filters from each filter
lot of 100 filters will be analyzed to determine the mean asbestos structure count. If the mean
count for all types of asbestos structures is found to be more than 10 structures/mm2, or if the
mean fiber count for asbestos fibers and bundles longer than or shorter than 5�cm is more than 0.1
fiber/mm2, the filter lot will be rejected. By comparison, this criterion is more restrictive than that
specified by EPA in AHERA (i.e., 18 structures/mm2 of filter area).
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B.5.2.2 Blank Contamination
To ensure that contamination by extraneous silicate mineral fibers during sample collection
and specimen preparation is insignificant (see criteria in Section B.5.2.1) compared with the
results reported on samples, a continuous program of blank measurements will be established.
This will include filter lot blanks (see Section B.5.2.1), field blanks (open and closed), laboratory
blanks, and laboratory clean area blanks.
Field Blanks -- Closed field blanks are filter cassettes that have been transported to the
sampling site and sent to the laboratory without being opened. Open field blanks are filter
cassettes, that have been transported to the sampling site, opened for a short time (< 30 seconds)
without any air having passed through the filter, and then sent to the laboratory. The number of
open and closed blanks that will be collected and analyzed is presented in Table B-1.
Laboratory Blanks -- Laboratory blanks are unused filters (or other sample device or
container) that are prepared and analyzed in the same manner as the field samples to verify that
reagents, tools, and equipment are free of the subject analyte and that contamination has not
occurred during the analysis process. The laboratory will analyze at least one blank for every ten
samples or one blank per prep series. Blanks are prepared and analyzed along with the other
samples. If the blank control criteria (Section B.5.2.1) are not met, the results for the samples
prepared with the contaminated blank are suspect and should not be reported (or reported and
flagged accordingly). The preparatian and analyses of samples should be stopped until the source
of contatnination is found and eliminated. Before sample analysis is resumed, contamination-free
conditions shall be demonstrated by preparing and analyzing two blanks that meet the blank
control criteria. Laboratory blank results shall be documented in the quality control log.
Laboratory blank count sheets should be maintained in the project folder along with the sample
results.
Laboratory Clean Area Blanks -- Clean area blanks are prepared whenever contamination
of a single laboratory prep blank exceeds the criteria specified in Section B.5.2.1 or whenever
cleaning or servicing of equipment has occurred. To check the clean area, an used filter is left
open on a bench top in the clean area for the duration of the sample prep process. The blank is
then prepared and analyzed using ISO Method 10312:1995. If the blank control criteria (see
Section B.5.2.1) are not met, the area is cleaned using a combination of HEPA-filter vacuuming
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and a thorough wet-wiping of all surfaces with amended water. In addition, air samples should be
taken in the sample prep room to verify clean air conditions. At least 2,500 liters of air should be
drawn through a 25-mm-diameter 0.45-,um pore size MCE filter using a calibrated air sampling
pump. The samples should then be analyzed using ISO Method 10312:1995. If blank control
criteria are not met, sample preparation shall stop until the source of contamination is found and
eliminated. Clean area sample results shall be documented in the Clean Area Blank Log.
B.5.3 Analytical Precision and Accuracy
Quality control checks will be performed on a routine basis to verify that the analysis
system is in control. Most laboratory Quality Control Programs include frequent quality tests for
both accuracy and precision. Because of the difficulty of preparing quantitative asbestos standard
materials, neither spiked samples nor known quantitative samples can be used on a routine basis
for asbestos analysis accuracy testing. Therefore, routine quality control testing for asbestos
focuses on precision checks, which involve a second count or multiple counts of a sample or a
portion of a sample.
B.5.3.1 Replicate Analysis
The precision of the analysis is determined by an evaluation of repeated analyses of
randomly selected samples. A replicate analysis will be performed on 5% of the samples analyzed
to assess the precision of the counting abilities of the individual analysts. A replicate analysis is a
second analysis of the same preparation, but not necessarily the same grid openings, performed by
the same microscopist as in the original analysis.
The conformance expectation for the replicate analysis is that the count from the original
analysis and the replicate analysis will fall within a 95% confidence interval for the average count,
or as follows:
LCL < A1 AZ < UCL
where:
A1 is the original count,
AZ is the replicate count,
LCL is the lower confidence limit,
UCL is the upper confidence limit.
QAPP
Section B
August 17, 2000
Revision 1
Page 20 of 28
Should either the original or replicate count fall outside the acceptance range, the grid is re-
examined to determine the cause of the count variation. The 95% confidence interval is based on
the Poisson distribution. For average counts less than or equal to 20 structures, Table F-1 in ISO
Method 10312:1995 (see Appendix C) should be used to derive the upper and lower 95%
confidence limits. For average counts greater than 470 structures, a normal approximation can be
used. The upper and lower confidence limits based on the normal approxima.tion are calculated as
follows:
where:
LCL = ,u - 1.96 x ✓�.c
UCL = �c + 1.96 x ✓�c
,u is the average count,
✓µ is the definition of the Poisson standard deviation.
B.5.3.2 Duplicate Analysis
A duplicate sample analysis is also performed on 5% of the samples analyzed to assess the
reproducibility of the analysis and quantify the analytical variability due to the filter preparation
procedure. A duplicate analysis is the analysis of a second TEM grid preparation prepared from a
, different area of the sample filter performed by the same microscopist as the original analysis.
_ The conformance expectation is similar to that for replicate analyses with one exception. That is,
the count from the original analysis and the duplicate analysis should fall within a 95% confidence
interval for the average count.
Q�P
section B
August 17, 2000
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Page 21 of 28
B.5.4 Veri�cation Counting
Due to the subjective component in the structure counting procedure, it is necessary that
recounts of some specimens be made by a different microscopist (i.e., a microscopist different
than the one that performed the original analysis) in order to minimi�.e the subjective effects.
Verification counting will involve re-examination of the same grid opening by a different
microscopist. Such recounts provide a means of maintaining comparability between counts made
by different microscopists. These quality assurance measurements will constitute approximately
10 percent of the analyses. Repeat results should not differ at the 5% significance level.
QAPP
Section B
August 17, 2000
Revision 1
Page 22 of 28
B6 INSTRUMENT/EQUIPMENT TESTING, INSPECTION,
AND MAINTENANCE REQUIREMENTS
B.6.1 Field Instrumentation/Equipment
Field equipment/instruments (e.g., sampling pumps, meteorological instrumentation) will
be checked and calibrated before they are shipped or carried to the field. The equipment and
instruments will be checked and calibrated at least daily in the field before and after use. Spare
equipment, such as air sampling pumps, precision rotameters, and flow control valves will be kept
on-site to minimize sampling downtime. Backup instruments (e.g., meteorological
instrumentation) will be available within one day of shipment from a supplier.
B.6.2 Laboratory Equipment/Instrumentation
As part of the (To Be Determined) Laboratory's QA/QC Program, a routine preventive
maintenance program is performed to minimize the occurrence of instrument failure and other
system malfunctions of their transmission and scanning electron microscopes. The laboratory has
an internal group and equipment manufacturer's service contract to perform routine scheduled
maintenance, and to repair or to coordinate with the vendor for the repair of the electron
microscope and related instruments. All laboratory instruments are maintained in accordance with
manufacturer's specifications and the requirements of ISO Method 10312:1995.
�
QAPP
Section B
August 17, 2000
Revision 1
Page 23 of 28
B7 INSTRUMENT CALIBRATION AND FREQUENCY
B.7.1 Field Instrument/Equipment Calibration
B.7.1.1 Air Sampling Pumps
The air sampling pumps with a flow control valve will be evaluated to ensure that they are
capable of maintaining a stable flow rate for a given static pressure drop; i.e., the pumps can
maintain an initial volume flow rate of within +/- 10% throughout the sampling period. Prior to
use the sampling pumps will be tested against the pressure drop created by a 25-mm-diameter,
0.45-,um pore size MCE filter with a 5-�cm pore size 1VICE backup diffusing filter and cellulose
support pad contained in a three-piece cassette with 50-mm cowl at a flow rate of approximately
6 liters per minute at STP.
B7.1.2 Airflow Calibration Procedure
A flow control valve will be used to regulate the flow rate through the sampling train
during sampling. The airflow rate will be determined both before, at the mid-point, and after
sampling using a calibrated precision rotameter (Manostat Mode136-546-215). The precision
rotameter (a secondary calibration standard) will be calibrated using a primary standard airflow
calibrator (Gilabrator electronic flow meter).
A detailed written record will be maintained of all calibrations. It will include all relevant
calibration data, including the following elements:
• Gilabrator model and serial number
• Rotameter model and serial number
• Sampling train (pump, flow control valve, and filter)
• X- and Y- coordinate calibration data ,
� • Intercept, slope, and correlation coefficient from a linear regression analysis of the
calibration data, and resulting linear regression equation that will be used to
determine the sampling flow rate
• Relevant calculations
• Dry bulb temperature and barometric pressure
: • Name of person/affiliation that performed the calibration and linear regression
analysis
QAPP
Section B
August 17, 2000
Revision 1
Page 24 of 28
B.7.2 Calibration of TEM
The TEM shall be aligned according to the specifications of the manufacturer. The TEM
screen magnification, electron dif&action (ED) camera constant, and energy dispersive X-ray
analysis (EDXA) system shall be calibrated in accordance with the specifications in ISO Method
10312:1995, Annex B(see Appendix B).
QAPP
Section B
August 17, 2000
Revision 1
Page 25 of 28
BS INSPECTION/ACCEPTANCE REQUIREMENTS FOR
SUPPLIES AND CONSUMABLES
B.8.1 Air Sampling Filter Media
Please see Section B.5.2.1 regarding the quality control check of the filter media.
Q�p
Section B
August 17, 2000
Revision 1
Page 26 of 28
B9 DATA ACQUI5ITION REQUIREMENTS (NON-DIIZECT MEASUREMENTS)
B.9.1 Precision
The performa.nce goals stated in Section A.7 "Quality Objectives and Criteria for
Measurement Data" assume a between-sample variability of 250% or less. The actual between-
sample component of variability will be established from the data using standard variance
component analyses. If the target precision is not achieved, the false-negative error rate will be
greater than the target rate of 5% and failure to obtain a statistically significant result will not
provide strong evidence against the null hypothesis being tested. If a statistically significant result
is obtained, the false-negative error rate is of little concern, since it is clear that a false negative
error has not occurred.
Laboratory precision (coefficient of variation), which is a component of between-sample
variability, will be estimated from duplicate analyses of a subset of samples. This will provide a
measure of the relative contribution of laboratory analysis to the total between-sample variability.
This information will be useful for performing statistical power calculations for follow-up air
monitoring surveys.
B.9.2 Completeness
�
An overall measure of completeness will be given by the percentage of samples specified
in the study design that yield usable data. The quality control criterion is > 95%.
B.9.3 Accuracy
Duplicate counts of a subset of randomly selected samples will be performed by having the
same microscopist count two sets of grids prepared from the same sample. The results of the
counts will be compared, and those which do not fall within the 95% confidence limits for a
Poisson variable will be subjected to a further recount and/or a count of a third preparation in an
attempt to resolve the discrepancy. A count by a second microscopist may also be employed.
In addition, it is expected that a subset of samples will be selected at random by the City of
Fort Worth's Quality Assurance Manager to be analyzed by an outside "second" laboratory.
QAPP
Section B
August 17, 2000
Revision 1
Page 27 of 28
B10 DATA MANAGEMENT
Commercially available computer hardware and software used to manage measurement
data is controlled to ensure the validity of the data generated. Controls include system testing to
ensure that no computational errors are generated and evaluation of any proposed changes to the
system before they are implemented. Commercially available software does not require testing,
but validation of representative calculations are required using alternative means of calculations.
B.10.1 Data Assessment
Sample data will be reviewed by the laboratory during the reduction, verification, and
reporting process. During data reduction, all data will be reviewed for correctness by the
microscopist. A second data reviewer will�also verify conectness of the data. Finally, the
Laboratory Director (To Be Determined) will provide one additional data review to verify
completeness and compliance with the project QAPP. The City of Fort Worth's Quality
Assurance Manager, will also select a random sample of the data for the same purpose. Any
deficiencies in the data will be documented and identified in the data report.
B.10.2 Data Management
Field and laboratory data will be entered into a Microsoft Excel spreadsheet to facilitate
organization, manipulation, and access to the data. Field data will include information such as
sampling date, sample number, sampling site, sample description and location, sample type, air
volume, and sampling period. Laboratory data will include information such as sample number,
sample date received and analyzed, type of analysis, magnification, grid location, grid square area,
filter type, number of grids examined, number of asbestiform structures counted, structure type
(fiber, bundle, cluster, or matrix), and structure length and width. An example format for
reporting the structure counting data is contained in Figure 7 of ISO Method 10312:1995 (see
Appendix B).
QAPP
Section B
August 17, 2000
Revision 1
Page 28 of 28
B.10.3 Statistical Analysis
The data collected during the building demolitions and at the landfill will be analyzed using
standard analysis of variance (ANOVA) techniques. The ANOVA is a formal statistical
procedure that tests whether two or more groups of data are significantly different, on average.
The natural logarithm of each sample concentration will be used in the comparisons. Log-
transforma.tion is used to make the variances more equal and to provide data that are better
approximated by a norma.l distribution. The use of a log-transforma.tion is equivalent to assuming
the data follow a log-normal distribution; the log-normal distribution is commonly assumed for
asbestos measurements and other environmental contaminants. Sample results reported as non-
detected will be replaced by the analytical sensitivity divided by two to calculate summary
statistics and to perform all statistical analyses. All statistical comparisons will be made at the
O.OS level of signi.ficance.
QAPP
Section C
August 1'7, 2000
Revision 1
Page 1 of 4
C ASSESSMENT/OVER5IGHT
C1 ASSESSMENT AND RESPONSE ACTIONS
C.l.l Performance and System Audits
C.1.1.1 Field Audits
The City of Fort Worth staff will be present during the study. The City's Technical
Project Officer will conduct periodic field audits. The audit will include, but not limited to the
examination of sample collection and equipment calibration procedures, sampling data and chain-
of-custody forms, and other sample collection and handling requirements specified in the QAPP.
The auditor will document any deviations from the QAPP so that they can be corrected in a timely
manner.
The auditor will independently measure the flow rate of at least 50% of the air samplers in
operation at the time of the audit. The relative accuracy (A%) of the audited flow rates will be
established as follows:
A% = 100% - RE%
where RE%, the relative error, is calculated as:
where:
RE% _ (F-A) / A x 100
F= flow rate measured by the field crew
A= flow rate measured by the auditor.
The performance objective for the relative accuracy will be set between 90% and 110%.
Prior to leaving the site, the auditor will debrief Tracy Bramlett regarding the results of the audit
and any recommendations, if necessary. The results of the audit will be presented in a written
report prepared by the auditor.
QAPP
Section C
June 2, 2000
Revision 0
Page 2 of 4
C.1.1.2 Laboratory Audit
Ms. Hoover (Quality Assurance Manager) or an independent laboratory quality assurance
" consultant selected by Ms. Hoover will conduct at least one quality assurance audit of the
Laboratory (To Be Determined). The first audit will be conducted at the onset of the project to
. verify that all procedures specified in the QAPP are understood and are being followed.
C.1.2 Corrective Actions
Sampling and analytical problems may occur during sample collection, sample handling
and documentation, sample preparation, laboratory analysis, and data entry and review.
Immediate on-the-spot corrective actions will be implemented whenever possible and will be
documented in the project record. Implementation of the corrective action will be confirmed in
writing by completing a Corrective Action Report (Figure C-1).
QAPP
Section C
June 2, 2000
Revision 0
Page 3 of 4
Originator: Date:
Project Name/Number: Corrective Action Number:
Description of Problem State Cause of Problem
(Give Date and Time Identified)
State Conective Action Planned QA Officer Comments:
(Include Persons Involved in Action)
Signatures Project Manager Comments:
QA Officer
Project Manager
Originator
Figure C-1. Corrective Action Report.
Q�P
Section C
June 2, 2000
Revision 0
Fage 4 of 4
C2 REPORTS TO MANAGEMENT
Effective communication is an integral part of a quality system. Planned reports provide a
structure to inform management of the project schedule, deviations from the approved QAPP,
impact of the deviations, and potential uncertainties in decisions based on the data.
The IHST Project Manager (Tracy Bramlett) will provide verbal progress reports to the
City of Fort Worth's Project Manager (Kathryn Hansen). These reports will include pertinent
informa.tion from the data processing and report writing progress reports and corrective action
reports, as well as the status of analytical data as determined from conversations with the
laboratory. Mr. Bramlett will promptly advise Ms. Hansen on any items that may need corrective
action.
A written report will be prepared for each field and laboratory audit. These reports will be
submitted to the City of Fort Worth's Project Manager.
QAPP
Section D
June 2, 2000
Revision 0
Page 1 of 3
D DATA VALIDATION AND USABILITY
Dl DATA REVIEW, VALIDATION, AND VERIFICATION REQUIREMENTS
The data will be reviewed and validated by the City of Fort Worth's Quality Assurance
Manager or by an independent quality assurance consultant (To Be Determined) selected by the
City of Fort Worth.
QAPP
Section D
June 2, 2000
Revision 0
Page 2 of 3
D2 VALIDATION AND VERIFICATION METHODS
The analytical laboratory will perform in-house analytical data reduction and verification
under the direction of the laboratory's quality assurance manager. The laboratory's quality
assurance manager is responsible for assessing data quality and advising of any data rated as
"unacceptable" or other notations which would caution the data user of possible unreliability.
The City of Fort Worth's quality assurance manager or an independent quality assurance
consultant (To Be Determined) will conduct a systematic review of the data to verify compliance
with the established quality criteria in the QAPP and ISO Method 10312:1995. The data review
will identify any out-of-control data points and data omissions. Based on the extent of the
deficiency and its importance in the overall data set, the laboratory ma.y be required to re-analyze
the sample. Included in the data validation of a sample set will be an assessment of chain-of-
custody and analyses of field quality control samples (open and closed field blanks).
The precision of the data will be determined by calculating the coefficient of variation for
the replicate and duplicate sample analyses as well as the analyses of the field duplicate samples.
QAPP
Section D
June 2, 2000
Revision 0
Page 3 of 3
D3 RECONCILIATION WITH DATA QUALITY OBJECTIVES
The proposed statistical methods to analyze the data and determine the significance of
departures (positive and negative) from the assumptions established in the Data Quality
Objectives are presented in Section B.10.
QAPP
Section E
June 2, 2000
Revision 0
Page 1 of 1
E1 REFERENCES
1. U.S. Environmental Protection Agency. EPA Guidance for Quality Assurance Project
Plans — EPA QA/G-5. EPA/600/R-98/018, February 1998.
2. City of Fort Worth, Texas, Project XL Proposal "Asbestos Management in the
Demolition of Substandar•d Structures as a Nuisance Abatement,"(September 30, 1999).
Prepared by Department of Environmental Management, City of Fort Worth, Texas
76102.
3. U.S. Environmental Protection Agency. Ambient Airborne Asbestos Levels in Alviso,
California. Prepared by John R. Kominsky and Ronald W. Freyberg. Contract No. 68-
CO-0048, Apri127, 1995.
4. U.S. Environmental Protection Agency. Ambient Air Monitoring at the Moss Landing
Harbor District: Moss Landing, California. Prepared by John R. Kominsky and Ronald
W. Freyberg. EPA Contract No. 68-D2-0058, October 17, 1990.
5. Kominsky, J.R., R.W. Freyberg, J.A. Brownlee, D.R. Greber. AHERA Clearance at
Twenty Abatement Sites. EPA/600/52-91/028, August 1991.
6. Berman, D.W. and Chatfield, E.7. (1990). Superfund Method for the Determination of
Asbestos in Ambient Air. Part 2: Technical Background Document. Prepared for the
Environmental Services Branch of the U.S. Environmental Protection Agency.
Washington, D.C. EPA/540/2-90/OOSb.
Q�p
Appendix A
June 2, 2000
Revision 0
Appendix A
Comparison of the Asbestos NESHAP and the Fort Worth Method
for the Demolition of Substandard Structures
Table - 1 Comparison of the Asbestos NESHAP and the Fort Worth Method
for Demolition of Substandard Structures
,. .. �. o- � o� �
.. .. ;o . � �
��� � � ., � �. ,
�• � '• A Unifni 5tates 11 Unite,i Siares
��� ��� Agenc/m?ntai Pr,�lxti�n ��', E PA E�encnmental Pratacticn � FOI�'T�OI�THv.
�9 1
ASBESTOS ASSESSMENT Not required. Full AHERA Level Asbestos Full AHERA Level ,4sbeslos
Assessment Assessmenl.
DEMOLITION NOTIFICATION Written noti(Cation as early a5 pOSsible Writteft notifCation at least ten woriCing 4Vritlen nolificahon a[ least TWO svorkiny
before, but no[ later Ihan the follo�ving days before work begins. deys before wcrk beyins.
� working day.
REMOVAL OF RACM PRIOR TO RP,CM not removed prior to demolition. Remove RACM under (ull containment if Rt\CM not remnveci pnor fo demoli�ian.
DEMOLITION Ihefe I5:
Note' SPRAY-ON FIREPROOFING
1. At Ieast 80 linear meters (260 li�ear AND LARGE QUANTITIES OF
feel) on pipes or at Ieast 15 square THERNIAL SYSTEM
meters (160 square feet) on other INSULATION WILL BE
facility wmponents; or ADDRESSED UNDER fl1LL
2. At Ieast 1 cubic meter (35 cubic (eet) CONTAiNMENT CONDITIONS.
off facility componenls where the
length o� area could not be .
measured previously.
Adequateiy wet asbeslos-containing
waste material. Afler wetting, sea� in
leak-tighl containers while wel. If
matenals will not fit into containers
wilhou! additional breakage, put
materials in Ieak-tight wrapping. Label
con[ainers or wrapped materials using
OSHA compliant waming labels.
EMISSIONS CONTROLS DL/RING �ischarge no Visible Emissions from Discharge no Visible Emissions from Discharye no Visible Emissions from
DEMOUTION R.4Cti1 or asbes[os-containing waste RACM w asbestos-coritaining waste R�CM or as-bestos-containing waste
matenaL , material. material.
HANDLING PROCEDURES FOR Adequately wet Ihe pertion of the faci�ity Adequately wet asbestos-containing Adeyuately wet THE FACILITY during
OEMOLITION ASBESTOS- Ihat Confains RACtiI dUling Ihe W�eCking waste matenai at all times aker the WfeChing Ope�atiUn
CONTAINING WASTE MATERIAL operation. demolition and keep wet during handling �
and loading for transport to a disposai Adequateiy �,vet DE�IOLITiON DEBRIS
� Adequately wet as6estos-mntaining site. at all hmes aker demolition and keep
waste material at all [imes aker � wet duriny handling and loadiny for
demolition and keep wet dunng handling Asbestos-containing waste materials Iransport to a disFosal site.
and loading for transport to a disposai demolished in place do not have to be
site. seaied in leak-tight containers or WASTE MATERIALS TO BE
wrapping, but may be transported and DISPOSED IN BULK WITHIN
Asbes�os-containing �,vaste materials do disposed of in buik. TRAILERS COVERED WITH TARPS.
not have to be sealed in leak-tight
containers or wrapping, bul may be Note: Does not apply to Category I Non-
transported and disposed of in bulk. Friabfe ACM waste and
Calegory II Non•Friable ACM
waste that did not become
crumbled, puiverized, or reduced
to powder.
TRANSPORTATION OF Mark vehicles used to ifansport Maf1( vehicles us2d to tfansPOft N1ark vehlcles usc9 to transport
�EMOLITION ASBESTOS- asbestos-containfny �,vaste material asbestos-containing waste mat2rial as6estos�containing wasle m2tenal
CONTAINING WASTE MATERIAL dunng ihe loading and unloading of during the loading and unloading of during Ihe loadiny and unloadiny of
waste so that signs are visible. waste so that signs are visible. wasle so Ihat signs are visible.
Mani(est RACM shipments. Mani(est RACM shipments. �vtanifest RACM shipmenls.
�ISPOSAI oF DEMOLITION Deposit all asbestos-containing was�e Oeposil ail asbestos-containing Waste Deposit all asbestos-containiny �riaste
ASBESTOS-CONTAiNING material as soon as practical at a Waste material as soon as p�actical at a waste matenal as soon a� praCtical dt a WaSte
WASTE MATERIAL disposal site approved for as6estos disposal sile approved (or asbestos disposal site approved for asbestos
disposal, unless it is Category I Plen- disposai, unless it is Calegory 1 Non- dis�sal, unless it is Catr�yory 1 Non
Friabie ACht that is not RACM. Fnable ACM that is nol RACM. Friable ACNi that is not Ri\CP.t
SITE SUPERVISION OURING At least one representahve �rained in the At least one �epresenlalive t�ained in the At leasl one represzNahve frained in the
DEMoli7ioN NESHAP shall be present on-site. NESHAP shall be present on-site. NESHAP shall be present on-site.
REcoRos � Ntaintain :vaste disposai records for at Maintain wasle disposal records for at Maintam waste di;posai records (or at
MAINTENANCE least hvo years. Ieas� two years. least hvo years.
STORMWATER MANAGEMENT Not specified Nol speci(ed Comply with Chapter 12.5, Artide �II,
� "Storm Water Protection," Code of the
City of Fort Worth. Use best
management practices to controi
runoff as necessary.
ou7000a n�rt MONtTOR�NG OSHA monitoring of �iorkers OSHA monitoring of warkers. AREA SAMPLING TO BE
PERFORMED AT ALl FOUR
CORNERS OF THE JOB SITE.
� OSHA monitoriny of svorkers.
WETTING PROCEDURES Adequa[ely wet. Adequately weL Utilize fire hose equipped with
variable rate noule to allow for
"mistin '
Q�P
Appendix B
June 2, 2000
Revision 0
Appendix B
ISO Method 10312:1995
Ambient Air - Determination of Asbestos Fibres --
Direct-Transfer Transmission Electron Microscopy Method
INTER�NATIONAL
STANDARD.
iso
10312
First edition
1995-05-01
Ambient air — Determination of asbestos
fibres — Direct-transfer transmission
electron microscopy method
Air ambiant — Determination des fibres d'amiante — Methode de
microscopie elecironique a transmission directe
=/�� —
-���
_�/= Reference number
�SO 10312:1995(El
Printed for you by Document Centerinc., 111 Industrial Road Suite 9, Belmont, CA 94002-4044 Phone: 650-591-7600 Fax: 650-591-761'
ISO 10312:1995(Ej
v
\
Contents
1 Scope ...........................................
2 Normative references ...................
3 Definitions .,.....,
.......................
4 Principle ...................................
5 Symbois ot units and abbreviations
6 Reagents
..................................
7 Apparatus .................................
8 Air sampie collection ,,,,,,,,,,,,,,,,
9 Procedure for analysis ..............
10 Performance characteristics ...,
11 Test report ...............................
Page
.............................................. 1
.............................................. 2
.............................................. 2
.............................................. 3
...................:...................... 4
............................................. 5
............................................. 5
........................................... 10
........................................... 11
.......................................... 18
.......................................... 19
Annexes
A Determination of operating conditions for plasma asher ...... 22
B Calibration procedures ........................................................... 23
C Structure counting criteria ...................................................... 25
D Fibre identification procedure ................................................ 33
E Determination of the concentrations of asbestos fibres and bundles
longer than 5 µm, and PCM equivalent asbestos fibres ....... 42
F Calculation of results ........................:..................................... ,t3
G Strategies for collection of air samples ,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,,, q7
H Methods for removal of gypsum fibres ................................. 4g
JBibliography ............................................................................ 49
� ISO 1995
Ali rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electrornc or mechanicai, including photocopying and
microfilm, without permission �n wnting from the publisher.
International Organization for 5tandardization
Case Postale 56 • CH-1211 GenBve 20 • Swrtzeriand
Printed in Switzerla�d
�l
o ISO ISO 10312:1995(E)
Foreword
ISO (the international Organization for Standardization) is a woridwide
federation of national standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for
which a technical committee has been established has the right to be
represented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take part in the work. ISO
collaborates ciosely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Pubiication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
Internationai Standard ISO 10312 was prepared by Technical Committee
ISO/TC 146, Air qualiry, Subcommittee SC 3, Ambient aimospheres.
Annexes A, B, C, D, E and F form an integral part of this International
Standard. Annexes G, H and J are for information only.
ISO 10312:7995(E)
� ISO
4
�
tntroduction
This International Standard is applicabie to the determination of airborne
asbestos in a wide range of ambient air situations, inciuding the interior
atmospheres of buildings, and for detailed evaluation of any atmosphere
in which asbestos structures are likely to be present. Because the best
availabie medical evidence indicates that the numerical fibre concentration
and the fibre sizes are the relevant parameters for evaluation of the
inhalation hazards, a fibre counting technique is the only logical approach.
Most fibres in ambient atmospheres are not asbestos, and therefore there
is a requirement for fibres to be identified. Many airborne asbestos fibres
in ambient atmospheres have diameters below the resolution limit of the
optical microscope. This Internationai Standard is based on transmission
electron microscopy, which has adequate resolution to allow detection of
small fibres and is currently the only technique capable of unequivocal
identification of the majority of individual fibres of asbestos. Asbestos is
often found, not as single fibres, but as very complex, aggregated struc-
tures which may or may not be also aggregated with other particles. The
fibres found suspended in an ambient atmosphere can often be identified
unequivocally, if a sufficient measurement effort is expended. However,
if each fibre were to be identified in this way, the analysis would become
prohibitively expensive. Because of instrumental deficiencies or because
of the nature of the particulate, some fibres cannot be positively identified
as asbestos, even though the measurements all indicate that they could
be asbestos. Subjective factors therefore contribute to this measurement,
and consequently a very precise definition of the procedure for identifica-
tion and enumeration of asbestos fibres is required. The method specified
in this International Standard is designed to provide the best description
possible of the nature, numerical concentration, and sizes of asbestos-
containing particles found in an air sample. This International Standard is
necessarily complex, because the instrumental techniques used are com-
plex, and also because a very detailed and logical procedure must be
specified to reduce the subjective aspects of the measurement. The
method of data recording specified in this International Standard is de-
signed to allow re-evaluation of the structure counting data as new med-
ical evidence becomes available. All of the feasible specimen preparation
techniques result in some modification of the airborne particulate. Even
the collection of particles from a three-dimensional airborne dispersion
onto a two-dimensional filter surface can be considered a modification of
the particulate, and some of the particles in most samples are modified
by the specimen preparation procedures. However, the procedures spec-
ified in this International Standard are designed to minimize the disturb-
ance of the coliected particulate material, and the effect of those
disturbances which do occur can be evaluated.
This International Standard describes the method of analysis for a single
air filter. However, one of the largest potential errors in characterizing
asbestos in ambient atmospheres is associated with the variability be-
tween filter samples. For this reason, it is necessary to design a replicate
sampling scheme in order to determine this International Standard's ac-
curacy and precision.
iv
a
p
INTERNATIONAL STANDARD o ISO
ISO 10312:1995(E�
Ambient air — Determination of asbestos fibres .—
Direct-transfer transmission electron microscopy
method
1 Scope
1.1 Substance determined
' This International Standard specifies a reference
method using transmission electron microscopy for
the determination of the concentration of asbestos
structures in ambient atmospheres and includes
measurement of the lengths, widths and aspect ratios
of the asbestos structures. The method allows deter-
' mination of the type(s) of asbestos fibres present. The
method cannot discriminate between individuai fibres
of the asbestos and non-asbestos analogues of the
same amphibole mineral.
1.2 Type of sample
The method is defined for polycarbonate capillary-pore
filters or cellulose ester (either mixed esters of cellu-
lose or cellulose nitrate) filters through which a known
volume of air has been drawn. The method is suitable
for determination of asbestos in both exterior and
building atmospheres.
1.3 Measuring range
The range of concentration which can be determined
is 50 structures(mm2 to 7 000 structures/mmZ on the
filter. The air concentrations represented by these
values are a function of the volume of air sampled.
There is no lower limit to the dimensions of asbestos
fibres which can be detected. In practice,
microscopists vary in their ability to detect very small
asbestos fibres. Therefore, a minimum length of
0,5 µm has been defined as the shortest fibre to be
incorporated in the reported results.
1.4 Limit of detection
The limit of detection theoretically can be lowered in-
definitely by filtration of progressively larger volumes
of air and by extending the examination of the speci-
mens in the electron microscope. In practice, the
lowest achievabie limit of detection for a particular
area of TEM specimen examined is controlled by the
total suspended particulate concentration.
For total suspended �particulate concentrations of ap-
proximately 10 µg/m , corresponding to clean, rural
atmospheres, and assuming filtration of 4 000 litres
of air, an analytical sensitivity of 0,5 structure(I can be
obtained, equivalent to a limit of detection of 1,8
structure�l, if an area of 0,195 mm2 of the TEM
specimens is examined. If higher total suspended
particulate concentrations are present, the volume of
air filtered must be reduced in order to maintain an
acceptable particulate loading on the filter, leading to
a proportionate increase in the analytical sensitivity.
Where this is the case, lower limits of detection can
be achieved by increasing the area of the TEM speci-
mens that is examined. In order to achieve lower
limits of detection tor fibres and bundles longer than
5 µm, and for PCM equivalent fibres, lower magni-
fications are spe,cified which permit more rapid ex-
amination of larger areas of the TEM specimens when
the examination is limited to these dimensions of fi-
bre. The direct analyticai method cannot be used if the
general particulate loading of the sample coilection
filter exceeds approximately 10 µg�cm2 of filter sur-
face, which corresponds to approximately 10 % cov-
erage of the collection filter by particulate. If the total
suspended particulate is largely organic material, the
limit of detection can be lowered significantly by using
an indirect preparation method.
130 10312:1995(E) � ISO -
2 Normative references
The following standards contain provisions which,
through reference in this text, constitute provisions
of this International Standard. At the time of pubiica-
tion, the editions indicated were valid. All standards
are subject to revision, and parties to agreements
based on this International Standard are encouraged
to investigate the possibility of applying the most re-
cent editions of the standards indicated below.
Members of IEC and ISO maintain registers of cur-
rently valid international Standards.
ISO 4225:1994, Air quality — General aspects — Vo-
cabulary.
ISO 4226:1993, Air quality — General aspects —
Units of ineasurement.
ISO Standard Handbook No. 2:1993, Quantities and
units.
ISO Standard Handbook No. 3:1989, Siatistical Meth-
ods.
3 Definitions
For the purposes of this International Standard, the
following definitions apply (see also ISO 4225).
3.1 acicular: The shape of an extremely slender
crystal with cross-sectional dimensions which are
smail relative to its length, i.e, needle-like.
3.2 amphibole: A group of rock-forming
ferromagnesium silicate minerals, closely related in
crysta) form and composition, with the nominal for-
mula:
Ao or �BZC5Tg022(OH,F,CI}2
where
A=K,Na
B= FeZ+, Mn, Mg, Ca, Na
C= AI, Cr, Ti, Fe3+, Mg, Fez+
T= Si, AI, Cr, Fe3+, Ti
In some varieties of amphibole, these elements can
be partially substituted by �i, Pb or Zn. Amphibole is
characterized by a cross-linked double chain of Si-O
tetrahedra with a silicon:oxygen ratio of 4:11, by co-
lumnar or fibrous prismatic crystals and by good
prismatic cleavage in two directions parallel to the
2
crystal faces and intersecting at angles of about 56°
and 124°.
3.3 amphibole asbestos: Amphibole in an
asbestiform habit.
3.4 analytical sensitivity: The calculated airborne
asbestos structure concentration in asbestos
structures/litre, equivalent to counting of one
asbestos structure in the analysis. The method in this
International Standard does not specify an analytical
sensitivity.
3.5 asbestiform: A specific type of mineral fibrosity
in which the fibres and fibrils possess high tensile
strength and fiexibility.
3.6 asbestos: A term applied to a group of silicate
minerals belonging to the serpentine and amphibole
groups which have crystallized in the asbestiform
habit, causing them to be easily separated into long,
thin, strong fibres when crushed or processed. The
Chemical Abstracts Service Registry Numbers of the
most common asbestos varieties are: chrysotile
(12001-29-5), crocidolite (1 200 1-28-4), grunerite
asbestos (amosite) (12172-73-5), anthophyliite
asbestos (77536-67-5), tremolite asbestos
(77536-68-6) and actinolite asbestos (77536-66-4�.
3.7 asbestos structure: A term applied to any con-
nected or overlapping grouping of asbestos fibres or
bundles, with or without other particles.
3.8 aspect ratio: The ratio of length to width of a
particle.
3.9 blank: A structure count made on TEM speci-
mens prepared from an unused filter, to determine
the background measurement.
3.10 camera length: The equivalent projection
length between the specimen and its electron dif-
fraction pattern, in the absence of lens action.
3.11 chrysotile: A fibrous mineral of the serpentine
group which has the nominal composition
Mg3s�2�5���'i�q
Most natural chrysotile deviates little from this nomi-
nal composition. In some varieties of chrysotile, minor
substitution of silicon by AI3+ may occur. Minor sub-
stitution of magnesium by AI3+, Fe2�, Fe3+ Niz+
Mn2+ and Co2+ may aiso be present. Chrysotile is the
most prevalent type of asbestos.
3.12 cleavage: The breaking of a mineral along one
of its crystallographic directions.
= . o ISO ISO 1Q312:1995jE)
F
3.13 cleavage fragment: A fragment of a crystal
that is bounded by cleavage faces.
3.14 ciuster: A structure in which two or more fi-
bres, or fibre bundles, are randomly oriented in a
connected grouping.
3.15 d-spacing: The distance between identical ad-
jacent and paraliel planes of atoms in a crystal.
3.16 electron diffraction: A technique in electron
microscopy by which the crystal structure of a speci-
men is examined.
3.17 electron scattering power: The extent to
which a thin layer of substance scatters e�ectrons
from their original directions.
3.18 energy dispersive X-ray analysis: Measure-
ment of the energies and intensities of X-rays by use
of a solid state detector and muitichannel analyser
system.
3.19 eucentric: The condition when the area of in-
terest of an object is placed on a tilting axis at the
intersection of the electron beam with that axis and
is in the plane of focus.
3.20 field blank: A filter cassette which has been
taken to the sampling site, opened, and then closed.
Such a filter is used to determine the background
structure count for the measurement.
3.21 fibril: A single fibre of asbestos, which cannot
be further separated longitudinally into smaller com-
ponents without losing its fibrous properties or ap-
pearances.
3.22 fibre: An elongated particle which has parallel
or stepped sides. For the purposes of this Interna-
tional Standard, a fibre is defined to have an aspect
ratio equal to or greater than 5:1 and a minimum
length of 0,5 µm.
3.23 fibre 6undle: A structure composed of parallel,
smaller diameter fibres attached along their lengths.
A fibre bundle may exhibit diverging fibres at one or
both ends.
3.24 fibrous structure: A fibre, or connected
grouping of fibres, with or without other particles.
3.25 habit: The characteristic crystal growth form,
(or combination of these forms), of a mineral, includ-
ing characteristic irregularities.
3.26 limit of detection: The caiculated airborne
asbestos structure concentration in structures per li-
tre, equivalent to counting 2,99 asbestos structures in
the analysis.
3.27 matrix: A structure in which one or more fi-
bres, or fibre bundles, touch, are attached to, or par-
tially concealed by, a single particle or connected
group of nonfibrous particles.
3.28 Milier index: A set of either three or four inte-
ger numbers used to specify the orientation of a
crystallographic piane in relation to the crystal axes.
3.29 PCM equivalent fibre: A fibre of aspect ratio
greater than or equal to 3:1, longer than 5 µm, and
which has a diameter between 0,2 µm and 3,0 µm.
3.30 PCM equivalent structure: A fibrous structure
of aspect ratio greater than or equal to 3:1, longer
than 5 µm, and which has a diameter between
0,2 µm and 3,0 µm.
3.31 primary structure: A fibrous structure that is
a separate entity in the TEM image.
3.32 replication: . A procedure in electron
microscopy specimen preparation in which a thin
copy, or replica, of a surface is made.
3.33 selected area electron diffraction: A tech-
nique in electron microscopy in which the crystal
structure of a small area of a sample is examined.
3.34 serpentine: A group of common rock-forming
minerals having the nominal formula
M9sS�2�efOH)4
3.35 structure: A single fibre, fibre bundle, cluster
or matrix.
3.36 twinning: The occurrence of crystals of the
same species joined together at a particular mutual
orientation, such that the relative orientations are re-
lated by a definite law.
3.37 unope�ed fibre: An asbestos fibre bundle of
large diameter which has not been separated into its
constituent fibrils or fibres.
3.38 zone-axis: The line or crystallographic direction
through the centre of a crystal which is parailel to the
intersection edges of the crystal faces defining the
crystal zone.
4 Principle
A sample of airborne particulate is coliected by draw-
ing a measured volume of air through either a
3
ISO 10312:1995�E)
capillary-pore polycarbonate membrane filter of maxi-
mum pore size 0,4 µm or a cellulose ester (either
mixed esters of cellulose or cellulose nitrate) mem-
brane filter of maximum pore size 0,45 µm by means
of a battery-powered or mains-powered pump. TEM
specimens are prepared from polycarbonate filters by
appiying a thin film of carbon to the filter surface by
vacuum evaporation. Small areas are cut from the
carbon-coated filter, supported on TEM specimen
grids, and the filter medium is dissolved away by a
solvent extraction procedure. This procedure leaves a
thin film of carbon which bridges the openings in the
TEM specimen grid, and which supports each particle
from the original filter in its original position. Cellulose
ester filters are chemica(ly treated to collapse the pore
structure of the filter, and the surface of the collapsed
fiiter is then etched in an oxygen plasma to ensure
that ail particles are exposed. A thin film of carbon is
evaporated onto the filter surface and smali areas are
cut from the filter. These sections are supported on
TEM specimen grids and the filter medium is dis-
soived away by a solvent extraction procedure.
The TEM specimen grids from either preparation
method are examined at both low and high magni-
fications to check that they are suitable for analysis
before carrying out a quantitative structure count on
randomly-selected grid openings. In the TEM analysis,
electron diffraction (ED) is used to examine the crystal
structure of a fibre, and its elementai composition is
determined by energy dispersive X-ray analysis
(EDXA). For a number of reasons, it is not possibie to
identify each fibre unequivocally, and fibres are clas-
sified according to the techniques which have been
used to identify them. A simple code is used to re-
cord, for each fibre, the manner in which it was cias-
sified. The fibre classification procedure is based on
successive inspection of the morphology, the electron
diffraction pattern for a selected area, and the qual-
itative and quantitative energy dispersive X-ray ana-
lyses. Confirmation of the identification of chrysotile
is done only by quantitative ED, and confirmation of
amphibole is done only by quantitative EDXA and
qua�titative zo�e axis ED.
In addition to isolated fibres, ambient air samples of-
ten contain more complex aggregates of fibres, with
or without other particles. Some particles are com-
posites of asbestos fibres with other materials. Indi-
vidual fibres and structures that are more complex are
referred to as "asbestos structures". A coding system
is used to record the type of fibrous structure, and to
provide the optimum description of each of these
complex structures. The two codes remove the re-
quirement to interpret the structure counting data
from the microscopist, and allow this evaluation to be
made later without the requirement for re-
4
examination of the TEM specimens. Several leveis of
analysis are specified, the higher levels providing a
more rigorous approach to the identification of fibres.
The procedure permits a minimum required fibre
identification criterion to be defined on the basis of
previous knowledge, or lack of it, about the particular
sample. Attempts are then made to achieve this min-
imum criterion for each fibre, and the degree of suc-
cess is recorded for each fibre. The lengths and
widths of all classified structures and fibres are re-
corded. The number of asbestos structures found on
a known area of the microscope sample, together
with the equivalent volume of air filtered through this
area, is used to calculate the airborne concentration
in asbestos structuresJlitre of air.
5 Symbols of units and abbreviations
5.1 Symbols of units (see also ISO 4226 and
ISO No. 2)
eV = electron volt
kV = kilovolt
I/min = litres per minute
µg = microgram (10-6 gram)
µm = micrometre (10-6 metre)
nm = nanometre (10-9 metre)
W = watt
5.2 Abbreviations
DMF Dimethylformamide
DE Electron diffraction
EDXA Energy dispersive X-ray analysis
FWHM
HEPA
MEC
PC
PCM
SAED
SEM
STEM
TEM
Full width, half maximum
High efficiency particle absolute
Mixed esters of cellulose
Polycarbonate
Phase contrast optical microscopy
Selected area electron diffraction
Scanning electron microscope
Scanning transmission electron microscope
Transmission electron microscope
o ISO
UICC Union Internationale Contre le Cancer
6 Reagents
During the analysis, unless otherwise stated, use only
reagents of recognized analytical grade and water
(6.11.
WARNING — Use the reagents in accordance with
the appropriate hea{th and safety regulations.
6.1 water, fibre-free.
A supply of freshly distilled, fibre-free water, or an-
other source of fibre-free, pyrogen-free water shall be
used.
6.2 Chloroform, analytical grade, distilled in glass,
preserved with 1 % (VM ethanol.
6.3 1-Methyi-2-pyrrolidone.
6.4 Dimethylformamide.
6.5 Glacial acetic acid.
6.6 Acetone.
7 Apparatus
7.1 Air sampling — Equipment and
consumable supplies
7.1.1 Filter cassette
Field monitors, comprising 25 mm to 50 mm diam-
eter three-piece cassettes, with cowls which project
less than 2 cm in front of the filter surface shall be
used for sample collection. The cassette shall be
loaded with either a capillary pore polycarbonate fiiter
of maximum pore size 0,4 µm or an MEC or cellulose
nitrate filter of maximum pore size 0,45 µm. Either
type of filter shall be backed by a 5 µm pore size MEC
or cellulose nitrate filter, and supported by a ceilulose
back-up pad. When the filters are in position, an elas-
tic cellulose band or adhesive tape shall be applied to
prevent air leakage. Suitable precautions shall be
taken to ensure that the filters are tightly clamped in
the assembly, so that significant air leakage around
the filter cannot occur.
Representative filters from the filter lot shall be ana-
lysed as specified in 9.7 for the presence of asbestos
structures before any are used for air sample coi-
lection.
ISO 10312:1995(E)
7.1.2 Sampling pump
The sampling pump shall be capable of a flow-rate
sufficient to achieve the desired analytical sensitivity.
The face velocity through the filter shall be between
4,0 cm/s and 25,0 cm/s. The sampling pump used
shall provide a non-fluctuating airflow through the fil-
ter, and shali maintain the initial volume flow-rate to
within ± 10 % throughout the sampling period. A
constant flow or critical orifice controlied pump meets
these requirements. Flexible tubing shall be used to
connect the filter cassette to the sampling pump. A
means for calibration of the flow-rate of each pump is
also required.
7.1.3 Stand
A stancl shall be used to hold the filter cassette at the
desired height for sampling, and shall be isolated from
the vibrations of the pump (7.1.2).
7.1.4 Variable area flowmeter
A calibrated variable are a flowmeter with a range of
approximately 1 I/min to 10 I/min is required for cali-
bration of the air sampling system.
The variable area flowmeter shall be cleaned before
use to avoid transfer of asbestos contamination from
the flowmeter to the sample being collected.
7,2 Specimen preparation laboratory
Asbestos, particularly chrysotile, is present in varying
quantities in many laboratory reagents. Many building
materials also contain significant amounts of asbestos
or other mineral fibres which may interfere with the
analysis if they are inadvertentiy introduced during
preparation of specimens. It is most important to en-
sure that, during preparation, contamination of TEM
specimens by any extraneous asbestos fibres is min-
imized. All specimen preparation steps shali therefore
be performed in an environment where contamination
of the sample is minimized. The primary requirement
of the sample preparation laboratory is that a blank
determination shall yield a result which will meet the
requirements specified in 9.7. A minimum facility
considered suitable for preparation of TEM specimens
is a laminar flow hood with positive pressure. How-
ever, it has been established that work practices in
specimen preparation appear to be more important
than the tape of clean handling facilities in use. Prep-
aration of samples shall be carried out only after ac-
ceptable blank values have been demonstrated.
NOTE 1 It is recommended that activities invoiving ma-
nipulation of bulk asbestos samples not be performed in the
5
ISO 10312:1995(E)
same area as TEM specimen preparation, because of the
possibilities of contaminating the TEM specimens.
7.3 Equipment for analysis
7.3.1 Transmission electron microscope
A TEM operating at an accelerating potential of
80 kV to 120 kV, with a resolution better than
1,0 nm, and a magnification range of approximately
x 300 to x 100 000 shall be used. The ability to obtain
a direct screen magnification of about x 100 000 is
� ISO "
necessary for inspection of fibre morphology; this
magnification may be obtained by supplementary op-
tical enlargement of the screen image by use of a
binocular if it cannot be obtained directly. It is also
required that the viewing screen of the microscope
be calibrated such that the lengths and widths of fibre
images down to 1 mm width can be measured in in-
crements of 1 mm, regardless of image orientation.
This requirement is often fulfiiled through the use of
a fluorescent screen with calibrated gradations in the
form of circles, as shown in figure 1.
4
5
6
7
Figure 1— Example of calibration markings on TEM viewing screen
6
ti
� o ISO
:
For Bragg angles less than 0,01 rad, the TEM shall be
capable of performing ED from an area of 0,6 µm2 or
less, selected from an in-focus image at a screen
magnification of x 20 000. This performance require-
ment defines the minimum separation between parti-
cles at which independent ED patterns can be
obtained from each particle. If SAED is used, the
performance of a particular instrument may normally
be calculated using the following equation
A= 0,785 4 x� M+ 2 OO0058312
/
where
A is the effective SAED area, in square
micrometres;
D is the diameter, in micrometres, of the
SAED aperture;
M is the magnification of the objective lens;
CS is the spherical aberration coefficient, in
millimetres, of the objective lens;
8 is the maximum required Bragg angle, in
radians.
It is not possible to reduce the effective SAED area
indefinitely by the use of progressively smaller SAED
apertures, because there is a fundamental limitation
imposed by the spherical aberration coefficie�t of the
objective lens.
If zone-axis ED analyses are to be performed, the
TEM shall incorporate a goniometer stage which per-
mits the TEM specimen to be either
a) rotated through 360°, combined _ with tilting
through at least + 30° to — 30° about an axis in
the plane of the specimen;
b? tilted through at least + 30° to — 30° about two
perpendicular axes in the plane of the specimen.
_ The analysis is greatly facilitated if the goniometer
permits eucentric tilting, although this is not essential.
If EDXA and zone-axis ED are required on the same
fibre, the goniometer shall be of a type which permits
tilting of the specimen and acquisition of EDXA spec-
tra without changing the specimen holder.
The TEM shall have an illumination and condenser
lens system capable of forming an electron probe of
diameter less than 250 nm.
NOTE 2 Use of an anti-contamination trap around the
specimen is recommended if the required instrumental
performance is to be obtained.
ISO 10312:1995(E)
7.3.2 Energy dispersive X-ray analyser
The TEM shall be equipped with an energy. dispersive
X-ray analyser capabie of achieving a resolution better
than 180 eV (FWHM} on the MnKa. Since the per-
formance of individua) combinations of TEM and
EDXA equipment is dependent on a number of ge-
ometrical factors, the required performance of the
combination of the TEM and X-ray analyser is speci-
fied in terms of the measured X-ray intensity obtained
from a fibre of small diameter, using a known electron
beam diameter. Solid state X-ray detectors are least
sensitive in the low energy region, and so measure-
ment of sodium in crocidolite shall be the perform-
ance criterion. The combination of electron
microscope and X-ray analyser shall yield, under rou-
tine analytical conditions, a background-subtracted
NaKa integrated peak count rate of more than 1 count
per second (cps) from a fibre ot UICC crocidolite,
50 nm in diameter or smaller, when irradiated by an
electron probe of 250 nm diameter or smaller at an
accelerating potential of 80 kV. The peak/background
ratio for this performance test shall exceed 1,0.
The EDXA unit shall provide the means for subtraction
of the background, identification of elementai peaks,
and calculation of background-subtracted peak areas.
7.3.3 Computer
Many repetitive numericai calculations are necessary,
and these may be performed conveniently by rela-
tively simple computer programmes. For analyses of
zone-axis ED pattern measurements, a computer with
adequate memory is required to accommodate the
more complex programmes involved.
7.3.4 Plasma asher
For preparation of TEM specimens from MEC filters,
a plasma asher, with a radio frequency power rating
of 50 W or higher, shall be used to etch the surface
of collapsed MEC filters. The asher shall be supplied
with a controlled oxygen flow, and shall be modified,
if necessary, to provide a vaive to control the speed
of air admission 'so that rapid air admission does not
disturb particulates from the surface of the filter after
the etching step.
NOTE 3 It is recommended that filters be fitted to the
oxygen suppiy and the air admission line.
7.3.5 Vacuum coating unit
A vacuum coating unit capable of producing a vacuum
better than 0,013 Pa shall be used for vacuum de-
position of carbon on the membrane filters. A sampie
7
(SO 10312:1995(E)
holder is required which will allow a glass microscope
slide to be continuously rotated during the coating
procedure.
NOTE 4 A mechanism which also allows the rotating
slide to be tilted through an angle of approximately 45°
during the coating procedure is recommended. A liquid ni-
trogen cold trap above the diffusion pump may be used to
minimize the possibiliry of contamination of the filter sur-
faces by oil from the pumping system. The vacuum coating
unit may also be used for deposition of the thin film of gold,
or other calibration material, when it is required on TEM
specimens as an internal calibration of ED patterns.
7.3.6 Sputter coater
A sputter coater with a gold target may be used for
deposition of gold onto TEM specimens as an integral
calibration of ED patterns. Other calibration materials
are acceptable. Experience has shown that a sputter
coater aliows better control of the thickness of the
calibration material.
7.3.7 Solvent washer f Jaffe washer)
The purpose of the Jaffe washer is to ailow dissol-
ution of the filter polymer while leaving an intact
evaporated carbon film supporting the fibres and
other particles from the filter surface. One design of
Glass Petri dish
(fd 100 mm x 15 mn
� ISO
a washer which has been found satisfactory for vari-
ous solvents and filter media is shown in figure 2. I�
general, either chloroform or 1-methyl-2-pyrrolidone
has been used for dissolving polycarbonate filters and
dimethylformamide or acetone has been used for
dissolving MEC or cellulose nitrate filters. The higher
evaporation rates of chloroform and acetone require
that a reservoir of 10 ml to 50 ml of solvent be used,
which may need replenishment during the procedure.
Dimethylformamide and 1-methyi-2-pyrrolidone have
lower vapour pressures and much smaller volumes
of solvent may be used. It is recommended that ail
washers be used in a fume hood, and when speci-
mens are not being inserted or removed, the Petri
dish lid shall be in place during the solvent dissolution.
The washer shali be cleaned before it is used for each
batch of specimens.
7.3.8 Condensation washer
For more rapid dissolution of the filter polymer, or if
difficulties are experienced in dissolving the filter
polymer, use a condensation washer, consisting of a
flask, condenser and cold finger assembly, with a
heating mantle and means for contro►ling the temper-
ature. A suitable assembly is shown in figure 3, using
either acetone or chloroform as the solvent, depend-
ing on the type of filter.
Dimensions in centimetres
Electron microscooe
NOTE — Solvent is added untii the meniscus contacts the underside of the stainless steel mesh bridge.
Figure 2— Example of design of soivent washer (Jaffe washerl
8
�tainless steel mesh
��idge (50 mesh)
o ISO
Condenser
Specimen
ISO 10312:1995(E
Water drain
Cold finger
E- Cold water source
�nt
nostaticaily controtled
ng mantle
Figure 3— Example of design of condensation washer
7.3.9 Slide warmer or oven
Use either a slide warmer or an oven for heating
slides during the preparation of TEM specimens from
MEC or cellulose nitrate filters. It is required to main-
tain a temperature of 65 °C to 70 °C.
7.3.10 Ultrasonic bath
An ultrasonic bath is necessary for cleaning the appa-
ratus used for TEM specimen preparation.
7.3.11 Carbon grating replica
A carbon grating replica with about 2 000 parallel lines
per millimetre shall be used to calibrate the magni-
fication of the TEM.
7.3.12 Calibration specimen grids for EDXA
TEM specimen grids prepared from dispersions of
calibration minerals are required for calibration of the
EDXA system. Some suitable calibration minerals are
riebeckite, chrysotile, halloysite, phlogopite, woilas-
tonite and bustamite. The mineral used for calibration
of the EDXA system for sodium shall be prepared
using a gold TEM grid.
7.3.13 Carbon rod sharpener
The use of necked carbon rods, or equivalent, allows
the carbon to be evaporated onto the filters with a
minimum of heating.
7.3.14 Disposable tip micropipettes
A disposable tip micropipette, capable of transferring
a volume of approximately 30 µl, is necessary for the
preparation of TEM specimen grids from MEC filters.
7.4 Consumable supplies
7.4.1 Copper electron microscope grids
Copper TEM grids with 200 mesh are recommended.
Grids which have grid openings of uniform size such
that they meet the requirement specified in 9.62 shall
be chosen. To facilitate the relocation of individual grid
openings for quality assurance purposes, the use of
grids with numerical or alphabetical indexing of indi-
vidual grid openings is recommended.
9
130 10312:9995(E)
7.4.2 Gold electron microscope grids
Gold TEM grids with 200 mesh are recommended to
mount TEM specimens when sodium measurements
are required in the fibre identification procedure. Grids
which have grid openings of uniform size such that
they meet the requirement specified in 9.6.2 shall be
chosen. To facilitate the relocation of individual grid
openings for quality assurance purposes, the use of
g�ids with numerical or alphabetical indexing of indi-
vidual grid openings is recommended.
7.4.3 Carbon rod electrodes
Spectrochemicaliy pure carbon rods, shall be used in
the vacuum evaporator (7.3.5) during carbon coating
of filters.
7.4.4 Routine electron microscopy tools and
supplies
Fine-point tweezers, scalpel holders and blades, mi-
croscope slides, double-coated adhesive tape, lens
tissue, gold wire, tungsten filaments and other routine
supplies are required.
7.4.5 Refere�ce asbestos samples
Asbestos samples, shall be for preparation of refer-
ence TEM specimens of the primary asbestos min-
erals. The UICC set of minerals is suitable for this
purpose.
8 Air sample collection
The desired analytical sensitivity is a parameter that
shall be established for the analysis prior to sample
collection. It is defined as the structure concentration
corresponding to the detection of one structure in the
analysis. For direct transfer methods of TEM speci-
men preparation, the analytical sensitivity is a function
of the volume of air sampled, the active area of the
collection filter, and the area of the TEM specimen
over which structures are counted. If total airborne
dust levels are high, it may be necessary to terminate
sampling before the required volume has been sam-
pled. If this happens, the analytical sensitivity required
can be achieved only by counting structures on more
grid openings, or by selective concentration of
asbestos structures using an indirect TEM specimen
preparation technique. Select the sampling rate and
the period of sampling to yield the required analytical
sensitivity, as detailed in table 1. Before air samples
10
� ISO
are collected, unused filters shall be analysed as de-
scribed in 9.7 to determine the mean asbestos struc-
ture count for blank filters.
Air samples shall be collected using filter cassettes
l7.1.1). During sampling, the cassette shall be sup-
ported on a stand (7.1.3) which is isolated from the
vibrations of the pump (7.1.2). The cassette shall be
held facing verticaily downwards at a height of ap-
proximately 1,5 m to 2,0 m above ground/floor level,
and shali be connected to the pump with a flexible
tube.
Measure the sampiing flow-rate at the front end of
the cassette, both at the beginning and end of the
sampling period, using a calibrated variable area
fiowmeter (7.1.4) temporarily attached to the iniet of
the cassette. The mean value of these� two mea-
surements shall be used to calculate the total air vol-
ume sampled.
Basic strategies for monitoring environmental sources
of airborne asbestos are described in annex G. After
sampling, a cap shall be placed over the open end of
the cassette, and the cassette packed with the fiiter
face-upwards for return to the laboratory. Field blank
filters shall also be included, as specified in 9.7, and
subrnitted to the remaining analytical procedures
along with the samples.
NOTES
5 In table 1 a collection filter area of 385 mm2 is assumed,
and the TEM grid openings are assumed to be 85 µm2
square. The limit of detection is defined as the upper 95 °/a
confidence limit of the Poisson distribution for a count of
0 structures. In the absence of background, this is equal to
2,99 times the analytical sensitivity. Backgrounds that are
different from 0 observed during analysis of blank filters will
degrade the limit of detection.
6 The analytical sensitivity S, expressed in number of
structures per litre, is calculated using the following
equation:
s kA rV
9
where
A� is the active area, in square millimetres, of
sampie coilection filter;
A9 is the mean area, in square miilimetres, of grid
openings examined;
is the number of grid openings examined;
is the volume of air sampied, in litres.
o ISO
ISO 10312:1995(E)
Table 1— Examples of the minimum number of grid openings requi�ed to achieve a particular analytical
sensitivity and �imit of detection
Analytical Limit of Volume of air sampled (litres)
sensitivity detection
structures(I structures(I 500 1 000 2 000 3 000 4 000 5 000
0,1 0,30 1066 533 267 178 134 107
0,2 0,60 533 267 134 89 67 54
0,3 0,90 356 178 89 60 45 36
0,4 1,2 267 134 67 45 34 27
0,5 1,5 214 107 54 36 27 22
0,7 2,1 153 77 39 26 20 16
1,0 3,0 107 54 27 18 14 11
2,0 6,0 54 27 14 9 7 6
3,0 9,0 36 18 9 6 5 4
4,0 12 27 14 7 5 4 4
5,0 15 22 11 6 4 4 4
7,0 21 16 8 4 4 4 4
10 30 11 6 4 4 4 4
9 Procedure for analysis
9.1 General
The techniques used to prepare TEM specimens are
different for polycarbonate and cellulose ester filters.
The preparation method to be used shall be either 9.3
or 9.4, depending on the type of inembrane filter used
for air sampling. Cleaning of the sample cassettes
before they are opened, preparation of the carbon
evaporator, criteria for acceptable specimen grids, and
the requirement for blank determinatioris are identical
for the two preparation techniques. TEM examination,
structure counting, fibre identification and reporting
of results are independent of the type of filter or
preparation technique used.
The ability to meet the blank sample criteria is de-
pendent on the cleanliness of equipment and sup-
plies. Consider all supplies such as microscope siides
and glassware as potential sources of asbestos con-
tamination. It is necessary to wash all glassware be-
fore it is used. Wash any tools or giassware which
come into contact with the air sampling filters or TEM
specimen preparations both before use and between
handling of individual samples. Where possible,
disposable supplies should be used.
9.2 Cleaning of sample cassettes
Asbestos fibres can adher to the exterior surfaces of
air sampling cassettes; and these fibres can be inad-
vertently transferred to the sampie during handling.
To prevent this possibility of contamination, and after
ensuring that the cassette is tightly sealed, wipe the
exterior surfaces of each sampling cassette before it
is placed in the clean facility or laminar flow hood.
9.3 Direct preparation of TEM specimens
from polycarbonate filters
9.3.1 Selection of fiiter area for carbon coating
Use a cleaned microscope slide to support represen-
tative portions of polycarbonate filter during the car-
bon evaporation. Double-coated adhesive tape is used
to attach the filter portions to the glass slide. Take
care not to stretch the polycarbonate filters during
handling. Using freshly cleaned tweezers, remove the
polycarbonate filter from the sampling cassette, and
place it on to a second cleaned glass microscope siide
which is used as a cutting surface. Using a freshly
cleaned curved scalpel blade, cut the filter by rocking
the blade from the point, pressing it into contact with
the filter. Repeat the process as necessary. Several
such portions may be mounted on the same micro-
scope slide. The scalpei blade and tweezers shall be
washed and dried between the handling of each filter.
Identify the filter portions by writing on the glass slide.
9.3.2 Carbo� coating of filter portions
Place the glass slide hoiding the filter portions on the
rotation-tilting device; approximately 10.cm to 12 cm
11
1�0 10312:1995(E)
from the evaporation source, and evacuate the
evaporator chamber l7.3.5) to a vacuum better than
0,013 Pa. The evaporation of carbon shall be per-
formed in very short bursts, separated by a few sec-
onds to allow the electrodes to cool. If evaporation
of carbon is too rapid, the strips of polycarbonate filter
will begin to curl, and cross-linking of the surface wili
occur. This cross-linking procedures a layer of polymer
which is relatively insoluble in organic solvents, and it
will not be possible to prepare satisfactory TEM
specimens. The thickness of carbon required is de-
pendent on the size of particles on the filter, and ap-
proximately 30 nm to 50 nm has been found to be
satisfactory. If the carbon film is too thin, large parti-
cles will break out of the fiim during the later stages
of preparation, and there wili be few complete and
undamaged grid openings on the specimen. Too thick
a carbon film will lead to a TEM image which is lack-
ing in contrast, and the ability to obtain ED patterns
wili be compromised. The carbon film thickness
should be the minimum possible, while retaining most
of the grid openings of the TEM specimen intact.
9.3.3 Preparation of the Jaffe washer
Place several pieces of lens tissue, as shown in
figure 2, on the stainless steel bridge (7.1.3) and fill
the washer (see 7.3.7) with chloroform (6.2} or
1-methyl-2-pyrrolidone (6.3) to a level where the
meniscus contacts the underside of the mesh, re-
sulting in saturation of the lens tissue.
9.3.4 Placing of specimens in the Jaffe washer
Using a curved scalpel blade, cut three 3 mm square
pieces of carbon-coated polycarbonate filter form the
carbon-coated filter portion. Select three squares to
represent the centre and the periphery of the active
surface of the filter. Place each square of filter, carbon
side up, on a TEM specimen grid, and place the grid
and filter on the saturated lens tissue in the Jaffe
washer. Place the three specimen grids from one
sample on the same piece of lens tissue. Any number
of separate pieces of lens tissue may be placed in the
same Jaffe washer. Cover the Jaffe washer with the
lid, and allow the washer to stand for at least 8 h.
NOTE 7 It has been found that some polycarbonate fii-
ters will not completely dissolve in the Jaffe washer, even
after exposure to chloroform for as long as 3 d. This prob-
lem is more severe if the surface of the filter was over-
heated during the carbon evaporation. it has been found
that the problem of residual undissolved filter polymer can
be overcome in several ways:
a) condensation washing of the grids, using chloroform as
the solvent, after the initial Jaffe washer treatment, can
12
o ISO
often remove much of the residuai filter medium in a
period of approximately 30 min. To carry out this pro-
cedure, transfer the piece of lens tissue supporting the
specimen grids to the cold finger of the condensation
washer (7.3.8), which has achieved stable operating
conditions. Operate the washer for approximately
30 min after inserting the grids;
b) used in a Jaffe washer, 1-methyl-2-pyrrolidone has been
found to be a more effective solvent than chloroform
for polycarbonate filters. This soivent is more effective
if the lens paper is not used and grids are placed di-
rectly on the stainless steel mesh of the Jaffe washer.
A dissolution period of 2 h to 6 h has been found to be
satisfactory. After dissolution is complete, remove the
stainless steel mesh from the Jaffe washer and allow
the grids to dry. 1-methyi-2-pyrrolidone evaporates very
slowly. If it is required to dry the grids more rapidiy,
transfer the stainless steel bridge into another Petri
dish, and add water (6.1) until the meniscus contacts
the underside of the mesh. After approximately
15 min, remove the mesh and allow the grids to dry. If
it is desired to retain water-soluble particle species on
the TEM grids, ethanol may be used instead of water
(6.1 � for the second wash;
c) a mixture of 20 °/a 1,2-diaminoethane
[ethylenediamine] and 80 % 1-methyl-2-pyrrolidone,
used in a Jaffe washer, completely dissolves
polycarbonate filters in 15 min, even if the surface oi
the filter has been overheated. To use this solvent,
place the grids directiy on the stainless steel mesh of
the Jaffe washer, do not use the lens paper. After a
period of 15 min, transfer the stainless steel bridge into
another Petri dish, and add water (6.1) until the
meniscus contacts the underside of the mesh. After
approximately 15 min, remove the mesh and allow the
grids to dry. If it is desired to retain water-soluble par-
ticle species on the TEM grids, ethanol may be used
instead of water (6.1) for the second wash.
9.3.5 Rapid preparation of TEM specimens from
PC flters
TEM specimens can be prepared rapidly from PC fil-
ters, if desired, by washing for approximately 1 h in a
Jaffe washer, foilowed by washing for 30 min in a
condensation washer using chloroform as the solvent.
The alternative filter dissolution procedures described
in note 7 may also be used.
9.4 Direct preparation of TEM specimens
from cellulose ester filters
9.4.1 Selection of area of filter for preparation
Using clean tweezers, remove the filter from the filter
cassette, and place it on a cleaned microscope slide.
Using a clean, curved scalpel blade, cut out a portion
of the filter.
o ISO
9.4.2 Preparation of solution for collapsing
ceilulose ester filters
Mix 35 ml of dimethylformamide f 6.4), and 15 ml of
glacial acetic acid (6.5) with 50 ml of water (6.1). Store
this mixture in a clean bottle, The mixture is stable
and suitable for use for up to 3 months after prepara-
tion.
9.4.3 Fiiter collapsing procedure
Using a micro�pipette with a disposable tip (7.3.14),
place 15 µl/cm to 25 µlJcm2 of the solution prepared
in 9.4.2 on a cleaned microscope slide, and using the
end of the pipette tip, spread the liquid over the area
to be occupied by the filter portion. Place the filter
portion, active surface upwards, on top of the sol-
ution, lowering the edge of the filter at an angle of
about 20° so that air bubbles are not created. Remove
any solution not absorbed by the filter by allowing a
paper tissue to contact the liquid at the edge of the
filter. More than one fiiter portion may be placed on
one slide. Place the slide either on a thermostatically
controlled slide warmer (7.3.9) at a temperature of
65 °C to 70 °C, or in an oven (7.3.9) at this temper-
ature, for 10 min. The fiiter collapses slowly to about
15 % of its original thickness. The procedure leaves
a thin, transparent polymer film, with particles and fi-
bres embedded in the upper surface.
9.4.4 Plasma etching of the filter surface
The optimum conditions and time for plasma etching
(see 7.3.4) have been determined experimentally from
the recovery of fine chrysotile fibrils on 0,8 µm pore
size MEC filters. The conditions required in a particular
plasma asher shall be established using the procedure
specified in annex A. Place the microscope slide
holding the collapsed filter portions in the plasma
asher, and etch for the time and under the conditions
� determined. Take care to ensure that the correct
conditions are respected. After etching, admit air
slowly to the chamber and remove the microscope
slide.
Adjust the air admission valve of the plasma asher
such that the time taken for the chamber to reach at-
mospheric pressure exceeds 2 min. Rapid air admis-
sion may disturb particulates on the surface of the
etched filter.
9.4.5 Carbon coating
Coat the microscope slide holding the collapsed filter
portions with carbon as specified in 9.3.2.
ISO 10312:1995(E)
9.4.6 Preparation of the Jaffe washer
Place several pieces of lens tissue on the stainless
steel bridge, and fiil the washer with
dimethylformamide (6.4) or acetone (6.6) to a level
where the meniscus contacts the underside of the
mesh, resulting in saturation of the lens tissue.
9.4.7 Placing of specimens in the Jaffe washer
Place the specimens in the Jaffe washer as specified
in 9.3.4. Specimens are normaliy cleared after ap-
proximately 4 h.
9.4.8 Rapid preparation of TEM specimens from
cellulose ester fiiters
An alternative washing procedure may be used to
prepare TEM specimens from cellulose ester filters
more rapidiy than can be achieved by the Jaffe
washing procedure. After the specimens have been
washed in a Jaffe washer for approximately 1 h,
transfer the piece of lens tissue supporting the
specimens to the cold finger of a condensation
washer (7.3.8) operating with acetone as the soivent
because dimethylformamide shall not be used in a
conde�sation washer. Operate the condensation
washer for approximately 30 min. This treatment re-
moves all the remaining filter polymer.
9.5 Criteria for acceptable TEM specimen
grids
Valid data cannot be obtained unless the TEM speci-
mens meet specified quality criteria. Examine the
TEM specimen grid in the electron microscope at a
sufficiently low magnification (x 300 to x 1 000) for
complete grid openings to be inspected. Reject the
grid if
a? the TEM specimen has not been cleared of filter
medium by the filter dissolution step. If the TEM
specimen exhibits areas of undissolved filter me-
dium, and if at least two of the three specimen
grids are not cleared, either additional washing
with solvent shall be carried out, or new speci-
mens shall be prepared from the filter;
b) the sample is overloaded with particulate. If the
specimen grid exhibits more than approximately
10 % obscuration on the majority of the grid
openings, the specimen shall be designated as
overloaded. This filter cannot be alanysed satis-
factorily using the direct preparation methods be-
cause the grid is too heavily loaded with debris to
allow separate examination of individual particies
by ED and EDXA, and� obscuration of fibres by
13
1�0 10312:1995(E)
other particulates may lead to underestimation of
the asbestos structure count;
c) the particulate deposits on the specimen are not
uniformly distributed from one grid opening to the
next. �f the particulate deposits on the specimen
are obviously not uniform from one grid opening
to the next, the specimen shall be designated as
non-uniform. This condition is a function either of
the air sampiing conditions or of the fundamentai
nature of the airborne particulate. Satisfactory
analysis of this filter may not be possible unless
a large number of grid openings is examined;
d) the TEM grid is too heavily loaded with fibrous
structures to make an accurate count. Accurate
counts cannot be made if the grid has more than
approximately 7 000 structures/mmZ; or
e) more than approximately 25 % of the grid
openings have broken carbon film over the whole
grid opening. Since the breakage of carbon film is
usually more frequent in areas of heavy deposit,
counting of the intact openings can lead to an
underestimate of the asbestos structure count.
NOTE 8 If the specimens are rejected because un-
acceptable numbers of grid openings exhibit broken
carbon replica, an additional carbon coating may be ap-
plied to the carbon coated filter, and new specimen
grids prepared. The larger particles can often be sup-
ported by using a thicker carbon film. If this action does
not produce acceptable specimen grids, this fiiter can-
not be analysed using the direct preparation methods.
If one or more of the conditions described in bi, c),
d) or e) exists, it may not be possible to analyse the
sample by this method.
9.6 Procedure for structure counting by TEM
9.6.1 General
The examination consists of a count of asbestos
structures which are present on a specified number
of grid openings. Fibres are classified into groups on
the basis of morphological observations, ED patterns
and EDXA spectra. The totai number of structures to
be counted depends on the statistical precision de-
sired. In the absence of asbestos structures, the area
of the TEM specimen grids which must be examined
depends on the analytical sensitivity required. The
precision of the structure count depe�ds not only on
the totai number of structures counted, but also on
their uniformity from one grid opening to the next.
Additionai structure counting will be necessary if
greater precision is required.
14
� ISO
In order that the estimate of the structure density on
the sampling filter shall not be based on the smali
area represented by one specimen grid, grid openings
shall be examined on two of the three specimen grids
prepared. Then combine the results in the caiculation
of the structure density. Structure counts shall be
made at a magnification of approximately x 20 000,
and shall be terminated at the end of the examination
of the grid opening on which the 100th asbestos
structure is observed, except that the count shall be
continued until a minimum of 4 grid openings have
been examined. Otherwise, the structure count shall
continue to that number of grid openings at which the
specified analytical sensitivity has been achieved.
NOTE 9 The normal range for the number of grid
openings which should be examined is from 4 to 20. If in-
sufficient air has been sampled through the filter, the cal-
culation in 9.6.4 can indicate that an impractically large
number of grid openings should be examined. When this
situation occurs, a larger value of ana�yticai sensitivity may
have to be accepted.
9.6.2 Measurement of inean grid opening area
The mean grid opening area shall be measured for the
type of TEM specime� grids in use. The standard de-
viation of the mean of 10 openings selected from 10
grids shouid be less than 5%. As an optional proce-
dure, or if the 5% standard deviation criterion cannot
be demonstrated, the dimensions of each grid open-
ing examined in the TEM shall be measured at a cali-
brated magnification.
9.6.3 TEM alignment and calibration procedures
Before structure counting is performed, align the TEM
according to instrumental specifications. Calibrate the
TEM and EDXA system according to the procedures
specified in annex B.
9.6.4 Determination of stopping point
Before structure counting is begun, calculate the area
of specimen to be examined in order to achieve the
selected analytical sensitivity. Caiculate the maximum
number of grid openings to be examined using the
following equation:
Af
k A9VS
where
is the number of grid openings to be ex-
amined, rounded upwards to the next
highest integer;
L
o ISO
Af is the area, in square millimetres, of sam-
ple filter;
A9 is the area, in square millimetres, of TEM
specimen grid opening;
V is the volume of air sampled, in litres;
S is the required analytical sensitivity, ex-
pressed in number of structures per litre.
9.6.5 General procedure for structure counting
and size analysis
Use at least two specimen grids prepared from the
fiiter in the structure count. Select at random several
grid openings from each grid, and combine the data
in the calculation of the results.
Use a form similar to that shown in figure 4 to record
the data. Insert the first specimen grid into the TEM.
NOTE 10 In order to facilitate quality assurance mea-
surements which require re-examination of the same grid
opening by different microscopists, the grid should be in-
serted into the specimen holder in a standard orientation
with the grid bars parallel and perpendicular to the axis of
the specimen holder. This will provide scan directions par-
allel to the edges of the grid opening. It should be ensured
that all microscopists begin scanning at the same starting
point on the grid opening, and that they use similar scan
patterns. This procedure permits rapid relocation of fibrous
structures for further examination if necessary.
Select a typicai grid opening and set the screen mag-
nification to the calibrated value (approximately
x 20 000). Adjust the sample height untii the features
in the centre of the TEM viewing screen are at the
eucentric point. Set the goniometer tiit angle to zero.
In column 1 of the data recording form, record the
number or letter used to identify the grid. In column
2, record the identification of the particular grid open-
ing. Position the specimen so that the grid opening is
positioned with one corner visible on the screen.
Move the image by adjustment of only one tra�slation
control, carefully examining the sample for fibres, until
the opposite side of the grid opening is encountered.
Move the image by a predetermined distance less
than one screen diameter, using the other translation
control, and scan the image in the reverse direction.
Continue the procedure in tnis manner until the entire
grid opening has been inspected in a pattern similar
to that shown in figure 5. When a fibrous structure is
detected, assign a sequential number to the primary
structure in column 3, perform the identification pro-
cedures required as detailed in annex E, and enter the
appropriate compositional classification on the struc-
ture counting form in column 5. Assign a
ISO 10312:1995(E1
morphological classification to the structure according
to the procedures specified in annex D, and record
this in column 6. Measure on the TEM viewing screen
the length and width of the image of the primary
structure, in millimetres, and record these mea-
surements in columns 7 and 8. For a disperse ciuster
or matrix, assign a compositional classification and a
morphological classification to each structure compo-
�ent, measure ihe length and width, and enter the
data in columns 4 to 8. Use column 4 of the data re-
cording form to tabulate the sequential number of
total structures taking into account structure compo-
nents. if non-asbestos fibres are observed, note their
presence and type, if known. After a fibrous structure
has been examined and measured, relocate the orig-
inal field of view accurately before continuing scan-
ning of the specimen. Failure to do this may cause
structures to be overlooked or counted twice. Con-
tinue the examination until the compietion of the grid
opening on which the 100th asbestos structure has
been recorded, or until the number of grid openings
required to achieve the specified analytical sensitivity,
calculated according to 9.6.4, have been examined
whichever occurs first. The data shall be drawn ap-
proximately equally from a minimum of two grids.
Regardless of the value calculated according to 9.6.4,
fibrous structures on a minimum of four openings
shall be counted.
9.6.6 Measurement of concentration for asbestos
fibres and bundles longer than 5 µm
Consider improving the statistical validity for meas-
urement of asbestos fibres and bund(es longer than
5 µm by additional examination at a lower magnifica-
tion, taking account only of the longer fibres and
bundles. Perform this extended examination for fibres
and bundles longer than 5 µm in accordance with the
procedures specified in annex E. Use a magnification
of approximately x 10 000 for counting all asbestos
fibres and bundles longer than 5 µm, or approximately
x 5 000 if only fibres and bundles within the diameter
range 0,2 µm to 3,0 µm are to be counted. Continue
the count until completion of the grid opening on
which 100 fibres and bundles have been recorded, or
until a sufficient area of the specimen has been ex-
amined to achieve the desired analytical sensitivity.
Only those structures which are identified as, or are
suspected to be, either chrysotile or one of the
amphibole minerals will be reported in either the
original or the extended TEM examination. Other ma-
terials, such as gypsum, ceilulose fibres, and filter
artifacts such as undissolved filter strands, will not be
inciuded in the fibre count. This restriction is intended
to ensure that the best statisticai validity is obtained
for the materials of interest.
15
ISO 10392:1995 jE)
TEM asbestos structure count (page of )
Report number : .................................
...............
Sample number : ....................................................
Filename : ..............................................................
Sample description : ..............................................
.................................................................................
......................... ........................................................
Preparation date : .................. By: ........................
Analysis date : ....................... By: ........................
Computer entry date: ........... By : ........................
� ISO
Air volume : ...................................................... litres
Sample filter area : ............................................ mmZ
Magnification : ..................
Grid opening dimension : .................................... µm
Level of analysis (C) : ....................................................
(A) : .......................................
Grid Number of
Grid opening structures Class Type of Length Width Comments
structure
primary totai mm mm
Figure 4— Example of structure counting form
16
S
First pass
� TEM field of view
ISO 10312:1995(E)
�- Gtid opening
Figure 5— Example of scanning procedure for TEM specimen examination
9.7 Blank and quality control determinations
Before air sampies are collected, a minimum of two
unused filters from each filter lot of 100 filters shall
be analysed to determine the mean asbestos struc-
ture count. If the mean count for all types of asbestos
structures is found to be more than 10 structures(
mmZ, or if the mean fibre count for asbestos fibres
and bundles longer than 5 µm is more than 0,1 fibre�
mm2, reject the filter lot.
To ensure that contamination by extraneous asbestos
fibres during specimen preparation is insignificant
compared with the results reported on samples, es-
tablish a continuous programme of blank mea-
surements. At least one field blank shail be processed
along with each batch of sampies. In addition, at least
one unused filter shall be included with every group
of samples prepared on one microscope slide.
Initially, and also at intervals afterwards, ensure that
samples of known asbestos concentrations can be
analysed satisfactorily. Since there is a subjective
component in the structure counting procedure, it is
necessary that recounts of some specimens be made
by different microscopists, in order to minimize the
subjective effects. Such recounts provide a means of
maintaining comparability between counts made by
different microscopists. Variability between and within
microscopists and between laboratories shall be
characterized. These quality assurance measurements
shall constitute approximately 10 % of the analyses.
Repeat results should not differ at the 5% signif-
icance level.
17
ISO 10312:1995(E)
9.8 Calculation of results
Calculate the results using the procedures detailed in
annex F. Prior to the TEM examination of the speci-
mens, the level of analysis was specified. Before the
results are calculated, the compositional and
morphological classifications to be included in the re-
sult shall be specified. The chi-squared uniformity test
shall be conducted using the number of primary
asbestos structures found on each grid opening, prior
to the application of the cluster and matrix counting
criteria. The concentration result shall be calculated
using the numbers of asbestos structures reported
after the application of the cluster and matrix counting
criteria.
10 Performance characteristics
10.1 General
It is important to use this analyticai method in con-
junction with a continuous quality control programme.
The quality control programme should include use of
standard samples, blank sampies, and both interlabo-
ratory and intralaboratory analyses.
10.2 Interferences and limitations of fibre
identification
Unequivocal identification of every chrysotile fibre is
not possible, due to both instrumental limitations and
the nature of some of the fibres. The requirement for
a calibrated ED pattern eliminates the possibility of an
incorrect identification of the fibre selected. However,
there is a possibility of misidentification of fibres for
which both the morphologies and the ED patterns are
reported on the basis of visual inspection only. The
only significant possibilities of misidentification occur
with halloysite, vermiculite scrolis or palygorskite, ali
of which can be discriminated from chrysotile by the
use of EDXA and by observation of the 0,73 nm (002)
reflection of chrysotile in the ED pattern.
As in the case of chrysotile fibres, complete identifi-
cation of every amphibole fibre is not possible due to
instrumental limitations and the nature of some of the
fibres. Moreover, complete identification of every
amphibole fibre is not practical due to the limitations
of both time and cost. Particles of a number of other
minerais with compositions similar to those of some
amphiboles could be erroneously classified as
amphibole when the classification criteria do not in-
clude zone-axis ED techniques. However, the re-
quirement for quantitative EDXA measurements on
all fibr�s as support for the random orientation ED
technique makes misidentification very unlikely, par-
18
� ISO
ticularly when other similar fibres in the same sample
have been identified as amphibole by zone-axis
methods. The possibility of misidentification is further
reduced with increasing aspect ratio, since it is rare
for the minerals with which amphibole may be con-
fused to display an asbestiform habit.
10.3 Precision and accuracy (see ISO
Standard Handbook No. 3)
10.3.1 Precision
The analytical precision that can be obtained is de-
pendent upon the number of structures counted, and
also on the uniformity of the particulate deposit on the
original filter. Assuming that the structures are ran-
domly deposited on the fiiter, if 100 structures are
counted and the loading is at least 3,5 structures/grid
opening, computer modeliing of the counting proce-
dure shows that a coefficient of variation of about
10 % can be expected. As the number of structures
counted decreases, the precision will also decrease
approximately as �N , where N is the number of
structures counted. In practice, particulate deposits
obtained by filtration of ambient air samples are rarely
ideally distributed, and it is found that the precision is
correspondingly reduced. Degradation of precision is
a consequence of several factors, such as:
a) non-uniformity of the filtered particulate deposit;
b) distorsion of the fibre distribution by application
of the structure counting criteria;
c) variation between microscopists in their interpre-
tation of the fibrous structures;
d) variation between microscopists in their ability to
detect and identify fibres.
The 95 % confidence interval about the rnean for a
single structure concentration measurement using
this analyticai method should be a�proximately
± 25 % when 100 structures are counted over 10 grid
openings.
10.3.2 Accuracy
There is no independent method available to deter-
mine the accuracy.
NOTE 11 It has been demonstrated that, after
polycarbonate membrane filters have been coated with
carbon, particulate material is transferred to the TEM
specimens without measurable losses. However, if the fil-
ters are heavily loaded by particulate material, some of this
may be lost before they are coated with carbon. Good
comparabiliry between the capillary-pore polycarbonate pro-
E
o ISO
cedure and the cellulose ester filter procedure has been
demonstrated for laboratory�enerated aerosols of
chrysotile asbestos.
10.3.3 I�terlaboratory and intralaboratory
analyses
Interlaboratory and intralaboratory analyses are re-
quired in order to monitor systematic errors that may
develop among microscopists when using this
method. These analyses should be designed to test
both the overall method and the performance of indi-
vidual microscopists. Repeating preparation of TEM
grids from different sectors of a filter, followed by
examination of the grids by a different microscopist,
is a test for the reproducibility of the whole method.
However, non-uniformity of the particulate deposit on
the fiiter may lead to differences which are not related
to the performance of the microscopists. Verified fibre
counting (counting of asbestos structures on the
same grid opening of a TEM grid by two or more op-
erators, followed by resolution of any discrepancies)
may be used both as a training aid and to determine
the performance of different microscopists. The use
of indexed TEM grids as described in 7.4.1 and 7.4.2
is recommended in order to facilitate relocation of
specific grid openings.
10.4 Limit of detection
The limit of detection of the method can be varied by
` choice of the area of the collection filter, the volume
of air sarripled and the area of the specimen examined
in the TEM. It is also a function of the background of
asbestos structures on unused filters. A limit of de-
tection shall be quoted for each sample analysis.
_ NOTE 12 In practice, the ►owest limit of detection is fre-
, quently determined by the total suspended particulate con-
centration, since each particle on the filter must be
separated from adjacent ones by a distance large enough
for the particle to be identified without interference.
Particulate loadings on sampling filters greater than
25 µg�cm2 usually preclude preparation of TEM specimens
by the direct methods. If the analysis is to be performed
with an acceptable expenditure of time, the area of the
specimen examined in the TEM for structures of ali sizes is
limited in most cases to between 10 and 20 grid openings.
In typical ambient or building atmospheres, it has been
found that an analytical sensitiviry of 1 structure�l can be
achieved. In some circumstances, where the atmosphere is
exceptionaily clean, this can be reduced to 0,1 structure/I
or �ower. For fibres and bundles longer than 5 µm, the re-
duced magnifications specified permit larger areas of the
TEM specimens to be examined with an acceptable ex-
penditure of time, resulting in proportionately lower limits
of detection. If no structures are found in the analysis, the
, upper 95 % confidence limit can be quoted as the upper
ISO 10312:1995(Ei
boundary of the concentration, corresponding to 2,99 time�
the analytical sensitiviry if a Poisson distribution of struc•
tures on the filter is assumed. This 95 °/a confidence limil
for 0 structures counted is taken as the detection limit.
Since there is sometimes contamination of unused sampies
filters by asbestos structures, this should also be taken into
account in the discussion of limits of detection.
11 Test report
The test report shall include at least the foliowing in-
formation:
a) reference to this International Standard;
b) identification of the sample;
c) the date and time of sampling, and all necessary
sampling data;
d) the date of the analysis;
e) the identity of the analyst;
f) any procedure used that is not specified in this
International Standard or regarded as optional;
g? a complete listing of the structure counting data
(the following data shouid be included: grid open-
ing number, structure number, identification cate-
gory, structure type, length and width of the
structure in micrometres, and any comments
concerning the structure);
h) a statement of the minimum acceptable identifi-
cation category and the maximum identification
category attempted (refer to tables D.1 and D.21;
i) a statement specifying which identification and
structure categories have been used to calculate
the concentration values;
j) separate concentration values for chrysotile and
amphibole structures, expressed in number of
asbestos structures per litre;
k) the 95 % confidence interval limits for the con-
centration values, expressed in number of
asbestos structures per litre;
I) the analytical sensitivity, expressed in number of
asbestos structures per litre;
m) the limit of detection, expressed in number of
asbestos structures per litre;
n) compositional data for the principal varieties of
amphibole, if present;
19
IS0 10312:1995�E)
0) items g) to m) for asbestos fibres and bundles
longer than 5 µm;
�. �
�
p) items g) to m) for PCM equivalent asbestos fibres
and bundles.
An exampie of a suitable format for the structure i
counting data is shown in figures 6 and 7.
Sample analysis information (page 1)
Laboratory name Report number
Sample: 456 Queen Street
Ashby de la Zouch
Exterior sample 1991-09-09
Date
Air volume:
Area of collection fiiter: 2 150,0 litres
Levei of analysis (chrysotile}: 385,0 mm2
Level of analysis (amphibole): CD or CMQ
Magnification used for fibre counting: ADQ
x 20 500
Aspect ratio for fibre definition: 5/1
Mean dimension of grid openings: 95,4 µm
initials of analyst: �MW
Number of grid openings examined: 10
Analytical sensitivity: 1,968 structuresii
Number of primary asbestos structures: � 3
Number of asbestos structures counted: 26
Number of asbestos structures > 5 µm : �
Number of asbestos fibres and bundles > 5 µm : 10
Number of PCM equivalent asbestos structures: 3
Number of PCM equivalent asbestos fibres: 5
Figure 6— Example of format for reporting sample and preparation data
20
o ISO
Sample analysis information (pages 2 and following)
Laboratoriy name Report number
Sample: 456 Queen Street
Ashby de la Zouch
Exterior sample 1991-09-09
TEM asbestos structure count - Raw data
Date
ISO 70312:1995(Ej
Numbe� of
Grid Grid �ructures �dentifi- Structure Length Width Comments
opening cation>> type
primary total µm µm
A F4-4 1 1 CD F 1,7 0,045
2 2 CMQ B 2,6 0,09
3 3 ADQ F 4,0 0,15 Crocidolite
E3-6 4 4 CD MC+O 3,5 1,3
E5-1 5 CD MD43 7,5 5,0
5 CD MB 7,7 0,30
6 CMQ MF 5,6 0,045
7 CD MB 5,1 0,30
8 CD MF 1,7 0,045
B F4-1 6 CD CD+O 6,5 3,0
9 CD CB 3,5 0,15
10 CD CF 3,5 0,045
11 CMQ CR+O 2,6 1,9
G5-1 7 CD CD31 6,1 3,2
12 CD CB 5,6 0,3
13 CMQ CF 4,0 0,045
14 CMQ CB 3,2 0,090
E4-4 8 15 CD B 1,5 0,23
9 16 AD F 8,7 0,15
C G4-4 10 CMQ CD42 25 5,6
17 CMQ CB 15 0,15
18 CMQ CF 9,4 0,045
19 ADQ CF 3,6 0,30 Tremolite
20 CM CF 4,2 0,045
E4-4 No tibres
E5-6 11 ADQ CD+3 9,4 2,5
21 ADQ CF 7,1 0,30 Amosite
22 ADQ CF 6,2 0,10 Crocidolite
23 CM CB 5,1 0,2
24 CM CR+O 3,3 1,8
F4-1 12 25 CMQ MC10 3,7 2,1
13 26 CD CC+O 7,4 0,5
1) Identification codes listed in tables D.1 and D.2.
Figure 7- Example of format for reporti�g structure counting data
21
ISO 10312:9995(E)
� ISO
Annex A
(normative)
Determination of operating conditions for plasma asher
A.1 Generai
During the preparation of TEM specimens from an
MEC or cellulose nitrate filter, the spongy structure
of the filter is collapsed into a thinner film of polymer
by the action of a solvent. Some of the particles on
the surface of the original filter become completely
buried in the polymer, and the specimen preparation
procedure incorporates a plasma etching step to
oxidize the surface layer of the polymer. Particles
buried by the filter coilapsing step are then exposed
so that they can become subsequently affixed to the
evaporated carbon fiim without altering their position
on the original filter. The amount of etching is criticai,
and individual ashers vary in performance. Therefore,
the piasma asher (7.3.4) shafl be calibrated to give a
known amount of etching of the surface of the col-
lapsed filter. This is carried out by adjusting the
radio-frequency power output and the oxygen flow-
rate, and measuring the time taken to completely
oxidize an uncollapsed cellulose ester filter with
25 mm diameter of the same type and pore size as
those used in the analysis.
22
A.2 Procedure
Place an unused cellulose ester fiiter, with 25 mm di-
ameter, of the same type as that being used, in the
centre of a glass microscope slide. Position the slide
approximately in the centre of the asher chamber.
Close the chamber and evacuate to a pressure of ap-
proximately 40 Pa, while admitting oxygen to the
chamber at a rate of 8 miJmin to 20 ml/min. Adjust
the tuning of the system so that the intensity of the
plasma in maximized. Measure the time required for
complete oxidation of the filter. Determine operating
parameters which resuit in complete oxydation of the
filter in a period of approximately 15 min. For etching
of coliapsed filters, these operating parameters shail
be used for a period of 8 min.
NOTE 13 Piasma oxidation at high radio-frequency pow-
ers will cause the filter to shrink and cur.l, foilowed by sud-
den violent ignition. At lower powers, the filter wiil remain
in position and wi�i slowly become thinner until it is nearly
transparent. It is recommended that a radio-frequency
power be used such that violent ignition does not occur.
When multiple filters are etched, the rate of etching is re-
duced, and the system should be calibrated accordingly.
_ o ISO ISO 10312:1995(E►
a
Annex B
(normative)
Calibration procedures
B.1 Calibration of the TEM
B.1.1 Calibration of TEM screen
magnification
The electron microscope should be aligned according
to the specifications of the manufacturer. initially, and
at regular intervals, calibrate the magnifications used
for the analysis using a diffraction grating replica
(7.3.11). Adjust the specimen height to the eucentric
position before carrying out the calibration. Measure
the distance on the fluorescent viewing screen occu-
pied by a convenient number of repeat distances of
the grating image, and calculate the magnification.
Always repeat the calibration after any instrumental
maintenance or change of operating conditions. The
magnification of the image on the viewing screen is
not the same as that obtained on photographic plates
or film. The ratio between these is a constant value
for the particular model of TEM.
6.1.2 Calibration of ED camera constant
Calibrate the camera constant of the TEM when used
in ED mode. Use a specimen g�id supporting a carbon
film on which a thin film of gold has been evaporated
or sputtered. Form an image of the gold film with the
specimen adjusted to the eucentric position and se-
lect ED conditions. Adjust the objective lens current
to optimize the pattern obtained, and measure the di-
ameters of the innermost two rings either on the flu-
orescent viewing screen or on a recorded image.
Calculate the radius-based camera constant, aL, for
both the fluorescent screen and the photographic
plate or film, using the following equation:
u _ aD
2,0 h2 + k2 + l2
where
� is the wavelength, in nanometres, of the
incident electrons;
G is the camera length, in millimetres;
a is the unit cell dimension of gold, in
nanometres (= 0,407 86 nm1;
D is the diameter, in millimetres, of the (hk!)
diffraction ring.
Using goid as the calibration material, the radius-
based camera constant is given by
aL = 0,117 74D mm•nm (smallest ring)
�L = 0,101 97D mm•nm (second ring)
B.2 Calibration of the EDXA system
Energy calibration of the EDXA system for a low en-
ergy and high energy peak shall be performed regu-
larly. Calibration of the intensity scale of the EDXA
system permits quantitative composition data, at an
accuracy of about 10 % of the elemental concen-
tration, to be obtained from EDXA spectra of refer-
ence silicate minerals involving the elements Na,
Mg, AI, Si, K, Ca, Mn and Fe, and applicable certified
reference materials. If quantitative determinations ai-e
required for minerals containing other elements, ref-
erence standards other than those referred to below
will be required. Weli-characterized mineral standards
permit calibration of any TEM-EDXA combination
which meets the instrumental specifications of 7.3.1
and 7.3.2, so that EDXA data from different instru-
ments can be compared. Reference minerals are re-
quired for the calibration; the criteria for selection
being that they should be silicate minerals with ma-
trices as close as possible to those of the amphiboles
or serpentine, and that small individual fragments of
the minerals are homogeneous in composition within
a few percent.
Determine the compositions of these standards by
electron microprobe analysis or chemicals methods.
Crush fragments of the same selected mineral stan-
dards and prepare filters by dispersal of the crushed
material in water and immediate filtration of the sus-
pensions. Prepare TEM specimens from these�filters
according to the procedures specified in ciause 9.
These TEM specimens can then be used to calibrate
any TEM-EDXA system so that comparable composi-
23
130 10312:1995(E)
tional results can be obtained from different instru-
ments.
NOTES
14 The microprobe analysis of the mineral standards are
carried out by conventional techniques which can be found
in annex J. The mineral is first embedded in a mount of
poly(methyl methacrylate) or epoxy resin. The mount is then
ground and polished to achieve a flat, polished surface of
the mineral fragment. This surface is then analysed, using
suitable reference standards, preferably oxide standards of
the individual elements wherever these are available. It is
necessary to take into account the water concentration in
the minerals, which in the case of chrysotile amounts to
13 % by mass. This water content may vary due to losses
in the vacuum system.
15 Aqueous suspensions of mineral standards should be
filtered immediately after preparation, since alkali and alkali
earth metals may be partially leached from minerals con-
taining these elements.
Express the results of the electron microprobe ana-
lyses as atomic or mass percentage ratios relative to
silicon. X-ray peak ratios of the same elements rela-
tive to silicon, obtained from the EDXA system, can
then be used to calculate the relationship between
peak area ratio and atomic or mass percentage ratio.
The technique was described by Cliff and Lorimer
(see annex J, reference [8)).
The X-rays generated in a thin specimen by an inci-
dent electron beam have a low probability of interact-
ing with the specimen. Thus, mass absorption and
fluorescence effects are negligible. In a silicate min-
eral specimen containing element i, the following
equation can be used to perform quantitative analyses
in the TEM:
C• A•
� — k� X ,
Cs� As
where
C; is the concentration or atomic percentage
of element i;
CS; is the concentration or atomic percentage
of silicon;
24
� ISO
A; is the elementaf integrated peak area for
element i;
AS; is the elemental integrated peak area for
silicon;
k; is the k-ratio for element i relative to sili-
con.
For a particular instrumental configuration and a par-
ticular particle size, the value of k; is constant.
To incorporate correction for the particle size effect
on peak area ratios (see annex J, references [35] and
[36], extend the Cliff and Lorimer technique by ob-
taining separate values of the constant k; for different
ranges of fibre diameter. It is recommended that 20
EDXA measurements be made for each range of fibre
diameters. Suitable ranges of fibre diamete� are:
< 0,25 µm; 0,25 µm to 0,5 µm; 0,5 µm to 1,0 µm;
> 1,0 µm.
Insert the TEM grid into the transmission electron
microscope, obtain an image at the calibrated higher
magnification of about x 20 000, and adjust the spec-
imen height to the eucentric point. If the X-ray detec-
tor is a side-entry variety, tilt the specimen towards
the X-ray detector. Select an isolated fibre or particle
less than 0,5 µm in width, and accumulate an EDXA
spectrum using an electron probe of suitable diam-
eter. When a well-defined spectrum has been ob-
tained, perform a background subtraction and
calculate the background-corrected peak areas for
each element listed, using energy windows centred
on the peaks. Calcu�ate the ratio of the peak area for
each specified element relative to the peak area for
silicon. All background-subtracted peak areas used for
calibration shall exceed 400 counts.
Repeat this procedure for 20 particles of each mineral
standard. Reject analyses of any obviousiy foreign
particles. Calculate the arithmetic mean concentration
to peak area ratio, k; (k-ratio), for each specified ele-
ment of each mineral standard and for each of the fi-
bre diameter ranges. Periodic routine checks shall be
carried out to ensure that there has been no degra-
dation of the detector performance. These k-ratios are
used to calculate the elem�ntal concentrations of un-
known fibres, using the Cliff and l.orimer relationship.
. o ISO
(SO 10312:1995(E)
Annex C
(normative)
Structure counting criteria
C.1 General
In addition to isolated fibres, other assemblages of
particles and fibres frequently occur in air samples.
Groupings of asbestos fibres and particles, referred to
as "asbestos structures", are defined as fibre bun-
dles, clusters and matrices. The numerical resu�t of a
TEM examination depends largely on whether the
analyst assigns such an assemblage of fibres as a
; single entity, or as the estimated number of individual
fibres which form the assemblage. It is therefore im-
portant that a logical system of counting criteria be
defined, so that the interpretation of these complex
structures is the same for ali analysts, and so that the
numerical result is meaningful. Imposition of specific
structure-counting criteria generally requires that
some interpretation, partially based on uncertain in-
formation on health effects, be made of each
asbestos structure found. It is not the intention of this
International Standard to make any interpretations
based on health effects, and it is intended that a clear
separation shall be made between recording of struc-
. ture counting data, and later interpretation of those
data. The system of coding specified in this Interna-
tionai Standard permits a clear morphological de-
scription of the structures to be recorded in a concise
manner suitable for later interpretation, if necessary,
by a range of different criteria, without the necessity
for re-examination of the specimens. In particular, the
coding system is designed to permit the dimensions
of each complex fibrous structure, and also whether
these structures contain fibres longer than 5 µm, to
' be recorded. This approach permits later evaluations
of the data to include considerations of particle
respirability and comparisons with historical indices
of asbestos exposure. Exampies of the various types
of morphological structure, and the manner in which
these shall be recorded, are shown in figure C.1.
C.2 Structure definitions and treatment
Each fibrous structure that is a separate entity shall
be designated as a primary structure. Each primary
structure shall be designated as a fibre, bundle, clus-
ter or matrix.
C.2.1 Fibre
Any particle with parallel or stepped sides, of mini-
mum length 0,5 µm, and with an aspect ratio of 5/1
or greater, shall be defined as a fibre. For chrysotile
asbestos, the single fibril shall be defined as a fibre.
A fibre with stepped sides shall be assigned a width
equai to the average of the minimum and maximum
widths. This average shall be used as the width in
determination of the aspect ratio.
C.2.2 Bundle
A grouping composed of apparently attached parallei
fibres shall be defined as a bundle, with a width equal
to an estimate of the mean bundle width, and a length
equal to the maximum length of the structure. The
overall aspect ratio of the bundle may have any value,
provided that it contains individual constituent fibres
with aspect ratios equal to or greater than 5/1. Bun-
dles may exhibit diverging fibres at one or both ends.
C.2.3 Cluster
An aggregate of two or more randomly oriented fi-
bres, with or without bundles, shall be defined as a
cluster. Clusters occur as two varieties.
C.2.3.1 disperse cluster (type D): Disperse and
open network, in which at least one of the individual
fibres or bundles can be separately identified and its
dimensions measured;
C.2.3.2 compact cluster (type C): Complex and
tightly bound network, in which one or both ends of
each individual fibre or bundle is (are) obscured, such
that the dimensions of individual fibres and bundles
cannot be unambiguously determined.
In practice, clusters can occur in which the character-
istics of both types of cluster occur in the same
structure. Where this occurs, the structure should be
defined as a disperse cluster, and then a logical pro-
cedure should be followed by recording structure
components according to the counting criteria. The .
procedure for treatment of ciusters is illustrated by
examples in figure C.2.
25
ISO 10312:1995(E)
26
a) Disperse cluster (type D)
c) Disperse matrix (type D)
�. �
Fibres
Bundles
, •, ��
� ..�
,;�� �� ��.
i�; :, �
' /'' :
. �..
b) Compact cluster (type C�
d► Compact metrix (type C)
Figure C.1 — Fundamental morphological structure types
�
o ISO
L 1
5µm
5µm
5 µm
5µm
ISO 10312:1995{E)
Count as 1 compact cluster containing more than 9 fi-
bres (all fibres shorter than 5 µm)
Record as CC+O
Count as 1 disperse cluster consisting of 5 fibres, 4
of which are longer than 5 µm
Record as CD54, followed by 5 fibres, each recorded
as CF
Count as 1 disperse cluster consisting of 4 fibres, 2
of which are longer than 5 µm, and 2 cluster residuais,
each containing more than 9 fibres
Record as CD+2, followed by 4 fibres, each recorded
as CF, and 2 cluster residual, each recorded as CR+O
Count as 1 disperse cluster consisting of 3 fibres, 2
bundles, 1 of which is longer than 5 µm, and 1 cluster
residual containing more than 9 fibres
Record as CD+1, followed by 3 fibres, each recorded
as CF, 2 bundles, each recorded as CB, and 1 cluster
residual recorded as CR+O
Figure C.2 — Examples of recording of complex asbestos clusters
27
ISO 1Q312:7995�E)
C.2.4 Matrix
One or more fibres, or fibre bundles, may be attached
to, or partially concealed by, a single particle or group
of overlapping nonfibrous particles. This structure
shall be defined as a matrix. The TEM image does not
discriminate between particles which are attached to
fibres, and those which have by chance overlapped in
the TEM image. (t is not known, therefore, whether
such a structure is actually a complex particle, or
whether it has arisen by a simple overlapping of par-
ticies and fibres on the filter.
Since a matrix structure may invoive more than one
fibre, it is important to define in detail how matrices
shall be counted. Matrices exhibit different character-
istics, and two types can be defined.
C.2.4.1 disperse matrix (type D): Structure con-
sisting of a particle or linked group of particles, with
overlapping or attached fibres or bundles in which at
least one of the individual fibres or bundles can be
separately identified and its dimensions measured.
C.2.4.2 compact matrix (type C): Structure con-
sisting of a particie or linked group of particles, in
which fibres or bundles can be seen either within the
structure or projecting from it, such that'the dimen-
sions of individual fibres and bundles cannot be un-
ambiguously determined.
In practice, matrices can occur in which the charac-
teristics of both types of matrix occur in the same
structure. Where this occurs, the structure should be
assigned as a disperse matrix, and then a logical pro-
cedure should be followed by recording structure
components according to the counting criteria. Exam-
ples of the procedure which shall be followed are
shown in figure C.3.
C.2.5 Asbestos structure larger than 5 µm
Any fibre, bundle, cluster or matrix for which the
largest dimension exceeds 5 µm. Asbestos structures
larger than 5 µm do not necessarily contain asbestos
fibres or bundles longer than 5 µm.
28
� ISO �
C.2.6 Asbestos fibre or bundle longer than
5 µm
An asbestos fibre of any width, or bundie of such fi-
bres, which has a lengtn exceeding 5 µm.
C•2.7 PCM equivalent structure ,
Any fibre, bundle, cluster or matrix with an aspect ra-
tio of 3/1 or greater, longer than 5 µm, and which has
a diameter between 0,2 µm and 3,0 µm. PCM equiv-
alent structures do not necessarily contain fibres or
bundles longer than 5 µm, or PCM equivalent fibres.
C•2•8 PCM equivalent fibre
Any particie with parallel or stepped sides, with an
aspect ratio ot 3/1 or greater, longer than 5 µm, and
which has a diameter between 0,2 µm and 3,0 µm.
For chrysotile, PCM equivalent fibres will always be
bundles.
C.3 Other structure counting criteria
C.3.1 Structures which intersect grid bars
A structure which intersects a grid bar shall only be
counted on two sides of the grid opening, as illus-
trated in figure C.4. Record the dimensions of the
structure such that the obscured portions of compo-
nents are taken to be equivalent to the unobscured
portions, as shown by the broken lines in figure C.4.
For example, the length of a fibre intersecting a grid
bar is taken to be twice the unobscured length.
Structures intersecting either of the other two sides
shali, not be included in the count.
C.3.2 Fibres which extend outside the field
of view
During scanning of a grid opening, count fibres which
extend outside the field of view systematically, so as
to avoid double-counting. In general, a rule should be
established so that fibres extending outside the field
of view in only two quadrants are counted. The pro-
cedure is illustrated by figure C.S. Measure the length
of each of these fibre by moving the specimen to lo-
cate the other end of the fibre, and then return to the
original field of view before continuing to scan the
specimen. Fibres without terminations within the field
of view shall not be counted.
�
o ISO
I i
5µm
( I
5µm
L I
5µm
ISO 10312:1995(E)
Count as 1 compact matrix, with all fibres shorter than
5 µm
Record as MC+O
Count as 1 disperse matrix consisting of 1 fibre shorter
than 5 µm
Fiecord as MD10, followed by 1 fibre recorded as MF
Count as 1 disperse matrix consisting of 5 fibres, all
longer than 5 µm
Record as MD55, followed by 5' fibres, each recorded
as MF
Count as 1 disperse matrix, consisting if 3 fibres, 1 of
which is longer than 5 µm, and 1 matrix residual con-
taining 3 fibres
Record as MD61, followed by 3 fibres, each recorded
as MF, and 1 matrix residuai recorded as MR30
5 µm
Figure C.3 — Examples of recording of complex asbestos matrices
29
ISO 10312:1995(E)
�
• •.
Scan direction ; � : •
. _ ....
Grid opening
� ' • �...,,���
Figure C.4 — Example of counting of structures which intersect grid bars
Scan direction
Count O�IIII�'IiIND '�—TEM field of view
Do not count
Do not count
Grid opening
Figure C.5 — Example of counting of fibres which extend outside the field of view
30
� ISO p
e
, m o ISO ISO 10312:1995(E1
<
C.4 Procedure for data recording
C.4.1 General
The morphological codes specified are designed to
facilitate computer data processing, and to allow re-
cording of a complete representation of the important
features of each asbestos structure. The procedure
requires that the microscopist classify each primary
fibrous structure into one of the four fundamental
categories: fibres, bundles, clusters and matrices.
C.4.2 Fibres
On the structure counting form, a fibre as defined in
C.2.1 shall be recorded by the designation "F". If the
fibre is a separately-counted part of a cluster or ma-
trix, the fibre shall be recorded by the designation
"CF", or "MF", depending on whether it is a compo-
nent of a cluster or matrix.
C.4.3 Bundles
On the structure counting form, a bundle as defined
in C.2.2 shaii be recorded by the designation "B". If
the bundle is a separately-counted part of a ciuster or
matrix, the bundie shall be recorded by the desig-
nation "CB", or "MB", depending on whether it is a
component of a cluster or matrix.
C.4.4 Disperse clusters (type D)
On the structure counting form, an isolated cluster of
type D as defined in C.2.3 shall be recorded by the
designation "CD", foliowed by a two-digit number.
The first digit represents the analyst's estimate of the
total number of fibres and bundles comprising the
structure. The digit shail be from 1 to 9, or designated
' as "+" if there are estimated to be more than 9
component fibres or bundles. The second digit shall
� represent, in the same manner, the total number of
fibres and bundles longer than 5 µm contained in the
structure. The overall dimensions of the cluster, in
two perpendicular directions representing the maxi-
mum dimensions, shall be recorded. In order of de-
creasing length, up to 5 component fibres or bundles
shall be separately recorded, using the codes "CF"
(cluster fibre) and "CB" (cluster bundle). If, after ac-
counting for prominent component fibres and bun-
dies, a group of clustered fibres remains, this shall be
recorded by the designation "CR" (ciuster residual).
If the remaining clustered fibres are present as more
than one localized group, it may be necessary to re-
cord more than one cluster residual. Do not record
more than 5 cluster residuals for any cluster. A cluster
residual shall be measured and assigned a two-digit
number, derived in the same manner as specified for
the overall c(uster. Optionally, if the number of com-
ponent fibres and bundies in either the original cluster
or the cluster residual is outside the range 1— 9, ad-
ditional information concerning the number of com-
ponent fibres and bundles may be noted in the
"comments" column.
C.4.5 Compact clusters (type C)
On the structure counting form, an isolated cluster of
type C as defined in C.2.3 shall be recorded by the
designation "CC", followed by a two-digit number.
The two-digit number describing the numbers of
component fibres and bundles shall be assigned in the
same manner as for clusters of type D. The overall
dimensions of the cluster in two perpendicular di-
rections shall be recorded in the same manner as for
clusters of type D. By definition, the constitutent fi-
bres and bundles of compact clusters cannot be sep-
arately measured; therefore, no separate tabulation
of component fibres or bundles can be made.
C.4.6 Disperse matrices (type D)
On the structure counting form, an isolated matrix of
type D as defined in C.2.4 shall be recorded by the
designation "MD", followed by a two-digit number.
The two-digit number shall be assigned in the same
manner as for clusters of type D. The overall dimen-
sions of the matrix in two perpendicular directions
shall be recorded in the same manner as for clusters
of type D. In order of decreasing length, up to 5
component fibres or bundles shall be separately re-
corded, using the codes "MF" (matrix fibre> and
"MB" (matrix bundle). If after accounting for promi-
nent component fibres and bundles, matrix material
containing asbestos fibres remains, this shall be re-
corded by the designation "MR" (matrix residual). If
the remaining matrix fibres are present as more than
one localized group, it may be necessary to record
more than one matrix residual. Do nat record more
than 5 matrix residuals for any matrix. A matrix re-
sidual shall be measured and assigned a two-digit
number, derived in the same manner as specified for
the overali matrix. Optionally, if the nurnber of com-
ponent fibres or bundles in either the original matrix
or the matrix residual is outside the range 1— 9, ad-
ditional information concerning the number of com-
ponent fibres and bundies may be noted in the
"comments" column.
C.4.7 Compact matrices (type C)
On the structure counting form, an isolated matrix of
type C as defined in C.2.4 shall be recorded by the
31
ISO 10312:1995(F)
designation "MC", followed by a two-digit number.
The two-digit number shall be assigned in the same
manner as for clusters of type D. The overall dimen-
sions of the matrix in two perpendicular directions
shall be recorded in the same manner as for clusters
of type D. By definition, the constitutent fibres and
bundles of compact matrices cannot be separately
measured; therefore, no separate tabulation of com-
ponent fibres or bundles can be made.
C.4.8 Procedure for recording of partially
obscured fibres and bundles
The proportion of the length of a fibre or bundle that
is obscured by other particulates shall be used as the
basis for determining whether a fibre or bundle is to
be recorded as a separate component or is to be
considered as a part of a matrix of type C or part of
a matrix residual. If the obscured length could not
possibiy be more than one-third of the totai length,
the fibre or bundle shall be considered a prominent
feature to be separately recorded. The assigned
length for each such partially obscured fibre or bundle
shall be equal to the visible length plus the maximum
possible contribution from the obscured portion. Fi-
bres or bundies which appear to cross the matrix, and
for which both ends can be located approximately,
shall be included in the maximum of 5 and recorded
according to the counting criteria as separate fibres
or bundles. If the obscured length could be more than
one third of the total length, the fibre or bundle shall
32
� ISO '-
be considered as a part of a compact matrix of type
C or part of a matrix residual.
C.5 Special considerations for counting
of PCM equivalent structures
Use 3/1 as the minimum aspect ratio for counting of
PCM equivalent structures. This aspect ratio defi�ition
is required in order to achieve comparability of the
resuits for this size range of structure with historicai
optical measurements, but use of this aspect ratio
definition does not significantly affect the ability to
interpret the whole fibre size distribution in terms of
a minimum 5/1 aspect ratio. Some applications may
require that a count tie made of PCM equivalent
structures only. The coding system permits discrimi-
nation between PCM equivalent structures that con-
tain fibres and bundles longer than 5 µm and those
that do not.
NOTE 16 In general, clusters and matrices will yieid
fewer components as the minimum dimensions specified
for countabie fibres are increased. Thus, it may be found
that a particular structure yields a higher number of com-
ponent fibres and bundles in a count for all fibre sizes than
it does at a reduced magnification when oniy fibres and
bundles longer than 5 µm are being counted. However, the
requirement that component fibres and bundles be recorded
in decreasing length order ensures that the data are con-
sistent for a particular structure, regardless of the size cat-
egory of fibres being counted and the magnification in use.
�
o ISO
Annex D
(normative)
Fibre identification procedure
D.1 General
The criteria used for identification of asbestos fibres
may be selected depending on the intended use of
the measurements. In some circumstances, there can
be a requirement that fibres shali be unequivocaliy
identified as a specific mineral species. In other cir-
cumstances, there can be sufficient knowledge about
the sample, so that rigorous identification of each fi-
bre need not be carried out. The time required to
perform the analysis, and therefore the cost of analy-
sis, can vary widely depending on the identification
criteria considered which are to be sufficiently defini-
tive. The combination of criteria considered definitive
for identif�cation of fibres in a particular analysis shall
be specified before the analysis is made, and this
combination of criteria shall be referred to as the
"level" of analysis. Various factors related to instru-
mentai limitations and the character of the sample
may prevent satisfaction of all of the specified fibre
identification criteria for a particular fibre. Therefore,
a record shall be made of the identification criteria
which were satisfied for each suspected asbestos fi-
bre included in the analysis. For example, if both ED
and EDXA were specified to be attempted for defini-
tive identification of each fibre, fibres with chrysotile
morphology which, for some reason, do not give an
ED pattern but which do yield an EDXA spectrum
corresponding to chrysotile, are categorized in a way
which conveys the level of confidence to be placed in
the identification.
D.2 ED and EDXA techniques
D.2.1 General
Initially, fibres are classified into two categories on the
basis of morphology: those fibres with tubular
morphology, and those fibres without tubular
morphology. Further analysis of each fibre is con-
ducted using ED and EDXA methods. The following
procedures should be used when fibres are examined
by ED and EDXA.
The crystal structures of some mineral fibres, such as
chrysotile, are easily damaged by the high current
densities required for EDXA examination. Therefore,
ISO 10312:1995(E)
investigation of these sensitive fibres by ED should
be completed before attempts are made to obtain
EDXA spectra from the fibres. When more stable fi-
bres, such as the amphiboles, are examined, EDXA
and ED may be used in either order.
D.2.2 ED techniques
The ED technique can be either qualitative or quanti-
tative. Qualitative ED consists of visual examination,
without detailed measurement, of the general char-
acteristics of the ED pattern obtained on the TEM
viewing screen from a randomly oriented fibre. ED
patterns obtained from fibres with cylindrical symme-
try, such as chrysotile, do not change when the fibres
are tilted about their axes, and patterns from randomly
oriented fibres of these minerals can be interpreted
quantitatively. For fibres which do not have cylindrical
symmetry, oniy those ED patterns obtained when the
fibre is oriented with a principal crystallographic axis
closely parallel with the incident electron beam direc-
tion can be interpreted quantitatively. This type of ED
pattern shall be referred to as a"zone-axis ED
pattern". In order to interpret a zone-axis ED pattern
quantitatively, it shail be recorded photographicaily
and its consistency with known mineral structures
shall be checked. A computer program may be used
to compare measurements of the zone-axis ED pat-
tern with corresponding data calculated from known
mineral structures. The zone-axis ED pattern obtained
by examination of a fibre in a particular orientation can
be insufficiently specific to permit unequivocal iden-
tification of the mineral fibre, but is is often possibie
to tilt the fibre to another angle and to record a dif-
ferent ED pattern corresponding to another zone-axis.
The angle between the two zone-axes can also be
checked for consistency with the structure of a sus-
pected mineral.
For visual examination of the ED pattern, the camera
length of the TEM should be set to a low value of
approximately 250 mm and the ED pattern should
then be viewed through the binoculars. This proce-
dure minimizes the possibie degradation of the fibre
by the electron irradiation. However, the pattern is
distorted by the tilt angle of the viewing screen. A
camera length of at (east 2 m should be used when
33
ISO 10312:1995(E)
the ED pattern is recorded, if accurate measurement
of the pattern is to be possible. It is necessary that,
when obtaining an ED pattern to be evaluated visually
or to be recorded, the sample height shall be properly
adjusted to the eucentric point and the image shall be
focussed in the plane of the selected area aperture.
If this is not done, there may be some components
of the ED pattern which do not originate from the
selected area. In general, it will be necessary to use
the smallest available EO aperture.
For accurate measurements of the ED pattern, an
internal calibration standard shall be used. A thin
coating of goid, or another suitable calibration mate-
rial, shall be applied to. the underside of the TEM
specimen. This coating may be applied either by vac-
uum evaporation or, more conveniently, by sputtering.
The polycrystalline gold film yields diffraction rings on
every ED pattern and these rings provide the required
calibration information.
To form an ED pattern, move the image of the fibre
to the centre of the viewing screen, adjust the height
of the specimen to the eucentric position, and insert
a suitable selected area aperture into the electron
beam so that the fibre, or a portion of it, occupies a
large proportion of the illuminated area. The size of
the aperture and the portion of the fibre shall be such
that particies other than the one to be examined are
excluded from the selected area. Observe the ED
pattern through the binoculars. During the observa-
tion, the objective lens current should be adjusted to
the point where the most complete ED pattern is ob-
tained. If an incomplete ED pattern is stili obtained,
move the particle around within the selected area to
attempt to optimize the ED pattern, or to eliminate
possible interferences from neighbouring particles.
If a zone-axis ED analysis is to be attempted on the
fibre, the sample sha�l be mounted in the appropriate
holder. The most convenient hoider allows complete
rotation of the specimen grid and tilting of the grid
about a single axis. Rotate the sample until the fibre
image indicates that the fibre is oriented with its
length coincident with the tilt axis of the goniometer,
and adjust the sample height until the fibre is at the
eucentric position. Tilt the fibre until an ED appears
which is a symmetrical, two dimensional array of
spots. 7he recognition of zone-axis alignment condi-
tions requires some experience on the part of the
operator. During tilting of the fibre to obtain zone-axis
conditions, the manner in which the intensities of the
spots vary should be observed. If weak reflections
34
� ISO
occur at some points on a matrix of strong reflections,
the possibility of twinning or multiple diffraction ex-
ists, and some caution should be exercised in the se-
lection of diffraction spots for measurement and
interpretation. A full discussion of electron diffraction
and multiple diffraction can be found in the references
by J.A. Gard C>>7 P.6. Hirsch et a1C14] and H.R. Wenck
[427 included in annex J. Not all zone-axis patterns
which can be obtained are definitive. Only those
which have closely spaced reflections corresponding
to low indices in at least one direction should be re-
corded. Patterns in which all d-spacings are less than
about 0,3 nm are not definitive. A useful guideline is
that the lowest angle reflections should be within the
radius of the first gold diffraction ring f 111), and that
patterns with smaller distances between reflections
are usually the most definitive. .
Five spots, ciosest to the centre spot, along two
intersecting lines of the zone-axis pattern shall be se-
lected for measurement, as shown in figure D.1. The
distances of these spots from the centre spot and the
four angles shown provide the required data for anai-
ysis. Since the centre spot is usually very overex-
posed, it does not provide a well-defined origin for
these measurements. The required distances shall
therefore be obtained by measuring between pairs of
spots symmetrically disposed about the centre spot,
preferabiy separated by several repeat distances. The
distances shall be measured with a precision of better
than 0,3 mm, and the angles to a precision of better
than 2,5°. The diameter of the first or second ring of
the calibration pattern (111 and 200) shall also be
measured with a precision of better than 0,3 mm.
Using gold as the calibration materiai, the radius-
based camera constant is given by
�L = 0,117 74D mm•nm (first ring)
�[. = 0,101 97D mm•nm (second ring)
D.2.3 EDXA measurements
Interpretation of the EDXA spectrum may be either
qualitative or quantitative. For qualitative interpretation
of a spectrum, the X-ray peaks originating from the
elements in the fibre are recorded. For quantitative
interpretation, the net peak areas, after background
subtraction, are obtained for the X-ray peaks originat-
ing from the elements in the fibre. This method pro-
vides quantitative interpretation for those minerals
which contain silicon. "
�
. o ISO , ISO 10312:1995(E)
�
�
Spot
�
�
Spo
• •
Spot 5
�
Spot 2 Spot 1
�
1
Figure D.1 — Example of ineasurement of zone-axis SAED patterns
To obtain an EDXA spectrum, move the image of the
fibre to the centre of the screen and remove the ob-
jective aperture. Se�ect an appropriate electron beam
diameter and deflect the beam so that it impinges on
the fibre. Depending on the instrumentation, it may
be necessary to tilt the specimen towards the X-ray
detector and, in some instruments, to use the Scan-
ning Transmission Electron Microscopy (STEM) mode
of operation.
The time for acquisition of a suitable spectrum varies
with the fibre diameter, and also with instrumental
factors. For quantitative interpretation, spectra should
have a statisticaily valid number of counts in each
peak. Analyses of small diameter fibres which contain
sodium are the most critical, since it is in the low en-
ergy range that the X-ray detector is least se�sitive.
Consequently, it is necessary to acquire a spectrum
for a period that is sufficiently long for the sodium to
be detected in such fibres. It has been found that
satisfactory quantitative an analyses can be obtained
if acquisition is continued until the background sub-
tracted silicon Ka peak integral exceeds 10 000
counts. The spectrum should then be manipulated to
subtract the background and to obtain the net areas
of the elemental peaks.
After quantitative EDXA classification of some fibres
by computer analysis of the net peak areas, it may be
possible to classify further fibres in the same sample
on the basis of comparison of spectra at the
intrument. Frequently, visua� comparisons can be
made after somewhat shorter acquisition times.
D.3 Interpretation of fibre analysis data
D.3.1 Chrysotile
The morphological structure of chrysotile is charac-
teristic, and with experience, can be recognized read-
ily. However, a few holder minerals have a similar
appearance, and morphological observation by itself
is inadequate for most samples. The ED pattern ob-
tained from chrysotile is quite specific for this minerai
if the specified characteristics of the pattern corre-
spond to those frorn reference chrysotile. However,
depending on the past history of the fibre, and on a
number of other factors, the crystal structure of a
particular fibre may be damaged, and it may not yield
and ED pattern. In this case, the EDXA spectrum may
be the only data available to supplement the
morphological observations.
D.3.2 Amphiboles
Since the fibre identification procedure for asbestos
fibres other than chrysotile can be involved and time-
consuming, computer programmes, such as that de-
veloped by B.L. Rhoades (see annex J, reference
35
ISO 1 Q312:1995(E)
[32]), are recommended for interpretation of zone-
axis ED patterns. The published literature contains
composition and crystallographic data for all of the
fibrous minerals likely to be encountered in TEM
analysis of air samples, and the compositional and
structural data from the unknown fibre should be
compared with the published data. Demonstration
that the measurements are consistent with the data
for a particular test mineral does not uniquely identify
the unknown, since the possibility exists that data
from other minerals may aiso be consistent. It is,
however, unlikely that a mineral of another structural
class could yield data consistent with that from an
amphibole fibre identified by quantitative EDXA and
two zone-axis ED patterns.
Suspected amphibole fibres should be classified ini-
tially on the basis of chemical composition. Either
qualitative or quantitative EDXA information may be
used as the basis for this classification. From the
published data on mineral compositions, a list of min-
erals which are consistent in composition with that
measured for the unknown fibre should be compiled.
To proceed further, it is necessary to obtain the first
zone-axis ED pattern, according to D.2.2.
It is possible to specify a particular zone-axis pattern
for identification of amphibole, since a few patterns
are often considered to be characteristic. Unfortu-
nately, for a fibre with random orientation on a TEM
grid, no specimen holder and goniometer currently
available will permit convenient and rapid location of
two preselected zone-axes. The most practical ap-
proach has been adopted, which is to accept those
low index patterns which are easily obtained, and then
to test their consistency with the structures of the
minerals already preselected on the basis of the EDXA
data. Even the structures of non-amphibole minerals
in this preselected list shall be tested against the
zone-axis data obtained for the unknown fibre, since
non-amphibole minerals in some orientations may
yield similar .patterns consistent with amphibole
structures.
The zone-axis ED interpretation shall inciude all min-
erals previously selected from the mineral data file as
being chemically compatible with the EDXA data. This
procedure will usually shorten the list of minerals for
which solutions have been found. A second set of
zone-axis data from another pattern obtained on the
36
� ISO
same fibre can then be processed, either as further
confirmation of the identification, or to attempt elim-
ination of an ambiguity. In addition, the angle meas-
ured between the orientations of the two zone-axes
can be checked for consistency with the structures
of the minerals. Caution should be exercised in ratio-
nalizing the inter-zone-axis angle, since if the fibre
co�tains c-axis twinning, the two zone-axis ED pat-
terns may originate from the separate twin crystals.
in practice, the full identification procedure will
normally be applied to very few fibres, unless precise
identification of all fibres is required for a particular
reason.
D.4 Fibre classification categories
It is not always possible to proceed to a definitive
identification of a fibre; this may be due to instru-
mental limitations or to the actual nature of the fibre.
In many analyses, a definitive identification of each
fibre may not actuaily be necessary if there is other
knowledge available about the sample, or if the con-
centration is below a level of interest. The analytical
procedure shall therefore take ir�to account both in-
strumentai limitations and varied analytical require-
ments. Accordingly, a system for fibre classification is
used to permit accurate recording of data. The ciassi-
fications are shown in tables D.1 and D.2, and are di-
rected towards identification of chrysotile and
amphibole respectively. Fibres shali be reported in
these categories.
The general principle to be followed in this analytical
procedure is first to define the most specific fibre
classification which is to be attempted, or the
"levei" of .analysis to be conducted. Then, for each
fibre examined, record the ciassification which is ac-
tually achieved. Depending on the intended use of the
results, criteria for acceptance of fibres as
"identified" can then be estabiished at any time after
completion of the analysis.
In an unknown sample, chrysotile wiii be regarded as
contirmed only if a recorded, calibrated ED pattern
from one fibre in the CD categories is obtained, or if
measurements of the ED pattern are recorded at the
instrument. Amphibole will be regarded as confirmed
only by obtaining recorded data which indicates ex-
clusively the presence of amphiboles for fibres clas-
sified in the AZQ, AZZ or AllQ categories.
, �
� o ISO
�
Cetegory
TM
CM
CD
CQ
CMQ
CDQ
NAM
Category
UF
AD
AX
ADX
AQ
AZ
ADQ
AZQ
AZZ
AZZQ
NAM
ISO 10312:1995(E)
Table D.1 — Classification of fibres with tubular morphology
Description
Tubufar Morphology, not sufficiently characteristic for classification as chrysotile
Characteristic Chrysotile Morphology
Chrysotile SAED pattern
Chrysotile composition by Quantitative EDXA
Chrysotile Morphology and composition by Quantitative EDXA
Chrysotile SAED pattern and composition by Quantitative EDXA
Non-Asbestos Mineral
Table D.2 — Classi�cation of fibres without tubular morphology
Description
Unidentified Fibre
Amphibole by random orientation SAED (shows layer pattern of 0,53 nm spacing)
Amphibole by qualitative EDXA. Spectrum has elemental components consistent with amphibole
Amphibole by random orientation SAED and qualitative EDXA
Amphibole by Quantitative EDXA
Amphibole by one Zone-axis SAED pattern
Amphibole by random orientation SAED and Quantitative EDXA
Amphibole by one Zone-axis SAED pattern and Quantitative EDXA
Amphibole by two Zone-axis SAED patierns, with consistent interaxial angle
Amphibole by two Zone-axis SAED patterns, with consistent interaxial angle, and Quantitative EDXA
Non-Asbestos Mineral
D.4.1 Procedure for classification of fibres
with tubular morphology suspected to be
chrysotile
Occasionally, fibres are encountered which have tu-
bular morphology similar to that of chrysotile, but
which cannot be characterized further either by ED
or EDXl�. They may be non-crystalline, in which case
ED techniques are not useful, or they may be in a
position on the grid which does not permit an EDXA
spectrum to be obtained. Alternatively, the fibre may
be of organic origin, but the morphology and compo-
sition may not be sufficiently definitive enough to 6e
disregarded. Accordingly, there is a requirement to
record each fibre, and to specify how confidently each
fibre can be identified. Classification of fibres will
meet with various degrees of success. Figure D.2
shows the ciassification procedure to be used for fi-
bres which display any tubular morphology. The chart
is self explanatory, and every fibre is either rejected
as a non-asbestos mineral (NAM), or classified in
some way which by some later criterion could still
contribute to the chrysotile fibre count.
Morphology is the first consideration, and if this is not
similar to that usually seen in chrysotile standard
samples, designate the initial classification as TM.
Regardless of the doubtful morphology, examine the
fibre by ED and EDXA methods according to
figure D.2. Where the morphology is more definitive,
it may be possible to classify the fibre as having
chrysotile morphology (CM).
37
ISO 10312:1995�E)
FIBRE WITH TUBULAR MORPHOLOGY
(
Is fibre morphology characteristic of that
displayed by reference chrysotilei
NO
TM
Examine by SAED
Pattern not Chrysotile
chrysotile pattern
Pattern not present
or indistinct
TM
Examine by quantitative EOXA
Composition not that Chrysotile
of chrysotile composition
No spectrum
TM
YES
CM
Examine by SAED
Chrysotile Pattern not
pattern chrysotile
Pattern not present
or indistinct
CM
Exami�e by quantitative EOXA
�
�����N�������� I orcnrysotue
No spectrum
CM [
Examine by qua�titative EDXA .
Composition not that Chrysotile
of chrysotite composition
No spectrum
NAM CD CDQ
Figure D.2 — Classification chart for fibre with tubular morphology
38
�
� ISO
e ISO
For classification as CM, the morphological character-
istics required are the following:
a1 the individuai fibrils should have high aspect ratios
exceeding 5/1, and be about 30 nm to 40 nm in
diameter;
b) the electron scattering power of the fibre at
60 kV to 100 kV accelerating potential should be
sufficiently low for the internal structure to be
visible;
c) there should be some evidence of an internal
structure suggesting a tubular appearance similar
to that shown by reference UICC chrysotile,
which may degrade in the electron beam.
Examine every fibre having these morphological char-
acteristics by the ED technique, and classify as
chrysotile by ED (CD) only those which give diffraction
patterns with the precise characteristics shown in
figure D.3. The relevant features in this pattern for
identification of chrysotile are as follows:
a) the (002) refiections should be examined to de-
termine that they correspond closely to a spacing
of 0,73 nm;
b) the layer line repeat distance should correspond
to 0,53 nm;
c) there shouid be "streaking" of the (110) and (130)
reflections.
Figure D.3 — Chrysotile SAED pattern
ISO 10312:1995(E)
Using the millimetre calibrations on the TEM viewing
screen, these observations can readily be made at the
instrument. If documentary proof of fibre identification
is required, record a TEM micrograph of at least one
representative fibre, and record its ED pattern on a
separate film or plate. This film or piate shall also carry
calibration rings from a known polycrystalline sub-
stance such as goid. This calibrated pattern is the only
documentary proof that the particular fibre is
chrysotile, and not some other tubular or scrolled
species such as halloysite, palygorskite, talc or
vermiculite. The proportion of fibres which can be
successfully identified as chrysotile by ED is variable,
and to some extent dependent on both the instru-
ment and the procedures of the operator. The fibres
that fail to yield an identifiable ED pattern will remain
in the TM or CM categories unless they are examined
by EDXA.
In the EDXA analysis of chrysotile there are only two
elements which are relevant. For fibre classification,
the EDXA analysis shall be quantitative. If the spec-
trum displays prominent peaks from magnesium and
silicon, with their areas in the appropriate ratio, and
with only minor peaks from other elements, classify
the fibre as chrysotile by quantitative EDXA, in the
categories CQ, CMQ, or CDQ, as appropriate.
D.4.2 Procedure for classification of fibres
without tubular morphology, suspected to be
amphibole
Every particle without tubular morphology and which
is not obviously of biological origin, with an aspect
ratio of 5�1 or greater, and having parallel or stepped
sides, shall be considered as a suspected amphibole
fibre. Further examination of the fibre by ED and
EDXA techniques will meet with a variable degree of
success, depending on the nature of the fibre and on
a number of instrumental limitations. It wiil not be
possible to identify every fibre completely, even if
time and cost are of no concern. Moreover, confir-
mation of the presence of amphibole can be acnieved
only by quantitative interpretation of zone-axis ED
patterns, a very time-consuming procedure. Accord-
ingiy, for routine samples from unknown sources, this
analytical procedure limits the requirement for zone-
axis ED work to a minimum of one fibre represen-
tative of each compositional class reported. In some
samples, it may be necessary to identify more fibres
by the zone-axis technique. When analysing samples
from well-characterized sources, the cost of identifi-
cation by zone-axis methods may not be justified.
The 0,53 nm layer spacing of the random orientation
ED pattern is not by itself diagnostic for amphibole,
However, the presence of c-axis twinning in many fi-
39
ISO 10312:1995(E)
bres leads to contributions to the layers in the pat-
terns by several individual parallel crystals of different
axial orientations. This apparently random positioning
of the spots along the layer lines, if also associated
with a high fibre aspect ratio, is a characteristic of
amphibole asbestos, and thus has some limited diag-
nostic value. If a pattern of this type is not obtained,
the identity of the fibre is still ambiguous, since the
absence of a recognizable pattern may be a conse-
quence of an unsuitable orientation relative to the
electron beam, or the fibre may be some other min-
eral species.
Figure D.4 shows the fibre classification chart to be
used for suspected amphibole fibres. This chart
shows all the classificatibn paths possible in analysis
of a suspected amphibole fibre, when examined sys-
tematically by ED and EDXA. Two routes are possible,
depending on whether an attempt to obtain an EDXA
spectrum or a random orientation ED pattern is made
first. The normal procedure for analysis of a sample
of unknown origin will be to examine the fibre by
random orientation ED, qualitative EDXA, quantitative
EDXA, and zone-axis ED, in this sequence. The final
fibre classification assigned will be defined either by
successful analysis at the maximum required level,
40
� ISO `'
or by the instrumental limitations. Any instrumental
limitations which affect the quality of the results shall
be noted. Record the maximum classification
achieved for each fibre on the counting sheet in the
appropriate column. The various classification catego-
ries can then be combined later in any desired way for
calculation of the fibre concentration. The complete
record of the results obtained when attempting to
identify each fibre can also be used to re-assess the
data if necessary.
In the unknown sample, zone-axis analysis will be re-
quired if the presence of amphibole is to be
unequivocaliy confirmed. For this level of analysis, at-
tempt to raise the classification of every suspected
amphibole fibre to the ADQ category by inspection of
the random orientation ED pattern and the EDXA
spectrum. In addition, examine at least one fibre from
each type of suspected amphibole found by zone-axis
methods to confirm their identification. In most cases,
because information exists about possible sources of
asbestos in close proximity to the air sarnpiing lo-
cation, some degree of ambiguity of identification can
be accepted. Lower levels of analysis can therefore
be accepted for these situations.
�
0 o ISO ISO 10312:1995(E)
FIBRE WITHOUT TUBULAR MORPHOLOGY
Ooes fi6re EDXA �peetrum show elemants Exemine by r�ndom
wn�istent with amphiholeT orie�t�tion SAED
VES NO
P�nern not present L.�yar p�ttern whh
NAM or indiatind 0,53 nm apxin0
No speclrum
Pettem dafinitety
� Uf not amphibole rype
UF NAM �
Doea quenti[ative EDXA
give fihre compoaition
tontiitent with
emphi6oleT Does EDXAapectrum Ooes EUXA spechvm
show elements tonaistent show elements cansistent
YES NO with emphibolel with emphibole7
NAM
NO YES YES NO
NAM AX ADx NAM
A�
No spectrum No spectrum
I� Lt zone•exi� SAED
pattem con�iatent wi�h
emphibole] UF AD
YES NO
No pattertt
An
Uniquefy
emphibole
so�ution
Is /st zone•azis SAED
�� pattern eon�i�tent with
� Does quantitative EOXA Does quentitative EDXA amphibole�
Is tst xone-axis SAEO give fibre composilion give fibre composition
pettern eoneistent with eonsietent with consi�lent with NO YES
amphi6ole) amphibofel amphibo�e7
NAM �
YES NO yES NO NO VES No petter�
qZ NAM
NAM ADn AD
No pattern
lo tat zone-axis SAED
UF Aa N� panern consistent with Are 2nd aone-axis SAED
Is tsl tone-axis SAED omphibole7 pettern �nd interexiel
atlem consiatent with angle can�ietent with
P NO VES amphi6ole7
Are 2nd ione-axia SAED amphibolei
pattemandinterexiel NAM YES NO
engle conaietent with VES NO
amphiba�e)
No pettern
� •— c
Uniquely
amphibale
�olution
No pattern
AOn
No pattern
An
Uniquely
amphibole
solution
Are 2nd zona•exi� SAED pettarn end intereziel
engle eonai�tenl with emphibolet
NO ' YES
No pattern
�a C
Uniquely
emphibole
solution
Azn
Uniquely
emphibole
wlution
U�iqualy
amphibole
w�ution
Uniquely
emphibole
solution
Figure D.4 — Classification chart for fibre without tubular morphology
41
ISO 10312:1995(E)
Annex E
(normative)
�
� ISO '
Determination of the concentrations of asbestos fibres and bundles longer
than 5 µm, and PCM equivalent asbestos fibres
In order to provide increased statistical precision and
improved analytical sensitivity for those asbestos fi-
bres and bundles longer than 5 µm, it may be decided
to perform additional fibre counting at a lower magni-
fication, taking accouni only into fibtes and bundles
within this dimensional range. The result shall be
specified as "number of asbestos fibres and bundles
longer than 5 µm". For this examination, use a mag-
nification of approximately x 10 000, and continue to
assign a morphological code to each structure ac-
cording to the procedures specified in annex C. Re-
cord fibres and bundles only if their lengths exceed
5 µm. Record cluster and matrix components only if
their lengths exceed 5 µm.
It may also be decided to provide increased statistical
precision and improved analytical sensitivity for
fibrous structures longer than 5 µm, with diameters
between 0,2 µm and 3,0 µm, which have historically
been the basis of risk estimation in the occupational
environment (PCM equivalent asbestos fibres). Use a
magnification of approximately x 5 000 for this ex-
tended fibre count. The result shall be specified as
"number of PCM equiValent asbestos fibres".
Asbestos structures within this dimensional range do
not necessarily incorporate asbestos fibres or bundles
longer than 5 µm.
42
Continue the extended sample examination until 100
asbestos structures have been counted, or until a
sufficient area of the specimen has been examined to
achieve the desired analytical sensitivity calculated
according to table 1. The grid openings examined shall
be divided approximately equally between a minimum
of two specimen grids. �
NOTES
17 The specimen area corresponding to the area of filter
examined in the PCM fibre counting methods is
0,785 mm2, and is equivalent to approximately 100 grid
openings of a 200 mesh grid.
18 Some National Standards require that asbestos fibres
longer than 2,5 µm, with diameters between 0,2 µm and
3,0 µm be counted. Use a magnification of x 5 000 for
counting fibres within these dimensional ranges.
19 The minimum aspect ratio for definition of a fibre in
PCM fibre counting methods and in some National Stan-
dards is 3/1. Use of a 3�1 aspect ratio is permitted in this
International Standard, if this aspect raiio is mentiored in
the test report.
The test reports shall include all of the items listed in
clause 11.
�
o ISO
Annex F
tnormative)
Calculation of results
F.1 General
The results should be calculated using the procedures
specified below. The results can be conveniently cal-
culated using a computer programme.
F.2 Test for uniformity of distribution of
fibrous structures on TEM grids
A chek shall be made using the chi-square test, to
determine whether the asbestos structures found on
individual grid openings are randomly and uniformly
distributed among the grid openings. If the total
number found in k grid openings is n, and the areas
of the k individual frid openings are designated A� to
Ak, then the total area of TEM specimen examined is
i=k
A=�A;
;_,
The fraction of the total area examined which is rep-
resented by the individual grid opening area, p;, is
given by A;/A. If the structures are randomly and uni-
formly dispersed over the k grid openings examined,
the expected number of structures falling in one grid
opening with area A; is np;. If the observed number of
structures found on that grid opening is n;, then
x2 _ �` �nt — nP�� 2
L, nPr
r=�
This value shall be compared with significance points
of the chi-square distribution, having (k— 1) degrees
of freedom. Significance levels lower than 0,1 % may
be cause for the sample analysis to be rejected, since
this correspond to a very inhomogeneous deposit. If
the structure count fails this test, the precision of the
result will be uncertain, and if new air samples cannot
be collected, additional grid openings may be exam-
ined or the sample may be prepared by an indirect
method.
ISO 10312:19951E)
F.3 Calculation of the analyticat
sensitivity
Calculate the required analytical sensitivity S, ex-
pressed in number of structures per litre, using the
following equation:
s = 9v
where
Af is the area, in square millimetres, of sam-
ple collection fi�ter;
A9 is the area, in square millimetres, of TEM
specimen grid opening;
k is the number of grid openings examined;
V is the volume of air sampled, in litres.
F.4 Calculation of the mean and
confidence interval of the structure
concentration
In the structure count made according to this Inter-
national Standard, a number of grid openings have
been sampled from a population of grid openings, and
it is required to determine the mean grid opening
structure count for the population on the basis of this
small sample. The interval about the sample mean
which, with 95 % confidence, contains the population
mean, is also required.
F.4.1 Calculation of the mean structure
concentration
Calculate the mean structure concentration C, ex-
pressed in number of structures per litre, using the
following equation:
C=Sn
43
ISO 10312:1995�E)
where
is the analytical sensitivity, expressed in
number of structures per litre;
is the total number of structures found on
all grid openings examined.
F.4.2 Caiculation of confidence intervals
The distribution of structures on the grid openings
should theoretically approximate to a Poisson distri-
bution. Because of fibre aggregation and size-
dependent identification effects, the actual structure
counting data often does not conform to the Poisson
distribution, particularly at high structure counts. An
assumption that the structure counting data are dis-
tributed according to the Poisson distribution can
therefore lead to confidence intervals narrower than
are justified by the data. Moreover, if the Poisson
distribution is assumed, the variance is related only to
the total number of structures counted. Thus, a par-
ticular structure count conducted on one grid opening
is considered to have the same confidence interval as
that for the same number of structures found on
many grid openings. However, the area of sample
actually counted is very smail in relation to the total
area of the filter, and for this reason, structures shall
be counted on a minimum of four grid openings taken
from different areas of the filter in order to ensure that
a representative evaluation of the deposit is made.
At high structure counts, where there are adequate
numbers of structures per grid opening to allow a
sample estimate of the variance to be made, the
distribution can be approximated to a Gaussian, with
independent values for the mean and variance. Where
the sample estimate of variance exceeds that implicit
in the Poissonian assumption, use of Gaussian statis-
tics with the variance defined by the actual data is the
most conservative approach to calculation of confi-
dence intervals.
At low structure counts, it is not possibie to obtain a
reliable sample estimate of the variance, and the
distribution also becomes asymmetric but not neces-
sarily Poissonian. For 30 structures and below, the
distribution becomes asymmetric enough for the fit
to a Gaussian to no longer be a reasonable one, and
estimates of sample variance are u�reliable. Accord-
i�gly, for counts below 31 structures, the assumption
of a Poisson distribution shail be made for calculation
of the confidence intervals.
44
r� �
F.4.3 Example of calculation of Poissonian
95 �'o confidence intervals
For total structure counts less than 4, the lower
95 % confidence limit corresponds to less than 1
structure. Therefore, it is not meaningful to quote
lower confidence interval points for structure counts
of less than 4, and the result shall be recorded as
"less than" the corresponding one-sided upper 95 %
confidence limit of the Poisson distribution, as fol-
lows:
0 structure = 2,99 times the analytical sensitivity
1 structure = 4,74 times the analyticai sensitivity
2 structures = 6,30 times the analytical sensitivity
3 structures = 7,75 times the analytical sensitivity
For total counts exceeding 4, the 95 % confidence
intervai shall be calculated using the values shown in
table F.1. Table F.1 gives the upper and lower limits
of the two-sided Poissonian 95 % confidence interval
for structure counts up to 470.
F.4.4 Example of calculation of Gaussian
95 % confidence intervals
Calculate the sampie estimate of variance s2 using the
following equation:
i=k
�(n; — nPr�Z
sz = ' _'
(k-1)
where
n; is the number of structures on the ith grid
opening;
n is the total number of structures found in
k grid openings;
p; is the fraction of the total area examined
represented by the ith grid opening;
k is the number of grid openings examined.
If the mean value of the structure count is calculated
to be n, the upper and lower values of the Gaussian
95 % confidence interval are given respectively by
and
n ts
�=k+�
k
�
o ISO
n ts
� k V
k
where
�„
4
n
r
s
k
is the upper 95 % confidence limit;
is the lower 95 % confidence limit;
is the total number of structures in all grid
openings examined;
is the value of Student's test (probability
0,975i for (k — 1) degrees of freedom;
is the standard deviation (square root of
sample estimate of variance);
is the number of grid openings examined.
F.4.5 Summary of procedure for calculation
of results
In summary, structure counting data shall be calcu-
lated as foilows:
No structures detected
The structure concentration shall be reported as
less than the concentration equivalent ot the one-
sided upper 95 % confidence limit of the Poisson
distribution. This is equal to 2,99 times the analyt-
ical sensitivity.
From 1 to 3 structures
When 1 to 3 structures are counted, the result
shall be reported as less than the corresponding
one-sided upper 95 % confidence limit for the
Poisson distribution. These are
1 structure = 4,74 times the analytical sensi-
tivity
2 structures = 6,30 times the analytical sensi-
tivity
3 structures = 7,75 times the analytical sensi-
tivity
From 4 to 30 structures
The mean structure concentration and the 95 %
confidence intervals shall be reported on the basis
of the Poissonian assumption, using the values
shown in table F.1.
ISO 10312:1995(E)
More than 30 structures
When more 30 structures are counted, both the
Gaussian 95 % confidence interval and the
Poissonian 95 % confidence interval shall be cal-
culated. The larger of these two intervals shall be
used to express the precision of the structure
concentration. When the Gaussian 95 % confi-
dence interval is selected for data reporting, the
Poissonian 95 % confidence interval shall also be
mentioned.
F.5 Calculation of structure length,
width, and aspect ratio distributions
The distributions ail approximate to logarithmic-
normal, and therefore the size range intervais for cal-
culation of the distribution shall be spaced
logarithmicaily. The other characteristics required for
the choice of size intervals are that they should allow
for a sufficient number of size classes, while still re-
taining a statistically.valid number of structures in
eacti class. Interpretation is also facilitated if each size
class repeats at 10 intervals, and if 5 µm is a size ciass
boundary. A ratio from one class to the next of 1,468
satisfies all of these requirements and this value shall
be used. The distributions, being approximately
logarithmic-normal, when presented graphically, shall
be plotted using a logarithmic ordinate scale and a
Gaussian abscissa.
F.5.1 Calculation of structure length
cumulative number distribution
This distribution allows the fraction of the total num-
ber of structures either shorter or longer than a given
length to be determined. It is calculated using the
following equation:
i=k
�n'
C'�}��k = �_ p x 100
�n;
r=i
where
C(P)k is the cumulative number percentage of
structures which have lengths less than
the upper bound of the kth class;
n; is the number of structures in the rth
length class;
P is the total number of length classes.
45
ISO 10312:1995(Ej
�, �
s
F.5.2 Calculation of structure width
cumulative number distribution
This distribution allows the fraction of the total num-
ber of structures either narrower or wider than a given
width to be determined. It is calculated in a similar
way to that used in F.5.1, but using the structure
widths.
F.5.3 Calculation of structure aspect ratio
cumulative number distribution
This distribution allows the fraction of the total num-
ber of structures which have aspect ratios either
smaller or larger than a given aspect ratio to be de-
termined. It is calculated in a similar way to that used
in F.5.1, but using the structure aspect ratios.
Table F.1 - Upper and lower limits of the Poissonian 95 9'o confidence intervai of a count
Structure Structure Structure
count �ower limit Upper limk Lower limit Upper limit
count count �ower limh Upper limit
� 0 3,689�� 46 33,678 61,358 92 74,164 112,83
� 0,025 5,572 47 34,534 62,501 93 75,061 113,94
z 0,242 7,225 48 35,392 63,642 94 75,959 115,04
3 0,619 8,767 49 36,251 64,787 95 76.858 116,14
4 7,090 10,242 50 37,112 65,919 96 77,757 117,24
5 1,624 11,669 51 37,973 67,056 97 78,657 118,34
6 2,202 13,060 52 38,837 68,192 98 79,557 119,44
7 2,814 14,423 53 39,701 69,326 99 80,458 120,53
8 3,454 15,764 54 40,567 70,459 100 81,360 121,66
9 4,715 17,085 55 41,433 71,591 110 90,400 132,61
10 4,795 18,391 56 42,301 72,721 120 99,490 143,52
� 1 5,491 19,683 57 43,171 73,851 130 108,61 154,39
12 6,201 20,962 58 44,041 74,979 140 117,77 165,23
13 6,922 22,231 59 44,912 76,106 150 126,96 176,04
14 7,654 23,490 60 45,785 77,232 160 136,17 186,83
15 8,396 24,741 61 46,658 78,357 170 145,41 197,59
16 9,146 25,983 62 47,533 79,482 180 154,66 208,33
17 9,904 27,219 63 48,409 80,605 190 163,94 219,05
18 10,668 28,448 64 49,286 81,727 200 173,24 229,75
19 11,440 29,671 65 50,164 82,848 210 182,56 240,43
2� 12,217 30,889 66 51,042 83,969 220 191,89 251,10
21 13,00 32,101 67 51,922 85,088 230 201,24 261,75
22 13,788 33,309 68 52,803 86,207 240 210,60 272,39
23 14,581 34,512 69 53,685 87,324 250 219,97 283,01
24 15,378 35,711 70 54,567 88,441 260 229,36 293,62
25 16,178 36,905 71 55,451 89,557 270 238,75 304,23
26 16,983 38,097 72 56,335 90,673 280 248,16 314,82
27 17,793 39,284 73 57,220 91,787 290 257,58 325,39
28 18,606 40,468 74 58,106 92,901 300 267,01 335,96
29 19,422 41,649 75 58,993 94,014 310 276,45 346,52
30 20,241 42,827 76 59,880 95,126 320 285,90 357,08
31 21,063 44,002 77 60,768 96,237 330 295,36 367,62
32 21,868 45,175 78 61,657 97,348 340 304,82 378,15
33 22,715 46,345 79 62,547 98,458 350 314,29 388,68
34 23,545 47,512 80 63,437 99,567 360 323,77 399,20
35 24,378 48,677 81 64,328 100,68 370 333,26 409,71
36 25,213 49,840 82 65,219 101,79 380 342,75 420,22
37 26,050 51,000 83 66,111 102,90 390 352,25 430,72
38 26,890 52,158 84 67,003 104,00 400 361,76 441,21
39 27,732 53,315 85 67,897 105,11 410 371,27 451,69
40 28,575 54,469 86 68,790 106,21 420 380,79 462,18
41 29,421 55,622 87 69,684 107,32 430 390,32 472,65
42 30,269 56,772 88 70,579 108,42 440 399,85 483,72
43 31,119 57,921 89 71,474 109,53 450 409,38 493,58
44 31,970 59,068 90 72,370 110,63 460 418,92 504,04
45 32,823 60,214 91 73,267 111,73 470 428,47 514,50
t) The one-sided upper 95 °/a confidence limit for 0 structures is 2,99.
46
n
�
G
o ISO
Annex G
(informative)
Strategies for coliection of air samples
G.1 General
An important part of the sampling strategy is a state-
me�t of the purpose of the sampiing programme. A
sufficient number of samples shouid be collected so
that the site is well characterized to the precision and
accuracy desired, and also ensure that sample filters
appropriately loaded for TEM analysis are obtained
from all of the sampling locations.
G.2 Air sample collection in the
outdoors environment
Weather conditions restrict the ability to collect satis-
factory air samples in the outdoors environment, and
whenever possible, sampling should be carried out in
low-wind, low-humidity conditions. Detailed records
of the weather conditions, windspeed and direction
during the sampling period should be made. All avail-
able i�formation concerning local topography, and the
types and positions of sources should be recorded.
Sequential multipoint sampling is necessary to pro-
vide adequate characterization of complex sites and
sources. It is recommended that multiple samples are
taken upwind and downwind of the site, with a mini-
ISO 10312:1995(E)
mum of two samples in the downwind position ex-
pected to experience the maximum airborne
concentration. The locations of the samplers shouid
be carefully recorded.
G.3 Air sample collection inside
buildings
Air samples are often collected inside buildings in
which asbestos-containing construction materials are
present, in order to determine whether these materi-
als contribute to the asbestos fibre concentration in
the building atmosphere. The optimum positions for
collection of air samples can only be determined after
a complete survey of the building to establish air
movement patterns. Multiple samples should be col-
lected in the area where asbestos building materials
are present, and control samples should be collected
in an adjacent area where no airborne asbestos fibres
would be expected. The intakes for air conditioning
systems are frequently used as the collection lo-
cations for control samples. Whenever possible, static
samples should be taken over a period exceeding
4 h during normal activity in the building, at face ve-
locities of between 4 cm/s and 25 cm/s.
47
ISO 10312:1995(E)
Annex H
(informative)
Methods for removal of gypsum fibres
it is common to find fibres of calcium sulfate
(gypsum) in airborne particulates collected in buiidings
and urban environments, and particularly in samples
collected where demolition or construction work is in
progress. The fibres are readily released when plas-
ters and cement products are disturbed. In some cir-
cumstances, particles of calcite or dolomite collected
on an air filter can react with atmospheric sulfur diox-
ide, to form long fibres of gypsum. Gypsum fibres can
give rise to high fibre counts by both opticai and
electron microscopy. The gypsum fibres are often
2 µm to 6 µm long, with aspect ratios greater than
10/1. Sometimes, these fibres appear similar to
amphibole asbestos fibres, and in some samples they
can be morphologically very similar to chrysotile. In
the TEM, the larger fibres have high contrast and at
high magnification often exhibit a characteristic
mottied appearance which changes under electron
beam irradiation. Some gypsum fibres, however, are
not easily discriminated from asbestos without ex-
amination by EDXA. TEM specimens which contain
many such gypsum fibres require an extended exam-
ination time in the TEM, because it is necessary to
W
� ISO �
examine each of these fibres by EDXA before it can
be rejected.
It is possibie to remove gypsum fibres selectively by
water extraction. A Jaffe washer (7.3.7), or a
condensation washer (7.3.8), should be prepared, but
using a water (6.1) as the solvent. The TEM speci-
mens, which have been previously prepared and ini-
tially examined in the TEM, should be placed in the
washer to allow dissolution of the fibres. If a Jaffe
washer is used, the treatment time can be reduced
by heating the washer to 90 °C to 100 °C for a few
minutes. If a condensation washer is used, the
gypsum fibres wi►I be dissolved by treatment for ap-
proximately 10 min. The effect of this treatment is to
remove the gypsum fibres, leaving carbon replicas
(7.3.11) �vhich are readily distinguished from asbestos
fibres.
NOTE 20 This procedure should be used only when ex-
amination of the untreated TEM specimen grids shows the
gypsum fibres to be isolated from any asbestos fibres
present. Losses of asbestos fibres may occur if matrices
of gypsum and asbestos are exposed to this procedure.
�- a ISO ISO 10312:1995(E)
� -
;
�
f
a
Annex J
(informative?
Bibliography
[1� Asbestos International Association (1979): Ref-
erence meihod for the determination of
asbestos fibre concenfrations at workplaces by
lighi microscopy (membrane filter methodJ. AIA
health and safety publication, recommended
technical method No. 1(RTM1?. Asbestos Inter-
national Association, 68 Gloucester Place,
London, W1 H 3HL, England.
[2] BRAOLEY, D.E. (1961): Replica and shadowing
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Microscopy, B�ackwell Scientific Publications,
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[3] BuROETr, G.J. and Roo�, A.P. (1982):
Membrane-filter, direct transfer technique for
the analysis of asbestos fibres or other inorganic
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Environmenial Science and Technofogy, 17,
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[4] CAMPBELL, W.J., BLAKE, R.L., BROWN, L.L.,
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Mineralogica( definitions and identification-
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[5] CHATFIELD, E.J. (1986): Asbestos measurements
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[6] CHATFIELD, E.J. (Editor) (1987): Asbestos fibre
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Research Foundation, Sheridan Park Research
Community, Mississauga, Ontario, Canada, L5K
1 B3.
[7] CHATFIEID, E.J. and LEwis, G.M. (1980): Devel-
opment and application of an analytical tech-
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[8] CLIFF, G. and LORIMER, G.W. (1975): The quan-
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(19631: Rock-formfig minerals. Longmans,
London.
[10] Federal Register (1987): Asbestos-containing
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1987, pp. 41826-41905.
[11] GAR�, J. A. (Editor) (1971): The Electron Optical
Invesiigation of Clays. Mineralogical Society, 41
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[12] GazE, R. (1965): The physicai and molecular
structure of asbestos. Annals of the New York
Academy of Science, Vol. 132, pp. 23-30.
[13] HAWTHORNE, F.C. (1983): The crystal chemistry
of the amphiboles. Canadian Mineralogist, Voi.
21, part 2, pp. 173-480.
[14J HiRscH, P.B., HowiE, A., NiCHo�SON, R.B.,
PASHLEY, D.W. and WHELAN, M.J. (1965): Elec-
tron microscopy of thin crystais. Butterworths,
London, pp. 18-23.
[15] HOLLAHAN, J.R, and BELL, A.T. (Editors) (1974):
Techniques and applications of plasma chemis-
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[16] International Centre for Diffraction Data (1987):
Powder diffraction file. Internationai Centre for
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[17� International Mineralogical Association (1978):
Nomenclature of amphiboles (compiled by B.E.
Leake); Canadian Mineralogist Vol. 16, p. 501.
[18] international Organization for Standardization
(Organisation internationale de normalisation)
(1993): ISO 8672:1993, Air quality — Determi-
nation of the number concentration of airborne
49
ISO 10312:'9995(Ej � ISO �
inorganic fibres by phase contrast optical
microscopy — Membrane filter method.
[19] JAFFE, M.S. (1948): Handling and washing fragile
replicas. J. Applied Physics, 19, p, 1187.
[20] JoY, D.C., ROMIG, Jr. and GOLDSTEIN, J.I. (Edi-
tors) (1986): Princip/es of analytical elecfron
microscopy. Plenum Press, New York and
�ondon.
[21] LEooux, R.L. (Editor) (1979): Short course in
mine�alogical iechniques of asbestos determi-
nation. Mineralogical Association of Canada,
Department of Mineralogy, Royal Ontario Mu-
seum, 100 Queen's Park, Toronto, Ontario
Canada M5S 2C6.
tional Safety and Health, 4676 Columbia Park-
way, Cincinnati, Ohio 45226, USA.
[29] NATAEILA, M.G. (1966): Experimenial statistics:
National Bureau of Standards Handbook 91. U.S.
Government Printing Office, Washington, D.C.
20402.
[30] ORTiz, L.W. and IsoM, B.L: (1974): Transfer
technique for electron microscopy of inembrane
filter samples. American lndusirial Hygiene As-
sociacion Journal, 35, 7, pp. 423-425.
[31] PEARSON, E.S. and HARTLEY, H.Q. (1958):
Biometrica tables for statisticians, Vol. 1,
Cambridge University Press, 32 East 57th
Street, New York, N.Y. 22, USA.
[22) LEVADIE, B. (Editor) (1984): Definitions for [32) RHOADES, B.L. (1976): XJDENT-A computer
asbestos and oiher health-related silicates. technique for the direct indexing of electron dif-
ASTM Special Technical Publication 834. Ameri- fraciion spot pafterns. Research Report 70/76.
can Society for Testing and Materials, 1916 Dept. of Mechanical Engineering, Univ. of
Race Street, Philadelphia, Pennsylvania 19103, Canterbury, Christchurch, New Zealand.
USA.
[23] MICHAEL, J.R. and WILLIAMS, D.B. (1987): A
consistent definition of probe size and spatial
resolution in the analytical electron microscope.
J. Mic., 147, pp. 289-303.
[24] MICHAELS, �. and CHISSICK, S.S. (Editors) (1979):
Asbesios: Properties, Applications and Hazards,
Vol, 1, Wiley, New York.
[25] National Bureau of Standards Special Publication
506 (1978): Workshop on asbesios: definitions
and measurement methods. U.S. Government
Printing Office, Washington, D.C. 20402.
[26] National Bureau of Standards Special Publication
619 {1982): Asbestos siandards: material and
analytical methods. U.S. Government Printing
Office, Washington, D.C. 20402.
[27) National Institute for Occupational Safety and
Health (1989): N/OSH Method 7400, Revision
#3, 5(15/89. U.S. Department of Health and Hu-
man Services, Public Health Service, Centers for
Disease Control, National Institute for Occupa-
tional Safety and Health, 4676 Columbia Park-
way, Cincinnati, Ohio 45226, USA.
[28] National Institute for Occupational Safety and
Health (1989�: N/OSH Method 7402, Revision
#1, 5/15/89. U.S. Department of Health and Hu-
man Services, Public Health Service, Centers for
Disease Control, Nationai Institute for Occupa-
50'
[33] R�tvG, S.J. (1980): Identification of amphibole fi-
bers, including asbestos, using common elec-
tron diffraction patterns. In: Electron Microscopy
and X-ray Applications to Environmental and
Occupational Health Analysis, (Ed. P.A. Russeil),
Vol. II, Ann Arbor Press, Ann Arbor, Michigan
48106, USA.
[34] RuSSE��, P.A. and HUTCHINGS, A.E. (1978):
Electron Microscopy and X-ray Applications to
Environmental and Occupational Health Analy-
sis. Ann Arbor Science Pubiishers Inc., P.O. Box
1425, Ann Arbor, Michigan 48106, USA.
[35] SMALL, J.A., HEINRICH, K.F.J., NEWBURY, D.E. and
MYKLEBUST, R.L. (1979): Progress in the devel-
opment of the peak-to-background method for
the quantitative analysis of single particlas with
the electron probe. Scanning Efeciron
Microscopy/1979�11, (O. Johari, Ed.). SEM Inc.,
AMF O'Hare, Chicago, Iliinois 60666, USA.
[36] SMALL, J.A., STEEL, E.6. and SHERIDAN, P.J.
(1985): Analytical standards for the analysis of
chrysotile asbestos in ambient environments.
Analytical Chemistry, 57, pp. 204-208.
[37] SMITH, J.E. and JORDAN, M.L. (1964): Math-
ematical and graphical interpretation of the log-
normal law for particle size distribution analysis.
J. Colloid Science, 19, pp. 549-559.
[38] SPURNY, K.R., ST08ER, H„ OPELIA, H. and
WE�SS, G. (1979): On the evaluation of fibrous
.�•
o ISO
particles in remote ambient air. Science of ihe
Total Environment/1979/II, pp. 1-40.
[39] SPURNY, K.R. (Editor) (1986): Physical and
chemica! characterization of individual airborne
particles. Wiley, New York.
[40] STEEL, E.B. and SMALI, J.A. (1985): Accuracy
of transmission electron microscopy for the
analysis of asbestos in ambient environments.
Analytical Chemistry, 57, pp. 209-213.
[41] STEEI, E.B. and WYLIE, A. (1981): Mineralogical
characteristics of asbestos. In: Geology of
ISO 10312:1995(Ej
Asbestos Deposiis, (P.H. Riorden, Ed.),
SME-AIME, pp. 93-101.
[42] WENK, H.R. (Editor) (1976): Eleciron microscopy
in mineralogy. Springer-Verlag, New York.
[43] YAOA, K. (1967): Study of chrysotile asbestos by
a high resolution electron microscope. Acta
Crystallographica, 23, pp. 704-707.
[44] ZussnnaN, J. (1979): The mineralogy of asbestos.
In: Asbestos: Properties, Applications and Haz-
ards, John Wiley and Sons, pp. 45-67.
51
ISO 10312:19951E��
� ISO �
.t
�
i
i
?.
ICS 13.040.20
Descriptors: air, quality, air pollution, tests, determination, particle density (concentratioN, asbestos, microscopic analysis.
Price based on 51 pages '
QAPP
Appendix C
June 2, 2000
Revision 0
Appendix C
_ Standard Operating Procedure for the
Screening Analysis of Soil and 5ediment Samples
for Asbestos Content
SOP:EIA-INGASED2.�OP
Asbestoe in Sedimejnts/Soils
1/11/99 �
Page 1 oP 7
EPA, xeqion I
Standard operating Proa�dura for the
sornening Analyeia o! Boil and &�dimant
Samples tor Asbestos Cahta�t
Pr�pared for: Offia• o� EAvironm�nt�l Measuremant
Aad Evaluntion
�.8. EPA, &�qiott I
R�visea by: L�'vl
8aott CliiterC, at, Invsstigation�
Ax►d Analyeie Ui� t, IIdE �
, �.___,--�_ � � , f -i Y
Agprov�d by:
Ag�ea Yn n ave, Ph.D., {ZA pfficer,j
ti nd Aaalysia Uuit, Q�i$;
Approv�d by : ! a 9 /3 ( .
abert . Maxtfaid, Man�ger, =nve�tiqa�ians
Aad Aanlyeis Dnit, OF.2�E
SOP:EIA-INGASED2.Spp
Asbestos in Sedime�ts/sails
1/11/99
Page 2 of 7
St ►_
This SOP details �he sampla analysis protocol for detertnining the ashestos
cont�nt of soi2 and sediment samples. Sample clean up with a sieve
washing is followed by stereo microscope and polarized light microscope
examittation. This protocol is a semi-quantitative methed, used only far
visually estimating percentage levels of asbestos in a soil or sedimerst
sample.
2 . O Pur�►88Q r
To ensure that the protocole for analysis of aebestoe in sedime�tfsoil
samples are consietently applied by all analysts.
3 o S�agR an4 Aptlication•
This protocol is not a�'reference" method. It was de�eloped ou� oi
neceaeity to facilitate finding asbestos fibars in a soil �r muc9
(sediment) sample that does not cantain any obvious asbestos filbers or
asbestos-containing building or product materials when examined�dry (or
wet) using a et�reo microscope at 10?C or 2oX magnificatian. It;has been
used for asbestos content in order to help delineate contaminated areas.
It has proven to be an extremely sensitive method capable of f ir�ding very
small amounts of asbestos fibere in a soil or sediment matrix.
Glasaware ar ather materials, supplies, etc., mentioned below in the
pracedures are those being used in this laboratory. Other mate�ia2s may
be substituted as long as the primary purpose of the protocol is followed,
namely: to find asbestos fibers in the sample. Identification of fibrous
components is accomplished by the routina Polari$ad Liqht Micro3aogy (PLidj
(with dispersion staining) method. (See EPA approved method references on
page S,)
�.o De�initians:
PLM - Polarized Light Microacopy
5.o Ssait� aaQ safstv Warainqs•
Asbestos fibers ca� have serious etfects on your health if irihaled.
Sample contai.ners should be initially opened in the HEPA fil'kered haod. Care
must be taken when handling any unknown samples to prevent airborne a6bestos.
PLEA8E RECYCL� THI6 PApER
SOP:EIA-ZNGASED2.5flP
Asbestos in SedimentsJSoils
1/I1/99
Page 3 of �
YTI PRQC E8
1. A representative portiort of the sample is removed from the eample container
after thoraughly mixing for homogeneity� Because asbestos fibers us�ally
cannot be seen because oi the compQsition of the sample matrix such as the
dirt, sand, mud, vegetation, water, etc., steps must be taken to cle�n up �he
sample ta the point where the asbestos fibers, if any, may be seen using the
stereomicrascope at lOX to 20 X magnification. A stereomiaresoope ie maadatorp
�or this protaool. '
2. To eliminate interfering particles, a 16mm ID by 15amm long, goo� quality
PYREX or KIMAX test tube (not a fraqi2e disposable tube) is used to gemove
portiane of the well-mixed soil/sediment sample from several places in the
sample cantainer by pushing it into the sample to accumulate a sample depth of
about 2.5 inches (65mm) in the test tube. A glase or plastic stirring roc2 is
usad to push the sample down into the tube and fibez-free (tap) wate� is added
for shaking purpases. The soil and water mixture is shaken vigorously to
loosen and separate the fines and other components of tha sample and:the
cant$nts of the test tube are then poured into a 3 inch ID, 60 mesh Q250
micrometers) sieve, This serv�s to eliminate, ox greatly reducer collloidal
material, ffne sand, silt and other nan-fibrous particulates from the samp].e.
More water is added to the tube, shaken and dumped into the sieve. i�epeat this
step until the tube is clean. The sample in the sieve is then rinsed untiil
clean (clear water running through the sieve} with a fairly fine, �r�ssuri2ed
stream af water from a plastic wash bottle.
All of the material remaining in the sieve is then washed from the si,eve screen
using a stream af water from the rinse battle into a square plastic caeighing
dish of abaut looml liquid capacity. Use just enough water to compl�tely cover
the sample in the dish about 1/8th inch or so for examina�ion with tt�e stereo
microscope. �
After the cleaned sample is transferred to the weighing dieh for exa�ination,
thoroughly rinse the sieve and test tube under running tap water (pre�ferably
aerated to minfmize splashing) and carryover wilZ not be a problem from eample
to sample. It is a good idea to carry out all washirig af the sample fines over
a plastic dishpan or other container set into th� sink basin in orderito
capture the fines and keep them from clogging the eink drain trap. A,;fter a
settling period, the overlying water may be poured off and the fines%�nud
dispoaed of separately. •
PLEASE &�CYCLE T$I$ PAPER
SOP:EIA-INGA5ED2.S p
AebestQs ih sedime�ts/sails
1/12/99
Page 4 of 7
NOTE:
5ince the purpose af the tesG is to find out if the eoil or mud samg
a significant amount of asbestos (>1�) that can be identified using
technique, ��1 porticns ot tha sampl� are to be eRa.2ain�d excet�t thos
��,i.ah umas ihrQuah th� dlove
contains
PLM
3. After examining them for asbestos fibers, floating pieces of a�ganic
material such as roots, sticke, leaves, etc., may be remaved to get`a better
view af the rest of the sample in the dish. Frequently, raot struct�res iound
in surface soils will trap asbestos fibers durinq the shaking procesis and are a
good place to look for the fibers. The sample is then caraf��lY and
systematically examined under the stereo microscope at lOX-20X magnification
for visible asbestos f ibers and fiber bundles. A good, bright, fo�used light
gource such as a Nicholas transformer-base external illuminator is v�ry helpful
here. The f ibers tend to stand out, shine, flash, etc., in the clean water
matrix. Poking and stirring the �ample �uith forcepe and/or dissectiMg needles
will help to Zocate the fibers. IP no fibera are seen, gantly shaking the
weighing dish to redistribute particles will sometimes turn ug previQusly
hidden fibers when scanning the sample a secand time. Suspect fibers are
removed with sharp forceps and placed upon a c2ean microscape slide, �
4. After picking as many suspect fibers ar other material from the�sample as
necessary to determine its content, the slide preparation is allowed ta dry and
prepared for PLM analysis using an appropriate high-dispersion refractive index
liquid and coverslip.
5. xext, the slide preparation is examined with a polarized liqht microscope
(PLM) with dispersion staining to fdentify any fibers found. Standa�d, EPA
approved PLM procedures axe used to identify any asbestos fibers fourid as to
specific type and form. The identification of asbestos using PLM is rapid and
unequivocal due to the unique optical crystallographic praperties of �
morpholagy, refractive indices, elongation, angle of extinction, dispersion and
hirefringence. S1ide preps are examined for each sample with suspect fibers to
confirm the presence of asbestas.
s. If asbestos fibers are identified, return to the sieved sample u,hcler the
stereo microscope, observe the remain3ng asbestos fibers and bundles af fibers,
and make a visual estimate of the percentage asbestos content in the �ho1a
sampl• including tne materfal prevfously wash�d tbrouqh the aiave. (This is
aIl based on asbestos fibers seen using lOX to 20X magnification undes� the
stereomicroscape.) Obviously, many of the finest fibers pass through�th2 sieve
and the finest ones remaining can't be seen at 20x magnification, but., this
protocol is not me�nt to be used as a auantitative method It is useful,
hawever, ta determine whether or not the soil or aediment is contaminated with
siqnificant amounts of asbestos. (> than 1� by volume).
PL�148E RECYCLE T8I8 PAPER
SOP;EIA-IN�ASED2.SbF
Asbestos in 5edime�tsJScils
1/11/99
Page 5 of �
7. As a rule, if asbestos fibera and%or fiber bundles can't be fouD�d
relatively quickly and eaei].y (one to two minutes) in tha cleaned up�sample
under the stereo microscope, the percent ashestos contant is most likely less
than Q.1$ and certainly less than 1.0� : Ona shauld be able to find;asbestos
fibers in a salnple containing more than 1.0� in a few seconds up to a one
miriute examination under the stereo microscope.
8. Usually, as much of the original sample as possible is returned'to the
ariginal sample container. If saving the fines is required for further
examination by other methods, use individual heakers to catch the sieve
washings containing the sand and silt componants.
9. The sample containers are then resealad before storage, disposal or return
to the organization that requested the analyses.
10. If further information is required on this protoco� or if anyone has found
a better way ta find and estimate asbestos fibers in muds or soils, please
contact:
Scott Cl�.fford or Dan Boudreau
USEPA, REGION 1
6� Westview St.
Lexington, MA 02421 Telephone; (781) 860-9340
APPRQVED EPA Bi1LIt AlQALX�IB PROTaCOL;
40 CFR FART 763, SUBPART F, APPENDIX A �
or, "ASBESTOS IDENTIFICATION'�- Waiter C. McCrone, 1987, McCrone Rasearch
Institut�� Chicago, Ill.
See alsa, ",�,sbestos content In Bul.k Insulation Samples• Visual Estimat�s and
Weight ComDosS.t�on"- US EPA, EPA-560/5-88-Q11, September, 1988.
PLEABE RECYCLE TIiIB FAPE&
SQP:EIA-ZNGASED2.SIOP
Asbestos in Sedim�nts/Soils
lJll/99
Page 6 vf 7
.�� 2��lvtical procequra Adde�dum for �ora Aocur��� Ouantitatioa•
. ADDENDIIli TO "PROTOCOL SOR BCxEENI�d B�IL AND SED2M�NT SA?iPLEB FOR�ASSHBT08
CONTEI�tT DBED 8Y TH� O.B. ENFZROAII�lENTAL PAOTBCTION At�ENCY� REOZON I LABdR.AT4RY"
A+idaadum dntad: Auguat 19sT
This acidendum can be used to more accurately quantitatQ the volume o� ashestos
in soil and sediment samples. It ie meant to give the analyst a good vieual
estimate af the fine materials volume which pass through the mesh sieve
relative tg the origina2 sample volume analyzed. It must be used in
canjunction with the above mentioned protocol.
$�mple Pr�paratian Anni�tioa�. Praaedure•
1. Transfer a well mixed gortion of homogenized soil into the�plastic
weigh dish. Cover the bottom of the dish with a thin {lcmp layer.
�uantitatively transfer the soil/sediment inta the test tuba using a
wide mouth funnel. Fiber-free (tap) water can be used to �elp wash
f ines into the test tube. A qlass or plastic stirring rod�is used ta
push tha sample down into the test tube end artd to break-u$'� atly soil
clumps. Wash tha test tube sidea down with a stream of water. Let
the soilJwater mix settle such that the valume of material'in the
test tube can be measured. Measure from the bottom of the�test tube
to the top of the settled soil with a ruler and record the value
(i. e. , 4.5c1n) .
After the soil volume measurement, continue the analytical'procedure
(i.e., shake vigorously to looaen and separate the fines, �pour
contents into sieve for clean-up, transfer sample companen� left in
sieve to weigh dish for examination, etc.)
After complete examination and determination af asbestas ccpntent of
the eample portion in the weigh aish which did not pass throttgh the �
sieve (using stereo microscope and PLMj,� the sample in the wei.gh dish
is quantitatively transferred back into the tast tube and allowed to
settle. After settling, the vvlume af material in the tes�. tube is
again measured and reoorded (i.e., 2.Ocm). .
PLEASE RECYCL$ THIS PAPE&
SOP:EIA-INGASED2.SQP
Asbestos in Sedime�ts/Soils
ljll/99
Page 7 of 7 �
Determine the asbestos contant of the sample as follows:
$ asbestos in samp2e Volume of eample which
portion which did not X did not pass throuqh
pasB through the sieve �iev�
Initial sample volume
PLEABE &ECYCL� THIB P�PER
QAPP
Appendix D
June 2, 2000
Revision 0
Appendix D
ASTM Standard Test Method D 4959-00
Determination of Water (Moisture) Content
of Soil by Direct Heating
���� Designation: D 4959 — 00
Standard Test Method for
Determination of Water (Moisture) Content of Soil By Direct
Heating'
This standard is issued under the fixed designation D 4959; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses iodicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
i. Scope
1.1 This test method covers procedures for determining the
water (moisture) content of soils by drying with direct heat,
such as using a hotplate, stove, blowtorch, etc.
1.2 This test method can be used as a substitute for Test
Method D 2216 when more rapid results are desired to expe-
dite other phases of testing and slightly less accurate results are
acceptabie.
13 When questions of accuracy between this test method
and Method D 2216 arise, Method D 2216 shall be the referee
method.
1.4 This test method is applicable for most soil types. For
some soils, sueh as those containing significant amounts of
halloysite, mica, montmorillonite, gypsum, or other hydrated
materials, highly organic soils or soils that contain dissolved
solids, (such as salt in the case of marine deposits), this test
method may not yield reliable water content values.
1.5 The values stated in SI units are to be regarded as
standard.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:
D 653 Terminology Relating to Soil, Rock, and Contained
Fluids2
D 2216 Test Method for Laboratory Determination of Water
(Moisture) Content of Soil and Rock2
D 3740 Pracrice for Minimum Requirements for Agencies
Engaged in the Testing and/or Inspection of Soil and Rock
as Used in Engineering Design and Construction2
D 4753 Specification for Evaluating, Selecting, and Speci-
fying Balances and Scales for Use in Testing Soil, Rock,
and Related Construcrion Materials2
� This test method is under the jurisdiction of ASTM Committee D-18 on Soil
and Rock and is the d'uect responsibility o£ Subcommittee D18.08 on Special and
Construction Control Tests.
Current edition appcnved Mazch t0, 2000. Published Aprit 2000. Originally
published as D 4959 — 89. Last previous edition D 4959 — 89 (1994).
Z Annual Book ojASTM Standards, Vol 04.08.
Copyright O ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
3. Terminology
3.1 Definitions All definirions are in accordance with
Terms and Symbols D 653.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 direct heating—a process by which the soil is dried by
conductive heating from the direct application of heat in excess
of 110�C to the specimen container, such as provided by a hot
piate, gas stove or burner, heatlamps, or other heat sources.
Direct application of heat by flame to the specimen is not
appropriate.
3.2.2 water (moistur•e) content—the ratio, expressed as a
percentage, of the mass of water in a given mass of soil to the
mass of the solid particles.
4. Summary of Test Method
4.1 A moist soil specimen is placed in a suitabie container
and its mass is determined. It is then subjected to drying by the
application of direct heat untii dry by appearance, removed
from the heat source, and its new mass is deternuned. This
procedure is repeated until the mass becomes constant within
specified limits.
4.2 The di$'erence between the masses of the moist speci-
men and the dried specimen is used as the mass of water
contained in the specimen. The water content (expressed as a
percentage) is determined by dividing the mass of water by the
dry mass of soil, mulriplied by 100. For a given soil type and
speeimen size, the time to achieve a constant dry mass can be
noted and used to estimate drying time for subsequent tests of
the same soil type using the same size specimen and drying
apparatus.
5. Significance and Use
5.1 The water content of a soil is used throughout geotech-
nicai engineering practice both in the laboratory and in the
field. The use of Test Method D 2216 for water content
determination can be time consuming and there are occasions
when a more expedient method is desirable. Drying by direct
heating is one such method. Results of this test method have
been demonstrated to be of satisfactory accuracy for use in
field control work, such as in the deternunation of water
content, and in the determination of in-place dry unit weight of
SOIIS.
5.2 The principal objection to the use of the direct heating
q� D 4959
for water content detetmination is the possibility of overheat-
ing the soil, thereby yieiding a water content higher than would
be deternuned by Test Method D 2216. While not eliminating
this possibility, the incremental drying procedure in this test
method wil( minimize its effects. Some heat sources have
settings or controls that can also be used to reduce overheating.
Loose fitting covers or enclosures can also be used to reduce
overheating while assisting in uniform heat distribution.
53 The behavior of a soil when subjected to direct heating
is dependent on its mineralogical composition, and as a result,
no one procedure is applicable for all types of soils or heat
sources. The general procedure of this test method applies to all
soils, but test details may need to be tailored to the soil being
tested.
5.4 When this test method is to be used repeatedly on the
same or similar soil from a given site, a correction factor can
usually be deternvned by making several comparisons between
the results of this test method and Test Method D 2216. A
conection factor is valid when the difference is consistent for
several comparisons, and is reconfirmed on a regular specified
basis.
5.5 This test method may not be appropriate when precise
results are required, or when minor variarions in water content
will affect the results of other test methods, such as borderline
situations where small variations in the measured water content
could affect acceptance or rejection.
5.6 This test method is not appropriate for specimens known
to contain flammable organics or contaminants, and other test
methods should be utilized in these situations.
Nore 1—The quality of the results produced by this test method is
dependent on the competence of the personnei performing it and the
suitability of the equipment and faciliries used. Agencies that meet the
criteria of Practice D 3740 are generally considered capable of competent
and objective testing/sampling/inspec6on. Users of this test method are
cautioned that compliance with Practice D 3740 dces not in itself ensure
reliable results . Reliable results depend on many factors; Practice D 3740
provides a means of evaluating some of those factors.
6. Interferences
6.1 When tesring sand and gravel size particles, addirional
care must be taken to avoid the possibility of particle shatter-
ing.
6.2 Due to the localized high temperatures in the soil during
testing, the physical characteristics of the soil may be altered.
Degradation of individual particles may occur, along with
vaporizarion, chemical transition, or loss of organics. There-
fore, specimens used in this test method should not be used for
other tests subsequent to drying (see Note 2).
Nore,2—The subsequent use of specimens dried by direct heating in
other test methods is discouraged.
7. Apparatus
7.1 Direct Heat Source Any source or heat that can be
d'uected to the soil specimen to raise the specimen temperature
to or above 110�C. Commonly used sources include electric,
gas, butane or oil-fired stoves, and hotplates, blowtorches, heat
lamps, hair driers, space heaters, etc. Heat sources that directly
apply open flame to the specimen may cause extreme degra-
darion of the specimen along with oxidarion of and depositing
of soot in the specimen and should not be used.
7.2 Balances A balance having a minimum capacity of 2
Kg, and meeting the requirements of Specification D 4753 for
a batance of 0.1-g readability.
7.3 Specimen Containers�uitable containers made of ma-
terial resistant to corrosion and a change in mass upon repeated
hearing, cooling, and cleaning. One container is needed for
each water content determination.
�.4 Container Handling Apparatus—Gloves or suitable
holder for moving hot containers after drying.
7.5 Miscellaneous (as needed}—Mi}cing tools such as spatu-
las, spoons, etc.; eye protection, such as safety glasses or
goggles; cigarette papers, and lrnives.
8. Hazards
8.1 Container holders or gloves are recommended for han-
dling hot containers. Some soil types can retain considerable
heat, and serious bums could result from improper handling.
8.2 Suitable eye protection such as safety glasses or goggles
is recommended due to the possibiliry of particle shattering
during heating, mi�cing, or mass detemvnarions.
83 Highly organic soils, and soils containing oil or other
contaminants may ignite during drying with direct heat
sources. Means for smothering $ames to prevent operator
injury or equipment damage should be available during testing.
Fumes given off from contaminated soils or wastes may be
toxic, and should be vented accordingly.
8.4 Due to the possibility of steam e�cplosions, or thermal
stress shattering of porous or brittle aggregates, a vented
covering over the sample container may be appropriate to
prevent operator injury or equipment damage. This also pre-
vents scattering of the test specimen during the drying cycle
while aiding in uniform heating of the specimen.
9. Samples
9.1 Perform the water content determination as soon as
pracrical after sampling to prevent water loss and damage to
potentially corrodible containers.
9.2 Prior to testing, store samples in non-corrodible airtight
containers at a temperature between approximately 3 and 30°C
and in an azea that prevents direct exposure to sunlight.
10. Test Specimens
10.1 Select a representative portion of the total sample. If a
layered soil or more than one soil type is encountered, select an
average portion or individual portions of each, and note which
portion(s) were tested in the report of the results.
10.1.1 For bulk samples, select the test specimen from the
material after it has been thoroughly mixed. The mass of moist
material selected shall be in accordance with Table l.
TABLE 1 Test Specimen Masses
Sieve Size Retaining More Than Minimum Mass of
10 % of Sample, mm Moist Specimen, g^
2.0 (No. 10) 200 to 300
4.75 (No. 4) 300 to 500
19.0 (No. �/s) 500 to 1000
"l.arger specimens may be used and are encouraged. Generaliy, inherent test
inaccuracies are minimized by using specimens with as large a mass as practicai.
q� D 4959
10.1.2 For smali samples, select a representative portion in
accordance with the following procedure:
10.1.2.1 For cohesionless soils, mix the material thoroughly,
then select a test specimen having a mass of moist material in
accordance with Table 1.
10.1.2.2 For cohesive soils, remove about 3 mm of material
from the exposed periphery of the sample and slice the
remaining specunen in half (to check if the material is layered),
prior to selecting the test specimen. If the soil is layered, see
10.1. Breaking or cutting of cohesive sampies to approximately
6 mm particles speeds drying and prevents crusring or over-
heating the surface while drying the interior.
10.2 Using a test specimen smaller than the minimum mass
indicated in Table 1 requires discretion, though it may be
adequate for the purpose of the test. Note a specimen having a
mass less than the previously indicated value in the report of
results.
Nore 3—When working with a small sample containing a relatively
large couse-grained particle, it may be appropriate not to include this
particle in the test specimen, depending on the use of test resu(ts. If this
is done, such exclusion should be noted in the report of the results.
10.3 When the result of a water content determinarion by
the use of this test method is to be compared to the results of
another method, such as Test Method D 2216, obtain a second
specimen during selection of the specimen for this comparison.
Take precaurions to obtain a specimen that represents the same
water content as closely as possible. Protect the comparison
specimens from water loss by transporting and storing the
specimens in sealed containers. A correetion factor can be
determined for use on subsequent water content deternvnations
on the same soil types from the same site when the difference
is relatively constant using several comparisons. Check the
conection factor on a regulaz, specified basis. Recognize that
different technicians, heat sources, and such may result in
different correcrion factors.
11. Conditioning
11.1 Prepare, process, and test all specimens as quickly as
possible to minimize unrecorded moisture loss.
11.2 Cut or break up the soil into small size aggregations to
aid in obtaining more uniform drying of the specimen, taking
care to avoid any loss of soil.
11.3 If the specimens are not being tested immediately,
place the specimens in containers that can be closed and stored
in an area not exposed to direct sunlight, to prevent loss of
moisture prior to initial mass determinations.
12. Procedure
12.1 Deternvne the mass of a clean, dry container, and
record.
12.2 Place the soil specimen in the container, and immedi-
ately deternune and record the mass of the soii and container.
12.3 Apply heat to the soil specimen and container, taking
care to avoid localized overheating. Continue hearing while
stirring the specimen to obtain even heat distriburion. Continue
applicarion of heat unrii the specimen first appears dry. A
comparatively uniform color should result. Avoid localized
bumt or darkened appearance of any part of the soil by
intemuttent mixing and stirring.
12.3.1 Experience with a particular soil type indicates when
shorter or longer initial drying periods can be used without
overheating.
Nore 4—A piece of dry, light-weight paper or tissue, such as cigarette
paper, placed on the surface of the appazently dry soil will curl or ripple
if the soil still contains significant water.
12.4 After an initial hearing period has been completed (soil
appears dry), remove the container and soil from the heat
source and cool to allow handling and prevent damage to the
balance. Determine and record the mass of the soil and
container.
12.5 Retum the container and soil to the heat source for an
additional application of heat.
12.6 V�th a small spatula or lmife, carefully stir and mix the
soil, taking care not to lose any soii.
12.7 Repeat 12.3 through 12.5 unfii the change between two
consecutive mass detemunations would have an insignificant
effect on the calculated water content. A change of 0.1 % or
less of the dry mass of the soii for the last two detemunations
should be acceptable for most specimens.
12.8 Use the final dry mass determination in calcularing the
water content.
12.9 When rourine testing of similar soils is contemplated,
the drying times and number of cycles may be established and
correlated for each heat source and used for subsequent
determinations. When pre-deternvned drying times and cycles
are utilized, periodic verification in accordance with the
procedure in 12.7 should be performed to assure that the results
of the final dry mass detemunation are equivalent.
13. Calculation
13.1 Calculate the water content of the soil as follows:
w=[(M� — MZ)/(Mz — M�)] X 100 = M,fM X 1Q0 (1)
where:
w = water content, %,
M� = mass of container and moist specimen, g,
M2 = mass of container and dried specimen; g,
M� = mass of container, g,
Mw = mass of water, g, and
MS = mass of solid particles, g.
14. Report
14.1 Report the foilowing informarion:
14.1.1 Identification of the sample (material) being tested,
by locarion (boring number, sample number, test number, etc.),
14.1.2 Water content of the specimen to the nearest 1%,
14,13 Indication of the test speciinen mass, including a note
if less than the minimum indicated in Table 1,
14.1.4 Indicarion of test specimens containing more than
one soil type (layered, and the like),
14.1.5 Indicarion of any material (size and amount) ex-
cluded from the test specimen,
14.1.6 Initial mass of test specimen prior to drying, and the
mass after the incremental drying periods,
14.1.7 Identificarion of the type of direct heat source, drying
settings, drying times, and number of cycles used, when
standardizecl drying is utilized, and
14.1.8 Identification of comparison test(s) if performed, the
q� D 4959
method of test utilized and any correcrion factors applied (see
Note 5).
NorE 5—Water content determinations conducted in accordance with
Test Method D 2216 or other methods may be rewrded on the same
report. This is not a mandatory requirement, but may be convenient when
the results of the two methods are to be compared.
15. Precision and Bias
15.1 Precision Test data on precision is not presented due
to the nature of the soil materials being tested by this test
method. It is not feasible and too costly at this time to have ten
or more agencies participate in a round-robin testing program.
Also, it is not feasible or too costly to produce mulriple
specimens that have uniform physical properties. Any variation
observed in the data is just as likely to be due to specimen
variation as operator or laboratory tesring variation.
15.2 The precision of this test method is operator-
dependent, and is a function of the care exercised in perform-
ing the steps of the procedure, giving particular attention to
careful controi and systematic reperirion of the procedures
used.
15.2.1 Subcommittee D18.08 is seeldng any data from users
of this test method that might be used to make a limited
statement on precision.
153 Bias There is no accepted reference value for this test
method, therefore, bias cannot be determined.
16. Keywords
16.1 acceptance tests; compaction control; density; direct
heating; laboratory moisture tests; moisture content; moisture
control; quality control; rapid method; soil moisture; test
procedure
SUIVIMARY OF CAANGES
In accordance with Committee D-18 policy, this section identifies the location of changes to this standard since
the last edition (1994) that may impact the use of this standard.
(1) Editorially revised the title.
(2) Editorially revised 1.2.
(3) Revised Secrion 2 to include Practice D 3740.
(� Revised Section 5 to include Note 1 referencing Practice
D 3740.
(5) Revised the numbering of exisring notes.
(� Revised precision and bias statement to conform to D-18
policy.
(� Added Summary of Changes.
The American Society fo� Testing and Materials takes no position respectlng the validity of any patent rights asserted in connection
with any ilem mentioned in this standard. Use�s of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibiliry.
This standa�d is sub%ect to revislon at any time by the responsible technical committee and must be �eviewed every five years and
if not revised, eithe� �eapproved or withdrawn. Yourcomments are invited eithe� forrevision of this slandard orfor additional slandards
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QAPP
Appendix E
August 17, 2000
Revision 1
Appendix E
EPA Method 100.1
Analytical Method for the
Determination of Asbestos Fibers in Water
PB83-260471
III lIII II II I I►1!Iliiil IIII IIII IIII III
ANA�YTICAL METh'00 FCR �ET�R"1�?!M'� ?G�
OF ASBESTOS FIBERS IN ��IA���
�y
Eric J. Chatfield and �?. Jane �illon
Flectron Optical Laboratory
Department of Apptied Physics
Ontario Research Foundation
Sheridan Park 2esearch Corranunity
Mississauga, Ontario, Canada LSK 133
Contract 68-03-2717
Project Officer
J. �1acArthur I.ong
Analytical Chemistry 3ranch
Environmental Research Laboratory
Athens, Georgia 30613
0
ENVtRONMENTAL RESEFRCH l�1BORATORY
OF�ICE OF REScARCH AND DE1E�OpMEuT
U.S. E�vIROr.m�ENTa� PROTECTi��v aGE"�CY
ATHEVS, GEORGIA 30613
r�raoouctc e.
NATIONAt TECHNICAL
INFORMATION SERVICE
uS :EP�p�yE�r p� ;C�r[AtE
coo�.•a,r.. ..� .....
�
TECHNICA� REPORT DATA
;!'�� ,,ar ,roJ lxun,� nr,��s nn rhr r� �:•rcr !�c ;"rr r�,m�..'r��nj�)
1 uC'Cat �v0 1. ]. HEGPIENT'S �CCES51f)MNC
EPA=600L4=84-04�..-- ---�--�..------------------ -- P�3H 3 ?60 4% J.
a��� �E a�u 5u8T�t�E ` 5 REPOA7 O47E �
Analytical Method f�r Determin��tion of Asbestos
Fibers in Water
. .�VTHJR�SI �
Eric J. Chatfield and P•1. Jane Dillon
) �ERFORh1�NG Or1G4N124TION NAME ANO AODRESS
Department of Applied Physics
Ontaric Research Foundation
Sheridan Park Research Corrmunity
Mississauga, Jntario, Canada L5K 1B3
12. yPQN50R�NG AGENC�' VAV1E AND 4DORE55
Environmental Research Laboratory--Athens GA
Office of Research and Development
U.S. Environme►ital Protecti�n A9ency
Athens, Georgia 30613
15. SUPF�EMENT.>RY NC�TEs
Pi RFORMING OA��nN124TiON C��DE
PERFORMING OR�iAN12ATION REPORT h0.
10. PROGRA�t EIEh
CBNCIA
,11. CONTRACT'Gaa
168-03-2717
1�, TYPE OF REPORT AND PER100 COVERED
Final, 10/78-9/31
14. SPONSORInIG AGENCV CODE
EPa!000�oi
An analytical method for measurement of asbestos fiber concentration in water
samples is described. Initially, the water sample is treated with ozone gas and
ultraviolet light to oxidize suspended organic materials. The water sample is then
filtered through, a 0.1, r�icrometer pore siz� capillary-pore polycarbonate filter,
after which the filt�r i� prepared by carbon extraction replication for examination
in a transmis�ion electron microscope (TEM}, Fibers ar� classified using selected
area electron diffraction and energy dispersive X-ray analysis. Measurement of
characteristic features on a recorded and calibrated selected area electron diffrac-
tion pattern is specified for precise ic+entification of chrysotile. Quantitative
determination of the chemical composition, and quantitative interpretation of at leas
one calibrated zone azis selected area diffraction pattern are specified for precise
identification of amphibole. Amphibole identif�catien procedures and generation of
the standard reporting format specified for the fiber count resii'ts are achieved
using two computer programs �that are integral to the analytical method.
�, KEV WORDS ANO DOCUMENT ANAIYSi$
_ �_ __ . -~_ _ DESCRIPTOpS _ _, _ b.IOENTIfiERS/OPEN ENOEO TEFMS �. COSATI I�li•1�1;(�rt�up
IYq, U�:,TRIBUT�ON STA?EMENT
RELEASE TO PUBLIC
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i
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�
DISCLAIMER
,
The ififormation in this document ha5 been funded wholly or in part
by the United States Environmental Protection Agency under Contract
No. 68-03-2117 to Ontario Research Foundation. It has been subject
to the Agency's peer and administrative review, and it has been
approved for publication as an EPA document. Mention ol trade names
or conunercial products does not constitute endorsement or recommen-
dation for us�.
ii
..�►---- — _ .. _ .
�
FOREWORD
Nearly every phase of environmental protection depends on a capability to
identify and measure specific pollutants in the environment. �s part of
this Laboratory's research on the occurrence, movement, transformation,
impact, and control of environmental contaminants, the ,analytical Chemistry
Branch develops and assesses new techniques for identifying and measuring
chemical constituents of water and soil.
A 3-year study was conducted to develop improvements in the analytical
method for determination of asbestos fiber concent.rations in water samples.
The research produced an improved sample preparation and analysis method-
ology, a rapid screen�ng technique to reduce analysis cost, and a new
rererence analytical method for asbestos in water. The analytical method
for de�ermining asbestos fibers in water is perceived as representing the
curre,it state-of-the-art.
William T. Donaldson
Acting Director
Environmental Research Laboratory
Athens, Georgia
iii
�
PREFACE
� The Preliminary interim Method for Determining Asbestos in Water was
issued by the U.S. Environmental Protection Aqency's Environmental Research
Laboratory in Athens, Georgia. 7h2 method was based on filtration of the
water sample through a sub-micrometer pore size membrane filter, followed by
preparation of the filter for direct examination and counting of the fibers
in a transmission electron microscope. Two alternative techniques were
specified: one in which a cellulose ester filter was prepared by dissolution
in a condensation washer; and another known as the carbon-coated NucleporeR
techn�que which used a polycarbonate fil�er. In January 1980 th� method was
revised (EPA-b00/4-80-005) to eliminate the condensation washer ��+?roach, and
d suggested statistical treatment of the fiber count data was incorporated.
The analytical me�hod published here is a furiher refinement oT tha_
revised interim method. Major additions include the introduction of
ozone-ultraviolet light oxidation prior to filtration, complete specification
of techniques to be used for fiber identification and fiber counting rules,
and incorporation of reference standard dispersions. A standardized
reporting format has also been introduced. The major deletion is �he low
temperature ashing technique for samples high in organic material content;
ashing is not required for the analysis of drinking water and drinking water
supplies when samples are treated using thf ozone-ultraviolet oxidation
techniGue. The "field-of-view" approach for examination also has been
deleted from the method. If a sampte is too heavily loaded for examination
of entire grid openings� d more reliable result is obtained by preparation of
a new fi?ter using a smaller volume of water.
iv
aBSTRACT
.an analytical nethod for measurement of asbestos fiber concentration in
water samples is described. Initially, the water sample is treated witn
ozone gas and �ltraviolet light to oxidize suspended organic materiais. The
water sample is then filtered through a 0.1 �m porP size capillary-pore
polycarbonate filter, after which the filter is prepared by carbon extraction
replication for examination in a transmission electron microscope ;TEM).
Fibers are classified using selected area electron diffraction (SAE01 anJ
energy dispersive X-ray anal�sis {EOXA). ��easurement of characteristic
features• on a recorded and calibrated SAED pattern is specified for precise
identification of chrysotile. Quantitative determinatiun of the chemicat
composition, and quantitative interpretation of at least one cal;brated zone
axis SAED pattern are specified for precise identification of ampnibole.
Amphibole identification procedures and generation of the standard reporting
format specified for th� fiber count results are achieved using two cem�uter
programs which are integral to the analytical method,
This analytical method is a further developmQnt of �he interim nethod
issued in 198C, and incorporates results of research performed under Contract
68-03-2717 under sponsorship of the U.S. Environmental Protection AQency.
This report covers a period from October 1978 to September 19�1 and the work
was cc�plzted as of September 1981.
�
�
CONTENiS
FOREWORD. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i i i
PREFACE. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . i v
A@STRACT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . v
FIGURES ................................ x
TABLES. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . xi
1.
Z.
3.
4.
5.
6.
SCOPE AND APPLICATION . . . . . . . . . . . . . . . . . . . .
SUMMARY OF METHOD . . . . . . . . . . . . . .
oEFtNtTIONS, UNITS ANO A66REVIATIONS� . . . . . . : . . . . . .
3.1 Definitions . . . . . . . . . . . . . . . . . . . .
3.2 Units . . . . . . . . . . . . . . . . . . . . .
3.3 Abbreviations . . . . . . . . . . . . . . . . . . .
EQUIPMEN7 AND APPARATUS . . . . . . . . . . . . . . . .
4.I Specimen Preparation�Laboratory . . . . . . . . . .
4.2 Instrumentation Requirements . . . . . . . . . .
4,2.1 Transmission Electron�Microscope . . . . .
4.2.2 Energy �ispersive X-ray Analyzer .....
4,2.3 Computer . . . . . . . . . . . . . . . .
4.2.4 Vacuum Evaporator . . . . . . . . . . . . .
4.2.5 Ozone Generator . . . . . . . . . . . . .
4.3 Apparatus, Supplies and Reagents . . . . . . . . . .
SAMPI.E COILECTION AND PRESERVATION . . . . . . . . . . . . . .
5.1 Sampie Container . . . . . . . . . . . . . . . . . .
5.2 Sample Collection . . . . . . . . . . . . . . . . .
5.3 Quantity of Sample . . . . . . . . . . . . . . .
5.4 Sample Preservation and Storage . . . . . . . . . .
PROCEDURE . . . . . . . . . . . . . . .
� 6.1 Cleantiness and Contamination Control . . . . . . .
6.2 Oxidatfon af Organics . . . . . . . . . . . . . . .
6.3 Filtration . . . . . . . . . . . . . . . . . . . .
6.3.1 General � . . . . . . . . . . . . . . . .
6.3.2 Filtration Procedure . . . . . . . . . .
6.4 Preparation af Electron Microscope�Grids ......
6.4.1 Preparation of Jaffe Washer .. ...
6.4.2 Selec�ion of FiitPr area for Carbon�Coating.
6.4,3 Carbon Coatinq of the Nucleoore Filter ...
6.4.4 Tran;fer of the Filter to Electron
Microscope Grids . . . . . . . . . . . .
6.5 Examination by Electron Microscop�/ . . . . . . .
6.5.1 Microscope Aiignment and Magnification
Calibration . . . . . . . . . . . . . .
vii
��
1
1
2
a
5
5
6
6
8
8
9
9
15
15
16
16
16
17
11
17
20
20
22
23
24
24
26
27
28
28
7.
10.
6.5.2 Calibration of EDXA System
6.5.3 Grid Preparation Acceptability � � � �
6.5.4 ?rocedure for fiber CounYinq � � � � �
6.5.5 Estimation of Mass Concentration �
fi.6 Fiber Counting Criteria . . . . . � � �
b.6.1 Fiber Counting Method . , � � � � � �
6.6.2 Fibers �hich Tour.h Grid Bars � . � � � � � �
6.6,3 Fibers Which Extend Outs�de the Field�of �
`Jiew . . . . .
6.6.4 Fibers with Stepoed Sides . . � � � � �
6.6.5 Fiber Bundles . � � � � � �
6.6.6 Aggreqates of Randomly Oriented�Fihers .��
6.6.7 Fibers Attached to Non-Fibrous Debris ��
6.7 Fiber ldentification Pr�cedures . � �
6.7.1 General , , , � � � � � � � � �
6.7.2 SAED and ��XA�Techniques . . . � � � � �
6.7.3 Analysis of Fiber :dentification Data. •��
6.7.4 Fiber Classification Categories � � �
6.7.5 ='rocedure for Classification of Fibers '�lith�
Tubular Morphology, Suspected to he
Chrysotile . . . . . .
6.7,6 Procedure for Classification of Fibers . �
Without Tubular MorDhology, Suspected to
be Amphihole . , , ,
6.8 Blank and Control Oeterminations . � � � � � � �
6.8.1 Blank Determinations . . � � � � � � � � �
6.8.2 Control Samples . . . � � � � � � � � �
CALCULP.TION OF RESULTS . . . . � � � � � � � � � � �
7.� Test for Unifor�nity of Fiber.0eposit•on Electron. �
Microscope Grids . . . .
i.2 Calculation of the Hean and Confidence.:nterval of� �
the Fiber Concentration
7.3 Estimated Mass Concentration� . � � � � � � � � � � �
7.4 Fiber length, '�lidth, �tass and Aspect�Ratio � � � � �
Distributions . . .
7.4.1 Fiber Length Cumulative.,vumber Oistribution.
7.4.2 Fiber Width Cumulative Number Distribution .
7.4.3 Fiber Length Cumulative Mass Distr9bution
7.4.4 Fiber Asaect Ratio Cumulative Number �
Distribution . .
7.4.5 Fiber �1ass Cumulative P�umber Distribution �
7.5 ;ndex of Fibrosity '
REPORTING � � � � � � � ' ' ' ' ' ' ' ' ' '
IIMITATIONS OF�ACCURACY � � � , � � � � � � � � � � � � � ' ' '
9.1 Errors and Limitations.of Identification� ������
9.2 Obscuration . . . � � � ' � '
9.3 Inadequate Dispersion � . . . . � � � � � � � � � �
9.4 Contamination , . � ' � � � � � ' � ' '
9. 5 Freez i ng . . . . . . . . . . . . . . . . . . . .
PRECISION AND ACCURACY� . . . � � � � � � � ' ' ' ' ' '
10.2 Genrral . . . . . . . . . . . . . . . . . . . . . .
10.2 Precisi,r� . . . . . . . . . . . . . . . . . . . . .
0
viii
29
?0
"sl
34
35
35
35
36
36
37
37
33
?a
38
39
43
45
4S
50
54
54
54
55
55
56
59
61
61
62
62
62
53
63
E3
65
55
66
66
66
66
67
67
67
�
10.2.1 Intra-Laboratory Comparison Using
Environmental Water Sources . . • • 67
10.2.2 Inter-Laboratory Comparison of Filters
Prepared Using Standard Dispersions
and Environmental '�ater Sources . . . . 67
10.3 Accuracy . . . . . . . . . . . . . . . . . . . 11
1C.3.1 Intra- and Inter-Laboratory Comparison
of Standard Oispersions of Asbestos
F i bers . . . . . . . . . . . . . . . . . 71
SELECTEO BI6l.I0GRAPHY . . . . . . . . . . . . . . . . . . . . . . . 74
APPENDIX A- TEST OATA ANO COMPUTER LISTtNGS
- FOR FIBER IDENTIFICATION , . . , . . . . . • • • • • »
APPENOtX 8- TEST DATA ANO COMPUTER LISTINGS
FOR OATA PROCESSIPJG ANO REP4RTING. . . . . . . . . . 176
ix
Nurrber
1.
2.
4,
SA.
56.
6.
7.
8.
9.
10.
11.
12.
13.
14,
15.
16A.
168,
17.
I8.
s
FIGURES
?aqe
Calibration �tarkinqs on TcM Viewing Screen . . . . . . . . . . . 7
Diagram of Ozone—UV Equipment . . 18
Ozone—U'J Oxidation of Water Samples �n Glass Bottles• � �� 19
'uclepore Oissolution Technique . . . . . . . . . . . . . � � � ��
Jaffe '�Jasher Oesign . . . . . . . . . � � � �5
Jaffe �iasher i n Use . . . . . . . . . . . � � � � � � � 25
Condensation '�Jasher . , , , , , , , , � � � � � ' ' ' ' �3
Sheet For Recording Water Samole•Data . . . . � � � � � 32
Sheet For Recording Fiber Classificatio�i and MeaS��rement�Data .� 33
Counting of Fibers Which Overlap Grid Bars .... � 35
Counting of Fibers Which Ext2nd Outside the Field o"�View . �� 36
Counting and Measurement of Fiber Bundles ... 37
Counting of Fiber Agqregates � � � � � . � � � ��
Counting and Measurement of Fibers�Attached to•Von—Fibrous ���
Oebris . . , 38
��leasurement of•Zone Axis�SAED Patterns. . . . . . � � � � • 41
Classificat?on Chart for Fiher '�lith Tubular '�orphology ,,,,, 47
TEM Microqraph of Chrysotile Fibril, showing Morphology ...,. 49
TEM Mi crogra�h of U ICC Canad i an Chr•ysot i 1 e F i her af ter ther;na t
Deqradation by Electron Seam Irradiation ..., a9
SAEO Pattern of Chrysotile Fiber �Nith Oi3gnostic Features l.abelled.50
Ciassification Chart for Fiber '�1ith�ut Tubular ��lorphology .... S?
x
�
�
ye
Number
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
TABLES
Paoe
Limitation of Analyticai Sensitivity by Volume of"Water Sample
Filtered . . . . . . . . . . . . . . . . . . . . . . . . 21
Siiicate Mineral�Standards . . . . . • • • • • • • 29
Classification of Fibers With iubular '�orphology . . . . . . . . 46
Classification of Fibers Without 7ubular ��orphology ....•. 46
Levels of Analysis for Amphibole . . . . . . . . 53
Intra-Laboratory Comparison of Environmental�Water�Samples ... 68
Inter-laboratory Comparison: Standard Dispersions . . . . . . . 69
Inter-laboratory Comparison: EnvironmentaT Water Samples ... 7�
Inter- ar.d Intra-Laboratory Comparison: Chrysotile ...... 72
Inter- and Intra-Laboratory Comparison: CroCidolite ...... 73
xi
ANaLYTICAL METN00 FOR OETERMINAtION OF ASBESTOS FIBERS IN '�►ATER
l. SCOPE AND APPLICATION
��
1.1 This method is applicable to drinking water and drinking water
suoplies, and should he used when the bes? available analytical
procedure is required.
1.2 The method determines the numerical concentration of asbestos
fibers, Lhe length and width of each fiber, and the estimated mass
Concentration of asbestos in the water. Fiber size and aspect
ratio distributions are also determined. •
1.3 The method permits, if required, identification of all mineral
fibers found in water. In particular, chrysotile can be
distinguished from the amphiboles, and fibers of specific
amphiboles can be identified.
1.4 The analyti.:al sensitivity which can be achieved depends primarily
on the amount of other particulate matter which is present in the
sample. This limits the proportion of the sample which can be
mounted for examination in the electron microscope. In drinkina
water which meets the �'�1`,JA turhidity criterion of 0.1 �VTJ, an �
asbestos concentration of 0.01 miilion fibers per liter (�1F�) can
be detected. The contamination level in ti�e laboratory environment
may degrade the sensitivity. 7he analytical sensitivity for the
determination of mass concentration is a`unction of the preceding
parameters and also depends on the si=e distribution of the
fibers. In Tow turbidity drinking �Hater the analytical sensitivity
is usualTy of the order of 0.1 nanogram per liter (ng/L).
1.5 It is beyond the scope of this document to provide detailed
instruction in electron microscopy, electron diffraction,
crystaTlogranhy or X—ray fluorescence techniques. It is assumed.
that those performing this analysis will be sufficiently
knoNiedgeable in these fields to understand the soecialized
techniques involved.
2. SUMMARY OF METH00
Water collected in a polyethyl�ne or glass container is treated with
ozone and ultraviolet light to oxi�ize organic matter. After mild
ultrasound treatment to dis�erse the `ibers uniformly, a�ncwn volume of
the water is filtered through a 0.1 micMometer (��n �'
) pore size
`IucleporeR polycarbonate filter. a carbon coati�g is then apniied in
vacuum to the active surf ace of the filter. The carbon layer coats and
retains in position the material which has been cotlected on the filter
�: surface. A small portion of the carbon—coated filter is placed on an
etectron microscope grid and the polycarbonate filter matP�ial is removed
by dissolution in an organic soivent. The carbon film co.�tatning the
original particulate, supported on the electron microscope grid, is then
� � examined in a transmission electron microscope (TEM) at a magnification
of about 20,000. In the TEM� selected area electron diffraction (SAE�)
is used to examine the crystal structure of a fiber, and its elemental
canposition is determined by energy dispersive X—ray analysis (EDXA).
Fibers are classified accordi�g to the techniques which have been used to
identify them. A simple �ode is used to record for each fiber the degree
to which the identification attempt was successful. The fiber
classification procedure �is based on successive inspection of the
morphology, the selected area electron diffraction pattern, and the
qualitative and quantitative energy dispersive X—ray analyses.
Confirmation of the iderttification of chrysotile is only by quantitative
SAED. anC confirmation of amphibole is only by quantitative EDXA and
quantitative zone axis SAED.
Several Tevels of analysis are specified, three for chrysotile and four
for amphibole� defined by the most specific fiber classification to be
attempted for all fibers. The procedure permits this target
classificatian to be defined on the basis of previous kno�xledge, or lack
of it, about the particular sample. Attempts are then made to raise the
classification of all fibers to this target classification, and to record
the degree of success in each case. rhe lengths and widths of all
identified fibers are recorded. The number of fibers found on a known
area of the microscooe sample, together with the equivalent volume of
water `ilte►� d chrough this area, are used to calculate the fiber
concentration in MFL. The mass concentration is �alculated in a similar
manner by surtmation of the volume of the identified fibers, assuming
their density to be that of the bulk material.
�. OEFINITIONS, UNITS AND ABBREVIATIONS
3.1 Definitions
Acicular — 7he shape shown by an extremely slender crystal with
smali cross—sectional dimensions.
Amphibole — A group of rock—forming ferromagnesian silicate
minerals, closely related in crystal form and composition
and having the general formula: A2_365{Si,AI}8Q2z(OH)2,
- where A• Mq, Fe+2� Ca, Na or K, and B� Mg� Fe+z,Fe+3
� or A1. Some of these elements may also be substituted by
Mn, Cr, Li, Pb, Ti or Zn. It is characterized by a
cross—linked dovble chain of Si-0 tetrahedra with a
silicon:oxygen ratio of 4:11, by columnar or fibrous
prismatic crysta�s and by good prismatic cleavage in
�, __ .
._.
two directions parailel to the crystal faces and
intersecting at angles of about 56° and 124°.
Amphibole Asbestos - Amphibote in an asbestiform habit. �f�
Analytical Sensitivity - The calculated concentration in
�'� L equivalent to countinq of one fiber.
�
Asbestos - A commercial term applied to a group of silicate
minerals that readily separate into thin, strong fibers
that are flexible, heat resistant and chemically inert.
Aspect Ratio - The ratio of length to w�dth in a particle.
Camera length - The equivalent projection length betNeen
the sample and its electron diffraction pattern, in the
absence of lens action.
Chrysotile - A minera] of the serpentine group: Mg3Si�05(OH)q,
It is a highly fibrous, silky var�ety of serpent��e, and
constitutps the most important type of asbestos.
Cleavage - The breaking of a mineral along its crystallographic
planes, thus reflecting crystal structure.
Cleavage rragment - A fraqment of a crystal that is bounded by
� cleavage faces.
d-Spacing - The separation between identical adjacent and
parallel planes of atoms in a crystal.
Diatom - A microscopic, sinqle-celled ptant of the class
Bacillariophyceae, which grows in both marine and fresh
water. Diatoms secrete walls of silica, called frustules,
in a great variety of forms.
Electron Scattering Power - The extent to which a thin layer of
a substance scatters electrons from their original path
directions.
Energy Oispersive X-ray Analysis - Measuremen*, of the energies
and intensities of X-rays by use of a solid state detector
and multichannel analyzer system.
Eucentric - The condition when an object is placed Nith its
center on a rotation ur tilting axis.
Fibril - A single fiber, which cannot be separated into smaller v
components without losing its fibro��s properties or
appearances.
�
3
xy
£
�
0
Fiber - A particle which has parall?1 or stepped sides, �n
aspect ratio equal to or yreater than 3:i, and is greater
than 0.5 um in length.
Fiber Aggregate - An assembly of randomly oriented fibers.
Fiber Bundle - A fiber composed of parallel, smaller diameter
fibers attached along their lengths.
Habit - The characteristic crystal form or combination of forms
of a mineral, including characteristic irregularities.
Miller Index - A set of three or faur integer numbers �sed to
specify the orientation of a crystallographic plane in
relation to the crystal axes.
Replication - A procedure in electron microscopy specimen
preparation in which a thin copy� or replica, of a surface
is made.
Selected Area Electron Diffraction - A technique in electron
microscopy in which the crystal structure of a sma]1 area
of a sample may be examined.
Serpentine - A roup of common rock-fo rtning minerats having the
. formuia: �Mg,Fe)3 Si205(OH)4.
Unopened Fiber - Large diameter asbestos fiber which has not
been separated into its constituent fibrils.
Zone Axis - That line or crystallographic direction through the
center of a crystal which is parallel to the intersection
edges of t�e r.rystal faces defining the crystal zone.
3.2 Units
eV
g/cm3
- eTectron volt
- grams per cubic centimeter
kV - kilavott
ug/L - mic�ograms per liter (10-6 grams per liter}
um - micrometer (1�r6 meter)
MFL - Million Fibers per Liter
ng/L - nanograms per liter (10-9 grams per liter}
nm - nanometer (10-9 meter)
f�
4
• ..._ . . . . . , .. . . ..- . .,. .. _ __.- _ . . � . ._
NTU — Yephelometric Turbi�iity Unit
PPm — parts per million
3.3 Abbreviations `�
,.
AWWA — American Water Works Association
EDXA — Energy Oispersive X—ray Analysis '�
HEPA — High Efficiency Particle Absolute
SAEO — Selected Area Electron Oiffraction
SEM � — Scanning Flectron Microscope
STEM — Scanning Transmission Electron �HicroScepe
TEM — Transmission Electron Microscope
UICC — Union Internationale Contre le Cancer (Tnternatio�al
Union Aqainst Cancer)
JV — Ultraviolet
4. EQUIPMENT AND APPARA?US
4.1 Specimen Preparation laboratory
Asbestos, oarticularly chrysotile� �s present in small quantities
in practically all laboratory reagents. Many buildinq materials
also contain significant amounts of asDestos or other mineral
fibers which may interfere with analysis. It is therefore
essential that all specimen preparation steps be performed in an
environment where contamination of the sample is minimized. The
primary requirement of the sample preparation laboratory is that a
blank determination using known fiber—free water must yield a
result which will meet the requirements specified in
Section 6.8.1. Preparation of samples should be carried out only
af ter acceptable blank values have been demonstrated.
The sample preparation areas should be a separate clean room with
no asbestos—containing materials such as flooring, ceilinq tiles,
insulation and heat—resistant products. The work surfaces should
be stainless steel or plastic—laminate. The room should be
operated under oositive pressure and have absolute (HEP.4) filters�
. electrostatic precipitation, o►� eauivalent, in the air supply, A
laminar flow hood is recommended for sample manipulation. It is
recommended that a supply of disposable labor�tory coats and �
disposable overshoes be obtained to be worn in th�� ctean room.
This will reduce the levels of�dust� and particularly asbestos,
which might be transferred inadvertently by the operator into the
� • m�
�
d
�
clean area. Normal electrical and water services are required. An
�. air extract (fume hood) is required to remove surplus ozone from
the area near the ozone 9enerator.
4.2 Instrumentation Requirements
� 4.2.1 Transmission Ele� cron Microscope
A transmission electron microscope having�an accelerat:ng
potential of a minimum of 80 kV, a resolution better than
1.0 nm, and a magnification range of 300 to 100,000 is
required. The ability to obtain a direct screen magnifi—
cation of at lcast 20,000 is necessary. An overall
magnification of about 100,000 is necessary for inspection
of fiber morphology; this magnification may be obtained by
supplementary optical enlargement of the screen image by
usa of a binocular if it cannot be obtained directly. It
is also required that the viewing screen be calibrated.(as
_ shown in figure 1) w9th concentric circles and a mitlimeter
scale such that the lengths and widths of fiber images down
to 1 mn width can be measured in increments of 1 mm.
...� For Bragg anqles less than 0.01 radians the instrument must
' be capable of perfarmi�g selected area electron diffraction
from an area of 0.6 um or �ess, selected from an in—focus
image at a screen ma�nification of 20,000. This perform—
ance requirement defines the minimum separation between
particles at which independent diffraction patterns can be
� obtained from each. The capability of a particular
instrument may nor�nally be calculated using the following
relationship:
A = � (M + 2000 CS93)2 .
where: A � Effective SAED area in �m2
D � Diameter of SAED aperture in um
M � Magnification of objective lens
�S • Objective lens spherical aberration
coefficient im m� '
s • Maximum Bragg angle in radians
Aithough almost all instruments of current manufacture �neet
these requireme�ts, many otder instruments which are still
in service do not. It is obviously not possibte to reduce
the area of analysis indefinitely by use of apertures
�
,
�
1
e
�
e
�
s
I
�
�
�`�
�
� , � '��
����� �� �'� '��
\�\�'� `�� � � .
\� `,
\, \�\ �`, �'', '',, �, `��
�� � � ` \ �
� ., `,, ;
', '� , �'� . `�� 1 �1
\ `\ \ l, ` � �, .+ , `
` • �� , • i ! � �i
I
i �'I ' 1� i ; i i i i i
z I �' i, i., a� �
� � �
' ' 1 � ' , �
; ,
�` �% ; � �� �
: � j' .� f . . � ;
/� % �,' �/ j I '� % %, /t �,
/ / / �� % I � �
�/ / �� .� l �� �
Figure 1. Calibration Markings on TEM �liewing Screen.
7
�
v
4
... . . . . . � - � � .. . ._ .. - �
smaller in diameter than
manufacturer, since there
� imposed by the spherical.
�, objective lens.
those sAecified by Che
is a fundamentai limitation
aberration coefficient af the
If zone axis SAED analyses are to be performed, it is
required that the electron microscope be fitted with a
goniameter stage which permits either a 360° rotation
combined with tilting thro�gF� at lea�t +30° to -30�, or
tilting throuqh at least +30 to -30 around two
perpendicular axes in the plane of the sample. The work is
greatty facilttated if the goniometer permits eucentric
tilting.
It is also essentiai that the electron microscope have an
illumination and condenser lens system capable cf for�ninq
an electron probe smaller than 100 nm in diameter.
Use of an anti-contamination trap around the specimen is
recommended if the required instrumental performance i5 to
be obtained.
4.2.2 Energy Dispersive X-ray 'Analyzer
An energy dispersive X-ray analyzer is required. Since the
performance of individual combinations of equipment is
critically dependent on a number of geometrical factors,
the req��ired performance of the combination of electron
microscope and X-ray analyzer is specified in terms of the
measured X-ray intensity f�om a small diameter fiber, using
a known electron beam diameter. X-ray detectors are
generally ieast sensitive in the low energy region, and so
measurement of sodium in crocidoli�e is selected as the
performance criterion. The combination of electron
microscope and X-ray analyzer must yield a background-
subtracted NaKa peak integral count rate of more than
1 count per seconG (cps) from a 50 nm diameter fiber of
UICC crocidolite irradiated by a lu0 ^m diameter electron
probe at an accelerating potential of 80 kY. The
eq��ivalent peaklbackground ratio should exceed 1.0.
The EOXA equipment must provide the means for sub�raction
of the background, identification of elemental oeaks, and
calculation of net Peak areas.
4.2.3 Computer
Many repetitive n��merical calculations are necassary, and
these can be perfarmed conveniently by relatively simple
cemputer Nrograms. For analyscs of zone axis diffraction
pattern measurements, a computer facility with minimum
available memory of 64K words is reauired to accommodate
0
-- � - � � ... � , . _ . ..--_-.-.�...,_._,. ._..._.�,.,--�.-_.,,
the more complex programs involved. Suggested orcgram
listings for standardized daLa reporting and fiber
identification routines are inclu�2d as part of this
analytic.31 procedure. (Appendices A and 6).
4.2:4 Vacuum Evaporator ��
A vacuum4evaporator capable of producing a vacuum better
than 10— Torr (0.013 Pa) is required for vacuum
deposition of carbon on to the potycarbonate filters. A
sample holder is desirable which allows a 51 x 75 mm glass
microscope slide to be tilted and ro�ated during the
coating procedure. Use of a?iquid nitrogen cold trap
abovA the diffusion pur�p will minimize the possibility �f
contam�nation of the filter surfaces by oil from the
pumping syst�m. The vacuum evapo�ator may also be used for
deposition of the thin film of aold� or other reference
material, required on e?ectron microscope samples for
calibration of electron diffraction patterns. For gold
deposition, a sputter coater may allow better control of
the process, and is therefore recommended.
4.2.5 Ozor,e Generator
An�ozone generator, in combination w�th ultraviolet light
irradiation, is used for the oxidation of organic material
in water samples. This procedure �s necessary on a11 water
samples. The generator should be capable of oenerating at
least 400 g of ozone p��r day at a concentration of at least
1� by weight when sup•�lied wi�h dry oxygen, ihe ozone
generator Model 6L-1 (PCI Ozone Corporation, 1 Fairfietd
Crescent, West Ca;dwe'1, New Jersey 07006) or equivalent
has been found to meet the requirements of this analytical
technique. .
4.3 Apparatus, Supplies and Reagents
4.3.1 Gas Supply to Ozone Generator
The ozone generator ca� be supolied by either compressed
air or oxygen. The input gas must be regulated to the
pressure specified by the generator manufacturer. It is
recommended that �xygen be provided in order to reduce the
possibility of acid formation in the sample.
4.3.2 Gas—Line Orying Tube
The ozone generator operates more efficiently when supplied
with dry axygen. An in—tine drying tube. filled with a
desiccant, followed by a 0.2 ��m pore size polytetra—
f)uoroethylene filter to prevent particulate from the
desiccant entering the ozone generator is recorr,mended.
w
, . . . - ---�-....�,_.,_ �
A Stainlzss st?el pressure filtration assembly (�1illipore
Corpor�tion, Bedford MA 01730, Cat. No. XX40 047 00) with a
0.2 �:m pore size FluoroporeR filter (Hillipore Corporation,
"� Cat. No. FGIP 041 00) in the normal filter posit�on and
silica gel in the reservoir have been found to be
_ . satisfactory for this purpose.
;� 4.3.3 In-Line Gas Fittration Assembly _
A filter is placed in the ozone line immediately before the
qas enters the sam�le. A 25 mm stainl�ss steel gas line
filter holder (Millipore Corporation, Cat. No. XX40 025 00)
or equivalent with a 0.2 um pore size Fluoropore filter
(Millipore Carporation, Cat. No. FGLP 025 00) or equivalent
is used in each ozone supply line to ensurP that the ozone
entering the sample is particle-free.
4.3.4 Ultraviolet lamp
A submersible short wavelenqth (254 nm) ultraviolet lamp is
required for the ozone-UV oxid�tiun treatment of water
samples. A 6 inch Pen-RayR ultraviolet lamp (Part No.
90-0004-I1) and power supply model SCT-4 (Ultra-Violet
Products Inc., 5100 '+�alnut Grove Avenue, San Gabriel,
California 91778) or equivalent have been found to meet
the requirements of this analytical technique,
4.3.5 Source of Known Fiber-�ree Water
For blank determinations, final v+ashing of analytical
equipment, and dilution of some samples, a source of water
which is free of both particles and fibers is required.
Fresh double-distflled water from a glass distillation
apparatus (ME6A-PURET''� manufactured by Corning and
available from all authorized Corning Laboratory Supply
Dealers) or equivalent is preferable, and has been found to
meet thiS requirement. De-ionized water, filtered through
a 0.1 um pore size yuclepore polycarbonate filter�has also
been found to be satisfactory, but the filtration 3ssembly
itself tends to contribute some oarticles to �he filtrate.
4.3.6 Filtration Apparatus
The water sample is filtered through a membrane filter of
either 41 mm diameter or 25 �Txn diameter. The filtration
assembly should be chosen to suit the size of filter in
r_ use. A glass frit support is required in order to obtain a
uniform deposit on the filter. The reservoir must be
easily cleaned in order to prevent sample cross-
- contamination. A 47 rrm analytical filter holder (Millipore
Corporation, Cat. ��o. XX10 047 00) or a 25 mm analytical
filter holder (Millipore Corporation, Cat. No; XX10 025 00)
10
..�.r �.
.� ..
or equivalent has been found to be suitable. `�hen us�ng
the larger diameter equipment it is necessary to filter
proportionately larger volumes of water.
4,3.7 Filtration Manifold
4.3.8
When a number of samples are to
fi7tration units can be operated
singie vac�um source by using a
manifold (Miltipo�e Corporation,
equivaleni. The manifold should
each port to be opened or closed
Vacuum Pump
be filtered, several
simultaneously from a
mul�iple port filtration
Cat. No. XX26 047 35) or
include valves to permit
independently.
A pump is required to provide a vacuum of 20 kPa for the
filtration of water samples. A water jet pump (Edwards
Nigh Vacuum Inc., Grand Island, NY 14072, Cat. No,
C1-0046-01-000-female connection or O1-0039-01-000-male
connection) or equivalent has been found to provide
sufficient vacuum for a 3-port filtration manifold and also
incorporates a non-return valve to prevent back-streaming.
4.3.9 Membrane Fiiters
The diameters of the membrane filters should be matched to
the diameters of the filtration apoaratus in use. For
filtration of water sarrples, two types of filters are
required:
- polycarbonate �apillary-pore membrane filters�
0.1 �m pore size (NuclFpore Corooration, 7035
Commerce Circle, Pleasanton, California 94566)
or equivalent, are used to collect the suspended
material•from a water sample.
mixed esters of cellulose mem.brane filters,
0.45 um pore size 7ype HA (Millipore
Corporation� Bedford, A1A OI730) or epuivalent,
are used as a support filter placed between the
glass frit of the filtration apparatus and the
polycarbonate filter.
4.3.10 Jaffe '�lasher
A Jaffe Washer is used for dissolution of �Vuciepore
fiiters. Several designs of JaFfe �ashE;� have been used
which are modifications of the original design. Provided
that the polycarbonate filter can be completely dissolved,
and that the materials used.in the different designs of
washer are demonstrably free of mineral fiber
contamination, the precise design is not considered
11
H
. _ .�.._._...�_ __. ._. _ . ._r____�__— --------- •- -��--- - - - - � ;-+�^�
important. Because of recent changes in the formulation of
Nuclepore polycarbonate filters which have degraded their
�
solubility in chloroform, a more complex dissolution
'�j procedure may be required. The additional steps in the
preparation are more easily completed if Lhe original
_ washer design is followed. This original design is
iilustrated �n Figure SA. Figure SB shows samples being
placed on a Jaffe 5lasher oP this design. Alternatively,
` methylene chloride may be substituted for chloroform, but
because this has a higher vapor pressure it is then
necessary to ensure that the Jaffe Washer is tightly sealed
to avoid exc2ssive evaporation.
4.3.11 Condensation Washer
A condensation wash�r may be useful if TEM specimens are
required more quickly than is possible if the Jaffe Washer
is used alone to dissoive some oatches of Nuclepore
polycarbonate filters. A condensation washer consists of a
system Hith controlled heating, controlled refluxing� and a
coid finger for holding the electron microscope sample
�rids. Fiqure 6 shows one model of the condensation washer
Cat. No. 16950, Ladd Research Industries, Inc,, P.O. Cox
901, Burlington, Vermont 05401} which has been found
sat i sf actory.
4.3.12 Electron Microscope Grids
Specimen grids of 200 mesh and 3 mn diameter are required
in both copRer and goTd. The grid o�eninQs should be
approximately 80 um square. The fiber count result
obtained is pr000rtional to the �nean area of the openings
examined. Therefore, it is important that an accurate
measurement of the dimensions of each grid openir,g can be
obtained. Since there is a wide range of quality in the
avaitable copper specimen grids, these should be examined
carefuily to establlsh the degree of uniformity of beth the
grid openings and the grid bars. Copper speci�nen grids
Cat. No. SPi �302CC and 3020T, SPI Supplies Oivi�ion of
Structure Probe, Inc., P.O. Box 342, West Chester, PA
19380, or equivalent, have been feund to meet the
requiremenLs. In addition, these grids have a mark at the
center openin�. ihis reference can be used to indicate the
location of openings which have been examined.
Alternatively, finder grids may be substituted if
re-examination of specific grid openings is to be
required. Gold specimen grid� Cat. No: 21b12, Ernest F.
FutTam, Inc., P.O. 8ox 444, Schenectady, N.Y. 12301, or
equivalent�, have been found t� meet the requirements for
gold grids.
12
4.3.13 Ultrasonic Bath
An ultrasonic bath is requ�red `or disAersinq particu�a�e
in sample containers and for general cleaning of
equipment. The size of unit se�ected is unimportant, and
should be related to the volume of work in proaress.
Bransonic �4ode1 8-52 (Branson Cieaning Fquipment Company,
Parrott Drive, Shelton Connecticut 06a84) has a pc�yer of
200 watts at a frequency of 5Q kHz and has been found to
meet the requirements.
4.3.14 Carbon Rod Electrodes
4.3.15
4.3.16
Spectrochemically pure carbon rods are required for use in
the vacuum evaporator during carbon coating of filters.
Type aGKSP, National Spectroscopic Electrodes, manufactured
by Union Carbide, or equivalent, have beer found to �eet
the requirements.
Carbon Rod Sharpener
This device is used to sharpen the carbon rods to a neck of
3.6 mm long ar,d 1.0 mm diameter. The use of necked rods,
or equivalent, allows the carbon layer to be apptied with �
minimum of h�eating of the oolycarbonate membrane. The
;harpener, Cat. No. 1204, Ernest F, Fuilam, Inc.,
Schenectady, N.Y. 12301, or equivalent, mePts the
requirements.
Standards
a) Reference Standard Fiber Suspensions. Glass amooules
of stable concentrated chrysotile or a�ahibole fiber
dispersions, {Electron Optical Laboratory, Ontario
Research �ound�tion, Sheridan Park, �1�ssissauga,
Ontario, Canada LSK 183) can be used to establish
quality assurance in analyticai programs. The
refarence suspensi�ns of known mass and numerical
fiber concentretions are used to generate control
samples for inclusion in anatytical programs.
b) �eference Silicate Mineral Standards on TE��1 Grids. For
calibration of the EDXA system, reference silicate
mineral standards are reouired (Electron Optical
Laboratory, Ontari� Research �ounda:ion, Sheridan
Park, Mississauga, Ontario, Canada LS!C 183).
c) Asbestos Butk Material. Chrysotile (Canadian!,
Chrysotile (Rhodesian), Crocidolite, Amosite. UICC
(Union Internationale Contre le Cancer) Standards.
Available from �uke Standards Ccm�any, 445 Sherman
Avenue� Palo Alto, CA 9a306.
13
4.3.17 Carbon Grating Replica
A carbon grating replica with about 2000 parallel lines
��' oer rtm (Cat. No. 10020, Ernest F. �ul�am, Inc.,
Schenectady, N.Y. 12301) or equivalent is required for
calibration of the maqnification of the TEM.
�- 4.3.18 Chloroform
Spectro rade chtorofo�-m, distilled in glass {vreserved Nith
lA (v/v� ethanol, Burdick 3 Jackson Laboratories Inc.,
Muskegon, Michiqan 49442) or equivalent, is required for
the dissolution of the polycarbonate filters.
4.3.19 Petri Dishes
Oisoosable plastic oetri dishes (Millipore Corp. Cat. No.
PO 10 047 00) or eq�iv3lent, are useful for storage of
Sample filters and �Ge�imen qrids. If charge build—up on
these dishes is experienced, it has been found that rinsing
them with a weak deterqent solution Nill reduce the problem.
4.3.20 Quartz PiPets
Quartz pipets are used to bubble ozone through the liquid
sample. These pipets are formed by heating quartz tubing
and drav+ing it to a tip of approxima�ely 0.35 mn inside
diameter. The pipet sh�uid be sufficientiy tong to reach
within 1 inch of the bottom of the sample bottle, to create
good mixing of the liquid during oxidation.
4.3.21 Mercuric Chloride Solution
A 0.01 molar solution of inercuric chloride may be required
for preservation of vrater samples. This is orepared by
dissolving 2.71 g of reagent grade mercuric chloride in
100 ml of fiber-free water. 7he solution is then filtered
tv+ice through the same 0.1 um pore size Nuclepore filter,
using the filtratio� apparatus �escribed in Section 4.3.6
and a conventional filtration flask.
4.3.22 Routine Electron Microscopy Preparation Supplies
Electron microscooy preparation supplies such as scalpets,
disposable scaloel blades (curved cutting edge)� �
douDle-sided adhesive tape, sharp point tweezers and
soecimen scissors are required. These items are available
from most EM supply houses. �
14
�_,�� _..__ _ . .. _ . _ .
...- .�.�. ._i1'oT.'j•�
� ' _' ' ' ' '. . . _ _ ._ . .�+. . . .. .�,. -c.. � v-0
- .-.-., ._.....su
Figure 3. Gzone-UV Oxidation of Water Samples in G9ass Bottles. The ozone
supply line has been split into two lines to permit simultaneous
oxidation of two samples. A valve and a filter holder are
incorporated in each of the supply lines to the samples.
An 1ir extract to r?move surplus ozone is required. If it is
necessary to check that the ozene generator is functioning within
the specffications, the output can be verified by normal chemical
methods. A suitable technique is to bubble the ozone through a
solution of potassium iodide and to titrate the displaced iodine
with sodium thiosulfate solution, usinq starch as an indicator.
8efore the ozone-UV treatment, place each polyethylene or gtass
bottle containing the water sample in the ultrasonic bath for a
period of 15 minutes. Mark the level of the liquid in the sample
bottle using a waterproof felt marlcer. The quartz pipets should be
thoroughly washed before each use, and �nstalled on the ozone
supply as indicated so that the tip is close to the bottem of the
sample bottle. The UV lama is also thoroughly washed and then
imnersed in the sample and switched on.
At an ozone concentrativn of 4; in oxygen, treat each sample with
about 1 liter/minute of gas for approximately 3 hours. At other
ozone concentrations, adjust the oxidation time so that each sample
receives about 10 grams of ozone. The qas flow rate should be
19
�
M
sufficient to produce a mixing action in the liquid but should not
splash sampie out of the container. It is not easy to indicate
when oxidation is complete, but this treatment as described has
" been found to be adequate for all water samples so far handled.
When oxidation is complete, remove the UV lamp and quartz pipet,
re—cap the bottle and place it in the ultrasonic bath for a period
of 15 minutes. This allows particulate released from the oxidized
� organic materials and the container surfaces to be unifornly
dispersed throughout the sample.
The water level in the bottle may have fallen, duP to evaporation
during the oxidation procedure. The toss of volume should be noted
and can be accounted for if it is significant. The sample should
be filtered irrmediately after it is removed from the ultrasonic
bath.
6.3 Filtration
6.3.1 Generat
The separation of suspended particulate by filtration of
the sample through a membrane filter is a critical step in
the analytical procedure. The objective is to produce a
Nuclepore filter on which the suspe�ded solids from the
sample are distributed uniformly, with a ninimum of
overlappinq of particles. The volume to be filtered
depends on the diameter of the filtration equipment in use,
the total suspended solids content of the sample, and in
some samples the volume depends on the fiber concentration
present.
Table 1 show5 the limitation of the analytical sen5itivity
as a*unction of the volume of water filtered. In
practice� it is usually found that the concentration of
suspende� solids limits the filtration volume. The maximum
particulate io�ding on the filter which can be tolerated is
about 2� ug/cm , with an oqtimum value of about
S uq/cm . Where the concentration of suspended solids is
known, the maximum vo�����e which can be used may be
estimated. Usually, however, nothing is known about the
sample and the best procedure is to prepa�-e several filters
using different volumes of the sample. It has been found
that suitable filter samples display a faint celoration �f
the surface, and with exper�ence over—loaded filters
usually can be recognized. ihe determination of a suitabie
volume to fitter is usually a matter of trial and error in
the analysis of samptes of relatively low total suspended
solids but high asbestos concentration.
No attempt should be made to filter sam�le volumes ]ess
than 10 mL for 25 rmn diameter equipment, and 50 mL for
47 mm diameter equipment. If smaller volumes are filtered
20
TABIE 1. LIMITaTION OF ANALYTICAI SENSITIVITY BY VOLUME OF WATFR SAh1PLE
FILTERED "
Volume Filtered (mL) �
Analytical Sensitivityl
UsingF2jtmm Diameter Using 47 mm3Diameter (Fibers�Liter) �
2 Filter
0. 1 0.6 1.5 x 10� �
I
0.5 2.8 3.0 x 106
1.0 5.7 1.5 x 106
2.0 11 0.8 x 106 �
5.0 28 3.0 x 105
10 57 1.5 x 105
I
ZS 1a2 6.0 x 104
50 Z85 3.0 x 104
100 570 1.5 x 104
1Concentration corresponding to 1 fiber detected in 20 grid openings of
nominal 200 mesh grid (approximately $0 ;.m square grid ooenings)
2Assuming Active Filter Area of 1.99 cm2 �
3AsSuming Active Filter Area of 11.34 cm2
21
�
�.
it is difficult to ensure that a uniform deoosit of
particulate wiil be obtained on the filter. Sampies of
high solids content, or of high fiber• content, may require
F" filtration of volumes less than these. Such samples should
� be diluted with fiber-free •Mater so that the volumes
_ filtered exceed the minima specified. Oilutions should be
made by transferring a known volume of the sampte to a
disposable plastic bea�cer and making up to a known volume
`� with fiber-free water. The mixture should be stirred
vigorously before sub-sampling takes place.
6.3.2 Filtration Procedure
a) The sample must be filtered irrsmediately after the
ozone-UV and ultrasonic bath treatment. tf for
any reason the sample has been stored for �nore
than a few hours after these treatments, it is
recommended that ozone-UV oxidation be repeated
for a short period of about 15 minutes, followed
by an additior�al 15 minutes in the ultrasonic
bath. •
b) Assemble the filtration base and turn on the
vacuum. The upper surface of the filtration base
(both the glass frit and the ground mating
surface) must be dry before the membrane filters
are installed. Place a 0.45 �,�m pore size type HA
Miliipore filter on the glass frit. If the
filter appears to become wet by capillary ac`.ion
on residual water in the glass frit it must be
discarded and replaced by another filter. Place
a 0.1 um pore size Nuclepore filter, shiny side
up, on top af the Millipore filter. If the
� Nuclepore filter becomes folded it must be
' discarded and replaced. The mating surface of
the reservoir component of the filtration
apparatus (the funnel) should be dried by shaking
off any surplus water and draining on paper tov,•el
or tissue. The funnel should be positianed on
the filters and firmly clamoed, taking care not
to disturb the filters. The vacuum should not be
released until the filtration has 5een completed.
It is necessary to comnent on the use of
filtration equipment which is still wet after
washing, Since improper �rocedures at this point
can very 5eriously compromise the results. If
the qlass frit is wet when the Millipore filter
is applied to it, capillary action will result in
some areas of the Millipore filter structure
being filled by water. When the Nuclepore filter
is applied to the surface of the Millipore filter
22
and the vacuum is appiied, the differential
pressure across the Mil)jpore filt?r will be
insufficient to overcome the surface tension of
the water in the filled areas. Thus no
fittration wili take place through the
correspondina areas of the PJucla�ore filter, and
a gros5ly non-uniform deposit of particulate �ill
be obtained.
c) Add the required volume of sample water to the
filtration funnel. Disposable plastic beakers
and pipets provide a�eans of ineasurinq the
required samp?? volume �Nithout introducing
problems of sample cross-contamination. The
reservoir may not be sufficiently large to
accorr�nodate the total volume to be filtered. In
this case more of the sample may be added d�ring
the.filtration, but this should be done carefully
and only when the rese�voir is more than half
full. In this way the addition will not disturb
or affect the uniformity of particulate already
deposited on the Nuclepore filter. Do not rinse
the sides of the funnel, and avoid other
manipulations which may disturb the particulate
deposit on the filter.
d) �isa55emble the filtration unit, and transfer the
�Vuclepore filter to a la�elled, clean petri
dish. Since the i��uclepore filters are mora
easily handled Nhile they are still wet, it is
recommended that the strip of filter to be �sed
for TE� samole preparation should be cut as
described in Section 6.4.2 before the filter is
dried. Place th� cover loose�y over the dish to
limit any dep�sition of dust onto the filter.
Dry the F'ilter under an infra-red heat lamp for a
short time before closing the pe�ri dish
completely. Discard the ��illipore filter.
6.4 Preparation of Electron ��icroscope Grids
Preparation of the grid for examination in the electron n��croscope
reQuires a high degree of man�,al dexterit� and is a critical step
in the procedure. The ohjer.tive is to replicate the filter suriace
by deposition of a carbon film and then to dissolve away the filter
i*self with a minimum of particle move�ent and breakage of the
carbon film. The filter dissolution procedure is iilus*.rated in
Figure 4.
23
vpRti��ES —C,R80N
� _ �� ' =poT NG
; �`
� �
°0�7Csa8GN:TE —
����R i
Q . o 0
�IECTRQN �—'
M�CAQSCOPE
, :,Q�O
6.4.I
�
CHLOROFORM
r— C4a80N
� �
�— �oi�
Figure 4. Nuclepore OissoTution Technique
Preparation of Jaffe '�lasher
Prepare th� Jaffe 'rlasher as illustrated in Fiaure 5A. The
stainless steel mesh is formed into a bridae slightly less
than 1 cm high, and placed in a 10 cm diameter glass oetri
dish with a tight fitting lid. A narrow strip of lens
cleaning tissue is placed over the bridqe with each end of
the tissue extending beyond the bridae to the base of the
petri dish. The other dimensions of the stainless steel
bridqe and the lenqth of the lens tissue are not cri*.ica1,
but those specified in Figure 5A have been found to be
satisfactory. After the assembly is complete, fill the
petri dish with ch;loroform to a level just below that of
the horizontal surfac? of the stainless steel bridqe. It
may be found that the Chloroform contacts the underside
surface of the stainless steel mesh; this is not critical.
Cover the petri dish with the tid and the Jaffe �asher is
ready for use. Each time the Jaffe '�►asher is used, the
lens tissue and solvent should be discarded artd replaced
with new lens tissue and fresh solvent. Appropriate
precautions should be taken �Nhen handlinq c�.loroform.
b.4.2 Selection of Filter Area for Carbon Coafing
- Poiycarbonat•e filters are easily stretched c'urinq handlina,
and cuttinq of areas fpr further preparation must be
performed with vreat care. The hest method is to use a
curved edqe scalpel blade to cut Che filter while it is in
24
Gl.AS$ PE'Ri DISH —, E�ECTRON MICROSCOPE
1 IOOmm • 15mm ) SPEC�MENS � 5T STEEL MESr+
• BR�O �E ! 50 mesn 1
�E
TI
�
1
� J �
1 :
l ��w •
.i���,ty� �c�
25
the plastic petri dish. Press the scalpei point on the
filter at the beginning of the desired cut, and rock the
blade downwards while maintaining pres5ure. It Nill be
found that a clean cut is obtained without stressing of the
p filter. The process should be repeated alonv ali four
directions to remove 3 rectangular portion from the active
filtration area of the filter. This filter portion should
;`- be seiected from along a diameter of the filter, and should
be about 3 rtvn wide by� a minimum of 15 mm lonq. Areas close
to the perimeter of the active filtration area should be
. avoided.
6.4.3 Carbon Coating of the yuclepore Fi)t�r
The ends of the selec*.ed filter strips should be attacha�
to a glass microscope slide using double-sided adhes�ve
tape. This must be performed carefully to ensure that the
filter strips lie flat on the slide and are not stretched.
The filter strips can be ide�tified by using a wax pencil
on the glass slide. Af*.er inserting the necked carbon rods
into the vacuum evapor�:or, place the glass slide on the
sample rotation and tilCing device. The separation between
the sampTe and the tips of the carbon rods should be about
` 7.5 Cm to 10 cm.
If desired, the am�unt of carbon to be evaporated can be
monitored instrumentaily so that a thickness of about 30 nm
to 50 nm is deposited on the fitter strips. Alternatively,
a porcelain fragment wilt serve as a simple carbon
deposition monitor. Place a small drop of silicone
diff usion.pump oil on the surface of a clean fragment of
white glazed porcelain. Locate the porcelain in the
evaporation chamber with the oil droplet towards the carbon
rods and at a distance from the carbon rods eaual to that
separating the rods from the filter strips. Carbon will
not deposit on the oil drop whereas it does on the other
areas of the porcelain. With experience, the correct
thickness can be monitored visually by observation of the
contrast between the darkened areas of the porcelain and
the unc�ated areas under the oil drop.
Pum$ down the evaporation chamber to a vacuum better than
1�- Torr (0.013 Pa). Use of a liquid nitrogen coid trap
above the diffusion pump wi�l minimize the possibility of
contamination of the filter surfaces by oil from the
pumping system. Continuously rotate a�d tilt the olass
siide holding the filter strips, whi�e the carbon is
evaporated in intermittent bursts, aliowing the rods to
cool between each evaporation. This proc�dure is necessary
to avoid overheatina of the filter strips. Overheating
tends to cross-link�the polycarbonate which then bzcomes
difficult to dissolve in chloroform.
26
6.4.4 �ransfer of the Filter to E'ectron '�icrosccoe Gri�s
Remove the glass slide c3rryinq the filrer strios f,�o� ttie
evaporator, and using the tecr.nique des�ribed in 5.a.2 cu�
four oieces slightly less th�n about 3.�m x 3 mn^ in siz�
from each filter strip. The souare of filter should 'it
within the circumferen�e of an electr�n micrr,scooe grid.
Three cf the filter pieces are to be �rA�,;r�d on 200 mesh
copper grids, and un'ess the anslysis is to be for
chrysotile only, a fcurth piece shr,uld be �repared on a 2pn
mesh gold grid. Tne specimens prepared on coo�er grids are
used f�r fiber counting and �ost EDxA er.amir.ations. The
preparation on the gold arid �s intended `or EOXA ;�ork on
ribers containing sodium.
Place a piece ��f t�e carbon-coated fi�ter, carbon s�de �:o,
on to the shiny side of an e'ectron .^ir_roscope gri���ng
fine tweezers, �.'ck up the orid and �ilter toqether ard
place quick:y on to the �hloroform-saturated ;ens tissue in
the Jaffe '�lasher, 35 shown in Fiqure 58. It is �mportant
that the sampl� be placed on the lens tissue quickly, since
hesitatio� whil� the sample is exposed to chloro`orm vapor
will cause it to curt. This is a simplified technioue
which does not involve drop�inq of chl�roform on to the
samples.
Some components of the oolycarbon�:te fil;.ers now available
dissplve in chloro`orm cnly very slowly. Conseauently, tne
grids rr.��ct Se left in the Jaffe '.Jasher for lonoer than 4
days, and the solvent r�ust he revlaced every day.
Oepend;ng �n the particular 'ot number of tnE filtzrs, even
=his period may be insuff,cient to y»ld sat'sfactor� qrids
clear of undissolved �lastic. In this event, or if a more
rapid samp'e preoaration is desired, after a ninimum period
of 3G minutes in the laffe Washer the lens oaper supporting
the grids may be transferred to the condensation washer as
illustrated in Figure 5. The condensation washer should
ther. be op�rated for ;, period of bet�Neen 30 and 60.minutes,
after tivhich the ;rids will have been clearPd of residual
pTastic. The rate of condensation in the washer is not
critical, �rovided that chlorofi'orm drias rapidly from the
cold finger for the �Nhole of the washing period and the
condensation level is above the samples.
�urinq the d?ssolut�o�, it is recommend?d that tne orids
not be al�owed to dry since this has been found to oreativ
increase the time re�iuired for compiete dissolution of the
polycarbonat2.
27
,,..._�► —_ _ _.__ _ . _ .- �- - - -- . _ _ . . . �.�...__�__. _ _ . - . .
e �
CONOENSER
SPECIMEN
�
COl�O wATER
SOURCE
ADAPTER
�COLD FINGER
_ , WATER
DRAIN
FL�:SK
r;J SOLVENT
t
ij
� THERMOSTATICAI.�Y
CONTRO�LED
� . H£ATING MANTLE
Figure 6. Condensation Washer.
0
6.5 Examination by Electron Microscopy
6.5.1 Microscope alignment and Magnification Calibration
• Atign the electron microsc�pe accordinc to the
specifications of the manufacturer. Initially, and at
regular intervals, carry out a catib�ation of the two
magnifications used for the analysis (aooroximately 20,OG0
and 2,000) u5ing a diffraction gratino replica. The
calibration should always be reoeated after any
instrume�tal maintenance or change of operating conditions.
The maqnification of the screen image is not the same as
that obtained on photographit plates or film. T�e ratio
between these is usually a constant value for the
instrument. It is most important that hefore thP
maanification Caiibra!ion is carried out the sa�ole he�aht
is adjusted so that the sample is in the eucentric position.
�•28
,^.. _,..w � ----- -�_�.. _ _ . .
u.5.2 Calibration of EDX,� System
The purpose of the calibration is to enable quantitat:ve
composition data, at an accuracy of about 10`= of the
elemental Concentration, to be obtained from EOxA spe�tra
of silicate minerals involving the elements sodium, _
mdgnesium, aluminum, silicon, potassium, calcium, mancar.ese �
and iron. If quar�citative det�rminations ar� reGuired �or
minerals containing other elements, suitable caliCration
information may be incorporated in the computer analysis.
The well-characterized standarc�s recommended �ermit
calibration of any TEM-EOXA combination which meets the J
instrumental svecifications of Sectian 4.2, so that data
f rom different instruments can be compared. The standar��s
used for calibration, and tne elements which thpy
represent, are shown in Table 2.
TABLE 2. SILICATE �'1INERAL STANOARDS
Elements Mineral Standard
Na, Fe, Si Riebeckite
Mg, Si Chrysotile
Al, Si 4a�loysite
K, Si Phlogo�ite
Ca, Si '�1o11astonite
M�, Si Bustamite
The compositions of these standards have been determ�ned by
microprobe analysis, and the TE��t grids were prepar?d from
fragments ef the same selected mineral specim�ns. They
permit the corrputer �roqram of Appendix A to 5e used with
any TEM-EDXA system.
Place the first grid into the microscope, forn an imaoe at
the calibrated hiqher magnification of ahout 20,000, ard
adjust the specimen height to the eucentric poir.t. Tilt
the specimen towards the X-ray detector as reouired by �he
instrument geometry. Select an isolated fiber or particl�
les5 than 0.5 u m in width, and dccumulate an E�XA soectrum
using an electron orobe of suitable diameter. �hen a wel?
defined spectr�;m hac been obtained� oerfor�n an aoprooria:e
background subtraction and obtain the net oeak araas for
each element listed. using ener�y windows centered on the
29
- -- -..
4
r
peaks and about 130 eV wide. Compute th? ra�io of the p?ak
area for each specified element relative to the peak area
for silicon. Repeat the procedure for about 20 particles
of each mineral standard. Analyses of any obvious foreign
particles should be rejected, and the data from any one
stardard should be reasonably s21f-consistent. Calculate
thp arithmetic mean peak area ratios for �ach specified
element of each mineral standard. fhese values are
rsquired initially as input for the fiber identification
program, and apart from occasional routine checks to ensure
that there has been no degradation of the detector
resolution, the calibration need not be repeated ��nless
there has been a change of instrumental operating
conditions.
6.5.3 �rid Preparation Acceptability
Inse►t the specimen qrid into the electron microscope and
adjust the magnification to a value sufficiently low (300 -
1000) so �tiat complete qrid openings can be inspected.
Examine at ieast 10 grid openings to evaluate the fiber and
total particula*e loadings, the uniformity of the
particulate depos�t, and the extent to which the carbon
film is unbroken. The grid must be rejected from further
analysis if:
a) the grid is too heavily loaded with fibers to perf orm
an accurate count. Accura�e counts cannot be
performed if the grid has mo^e than about 50 fibers
per grid opening. A new grid pr�paration must be made
using either a smaller volume of w�ter or a suitable
volume of the water diluted with fiber-free water;
b) the overall distribution o
noticeably non-uniform. A
be made, paying particular
particulate dispersal and
f tFe deaosited d�bris is
new qrid preparation mu5t
attention to proper
filtration procedures;
c) the arid is too heavily loaded with debris to allow
examination of individual particles by SAED and EDXA.
A new grid preparation must be made using either a
smaller volume af water or a dilution of the original
water sample;
d) a larqe proportion of the grid ope�ings have br�ken
carbon film. Since the breakaqe is usualiy more
frequent in areas of heavy deposit, counting of Lhe
intact openings could lead to biased results.
Therefore, a new grid preparation must be made from a
more cor;,pletely dispersed sample, a reduced volume of
sample, or alternativety, a thicker carbon film �ay be
necessary to support the larger particles.
30
6.5.4 Procedure for Fiber Countinq
The number of fibers to be counted depends on the
statistical precision de5ired. In the absence of fibers, ^
the area of the electron microscooe qrids which must be
examined depends on the analyticai sensitivity required.
For statisticat reasons, d;scussed in Section 7.2, the
fibers on a minimum of 4 grid openings must be counted.
The precision of the fiber ccunt depends no� oniy on the �
total mimber of fibers counted, but al:� nn their
uniformit.y from one grid ope�ing to 'the next. In practice,
it has been found that terminat°on of the fi5er count at a
minimum of 100 fibers or 20 grid openings, ��hichever occurs
first, yields results �Nhich usually require no further
refinement. Additional fiber countiny will be necessary if
greater G�ecision is required.
At least three grids prepared from the filter must be used
in the fiber count. �everal grid ooenings are to be
selected from each grid, and the data are a11 incorporated
in the catculation of the results. This permits the
measurements to be spread across a diameter of �he oriqinal
filter, so that any qross deviations from a uniform
deposi�ion of fibers should be detected.
Figures 7 and 8 show specimen fiber counting raw data
sheets which represent the minimum standard of data
reportinq for this analytical procedure. Figure 7 shews
page 1 of the raw da�a t�bulation, ��hich contains all
specimen preoaration details. Figure 8 is a continuation
sheet for the fiber classification ar,d �easurement data;
several of these sheets may be required for ana�ysis of a
sample.
Select a typical grid opening from one of the grids. Set
the magnification to the calibrated higher value (about
20,000). Adjust the sample height until the featur�s in
the center of the screen are at the eucentric point. Check
that the goniometer tilt is set at zero. Reduce the
maanification to the lower calibrated value of about 2,000.
heasure both dimensions of the grid opening imag� in
millimeters, u5ing the markings on the fluorescent screen.
In columns l and 2 specify the sequential number of the
grid opening, and its dimensions. These t�No coTumns are
not used again unt��l fiber counting is co�rtnenced in the
next grid opening to be examinea. Adjust the magnificati�n
to the upper calibrated �iatue, close to 20,000, �nd
position the grid ooening so that one corner is visib�e on
the screen. Move the imaqe by adjustment of only �ne
translation control, careful'�• oxamining 'he sample for
fibers, ��ntil the opposite side of the opening is
encountered. Move the image by one screen ��idth �sing the
31
�
�,
ASBE570S ANA�YSIS - aATER SAMPLE DATA
'cu' --{ SAMPLE:
J08: I
', PREP: By _ Oate - - �OUNT: By Oate - - P40CESS: By
[NSTRUMEYT: MAGtvIFICATI0N5: Grid Count
OIL'JTIONS: 0 '
I 1 Volume Taken (ml) Final Volume ;ml; _
2 Volume 7aken (mL) �inal Volume (mL)
fINAI PREPARATtON FIL'RATiON: Vol. Piltered (mL)
• COCE '
1 i
� �
Date - - I
Ac:ive Area {cm�)
�
i
„— -- �
COMMENTS: (for inClusion in computer print-out; Tormat in 5 lines of 50 characters) �
I
�
;
FIBER CLASSIFICATIQNS: !
COIiNT. NAM �M CM C� CQ C�!Q CC�O Jf AD �X �DX AQ A00 �ZO a.Z? i
PROCESS• '
� fI6ER TYPE � CLASS;FI�.1'ION ; Ft?Et2 'yP` � CLMS�:=tCr�iGr� �
NOTES: Pr�paration:
� Examination:
i
I
I
Figure 7. Sheet for R�cording Water Sample Oata.
�?
a
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33
-----'-r'"
-�.._ __ .
y.
other translation control, and then scan the ir.,aqe in the
reverse direction. Continue in fihis manner until the
entire grid opening has been inspected. �lhen a fiber is
<> detected, classify i� according to the procedures descrihed
in Section 6.7, and then insert the approoriaLe
classification on the data sheet. "�easure the lenath and
width of the fiber imaqe in millimeters and record th?se i�.
� the appropriate columns of the data sheet. Do not record
fibers of obvious biological origin or diatom fragments.
Continue the examination until I00 fibers have been
recorded in all classification categories of interest, or
until 20 grid openinos have been inspected. The data
should be drawn approximately equally from the three
grids. In all samples, fibers on a�ninimum of 4 grid
openings must be counted. Fibers less than 0.5 um in
. length will not be incorporated in the fiber concentration
calculation.
6.5.5 Estimation of Mass Concentration
If the primary objective of the analysis is to determine
the mass concentration, the fiber countinq should be
approached in a different manner. The number of fibers
which must be counted in order to achieve a reliable
estimate of the mass concen}ration depends primarily upon
the range of the fiber diametzr distribution. The mass
concentration measurement is most sensitive to fibers of
" � iarge diameter, which unfortunately are among those which
occur infrequently. When [he diameter distribution is
narrow, such as that found in the tase of chrysotile
fibrils, then the mass concentration has ap�roximately the
same precision as that of the number concentration.
, However, the mass concentration may be actually meaningless
when calculated from a low number of fibers observed during
a routine fiber count, if these fibers have a broad
. distribution of widths.
If the mass concentration is the pri,nary interest, and the
precision required is greater than is possib'e from the
normal fiber count, a dif`erent approach to the fiber coun�
must be used. Initially, establish the larvest �idth of
fiber which can be detected on the grid by a cursory
survey, at a reduced magnif�cation, of a laroe number of
grid openings (about 50). Calculate the volume of this
fiber. Adjust the magnification to a value such that a
width of 1 mm on the screen corresponds to 10� of the width
of the previously selected larqe fiber. Carry out �
routine fiber Count for a minimum of 100�fibers, recordina
onty fiber images greater than 1 mm in width. Continue
Countinq until the total volume of fibers is at least 10
times the volume of the originally selected large `iber.
The precision and accuracy of this technique has not been
34
M
investiqated fully, but for samples �Nith broad width
distributions it is capable of yieldino ;ignificantly more
precise mass determinations than are obtainab)e by the
conventional fiber count.
7he remaining problem concerns the assumption that the �
widths also represent the thicknesses cf the fihers.
Heasurements of particle thicknesses can be made
separately, using the shadow castina technivue. Before the
filter is carbon coated, apply a vacuum coating of
platinum-carbon or gold to the active surface of the ~
Nuclepore filter at an anqle of 45°, In the TEM, the
fibers will then display shadows on the carbon film which
approximate to their thicknesses. Suitable techniques for
shadowing are described in the o��er by D.E. Bradley
inctuded ,n the Selected Bibliogr,:phy.
6.6 Fiber Counting Criteria
6.6.1 Fiber Counting Method
Fiber counting with this analytical �nethod will be
performed only by the qrid openinq technique. If a
specimen grid is too heavily loaded for examination of
entire grid openings, a more reliable result is obtained hy
preparation of a new filter, usinq a smaller volume of
sample.
6.6.2 Fibers blhich Touch Grid Bars
A fiber which intersects a grid bar will be counted only
for two sides of the grid openinq, as illustrated in
Figure 9. The length of the fiber will be rec�rded as
twice the visible lenqth. Fibers in�ersecting either of
the other two sides wilt not be included in the count.
�
00 NOT COUNf
r� � � � �
' � CouNr as � i
.... . � I
� �:,, . �. ,
�1:..!� ; .� ti , JO NOT
b,•;.,.�..,. / 1:` CCUNt
COUHi 4S/ ��
� / —: `w--� _: �
Figure 9. Count1ng of Fibers Which Overlap Grid 3ars.
35
w
This procedure ens��res that the numerical count will be
accurate, and that the best average estimate of length has
� been made.
6.6.3 Fibers Which Extend Outside the field of View
Ouring scanning of a grid openinq, fibers which extend
� outside of the field of view must be counted systematically
to avoid double—countinq. In qeneral, a rule must be
established so that fibers extending outsi�e the field of
view in onTy two quadrants are counted. Fibers without
terminations in the field of view must not be counted. The
procedure is illustrated by fiqure 10. The lenqth of each
fiber counted is established by moving thP sample, and then
returnirtg to the original field of view before scanning is
continued.
�
Figure 14. Counting of �ibers Which Extend Outside the Fi•eld of View.
,
6.6.4 Fibers with Stepped Sides "
A fiber with stepped sides will he assianed a�Nidth mid-way
betr�een the minimum and maximum widths.
36
eucentric oosirion. Tift the fiber until a pattern apoears
which is a symmetrical, two dimensional array of soots.
The recognition of zor,e axis alignment c�nditions reGuires
some experience on the part of the overator. During
tiltir.g of the fiber to obtain Zone axis conditions, the
m�nner �n which the intensities of the spots vary sheuld be
observed. If �Nea� reflections occur at so�e points on a
matrix of strong reflections, t_he Dossibility of multiple
diffraction exists, ar,d some caution should be exercised in
selection of diffraction spots for r��easurement. A full
discussion �f electron diffraction and multipie diffraction
can be found in the references by J.A. Gard, P.�. Hirsch et
al, and H.R. Wenk, included in the Selected Bibliography.
Not all zone axis patterns which can be obtained ar� useful
or definitive. Only those which have �losely—spaced
reflactions correspondino to low indices in at least one
direction should be recorded. Patterns in Nhich all
d—spacings are less than about 0.3 nm �re not useful and
are usually very wasteful in computer time. A useful
guideline is that the lowest angle reflections should be
��ithin the radius of the first gold diffraction ring (111),
and that patterns with smalier distances between
reflections are usually the most definitive.
Five sp�ts, closest to the center spot, along two
intersecting lines of the zone axis pattern must be
SeleCted for measurement, as �llustrated in Fig�re 14.
•
SPOTI
SPOT 3 �POT 2
•
e2 e� �
SPOT 4 e3 •
� ea
•
�
SPOT 5
•
Figure I4, Measurement of Zone Axis SAED Patterns. -
41
�
�
�
The distances of these spots from the center s�ot and �hP
tour angles shor+n are the input for the comvuter proqram.
Since the center spot is usually vzry over-exposed, it dees
not form a suitable or;gin fcr measurerrent. The reauired
distances must therefore be obtained by measuring between
pairs of spots symmetrically disposed about the center
spot, preferably separated by several repeat distances.
The distances must be measured with a precision of better
tt,an 0.3 mm� and the angles be'ter than 2.5°. The
diameter of the first or Second ring of the calibration
pattern (111 and 200j must also be measured with the 5ame
precision. _
The camera Constant (aL) required for the computer program
is 7iven by:
where:
al = aD
h2+ k2 + }2
a� Wavelength of �;�e inci�ent electrons
L= Effective camera lengtn in rtm
0
a= Unit cell dimension in Hrgstroms
0� Diameter of the (h, k, 1) diffraction
ring5 in millimeters
h, k, 1= Miller indices of tne sca:terina olane
of the crystal.
Using gold, the camera constant is qiven by:
�� � 2.3548 D (`irst rinq)
aL � 2.0393 D (second ring)
Analysis of a fiber by EOXA is required in this analytical
procedure. Interpretation of the EDX� spectrum may be
eithPr qualitative or quantitative. For qualitative
interpretation of a spectrum, the elements oriqinatinu from
the fiber are recorded. For quantitative interpretation,
the net peak areas, after backqround subtraction, are
obtained f�r the elements originatino frcm the fiber, As
discussed in Section 6.5.2, this method provides f�r
quantitative interpretation for tt;ose minerals which
contain silicon.
, 42
To obtain an E�XA sp?ctrum move the imaqe uf thA Fiber to
the center of the screen and remove the objective aoer�ur•�.
Select an appropriate electron beam dia�eter and defler_t
the spot to impin9e on the fiber. DeoPnding on the
instrumentation, it may be necessary to tilt the samole arc
in some instruments to use Scanning Transmisci�n _l�c�ron
Microscopy (STEM) moda of operation,
The ti�e for acouisition of a suikabte spectrum varies ��ith
the fiber diamet��, and a15o with instr��mental factors,
For quantitative interpretation, spectra should have a
statistically valid number of counts in each peak.
A.nalyses of small diameter fibers which contain sodium ar?
the most criticai, sinc�� it is in the lew eneroy range that
the X—ray detector is �east sensitive. �ctor�ingly, it is
necessary to acquire a spectrum for a sufficiently long
period that the presence of sodium can be detected in such
fibers. It has been found that satisfactory quantitative
analyses ca� be obtained if acquisition is ��nti�ued until
the background-subtracted silicon K� peak integral exceeds
10000 counts. The spectrum should then be manipulat2d to
subtract the background and t� obtain the net areas of the
elemental peaks.
After quantitative EOXA classification of some fi5ers by
computer analysis of the net oeak areas, it�may be possible
to classify further fibers in the same sample on the basis
of compar�son of spectra at the instrument. Freouently,
visual com�arisons can be made after so�e�hat shorter
aCquisition times.
6.7.3 Anal�sis of r"iber ldentification Cata
Since the fiber identification procedure can 5e involved
and time—consuming, a Fortren computer program has been
provided, the listing of which is given in Appendix A.
This program permits the EDXA and zone axis SAE�
measurements to be �ampared avainst a library of
compositional and structural data for 226 minerals. The
mineral library includes fibrous species which have been
listed by several authors, toaether with other �inerals
which are known to be similar to amphibole in either their
compositions or somE aspects of their crystalloqrapny,
AddiLional minerals may be added to the library if the� ar�
thouqht to be of concern in particular s�tuations.
Rejection of a mineral by the program indicates thaL ei�her
the compositional or crystallo�raphic data for the �ineral
in the library are inconsistent with the mP_a5urem�r,�5 Tade
on the unknown fiber. Oemonstration that the �easureTer�s
are consistent with the data for a particular test �irera'
daes not uniauely identify the unknown, since thP
possibility exists that data from oth?r minerals �ay �lso
43
�
be consistent. It is, however, very unlikely that a mineral
vf another structural class could yield.data consistent with
that from an amphibole fiber identified uniquely by quanti-
tative EDXA and two zone axis SAED patterns.
:°'. The computer program classifie5 fibers initially on the
� basis of chemical composition. Either Qualitative or
auantitative EOXA information may be entered. The
` procedure using qualitative EDXA consists of entering the
� list of elements which originate from the particle. F�r
quantitative EGXA (silicon-containing minerals only), the
list of elements and the areas under the corresponding
X-ray emission peaks, after hackground correction, form the
inpu+ data for the computer program. The width of the
fiber is also required as input into the proqram. The
program will select from the file a list of minerals which
are consistent in composition with that measured for t'�e
< unknown fiber. To proceed further, it is necessary to
-'obtain the first zone axis SAED pattern, according to the
`instructions in Section 6.7.2.
It would be attractive to specify a partic�lar zo:ie axis
pattern to be obtained for confirmation of amphibole,
particularly if such a pattern could be considered
characteristic. Unfortunstely, for a fiber with random
orientation on the qrid, no specimen holder and aoniometer
currently available �ill permit convenient and rapid
location of two pre-selected zone axes. �The most practic3l
approach has been adopted, which is to accept those low �
index patterns whiCh are easily obtained, and then to test
their consistency with the structures of the minerals
already pre-selected on the basis of the EDXA data. Even
the structures of non-amphihale minerals in this pre-
selected list must be tested against the zone axis data
obtained for the unknown fiber, since non-amphibole
minerals may yield similar patterns consistent with
amphibole structures in some orientations.
The zone dxis SAEO inter�retation part of the proqram wili
cons'de►' all mine�als previously selected from the file as
being chemically compatible witi� the EDXA data. It will
then return a second and usually reduced �ist of minerals
for which solutions have been found. A second set of zone
axis data from another pattern obtained on the s�me fiber
can then be processed either as further confirmation or ;,o
attempt elimination of an ar^biguity. In�.addition, the anqle
measured between the orientations of the two Zone axes car
be entered into the corrputer to be checked for consistency
with the structures of minera;s. Caution should be
exercise� in rationalizing the inter-zone axis anqle, since
if the fiber Contains c-axis twinnin the two zone axis
SAED patterns may originate from theyseparate twin crystals.
44
In pr�ctice, thp full proqram will normall�� 5e aoplio� ��
very few fibers, unless precise identification of �11
fibers is reouired.
6.7.4 Fiber Classification Categories
It is not always possibl2 to proceed to a definitive
identification of a fiber; this may be due to instrumental
limitations or to the actual nacure of the fiber. In many
analyses a definitive identification of each fiber may not
actually be necessary if there is other knowledqe available
about the sample, or if the concentration is belo�x a level
of interest. The analytical procedure must ther?fore take
account of both instrumental limitations and varied
analytical require�ents. Accordinqly, a system of fiber
classification has been devised to �ermit accurate
recording of data. The classifications are shown in Tahles
3 and 4, and are dir�cted tewards identification of
chrysotile and amphibole respectively. Fiber; wiil be
reported in these categories.
7he general principle to be followed in this analytical
procedure is first to define the most soecific fiber
classification (target classification) which is to he
attempted. Then, for each fiber examined, the classifica-
tion �Nhich is actuatl� achi2ved is recorded. �epending on
the intended use of the results, criteria for acce�tance of
fi�bers as "identiried" can then be established at any time
after completion o` the anaiysis.
In an unknown sample, chrysotile will be reQarded as
confirmed only if a recorde�, calibrated SAEO pattern from
one fiber in the CD category is ohtained. Amphibole .rill
be regarded as confirrred only by obtaining recoroed data
which yields exclusively amphibole solutions for fibers
classified in the AZQ, aZZ or AllQ categeries,
6.7.5 Procedure for Classification of Fibers �ith Tuhular
Morphology, Suspected to be Chrysotile
hlany fi5ers are encountered which have tubular morpholoa��
similar to that of chrysotile, but which de�y further
attempts at cha�acterization by either SAEO or EGX;�. They
may be nor�-crystallire, in which case :i�ED techniaues ar�
not usefui, or the� may be in a position on the ari�' ;�h��h
does not permit an EDXA soectrum t� be obtained.
Alternatively, the fiber may be of organic oriQin, but not
sufficiently definitive that it can be disre�arded.
Classification attempts will meet with varicus degrees c�
sucCess. Figure 15 shows the C13s5ifica�ion nroced�,re to
be used for fibers which display any tUbular ,�crpnoloa�i.
45
TM
CM
CD
CQ
CMQ
COQ
NAM
TABLE 3. CLASSIFICATION OF FIBcRS '�ITH TUBUTAR MORPHOLOGY
- Tubular Morphology not sufficiently characteristic
•for classification as chrysotile
- Characteristic Chrysotile Morphology
- Chrysotile SAED pcttern
- Chrysotile composition by Quantitative EDXA
- Chrysotile Morphology and composition by
Quantitative EDXA
- Chrysotile SAED pattern and composition by
Quantitative E�XA
- Non-Asbestos Mineral
TABLE 4. CLASSIFICATION OF FISERS WITHOUT TUBULAR �iORPHOLOGY
UF - Unidentified Fiber
AD - Amphibole by random orientation S�ED (shows layer
pattern of 0.53 nn spacing}
�
AX - Amphibole by q�alitative ED��1. Spectrum �as ele�ental
- components consistent with amphibole
ADX - Amph:bole by random orientation SAcD and Qualitative
EDX�
AQ - Pmphibole by Qvantitatire E�XA
A2 - Amphibole by one Zone Axis SAED
AOQ - Amphibole by random orientation SAEO and Quantitative
EDXA
AZQ - Amphibole by one Zone Axis SAED pattern and Quantitative
EDXA
All - �Amphibole by two Zone �xis SAED patterns with consistent
inter-axial angle
AllQ - Pmphibole by two Zone Axis SAED patterns, consistent
inter-axial anqle and Quantitative EDYA
VAM - Non-Asbestos Mineral
46
FIBEFi WITH TUBULAR MORPHO�OGY
IS tiber morphology :naraCtzrtstic
of [hat displjyed b•� r=rere�ce C��/SOL�12?
�xaMine by SAEO
Fat:ern nut I Ch r+sotile
:��ySOtile Dattern
�at:ern nu: 7r?Sen!
or ind:Stir.CC
TM �
Examine Dy audntitattv2 :�X:.
�Om00'lt'Gn n0[ i,hr�50Li12
Chdt o` Chrysotile CCmDO51C1C�
t�a Scec�rum
NCM TM CO
�
�
i
�,camine �v SAED
�hrySOC'�^ �3C�@�'1 ^OC
�at_ern c�rysct�te
°�CCe�n noc :r=sent
or indi5t�nc�
CM
�,cam+ne �Y quanti:a�i•�e ;�fA
���j�50t1i2 :OR�DOS1!'011 f10:
coTposit�on � Chat �f Cnriso;ile
VO $DeC_r;�m
] cM �
E,camine oy quantira;i•�e E�xA
::omoos�:•cn �ot
C��at of �hrysot�le
'lo Soec:rum
' CD
:��ySOCt'.B
�:m0051:'�n
Figure 15. Classification Chart for Fiber '�lith Tubular l�lorphology.
�
�
0
47
�
The chart is selr explanatory, an� essentially every fiCer
is either rejected as a non-asbestos mineral (PaA.M), or
classified in some way which could still contribute to the
chrysotile fiber count.
Morphology is the first consideration, and if this is not
similar to that usually seen in chrysotile standard
samples, the initial classification is TM. Regardless of
the doubtf��l morphology, the fiber ��ill still be examined
by SAED and EDXA methods according to Figure 15. Where the
morphotogy is m�re def�;�itive, it may be possible to
classify the fiber as having chrysotile morphology (CM;.
The morpho��gical characteristics required will be:
a) the individual fibri:s shoul� have high aspect ratios
exceeding 10:1 and be about 40 nm in diameter;
b) the electron scattering power of the fiber at 60 to
100 kV acceleratinq potential should be sufficiently
low for internal structure to be visible; and '
c) there should be some evidence of internal structure
sugqesting a tubular appearance similar to that shown
in Figure 16A, which may degrade in the electron beam
to the appearance shown in Figure 166.
Every fiber having these morphological characteristics will
be exa�ined by the SAED technique, and only those which
give diffraCtion patterns with the precise characteristics
of Figure 17 wiil be classified as chrysotile by SAED (C�},
The relevant features in this pattern for identificati�n of
chrysotile are indicated. The (002) reflections should be
�examined to determine that they correspond approximately to
a spacing of 0.73 nm, and the layer line repeat distance
should correspond to 0.53 nm. There should also be
"streaking" of the (110} and (I30) reflections. Using the
millimeter calibrations on the microscope viewing screen,.
these observations can readily be Tade at the instrument.
A TEM micrograph of at least one representative fiber will
be recorded, and its SAED pattern wi11 also be recorded on
a separate film or plate. This ptate xill also carry cali-
bration rings from a knowrl polvcrystalline substance such
as gold. This calibrated oattern i� the _o�nl� documentary
proof that the particular fiber is chrysotiTe- and not some
other tubular or scrolled saecies such as ha�loysite, paly-
gorskite, talc or vermiculite. The proportion of fibers
which can be success`ully identified as chrySotiTe by SAED
is variable, and to sone extent depend2nc on both the
instru�ent and the precedures of �he operator. The fiber�
that fail tr, yield an ider.tifiable SAE� pattern .will remain
in the TM or Gh categories unless they are examined by cDXH.
48
,,._,.:__.
Figure 16A. TEM Micrograph of Chrysotile Fib�il, showing htorphology.
.� ;
• . ;. ' .
, ,,
Figure 166. TEM t-�icrograph of UICC Canadian Chrysotile Fiber after
Thermal Degradation by Electron Beam Irradiation.
49
�
�
r
� __
�
�
, .DS7nm
/ -
� tiQ, �
t30 �
i
Figure 17. SAED Pattern of Chrysotile Fiber with Diagnoscic Features Labelled.
Necessary criteria are the presence of 0.73 nm spacing fpr the
002 reflections, 0.53 nm spacing for the laver line repeat and
characteristic streaking of the 110 and 130 reflections.
6.7.6
In the �oza anaiysis of cnrysotii� there are only two
elements which are relevant. For fiber classification, the
EDXA analysis must be auantitative. If the soectrum
displays prominent peaks from magnesium and silicon, with
their arpas in the ap�ropriate rdtio, and with only minor
peaks from other elements, the fiber wiTl be classified as
chrysotite by ouantitative EDXA, in the cateqories CQ, CMQ
or COQ, as appropriate.
For chrysotile analyses there are essentially three
possible levels of analysis:
1. morphoioqical and SAEO discrimination only (Tarqet
classification CD);
2. in addition, EDXA of only those fibers unclassified by
SAEO (Tarqet classification CO);
3. EOXA in addition to SAED on all fibers (Target
classification COQ).
Procedure for Classifitation of Fibers Without Tubular
horphology, Suspected to be A.mphibole
Every particle without tubular morphology and which is not
obviously of biological origin, with an asoect ratio c� 3
to 1 or greater and having parallel or stepped sides, wi11
be considered as a suspected amph��bole f;ber. Furthzr
examination of the fiber by SAE� and E�XA techniaues wil�
50
meet with a variable daqree of success, de�endinq on th�
nature of the fiber and on a number of instrument�l
limitations. It wi11 not be posSitilQ to identify every
fiber completely, even if time and cost were of no concern.
t4oreover, confirmation of the presence of amphibole can he
achieved only by quantitative interpretation of zene axis
SAEO pattern5, a very time-consuming procedure,
Accordingly, for routine samples fron unknown sources, this
analytical procedure limits the reeuirement for zone axis
SAED work to a minimu� of one fiber represent�tive of each
compoSitional cldss reported. in some samptes, it may be
necessary to identify more fibers by the zone axis
technique. When analy2ing samoles from ��ell-character�zed
sources, the cost of identification by zone axis mP*nods
may not be justified,
The 0.53 nm layer spacinq of the ran�om orientation SAc"D
pattern is not by itself diagnostic for amphibo�e.
However, the presenCe of c-axis twinning in many fibers
leads to contributions to the tayers in the patterns by
several individual parallel crystals of different axial
orientations. This apoarently random positioning of the
spots along the layer tines, if also associated �ith a high
fiber aspect ratio, is a characteristic of amphibole
asbestos, and thus has some limited diaanostic value. If a
pattern of this type is not obtained, the identity of the
fiber is stili amb�4uous, since the absence of a
recognizable pattern may be a consequence of an unsuitabl?
�rientation relative to the electron bea�, or the fiber may
be some other mineral species.
Figure 18 shows the fiber ciassification chart for
suspected amphibole fibers. This Chart ShOwS all the
classification paths possible in analysis of a suspected
amphibole fiber, when examined systematicaliy by SAED and
EOXA. Initially two routes are oossible, deoending on
whether an attempt to obtain an EDXA soectrum or a rardom
orientation SAED pattern is made first. The normal
procedure for analysis of a sample of ur,known oriqin will
be to exam;ne the fiber by random orientation SaED�
qualitative EDXR, quant;�ative cCXA, and zone dxis =.=.`0, in
this sequence. The final fiber classification assiQnea
wi;l be defined either by successful analysis a� the target
level er by the instrumenta' limi���ionS, Th� maximum
classif;cat�on achieved for each fiber will be recorded en
tne �ounting sheet in the approoriate Column. T;e var�o�s
ciassification cateqories can then he comhin�d �n any
desired k�ay for calculation of the f?5er cencentration, and
a complete record or" the results frcm each fiber is
msintained for r��ssessment of the data if necessary.
clJ
f
� /i7CP wITHOUT "UBVI�� yC9ov7���Y
z..... . p�. '�e�. ::�i x.;... :��•'•r -. ..rnu�
' ...H, .1.'en<i � �.• , . . ;�[;
- . . ��0'.KI� an
I
.. �y . � � .�.. ..�. . . .
.iC..�. l,il ^' ..�t�.
I�Y�V ' •
� 'b :>e!:rv�
a�':<.. .r• . .! .
� �
��. �_�...<'• '.Y.
...... I�Y 1 .
� l�� _�_.,
� . � ��f. YJYI 3�
.. Jql Jw1+I�t�.� :)�1 I . �
�Hr }ppf. an �
�'l` �
' ��on�xl�' I .
Jp.� :•� :�;:•u t .�e� :)�: . .
•'r�e+: ,� � ����t .�. i .. .� �
. �S � i ✓o••eo i�e _e 1
I Ndu !
• �� .. ( .i . .i
.. � � r� ' 'aii :G�� �_�M: _
r0Q ` �
; � y - C :•I � '�(:' f .
. ,::� . �l
:,,:•_ V . . - �-,l ;_�
, . w
, ,
..:
, . , ..:. .. ..
..... ...,.
:�.:... :., .. .: =
:..
, ,.� � .� ...
�____ � �p :.�:..�
� � �
� � _, ^ ' 'e^.'E: �v . � . , �". . . .. ' � i -- .�.
aoi:� ;—`_' . a2 i
� � IR1` .. ' `1GN1 '
� � i i l. V�ry' .. ..a . .. � ,�. .�.. i
' � ..�a I (y�y� �v�� :G] '
�. T
i i ,�. '' i ,a � _c �,,,,
, :Z� � �` � T :�, � - � �: . :. -:� .
� ,:�:::,.�- .. .. . �,
.Q .� _�
; ;�= '`� .. .. .� -�,�`_
. r-.---�--� `=� 1. j ,...
., :
m -�^
i .��� ' �Z.
, �o s�.n � �� _
'� �� ,b :... . ��. .
: ,� -,�1,- °Cp'
�
,•z; : �:.... �z� �:� _ . .
+�c+ x'< *c �'>°
.i•d .t r• . .
?[: �0' �`
:•a : � t:;: �
-:e.:,..;� �. . . , �
. ~_L � .:�
V�YI JZ� �i. �
.t' 1+ . .
4� �
Figure 18. Classification Cnart for F�ber 'rlithout Tubular ��tor�holooy.
Bold Lines indicate the Preferred Paths.
52
Dependinq on the particular situat�on, rour leve?5 n�
analysis can be defined in r_his analyticat �rocedure, and
these are shown in Table 5.
In the routine unknown sam�le, a levet 3 analysis �ill be
required if the presence of amphibo'e is to be confir�ed.
For this level of analysis, attemGts �il? be made to raise
the classification of ev�ry fiber to the PGq category. tn
addition, at least one fiber from each type of suspectpd
amphibole found will be examined by zone axis S�ED �ethods
to confirm the identification,
TABLE 5. LEVELS OF ANA�YSIS FOR AMPHi30LE
Level of �pp�ication Target Required Classification
Analysis Classification for Confirm�tion of
for all Fibers Amphibole in e Proportion
of th2 �ibers
1
2
3
4
Routine monitoring of
known and well-charact-
erized sources for one
mineral fiber type.
Routine monitoring of
known and well-charact-
erized sources where
discrimination Letween
two or more amphiboie
fiber types is required.
Routine samples from
uncharacterized sources
in which pr.esence or
absence of amphibole
is to be confirmed.
Samples where precise
identification of all
amphibole fibers i;
an impor*.ant issue.
ADx
ADQ
aoQ
azQ
53
Not Applicable
P�ot Appl'cable
All, AZQ or AllQ -
Sol�!tions must
inc;ude only
amphiboles.
AZLQ - Solutions
must incluc� on�y
am�hibol?5.
w
�
�
.
6.6 Blank and Control Determinations
To ensure that contamination by ex�raneous fibers durinq sa�o'e
preparat�on is insignificant �ompared with the results reported on
� Samples, it is necessary t� establish a continuous proGram of blank
measurPments. Initially, and at intervals durinq an analytica'
program, it is also necessary to ensure that samples of known fiber
concentrations ca� be ar��lyzed satisfactorily.
6.8.1 Blank Determinations
At least one blank determination will be made along wi�h
every group of samples prepared at any one time. For the
blank determination, a 0.1 �m �uclepore filter will 5e
prepared by filtration of 100 mL of oze�e-UV tr�ated
fiber-free water if using ZS rrm diameter equipment, and
500 mL treated water if using 47 mm diameter equipment. If
the samples have been preserved with mercuric chloride, an
equivalent amount of the solution should be added to the
water used for the preparation of the blank. This blank
filter will be carbon coated at the same time as the group
of samples, and solvent extracted in the same Jaffe
'�asher. All aspects of the samqle preparation will then be
i,aentir.al to those for the actual samples. Ail fibers on
20 grid openings of the b�ank sample ��ill be recorded. Yhe
mean fiber concentration for the blank must te less than
0.05 MFL or less than lo of the loweSt individual value
reported in the sampies concerned, whichever is the arPater
value. If a value higher than these criteria is
encountered, satisfar_tory blank values must be denonstra=ed
before further analyses are carried out. If it is
susoectec �:�at ssmp'es could have been contaminated during
the original preparation, the duplicate bottles should be
used for the repreparation of the samples concerned.
6.8.2 Control Samples
Control samples must be incorporated into sample anaiysis
` programs in order to demonstrate that the expected results
can be produced from sampies of known fiber concentration.
; Such reference suspensions can be prepared using a�poules
; of stable fiber dispersions listed in Section 4.3.10. It is
recommended that the range of fiber concentrations found in
the real samples should be simulated using the rAference
suspensions. The sealed am�oules of fiber dispersions
become unstable when they ar? opened, and the fiber
concentration value should not be rel'ed upon for more than
8 hours after opening. Accordingly, it is recommended
that, upon opening a dispersion concentrate ampo�le,
severat reference susoensions of �ifferent fiber
` concentrations be prepared in sample bottles. These
54
botties can tf�en be stored for �reoar,jtior. and anal�.sis
along with water sampies of urknown fiber Conrontrations.
7. C�LCUI:aTION OF RESULTS
The result� are conveniently calculated usino � �qmDu�er �ragram, the �
listin� of which is provided in Appendix B. �The r�e:hods by wh;ch the
calculations are made are described below.
7.1 Test for Uniformity of Fiber Deposit on Elect�on Hicroscooe Urids
�
A check must be made using the chi-square test, to determine
whether the fibers found on individual grid ooenings are randomly
and uniformly distributed among the qrid openings. If the tota'
number or fibers fcund in k grid openinas is n, and the 3r2�S or
the k individual grid openinqs are designated A1 to AK, ttien
the total area examined is
i = k
A = � Qi
i = 1
The fraction of the total area exar�ined which is re�:-esented by the
individual grid opening area, ��� is qiJen by A�/F, If the
fibers are randomly dnd uniformly diseersed over the k qr�d
openings counted, the expected number of fibers fal�inq in one ar�d
opening with area AT is rN�. If the observed n;,mb��r fcund on �
that grid opening �s n�, then:
i = k
2 _ � (�i - np��2
'� n p
i=1 �
This value is comp�red with significance p01r,tS of the ;t2
distribution, having (k - 1} deqrees or freedom. Sianificance
levelc lower than O.lo are cause for tne sampt� analysi�s to be
rejected, since this corresoonds to a very tnhOm002n?Ou5 de�os�t.
If this occurs, a new filter should �e preparQd, oaving r*ore
attention to both uniform dispersal of the sus�ension ard the ry
fittration procedure �s descri�ed in Secti�n 6.3.2.
55
�
1.2 Calculation of the �ean and ConfiCence Int�rval
of the Fiber Concentration
In the fiber count, a maximum of 20 grid openings have b��n �.9�Gi?C
from a population of grid openinqs, and it is r?Qu�red to Cei? ^"�^�
[he mean grid ooenin5 fiber count for the pcpula*.ion on t��e bd5�5
of thi5 Samplinc. The interval about the samole Tean,'which, ��'.:r
95o confidence, :ontai�s the population mean, is a;so recuired.
The distribution of fibers on the qrid open�n�s should theoreti-
Cally approximate d Poisson distribution. 6eca��se o` fi�er
aggregation and s�ize-dependent Tdent�r'icatior, ef�ects, the fi�er
count �ata often do �ot conform to the Poisson distribution,
particularly at high fiber co�nts. Sim�;e assumotion of a P�issnn
distribution �ay therefer� lead to confidence inte��vais narr�wer
than are justified by the data. �oreover, if a Poisson
distribution is assumed, the variance is fixed in r�lation to �re
total number cf fibers counted. Thus a particular f�ber c^unt
conducted on one grid opening is considered to hava the sam�
confidence intzrval as that �or the sar.,e number of fibers f�urd cn
many qrid openings. Nowever, the area of sample actualiy c•.ur.:eC
is very smali in relation to the total area of the filt�r, and f�r
this reason fibers must be counted on a mininum of a orid coenino5
taken from different areas of the filter in order to ?ns�re
representative evaluation of the deposit.
At high fiber counts, where there are adeQuate numbers of fibers
per grid opening �o ailoW a saRpla 2stimate of the vari�nce to Ce
made, the distributio�� can be apRrax��ated to Gaussian, �Xi�h
independent values for the Tean and variarce. ��here the �a�ole
estimate of variance exceeds that implicit in the Poisscrian
as3umption, use of Gaussian stati5tics with the variance Cefine� b�
the actual data is the mo�t conservative approach to calc�lation �f
con.`idence in[ervals.
�t low fiber counts, it is not possible :o obtain a r�liable saTcie
estimate of the variance, and the di5tribution olso becoR�s
asyr,�metrfc, but not necessarity �oissonian. For 3C fibers and
below, the distribution becomes sufficiently rs��rrnaetric that the
G�3ussian fit is no lon�er a reasonable one� an0 sar.ple variar.ce
estimates are unreliable, accordingly, for fiber counrs be'ow ?:
fibers, the assumption of a QoisSon �is�ri5ution �us: Ce �a�� .`�r
ca:culation of the confiden^e intervals.
For total fiber counts less than 5, the lower 95: c�nfi�e�ce va�,�
�orresponds to one fiber or less, and in addi*ion� tne uo�eY ?��:
Confidence value corresaondino to a fi5er count of Zero is ?.��
fibers. Therefore, it is not me�ningful to auote lower C�nf:�cr��
intervat points for fiber ccunts of less than 5, an� the �esu�:
should be spetified as "less than" the CorroSoo�dtnq �o�sscn �ce�r
95'; confidence value. �
56
For fiber counts highe� than 30, the sample estimate of variarce is
a'so calculatee, and the lar�er of the two corfida_nce in�ervals is
seiected. for calculation �f N��sson 95'; conr"idence ;ntervals,
, Tabte 40 cr the reference by E.S. rE��rson and H,G. �artley should
be used, with an extension to an a.xpectation of 100. Fcr ^ore :han
100 fibers� the Poisson distrib�tion can be accurately approxi:�ate� ,
by a GausSian distribution, still using the F�isson varianc�
esL�mate. For counts of more than 30 fibers, the 95'� cenridence
interval based on a sanple estimate of variance is calculated usinc
the Student'S "t" distribution. For the two—sided Student's "t"
calculation, k values of grid opening fiber count are compared w�t:� -
the expected values for the areas of the grid openinos concerned.
In summary, fiber counting data �ill te reported as follows;
yo fibers detected
The value will be reported a� i�_s than 369�= of the
concentration eouivalent t� one fiber.
1 to 4 fibers
When 1 to 4 fibers are counted, the resulG will be re�erted
as less than the corresponding upper 95`� confidence limit
(P0155on).
5 to 30 fibers
,Nean and �So confidence intervals �ill be reported on the
ba5i5 of the Poisson assu�Gtion.
�ore than 30 fibers
when more than 30 fibers are count2�, both :he Gaussian 95`�
confidence interval �nd the Poisson 95�= co-fi�ence interva�
will be calculated. The larger of these 2 intervals :v;ll
be se)ected for data reporting, �hen tne Gaussian 95':
ConfidenCe interval is SeleCted fpr dat3 reporting� the
Poisson interval will also be noted.
Fiber counts performed on less than a or;o openin�s yielc very �;;e
95� confiaence intervais when �sino Gaussian s�aristics. This �s
be�ause �he value of Student's "t" is very large for 1 and :
degrees of freedcm, accordingly, fiber counts Tust not b� �ace rn
1e55 than 4 grid openings.
57
r
The samole estimate of variance S2 is first calculated:
i = k
� (n� - np�)�
SZ _ i = I
(k - 1)
where:
n� � N��mber of fibers on the i'th grid ooening
n = Total number of Fibers found in k grid oper,ings
p� = Fraction of the total area eza�ninec� re�resented by
the i'th grid opening
k � Number of grid openings
for the 95� confidence interval, the valuo of t0.975 is obtained
from tables for (k - 1) degrees of freedom. If the :nean value of
fiber count is calculated to he n, the uo�er and lower valu�s �f
the 95o confidence interval are given by:
where:
n � n+ts
� y �
n� = n '�k
n� . Upper 95': confidence limit
n� � lower 95; Confi�ence limit
n �'+1ean number of fiber, Ger grid ooening
s � S[andard deviation (square root of Sampl� esti�na:e
of varianCe)
k � Number e' grid ooeninqs
58
The fiber Concentration in MFL which corresponds to counting of one
fiber is giver� Dy:
where:
AfxRp
� �1 x V x 1000
Af = Ef�Qctive fittration dr�a of filter �nembr�ne in
mm used for filtration of livuid samole
A = Total �rea ex3mined in rrm2
v = Oriqinat volurre of sample filtered (mL1
Rp � Ditution ratio of oriqinat sample
The mean concentration i� MFL is obtained by multiolyino the mean
number of fibers �er orid ooenirg by kC, To ob�ain the upper and
lower 95.'.' confidence l�mits for the concentration �in .�IF�) mul�i�1�
the values n� and n� hy kC.
7.3 Estimated Mass Concentration
The mass ef each amphibole fiber in r�icrograms is ca�cutaied ��sina
the relationship; -
whe�e:
M- L x'v12 x 0 x 10�6
�� = Mass in microqrams
� � Length i n ::m
'� = W1dth in :m
� � Density of fiber in q/c�r3
59
0
For chrysotile, the mass may be calc:�lated us�r.g the relat�ensni�
for a cylinder:
M = 4xLxW2xDx 10"°
The estimated mass conc�ntration is then giver. b�:
where:
i = n
M� = C x� Mi x 106
i=1
M,. � Mass concentration in ;.g/L
C = fiber concentration in MFL, �.rhich corresponrs to
counting of one fiber
Mq = Mass of the i'th fiber, in micrograms
n = 7otal number of fibers found in k orid openings
The densities to be assumed are as follows:
Chrysotile 2.55 g/cm3
Crocida)ite 3.37 g/cm3
Cummingtonite 3.28 a/c�n3
Grunerite 3.52 g/cm3
Amosite 3,43 g/cm3
Anthoohyllite 3.00 g/cm3
Tremolite 3.00 g/c�n3
Attinolite 3.10 g/cm3
Unknown Amohibole 3.20 g/c�n3
1.4 Fiber �ength, Width, MaSs and Aspect Ratio Distributicns
The ��istributions all approximate to logar�thmic-normal, and so the
siz� range interva�s for calculation of the distribution must be
spaced logarithmicdlly. The other characteri:tics reauired for the
choice of size intervals are that they should al'ow `or a
sufficient number of size classes, while stili retaining a
statistically-valid number of fibers in each class. Interpre�atien
is also facititated if each size class repeats at decade
intervals. A ratio from one class to the next of 1.468 sztisfies
all �f these requirements. The other constraints are that the
length distribution should include 0.5 um as one intervat point�
since this is the minimum length to be cou�ted in the method, and
the rninimum aspect ratio is by definition ?.0, The resulting size
classes for the various distributions can be seen in the exam�le
shown in Appendix 6. The distributions, being approximately
logarithmic-normal, must be plotted using a logarithmic �r�ina�e
scale and a Gaussian abscissa.
7.4.1 Fiber Length Cumulative Number �istribution
This distrih!►tion allows the fraction of the total number
of fibers either ;horter or longer than a qiven lenvth to
be determined. It is calculated using the�relationship:
where:
i=k
� n�
�(N)k � = N X 100
� �i
i=1
�(Nj� = CuR�lat;ve nu�ber percentage of fibers
which have lengths less ttian the upper
bound of the k'th class
�
�
ni = PJumber of fibers in the i'th tength class'
. y
N = Total number of lPngth classes
bl
M
7.4.2 Fiber '�idth Cumulative Number Oistribution
This distri5ution allows the fracti�n of the tot�l number of
fibers either narrower or wider thdn a given width �o be
� determined. It is calculated in a;imilar way to `hat used
in 7.4.1 for the len5th di5tribution.
7.4.3 Fiber Lenath C��mulative ��ass Distribution
" This distribution allows the fraction of the total mass
incorporated in fibers either shorter or longer than a give�
length to be determine�. Tt is computed using the
relationship:
i =k j =n�
� � l�w� `
i = 1 .7 = 1
�(M�k i= N j=;�i x 100
� � l���z
i = 1 j = i
where:
C�M�k = Cumulative mass percentage of fib�rs which
have lengths less than the upper bound of
the k'th class
n� = Number of fibers in the i'th length class
1� = Length of the j'th fiber in the i'th
length clas�
w� _':Jidth of the j'th fiber in the i'th length
class
N = Total r�umber of length classes
7.4.4 Fiber Aspect Ratio Cumulative '�umber Distribution
This distribution aliows the fraction of the total nurber of
- fibers which have aspect ratio� either smaller or larger
than a given aspect ratio to be determined. lt is
62 � •
calculated in a similar way t� that used in 7,4.1 fcr �ha
tength distributian.
7.4.5 Fiber Mass Cumul�tive Number Dis�ribution
This distribution allo��s the fraction of the total number '
of fibers which have masses either smaller or laroer than a
given mass to be determined. 1t is calculated by placing
the f�bers into loqarithmically-spaced mass cateqories,
after which the cumulative frequency �istribution is
obta�ned in a similar way to that used in 7.4.1 for the "
length distribution.
7.5 Index of Fibrosity
It is possibte to discriminate between anphibole asbestos fiters
and amphibole cleavage fragments on the basis of the distribu�ion
of their aspect ratios. The concept of fibrosity in a miner�l
embodies a high median aspect ratio, together with a large �predd
of aspect ratios above the median value. A single number can be
used to describe the fibrosity of a mineral fiber dispersion, and
in many cases the value can be used to state if the mate,�ial i; or
is not asbestos. The fibrosity index can be defined thus:
F�R9
wher� R is the median ot the asoect ratio distribution and q is `he
geome�r�c standard d2viation of thz aspect rat�o distribution above
the median. The value of g is obtained from th�t portion of the
distribution lying between one and two georretric standard
deviations above the median. Meaninqful values of the index of
fibrosity can be obtained for most waterborne fi�er �isoersions if
jmore than 50 fibers h;ve.been measured.
The fibrosity index as def;ned above has values exceedina 100 for
waterbcrne dispersions of asbestos. Values below SC indicate a
distribution characteristiC of cleavage fragm�nts, or o�e from
which the hiqh aspect ratio fibers have been ;electively removed.
8. REPORTING
The computer progrjm provided in .appendix B satis`ies all of �he
reporting requirements for this anatytical metnod, �nd it is reccmrrended
that this format be used. The size classifications used must be the sar�e
as those in Appendix B.
63
.
V
8.1 Before tre fiber count data can be processed i� qive conCentr3ti0n
values, a d�cision must be �ade as to which fiber classifications
ar� to be considered adequate as identification of the fiber
species in question. This decis�on �ill de�end on how much is
known about the particular Source from �Nhich the sam�le was
collected.
For a sample from a completely uncharacterized soures, tne
fol�owing procedure will be used to accumulate the classified
fibers:
a} Confinned Amph�bole: AllQ t AZQ * All
(solutions must incl�de onl�
amphiboles)
b) Amphibole Sest Estimate*: AllQ + AZQ + All + aZ +
AoQ + aQ
c) Suspected Amphibole: ADX + AX + AO
d) Confirmed Chrysotile: coq * Cd
e) ChryscLile 3est �stimate*: CDQ + CO + C�tQ + CC
f) Suspected Chrysatile: CM
*NOTE: Best estimate can be reported only if some fibers are also
reported in the confirmed cateqory, oth?rwise all fiber
classifications must be reoorted as suspected amnhibole or
chr�sotile.
8.? The concentration in i�iFl, together with 95� confidence intervals,
wili be reported for the groupings in Section 8.1 (a) to (f).
8.3 Two significant fig�res �vill normally be used for cencentrations
greater than 1 MFL, and one significant figure for concentrations
less than 1 MFL.
8.4 For confirmation of chrysoti�e, a micrograph and a calibrated
diffraction pattern will be provided from a typical fiber. The
identification features in Figure l� must be visible on the
diffraction pattern.
For confirmation of amphibole, either (1) or (2) or (3) below �ust
_ be provided for a typical fiber of each amphibole variety
= reported. The data provided must yield solutions which irc,ude
only amphibole.
.
r
1) A micrograph, a calibrated zone axis SaEO pattern, and
an EDXA spectrum toge�her with po_ak area �neasurements
and EDXA calibration data;
64
2) a microqraph, and two calibrated zone axis Sa�C
patterns with a�easurement of the anQular r�ta'�on
between the two o�:[terns; �
3) A micronraph, twn ca ibra�e� zo�� axis S�c� Ddtt?rn5
with a �:easurement ot t��e anq��iar ro'���ticn het�NQ�n `he �
two patterns, and an ED"? spectr�;m tc�ether with ceak
area reasurements and EDX,� calibratio,� data.
8.5 Tabula`_e the length, wid�h ar,d aspect ratio distributions.
�
6.6 Report '.:he estimatrd mass conce�tration in �g/L for each of the
grouaings in Section 8.1 (a) to (f).
8.7 One significant figure will normally be used for report�ng mass
concentration.
8•8 Report the concentr3tion.in MFL co�resoonding to one fiber
detected.
8.9 Report the total number of fibers counted in eacn of the groupir.gs
in Section 8.1 (a) to (f;.
$.10 Report the X2 value for ea�h of the groupings in Section 8.t (al
to (f).
8.11 Report t��e nu��ber of fiber aggregates not included in the fiber
count
8.12 Report an� specia'. circumstances �:�r cbservations s�ch as
aggr�gation, presence of organic mat�rials, amount o; �ebris,
presence of othe; fibers and their probable ident;�y ;f known,
9. l I hI TAT IONS Of ACCURr1C Y
9.1 C;�rors and Limitations of Idertification
Complete identiPication of every chrysotile fiber is not possibie,
due to both instrumental limitations and the nature of some of the
fibers. The requiremen� for a calibrated SAED pattern eliminates
the possibility of an incorrect identification of the fiber
selected. However, there is a possibility of �nisidentification of
other chrysotiTe fibers for wh?ch both morphology and SAED pattern
are reported on the basis of visual insaection onl�. The cnly
significant possibilittes of misidentification occur with
halloysite, ve r,niculite scrolls or palygorskite, all of :vhich can
be discrimina�ed from chrysotile by the ;:se of �OXA and bv
observation of the 0.73 r,m (002) reflection of chr�so'_ile in the
SAED pattern.
as in the case of chrysotile fibers, cemplet� id2ntir;cstion or �
every amphibole fiber is not possible due to ins�r;,mental
65
�
limitations and the nature of some of the fiber5. ��oreover,
complet: identification of every amphibole f�ber is usually noL
practical due to limitat�ons of both time and cost. Particles of
`�A number of other minerals having camp�sitions similar to those of
some amphiboles could be erroneously classified as amphibole Nhen
the classification criteria do not include zone axis SAED
� techniques. However, the requirement for quantitative E�xa
measurements on all fiber; as Supoort for the random orientation
„. SAED technique makes misidentification very unlikely, particularl,✓
when other similar fibers in the same sample have been identified
as amphibole by zone axis methods. The possibility of
misidentification is further reduced �ith increasing aspect ratio,
since many of the minerals with which amphibole may be confused do
not display its prominent cleavage parailel ta the c-axis.
9.2 Obscuration
If large amounts of other materials 3re present, some asbestos
fibers may not be vbserved because of physical overlapping. This
will result in low values for the reported asbestos content.
9.3 Inadequate Dispersion
If the initiai water sample contains organic material which is
incompletely oxidized in the ozone-UV treatment, it wi11 not be
possible to disperse any fibers associated with the organic
material. This may lead to adhesion of some fibers to the
container walls and aliquots taken during fittration will then not
be representative. It may also lead to a larqe proportion of fiber
aggregates Nhich are either not tr�ansferred during the replication
and fi]ter dissolution step or which cannot be counted during the
sample examination. The result obtainEd from such an analysis �H.11
be low. The sample will also be inade4uately disoersed if it is
not treated in an ultrasonic bath prior tc filtration, and
therefore instructions regardiRg this treatment must be followed
closely.
9.4 Contamination
' Contamination by introduction of extraneous fibers during the
analysis is an important source of erroneous results� particularly
for chrysotile. The possibility of contamination, tharefore,
should always be a consideration.
9.5 freezing
7he effect of freezing on asbestos fibers is not known but ttiere is
reason to suspect that fiber breakdown could occur and result in a
higher fiber co�nt than was present in the oriQinal sample.
7herefore, the sample should be transported to the lshoratory and
stored under conditions that will avoid freezing.
�
10. PRECISIaN aND �CCURaCY
10.1 Generai
The precision that can be obtained is dependPnt upon �he nu�oer o.`
fibers courtted, and on the uniformit� of particulate deo�sit on the
original filter. If 100 f?bers are counted �nd the ioadina is at
least 3.5 fibers/grid square, c�mputer modeling of the countinq .
procedure shows that a relative standard deviatior, of about 1C�� can
be expected. As the number of fibers counted decreases, the
precision will also decrease approximately as �V where N is the
number of fibers counted. In actual practice, some degradation
from this precision will be observed. fhis degraCation is a
consequence of sample preparation errors, non-unifo mity of che
filtered par*icuiate depo�it, and fiber identificaticn variability
between operators and between instr�ments. the 95'a confidenc�
interval about the mean for a single fiber cnncer�tration
mea�urement using this analytical method should be about j25'; when
about 100 fibers are counted over 20 grid ooe��ngs. For these
conditions the precision of the cempu:ed mass concentration is
generally lower than the precision for the fiber number
concentration. The precision to be expected for a single
determination �f mass concentration is critically dependent on :he
fiber width distribution. For a result oased on �easurernent of a
minimum of about 100 fibers, the 95'� confidence interval about the
mean computed mass concentration may vary between ;25-; and =60`:.
If better precision is reauired for a mass dete rnination, the
alternative counting method described in S?ction 6.5.5 should ae
used.
10.2 Precision
10.2.1 Intra-Laboratory Ccmparison Using cnvironmental �ater
Sources
Tabie 6 shows the results obtained from analysis of 10
replicate samples from each of 8 water sampling locations.
rour of these locarions were associated with a source of
chrysotile and four associated with a source of amph�bole.
It can be seen that the relative standard deviations of the
number concentrations range between 13� and 22`�. The
corresponding relative standard deviations for �he mass
concentrations range bet�Neen 29`� and 69°�.
10.2.2 Inter-l.aboratory Comparison of Filters Pr�pared :�si�g
Standard Dispersions ard Environmental 'Nater Sources
Tabies 7 and 8 show the fiber c�unting result� ob�ained
«hen sectors of filters prepared in the ORF Labora�ory were
distributed to six laboratories considered experienced in
asbestos analy5i5 by the identification and countinq
techniques incorporated in this manual. The samples as
6�7
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can be seen that the r^lative standar� deviations for ?he
Six results on each of the stan�ard dispers;�n fi�te�s ��c
r.ot exceed 27a. In Table 8, the environmental ��ater "
sources useC to prepare the filter samples containee
similar types of suspended materials as those usec to
generate the intra-laborator� resul[5 �n Tab'e 6. i�e
re)ative standard deviations do not exce�d 29";, which
appears higher than the values obt3ined for the �
intra-laboracory res�lts. Nowever� when the 6
inter-laboratory results are compared �ith the 10
intra-laboratory vatues, there is no stat�sticall�
Sionificant difference to indiCate that there has 5e�n �n�
degradation of precision.
10.3 Accuracy
10.3.1 Intra- and Inter-Laboratory Ccmparison of Standard
Dispersions of Asbestos Fibers
Tables 9 and 10 shoM the results obtained betNeen two
taboratories when stable aqueous �iber disporsions of kncwn
mass Concentrations �ere anatyted. The fibo.r
conCentrations reported displayed no siqnifi�ant differance
between vaiues frcn the t�o iaboratories. The relativ�
standard deviation of the mean fiber concentr�tion was 17",
for chrysocile an� 16�: for crocidotite. The CorreS�G�Cing
relative Standdrd deviat�on5 `or the mas5 ConCentration
were 16�� for chrysotile, and 37�; for croc��o�ite. ;h�
highe� variability for crocidolitp �s a consecuence of the
lcw statistica� reliabit;ty of the �arqe diameter fi5er
counts. The computed mean mass conce�t�aticn for
chrysotile was about 46�� hi�her tha� ��e knpwn mass
concentration. This �ay be a consequence o` the d�ff�c�;*v
of diameter measurement for sinqle chrysotiie fi�rils �r �
the assumption of the bulk value for the �ensi�y. The
computed mean value for �ass concentra�ion far tne
crocidolite sample was 67.a �qIL, which is very cl�se to
the k�own concentration of 50 �gJl.
71
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76