[Code of Federal Regulations]
[Title 40, Volume 29]
[Revised as of July 1, 2004]
From the U.S. Government Printing Office via GPO Access
[CITE: 40CFR763.99]
[Page 752-821]
TITLE 40--PROTECTION OF ENVIRONMENT
CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)
PART 763_ASBESTOS--Table of Contents
Subpart E_Asbestos-Containing Materials in Schools
Sec. 763.99 Exclusions.
(a) A local education agency shall not be required to perform an
inspection under Sec. 763.85(a) in any sampling area as defined in 40
CFR 763.103 or homogeneous area of a school building where:
(1) An accredited inspector has determined that, based on sampling
records, friable ACBM was identified in that homogeneous or sampling
area during an inspection conducted before December 14, 1987. The
inspector shall sign and date a statement to that effect with his or her
State of accreditation and if applicable, accreditation number and,
within 30 days after such determination, submit a copy of the statement
to the person designated under Sec. 763.84 for inclusion in the
management plan. However, an accredited inspector shall assess the
friable ACBM under Sec. 763.88.
(2) An accredited inspector has determined that, based on sampling
records, nonfriable ACBM was identified in that homogeneous or sampling
area during an inspection conducted before December 14, 1987. The
inspector shall sign and date a statement to that effect with his or her
State of accreditation and if applicable, accreditation number and,
within 30 days after such determination, submit a copy of the statement
to the person designated under Sec. 763.84 for inclusion in the
management plan. However, an accredited inspector shall identify whether
material that was nonfriable has become friable since that previous
inspection and shall assess the newly-friable ACBM under Sec. 763.88.
(3) Based on sampling records and inspection records, an accredited
inspector has determined that no ACBM is present in the homogeneous or
sampling area and the records show that the area was sampled, before
December 14, 1987 in substantial compliance with
[[Page 753]]
Sec. 763.85(a), which for purposes of this section means in a random
manner and with a sufficient number of samples to reasonably ensure that
the area is not ACBM.
(i) The accredited inspector shall sign and date a statement, with
his or her State of accreditation and if applicable, accreditation
number that the homogeneous or sampling area determined not to be ACBM
was sampled in substantial compliance with Sec. 763.85(a).
(ii) Within 30 days after the inspector's determination, the local
education agency shall submit a copy of the inspector's statement to the
EPA Regional Office and shall include the statement in the management
plan for that school.
(4) The lead agency responsible for asbestos inspection in a State
that has been granted a waiver from Sec. 763.85(a) has determined that,
based on sampling records and inspection records, no ACBM is present in
the homogeneous or sampling area and the records show that the area was
sampled before December 14, 1987, in substantial compliance with Sec.
763.85(a). Such determination shall be included in the management plan
for that school.
(5) An accredited inspector has determined that, based on records of
an inspection conducted before December 14, 1987, suspected ACBM
identified in that homogeneous or sampling area is assumed to be ACM.
The inspector shall sign and date a statement to that effect, with his
or her State of accreditation and if applicable, accreditation number
and, within 30 days of such determination, submit a copy of the
statement to the person designated under Sec. 763.84 for inclusion in
the management plan. However, an accredited inspector shall identify
whether material that was nonfriable suspected ACBM assumed to be ACM
has become friable since the previous inspection and shall assess the
newly friable material and previously identified friable suspected ACBM
assumed to be ACM under Sec. 763.88.
(6) Based on inspection records and contractor and clearance
records, an accredited inspector has determined that no ACBM is present
in the homogeneous or sampling area where asbestos removal operations
have been conducted before December 14, 1987, and shall sign and date a
statement to that effect and include his or her State of accreditation
and, if applicable, accreditation number. The local education agency
shall submit a copy of the statement to the EPA Regional Office and
shall include the statement in the management plan for that school.
(7) An architect or project engineer responsible for the
construction of a new school building built after October 12, 1988, or
an accredited inspector signs a statement that no ACBM was specified as
a building material in any construction document for the building, or,
to the best of his or her knowledge, no ACBM was used as a building
material in the building. The local education agency shall submit a copy
of the signed statement of the architect, project engineer, or
accredited inspector to the EPA Regional Office and shall include the
statement in the management plan for that school.
(b) The exclusion, under paragraphs (a) (1) through (4) of this
section, from conducting the inspection under Sec. 763.85(a) shall
apply only to homogeneous or sampling areas of a school building that
were inspected and sampled before October 17, 1987. The local education
agency shall conduct an inspection under Sec. 763.85(a) of all areas
inspected before October 17, 1987, that were not sampled or were not
assumed to be ACM.
(c) If ACBM is subsequently found in a homogeneous or sampling area
of a local education agency that had been identified as receiving an
exclusion by an accredited inspector under paragraphs (a) (3), (4), (5)
of this section, or an architect, project engineer or accredited
inspector under paragraph (a)(7) of this section, the local education
agency shall have 180 days following the date of identification of ACBM
to comply with this subpart E.
[[Page 754]]
Appendix A to Subpart E of Part 763--Interim Transmission Electron
Microscopy Analytical Methods--Mandatory and Nonmandatory--and Mandatory
Section to Determine Completion of Response Actions
I. Introduction
The following appendix contains three units. The first unit is the
mandatory transmission electron microscopy (TEM) method which all
laboratories must follow; it is the minimum requirement for analysis of
air samples for asbestos by TEM. The mandatory method contains the
essential elements of the TEM method. The second unit contains the
complete non-mandatory method. The non-mandatory method supplements the
mandatory method by including additional steps to improve the analysis.
EPA recommends that the non-mandatory method be employed for analyzing
air filters; however, the laboratory may choose to employ the mandatory
method. The non-mandatory method contains the same minimum requirements
as are outlined in the mandatory method. Hence, laboratories may choose
either of the two methods for analyzing air samples by TEM.
The final unit of this Appendix A to subpart E defines the steps
which must be taken to determine completion of response actions. This
unit is mandatory.
II. Mandatory Transmission Electron Microscopy Method
A. Definitions of Terms
1. Analytical sensitivity--Airborne asbestos concentration
represented by each fiber counted under the electron microscope. It is
determined by the air volume collected and the proportion of the filter
examined. This method requires that the analytical sensitivity be no
greater than 0.005 structures/cm\3\.
2. Asbestiform--A specific type of mineral fibrosity in which the
fibers and fibrils possess high tensile strength and flexibility.
3. Aspect ratio--A ratio of the length to the width of a particle.
Minimum aspect ratio as defined by this method is equal to or greater
than 5:1.
4. Bundle--A structure composed of three or more fibers in a
parallel arrangement with each fiber closer than one fiber diameter.
5. Clean area--A controlled environment which is maintained and
monitored to assure a low probability of asbestos contamination to
materials in that space. Clean areas used in this method have HEPA
filtered air under positive pressure and are capable of sustained
operation with an open laboratory blank which on subsequent analysis has
an average of less than 18 structures/mm\2\ in an area of 0.057 mm\2\
(nominally 10 200-mesh grid openings) and a maximum of 53 structures/
mm\2\ for any single preparation for that same area.
6. Cluster--A structure with fibers in a random arrangement such
that all fibers are intermixed and no single fiber is isolated from the
group. Groupings must have more than two intersections.
7. ED--Electron diffraction.
8. EDXA--Energy dispersive X-ray analysis.
9. Fiber--A structure greater than or equal to 0.5 [mu]m in length
with an aspect ratio (length to width) of 5:1 or greater and having
substantially parallel sides.
10. Grid--An open structure for mounting on the sample to aid in its
examination in the TEM. The term is used here to denote a 200-mesh
copper lattice approximately 3 mm in diameter.
11. Intersection--Nonparallel touching or crossing of fibers, with
the projection having an aspect ratio of 5:1 or greater.
12. Laboratory sample coordinator--That person responsible for the
conduct of sample handling and the certification of the testing
procedures.
13. Filter background level--The concentration of structures per
square millimeter of filter that is considered indistinguishable from
the concentration measured on a blank (filters through which no air has
been drawn). For this method the filter background level is defined as
70 structures/mm\2\.
14. Matrix--Fiber or fibers with one end free and the other end
embedded in or hidden by a particulate. The exposed fiber must meet the
fiber definition.
15. NSD--No structure detected.
16. Operator--A person responsible for the TEM instrumental analysis
of the sample.
17. PCM--Phase contrast microscopy.
18. SAED--Selected area electron diffraction.
19. SEM--Scanning electron microscope.
20. STEM--Scanning transmission electron microscope.
21. Structure--a microscopic bundle, cluster, fiber, or matrix which
may contain asbestos.
22. S/cm\3\--Structures per cubic centimeter.
23. S/mm\2\--Structures per square millimeter.
24. TEM--Transmission electron microscope.
B. Sampling
1. The sampling agency must have written quality control procedures
and documents which verify compliance.
2. Sampling operations must be performed by qualified individuals
completely independent of the abatement contractor to avoid possible
conflict of interest (References 1, 2, 3, and 5 of Unit II.J.).
[[Page 755]]
3. Sampling for airborne asbestos following an abatement action must
use commercially available cassettes.
4. Prescreen the loaded cassette collection filters to assure that
they do not contain concentrations of asbestos which may interfere with
the analysis of the sample. A filter blank average of less than 18 s/
mm\2\ in an area of 0.057 mm\2\ (nominally 10 200-mesh grid openings)
and a single preparation with a maximum of 53 s/mm\2\ for that same area
is acceptable for this method.
5. Use sample collection filters which are either polycarbonate
having a pore size less than or equal to 0.4 [mu]m or mixed cellulose
ester having a pore size less than or equal to 0.45 [mu]m.
6. Place these filters in series with a 5.0 [mu]m backup filter (to
serve as a diffuser) and a support pad. See the following Figure 1:
[[Page 756]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.001
7. Reloading of used cassettes is not permitted.
8. Orient the cassette downward at approximately 45 degrees from the
horizontal.
9. Maintain a log of all pertinent sampling information.
[[Page 757]]
10. Calibrate sampling pumps and their flow indicators over the
range of their intended use with a recognized standard. Assemble the
sampling system with a representative filter (not the filter which will
be used in sampling) before and after the sampling operation.
11. Record all calibration information.
12. Ensure that the mechanical vibrations from the pump will be
minimized to prevent transferral of vibration to the cassette.
13. Ensure that a continuous smooth flow of negative pressure is
delivered by the pump by damping out any pump action fluctuations if
necessary.
14. The final plastic barrier around the abatement area remains in
place for the sampling period.
15. After the area has passed a thorough visual inspection, use
aggressive sampling conditions to dislodge any remaining dust. (See
suggested protocol in Unit III.B.7.d.)
16. Select an appropriate flow rate equal to or greater than 1 liter
per minute (L/min) or less than 10 L/min for 25 mm cassettes. Larger
filters may be operated at proportionally higher flow rates.
17. A minimum of 13 samples are to be collected for each testing
site consisting of the following:
a. A minimum of five samples per abatement area.
b. A minimum of five samples per ambient area positioned at
locations representative of the air entering the abatement site.
c. Two field blanks are to be taken by removing the cap for not more
than 30 seconds and replacing it at the time of sampling before sampling
is initiated at the following places:
i. Near the entrance to each abatement area.
ii. At one of the ambient sites. (DO NOT leave the field blanks open
during the sampling period.)
d. A sealed blank is to be carried with each sample set. This
representative cassette is not to be opened in the field.
18. Perform a leak check of the sampling system at each indoor and
outdoor sampling site by activating the pump with the closed sampling
cassette in line. Any flow indicates a leak which must be eliminated
before initiating the sampling operation.
19. The following Table I specifies volume ranges to be used:
[[Page 758]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.002
20. Ensure that the sampler is turned upright before interrupting
the pump flow.
21. Check that all samples are clearly labeled and that all
pertinent information has been enclosed before transfer of the samples
to the laboratory.
22. Ensure that the samples are stored in a secure and
representative location.
23. Do not change containers if portions of these filters are taken
for other purposes.
24. A summary of Sample Data Quality Objectives is shown in the
following Table II:
[[Page 759]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.003
C. Sample Shipment
Ship bulk samples to the analytical laboratory in a separate
container from air samples.
D. Sample Receiving
1. Designate one individual as sample coordinator at the laboratory.
While that individual will normally be available to receive samples, the
coordinator may train and supervise others in receiving procedures for
those times when he/she is not available.
2. Bulk samples and air samples delivered to the analytical
laboratory in the same container shall be rejected.
E. Sample Preparation
1. All sample preparation and analysis shall be performed by a
laboratory independent of the abatement contractor.
2. Wet-wipe the exterior of the cassettes to minimize contamination
possibilities before taking them into the clean room facility.
3. Perform sample preparation in a well-equipped clean facility.
Note: The clean area is required to have the following minimum
characteristics. The area or hood must be capable of maintaining a
positive pressure with make-up air being HEPA-filtered. The cumulative
analytical blank concentration must average less than 18 s/mm\2\ in an
area of 0.057 mm\2\ (nominally 10 200-mesh grid openings) and a single
preparation with a maximum of 53 s/mm\2\ for that same area.
4. Preparation areas for air samples must not only be separated from
preparation areas for bulk samples, but they must be prepared in
separate rooms.
5. Direct preparation techniques are required. The object is to
produce an intact film containing the particulates of the filter surface
which is sufficiently clear for TEM analysis.
a. TEM Grid Opening Area measurement must be done as follows:
i. The filter portion being used for sample preparation must have
the surface collapsed using an acetone vapor technique.
ii. Measure 20 grid openings on each of 20 random 200-mesh copper
grids by placing a grid on a glass and examining it under the PCM. Use a
calibrated graticule to measure the average field diameters. From the
data, calculate the field area for an average grid opening.
iii. Measurements can also be made on the TEM at a properly
calibrated low magnification or on an optical microscope at a
magnification of approximately 400X by using an eyepiece fitted with a
scale that has been calibrated against a stage micrometer. Optical
microscopy utilizing manual or automated procedures may be used
providing instrument calibration can be verified.
b. TEM specimen preparation from polycarbonate (PC) filters.
Procedures as described in Unit III.G. or other equivalent methods may
be used.
c. TEM specimen preparation from mixed cellulose ester (MCE)
filters.
i. Filter portion being used for sample preparation must have the
surface collapsed using an acetone vapor technique or the Burdette
procedure (Ref. 7 of Unit II.J.)
ii. Plasma etching of the collapsed filter is required. The
microscope slide to which the collapsed filter pieces are attached is
placed in a plasma asher. Because plasma ashers vary greatly in their
performance, both from unit to unit and between different positions in
the asher chamber, it is difficult to specify the conditions that should
be used. Insufficient etching will result in a failure to expose
embedded filters, and too much etching may result in loss of particulate
from the surface. As an interim measure, it is recommended that the time
for ashing of a
[[Page 760]]
known weight of a collapsed filter be established and that the etching
rate be calculated in terms of micrometers per second. The actual
etching time used for the particulate asher and operating conditions
will then be set such that a 1-2 [mu]m (10 percent) layer of collapsed
surface will be removed.
iii. Procedures as described in Unit III. or other equivalent
methods may be used to prepare samples.
F. TEM Method
1. An 80-120 kV TEM capable of performing electron diffraction with
a fluorescent screen inscribed with calibrated gradations is required.
If the TEM is equipped with EDXA it must either have a STEM attachment
or be capable of producing a spot less than 250 nm in diameter at
crossover. The microscope shall be calibrated routinely for
magnification and camera constant.
2. Determination of Camera Constant and ED Pattern Analysis. The
camera length of the TEM in ED operating mode must be calibrated before
ED patterns on unknown samples are observed. This can be achieved by
using a carbon-coated grid on which a thin film of gold has been
sputtered or evaporated. A thin film of gold is evaporated on the
specimen TEM grid to obtain zone-axis ED patterns superimposed with a
ring pattern from the polycrystalline gold film. In practice, it is
desirable to optimize the thickness of the gold film so that only one or
two sharp rings are obtained on the superimposed ED pattern. Thicker
gold film would normally give multiple gold rings, but it will tend to
mask weaker diffraction spots from the unknown fibrous particulate.
Since the unknown d-spacings of most interest in asbestos analysis are
those which lie closest to the transmitted beam, multiple gold rings are
unnecessary on zone-axis ED patterns. An average camera constant using
multiple gold rings can be determined. The camera constant is one-half
the diameter of the rings times the interplanar spacing of the ring
being measured.
3. Magnification Calibration. The magnification calibration must be
done at the fluorescent screen. The TEM must be calibrated at the grid
opening magnification (if used) and also at the magnification used for
fiber counting. This is performed with a cross grating replica (e.g.,
one containing 2,160 lines/mm). Define a field of view on the
fluorescent screen either by markings or physical boundaries. The field
of view must be measurable or previously inscribed with a scale or
concentric circles (all scales should be metric). A logbook must be
maintained, and the dates of calibration and the values obtained must be
recorded. The frequency of calibration depends on the past history of
the particular microscope. After any maintenance of the microscope that
involved adjustment of the power supplied to the lenses or the high-
voltage system or the mechanical disassembly of the electron optical
column apart from filament exchange, the magnification must be
recalibrated. Before the TEM calibration is performed, the analyst must
ensure that the cross grating replica is placed at the same distance
from the objective lens as the specimens are. For instruments that
incorporate a eucentric tilting specimen stage, all specimens and the
cross grating replica must be placed at the eucentric position.
4. While not required on every microscope in the laboratory, the
laboratory must have either one microscope equipped with energy
dispersive X-ray analysis or access to an equivalent system on a TEM in
another laboratory.
5. Microscope settings: 80-120 kV, grid assessment 250-1,000X, then
15,000-20,000X screen magnification for analysis.
6. Approximately one-half (0.5) of the predetermined sample area to
be analyzed shall be performed on one sample grid preparation and the
remaining half on a second sample grid preparation.
7. Individual grid openings with greater than 5 percent openings
(holes) or covered with greater than 25 percent particulate matter or
obviously having nonuniform loading must not be analyzed.
8. Reject the grid if:
a. Less than 50 percent of the grid openings covered by the replica
are intact.
b. The replica is doubled or folded.
c. The replica is too dark because of incomplete dissolution of the
filter.
9. Recording Rules.
a. Any continuous grouping of particles in which an asbestos fiber
with an aspect ratio greater than or equal to 5:1 and a length greater
than or equal to 0.5 [mu]m is detected shall be recorded on the count
sheet. These will be designated asbestos structures and will be
classified as fibers, bundles, clusters, or matrices. Record as
individual fibers any contiguous grouping having 0, 1, or 2 definable
intersections. Groupings having more than 2 intersections are to be
described as cluster or matrix. An intersection is a nonparallel
touching or crossing of fibers, with the projection having an aspect
ratio of 5:1 or greater. See the following Figure 2:
[[Page 761]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.004
[[Page 762]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.005
i. Fiber. A structure having a minimum length greater than or equal
to 0.5 [mu]m and an aspect ratio (length to width) of 5:1 or greater and
substantially parallel sides. Note the appearance of the end of the
fiber, i.e., whether it is flat, rounded or dovetailed.
ii. Bundle. A structure composed of three or more fibers in a
parallel arrangement with each fiber closer than one fiber diameter.
iii. Cluster. A structure with fibers in a random arrangement such
that all fibers are intermixed and no single fiber is isolated from the
group. Groupings must have more than two intersections.
iv. Matrix. Fiber or fibers with one end free and the other end
embedded in or hidden by a particulate. The exposed fiber must meet the
fiber definition.
b. Separate categories will be maintained for fibers less than 5
[mu]m and for fibers equal to or greater than 5 [mu]m in length.
c. Record NSD when no structures are detected in the field.
d. Visual identification of electron diffraction (ED) patterns is
required for each asbestos structure counted which would cause the
[[Page 763]]
analysis to exceed the 70 s/mm\2\ concentration. (Generally this means
the first four fibers identified as asbestos must exhibit an
identifiable diffraction pattern for chrysotile or amphibole.)
e. The micrograph number of the recorded diffraction patterns must
be reported to the client and maintained in the laboratory's quality
assurance records. In the event that examination of the pattern by a
qualified individual indicates that the pattern has been misidentified
visually, the client shall be contacted.
f. Energy Dispersive X-ray Analysis (EDXA) is required of all
amphiboles which would cause the analysis results to exceed the 70 s/
mm\2\ concentration. (Generally speaking, the first 4 amphiboles would
require EDXA.)
g. If the number of fibers in the nonasbestos class would cause the
analysis to exceed the 70 s/mm\2\ concentration, the fact that they are
not asbestos must be confirmed by EDXA or measurement of a zone axis
diffraction pattern.
h. Fibers classified as chrysotile must be identified by diffraction
or X-ray analysis and recorded on a count sheet. X-ray analysis alone
can be used only after 70 s/mm\2\ have been exceeded for a particular
sample.
i. Fibers classified as amphiboles must be identified by X-ray
analysis and electron diffraction and recorded on the count sheet. (X-
ray analysis alone can be used only after 70 s/mm\2\ have been exceeded
for a particular sample.)
j. If a diffraction pattern was recorded on film, record the
micrograph number on the count sheet.
k. If an electron diffraction was attempted but no pattern was
observed, record N on the count sheet.
l. If an EDXA spectrum was attempted but not observed, record N on
the count sheet.
m. If an X-ray analysis spectrum is stored, record the file and disk
number on the count sheet.
10. Classification Rules.
a. Fiber. A structure having a minimum length greater than or equal
to 0.5 [mu]m and an aspect ratio (length to width) of 5:1 or greater and
substantially parallel sides. Note the appearance of the end of the
fiber, i.e., whether it is flat, rounded or dovetailed.
b. Bundle. A structure composed of three or more fibers in a
parallel arrangement with each fiber closer than one fiber diameter.
c. Cluster. A structure with fibers in a random arrangement such
that all fibers are intermixed and no single fiber is isolated from the
group. Groupings must have more than two intersections.
d. Matrix. Fiber or fibers with one end free and the other end
embedded in or hidden by a particulate. The exposed fiber must meet the
fiber definition.
11. After finishing with a grid, remove it from the microscope, and
replace it in the appropriate grid holder. Sample grids must be stored
for a minimum of 1 year from the date of the analysis; the sample
cassette must be retained for a minimum of 30 days by the laboratory or
returned at the client's request.
G. Sample Analytical Sequence
1. Under the present sampling requirements a minimum of 13 samples
is to be collected for the clearance testing of an abatement site. These
include five abatement area samples, five ambient samples, two field
blanks, and one sealed blank.
2. Carry out visual inspection of work site prior to air monitoring.
3. Collect a minimum of 5 air samples inside the work site and 5
samples outside the work site. The indoor and outdoor samples shall be
taken during the same time period.
4. Remaining steps in the analytical sequence are contained in Unit
IV of this Appendix.
H. Reporting
1. The following information must be reported to the client for each
sample analyzed:
a. Concentration in structures per square millimeter and structures
per cubic centimeter.
b. Analytical sensitivity used for the analysis.
c. Number of asbestos structures.
d. Area analyzed.
e. Volume of air sampled (which must be initially supplied to lab by
client).
f. Copy of the count sheet must be included with the report.
g. Signature of laboratory official to indicate that the laboratory
met specifications of the method.
h. Report form must contain official laboratory identification
(e.g., letterhead).
i. Type of asbestos.
I. Quality Control/Quality Assurance Procedures (Data Quality
Indicators)
Monitoring the environment for airborne asbestos requires the use of
sensitive sampling and analysis procedures. Because the test is
sensitive, it may be influenced by a variety of factors. These include
the supplies used in the sampling operation, the performance of the
sampling, the preparation of the grid from the filter and the actual
examination of this grid in the microscope. Each of these unit
operations must produce a product of defined quality if the analytical
result is to be a reliable and meaningful test result. Accordingly, a
series of control checks and reference standards are to be performed
along with the sample analysis as indicators that the materials used are
adequate and the
[[Page 764]]
operations are within acceptable limits. In this way, the quality of the
data is defined and the results are of known value. These checks and
tests also provide timely and specific warning of any problems which
might develop within the sampling and analysis operations. A description
of these quality control/quality assurance procedures is summarized in
the following Table III:
[GRAPHIC] [TIFF OMITTED] TC01AP92.006
1. When the samples arrive at the laboratory, check the samples and
documentation for completeness and requirements before initiating the
analysis.
2. Check all laboratory reagents and supplies for acceptable
asbestos background levels.
3. Conduct all sample preparation in a clean room environment
monitored by laboratory blanks. Testing with blanks must also be done
after cleaning or servicing the room.
4. Prepare multiple grids of each sample.
[[Page 765]]
5. Provide laboratory blanks with each sample batch. Maintain a
cumulative average of these results. If there are more than 53 fibers/mm
\2\ per 10 200-mesh grid openings, the system must be checked for
possible sources of contamination.
6. Perform a system check on the transmission electron microscope
daily.
7. Make periodic performance checks of magnification, electron
diffraction and energy dispersive X-ray systems as set forth in Table
III under Unit II.I.
8. Ensure qualified operator performance by evaluation of replicate
analysis and standard sample comparisons as set forth in Table III under
Unit II.I.
9. Validate all data entries.
10. Recalculate a percentage of all computations and automatic data
reduction steps as specified in Table III under Unit II.I.
11. Record an electron diffraction pattern of one asbestos structure
from every five samples that contain asbestos. Verify the identification
of the pattern by measurement or comparison of the pattern with patterns
collected from standards under the same conditions. The records must
also demonstrate that the identification of the pattern has been
verified by a qualified individual and that the operator who made the
identification is maintaining at least an 80 percent correct visual
identification based on his measured patterns.
12. Appropriate logs or records must be maintained by the analytical
laboratory verifying that it is in compliance with the mandatory quality
assurance procedures.
J. References
For additional background information on this method, the following
references should be consulted.
1. ``Guidance for Controlling Asbestos-Containing Materials in
Buildings,'' EPA 560/5-85-024, June 1985.
2. ``Measuring Airborne Asbestos Following an Abatement Action,''
USEPA, Office of Pollution Prevention and Toxics, EPA 600/4-85-049,
1985.
3. Small, John and E. Steel. Asbestos Standards: Materials and
Analytical Methods. N.B.S. Special Publication 619, 1982.
4. Campbell, W.J., R.L. Blake, L.L. Brown, E.E. Cather, and J.J.
Sjoberg. Selected Silicate Minerals and Their Asbestiform Varieties.
Information Circular 8751, U.S. Bureau of Mines, 1977.
5. Quality Assurance Handbook for Air Pollution Measurement System.
Ambient Air Methods, EPA 600/4-77-027a, USEPA, Office of Research and
Development, 1977.
6. Method 2A: Direct Measurement of Gas Volume through Pipes and
Small Ducts. 40 CFR Part 60 Appendix A.
7. Burdette, G.J., Health & Safety Exec. Research & Lab. Services
Div., London, ``Proposed Analytical Method for Determination of Asbestos
in Air.''
8. Chatfield, E.J., Chatfield Tech. Cons., Ltd., Clark, T., PEI
Assoc., ``Standard Operating Procedure for Determination of Airborne
Asbestos Fibers by Transmission Electron Microscopy Using Polycarbonate
Membrane Filters,'' WERL SOP 87-1, March 5, 1987.
9. NIOSH Method 7402 for Asbestos Fibers, 12-11-86 Draft.
10. Yamate, G., Agarwall, S.C., Gibbons, R.D., IIT Research
Institute, ``Methodology for the Measurement of Airborne Asbestos by
Electron Microscopy,'' Draft report, USEPA Contract 68-02-3266, July
1984.
11. ``Guidance to the Preparation of Quality Assurance Project
Plans,'' USEPA, Office of Pollution Prevention and Toxics, 1984.
III. Nonmandatory Transmission Electron Microscopy Method
A. Definitions of Terms
1. Analytical sensitivity--Airborne asbestos concentration
represented by each fiber counted under the electron microscope. It is
determined by the air volume collected and the proportion of the filter
examined. This method requires that the analytical sensitivity be no
greater than 0.005 s/cm\3\.
2. Asbestiform--A specific type of mineral fibrosity in which the
fibers and fibrils possess high tensile strength and flexibility.
3. Aspect ratio--A ratio of the length to the width of a particle.
Minimum aspect ratio as defined by this method is equal to or greater
than 5:1.
4. Bundle--A structure composed of three or more fibers in a
parallel arrangement with each fiber closer than one fiber diameter.
5. Clean area--A controlled environment which is maintained and
monitored to assure a low probability of asbestos contamination to
materials in that space. Clean areas used in this method have HEPA
filtered air under positive pressure and are capable of sustained
operation with an open laboratory blank which on subsequent analysis has
an average of less than 18 structures/mm\2\ in an area of 0.057 mm\2\
(nominally 10 200 mesh grid openings) and a maximum of 53 structures/
mm\2\ for no more than one single preparation for that same area.
6. Cluster--A structure with fibers in a random arrangement such
that all fibers are intermixed and no single fiber is isolated from the
group. Groupings must have more than two intersections.
7. ED--Electron diffraction.
8. EDXA--Energy dispersive X-ray analysis.
9. Fiber--A structure greater than or equal to 0.5 [mu]m in length
with an aspect ratio (length to width) of 5:1 or greater and having
substantially parallel sides.
[[Page 766]]
10. Grid--An open structure for mounting on the sample to aid in its
examination in the TEM. The term is used here to denote a 200-mesh
copper lattice approximately 3 mm in diameter.
11. Intersection--Nonparallel touching or crossing of fibers, with
the projection having an aspect ratio of 5:1 or greater.
12. Laboratory sample coordinator--That person responsible for the
conduct of sample handling and the certification of the testing
procedures.
13. Filter background level--The concentration of structures per
square millimeter of filter that is considered indistinguishable from
the concentration measured on blanks (filters through which no air has
been drawn). For this method the filter background level is defined as
70 structures/mm\2\.
14. Matrix--Fiber or fibers with one end free and the other end
embedded in or hidden by a particulate. The exposed fiber must meet the
fiber definition.
15. NSD--No structure detected.
16. Operator--A person responsible for the TEM instrumental analysis
of the sample.
17. PCM--Phase contrast microscopy.
18. SAED--Selected area electron diffraction.
19. SEM--Scanning electron microscope.
20. STEM--Scanning transmission electron microscope.
21. Structure--a microscopic bundle, cluster, fiber, or matrix which
may contain asbestos.
22. S/cm\3\--Structures per cubic centimeter.
23. S/mm\2\--Structures per square millimeter.
24. TEM--Transmission electron microscope.
B. Sampling
1. Sampling operations must be performed by qualified individuals
completely independent of the abatement contractor to avoid possible
conflict of interest (See References 1, 2, and 5 of Unit III.L.) Special
precautions should be taken to avoid contamination of the sample. For
example, materials that have not been prescreened for their asbestos
background content should not be used; also, sample handling procedures
which do not take cross contamination possibilities into account should
not be used.
2. Material and supply checks for asbestos contamination should be
made on all critical supplies, reagents, and procedures before their use
in a monitoring study.
3. Quality control and quality assurance steps are needed to
identify problem areas and isolate the cause of the contamination (see
Reference 5 of Unit III.L.). Control checks shall be permanently
recorded to document the quality of the information produced. The
sampling firm must have written quality control procedures and documents
which verify compliance. Independent audits by a qualified consultant or
firm should be performed once a year. All documentation of compliance
should be retained indefinitely to provide a guarantee of quality. A
summary of Sample Data Quality Objectives is shown in Table II of Unit
II.B.
4. Sampling materials.
a. Sample for airborne asbestos following an abatement action using
commercially available cassettes.
b. Use either a cowling or a filter-retaining middle piece.
Conductive material may reduce the potential for particulates to adhere
to the walls of the cowl.
c. Cassettes must be verified as ``clean'' prior to use in the
field. If packaged filters are used for loading or preloaded cassettes
are purchased from the manufacturer or a distributor, the manufacturer's
name and lot number should be entered on all field data sheets provided
to the laboratory, and are required to be listed on all reports from the
laboratory.
d. Assemble the cassettes in a clean facility (See definition of
clean area under Unit III.A.).
e. Reloading of used cassettes is not permitted.
f. Use sample collection filters which are either polycarbonate
having a pore size of less than or equal to 0.4 [mu]m or mixed cellulose
ester having a pore size of less than or equal to 0.45 [mu]m.
g. Place these filters in series with a backup filter with a pore
size of 5.0 [mu]m (to serve as a diffuser) and a support pad. See the
following Figure 1:
[[Page 767]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.007
h. When polycarbonate filters are used, position the highly
reflective face such that the incoming particulate is received on this
surface.
i. Seal the cassettes to prevent leakage around the filter edges or
between cassette part joints. A mechanical press may be useful to
achieve a reproducible leak-free seal.
[[Page 768]]
Shrink fit gel-bands may be used for this purpose and are available from
filter manufacturers and their authorized distributors.
j. Use wrinkle-free loaded cassettes in the sampling operation.
5. Pump setup.
a. Calibrate the sampling pump over the range of flow rates and
loads anticipated for the monitoring period with this flow measuring
device in series. Perform this calibration using guidance from EPA
Method 2A each time the unit is sent to the field (See Reference 6 of
Unit III.L.).
b. Configure the sampling system to preclude pump vibrations from
being transmitted to the cassette by using a sampling stand separate
from the pump station and making connections with flexible tubing.
c. Maintain continuous smooth flow conditions by damping out any
pump action fluctuations if necessary.
d. Check the sampling system for leaks with the end cap still in
place and the pump operating before initiating sample collection. Trace
and stop the source of any flow indicated by the flowmeter under these
conditions.
e. Select an appropriate flow rate equal to or greater than 1 L/min
or less than 10 L/min for 25 mm cassettes. Larger filters may be
operated at proportionally higher flow rates.
f. Orient the cassette downward at approximately 45 degrees from the
horizontal.
g. Maintain a log of all pertinent sampling information, such as
pump identification number, calibration data, sample location, date,
sample identification number, flow rates at the beginning, middle, and
end, start and stop times, and other useful information or comments. Use
of a sampling log form is recommended. See the following Figure 2:
[[Page 769]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.008
h. Initiate a chain of custody procedure at the start of each
sampling, if this is requested by the client.
i. Maintain a close check of all aspects of the sampling operation
on a regular basis.
j. Continue sampling until at least the minimum volume is collected,
as specified in the following Table I:
[[Page 770]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.009
k. At the conclusion of sampling, turn the cassette upward before
stopping the flow to minimize possible particle loss. If the sampling is
resumed, restart the flow before reorienting the cassette downward. Note
the condition of the filter at the conclusion of sampling.
l. Double check to see that all information has been recorded on the
data collection forms and that the cassette is securely closed and
appropriately identified using a waterproof label. Protect cassettes in
individual clean resealed polyethylene bags. Bags are to be used for
storing cassette caps when they are removed for sampling purposes. Caps
and plugs should only be removed or replaced using clean hands or clean
disposable plastic gloves.
m. Do not change containers if portions of these filters are taken
for other purposes.
[[Page 771]]
6. Minimum sample number per site. A minimum of 13 samples are to be
collected for each testing consisting of the following:
a. A minimum of five samples per abatement area.
b. A minimum of five samples per ambient area positioned at
locations representative of the air entering the abatement site.
c. Two field blanks are to be taken by removing the cap for not more
than 30 sec and replacing it at the time of sampling before sampling is
initiated at the following places:
i. Near the entrance to each ambient area.
ii. At one of the ambient sites.
(Note: Do not leave the blank open during the sampling period.)
d. A sealed blank is to be carried with each sample set. This
representative cassette is not to be opened in the field.
7. Abatement area sampling.
a. Conduct final clearance sampling only after the primary
containment barriers have been removed; the abatement area has been
thoroughly dried; and, it has passed visual inspection tests by
qualified personnel. (See Reference 1 of Unit III.L.)
b. Containment barriers over windows, doors, and air passageways
must remain in place until the TEM clearance sampling and analysis is
completed and results meet clearance test criteria. The final plastic
barrier remains in place for the sampling period.
c. Select sampling sites in the abatement area on a random basis to
provide unbiased and representative samples.
d. After the area has passed a thorough visual inspection, use
aggressive sampling conditions to dislodge any remaining dust.
i. Equipment used in aggressive sampling such as a leaf blower and/
or fan should be properly cleaned and decontaminated before use.
ii. Air filtration units shall remain on during the air monitoring
period.
iii. Prior to air monitoring, floors, ceiling and walls shall be
swept with the exhaust of a minimum one (1) horsepower leaf blower.
iv. Stationary fans are placed in locations which will not interfere
with air monitoring equipment. Fan air is directed toward the ceiling.
One fan shall be used for each 10,000 ft \3\ of worksite.
v. Monitoring of an abatement work area with high-volume pumps and
the use of circulating fans will require electrical power. Electrical
outlets in the abatement area may be used if available. If no such
outlets are available, the equipment must be supplied with electricity
by the use of extension cords and strip plug units. All electrical power
supply equipment of this type must be approved Underwriter Laboratory
equipment that has not been modified. All wiring must be grounded.
Ground fault interrupters should be used. Extreme care must be taken to
clean up any residual water and ensure that electrical equipment does
not become wet while operational.
vi. Low volume pumps may be carefully wrapped in 6-mil polyethylene
to insulate the pump from the air. High volume pumps cannot be sealed in
this manner since the heat of the motor may melt the plastic. The pump
exhausts should be kept free.
vii. If recleaning is necessary, removal of this equipment from the
work area must be handled with care. It is not possible to completely
decontaminate the pump motor and parts since these areas cannot be
wetted. To minimize any problems in this area, all equipment such as
fans and pumps should be carefully wet wiped prior to removal from the
abatement area. Wrapping and sealing low volume pumps in 6-mil
polyethylene will provide easier decontamination of this equipment. Use
of clean water and disposable wipes should be available for this
purpose.
e. Pump flow rate equal to or greater than 1 L/min or less than 10
L/min may be used for 25 mm cassettes. The larger cassette diameters may
have comparably increased flow.
f. Sample a volume of air sufficient to ensure the minimum
quantitation limits. (See Table I of Unit III.B.5.j.)
8. Ambient sampling.
a. Position ambient samplers at locations representative of the air
entering the abatement site. If makeup air entering the abatement site
is drawn from another area of the building which is outside of the
abatement area, place the pumps in the building, pumps should be placed
out of doors located near the building and away from any obstructions
that may influence wind patterns. If construction is in progress
immediately outside the enclosure, it may be necessary to select another
ambient site. Samples should be representative of any air entering the
work site.
b. Locate the ambient samplers at least 3 ft apart and protect them
from adverse weather conditions.
c. Sample same volume of air as samples taken inside the abatement
site.
C. Sample Shipment
1. Ship bulk samples in a separate container from air samples. Bulk
samples and air samples delivered to the analytical laboratory in the
same container shall be rejected.
2. Select a rigid shipping container and pack the cassettes upright
in a noncontaminating nonfibrous medium such as a bubble pack. The use
of resealable polyethylene bags may help to prevent jostling of
individual cassettes.
3. Avoid using expanded polystyrene because of its static charge
potential. Also avoid using particle-based packaging materials because
of possible contamination.
4. Include a shipping bill and a detailed listing of samples
shipped, their descriptions
[[Page 772]]
and all identifying numbers or marks, sampling data, shipper's name, and
contact information. For each sample set, designate which are the
ambient samples, which are the abatement area samples, which are the
field blanks, and which is the sealed blank if sequential analysis is to
be performed.
5. Hand-carry samples to the laboratory in an upright position if
possible; otherwise choose that mode of transportation least likely to
jar the samples in transit.
6. Address the package to the laboratory sample coordinator by name
when known and alert him or her of the package description, shipment
mode, and anticipated arrival as part of the chain of custody and sample
tracking procedures. This will also help the laboratory schedule timely
analysis for the samples when they are received.
D. Quality Control/Quality Assurance Procedures (Data Quality
Indicators)
Monitoring the environment for airborne asbestos requires the use of
sensitive sampling and analysis procedures. Because the test is
sensitive, it may be influenced by a variety of factors. These include
the supplies used in the sampling operation, the performance of the
sampling, the preparation of the grid from the filter and the actual
examination of this grid in the microscope. Each of these unit
operations must produce a product of defined quality if the analytical
result is to be a reliable and meaningful test result. Accordingly, a
series of control checks and reference standards is performed along with
the sample analysis as indicators that the materials used are adequate
and the operations are within acceptable limits. In this way, the
quality of the data is defined, and the results are of known value.
These checks and tests also provide timely and specific warning of any
problems which might develop within the sampling and analysis
operations. A description of these quality control/quality assurance
procedures is summarized in the text below.
1. Prescreen the loaded cassette collection filters to assure that
they do not contain concentrations of asbestos which may interfere with
the analysis of the sample. A filter blank average of less than 18 s/
mm\2\ in an area of 0.057 mm\2\ (nominally 10 200-mesh grid openings)
and a maximum of 53 s/mm\2\ for that same area for any single
preparation is acceptable for this method.
2. Calibrate sampling pumps and their flow indicators over the range
of their intended use with a recognized standard. Assemble the sampling
system with a representative filter--not the filter which will be used
in sampling--before and after the sampling operation.
3. Record all calibration information with the data to be used on a
standard sampling form.
4. Ensure that the samples are stored in a secure and representative
location.
5. Ensure that mechanical calibrations from the pump will be
minimized to prevent transferral of vibration to the cassette.
6. Ensure that a continuous smooth flow of negative pressure is
delivered by the pump by installing a damping chamber if necessary.
7. Open a loaded cassette momentarily at one of the indoor sampling
sites when sampling is initiated. This sample will serve as an indoor
field blank.
8. Open a loaded cassette momentarily at one of the outdoor sampling
sites when sampling is initiated. This sample will serve as an outdoor
field blank.
9. Carry a sealed blank into the field with each sample series. Do
not open this cassette in the field.
10. Perform a leak check of the sampling system at each indoor and
outdoor sampling site by activating the pump with the closed sampling
cassette in line. Any flow indicates a leak which must be eliminated
before initiating the sampling operation.
11. Ensure that the sampler is turned upright before interrupting
the pump flow.
12. Check that all samples are clearly labeled and that all
pertinent information has been enclosed before transfer of the samples
to the laboratory.
E. Sample Receiving
1. Designate one individual as sample coordinator at the laboratory.
While that individual will normally be available to receive samples, the
coordinator may train and supervise others in receiving procedures for
those times when he/she is not available.
2. Adhere to the following procedures to ensure both the continued
chain-of-custody and the accountability of all samples passing through
the laboratory:
a. Note the condition of the shipping package and data written on it
upon receipt.
b. Retain all bills of lading or shipping slips to document the
shipper and delivery time.
c. Examine the chain-of-custody seal, if any, and the package for
its integrity.
d. If there has been a break in the seal or substantive damage to
the package, the sample coordinator shall immediately notify the shipper
and a responsible laboratory manager before any action is taken to
unpack the shipment.
e. Packages with significant damage shall be accepted only by the
responsible laboratory manager after discussions with the client.
3. Unwrap the shipment in a clean, uncluttered facility. The sample
coordinator or his or her designee will record the contents, including a
description of each item and all identifying numbers or marks. A
[[Page 773]]
Sample Receiving Form to document this information is attached for use
when necessary. (See the following Figure 3.)
[GRAPHIC] [TIFF OMITTED] TC01AP92.010
[[Page 774]]
Note: The person breaking the chain-of-custody seal and itemizing
the contents assumes responsibility for the shipment and signs documents
accordingly.
4. Assign a laboratory number and schedule an analysis sequence.
5. Manage all chain-of-custody samples within the laboratory such
that their integrity can be ensured and documented.
F. Sample Preparation
1. Personnel not affiliated with the Abatement Contractor shall be
used to prepare samples and conduct TEM analysis. Wet-wipe the exterior
of the cassettes to minimize contamination possibilities before taking
them to the clean sample preparation facility.
2. Perform sample preparation in a well-equipped clean facility.
Note: The clean area is required to have the following minimum
characteristics. The area or hood must be capable of maintaining a
positive pressure with make-up air being HEPA filtered. The cumulative
analytical blank concentration must average less than 18 s/mm\2\ in an
area of 0.057 s/mm\2\ (nominally 10 200-mesh grid openings) with no more
than one single preparation to exceed 53 s/mm\2\ for that same area.
3. Preparation areas for air samples must be separated from
preparation areas for bulk samples. Personnel must not prepare air
samples if they have previously been preparing bulk samples without
performing appropriate personal hygiene procedures, i.e., clothing
change, showering, etc.
4. Preparation. Direct preparation techniques are required. The
objective is to produce an intact carbon film containing the
particulates from the filter surface which is sufficiently clear for TEM
analysis. Currently recommended direct preparation procedures for
polycarbonate (PC) and mixed cellulose ester (MCE) filters are described
in Unit III.F.7. and 8. Sample preparation is a subject requiring
additional research. Variation on those steps which do not substantively
change the procedure, which improve filter clearing or which reduce
contamination problems in a laboratory are permitted.
a. Use only TEM grids that have had grid opening areas measured
according to directions in Unit III.J.
b. Remove the inlet and outlet plugs prior to opening the cassette
to minimize any pressure differential that may be present.
c. Examples of techniques used to prepare polycarbonate filters are
described in Unit III.F.7.
d. Examples of techniques used to prepare mixed cellulose ester
filters are described in Unit III.F.8.
e. Prepare multiple grids for each sample.
f. Store the three grids to be measured in appropriately labeled
grid holders or polyethylene capsules.
5. Equipment.
a. Clean area.
b. Tweezers. Fine-point tweezers for handling of filters and TEM
grids.
c. Scalpel Holder and Curved No. 10 Surgical Blades.
d. Microscope slides.
e. Double-coated adhesive tape.
f. Gummed page reinforcements.
g. Micro-pipet with disposal tips 10 to 100 [mu]L variable volume.
h. Vacuum coating unit with facilities for evaporation of carbon.
Use of a liquid nitrogen cold trap above the diffusion pump will
minimize the possibility of contamination of the filter surface by oil
from the pumping system. The vacuum-coating unit can also be used for
deposition of a thin film of gold.
i. Carbon rod electrodes. Spectrochemically pure carbon rods are
required for use in the vacuum evaporator for carbon coating of filters.
j. Carbon rod sharpener. This is used to sharpen carbon rods to a
neck. The use of necked carbon rods (or equivalent) allows the carbon to
be applied to the filters with a minimum of heating.
k. Low-temperature plasma asher. This is used to etch the surface of
collapsed mixed cellulose ester (MCE) filters. The asher should be
supplied with oxygen, and should be modified as necessary to provide a
throttle or bleed valve to control the speed of the vacuum to minimize
disturbance of the filter. Some early models of ashers admit air too
rapidly, which may disturb particulates on the surface of the filter
during the etching step.
l. Glass petri dishes, 10 cm in diameter, 1 cm high. For prevention
of excessive evaporation of solvent when these are in use, a good seal
must be provided between the base and the lid. The seal can be improved
by grinding the base and lid together with an abrasive grinding
material.
m. Stainless steel mesh.
n. Lens tissue.
o. Copper 200-mesh TEM grids, 3 mm in diameter, or equivalent.
p. Gold 200-mesh TEM grids, 3 mm in diameter, or equivalent.
q. Condensation washer.
r. Carbon-coated, 200-mesh TEM grids, or equivalent.
s. Analytical balance, 0.1 mg sensitivity.
t. Filter paper, 9 cm in diameter.
u. Oven or slide warmer. Must be capable of maintaining a
temperature of 65-70 [deg]C.
v. Polyurethane foam, 6 mm thickness.
w. Gold wire for evaporation.
6. Reagents.
a. General. A supply of ultra-clean, fiber-free water must be
available for washing of all components used in the analysis. Water
[[Page 775]]
that has been distilled in glass or filtered or deionized water is
satisfactory for this purpose. Reagents must be fiber-free.
b. Polycarbonate preparation method--chloroform.
c. Mixed Cellulose Ester (MCE) preparation method--acetone or the
Burdette procedure (Ref. 7 of Unit III.L.).
7. TEM specimen preparation from polycarbonate filters.
a. Specimen preparation laboratory. It is most important to ensure
that contamination of TEM specimens by extraneous asbestos fibers is
minimized during preparation.
b. Cleaning of sample cassettes. Upon receipt at the analytical
laboratory and before they are taken into the clean facility or laminar
flow hood, the sample cassettes must be cleaned of any contamination
adhering to the outside surfaces.
c. Preparation of the carbon evaporator. If the polycarbonate filter
has already been carbon-coated prior to receipt, the carbon coating step
will be omitted, unless the analyst believes the carbon film is too
thin. If there is a need to apply more carbon, the filter will be
treated in the same way as an uncoated filter. Carbon coating must be
performed with a high-vacuum coating unit. Units that are based on
evaporation of carbon filaments in a vacuum generated only by an oil
rotary pump have not been evaluated for this application, and must not
be used. The carbon rods should be sharpened by a carbon rod sharpener
to necks of about 4 mm long and 1 mm in diameter. The rods are installed
in the evaporator in such a manner that the points are approximately 10
to 12 cm from the surface of a microscope slide held in the rotating and
tilting device.
d. Selection of filter area for carbon coating. Before preparation
of the filters, a 75 mmx50 mm microscope slide is washed and dried. This
slide is used to support strips of filter during the carbon evaporation.
Two parallel strips of double-sided adhesive tape are applied along the
length of the slide. Polycarbonate filters are easily stretched during
handling, and cutting of areas for further preparation must be performed
with great care. The filter and the MCE backing filter are removed
together from the cassette and placed on a cleaned glass microscope
slide. The filter can be cut with a curved scalpel blade by rocking the
blade from the point placed in contact with the filter. The process can
be repeated to cut a strip approximately 3 mm wide across the diameter
of the filter. The strip of polycarbonate filter is separated from the
corresponding strip of backing filter and carefully placed so that it
bridges the gap between the adhesive tape strips on the microscope
slide. The filter strip can be held with fine-point tweezers and
supported underneath by the scalpel blade during placement on the
microscope slide. The analyst can place several such strips on the same
microscope slide, taking care to rinse and wet-wipe the scalpel blade
and tweezers before handling a new sample. The filter strips should be
identified by etching the glass slide or marking the slide using a
marker insoluble in water and solvents. After the filter strip has been
cut from each filter, the residual parts of the filter must be returned
to the cassette and held in position by reassembly of the cassette. The
cassette will then be archived for a period of 30 days or returned to
the client upon request.
e. Carbon coating of filter strips. The glass slide holding the
filter strips is placed on the rotation-tilting device, and the
evaporator chamber is evacuated. The evaporation must be performed in
very short bursts, separated by some seconds to allow the electrodes to
cool. If evaporation is too rapid, the strips of polycarbonate filter
will begin to curl, which will lead to cross-linking of the surface
material and make it relatively insoluble in chloroform. An experienced
analyst can judge the thickness of carbon film to be applied, and some
test should be made first on unused filters. If the film is too thin,
large particles will be lost from the TEM specimen, and there will be
few complete and undamaged grid openings on the specimen. If the coating
is too thick, the filter will tend to curl when exposed to chloroform
vapor and the carbon film may not adhere to the support mesh. Too thick
a carbon film will also lead to a TEM image that is lacking in contrast,
and the ability to obtain ED patterns will be compromised. The carbon
film should be as thin as possible and remain intact on most of the grid
openings of the TEM specimen intact.
f. Preparation of the Jaffe washer. The precise design of the Jaffe
washer is not considered important, so any one of the published designs
may be used. A washer consisting of a simple stainless steel bridge is
recommended. Several pieces of lens tissue approximately 1.0 cmx0.5 cm
are placed on the stainless steel bridge, and the washer is filled with
chloroform to a level where the meniscus contacts the underside of the
mesh, which results in saturation of the lens tissue. See References 8
and 10 of Unit III.L.
g. Placing of specimens into the Jaffe washer. The TEM grids are
first placed on a piece of lens tissue so that individual grids can be
picked up with tweezers. Using a curved scalpel blade, the analyst
excises three 3 mm square pieces of the carbon-coated polycarbonate
filter from the filter strip. The three squares are selected from the
center of the strip and from two points between the outer periphery of
the active surface and the center. The piece of filter is placed on a
TEM specimen grid with the shiny side of the TEM grid facing upwards,
and the whole assembly is placed boldly onto the saturated lens tissue
in the Jaffe washer. If carbon-coated grids are used, the filter should
be
[[Page 776]]
placed carbon-coated side down. The three excised squares of filters are
placed on the same piece of lens tissue. Any number of separate pieces
of lens tissue may be placed in the same Jaffe washer. The lid is then
placed on the Jaffe washer, and the system is allowed to stand for
several hours, preferably overnight.
h. Condensation washing. It has been found that many polycarbonate
filters will not dissolve completely in the Jaffe washer, even after
being exposed to chloroform for as long as 3 days. This problem becomes
more serious if the surface of the filter was overheated during the
carbon evaporation. The presence of undissolved filter medium on the TEM
preparation leads to partial or complete obscuration of areas of the
sample, and fibers that may be present in these areas of the specimen
will be overlooked; this will lead to a low result. Undissolved filter
medium also compromises the ability to obtain ED patterns. Before they
are counted, TEM grids must be examined critically to determine whether
they are adequately cleared of residual filter medium. It has been found
that condensation washing of the grids after the initial Jaffe washer
treatment, with chloroform as the solvent, clears all residual filter
medium in a period of approximately 1 hour. In practice, the piece of
lens tissue supporting the specimen grids is transferred to the cold
finger of the condensation washer, and the washer is operated for about
1 hour. If the specimens are cleared satisfactorily by the Jaffe washer
alone, the condensation washer step may be unnecessary.
8. TEM specimen preparation from MCE filters.
a. This method of preparing TEM specimens from MCE filters is
similar to that specified in NIOSH Method 7402. See References 7, 8, and
9 of Unit III.L.
b. Upon receipt at the analytical laboratory, the sample cassettes
must be cleaned of any contamination adhering to the outside surfaces
before entering the clean sample preparation area.
c. Remove a section from any quadrant of the sample and blank
filters.
d. Place the section on a clean microscope slide. Affix the filter
section to the slide with a gummed paged reinforcement or other suitable
means. Label the slide with a water and solvent-proof marking pen.
e. Place the slide in a petri dish which contains several paper
filters soaked with 2 to 3 mL acetone. Cover the dish. Wait 2 to 4
minutes for the sample filter to fuse and clear.
f. Plasma etching of the collapsed filter is required.
i. The microscope slide to which the collapsed filter pieces are
attached is placed in a plasma asher. Because plasma ashers vary greatly
in their performance, both from unit to unit and between different
positions in the asher chamber, it is difficult to specify the
conditions that should be used. This is one area of the method that
requires further evaluation. Insufficient etching will result in a
failure to expose embedded filters, and too much etching may result in
loss of particulate from the surface. As an interim measure, it is
recommended that the time for ashing of a known weight of a collapsed
filter be established and that the etching rate be calculated in terms
of micrometers per second. The actual etching time used for a particular
asher and operating conditions will then be set such that a 1-2 [mu]m
(10 percent) layer of collapsed surface will be removed.
ii. Place the slide containing the collapsed filters into a low-
temperature plasma asher, and etch the filter.
g. Transfer the slide to a rotating stage inside the bell jar of a
vacuum evaporator. Evaporate a 1 mmx5 mm section of graphite rod onto
the cleared filter. Remove the slide to a clean, dry, covered petri
dish.
h. Prepare a second petri dish as a Jaffe washer with the wicking
substrate prepared from filter or lens paper placed on top of a 6 mm
thick disk of clean spongy polyurethane foam. Cut a V-notch on the edge
of the foam and filter paper. Use the V-notch as a reservoir for adding
solvent. The wicking substrate should be thin enough to fit into the
petri dish without touching the lid.
i. Place carbon-coated TEM grids face up on the filter or lens
paper. Label the grids by marking with a pencil on the filter paper or
by putting registration marks on the petri dish lid and marking with a
waterproof marker on the dish lid. In a fume hood, fill the dish with
acetone until the wicking substrate is saturated. The level of acetone
should be just high enough to saturate the filter paper without creating
puddles.
j. Remove about a quarter section of the carbon-coated filter
samples from the glass slides using a surgical knife and tweezers.
Carefully place the section of the filter, carbon side down, on the
appropriately labeled grid in the acetone-saturated petri dish. When all
filter sections have been transferred, slowly add more solvent to the
wedge-shaped trough to bring the acetone level up to the highest
possible level without disturbing the sample preparations. Cover the
petri dish. Elevate one side of the petri dish by placing a slide under
it. This allows drops of condensed solvent vapors to form near the edge
rather than in the center where they would drip onto the grid
preparation.
G. TEM Method
1. Instrumentation.
a. Use an 80-120 kV TEM capable of performing electron diffraction
with a fluorescent screen inscribed with calibrated gradations. If the
TEM is equipped with EDXA it must either have a STEM attachment or be
capable of producing a spot less than 250 nm
[[Page 777]]
in diameter at crossover. The microscope shall be calibrated routinely
(see Unit III.J.) for magnification and camera constant.
b. While not required on every microscope in the laboratory, the
laboratory must have either one microscope equipped with energy
dispersive X-ray analysis or access to an equivalent system on a TEM in
another laboratory. This must be an Energy Dispersive X-ray Detector
mounted on TEM column and associated hardware/software to collect, save,
and read out spectral information. Calibration of Multi-Channel Analyzer
shall be checked regularly for A1 at 1.48 KeV and Cu at 8.04 KeV, as
well as the manufacturer's procedures.
i. Standard replica grating may be used to determine magnification
(e.g., 2160 lines/mm).
ii. Gold standard may be used to determine camera constant.
c. Use a specimen holder with single tilt and/or double tilt
capabilities.
2. Procedure.
a. Start a new Count Sheet for each sample to be analyzed. Record on
count sheet: analyst's initials and date; lab sample number; client
sample number microscope identification; magnification for analysis;
number of predetermined grid openings to be analyzed; and grid
identification. See the following Figure 4:
[[Page 778]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.011
b. Check that the microscope is properly aligned and calibrated
according to the manufacturer's specifications and instructions.
c. Microscope settings: 80-120 kV, grid assessment 250-1000X, then
15,000-20,000X screen magnification for analysis.
d. Approximately one-half (0.5) of the predetermined sample area to
be analyzed shall be performed on one sample grid preparation and the
remaining half on a second sample grid preparation.
e. Determine the suitability of the grid.
[[Page 779]]
i. Individual grid openings with greater than 5 percent openings
(holes) or covered with greater than 25 percent particulate matter or
obviously having nonuniform loading shall not be analyzed.
ii. Examine the grid at low magnification (<1000X) to determine its
suitability for detailed study at higher magnifications.
iii. Reject the grid if:
(1) Less than 50 percent of the grid openings covered by the replica
are intact.
(2) It is doubled or folded.
(3) It is too dark because of incomplete dissolution of the filter.
iv. If the grid is rejected, load the next sample grid.
v. If the grid is acceptable, continue on to Step 6 if mapping is to
be used; otherwise proceed to Step 7.
f. Grid Map (Optional).
i. Set the TEM to the low magnification mode.
ii. Use flat edge or finder grids for mapping.
iii. Index the grid openings (fields) to be counted by marking the
acceptable fields for one-half (0.5) of the area needed for analysis on
each of the two grids to be analyzed. These may be marked just before
examining each grid opening (field), if desired.
iv. Draw in any details which will allow the grid to be properly
oriented if it is reloaded into the microscope and a particular field is
to be reliably identified.
g. Scan the grid.
i. Select a field to start the examination.
ii. Choose the appropriate magnification (15,000 to 20,000X screen
magnification).
iii. Scan the grid as follows.
(1) At the selected magnification, make a series of parallel
traverses across the field. On reaching the end of one traverse, move
the image one window and reverse the traverse.
Note: A slight overlap should be used so as not to miss any part of
the grid opening (field).
(2) Make parallel traverses until the entire grid opening (field)
has been scanned.
h. Identify each structure for appearance and size.
i. Appearance and size: Any continuous grouping of particles in
which an asbestos fiber within aspect ratio greater than or equal to 5:1
and a length greater than or equal to 0.5 [mu]m is detected shall be
recorded on the count sheet. These will be designated asbestos
structures and will be classified as fibers, bundles, clusters, or
matrices. Record as individual fibers any contiguous grouping having 0,
1, or 2 definable intersections. Groupings having more than 2
intersections are to be described as cluster or matrix. See the
following Figure 5:
[[Page 780]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.012
[[Page 781]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.013
An intersection is a non-parallel touching or crossing of fibers, with
the projection having an aspect ratio of 5:1 or greater. Combinations
such as a matrix and cluster, matrix and bundle, or bundle and cluster
are categorized by the dominant fiber quality--cluster, bundle, and
matrix, respectively. Separate categories will be maintained for fibers
less than 5 [mu]m and for fibers greater than or equal to 5 [mu]m in
length. Not required, but useful, may be to record the fiber length in 1
[mu]m intervals. (Identify each structure morphologically and analyze it
as it enters the ``window''.)
(1) Fiber. A structure having a minimum length greater than 0.5
[mu]m and an aspect ratio (length to width) of 5:1 or greater and
substantially parallel sides. Note the appearance of the end of the
fiber, i.e., whether it is flat, rounded or dovetailed, no
intersections.
(2) Bundle. A structure composed of 3 or more fibers in a parallel
arrangement with each fiber closer than one fiber diameter.
(3) Cluster. A structure with fibers in a random arrangement such
that all fibers are intermixed and no single fiber is isolated from the
group; groupings must have more than 2 intersections.
[[Page 782]]
(4) Matrix. Fiber or fibers with one end free and the other end
embedded in or hidden by a particulate. The exposed fiber must meet the
fiber definition.
(5) NSD. Record NSD when no structures are detected in the field.
(6) Intersection. Non-parallel touching or crossing of fibers, with
the projection having an aspect ratio 5:1 or greater.
ii. Structure Measurement.
(1) Recognize the structure that is to be sized.
(2) Memorize its location in the ``window'' relative to the sides,
inscribed square and to other particulates in the field so this exact
location can be found again when scanning is resumed.
(3) Measure the structure using the scale on the screen.
(4) Record the length category and structure type classification on
the count sheet after the field number and fiber number.
(5) Return the fiber to its original location in the window and scan
the rest of the field for other fibers; if the direction of travel is
not remembered, return to the right side of the field and begin the
traverse again.
i. Visual identification of Electron Diffraction (ED) patterns is
required for each asbestos structure counted which would cause the
analysis to exceed the 70 s/mm\2\ concentration. (Generally this means
the first four fibers identified as asbestos must exhibit an
identifiable diffraction pattern for chrysotile or amphibole.)
i. Center the structure, focus, and obtain an ED pattern. (See
Microscope Instruction Manual for more detailed instructions.)
ii. From a visual examination of the ED pattern, obtained with a
short camera length, classify the observed structure as belonging to one
of the following classifications: chrysotile, amphibole, or nonasbestos.
(1) Chrysotile: The chrysotile asbestos pattern has characteristic
streaks on the layer lines other than the central line and some
streaking also on the central line. There will be spots of normal
sharpness on the central layer line and on alternate lines (2nd, 4th,
etc.). The repeat distance between layer lines is 0.53 nm and the center
doublet is at 0.73 nm. The pattern should display (002), (110), (130)
diffraction maxima; distances and geometry should match a chrysotile
pattern and be measured semiquantitatively.
(2) Amphibole Group [includes grunerite (amosite), crocidolite,
anthophyllite, tremolite, and actinolite]: Amphibole asbestos fiber
patterns show layer lines formed by very closely spaced dots, and the
repeat distance between layer lines is also about 0.53 nm. Streaking in
layer lines is occasionally present due to crystal structure defects.
(3) Nonasbestos: Incomplete or unobtainable ED patterns, a
nonasbestos EDXA, or a nonasbestos morphology.
iii. The micrograph number of the recorded diffraction patterns must
be reported to the client and maintained in the laboratory's quality
assurance records. The records must also demonstrate that the
identification of the pattern has been verified by a qualified
individual and that the operator who made the identification is
maintaining at least an 80 percent correct visual identification based
on his measured patterns. In the event that examination of the pattern
by the qualified individual indicates that the pattern had been
misidentified visually, the client shall be contacted. If the pattern is
a suspected chrysotile, take a photograph of the diffraction pattern at
0 degrees tilt. If the structure is suspected to be amphibole, the
sample may have to be tilted to obtain a simple geometric array of
spots.
j. Energy Dispersive X-Ray Analysis (EDXA).
i. Required of all amphiboles which would cause the analysis results
to exceed the 70 s/mm\2\ concentration. (Generally speaking, the first 4
amphiboles would require EDXA.)
ii. Can be used alone to confirm chrysotile after the 70 s/mm\2\
concentration has been exceeded.
iii. Can be used alone to confirm all nonasbestos.
iv. Compare spectrum profiles with profiles obtained from asbestos
standards. The closest match identifies and categorizes the structure.
v. If the EDXA is used for confirmation, record the properly labeled
spectrum on a computer disk, or if a hard copy, file with analysis data.
vi. If the number of fibers in the nonasbestos class would cause the
analysis to exceed the 70 s/mm\2\ concentration, their identities must
be confirmed by EDXA or measurement of a zone axis diffraction pattern
to establish that the particles are nonasbestos.
k. Stopping Rules.
i. If more than 50 asbestiform structures are counted in a
particular grid opening, the analysis may be terminated.
ii. After having counted 50 asbestiform structures in a minimum of 4
grid openings, the analysis may be terminated. The grid opening in which
the 50th fiber was counted must be completed.
iii. For blank samples, the analysis is always continued until 10
grid openings have been analyzed.
iv. In all other samples the analysis shall be continued until an
analytical sensitivity of 0.005 s/cm\3\ is reached.
l. Recording Rules. The count sheet should contain the following
information:
i. Field (grid opening): List field number.
ii. Record ``NSD'' if no structures are detected.
iii. Structure information.
[[Page 783]]
(1) If fibers, bundles, clusters, and/or matrices are found, list
them in consecutive numerical order, starting over with each field.
(2) Length. Record length category of asbestos fibers examined.
Indicate if less than 5 [mu]m or greater than or equal to 5 [mu]m.
(3) Structure Type. Positive identification of asbestos fibers is
required by the method. At least one diffraction pattern of each fiber
type from every five samples must be recorded and compared with a
standard diffraction pattern. For each asbestos fiber reported, both a
morphological descriptor and an identification descriptor shall be
specified on the count sheet.
(4) Fibers classified as chrysotile must be identified by
diffraction and/or X-ray analysis and recorded on the count sheet. X-ray
analysis alone can be used as sole identification only after 70s/mm\2\
have been exceeded for a particular sample.
(5) Fibers classified as amphiboles must be identified by X-ray
analysis and electron diffraction and recorded on the count sheet. (X-
ray analysis alone can be used as sole identification only after 70s/
mm\2\ have been exceeded for a particular sample.)
(6) If a diffraction pattern was recorded on film, the micrograph
number must be indicated on the count sheet.
(7) If an electron diffraction was attempted and an appropriate
spectra is not observed, N should be recorded on the count sheet.
(8) If an X-ray analysis is attempted but not observed, N should be
recorded on the count sheet.
(9) If an X-ray analysis spectrum is stored, the file and disk
number must be recorded on the count sheet.
m. Classification Rules.
i. Fiber. A structure having a minimum length greater than or equal
to 0.5 [mu]m and an aspect ratio (length to width) of 5:1 or greater and
substantially parallel sides. Note the appearance of the end of the
fiber, i.e., whether it is flat, rounded or dovetailed.
ii. Bundle. A structure composed of three or more fibers in a
parallel arrangement with each fiber closer than one fiber diameter.
iii. Cluster. A structure with fibers in a random arrangement such
that all fibers are intermixed and no single fiber is isolated from the
group. Groupings must have more than two intersections.
iv. Matrix. Fiber or fibers with one end free and the other end
embedded in or hidden by a particulate. The exposed fiber must meet the
fiber definition.
v. NSD. Record NSD when no structures are detected in the field.
n. After all necessary analyses of a particle structure have been
completed, return the goniometer stage to 0 degrees, and return the
structure to its original location by recall of the original location.
o. Continue scanning until all the structures are identified,
classified and sized in the field.
p. Select additional fields (grid openings) at low magnification;
scan at a chosen magnification (15,000 to 20,000X screen magnification);
and analyze until the stopping rule becomes applicable.
q. Carefully record all data as they are being collected, and check
for accuracy.
r. After finishing with a grid, remove it from the microscope, and
replace it in the appropriate grid hold. Sample grids must be stored for
a minimum of 1 year from the date of the analysis; the sample cassette
must be retained for a minimum of 30 days by the laboratory or returned
at the client's request.
H. Sample Analytical Sequence
1. Carry out visual inspection of work site prior to air monitoring.
2. Collect a minimum of five air samples inside the work site and
five samples outside the work site. The indoor and outdoor samples shall
be taken during the same time period.
3. Analyze the abatement area samples according to this protocol.
The analysis must meet the 0.005 s/cm\3\ analytical sensitivity.
4. Remaining steps in the analytical sequence are contained in Unit
IV. of this Appendix.
I. Reporting
The following information must be reported to the client. See the
following Table II:
[[Page 784]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.014
1. Concentration in structures per square millimeter and structures
per cubic centimeter.
2. Analytical sensitivity used for the analysis.
3. Number of asbestos structures.
4. Area analyzed.
5. Volume of air samples (which was initially provided by client).
6. Average grid size opening.
7. Number of grids analyzed.
8. Copy of the count sheet must be included with the report.
[[Page 785]]
9. Signature of laboratory official to indicate that the laboratory
met specifications of the AHERA method.
10. Report form must contain official laboratory identification
(e.g., letterhead).
11. Type of asbestos.
J. Calibration Methodology
Note: Appropriate implementation of the method requires a person
knowledgeable in electron diffraction and mineral identification by ED
and EDXA. Those inexperienced laboratories wishing to develop
capabilities may acquire necessary knowledge through analysis of
appropriate standards and by following detailed methods as described in
References 8 and 10 of Unit III.L.
1. Equipment Calibration. In this method, calibration is required
for the air-sampling equipment and the transmission electron microscope
(TEM).
a. TEM Magnification. The magnification at the fluorescent screen of
the TEM must be calibrated at the grid opening magnification (if used)
and also at the magnification used for fiber counting. This is performed
with a cross grating replica. A logbook must be maintained, and the
dates of calibration depend on the past history of the particular
microscope; no frequency is specified. After any maintenance of the
microscope that involved adjustment of the power supplied to the lenses
or the high-voltage system or the mechanical disassembly of the electron
optical column apart from filament exchange, the magnification must be
recalibrated. Before the TEM calibration is performed, the analyst must
ensure that the cross grating replica is placed at the same distance
from the objective lens as the specimens are. For instruments that
incorporate an eucentric tilting specimen stage, all speciments and the
cross grating replica must be placed at the eucentric position.
b. Determination of the TEM magnification on the fluorescent screen.
i. Define a field of view on the fluorescent screen either by
markings or physical boundaries. The field of view must be measurable or
previously inscribed with a scale or concentric circles (all scales
should be metric).
ii. Insert a diffraction grating replica (for example a grating
containing 2,160 lines/mm) into the specimen holder and place into the
microscope. Orient the replica so that the grating lines fall
perpendicular to the scale on the TEM fluorescent screen. Ensure that
the goniometer stage tilt is 0 degrees.
iii. Adjust microscope magnification to 10,000X or 20,000X. Measure
the distance (mm) between two widely separated lines on the grating
replica. Note the number of spaces between the lines. Take care to
measure between the same relative positions on the lines (e.g., between
left edges of lines).
Note: The more spaces included in the measurement, the more accurate
the final calculation. On most microscopes, however, the magnification
is substantially constant only within the central 8-10 cm diameter
region of the fluorescent screen.
iv. Calculate the true magnification (M) on the fluorescent screen:
M=XG/Y
where:
X=total distance (mm) between the designated grating lines;
G=calibration constant of the grating replica (lines/mm):
Y=number of grating replica spaces counted along X.
c. Calibration of the EDXA System. Initially, the EDXA system must
be calibrated by using two reference elements to calibrate the energy
scale of the instrument. When this has been completed in accordance with
the manufacturer's instructions, calibration in terms of the different
types of asbestos can proceed. The EDXA detectors vary in both solid
angle of detection and in window thickness. Therefore, at a particular
accelerating voltage in use on the TEM, the count rate obtained from
specific dimensions of fiber will vary both in absolute X-ray count rate
and in the relative X-ray peak heights for different elements. Only a
few minerals are relevant for asbestos abatement work, and in this
procedure the calibration is specified in terms of a ``fingerprint''
technique. The EDXA spectra must be recorded from individual fibers of
the relevant minerals, and identifications are made on the basis of
semiquantitative comparisons with these reference spectra.
d. Calibration of Grid Openings.
i. Measure 20 grid openings on each of 20 random 200-mesh copper
grids by placing a grid on a glass slide and examining it under the PCM.
Use a calibrated graticule to measure the average field diameter and use
this number to calculate the field area for an average grid opening.
Grids are to be randomly selected from batches up to 1,000.
Note: A grid opening is considered as one field.
ii. The mean grid opening area must be measured for the type of
specimen grids in use. This can be accomplished on the TEM at a properly
calibrated low magnification or on an optical microscope at a
magnification of approximately 400X by using an eyepiece fitted with a
scale that has been calibrated against a stage micrometer. Optical
microscopy utilizing manual or automated procedures may be used
providing instrument calibration can be verified.
e. Determination of Camera Constant and ED Pattern Analysis.
i. The camera length of the TEM in ED operating mode must be
calibrated before ED patterns on unknown samples are observed. This can
be achieved by using a carbon-coated grid on which a thin film of gold
has been
[[Page 786]]
sputtered or evaporated. A thin film of gold is evaporated on the
specimen TEM grid to obtain zone-axis ED patterns superimposed with a
ring pattern from the polycrystalline gold film.
ii. In practice, it is desirable to optimize the thickness of the
gold film so that only one or two sharp rings are obtained on the
superimposed ED pattern. Thicker gold film would normally give multiple
gold rings, but it will tend to mask weaker diffraction spots from the
unknown fibrous particulates. Since the unknown d-spacings of most
interest in asbestos analysis are those which lie closest to the
transmitted beam, multiple gold rings are unnecessary on zone-axis ED
patterns. An average camera constant using multiple gold rings can be
determined. The camera constant is one-half the diameter, D, of the
rings times the interplanar spacing, d, of the ring being measured.
K. Quality Control/Quality Assurance Procedures (Data Quality
Indicators)
Monitoring the environment for airborne asbestos requires the use of
sensitive sampling and analysis procedures. Because the test is
sensitive, it may be influenced by a variety of factors. These include
the supplies used in the sampling operation, the performance of the
sampling, the preparation of the grid from the filter and the actual
examination of this grid in the microscope. Each of these unit
operations must produce a product of defined quality if the analytical
result is to be a reliable and meaningful test result. Accordingly, a
series of control checks and reference standards is performed along with
the sample analysis as indicators that the materials used are adequate
and the operations are within acceptable limits. In this way, the
quality of the data is defined and the results are of known value. These
checks and tests also provide timely and specific warning of any
problems which might develop within the sampling and analysis
operations. A description of these quality control/quality assurance
procedures is summarized in the following Table III:
[[Page 787]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.015
1. When the samples arrive at the laboratory, check the samples and
documentation for completeness and requirements before initiating the
analysis.
2. Check all laboratory reagents and supplies for acceptable
asbestos background levels.
3. Conduct all sample preparation in a clean room environment
monitored by laboratory blanks and special testing after cleaning or
servicing the room.
4. Prepare multiple grids of each sample.
5. Provide laboratory blanks with each sample batch. Maintain a
cumulative average of these results. If this average is greater than 53
f/mm \2\ per 10 200-mesh grid openings, check the system for possible
sources of contamination.
6. Check for recovery of asbestos from cellulose ester filters
submitted to plasma asher.
7. Check for asbestos carryover in the plasma asher by including a
blank alongside the positive control sample.
[[Page 788]]
8. Perform a systems check on the transmission electron microscope
daily.
9. Make periodic performance checks of magnification, electron
diffraction and energy dispersive X-ray systems as set forth in Table
III of Unit III.K.
10. Ensure qualified operator performance by evaluation of replicate
counting, duplicate analysis, and standard sample comparisons as set
forth in Table III of Unit III.K.
11. Validate all data entries.
12. Recalculate a percentage of all computations and automatic data
reduction steps as specified in Table III.
13. Record an electron diffraction pattern of one asbestos structure
from every five samples that contain asbestos. Verify the identification
of the pattern by measurement or comparison of the pattern with patterns
collected from standards under the same conditions.
The outline of quality control procedures presented above is viewed as
the minimum required to assure that quality data is produced for
clearance testing of an asbestos abated area. Additional information may
be gained by other control tests. Specifics on those control procedures
and options available for environmental testing can be obtained by
consulting References 6, 7, and 11 of Unit III.L.
L. References
For additional background information on this method the following
references should be consulted.
1. ``Guidelines for Controlling Asbestos-Containing Materials in
Buildings,'' EPA 560/5-85-024, June 1985.
2. ``Measuring Airborne Asbestos Following an Abatement Action,''
USEP/Office of Pollution Prevention and Toxics, EPA 600/4-85-049, 1985.
3. Small, John and E. Steel. Asbestos Standards: Materials and
Analytical Methods. N.B.S. Special Publication 619, 1982.
4. Campbell, W.J., R.L. Blake, L.L. Brown, E.E. Cather, and J.J.
Sjoberg. Selected Silicate Minerals and Their Asbestiform Varieties.
Information Circular 8751, U.S. Bureau of Mines, 1977.
5. Quality Assurance Handbook for Air Pollution Measurement System.
Ambient Air Methods, EPA 600/4-77-027a, USEPA, Office of Research and
Development, 1977.
6. Method 2A: Direct Measurement of Gas Volume Through Pipes and
Small Ducts. 40 CFR Part 60 Appendix A.
7. Burdette, G.J. Health & Safety Exec., Research & Lab. Services
Div., London, ``Proposed Analytical Method for Determination of Asbestos
in Air.''
8. Chatfield, E.J., Chatfield Tech. Cons., Ltd., Clark, T., PEI
Assoc. ``Standard Operating Procedure for Determination of Airborne
Asbestos Fibers by Transmission Electron Microscopy Using Polycarbonate
Membrane Filters.'' WERL SOP 87-1, March 5, 1987.
9. NIOSH. Method 7402 for Asbestos Fibers, December 11, 1986 Draft.
10. Yamate, G., S.C. Agarwall, R.D. Gibbons, IIT Research Institute,
``Methodology for the Measurement of Airborne Asbestos by Electron
Microscopy.'' Draft report, USEPA Contract 68-02-3266, July 1984.
11. Guidance to the Preparation of Quality Assurance Project Plans.
USEPA, Office of Pollution Prevention and Toxics, 1984.
IV. Mandatory Interpretation of Transmission Electron Microscopy Results
to Determine Completion of Response Actions
A. Introduction
A response action is determined to be completed by TEM when the
abatement area has been cleaned and the airborne asbestos concentration
inside the abatement area is no higher than concentrations at locations
outside the abatement area. ``Outside'' means outside the abatement
area, but not necessarily outside the building. EPA reasons that an
asbestos removal contractor cannot be expected to clean an abatement
area to an airborne asbestos concentration that is lower than the
concentration of air entering the abatement area from outdoors or from
other parts of the building. After the abatement area has passed a
thorough visual inspection, and before the outer containment barrier is
removed, a minimum of five air samples inside the abatement area and a
minimum of five air samples outside the abatement area must be
collected. Hence, the response action is determined to be completed when
the average airborne asbestos concentration measured inside the
abatement area is not statistically different from the average airborne
asbestos concentration measured outside the abatement area.
The inside and outside concentrations are compared by the Z-test, a
statistical test that takes into account the variability in the
measurement process. A minimum of five samples inside the abatement area
and five samples outside the abatement area are required to control the
false negative error rate, i.e., the probability of declaring the
removal complete when, in fact, the air concentration inside the
abatement area is significantly higher than outside the abatement area.
Additional quality control is provided by requiring three blanks
(filters through which no air has been drawn) to be analyzed to check
for unusually high filter contamination that would distort the test
results.
When volumes greater than or equal to 1,199 L for a 25 mm filter and
2,799 L for a 37 mm filter have been collected and the average number of
asbestos structures on samples inside the abatement area is no greater
than 70 s/mm \2\ of filter, the response action
[[Page 789]]
may be considered complete without comparing the inside samples to the
outside samples. EPA is permitting this initial screening test to save
analysis costs in situations where the airborne asbestos concentration
is sufficiently low so that it cannot be distinguished from the filter
contamination/background level (fibers deposited on the filter that are
unrelated to the air being sampled). The screening test cannot be used
when volumes of less than 1,199 L for 25 mm filter or 2,799 L for a 37
mm filter are collected because the ability to distinguish levels
significantly different from filter background is reduced at low
volumes.
The initial screening test is expressed in structures per square
millimeter of filter because filter background levels come from sources
other than the air being sampled and cannot be meaningfully expressed as
a concentration per cubic centimeter of air. The value of 70 s/mm\2\ is
based on the experience of the panel of microscopists who consider one
structure in 10 grid openings (each grid opening with an area of 0.0057
mm\2\) to be comparable with contamination/background levels of blank
filters. The decision is based, in part, on Poisson statistics which
indicate that four structures must be counted on a filter before the
fiber count is statistically distinguishable from the count for one
structure. As more information on the performance of the method is
collected, this criterion may be modified. Since different combinations
of the number and size of grid openings are permitted under the TEM
protocol, the criterion is expressed in structures per square millimeter
of filter to be consistent across all combinations. Four structures per
10 grid openings corresponds to approximately 70 s/mm\2\.
B. Sample Collection and Analysis
1. A minimum of 13 samples is required: five samples collected
inside the abatement area, five samples collected outside the abatement
area, two field blanks, and one sealed blank.
2. Sampling and TEM analysis must be done according to either the
mandatory or nonmandatory protocols in Appendix A. At least 0.057 mm\2\
of filter must be examined on blank filters.
C. Interpretation of Results
1. The response action shall be considered complete if either:
a. Each sample collected inside the abatement area consists of at
least 1,199 L of air for a 25 mm filter, or 2,799 L of air for a 37 mm
filter, and the arithmetic mean of their asbestos structure
concentrations per square millimeter of filter is less than or equal to
70 s/mm\2\; or
b. The three blank samples have an arithmetic mean of the asbestos
structure concentration on the blank filters that is less than or equal
to 70 s/mm\2\ and the average airborne asbestos concentration measured
inside the abatement area is not statistically higher than the average
airborne asbestos concentration measured outside the abatement area as
determined by the Z-test. The Z-test is carried out by calculating
[GRAPHIC] [TIFF OMITTED] TC01AP92.016
where YI is the average of the natural logarithms of the
inside samples and YO is the average of the natural
logarithms of the outside samples, nI is the number of inside
samples and nO is the number of outside samples. The response
action is considered complete if Z is less than or equal to 1.65.
Note: When no fibers are counted, the calculated detection limit for
that analysis is inserted for the concentration.
2. If the abatement site does not satisfy either (1) or (2) of this
Section C, the site must be recleaned and a new set of samples
collected.
D. Sequence for Analyzing Samples
It is possible to determine completion of the response action
without analyzing all samples. Also, at any point in the process, a
decision may be made to terminate the analysis of existing samples,
reclean the abatement site, and collect a new set of samples. The
following sequence is outlined to minimize the number of analyses needed
to reach a decision.
1. Analyze the inside samples.
2. If at least 1,199 L of air for a 25 mm filter or 2,799 L of air
for a 37 mm filter is collected for each inside sample and the
arithmetic mean concentration of structures per square millimeter of
filter is less than or equal to 70 s/mm\2\, the response action is
complete and no further analysis is needed.
3. If less than 1,199 L of air for a 25 mm filter or 2,799 L of air
for a 37 mm filter is collected for any of the inside samples, or the
arithmetic mean concentration of structures per square millimeter of
filter is greater than 70 s/mm\2\, analyze the three blanks.
4. If the arithmetic mean concentration of structures per square
millimeter on the blank filters is greater than 70 s/mm\2\, terminate
the analysis, identify and correct the source of blank contamination,
and collect a new set of samples.
5. If the arithmetic mean concentration of structures per square
millimeter on the blank filters is less than or equal to 70 s/mm\2\,
analyze the outside samples and perform the Z-test.
[[Page 790]]
6. If the Z-statistic is less than or equal to 1.65, the response
action is complete. If the Z-statistic is greater than 1.65, reclean the
abatement site and collect a new set of samples.
[52 FR 41857, Oct. 30, 1987]
Appendix B to Subpart E of Part 763 [Reserved]
Appendix C to Subpart E of Part 763--Asbestos Model Accreditation Plan
I. Asbestos Model Accreditation Plan for States
The Asbestos Model Accreditation Plan (MAP) for States has eight
components:
(A) Definitions
(B) Initial Training
(C) Examinations
(D) Continuing Education
(E) Qualifications
(F) Recordkeeping Requirements for Training Providers
(G) Deaccreditation
(H) Reciprocity
A. Definitions
For purposes of Appendix C:
1. ``Friable asbestos-containing material (ACM)'' means any material
containing more than one percent asbestos which has been applied on
ceilings, walls, structural members, piping, duct work, or any other
part of a building, which when dry, may be crumbled, pulverized, or
reduced to powder by hand pressure. The term includes non-friable
asbestos-containing material after such previously non-friable material
becomes damaged to the extent that when dry it may be crumbled,
pulverized, or reduced to powder by hand pressure.
2. ``Friable asbestos-containing building material (ACBM)'' means
any friable ACM that is in or on interior structural members or other
parts of a school or public and commercial building.
3. ``Inspection'' means an activity undertaken in a school building,
or a public and commercial building, to determine the presence or
location, or to assess the condition of, friable or non-friable
asbestos-containing building material (ACBM) or suspected ACBM, whether
by visual or physical examination, or by collecting samples of such
material. This term includes reinspections of friable and non-friable
known or assumed ACBM which has been previously identified. The term
does not include the following:
a. Periodic surveillance of the type described in 40 CFR 763.92(b)
solely for the purpose of recording or reporting a change in the
condition of known or assumed ACBM;
b. Inspections performed by employees or agents of Federal, State,
or local government solely for the purpose of determining compliance
with applicable statutes or regulations; or
c. visual inspections of the type described in 40 CFR 763.90(i)
solely for the purpose of determining completion of response actions.
4. ``Major fiber release episode'' means any uncontrolled or
unintentional disturbance of ACBM, resulting in a visible emission,
which involves the falling or dislodging of more than 3 square or linear
feet of friable ACBM.
5. ``Minor fiber release episode'' means any uncontrolled or
unintentional disturbance of ACBM, resulting in a visible emission,
which involves the falling or dislodging of 3 square or linear feet or
less of friable ACBM.
6. ``Public and commercial building'' means the interior space of
any building which is not a school building, except that the term does
not include any residential apartment building of fewer than 10 units or
detached single-family homes. The term includes, but is not limited to:
industrial and office buildings, residential apartment buildings and
condominiums of 10 or more dwelling units, government-owned buildings,
colleges, museums, airports, hospitals, churches, preschools, stores,
warehouses and factories. Interior space includes exterior hallways
connecting buildings, porticos, and mechanical systems used to condition
interior space.
7. ``Response action'' means a method, including removal,
encapsulation, enclosure, repair, and operation and maintenance, that
protects human health and the environment from friable ACBM.
8. ``Small-scale, short-duration activities (SSSD)'' are tasks such
as, but not limited to:
a. Removal of asbestos-containing insulation on pipes.
b. Removal of small quantities of asbestos-containing insulation on
beams or above ceilings.
c. Replacement of an asbestos-containing gasket on a valve.
d. Installation or removal of a small section of drywall.
e. Installation of electrical conduits through or proximate to
asbestos-containing materials.
SSSD can be further defined by the following considerations:
f. Removal of small quantities of ACM only if required in the
performance of another maintenance activity not intended as asbestos
abatement.
g. Removal of asbestos-containing thermal system insulation not to
exceed amounts greater than those which can be contained in a single
glove bag.
h. Minor repairs to damaged thermal system insulation which do not
require removal.
i. Repairs to a piece of asbestos-containing wallboard.
j. Repairs, involving encapsulation, enclosure, or removal, to small
amounts of friable
[[Page 791]]
ACM only if required in the performance of emergency or routine
maintenance activity and not intended solely as asbestos abatement. Such
work may not exceed amounts greater than those which can be contained in
a single prefabricated mini-enclosure. Such an enclosure shall conform
spatially and geometrically to the localized work area, in order to
perform its intended containment function.
B. Initial Training
Training requirements for purposes of accreditation are specified
both in terms of required subjects of instruction and in terms of length
of training. Each initial training course has a prescribed curriculum
and number of days of training. One day of training equals 8 hours,
including breaks and lunch. Course instruction must be provided by EPA
or State-approved instructors. EPA or State instructor approval shall be
based upon a review of the instructor's academic credentials and/or
field experience in asbestos abatement.
Beyond the initial training requirements, individual States may wish
to consider requiring additional days of training for purposes of
supplementing hands-on activities or for reviewing relevant state
regulations. States also may wish to consider the relative merits of a
worker apprenticeship program. Further, they might consider more
stringent minimum qualification standards for the approval of training
instructors. EPA recommends that the enrollment in any given course be
limited to 25 students so that adequate opportunities exist for
individual hands-on experience.
States have the option to provide initial training directly or
approve other entities to offer training. The following requirements are
for the initial training of persons required to have accreditation under
TSCA Title II.
Training requirements for each of the five accredited disciplines
are outlined below. Persons in each discipline perform a different job
function and distinct role. Inspectors identify and assess the condition
of ACBM, or suspect ACBM. Management planners use data gathered by
inspectors to assess the degree of hazard posed by ACBM in schools to
determine the scope and timing of appropriate response actions needed
for schools. Project designers determine how asbestos abatement work
should be conducted. Lastly, workers and contractor/supervisors carry
out and oversee abatement work. In addition, a recommended training
curriculum is also presented for a sixth discipline, which is not
federally-accredited, that of ``Project Monitor.'' Each accredited
discipline and training curriculum is separate and distinct from the
others. A person seeking accreditation in any of the five accredited MAP
disciplines cannot attend two or more courses concurrently, but may
attend such courses sequentially.
In several instances, initial training courses for a specific
discipline (e.g., workers, inspectors) require hands-on training. For
asbestos abatement contractor/supervisors and workers, hands-on training
should include working with asbestos-substitute materials, fitting and
using respirators, use of glovebags, donning protective clothing, and
constructing a decontamination unit as well as other abatement work
activities.
1. Workers
A person must be accredited as a worker to carry out any of the
following activities with respect to friable ACBM in a school or public
and commercial building: (1) A response action other than a SSSD
activity, (2) a maintenance activity that disturbs friable ACBM other
than a SSSD activity, or (3) a response action for a major fiber release
episode. All persons seeking accreditation as asbestos abatement workers
shall complete at least a 4-day training course as outlined below. The
4-day worker training course shall include lectures, demonstrations, at
least 14 hours of hands-on training, individual respirator fit testing,
course review, and an examination. Hands-on training must permit workers
to have actual experience performing tasks associated with asbestos
abatement. A person who is otherwise accredited as a contractor/
supervisor may perform in the role of a worker without possessing
separate accreditation as a worker.
Because of cultural diversity associated with the asbestos
workforce, EPA recommends that States adopt specific standards for the
approval of foreign language courses for abatement workers. EPA further
recommends the use of audio-visual materials to complement lectures,
where appropriate.
The training course shall adequately address the following topics:
(a) Physical characteristics of asbestos. Identification of
asbestos, aerodynamic characteristics, typical uses, and physical
appearance, and a summary of abatement control options.
(b) Potential health effects related to asbestos exposure. The
nature of asbestos-related diseases; routes of exposure; dose-response
relationships and the lack of a safe exposure level; the synergistic
effect between cigarette smoking and asbestos exposure; the latency
periods for asbestos-related diseases; a discussion of the relationship
of asbestos exposure to asbestosis, lung cancer, mesothelioma, and
cancers of other organs.
(c) Employee personal protective equipment. Classes and
characteristics of respirator types; limitations of respirators; proper
selection, inspection; donning, use, maintenance, and storage procedures
for respirators; methods for field testing of the
[[Page 792]]
facepiece-to-face seal (positive and negative-pressure fit checks);
qualitative and quantitative fit testing procedures; variability between
field and laboratory protection factors that alter respiratory fit
(e.g., facial hair); the components of a proper respiratory protection
program; selection and use of personal protective clothing; use,
storage, and handling of non-disposable clothing; and regulations
covering personal protective equipment.
(d) State-of-the-art work practices. Proper work practices for
asbestos abatement activities, including descriptions of proper
construction; maintenance of barriers and decontamination enclosure
systems; positioning of warning signs; lock-out of electrical and
ventilation systems; proper working techniques for minimizing fiber
release; use of wet methods; use of negative pressure exhaust
ventilation equipment; use of high-efficiency particulate air (HEPA)
vacuums; proper clean-up and disposal procedures; work practices for
removal, encapsulation, enclosure, and repair of ACM; emergency
procedures for sudden releases; potential exposure situations; transport
and disposal procedures; and recommended and prohibited work practices.
(e) Personal hygiene. Entry and exit procedures for the work area;
use of showers; avoidance of eating, drinking, smoking, and chewing (gum
or tobacco) in the work area; and potential exposures, such as family
exposure.
(f) Additional safety hazards. Hazards encountered during abatement
activities and how to deal with them, including electrical hazards, heat
stress, air contaminants other than asbestos, fire and explosion
hazards, scaffold and ladder hazards, slips, trips, and falls, and
confined spaces.
(g) Medical monitoring. OSHA and EPA Worker Protection Rule
requirements for physical examinations, including a pulmonary function
test, chest X-rays, and a medical history for each employee.
(h) Air monitoring. Procedures to determine airborne concentrations
of asbestos fibers, focusing on how personal air sampling is performed
and the reasons for it.
(i) Relevant Federal, State, and local regulatory requirements,
procedures, and standards. With particular attention directed at
relevant EPA, OSHA, and State regulations concerning asbestos abatement
workers.
(j) Establishment of respiratory protection programs.
(k) Course review. A review of key aspects of the training course.
2. Contractor/Supervisors
A person must be accredited as a contractor/supervisor to supervise
any of the following activities with respect to friable ACBM in a school
or public and commercial building: (1) A response action other than a
SSSD activity, (2) a maintenance activity that disturbs friable ACBM
other than a SSSD activity, or (3) a response action for a major fiber
release episode. All persons seeking accreditation as asbestos abatement
contractor/supervisors shall complete at least a 5-day training course
as outlined below. The training course must include lectures,
demonstrations, at least 14 hours of hands-on training, individual
respirator fit testing, course review, and a written examination. Hands-
on training must permit supervisors to have actual experience performing
tasks associated with asbestos abatement.
EPA recommends the use of audiovisual materials to complement
lectures, where appropriate.
Asbestos abatement supervisors include those persons who provide
supervision and direction to workers performing response actions.
Supervisors may include those individuals with the position title of
foreman, working foreman, or leadman pursuant to collective bargaining
agreements. At least one supervisor is required to be at the worksite at
all times while response actions are being conducted. Asbestos workers
must have access to accredited supervisors throughout the duration of
the project.
The contractor/supervisor training course shall adequately address
the following topics:
(a) The physical characteristics of asbestos and asbestos-containing
materials. Identification of asbestos, aerodynamic characteristics,
typical uses, physical appearance, a review of hazard assessment
considerations, and a summary of abatement control options.
(b) Potential health effects related to asbestos exposure. The
nature of asbestos-related diseases; routes of exposure; dose-response
relationships and the lack of a safe exposure level; synergism between
cigarette smoking and asbestos exposure; and latency period for
diseases.
(c) Employee personal protective equipment. Classes and
characteristics of respirator types; limitations of respirators; proper
selection, inspection, donning, use, maintenance, and storage procedures
for respirators; methods for field testing of the facepiece-to-face seal
(positive and negative-pressure fit checks); qualitative and
quantitative fit testing procedures; variability between field and
laboratory protection factors that alter respiratory fit (e.g., facial
hair); the components of a proper respiratory protection program;
selection and use of personal protective clothing; and use, storage, and
handling of non-disposable clothing; and regulations covering personal
protective equipment.
(d) State-of-the-art work practices. Proper work practices for
asbestos abatement activities, including descriptions of proper
construction and maintenance of barriers and
[[Page 793]]
decontamination enclosure systems; positioning of warning signs; lock-
out of electrical and ventilation systems; proper working techniques for
minimizing fiber release; use of wet methods; use of negative pressure
exhaust ventilation equipment; use of HEPA vacuums; and proper clean-up
and disposal procedures. Work practices for removal, encapsulation,
enclosure, and repair of ACM; emergency procedures for unplanned
releases; potential exposure situations; transport and disposal
procedures; and recommended and prohibited work practices. New
abatement-related techniques and methodologies may be discussed.
(e) Personal hygiene. Entry and exit procedures for the work area;
use of showers; and avoidance of eating, drinking, smoking, and chewing
(gum or tobacco) in the work area. Potential exposures, such as family
exposure, shall also be included.
(f) Additional safety hazards. Hazards encountered during abatement
activities and how to deal with them, including electrical hazards, heat
stress, air contaminants other than asbestos, fire and explosion
hazards, scaffold and ladder hazards, slips, trips, and falls, and
confined spaces.
(g) Medical monitoring. OSHA and EPA Worker Protection Rule
requirements for physical examinations, including a pulmonary function
test, chest X-rays and a medical history for each employee.
(h) Air monitoring. Procedures to determine airborne concentrations
of asbestos fibers, including descriptions of aggressive air sampling,
sampling equipment and methods, reasons for air monitoring, types of
samples and interpretation of results.
EPA recommends that transmission electron microscopy (TEM) be used
for analysis of final air clearance samples, and that sample analyses be
performed by laboratories accredited by the National Institute of
Standards and Technology's (NIST) National Voluntary Laboratory
Accreditation Program (NVLAP).
(i) Relevant Federal, State, and local regulatory requirements,
procedures, and standards, including:
(i) Requirements of TSCA Title II.
(ii) National Emission Standards for Hazardous Air Pollutants (40
CFR part 61), Subparts A (General Provisions) and M (National Emission
Standard for Asbestos).
(iii) OSHA standards for permissible exposure to airborne
concentrations of asbestos fibers and respiratory protection (29 CFR
1910.134).
(iv) OSHA Asbestos Construction Standard (29 CFR 1926.58). (v)EPA
Worker Protection Rule, (40 CFR part 763, Subpart G).
(j) Respiratory Protection Programs and Medical Monitoring Programs.
(k) Insurance and liability issues. Contractor issues; worker's
compensation coverage and exclusions; third-party liabilities and
defenses; insurance coverage and exclusions.
(l) Recordkeeping for asbestos abatement projects. Records required
by Federal, State, and local regulations; records recommended for legal
and insurance purposes.
(m) Supervisory techniques for asbestos abatement activities.
Supervisory practices to enforce and reinforce the required work
practices and discourage unsafe work practices.
(n) Contract specifications. Discussions of key elements that are
included in contract specifications.
(o) Course review. A review of key aspects of the training course.
3. Inspector
All persons who inspect for ACBM in schools or public and commercial
buildings must be accredited. All persons seeking accreditation as an
inspector shall complete at least a 3-day training course as outlined
below. The course shall include lectures, demonstrations, 4 hours of
hands-on training, individual respirator fit-testing, course review, and
a written examination.
EPA recommends the use of audiovisual materials to complement
lectures, where appropriate. Hands-on training should include conducting
a simulated building walk-through inspection and respirator fit testing.
The inspector training course shall adequately address the following
topics:
(a) Background information on asbestos. Identification of asbestos,
and examples and discussion of the uses and locations of asbestos in
buildings; physical appearance of asbestos.
(b) Potential health effects related to asbestos exposure. The
nature of asbestos-related diseases; routes of exposure; dose-response
relationships and the lack of a safe exposure level; the synergistic
effect between cigarette smoking and asbestos exposure; the latency
periods for asbestos-related diseases; a discussion of the relationship
of asbestos exposure to asbestosis, lung cancer, mesothelioma, and
cancers of other organs.
(c) Functions/qualifications and role of inspectors. Discussions of
prior experience and qualifications for inspectors and management
planners; discussions of the functions of an accredited inspector as
compared to those of an accredited management planner; discussion of
inspection process including inventory of ACM and physical assessment.
(d) Legal liabilities and defenses. Responsibilities of the
inspector and management planner; a discussion of comprehensive general
liability policies, claims-made, and occurrence policies, environmental
and pollution liability policy clauses; state liability insurance
requirements; bonding and the relationship of insurance availability to
bond availability.
(e) Understanding building systems. The interrelationship between
building systems,
[[Page 794]]
including: an overview of common building physical plan layout; heat,
ventilation, and air conditioning (HVAC) system types, physical
organization, and where asbestos is found on HVAC components; building
mechanical systems, their types and organization, and where to look for
asbestos on such systems; inspecting electrical systems, including
appropriate safety precautions; reading blueprints and as-built
drawings.
(f) Public/employee/building occupant relations. Notifying employee
organizations about the inspection; signs to warn building occupants;
tact in dealing with occupants and the press; scheduling of inspections
to minimize disruptions; and education of building occupants about
actions being taken.
(g) Pre-inspection planning and review of previous inspection
records. Scheduling the inspection and obtaining access; building record
review; identification of probable homogeneous areas from blueprints or
as-built drawings; consultation with maintenance or building personnel;
review of previous inspection, sampling, and abatement records of a
building; the role of the inspector in exclusions for previously
performed inspections.
(h) Inspecting for friable and non-friable ACM and assessing the
condition of friable ACM. Procedures to follow in conducting visual
inspections for friable and non-friable ACM; types of building materials
that may contain asbestos; touching materials to determine friability;
open return air plenums and their importance in HVAC systems; assessing
damage, significant damage, potential damage, and potential significant
damage; amount of suspected ACM, both in total quantity and as a
percentage of the total area; type of damage; accessibility; material's
potential for disturbance; known or suspected causes of damage or
significant damage; and deterioration as assessment factors.
(i) Bulk sampling/documentation of asbestos. Detailed discussion of
the ``Simplified Sampling Scheme for Friable Surfacing Materials (EPA
560/5-85-030a October 1985)''; techniques to ensure sampling in a
randomly distributed manner for other than friable surfacing materials;
sampling of non-friable materials; techniques for bulk sampling;
inspector's sampling and repair equipment; patching or repair of damage
from sampling; discussion of polarized light microscopy; choosing an
accredited laboratory to analyze bulk samples; quality control and
quality assurance procedures. EPA's recommendation that all bulk samples
collected from school or public and commercial buildings be analyzed by
a laboratory accredited under the NVLAP administered by NIST.
(j) Inspector respiratory protection and personal protective
equipment. Classes and characteristics of respirator types; limitations
of respirators; proper selection, inspection; donning, use, maintenance,
and storage procedures for respirators; methods for field testing of the
facepiece-to-face seal (positive and negative-pressure fit checks);
qualitative and quantitative fit testing procedures; variability between
field and laboratory protection factors that alter respiratory fit
(e.g., facial hair); the components of a proper respiratory protection
program; selection and use of personal protective clothing; use,
storage, and handling of non-disposable clothing.
(k) Recordkeeping and writing the inspection report. Labeling of
samples and keying sample identification to sampling location;
recommendations on sample labeling; detailing of ACM inventory;
photographs of selected sampling areas and examples of ACM condition;
information required for inclusion in the management plan required for
school buildings under TSCA Title II, section 203 (i)(1). EPA recommends
that States develop and require the use of standardized forms for
recording the results of inspections in schools or public or commercial
buildings, and that the use of these forms be incorporated into the
curriculum of training conducted for accreditation.
(l) Regulatory review. The following topics should be covered:
National Emission Standards for Hazardous Air Pollutants (NESHAP; 40 CFR
part 61, Subparts A and M); EPA Worker Protection Rule (40 CFR part 763,
Subpart G); OSHA Asbestos Construction Standard (29 CFR 1926.58); OSHA
respirator requirements (29 CFR 1910.134); the Asbestos-Containing
Materials in School Rule (40 CFR part 763, Subpart E; applicable State
and local regulations, and differences between Federal and State
requirements where they apply, and the effects, if any, on public and
nonpublic schools or commercial or public buildings.
(m) Field trip. This includes a field exercise, including a walk-
through inspection; on-site discussion about information gathering and
the determination of sampling locations; on-site practice in physical
assessment; classroom discussion of field exercise.
(n) Course review. A review of key aspects of the training course.
4. Management Planner
All persons who prepare management plans for schools must be
accredited. All persons seeking accreditation as management planners
shall complete a 3-day inspector training course as outlined above and a
2-day management planner training course. Possession of current and
valid inspector accreditation shall be a prerequisite for admission to
the management planner training course. The management planner course
shall include lectures, demonstrations, course review, and a written
examination.
[[Page 795]]
EPA recommends the use of audiovisual materials to complement
lectures, where appropriate.
TSCA Title II does not require accreditation for persons performing
the management planner role in public and commercial buildings.
Nevertheless, such persons may find this training and accreditation
helpful in preparing them to design or administer asbestos operations
and maintenance programs for public and commercial buildings.
The management planner training course shall adequately address the
following topics:
(a) Course overview. The role and responsibilities of the management
planner; operations and maintenance programs; setting work priorities;
protection of building occupants.
(b) Evaluation/interpretation of survey results. Review of TSCA
Title II requirements for inspection and management plans for school
buildings as given in section 203(i)(1) of TSCA Title II; interpretation
of field data and laboratory results; comparison of field inspector's
data sheet with laboratory results and site survey.
(c) Hazard assessment. Amplification of the difference between
physical assessment and hazard assessment; the role of the management
planner in hazard assessment; explanation of significant damage, damage,
potential damage, and potential significant damage; use of a description
(or decision tree) code for assessment of ACM; assessment of friable
ACM; relationship of accessibility, vibration sources, use of adjoining
space, and air plenums and other factors to hazard assessment.
(d) Legal implications. Liability; insurance issues specific to
planners; liabilities associated with interim control measures, in-house
maintenance, repair, and removal; use of results from previously
performed inspections.
(e) Evaluation and selection of control options. Overview of
encapsulation, enclosure, interim operations and maintenance, and
removal; advantages and disadvantages of each method; response actions
described via a decision tree or other appropriate method; work
practices for each response action; staging and prioritizing of work in
both vacant and occupied buildings; the need for containment barriers
and decontamination in response actions.
(f) Role of other professionals. Use of industrial hygienists,
engineers, and architects in developing technical specifications for
response actions; any requirements that may exist for architect sign-off
of plans; team approach to design of high-quality job specifications.
(g) Developing an operations and maintenance (O&M) plan. Purpose of
the plan; discussion of applicable EPA guidance documents; what actions
should be taken by custodial staff; proper cleaning procedures; steam
cleaning and HEPA vacuuming; reducing disturbance of ACM; scheduling O&M
for off-hours; rescheduling or canceling renovation in areas with ACM;
boiler room maintenance; disposal of ACM; in-house procedures for ACM--
bridging and penetrating encapsulants; pipe fittings; metal sleeves;
polyvinyl chloride (PVC), canvas, and wet wraps; muslin with straps,
fiber mesh cloth; mineral wool, and insulating cement; discussion of
employee protection programs and staff training; case study in
developing an O&M plan (development, implementation process, and
problems that have been experienced).
(h) Regulatory review. Focusing on the OSHA Asbestos Construction
Standard found at 29 CFR 1926.58; the National Emission Standard for
Hazardous Air Pollutants (NESHAP) found at 40 CFR part 61, Subparts A
(General Provisions) and M (National Emission Standard for Asbestos);
EPA Worker Protection Rule found at 40 CFR part 763, Subpart G; TSCA
Title II; applicable State regulations.
(i) Recordkeeping for the management planner. Use of field
inspector's data sheet along with laboratory results; on-going
recordkeeping as a means to track asbestos disturbance; procedures for
recordkeeping. EPA recommends that States require the use of
standardized forms for purposes of management plans and incorporate the
use of such forms into the initial training course for management
planners.
(j) Assembling and submitting the management plan. Plan requirements
for schools in TSCA Title II section 203(i)(1); the management plan as a
planning tool.
(k) Financing abatement actions. Economic analysis and cost
estimates; development of cost estimates; present costs of abatement
versus future operation and maintenance costs; Asbestos School Hazard
Abatement Act grants and loans.
(l) Course review. A review of key aspects of the training course.
5. Project Designer
A person must be accredited as a project designer to design any of
the following activities with respect to friable ACBM in a school or
public and commercial building: (1) A response action other than a SSSD
maintenance activity, (2) a maintenance activity that disturbs friable
ACBM other than a SSSD maintenance activity, or (3) a response action
for a major fiber release episode. All persons seeking accreditation as
a project designer shall complete at least a minimum 3-day training
course as outlined below. The project designer course shall include
lectures, demonstrations, a field trip, course review and a written
examination.
EPA recommends the use of audiovisual materials to complement
lectures, where appropriate.
[[Page 796]]
The abatement project designer training course shall adequately
address the following topics:
(a) Background information on asbestos. Identification of asbestos;
examples and discussion of the uses and locations of asbestos in
buildings; physical appearance of asbestos.
(b) Potential health effects related to asbestos exposure. Nature of
asbestos-related diseases; routes of exposure; dose-response
relationships and the lack of a safe exposure level; the synergistic
effect between cigarette smoking and asbestos exposure; the latency
period of asbestos-related diseases; a discussion of the relationship
between asbestos exposure and asbestosis, lung cancer, mesothelioma, and
cancers of other organs.
(c) Overview of abatement construction projects. Abatement as a
portion of a renovation project; OSHA requirements for notification of
other contractors on a multi-employer site (29 CFR 1926.58).
(d) Safety system design specifications. Design, construction, and
maintenance of containment barriers and decontamination enclosure
systems; positioning of warning signs; electrical and ventilation system
lock-out; proper working techniques for minimizing fiber release; entry
and exit procedures for the work area; use of wet methods; proper
techniques for initial cleaning; use of negative-pressure exhaust
ventilation equipment; use of HEPA vacuums; proper clean-up and disposal
of asbestos; work practices as they apply to encapsulation, enclosure,
and repair; use of glove bags and a demonstration of glove bag use.
(e) Field trip. A visit to an abatement site or other suitable
building site, including on-site discussions of abatement design and
building walk-through inspection. Include discussion of rationale for
the concept of functional spaces during the walk-through.
(f) Employee personal protective equipment. Classes and
characteristics of respirator types; limitations of respirators; proper
selection, inspection; donning, use, maintenance, and storage procedures
for respirators; methods for field testing of the facepiece-to-face seal
(positive and negative-pressure fit checks); qualitative and
quantitative fit testing procedures; variability between field and
laboratory protection factors that alter respiratory fit (e.g., facial
hair); the components of a proper respiratory protection program;
selection and use of personal protective clothing; use, storage, and
handling of non-disposable clothing.
(g) Additional safety hazards. Hazards encountered during abatement
activities and how to deal with them, including electrical hazards, heat
stress, air contaminants other than asbestos, fire, and explosion
hazards.
(h) Fiber aerodynamics and control. Aerodynamic characteristics of
asbestos fibers; importance of proper containment barriers; settling
time for asbestos fibers; wet methods in abatement; aggressive air
monitoring following abatement; aggressive air movement and negative-
pressure exhaust ventilation as a clean-up method.
(i) Designing abatement solutions. Discussions of removal,
enclosure, and encapsulation methods; asbestos waste disposal.
(j) Final clearance process. Discussion of the need for a written
sampling rationale for aggressive final air clearance; requirements of a
complete visual inspection; and the relationship of the visual
inspection to final air clearance.
EPA recommends the use of TEM for analysis of final air clearance
samples. These samples should be analyzed by laboratories accredited
under the NIST NVLAP.
(k) Budgeting/cost estimating. Development of cost estimates;
present costs of abatement versus future operation and maintenance
costs; setting priorities for abatement jobs to reduce costs.
(l) Writing abatement specifications. Preparation of and need for a
written project design; means and methods specifications versus
performance specifications; design of abatement in occupied buildings;
modification of guide specifications for a particular building; worker
and building occupant health/medical considerations; replacement of ACM
with non-asbestos substitutes.
(m) Preparing abatement drawings. Significance and need for
drawings, use of as-built drawings as base drawings; use of inspection
photographs and on-site reports; methods of preparing abatement
drawings; diagramming containment barriers; relationship of drawings to
design specifications; particular problems related to abatement
drawings.
(n) Contract preparation and administration.
(o) Legal/liabilities/defenses. Insurance considerations; bonding;
hold-harmless clauses; use of abatement contractor's liability
insurance; claims made versus occurrence policies.
(p) Replacement. Replacement of asbestos with asbestos-free
substitutes.
(q) Role of other consultants. Development of technical
specification sections by industrial hygienists or engineers; the multi-
disciplinary team approach to abatement design.
(r) Occupied buildings. Special design procedures required in
occupied buildings; education of occupants; extra monitoring
recommendations; staging of work to minimize occupant exposure;
scheduling of renovation to minimize exposure.
(s) Relevant Federal, State, and local regulatory requirements,
procedures and standards, including, but not limited to:
(i) Requirements of TSCA Title II.
(ii) National Emission Standards for Hazardous Air Pollutants, (40
CFR part 61) subparts A (General Provisions) and M (National Emission
Standard for Asbestos).
[[Page 797]]
(iii) OSHA Respirator Standard found at 29 CFR 1910.134.
(iv) EPA Worker Protection Rule found at 40 CFR part 763, subpart G.
(v) OSHA Asbestos Construction Standard found at 29 CFR 1926.58.
(vi) OSHA Hazard Communication Standard found at 29 CFR 1926.59.
(t) Course review. A review of key aspects of the training course.
6. Project Monitor
EPA recommends that States adopt training and accreditation
requirements for persons seeking to perform work as project monitors.
Project monitors observe abatement activities performed by contractors
and generally serve as a building owner's representative to ensure that
abatement work is completed according to specification and in compliance
with all relevant statutes and regulations. They may also perform the
vital role of air monitoring for purposes of determining final
clearance. EPA recommends that a State seeking to accredit individuals
as project monitors consider adopting a minimum 5-day training course
covering the topics outlined below. The course outlined below consists
of lectures and demonstrations, at least 6 hours of hands-on training,
course review, and a written examination. The hands-on training
component might be satisfied by having the student simulate
participation in or performance of any of the relevant job functions or
activities (or by incorporation of the workshop component described in
item ``n'' below of this unit).
EPA recommends that the project monitor training course adequately
address the following topics:
(a) Roles and responsibilities of the project monitor. Definition
and responsibilities of the project monitor, including regulatory/
specification compliance monitoring, air monitoring, conducting visual
inspections, and final clearance monitoring.
(b) Characteristics of asbestos and asbestos-containing materials.
Typical uses of asbestos; physical appearance of asbestos; review of
asbestos abatement and control techniques; presentation of the health
effects of asbestos exposure, including routes of exposure, dose-
response relationships, and latency periods for asbestos-related
diseases.
(c) Federal asbestos regulations. Overview of pertinent EPA
regulations, including: NESHAP, 40 CFR part 61, subparts A and M; AHERA,
40 CFR part 763, subpart E; and the EPA Worker Protection Rule, 40 CFR
part 763, subpart G. Overview of pertinent OSHA regulations, including:
Construction Industry Standard for Asbestos, 29 CFR 1926.58; Respirator
Standard, 29 CFR 1910.134; and the Hazard Communication Standard, 29 CFR
1926.59. Applicable State and local asbestos regulations; regulatory
interrelationships.
(d) Understanding building construction and building systems.
Building construction basics, building physical plan layout;
understanding building systems (HVAC, electrical, etc.); layout and
organization, where asbestos is likely to be found on building systems;
renovations and the effect of asbestos abatement on building systems.
(e) Asbestos abatement contracts, specifications, and drawings.
Basic provisions of the contract; relationships between principle
parties, establishing chain of command; types of specifications,
including means and methods, performance, and proprietary and
nonproprietary; reading and interpreting records and abatement drawings;
discussion of change orders; common enforcement responsibilities and
authority of project monitor.
(f) Response actions and abatement practices. Pre-work inspections;
pre-work considerations, precleaning of the work area, removal of
furniture, fixtures, and equipment; shutdown/modification of building
systems; construction and maintenance of containment barriers, proper
demarcation of work areas; work area entry/exit, hygiene practices;
determining the effectiveness of air filtration equipment; techniques
for minimizing fiber release, wet methods, continuous cleaning;
abatement methods other than removal; abatement area clean-up
procedures; waste transport and disposal procedures; contingency
planning for emergency response.
(g) Asbestos abatement equipment. Typical equipment found on an
abatement project; air filtration devices, vacuum systems, negative
pressure differential monitoring; HEPA filtration units, theory of
filtration, design/construction of HEPA filtration units, qualitative
and quantitative performance of HEPA filtration units, sizing the
ventilation requirements, location of HEPA filtration units, qualitative
and quantitative tests of containment barrier integrity; best available
technology.
(h) Personal protective equipment. Proper selection of respiratory
protection; classes and characteristics of respirator types, limitations
of respirators; proper use of other safety equipment, protective
clothing selection, use, and proper handling, hard/bump hats, safety
shoes; breathing air systems, high pressure v. low pressure, testing for
Grade D air, determining proper backup air volumes.
(i) Air monitoring strategies. Sampling equipment, sampling pumps
(low v. high volume), flow regulating devices (critical and limiting
orifices), use of fibrous aerosol monitors on abatement projects;
sampling media, types of filters, types of cassettes, filter
orientation, storage and shipment of filters; calibration techniques,
primary calibration standards, secondary calibration standards,
temperature/pressure effects, frequency of calibration, recordkeeping
and
[[Page 798]]
field work documentation, calculations; air sample analysis, techniques
available and limitations of AHERA on their use, transmission electron
microscopy (background to sample preparation and analysis, air sample
conditions which prohibit analysis, EPA's recommended technique for
analysis of final air clearance samples), phase contrast microscopy
(background to sample preparation, and AHERA's limits on the use of
phase contrast microscopy), what each technique measures; analytical
methodologies, AHERA TEM protocol, NIOSH 7400, OSHA reference method
(non clearance), EPA recommendation for clearance (TEM); sampling
strategies for clearance monitoring, types of air samples (personal
breathing zone v. fixed-station area) sampling location and objectives
(pre-abatement, during abatement, and clearance monitoring), number of
samples to be collected, minimum and maximum air volumes, clearance
monitoring (post-visual-inspection) (number of samples required,
selection of sampling locations, period of sampling, aggressive
sampling, interpretations of sampling results, calculations), quality
assurance; special sampling problems, crawl spaces, acceptable samples
for laboratory analysis, sampling in occupied buildings (barrier
monitoring).
(j) Safety and health issues other than asbestos. Confined-space
entry, electrical hazards, fire and explosion concerns, ladders and
scaffolding, heat stress, air contaminants other than asbestos, fall
hazards, hazardous materials on abatement projects.
(k) Conducting visual inspections. Inspections during abatement,
visual inspections using the ASTM E1368 document; conducting inspections
for completeness of removal; discussion of ``how clean is clean?''
(l) Legal responsibilities and liabilities of project monitors.
Specification enforcement capabilities; regulatory enforcement;
licensing; powers delegated to project monitors through contract
documents.
(m) Recordkeeping and report writing. Developing project logs/daily
logs (what should be included, who sees them); final report preparation;
recordkeeping under Federal regulations.
(n) Workshops (6 hours spread over 3 days). Contracts,
specifications, and drawings: This workshop could consist of each
participant being issued a set of contracts, specifications, and
drawings and then being asked to answer questions and make
recommendations to a project architect, engineer or to the building
owner based on given conditions and these documents.
Air monitoring strategies/asbestos abatement equipment: This
workshop could consist of simulated abatement sites for which sampling
strategies would have to be developed (i.e., occupied buildings,
industrial situations). Through demonstrations and exhibition, the
project monitor may also be able to gain a better understanding of the
function of various pieces of equipment used on abatement projects (air
filtration units, water filtration units, negative pressure monitoring
devices, sampling pump calibration devices, etc.).
Conducting visual inspections: This workshop could consist, ideally,
of an interactive video in which a participant is ``taken through'' a
work area and asked to make notes of what is seen. A series of questions
will be asked which are designed to stimulate a person's recall of the
area. This workshop could consist of a series of two or three videos
with different site conditions and different degrees of cleanliness.
C. Examinations
1. Each State shall administer a closed book examination or
designate other entities such as State-approved providers of training
courses to administer the closed-book examination to persons seeking
accreditation who have completed an initial training course.
Demonstration testing may also be included as part of the examination. A
person seeking initial accreditation in a specific discipline must pass
the examination for that discipline in order to receive accreditation.
For example, a person seeking accreditation as an abatement project
designer must pass the State's examination for abatement project
designer.
States may develop their own examinations, have providers of
training courses develop examinations, or use standardized examinations
developed for purposes of accreditation under TSCA Title II. In
addition, States may supplement standardized examinations with questions
about State regulations. States may obtain commercially developed
standardized examinations, develop standardized examinations
independently, or do so in cooperation with other States, or with
commercial or non-profit providers on a regional or national basis. EPA
recommends the use of standardized, scientifically-validated testing
instruments, which may be beneficial in terms of both promoting
competency and in fostering accreditation reciprocity between States.
Each examination shall adequately cover the topics included in the
training course for that discipline. Each person who completes a
training course, passes the required examination, and fulfills whatever
other requirements the State imposes must receive an accreditation
certificate in a specific discipline. Whether a State directly issues
accreditation certificates, or authorizes training providers to issue
accreditation certificates, each certificate issued to an accredited
person must contain the following minimum information:
a. A unique certificate number
b. Name of accredited person
[[Page 799]]
c. Discipline of the training course completed.
d. Dates of the training course.
e. Date of the examination.
f. An expiration date of 1 year after the date upon which the person
successfully completed the course and examination.
g. The name, address, and telephone number of the training provider
that issued the certificate.
h. A statement that the person receiving the certificate has
completed the requisite training for asbestos accreditation under TSCA
Title II.
States or training providers who reaccredit persons based upon
completion of required refresher training must also provide
accreditation certificates with all of the above information, except the
examination date may be omitted if a State does not require a refresher
examination for reaccreditation.
Where a State licenses accredited persons but has authorized
training providers to issue accreditation certificates, the State may
issue licenses in the form of photo-identification cards. Where this
applies, EPA recommends that the State licenses should include all of
the same information required for the accreditation certificates. A
State may also choose to issue photo-identification cards in addition to
the required accreditation certificates.
Accredited persons must have their initial and current accreditation
certificates at the location where they are conducting work.
2. The following are the requirements for examination in each
discipline:
a. Worker:
i. 50 multiple-choice questions
ii. Passing score: 70 percent correct
b. Contractor/Supervisor:
i. 100 multiple-choice questions
ii. Passing score: 70 percent correct
c. Inspector:
i. 50 Multiple-choice questions
ii. Passing score: 70 percent correct
d. Management Planner:
i. 50 Multiple-choice questions
ii. Passing score: 70 percent correct
e. Project Designer:
i. 100 multiple-choice questions
ii. Passing score: 70 percent correct
D. Continuing Education
For all disciplines, a State's accreditation program shall include
annual refresher training as a requirement for reaccreditation as
indicated below:
1. Workers: One full day of refresher training.
2. Contractor/Supervisors: One full day of refresher training.
3. Inspectors: One half-day of refresher training.
4. Management Planners: One half-day of inspector refresher training
and one half-day of refresher training for management planners.
5. Project Designers: One full day of refresher training.
The refresher courses shall be specific to each discipline.
Refresher courses shall be conducted as separate and distinct courses
and not combined with any other training during the period of the
refresher course. For each discipline, the refresher course shall review
and discuss changes in Federal, State, and local regulations,
developments in state-of-the-art procedures, and a review of key aspects
of the initial training course as determined by the State. After
completing the annual refresher course, persons shall have their
accreditation extended for an additional year from the date of the
refresher course. A State may consider requiring persons to pass
reaccreditation examinations at specific intervals (for example, every 3
years).
EPA recommends that States formally establish a 12-month grace
period to enable formerly accredited persons with expired certificates
to complete refresher training and have their accreditation status
reinstated without having to re-take the initial training course.
E. Qualifications
In addition to requiring training and an examination, a State may
require candidates for accreditation to meet other qualification and/or
experience standards that the State considers appropriate for some or
all disciplines. States may choose to consider requiring qualifications
similar to the examples outlined below for inspectors, management
planners and project designers. States may modify these examples as
appropriate. In addition, States may want to include some requirements
based on experience in performing a task directly as a part of a job or
in an apprenticeship role. They may also wish to consider additional
criteria for the approval of training course instructors beyond those
prescribed by EPA.
1. Inspectors: Qualifications - possess a high school diploma.
States may want to require an Associate's Degree in specific fields
(e.g., environmental or physical sciences).
2. Management Planners: Qualifications - Registered architect,
engineer, or certified industrial hygienist or related scientific field.
3. Project Designers: Qualifications - registered architect,
engineer, or certified industrial hygienist.
4. Asbestos Training Course Instructor: Qualifications - academic
credentials and/or field experience in asbestos abatement.
EPA recommends that States prescribe minimum qualification standards
for training instructors employed by training providers.
[[Page 800]]
F. Recordkeeping Requirements for Training Providers
All approved providers of accredited asbestos training courses must
comply with the following minimum recordkeeping requirements.
1. Training course materials. A training provider must retain copies
of all instructional materials used in the delivery of the classroom
training such as student manuals, instructor notebooks and handouts.
2. Instructor qualifications. A training provider must retain copies
of all instructors' resumes, and the documents approving each instructor
issued by either EPA or a State. Instructors must be approved by either
EPA or a State before teaching courses for accreditation purposes. A
training provider must notify EPA or the State, as appropriate, in
advance whenever it changes course instructors. Records must accurately
identify the instructors that taught each particular course for each
date that a course is offered.
3. Examinations. A training provider must document that each person
who receives an accreditation certificate for an initial training course
has achieved a passing score on the examination. These records must
clearly indicate the date upon which the exam was administered, the
training course and discipline for which the exam was given, the name of
the person who proctored the exam, a copy of the exam, and the name and
test score of each person taking the exam. The topic and dates of the
training course must correspond to those listed on that person's
accreditation certificate. States may choose to apply these same
requirements to examinations for refresher training courses.
4. Accreditation certificates. The training providers or States,
whichever issues the accreditation certificate, shall maintain records
that document the names of all persons who have been awarded
certificates, their certificate numbers, the disciplines for which
accreditation was conferred, training and expiration dates, and the
training location. The training provider or State shall maintain the
records in a manner that allows verification by telephone of the
required information.
5. Verification of certificate information. EPA recommends that
training providers of refresher training courses confirm that their
students possess valid accreditation before granting course admission.
EPA further recommends that training providers offering the initial
management planner training course verify that students have met the
prerequisite of possessing valid inspector accreditation at the time of
course admission.
6. Records retention and access. (a) The training provider shall
maintain all required records for a minimum of 3 years. The training
provider, however, may find it advantageous to retain these records for
a longer period of time.
(b) The training provider must allow reasonable access to all of the
records required by the MAP, and to any other records which may be
required by States for the approval of asbestos training providers or
the accreditation of asbestos training courses, to both EPA and to State
Agencies, on request. EPA encourages training providers to make this
information equally accessible to the general public.
(c) If a training provider ceases to conduct training, the training
provider shall notify the approving government body (EPA or the State)
and give it the opportunity to take possession of that providers
asbestos training records.
G. Deaccreditation
1. States must establish criteria and procedures for deaccrediting
persons accredited as workers, contractor/supervisors, inspectors,
management planners, and project designers. States must follow their own
administrative procedures in pursuing deaccreditation actions. At a
minimum, the criteria shall include:
(a) Performing work requiring accreditation at a job site without
being in physical possession of initial and current accreditation
certificates;
(b) Permitting the duplication or use of one's own accreditation
certificate by another;
(c) Performing work for which accreditation has not been received;
or
(d) Obtaining accreditation from a training provider that does not
have approval to offer training for the particular discipline from
either EPA or from a State that has a contractor accreditation plan at
least as stringent as the EPA MAP.
EPA may directly pursue deaccreditation actions without reliance on
State deaccreditation or enforcement authority or actions. In addition
to the above-listed situations, the Administrator may suspend or revoke
the accreditation of persons who have been subject to a final order
imposing a civil penalty or convicted under section 16 of TSCA, 15
U.S.C. 2615 or 2647, for violations of 40 CFR part 763, or section 113
of the Clean Air Act, 42 U.S.C. 7413, for violations of 40 CFR part 61,
subpart M.
2. Any person who performs asbestos work requiring accreditation
under section 206(a) of TSCA, 15 U.S.C. 2646(a), without such
accreditation is in violation of TSCA. The following persons are not
accredited for purposes of section 206(a) of TSCA:
(a) Any person who obtains accreditation through fraudulent
representation of training or examination documents;
(b) Any person who obtains training documentation through fraudulent
means;
[[Page 801]]
(c) Any person who gains admission to and completes refresher
training through fraudulent representation of initial or previous
refresher training documentation; or
(d) Any person who obtains accreditation through fraudulent
representation of accreditation requirements such as education,
training, professional registration, or experience.
H. Reciprocity
EPA recommends that each State establish reciprocal arrangements
with other States that have established accreditation programs that meet
or exceed the requirements of the MAP. Such arrangements might address
cooperation in licensing determinations, the review and approval of
training programs and/or instructors, candidate testing and exam
administration, curriculum development, policy formulation, compliance
monitoring, and the exchange of information and data. The benefits to be
derived from these arrangements include a potential cost-savings from
the reduction of duplicative activity and the attainment of a more
professional accredited workforce as States are able to refine and
improve the effectiveness of their programs based upon the experience
and methods of other States.
II. EPA Approval Process for State Accreditation Programs
A. States may seek approval for a single discipline or all
disciplines as specified in the MAP. For example, a State that currently
only requires worker accreditation may receive EPA approval for that
discipline alone. EPA encourages States that currently do not have
accreditation requirements for all disciplines required under section
206(b)(2) of TSCA, 15 U.S.C. 2646(b)(2), to seek EPA approval for those
disciplines the State does accredit. As States establish accreditation
requirements for the remaining disciplines, the requested information
outlined below should be submitted to EPA as soon as possible. Any State
that had an accreditation program approved by EPA under an earlier
version of the MAP may follow the same procedures to obtain EPA approval
of their accreditation program under this MAP.
B. Partial approval of a State Program for the accreditation of one
or more disciplines does not mean that the State is in full compliance
with TSCA where the deadline for that State to have adopted a State Plan
no less stringent than the MAP has already passed. State Programs which
are at least as stringent as the MAP for one or more of the accredited
disciplines may, however, accredit persons in those disciplines only.
C. States seeking EPA approval or reapproval of accreditation
programs shall submit the following information to the Regional Asbestos
Coordinator at their EPA Regional office:
1. A copy of the legislation establishing or upgrading the State's
accreditation program (if applicable).
2. A copy of the State's accreditation regulations or revised
regulations.
3. A letter to the Regional Asbestos Coordinator that clearly
indicates how the State meets the program requirements of this MAP.
Addresses for each of the Regional Asbestos Coordinators are shown
below:
EPA, Region I, (ATC-111) Asbestos Coordinator, JFK Federal Bldg.,
Boston, MA 02203-2211, (617) 565-3836.
EPA, Region II, (MS-500), Asbestos Coordinator, 2890 Woodbridge Ave.,
Edison, NJ 08837-3679, (908) 321-6671.
EPA, Region III, (3AT-33), Asbestos Coordinator, 841 Chestnut Bldg.,
Philadelphia, PA 19107, (215) 597-3160.
EPA, Region IV, Asbestos Coordinator, 345 Courtland St., N.E., Atlanta,
GA 30365, (404) 347-5014.
EPA, Region V, (SP-14J), Asbestos Coordinator, 77 W. Jackson Blvd.,
Chicago, IL 60604-3590, (312) 886-6003.
EPA, Region VI, (6T-PT), Asbestos Coordinator, 1445 Ross Ave. Dallas, TX
75202-2744, (214) 655-7244.
EPA, Region VII, (ARTX/ASBS), Asbestos Coordinator, 726 Minnesota Ave.,
Kansas City, KS 66101, (913) 551-7020.
EPA, Region VIII, (8AT-TS), Asbestos Coordinator, 1 Denver Place, Suite
500 999 - 18th St., Denver, CO 80202-2405, (303) 293-1442.
EPA, Region IX, (A-4-4), Asbestos Coordinator, 75 Hawthorne St., San
Francisco, CA 94105, (415) 744-1128.
EPA, Region X, (AT-083), Asbestos Coordinator, 1200 Sixth Ave., Seattle,
WA 98101, (206) 553-4762.
EPA maintains a listing of all those States that have applied for
and received EPA approval for having accreditation requirements that are
at least as stringent as the MAP for one or more disciplines. Any
training courses approved by an EPA-approved State Program are
considered to be EPA-approved for purposes of accreditation.
III. Approval of Training Courses
Individuals or groups wishing to sponsor training courses for
disciplines required to be accredited under section 206(b)(1)(A) of
TSCA, 15 U.S.C. 2646(b)(1)(A), may apply for approval from States that
have accreditation program requirements that are at least as stringent
as this MAP. For a course to receive approval, it must meet the
requirements for the course as outlined in this MAP, and any other
requirements imposed by the State from which approval is being sought.
Courses that have been approved by a State with an accreditation program
at least as stringent as this MAP are approved under section 206(a) of
TSCA, 15 U.S.C.
[[Page 802]]
2646(a), for that particular State, and also for any other State that
does not have an accreditation program as stringent as this MAP.
A. Initial Training Course Approval
A training provider must submit the following minimum information to
a State as part of its application for the approval of each training
course:
1. The course provider's name, address, and telephone number.
2. A list of any other States that currently approve the training
course.
3. The course curriculum.
4. A letter from the provider of the training course that clearly
indicates how the course meets the MAP requirements for:
a. Length of training in days.
b. Amount and type of hands-on training.
c. Examination (length, format, and passing score).
d. Topics covered in the course.
5. A copy of all course materials (student manuals, instructor
notebooks, handouts, etc.).
6. A detailed statement about the development of the examination
used in the course.
7. Names and qualifications of all course instructors. Instructors
must have academic and/or field experience in asbestos abatement.
8. A description of and an example of the numbered certificates
issued to students who attend the course and pass the examination.
B. Refresher Training Course Approval
The following minimum information is required for approval of
refresher training courses by States:
1. The length of training in half-days or days.
2. The topics covered in the course.
3. A copy of all course materials (student manuals, instructor
notebooks, handouts, etc.).
4. The names and qualifications of all course instructors.
Instructors must have academic and/or field experience in asbestos
abatement.
5. A description of and an example of the numbered certificates
issued to students who complete the refresher course and pass the
examination, if required.
C. Withdrawal of Training Course Approval
States must establish criteria and procedures for suspending or
withdrawing approval from accredited training programs. States should
follow their own administrative procedures in pursuing actions for
suspension or withdrawal of approval of training programs. At a minimum,
the criteria shall include:
(1) Misrepresentation of the extent of a training course's approval
by a State or EPA;
(2) Failure to submit required information or notifications in a
timely manner;
(3) Failure to maintain requisite records;
(4) Falsification of accreditation records, instructor
qualifications, or other accreditation information; or
(5) Failure to adhere to the training standards and requirements of
the EPA MAP or State Accreditation Program, as appropriate.
In addition to the criteria listed above, EPA may also suspend or
withdraw a training course's approval where an approved training course
instructor, or other person with supervisory authority over the delivery
of training has been found in violation of other asbestos regulations
administered by EPA. An administrative or judicial finding of violation,
or execution of a consent agreement and order under 40 CFR 22.18,
constitutes evidence of a failure to comply with relevant statutes or
regulations. States may wish to adopt this criterion modified to include
their own asbestos statutes or regulations. EPA may also suspend or
withdraw approval of training programs where a training provider has
submitted false information as a part of the self-certification required
under Unit V.B. of the revised MAP.
Training course providers shall permit representatives of EPA or the
State which approved their training courses to attend, evaluate, and
monitor any training course without charge. EPA or State compliance
inspection staff are not required to give advance notice of their
inspections. EPA may suspend or withdraw State or EPA approval of a
training course based upon the criteria specified in this Unit III.C.
IV. EPA Procedures for Suspension or Revocation of Accreditation or
Training Course Approval.
A. If the Administrator decides to suspend or revoke the
accreditation of any person or suspend or withdraw the approval of a
training course, the Administrator will notify the affected entity of
the following:
1. The grounds upon which the suspension, revocation, or withdrawal
is based.
2. The time period during which the suspension, revocation, or
withdrawal is effective, whether permanent or otherwise.
3. The conditions, if any, under which the affected entity may
receive accreditation or approval in the future.
4. Any additional conditions which the Administrator may impose.
5. The opportunity to request a hearing prior to final Agency action
to suspend or revoke accreditation or suspend or withdraw approval.
[[Page 803]]
B. If a hearing is requested by the accredited person or training
course provider pursuant to the preceding paragraph, the Administrator
will:
1. Notify the affected entity of those assertions of law and fact
upon which the action to suspend, revoke, or withdraw is based.
2. Provide the affected entity an opportunity to offer written
statements of facts, explanations, comments, and arguments relevant to
the proposed action.
3. Provide the affected entity such other procedural opportunities
as the Administrator may deem appropriate to ensure a fair and impartial
hearing.
4. Appoint an EPA attorney as Presiding Officer to conduct the
hearing. No person shall serve as Presiding Officer if he or she has had
any prior connection with the specific case.
C. The Presiding Officer appointed pursuant to the preceding
paragraph shall:
1. Conduct a fair, orderly, and impartial hearing, without
unnecessary delay.
2. Consider all relevant evidence, explanation, comment, and
argument submitted pursuant to the preceding paragraph.
3. Promptly notify the affected entity of his or her decision and
order. Such an order is a final Agency action.
D. If the Administrator determines that the public health, interest,
or welfare warrants immediate action to suspend the accreditation of any
person or the approval of any training course provider, the
Administrator will:
1. Notify the affected entity of the grounds upon which the
emergency suspension is based;
2. Notify the affected entity of the time period during which the
emergency suspension is effective.
3. Notify the affected entity of the Administrator's intent to
suspend or revoke accreditation or suspend or withdraw training course
approval, as appropriate, in accordance with Unit IV.A. above. If such
suspension, revocation, or withdrawal notice has not previously been
issued, it will be issued at the same time the emergency suspension
notice is issued.
E. Any notice, decision, or order issued by the Administrator under
this section, and any documents filed by an accredited person or
approved training course provider in a hearing under this section, shall
be available to the public except as otherwise provided by section 14 of
TSCA or by 40 CFR part 2. Any such hearing at which oral testimony is
presented shall be open to the public, except that the Presiding Officer
may exclude the public to the extent necessary to allow presentation of
information which may be entitled to confidential treatment under
section 14 of TSCA or 40 CFR part 2.
V. Implementation Schedule
The various requirements of this MAP become effective in accordance
with the following schedules:
A. Requirements applicable to State Programs
1. Each State shall adopt an accreditation plan that is at least as
stringent as this MAP within 180 days after the commencement of the
first regular session of the legislature of the State that is convened
on or after April 4, 1994.
2. If a State has adopted an accreditation plan at least as
stringent as this MAP as of April 4, 1994, the State may continue to:
a. Conduct TSCA training pursuant to this MAP.
b. Approve training course providers to conduct training and to
issue accreditation that satisfies the requirements for TSCA
accreditation under this MAP.
c. Issue accreditation that satisfies the requirements for TSCA
accreditation under this MAP.
3. A State that had complied with an earlier version of the MAP, but
has not adopted an accreditation plan at least as stringent as this MAP
by April 4, 1994, may:
a. Conduct TSCA training which remains in compliance with the
requirements of Unit V.B. of this MAP. After such training has been
self-certified in accordance with Unit V.B. of this MAP, the State may
issue accreditation that satisfies the requirement for TSCA
accreditation under this MAP.
b. Sustain its approval for any training course providers to conduct
training and issue TSCA accreditation that the State had approved before
April 4, 1994, and that remain in compliance with Unit V.B. of this MAP.
c. Issue accreditation pursuant to an earlier version of the MAP
that provisionally satisfies the requirement for TSCA accreditation
until October 4, 1994.
Such a State may not approve new TSCA training course providers to
conduct training or to issue TSCA accreditation that satisfies the
requirements of this MAP until the State adopts an accreditation plan
that is at least as stringent as this MAP.
4. A State that had complied with an earlier version of the MAP, but
fails to adopt a plan as stringent as this MAP by the deadline
established in Unit V.A.1., is subject to the following after that
deadline date:
a. The State loses any status it may have held as an EPA-approved
State for accreditation purposes under section 206 of TSCA, 15 U.S.C.
2646.
b. All training course providers approved by the State lose State
approval to conduct training and issue accreditation that satisfies the
requirements for TSCA accreditation under this MAP.
[[Page 804]]
c. The State may not:
i. Conduct training for accreditation purposes under section 206 of
TSCA, 15 U.S.C. 2646.
ii. Approve training course providers to conduct training or issue
accreditation that satisfies the requirements for TSCA accreditation; or
iii. Issue accreditation that satisfies the requirement for TSCA
accreditation.
EPA will extend EPA-approval to any training course provider that
loses State approval because the State does not comply with the
deadline, so long as the provider is in compliance with Unit V.B. of
this MAP, and the provider is approved by a State that had complied with
an earlier version of the MAP as of the day before the State loses its
EPA approval.
5. A State that does not have an accreditation program that
satisfies the requirements for TSCA accreditation under either an
earlier version of the MAP or this MAP, may not:
a. Conduct training for accreditation purposes under section 206 of
TSCA, 15 U.S.C. 2646;
b. Approve training course providers to conduct training or issue
accreditation that satisfies the requirements for TSCA accreditation; or
c. Issue accreditation that satisfies the requirement for TSCA
accreditation.
B. Requirements applicable to Training Courses and Providers
As of October 4, 1994, an approved training provider must certify to
EPA and to any State that has approved the provider for TSCA
accreditation, that each of the provider's training courses complies
with the requirements of this MAP. The written submission must document
in specific detail the changes made to each training course in order to
comply with the requirements of this MAP and clearly state that the
provider is also in compliance with all other requirements of this MAP,
including the new recordkeeping and certificate provisions. Each
submission must include the following statement signed by an authorized
representative of the training provider: ``Under civil and criminal
penalties of law for the making or submission of false or fraudulent
statements or representations (18 U.S.C. 1001 and 15 U.S.C. 2615), I
certify that the training described in this submission complies with all
applicable requirements of Title II of TSCA, 40 CFR part 763, Appendix C
to Subpart E, as revised, and any other applicable Federal, state, or
local requirements.'' A consolidated self-certification submission from
each training provider that addresses all of its approved training
courses is permissible and encouraged.
The self-certification must be sent via registered mail, to EPA
Headquarters at the following address: Attn. Self-Certification Program,
Field Programs Branch, Chemical Management Division (7404), Office of
Pollution Prevention and Toxics, Environmental Protection Agency, 1200
Pennsylvania Ave., NW., Washington, DC 20460. A duplicate copy of the
complete submission must also be sent to any States from which approval
had been obtained.
The timely receipt of a complete self-certification by EPA and all
approving States shall have the effect of extending approval under this
MAP to the training courses offered by the submitting provider. If a
self-certification is not received by the approving government bodies on
or before the due date, the affected training course is not approved
under this MAP. Such training providers must then reapply for approval
of these training courses pursuant to the procedures outlined in Unit
III.
C. Requirements applicable to Accredited Persons.
Persons accredited by a State with an accreditation program no less
stringent than an earlier version of the MAP or by an EPA-approved
training provider as of April 3, 1994, are accredited in accordance with
the requirements of this MAP, and are not required to retake initial
training. They must continue to comply with the requirements for annual
refresher training in Unit I.D. of the revised MAP.
D. Requirements applicable to Non-Accredited Persons.
In order to perform work requiring accreditation under TSCA Title
II, persons who are not accredited by a State with an accreditation
program no less stringent than an earlier version of the MAP or by an
EPA-approved training provider as of April 3, 1994, must comply with the
upgraded training requirements of this MAP by no later than October 4,
1994. Non-accredited persons may obtain initial accreditation on a
provisional basis by successfully completing any of the training
programs approved under an earlier version of the MAP, and thereby
perform work during the first 6 months after this MAP takes effect.
However, by October 4, 1994, these persons must have successfully
completed an upgraded training program that fully complies with the
requirements of this MAP in order to continue to perform work requiring
accreditation under section 206 of TSCA, 15 U.S.C. 2646.
[59 FR 5251, Feb. 3, 1994, as amended at 60 FR 31922, June 19, 1995]
[[Page 805]]
Appendix D to Subpart E of Part 763--Transport and Disposal of Asbestos
Waste
For the purposes of this appendix, transport is defined as all
activities from receipt of the containerized asbestos waste at the
generation site until it has been unloaded at the disposal site. Current
EPA regulations state that there must be no visible emissions to the
outside air during waste transport. However, recognizing the potential
hazards and subsequent liabilities associated with exposure, the
following additional precautions are recommended.
Recordkeeping. Before accepting wastes, a transporter should
determine if the waste is properly wetted and containerized. The
transporter should then require a chain-of-custody form signed by the
generator. A chain-of-custody form may include the name and address of
the generator, the name and address of the pickup site, the estimated
quantity of asbestos waste, types of containers used, and the
destination of the waste. The chain-of-custody form should then be
signed over to a disposal site operator to transfer responsibility for
the asbestos waste. A copy of the form signed by the disposal site
operator should be maintained by the transporter as evidence of receipt
at the disposal site.
Waste handling. A transporter should ensure that the asbestos waste
is properly contained in leak-tight containers with appropriate labels,
and that the outside surfaces of the containers are not contaminated
with asbestos debris adhering to the containers. If there is reason to
believe that the condition of the asbestos waste may allow significant
fiber release, the transporter should not accept the waste. Improper
containerization of wastes is a violation of the NESHAPs regulation and
should be reported to the appropriate EPA Regional Asbestos NESHAPs
contact below:
Region I
Asbestos NESHAPs Contact, Air Management Division, USEPA, Region I,
JFK Federal Building, Boston, MA 02203, (617) 223-3266.
Region II
Asbestos NESHAPs Contact, Air & Waste Management Division, USEPA,
Region II, 26 Federal Plaza, New York, NY 10007, (212) 264-6770.
Region III
Asbestos NESHAPs Contact, Air Management Division, USEPA, Region
III, 841 Chestnut Street, Philadelphia, PA 19107, (215) 597-9325.
Region IV
Asbestos NESHAPs Contact, Air, Pesticide & Toxic Management, USEPA,
Region IV, 345 Courtland Street, NE., Atlanta, GA 30365, (404) 347-4298.
Region V
Asbestos NESHAPs Contact, Air Management Division, USEPA, Region V,
77 West Jackson Boulevard, Chicago, IL 60604, (312) 353-6793.
Region VI
Asbestos NESHAPs Contact, Air & Waste Management Division, USEPA,
Region VI, 1445 Ross Avenue, Dallas, TX 75202, (214) 655-7229.
Region VII
Asbestos NESHAPs Contact, Air & Waste Management Division, USEPA,
Region VII, 726 Minnesota Avenue, Kansas City, KS 66101, (913) 236-2896.
Region VIII
Asbestos NESHAPs Contact, Air & Waste Management Division, USEPA,
Region VIII, 999 18th Street, Suite 500, Denver, CO 80202, (303) 293-
1814.
Region IX
Asbestos NESHAPs Contact, Air Management Division, USEPA, Region IX,
215 Fremont Street, San Francisco, CA 94105, (415) 974-7633.
Region X
Asbestos NESHAPs Contact, Air & Toxics Management Division, USEPA,
Region X, 1200 Sixth Avenue, Seattle, WA 98101, (206) 442-2724.
Once the transporter is satisfied with the condition of the asbestos
waste and agrees to handle it, the containers should be loaded into the
transport vehicle in a careful manner to prevent breaking of the
containers. Similarly, at the disposal site, the asbestos waste
containers should be transferred carefully to avoid fiber release.
Waste transport. Although there are no regulatory specifications
regarding the transport vehicle, it is recommended that vehicles used
for transport of containerized asbestos waste have an enclosed carrying
compartment or utilize a canvas covering sufficient to contain the
transported waste, prevent damage to containers, and prevent fiber
release. Transport of large quantities of asbestos waste is commonly
conducted in a 20-cubic-yard ``roll off'' box, which should also be
covered. Vehicles that use compactors to reduce waste volume should not
be used because these will cause the waste containers to rupture. Vacuum
trucks used to transport
[[Page 806]]
waste slurry must be inspected to ensure that water is not leaking from
the truck.
Disposal involves the isolation of asbestos waste material in order
to prevent fiber release to air or water. Landfilling is recommended as
an environmentally sound isolation method because asbestos fibers are
virtually immobile in soil. Other disposal techniques such as
incineration or chemical treatment are not feasible due to the unique
properties of asbestos. EPA has established asbestos disposal
requirements for active and inactive disposal sites under NESHAPs (40
CFR Part 61, subpart M) and specifies general requirements for solid
waste disposal under RCRA (40 CFR Part 257). Advance EPA notification of
the intended disposal site is required by NESHAPs.
Selecting a disposal facility. An acceptable disposal facility for
asbestos wastes must adhere to EPA's requirements of no visible
emissions to the air during disposal, or minimizing emissions by
covering the waste within 24 hours. The minimum required cover is 6
inches of nonasbestos material, normally soil, or a dust-suppressing
chemical. In addition to these Federal requirements, many state or local
government agencies require more stringent handling procedures. These
agencies usually supply a list of ``approved'' or licensed asbestos
disposal sites upon request. Solid waste control agencies are listed in
local telephone directories under state, county, or city headings. A
list of state solid waste agencies may be obtained by calling the RCRA
hotline: 1-800-424-9346 (382-3000 in Washington, DC). Some landfill
owners or operators place special requirements on asbestos waste, such
as placing all bagged waste into 55-gallon metal drums. Therefore,
asbestos removal contractors should contact the intended landfill before
arriving with the waste.
Receiving asbestos waste. A landfill approved for receipt of
asbestos waste should require notification by the waste hauler that the
load contains asbestos. The landfill operator should inspect the loads
to verify that asbestos waste is properly contained in leak-tight
containers and labeled appropriately. The appropriate EPA Regional
Asbestos NESHAPs Contact should be notified if the landfill operator
believes that the asbestos waste is in a condition that may cause
significant fiber release during disposal. In situations when the wastes
are not properly containerized, the landfill operator should thoroughly
soak the asbestos with a water spray prior to unloading, rinse out the
truck, and immediately cover the wastes with nonasbestos material prior
to compacting the waste in the landfill.
Waste deposition and covering. Recognizing the health dangers
associated with asbestos exposure, the following procedures are
recommended to augment current federal requirements:
Designate a separate area for asbestos waste
disposal. Provide a record for future landowners that asbestos waste has
been buried there and that it would be hazardous to attempt to excavate
that area. (Future regulations may require property deeds to identify
the location of any asbestos wastes and warn against excavation.)
Prepare a separate trench to receive asbestos
wastes. The size of the trench will depend upon the quantity and
frequency of asbestos waste delivered to the disposal site. The
trenching technique allows application of soil cover without disturbing
the asbestos waste containers. The trench should be ramped to allow the
transport vehicle to back into it, and the trench should be as narrow as
possible to reduce the amount of cover required. If possible, the trench
should be aligned perpendicular to prevailing winds.
Place the asbestos waste containers into the
trench carefully to avoid breaking them. Be particularly careful with
plastic bags because when they break under pressure asbestos particles
can be emitted.
Completely cover the containerized waste within
24 hours with a minimum of 6 inches of nonasbestos material. Improperly
containerized waste is a violation of the NESHAPs and EPA should be
notified.
However, if improperly containerized waste is received at the
disposal site, it should be covered immediately after unloading. Only
after the wastes, including properly containerized wastes, are
completely covered, can the wastes be compacted or other heavy equipment
run over it. During compacting, avoid exposing wastes to the air or
tracking asbestos material away from the trench.
For final closure of an area containing asbestos
waste, cover with at least an additional 30 inches of compacted
nonasbestos material to provide a 36-inch final cover. To control
erosion of the final cover, it should be properly graded and vegetated.
In areas of the United States where excessive soil erosion may occur or
the frost line exceeds 3 feet, additional final cover is recommended. In
desert areas where vegetation would be difficult to maintain, 3-6 inches
of well graded crushed rock is recommended for placement on top of the
final cover.
Controlling public access. Under the current NESHAPs regulation, EPA
does not require that a landfill used for asbestos disposal use warning
signs or fencing if it meets the requirement to cover asbestos wastes.
However, under RCRA, EPA requires that access be controlled to prevent
exposure of the public to potential health and safety hazards at the
disposal site. Therefore, for liability protection of operators of
landfills that handle asbestos, fencing and warning signs are
recommended to control public access when natural barriers do not exist.
Access to a
[[Page 807]]
landfill should be limited to one or two entrances with gates that can
be locked when left unattended. Fencing should be installed around the
perimeter of the disposal site in a manner adequate to deter access by
the general public. Chain-link fencing, 6-ft high and topped with a
barbed wire guard, should be used. More specific fencing requirements
may be specified by local regulations. Warning signs should be displayed
at all entrances and at intervals of 330 feet or less along the property
line of the landfill or perimeter of the sections where asbestos waste
is deposited. The sign should read as follows:
ASBESTOS WASTE DISPOSAL SITE
BREATHING ASBESTOS DUST MAY CAUSE LUNG DISEASE AND CANCER
Recordkeeping. For protection from liability, and considering
possible future requirements for notification on disposal site deeds, a
landfill owner should maintain documentation of the specific location
and quantity of the buried asbestos wastes. In addition, the estimated
depth of the waste below the surface should be recorded whenever a
landfill section is closed. As mentioned previously, such information
should be recorded in the land deed or other record along with a notice
warning against excavation of the area.
[52 FR 41897, Oct. 30, 1987, as amended at 62 FR 1834, Jan. 14, 1997]
Appendix E to Subpart E of Part 763--Interim Method of the Determination
of Asbestos in Bulk Insulation Samples
Section 1, Polarized Light Microscopy
1.1 Principle and Applicability
Bulk samples of building materials taken for asbestos identification
are first examined for homogeneity and preliminary fiber identification
at low magnification. Positive identification of suspect fibers is made
by analysis of subsamples with the polarized light microscope.
The principles of optical mineralogy are well established.\1\ \2\ A
light microscope equipped with two polarizing filters is used to observe
specific optical characteristics of a sample. The use of plane polarized
light allows the determination of refractive indices along specific
crystallographic axes. Morphology and color are also observed. A
retardation plate is placed in the polarized light path for
determination of the sign of elongation using orthoscopic illumination.
Orientation of the two filters such that their vibration planes are
perpendicular (crossed polars) allows observation of the birefringence
and extinction characteristics of anisotropic particles.
Quantitative analysis involves the use of point counting. Point
counting is a standard technique in petrography for determining the
relative areas occupied by separate minerals in thin sections of rock.
Background information on the use of point counting \2\ and the
interpretation of point count data \3\ is available.
This method is applicable to all bulk samples of friable insulation
materials submitted for identification and quantitation of asbestos
components.
1.2 Range
The point counting method may be used for analysis of samples
containing from 0 to 100 percent asbestos. The upper detection limit is
100 percent. The lower detection limit is less than 1 percent.
1.3 Interferences
Fibrous organic and inorganic constituents of bulk samples may
interfere with the identification and quantitation of the asbestos
mineral content. Spray-on binder materials may coat fibers and affect
color or obscure optical characteristics to the extent of masking fiber
identity. Fine particles of other materials may also adhere to fibers to
an extent sufficient to cause confusion in identification. Procedures
that may be used for the removal of interferences are presented in
Section 1.7.2.2.
1.4 Precision and Accuracy
Adequate data for measuring the accuracy and precision of the method
for samples with various matrices are not currently available. Data
obtained for samples containing a single asbestos type in a simple
matrix are available in the EPA report Bulk Sample Analysis for Asbestos
Content: Evaluation of the Tentative Method.\4\
1.5 Apparatus
1.5.1 Sample Analysis
A low-power binocular microscope, preferably stereoscopic, is used
to examine the bulk insulation sample as received.
Microscope: binocular, 10-45X (approximate).
Light Source: incandescent or fluorescent.
Forceps, Dissecting Needles, and Probes
Glassine Paper or Clean Glass Plate
Compound microscope requirements: A polarized light microscope
complete with polarizer, analyzer, port for wave retardation plate,
360[deg] graduated rotating stage, substage condenser, lamp, and lamp
iris.
Polarized Light Microscope: described above.
Objective Lenses: 10X, 20X, and 40X or near
equivalent.
Dispersion Staining Objective Lens (optional)
Ocular Lens: 10X minimum.
Eyepiece Reticle: cross hair or 25 point Chalkley
Point Array.
[[Page 808]]
Compensator Plate: 550 millimicron retardation.
1.5.2 Sample Preparation
Sample preparation apparatus requirements will depend upon the type
of insulation sample under consideration. Various physical and/or
chemical means may be employed for an adequate sample assessment.
Ventilated Hood or negative pressure glove box.
Microscope Slides
Coverslips
Mortar and Pestle: agate or porcelain. (optional)
Wylie Mill (optional)
Beakers and Assorted Glassware (optional)
Certrifuge (optional)
Filtration apparatus (optional)
Low temperature asher (optional)
1.6 Reagents
1.6.1 Sample Preparation
Distilled Water (optional)
Dilute CH3COOH: ACS reagent grade (optional)
Dilute HCl: ACS reagent grade (optional)
Sodium metaphosphate (NaPO3)6
(optional)
1.6.2 Analytical Reagents
Refractive Index Liquids: 1.490-1.570, 1.590-1.720 in increments of
0.002 or 0.004.
Refractive Index Liquids for Dispersion Staining:
high-dispersion series, 1.550, 1.605, 1.630 (optional).
UICC Asbestos Reference Sample Set: Available from:
UICC MRC Pneumoconiosis Unit, Llandough Hospital, Penarth, Glamorgan CF6
1XW, UK, and commercial distributors.
Tremolite-asbestos (source to be determined)
Actinolite-asbestos (source to be determined)
1.7 Procedures
Note: Exposure to airborne asbestos fibers is a health hazard. Bulk
samples submitted for analysis are usually friable and may release
fibers during handling or matrix reduction steps. All sample and slide
preparations should be carried out in a ventilated hood or glove box
with continuous airflow (negative pressure). Handling of samples without
these precautions may result in exposure of the analyst and
contamination of samples by airborne fibers.
1.7.1 Sampling
Samples for analysis of asbestos content shall be taken in the
manner prescribed in Reference 5 and information on design of sampling
and analysis programs may be found in Reference 6. If there are any
questions about the representative nature of the sample, another sample
should be requested before proceeding with the analysis.
1.7.2 Analysis
1.7.2.1 Gross Examination
Bulk samples of building materials taken for the identification and
quantitation of asbestos are first examined for homogeneity at low
magnification with the aid of a stereomicroscope. The core sample may be
examined in its container or carefully removed from the container onto a
glassine transfer paper or clean glass plate. If possible, note is made
of the top and bottom orientation. When discrete strata are identified,
each is treated as a separate material so that fibers are first
identified and quantified in that layer only, and then the results for
each layer are combined to yield an estimate of asbestos content for the
whole sample.
1.7.2.2 Sample Preparation
Bulk materials submitted for asbestos analysis involve a wide
variety of matrix materials. Representative subsamples may not be
readily obtainable by simple means in heterogeneous materials, and
various steps may be required to alleviate the difficulties encountered.
In most cases, however, the best preparation is made by using forceps to
sample at several places from the bulk material. Forcep samples are
immersed in a refractive index liquid on a microscope slide, teased
apart, covered with a cover glass, and observed with the polarized light
microscope.
Alternatively, attempts may be made to homogenize the sample or
eliminate interferences before further characterization. The selection
of appropriate procedures is dependent upon the samples encountered and
personal preference. The following are presented as possible sample
preparation steps.
A mortar and pestle can sometimes be used in the size reduction of
soft or loosely bound materials though this may cause matting of some
samples. Such samples may be reduced in a Wylie mill. Apparatus should
be clean and extreme care exercised to avoid cross-contamination of
samples. Periodic checks of the particle sizes should be made during the
grinding operation so as to preserve any fiber bundles present in an
identifiable form. These procedures are not recommended for samples that
contain amphibole minerals or vermiculite. Grinding of amphiboles may
result in the separation of fiber bundles or the production of cleavage
fragments with aspect ratios greater than 3:1. Grinding of vermiculite
may also produce fragments with aspect ratios greater than 3:1.
Acid treatment may occasionally be required to eliminate
interferences. Calcium carbonate, gypsum, and bassanite (plaster) are
frequently present in sprayed or trowelled insulations. These materials
may be removed by treatment with warm dilute acetic acid. Warm dilute
hydrochloric acid
[[Page 809]]
may also be used to remove the above materials. If acid treatment is
required, wash the sample at least twice with distilled water, being
careful not to lose the particulates during decanting steps.
Centrifugation or filtration of the suspension will prevent significant
fiber loss. The pore size of the filter should be 0.45 micron or less.
Caution: prolonged acid contact with the sample may alter the optical
characteristics of chrysotile fibers and should be avoided.
Coatings and binding materials adhering to fiber surfaces may also
be removed by treatment with sodium metaphosphate.\7\ Add 10 mL of 10g/L
sodium metaphosphate solution to a small (0.1 to 0.5 mL) sample of bulk
material in a 15-mL glass centrifuge tube. For approximately 15 seconds
each, stir the mixture on a vortex mixer, place in an ultrasonic bath
and then shake by hand. Repeat the series. Collect the dispersed solids
by centrifugation at 1000 rpm for 5 minutes. Wash the sample three times
by suspending in 10 mL distilled water and recentrifuging. After
washing, resuspend the pellet in 5 mL distilled water, place a drop of
the suspension on a microscope slide, and dry the slide at 110 [deg]C.
In samples with a large portion of cellulosic or other organic
fibers, it may be useful to ash part of the sample and view the residue.
Ashing should be performed in a low temperature asher. Ashing may also
be performed in a muffle furnace at temperatures of 500 [deg]C or lower.
Temperatures of 550 [deg]C or higher will cause dehydroxylation of the
asbestos minerals, resulting in changes of the refractive index and
other key parameters. If a muffle furnace is to be used, the furnace
thermostat should be checked and calibrated to ensure that samples will
not be heated at temperatures greater than 550 [deg]C.
Ashing and acid treatment of samples should not be used as standard
procedures. In order to monitor possible changes in fiber
characteristics, the material should be viewed microscopically before
and after any sample preparation procedure. Use of these procedures on
samples to be used for quantitation requires a correction for percent
weight loss.
1.7.2.3 Fiber Identification
Positive identification of asbestos requires the determination of
the following optical properties.
Morphology
Color and pleochroism
Refractive indices
Birefringence
Extinction characteristics
Sign of elongation
Table 1-1 lists the above properties for commercial asbestos fibers.
Figure 1-1 presents a flow diagram of the examination procedure. Natural
variations in the conditions under which deposits of asbestiform
minerals are formed will occasionally produce exceptions to the
published values and differences from the UICC standards. The sign of
elongation is determined by use of the compensator plate and crossed
polars. Refractive indices may be determined by the Becke line test.
Alternatively, dispersion staining may be used. Inexperienced operators
may find that the dispersion staining technique is more easily learned,
and should consult Reference 9 for guidance. Central stop dispersion
staining colors are presented in Table 1-2. Available high-dispersion
(HD) liquids should be used.
Table 1-1--Optical Properties of Asbestoc Fibers
----------------------------------------------------------------------------------------------------------------
Refrac- tive indices \b\
Mineral Morphology, color ----------------------------- Birefring- Extinction Sign of
\a\ [alpha] [gamma] ence elonation
----------------------------------------------------------------------------------------------------------------
Chrysotile Wavy fibers. Fiber 1.493-1.560 1.517-1.562\f\ .008 [verbar] to +
(asbestiform bundles have (normally fiber length. (length
serpentine). splayed ends and 1.556). slow)
``kinks''. Aspect
ratio typically
10:1.
Colorless \3\,
nonpleochroic.
Amosite Straight, rigid 1.635-1.696 1.655-1.729 .020-.033 [verbar] to +
(asbestiform fibers. Aspect \f\ (normally fiber length. (length
grunerite). ratio typically 1.696-1.710. slow)
10:1.
Colorless to
brown,
nonpleochroic or
weakly so. Opaque
inclusions may be
present.
Crocidolite Straight, rigid 1.654-1.701 1.668-1.717\3e .014-.016 [verbar] to -
(asbestiform fibers. Thick \ (normally fiber length. (length
Riebeckite). fibers and bundles close to fast)
common, blue to 1.700).
purple-blue in
color. Pleochroic.
Birefringence is
generally masked
by blue color.
Antho- phyllite- Straight fibers and 1.596-1.652 1.615-1.676 .019-.024 [verbar] to +
asbestos. acicular cleavage \f\. fiber length. (length
fragments.\d\ Some slow)
composite fibers.
Aspect ratio
<10:1. Colorless
to light brown.
[[Page 810]]
Tremolite- Normally present as 1.599-1.668 1.622-1.688 .023-.020 Oblique +
actinolite- acicular or \f\. extinction, (length
asbestos. prismatic cleavage 10-20[deg] slow)
fragments.\d\ for
Single crystals fragments.
predominate, Composite
aspect ratio fibers
<10:1. Colorless show[hairsp][
to pale green. verbar]
extinction.
----------------------------------------------------------------------------------------------------------------
\a\ From reference 5; colors cited are seen by observation with plane polarized light.
\b\ From references 5 and 8.
\c\ Fibers subjected to heating may be brownish.
\d\ Fibers defined as having aspect ratio 3:1.
\e\ to fiber length.
\f\ [verbar]To fiber length.
[[Page 811]]
[GRAPHIC] [TIFF OMITTED] TC01AP92.017
[[Page 812]]
Table 1-2--Central Stop Dispersion Staining Colors \a\
----------------------------------------------------------------------------------------------------------------
Mineral RI Liquid [eta] [eta][verbar]
----------------------------------------------------------------------------------------------------------------
Chrysotile.............................. 1.550 \HD\ Blue...................... Blue-magenta
Amosite................................. 1.680 Blue-magenta to pale blue. Golden-yellow
1.550\HD\ Yellow to white........... Yellow to white
Crocidolite \b\......................... 1.700 Red magenta............... Blue-magenta
1.550\HD\ Yellow to white........... Yellow to white
Anthophyllite........................... 1.605\HD\ Blue...................... Gold to gold-magenta
Tremolite............................... 1.605\HD c\ Pale blue................. Gold
Actinolite.............................. 1.605\HD\ Gold-magenta to blue...... Gold
1.630\HD c\ Magenta................... Golden-yellow
----------------------------------------------------------------------------------------------------------------
\a\ From reference 9.
\b\ Blue absorption color.
\c\ Oblique extinction view.
1.7.2.4 Quantitation of Asbestos Content
Asbestos quantitation is performed by a point-counting procedure or
an equivalent estimation method. An ocular reticle (cross-hair or point
array) is used to visually superimpose a point or points on the
microscope field of view. Record the number of points positioned
directly above each kind of particle or fiber of interest. Score only
points directly over asbestos fibers or nonasbestos matrix material. Do
not score empty points for the closest particle. If an asbestos fiber
and a matrix particle overlap so that a point is superimposed on their
visual intersection, a point is scored for both categories. Point
counting provides a determination of the area percent asbestos. Reliable
conversion of area percent to percent of dry weight is not currently
feasible unless the specific gravities and relative volumes of the
materials are known.
For the purpose of this method, ``asbestos fibers'' are defined as
having an aspect ratio greater than 3:1 and being positively identified
as one of the minerals in Table 1-1.
A total of 400 points superimposed on either asbestos fibers or
nonasbestos matrix material must be counted over at least eight
different preparations of representative subsamples. Take eight forcep
samples and mount each separately with the appropriate refractive index
liquid. The preparation should not be heavily loaded. The sample should
be uniformly dispersed to avoid overlapping particles and allow 25-50
percent empty area within the fields of view. Count 50 nonempty points
on each preparation, using either
A cross-hair reticle and mechanical stage; or
A reticle with 25 points (Chalkley Point Array) and
counting at least 2 randomly selected fields.
For samples with mixtures of isotropic and anisotropic materials
present, viewing the sample with slightly uncrossed polars or the
addition of the compensator plate to the polarized light path will allow
simultaneous discrimination of both particle types. Quantitation should
be performed at 100X or at the lowest magnification of the polarized
light microscope that can effectively distinguish the sample components.
Confirmation of the quantitation result by a second analyst on some
percentage of analyzed samples should be used as standard quality
control procedure.
The percent asbestos is calculated as follows:
% asbestos=(a/n) 100%
where
a=number of asbestos counts,
n=number of nonempty points counted (400).
If a=0, report ``No asbestos detected.'' If 0< a[lE]3, report ``<1%
asbestos''.
The value reported should be rounded to the nearest percent.
1.8 References
1. Paul F. Kerr, Optical Mineralogy, 4th ed., New York, McGraw-Hill,
1977.
2. E. M. Chamot and C. W. Mason, Handbook of Chemical Microscopy,
Volume One, 3rd ed., New York: John Wiley & Sons, 1958.
3. F. Chayes, Petrographic Modal Analysis: An Elementary Statistical
Appraisal, New York: John Wiley & Sons, 1956.
4. E. P. Brantly, Jr., K. W. Gold, L. E. Myers, and D. E. Lentzen,
Bulk Sample Analysis for Asbestos Content: Evaluation of the Tentative
Method, U.S. Environmental Protection Agency, October 1981.
5. U.S. Environmental Protection Agency, Asbestos-Containing
Materials in School Buildings: A Guidance Document, Parts 1 and 2, EPA/
OPPT No. C00090, March 1979.
6. D. Lucas, T. Hartwell, and A. V. Rao, Asbestos-Containing
Materials in School Buildings: Guidance for Asbestos Analytical
Programs, EPA 560/13-80-017A, U.S. Environmental Protection Agency,
December 1980, 96 pp.
7. D. H. Taylor and J. S. Bloom, Hexametaphosphate pretreatment of
insulation samples for identification of fibrous constituents,
Microscope, 28, 1980.
8. W. J. Campbell, R. L. Blake, L. L. Brown, E. E. Cather, and J. J.
Sjoberg. Selected Silicate Minerals and Their Asbestiform Varieties:
Mineralogical Definitions and Identification-Characterization, U.S.
Bureau of Mines Information Circular 8751, 1977.
9. Walter C. McCrone, Asbestos Particle Atlas, Ann Arbor: Ann Arbor
Science Publishers, June 1980.
[[Page 813]]
Section 2, X-Ray Powder Diffraction
2.1 Principle and Applicability
The principle of X-ray powder diffraction (XRD) analysis is well
established.\1 2\ Any solid, crystalline material will diffract an
impingent beam of parallel, monochromatic X-rays whenever Bragg's Law,
[lambda] = 2d sin [thetas],
is satisfied for a particular set of planes in the crystal lattice,
where
[lambda] = the X-ray wavelength, A;
d = the interplanar spacing of the set of reflecting lattice planes, A;
and
[thetas] = the angle of incidence between the X-ray beam and the
reflecting lattice planes.
By appropriate orientation of a sample relative to the incident X-ray
beam, a diffraction pattern can be generated that, in most cases, will
be uniquely characteristic of both the chemical composition and
structure of the crystalline phases present.
Unlike optical methods of analysis, however, XRD cannot determine
crystal morphology. Therefore, in asbestos analysis, XRD does not
distinguish between fibrous and nonfibrous forms of the serpentine and
amphibole minerals (Table 2-1). However, when used in conjunction with
optical methods such as polarized light microscopy (PLM), XRD techniques
can provide a reliable analytical method for the identification and
characterization of asbestiform minerals in bulk materials.
For qualitative analysis by XRD methods, samples are initially
scanned over limited diagnostic peak regions for the serpentine (7.4 A)
and amphibole (8.2-8.5 A) minerals (Table 2-2). Standard slow-scanning
methods for bulk sample analysis may be used for materials shown by PLM
to contain significant amounts of asbestos (5-10 percent).
Detection of minor or trace amounts of asbestos may require special
sample preparation and step-scanning analysis. All samples that exhibit
diffraction peaks in the diagnostic regions for asbestiform minerals are
submitted to a full (5[deg]-60[deg] 2[thetas]; 1[deg] 2[thetas]/min)
qualitative XRD scan, and their diffraction patterns are compared with
standard reference powder diffraction patterns \3\ to verify initial
peak assignments and to identify possible matrix interferences when
subsequent quantitative analysis will be performed.
Table 2-1--The Asbestos Minerals and Their Nonasbestiform Analogs
------------------------------------------------------------------------
Asbestiform Nonasbestiform
------------------------------------------------------------------------
SERPENTINE ............................
Chrysotile Antigorite, lizardite
AMPHIBOLE ............................
Anthophyllite asbestos Anthophyllite
Cummingtonite-grunerite asbestos Cummingtonite-grunerite
(``Amosite'')
Crocidolite Riebeckite
Tremolite asbestos Tremolite
Actinolite asbestos Actinolite
------------------------------------------------------------------------
Table 2-2--Principal Lattice Spacings of Asbestiform Minerals a
----------------------------------------------------------------------------------------------------------------
Principal d-spacings (A) and relative
intensities JCPDS Powder diffraction file
Minerals ---------------------------------------- \3\ number
----------------------------------------------------------------------------------------------------------------
Chrysotile............................... 7.37100 3.6570 4.5750 21-543b
7.36100 3.6680 2.4565 25-645
7.10100 2.3380 3.5570 22-1162 (theoretical)
``Amosite''.............................. 8.33100 3.0670 2.75670 17-745 (nonfibrous)
8.22100 3.06085 3.2570 27-1170 (UICC)
Anthophyllite............................ 3.05100 3.2460 8.2655 9-455
3.06100 8.3370 3.2350 16-401 (synthetic)
Anthophyllite............................ 2.72100 2.54100 3.48080 25-157
Crocidolite.............................. 8.35100 3.1055 2.72035 27-1415 (UICC)
Tremolite................................ 8.38100 3.12100 2.70590 13-437b
2.706100 3.1495 8.4340 20-1310b (synthetic)
3.13100 2.70660 8.4440 23-666 (synthetic mixture
with richterite)
----------------------------------------------------------------------------------------------------------------
a This information is intended as a guide, only. Complete powder diffraction data, including mineral type and
source, should be referred to, to ensure comparability of sample and reference materials where possible.
Additional precision XRD data on amosite, crocidolite, tremolite, and chrysotile are available from the U.S.
Bureaus of Mines.\4\
b Fibrosity questionable.
Accurate quantitative analysis of asbestos in bulk samples by XRD is
critically dependent on particle size distribution, crystallite size,
preferred orientation and matrix absorption effects, and comparability
of standard reference and sample materials. The most intense diffraction
peak that has been shown to be free from interference by prior
qualitative XRD analysis is selected for quantitation of each
asbestiform mineral. A ``thin-layer'' method of analysis \5 6\ is
recommended in which, subsequent to comminution of the bulk material to
10 [mu]m by suitable cryogenic milling techniques, an accurately known
amount of the sample is deposited on a silver membrane filter. The mass
of
[[Page 814]]
asbestiform material is determined by measuring the integrated area of
the selected diffraction peak using a step-scanning mode, correcting for
matrix absorption effects, and comparing with suitable calibration
standards. Alternative ``thick-layer'' or bulk methods,\7 8\ may be used
for semiquantitative analysis.
This XRD method is applicable as a confirmatory method for
identification and quantitation of asbestos in bulk material samples
that have undergone prior analysis by PLM or other optical methods.
2.2 Range and Sensitivity
The range of the method has not been determined.
The sensitivity of the method has not been determined. It will be
variable and dependent upon many factors, including matrix effects
(absoprtion and interferences), diagnostic reflections selected, and
their relative intensities.
2.3 Limitations
2.3.1 Interferences
Since the fibrous and nonfibrous forms of the serpentine and
amphibole minerals (Table 2-1) are indistinguishable by XRD techniques
unless special sample preparation techniques and instrumentation are
used,\9\ the presence of nonasbestiform serpentines and amphiboles in a
sample will pose severe interference problems in the identification and
quantitative analysis of their asbestiform analogs.
The use of XRD for identification and quantitation of asbestiform
minerals in bulk samples may also be limited by the presence of other
interfering materials in the sample. For naturally occurring materials
the commonly associated asbestos-related mineral interferences can
usually be anticipated. However, for fabricated materials the nature of
the interferences may vary greatly (Table 2-3) and present more serious
problems in identification and quantitation.\10\ Potential interferences
are summarized in Table 2-4 and include the following:
Chlorite has major peaks at 7.19 A and 3.58 A That
interfere with both the primary (7.36 A) and secondary (3.66 A) peaks
for chrysotile. Resolution of the primary peak to give good quantitative
results may be possible when a step-scanning mode of operation is
employed.
Halloysite has a peak at 3.63 A that interferes with
the secondary (3.66 A) peak for chrysotile.
Kaolinite has a major peak at 7.15 A that may
interfere with the primary peak of chrysotile at 7.36 A when present at
concentrations of 10 percent. However, the secondary
chrysotile peak at 3.66 A may be used for quantitation.
Gypsum has a major peak at 7.5 A that overlaps the
7.36 A peak of chrysotile when present as a major sample constituent.
This may be removed by careful washing with distilled water, or be
heating to 300 [deg]C to convert gypsum to plaster of paris.
Cellulose has a broad peak that partially overlaps
the secondary (3.66 A) chrysotile peak.\8\
Overlap of major diagnostic peaks of the amphibole
asbestos minerals, amosite, anthophyllite, crocidolite, and tremolite,
at approximately 8.3 A and 3.1 A causes mutual interference when these
minerals occur in the presence of one another. In some instances,
adquate resolution may be attained by using step-scanning methods and/or
by decreasing the collimator slit width at the X-ray port.
Table 2-3--Common Constituents in Insulation and Wall Materials
A. Insulation materials
Chrysotile
``Amosite''
Crocidolite
*Rock wool
*Slag wool
*Fiber glass
Gypsum (CaSO4 [middot] 2H2O)
Vermiculite (micas)
*Perlite
Clays (kaolin)
*Wood pulp
*Paper fibers (talc, clay, carbonate fillers)
Calcium silicates (synthetic)
Opaques (chromite, magnetite inclusions in serpentine)
Hematite (inclusions in ``amosite'')
Magnesite
*Diatomaceous earth
B. Spray finishes or paints
Bassanite
Carbonate minerals (calcite, dolomite, vaterite)
Talc
Tremolite
Anthophyllite
Serpentine (including chrysotile)
Amosite
Crocidolite
*Mineral wool
*Rock wool
*Slag wool
*Fiber glass
Clays (kaolin)
Micas
Chlorite
Gypsum (CaSO4 [middot] 2H2O)
Quartz
*Organic binders and thickeners
Hyrdomagnesite
Wollastonite
Opaques (chromite, magnetite inclusions in serpentine)
Hematite (inclusions in ``amosite'')
[[Page 815]]
*Amorphous materials----contribute only to overall scattered
radiation and increased background radiation.
Table 2-4--Interferences in XRD Analysis Asbestiform Minerals
------------------------------------------------------------------------
Primary
diagnostic
peaks
Asbestiform mineral (approximate Interference
d-spacings,
in A)
------------------------------------------------------------------------
Serpentine ............
Chrysotile 7.4 Nonasbestiform
serpentines
(antigorite,
lizardite)
Chlorite
Kaolinite
Gypsum
3.7 Chlorite
Halloysite
Cellulose
Amphibole ............
``Amosite'' 3.1 Nonasbestiform
Anthophyllite <3-ln [>||<3-ln (cummingtonite-
|<3-ln ]> grunerite,
Crocidolite anthophyllite,
Tremolite riebeckite,
tremolite)
Mutual interferences
Carbonates
Talc
8.3 Mutual interferences
------------------------------------------------------------------------
Carbonates may also interfere with quantitative
analysis of the amphibole asbestos minerals, amosite, anthophyllite,
crocidolite, and tremolite. Calcium carbonate (CaCO3) has a
peak at 3.035 A that overlaps major amphibole peaks at approximately 3.1
A when present in concentrations of 5 percent. Removal of
carbonates with a dilute acid wash is possible; however, if present,
chrysotile may be partially dissolved by this treatment.\11\
A major talc peak at 3.12 A interferes with the
primary tremolite peak at this same position and with secondary peaks of
crocidolite (3.10 A), amosite (3.06 A), and anthophyllite (3.05 A). In
the presence of talc, the major diagnostic peak at approximately 8.3 A
should be used for quantitation of these asbestiform minerals.
The problem of intraspecies and matrix interferences is further
aggravated by the variability of the silicate mineral powder diffraction
patterns themselves, which often makes definitive identification of the
asbestos minerals by comparison with standard reference diffraction
patterns difficult. This variability results from alterations in the
crystal lattice associated with differences in isomorphous substitution
and degree of crystallinity. This is especially true for the amphiboles.
These minerals exhibit a wide variety of very similar chemical
compositions, with the result being that their diffraction patterns are
chracterized by having major (110) reflections of the monoclinic
amphiboles and (210) reflections of the orthorhombic anthophyllite
separated by less than 0.2 A.\12\
2.3.2 Matrix Effects
If a copper X-ray source is used, the presence of iron at high
concentrations in a sample will result in significant X-ray
fluorescence, leading to loss of peak intensity along with increased
background intensity and an overall decrease in sensitivity. This
situation may be corrected by choosing an X-ray source other than
copper; however, this is often accompanied both by loss of intensity and
by decreased resolution of closely spaced reflections. Alternatively,
use of a diffracted beam monochromator will reduce background
fluorescent raditation, enabling weaker diffraction peaks to be
detected.
X-ray absorption by the sample matrix will result in overall
attenuation of the diffracted beam and may seriously interfere with
quantitative analysis. Absorption effects may be minimized by using
sufficiently ``thin'' samples for analysis.\5 13 14\ However, unless
absorption effects are known to be the same for both samples and
standards, appropriate corrections should be made by referencing
diagnostic peak areas to an internal standard \7 8\ or filter substrate
(Ag) peak.\5 6\
2.3.3 Particle Size Dependence
Because the intensity of diffracted X-radiation is particle-size
dependent, it is essential for accurate quantitative analysis that both
sample and standard reference materials have similar particle size
distributions. The optimum particle size range for quantitative analysis
of asbestos by XRD has been reported to be 1 to 10 [mu] m.\15\
Comparability of sample and standard reference material particle size
distributions should be verified by optical microscopy (or another
suitable method) prior to analysis.
2.3.4 Preferred Orientation Effects
Preferred orientation of asbestiform minerals during sample
preparation often poses a serious problem in quantitative analysis by
XRD. A number of techniques have been developed for reducing preferred
orientation effects in ``thick layer'' samples.\7 8 15\ However, for
``thin'' samples on membrane filters, the preferred orientation effects
seem to be both reproducible and favorable to enhancement of the
principal diagnostic reflections of asbestos minerals, actually
increasing the overall sensitivity of the method.\12 14\ (Further
investigation into preferred orientation effects in both thin layer and
bulk samples is required.)
2.3.5 Lack of Suitably Characterized Standard Materials
The problem of obtaining and characterizing suitable reference
materials for asbestos analysis is clearly recognized. NIOSH has
[[Page 816]]
recently directed a major research effort toward the preparation and
characterization of analytical reference materials, including asbestos
standards; 16 17 however, these are not available in large
quantities for routine analysis.
In addition, the problem of ensuring the comparability of standard
reference and sample materials, particularly regarding crystallite size,
particle size distribution, and degree of crystallinity, has yet to be
adequately addressed. For example, Langer et al.\18\ have observed that
in insulating matrices, chrysotile tends to break open into bundles more
frequently than amphiboles. This results in a line-broadening effect
with a resultant decrease in sensitivity. Unless this effect is the same
for both standard and sample materials, the amount of chrysotile in the
sample will be underestimated by XRD analysis. To minimize this problem,
it is recommended that standardized matrix reduction procedures be used
for both sample and standard materials.
2.4 Precision and Accuracy
Precision of the method has not been determined.
Accuracy of the method has not been determined.
2.5 Apparatus
2.5.1 Sample Preparation
Sample preparation apparatus requirements will depend upon the
sample type under consideration and the kind of XRD analysis to be
performed.
Mortar and Pestle: Agate or porcelain.
Razor Blades
Sample Mill: SPEX, Inc., freezer mill or equivalent.
Bulk Sample Holders
Silver Membrane Filters: 25-mm diameter, 0.45-[mu] m
pore size. Selas Corp. of America, Flotronics Div., 1957 Pioneer Road,
Huntington Valley, PA 19006.
Microscope Slides
Vacuum Filtration Apparatus: Gelman No. 1107 or
equivalent, and side-arm vacuum flask.
Microbalance
Ultrasonic Bath or Probe: Model W140, Ultrasonics,
Inc., operated at a power density of approximately 0.1 W/mL, or
equivalent.
Volumetric Flasks: 1-L volume.
Assorted Pipettes
Pipette Bulb
Nonserrated Forceps
Polyethylene Wash Bottle
Pyrex Beakers: 50-mL volume.
Desiccator
Filter Storage Cassettes
Magnetic Stirring Plate and Bars
Porcelain Crucibles
Muffle Furnace or Low Temperature Asher
2.5.2 Sample Analysis
Sample analysis requirements include an X-ray diffraction unit,
equipped with:
Constant Potential Generator; Voltage and mA
Stabilizers
Automated Diffractometer with Step-Scanning Mode
Copper Target X-Ray Tube: High intensity, fine focus,
preferably.
X-Ray Pulse Height Selector
X-Ray Detector (with high voltage power supply):
Scintillation or proportional counter.
Focusing Graphite Crystal Monochromator; or Nickel
Filter (if copper source is used, and iron fluorescence is not a serious
problem).
Data Output Accessories:
Strip Chart Recorder
Decade Scaler/Timer
Digital Printer
Sample Spinner (optional).
Instrument Calibration Reference Specimen: [alpha]-
quartz reference crystal (Arkansas quartz standard, 180-147-00,
Philips Electronics Instruments, Inc., 85 McKee Drive, Mahwah, NJ 07430)
or equivalent.
2.6 Reagents
2.6.1 Standard Reference Materials
The reference materials listed below are intended to serve as a
guide. Every attempt should be made to acquire pure reference materials
that are comparable to sample materials being analyzed.
Chrysotile: UICC Canadian, or NIEHS Plastibest. (UICC
reference materials available from: UICC, MRC Pneumoconiosis Unit,
Llandough Hospital, Penarth, Glamorgan, CF61XW, UK).
Crocidolite: UICC
Amosite: UICC
Anthophyllite: UICC
Tremolite Asbestos: Wards Natural Science
Establishment, Rochester, N.Y.; Cyprus Research Standard, Cyprus
Research, 2435 Military Ave., Los Angeles, CA 90064 (washed with dilute
HCl to remove small amount of calcite impurity); India tremolite,
Rajasthan State, India.
Actinolite Asbestos
2.6.2 Adhesive
Tape, petroleum jelly, etc. (for attaching silver membrane filters
to sample holders).
2.6.3 Surfactant
1 percent aerosol OT aqueous solution or equivalent.
2.6.4 Isopropanol
ACS Reagent Grade.
[[Page 817]]
2.7 Procedure
2.7.1 Sampling
Samples for analysis of asbestos content shall be collected as
specified in EPA Guidance Document C0090, Asbestos-Containing
Materials in School Buildings.\10\
2.7.2 Analysis
All samples must be analyzed initially for asbestos content by PLM.
XRD should be used as an auxiliary method when a second, independent
analysis is requested.
Note: Asbestos is a toxic substance. All handling of dry materials
should be performed in an operating fume hood.
2.7.2.1 Sample Preparation
The method of sample preparation required for XRD analysis will
depend on: (1) The condition of the sample received (sample size,
homogeneity, particle size distribution, and overall composition as
determined by PLM); and (2) the type of XRD analysis to be performed
(qualitative, quantitative, thin layer or bulk).
Bulk materials are usually received as inhomogeneous mixtures of
complex composition with very wide particle size distributions.
Preparation of a homogeneous, representative sample from asbestos-
containing materials is particularly difficult because the fibrous
nature of the asbestos minerals inhibits mechanical mixing and stirring,
and because milling procedures may cause adverse lattice alterations.
A discussion of specific matrix reduction procedures is given below.
Complete methods of sample preparation are detailed in Sections 2.7.2.2
and 2.7.2.3.
Note: All samples should be examined microscopically before and
after each matrix reduction step to monitor changes in sample particle
size, composition, and crystallinity, and to ensure sample
representativeness and homogeneity for analysis.
2.7.2.1.1 Milling-- Mechanical milling of asbestos materials has
been shown to decrease fiber crystallinity, with a resultant decrease in
diffraction intensity of the specimen; the degree of lattice alteration
is related to the duration and type of milling
process.19,&thnsp[gE]22 Therefore, all milling times should
be kept to a minimum.
For qualitative analysis, particle size is not usually of critical
importance and initial characterization of the material with a minimum
of matrix reduction is often desirable to document the composition of
the sample as received. Bulk samples of very large particle size
(2-3 mm) should be comminuted to 100 [mu]m. A mortar and
pestle can sometimes be used in size reduction of soft or loosely bound
materials though this may cause matting of some samples. Such samples
may be reduced by cutting with a razor blade in a mortar, or by grinding
in a suitable mill (e.g., a microhammer mill or equivalent). When using
a mortar for grinding or cutting, the sample should be moistened with
ethanol, or some other suitable wetting agent, to minimize exposures.
For accurate, reproducible quantitative analysis, the particle size
of both sample and standard materials should be reduced to 10 [mu]m (see
Section 2.3.3). Dry ball milling at liquid nitrogen temperatures (e.g.,
Spex Freezer Mill, or equivalent) for a maximum time of 10 min. is
recommended to obtain satisfactory particle size distributions while
protecting the integrity of the crystal lattice. \5\ Bulk samples of
very large particle size may require grinding in two stages for full
matrix reduction to <10 [mu]m. \8, 16\
Final particle size distributions should always be verified by
optical microscopy or another suitable method.
2.7.2.1.2 Low temperature ashing-- For materials shown by PLM to
contain large amounts of gypsum, cellulosic, or other organic materials,
it may be desirable to ash the samples prior to analysis to reduce
background radiation or matrix interference. Since chrysotile undergoes
dehydroxylation at temperatures between 550 [deg]C and and 650 [deg]C,
with subsequent transformation to forsterite,\23, 24\ ashing
temperatures should be kept below 500 [deg]C. Use of a low temperature
asher is recommended. In all cases, calibration of the oven is essential
to ensure that a maximum ashing temperature of 500 [deg]C is not
exceeded.
2.7.2.1.3 Acid leaching--Because of the interference caused by
gypsum and some carbonates in the detection of asbestiform minerals by
XRD (see Section 2.3.1), it may be necessary to remove these
interferents by a simple acid leaching procedure prior to analysis (see
Section 1.7.2.2).
2.7.2.2 Qualitative Analysis
2.7.2.2.1 Initial screening of bulk material-- Qualitative analysis
should be performed on a representative, homogeneous portion of the
sample with a minimum of sample treatment.
1. Grind and mix the sample with a mortar and pestle (or equivalent
method, see Section 2.7.2.1.1.) to a final particle size sufficiently
small (100 [mu]m) to allow adequate packing into the sample holder.
2. Pack the sample into a standard bulk sample holder. Care should
be taken to ensure that a representative portion of the milled sample is
selected for analysis. Particular care should be taken to avoid possible
size segregation of the sample. (Note: Use of a back-packing method \25\
of bulk sample preparation may reduce preferred orientation effects.)
3. Mount the sample on the diffractometer and scan over the
diagnostic peak regions for the serpentine (67.4 A) and amphibole (8.2-
[[Page 818]]
8.5 A) minerals (see Table 2-2). The X-ray diffraction equipment should
be optimized for intensity. A slow scanning speed of 1[deg]
2[thetas]/min is recommended for adequate resolution. Use of
a sample spinner is recommended.
4. Submit all samples that exhibit diffraction peaks in the
diagnostic regions for asbestiform minerals to a full qualitative XRD
scan (5[deg]-60[deg] 2[thetas]; 1[deg]2[thetas]/
min) to verify initial peak assignments and to identify potential matrix
interferences when subsequent quantitative analysis is to be performed.
5. Compare the sample XRD pattern with standard reference powder
diffraction patterns (i.e., JCPDS powder diffraction data \3\ or those
of other well-characterized reference materials). Principal lattice
spacings of asbestiform minerals are given in Table 2-2; common
constituents of bulk insulation and wall materials are listed in Table
2-3.
2.7.2.2.2 Detection of minor or trace constituents-- Routine
screening of bulk materials by XRD may fail to detect small
concentrations (<5 percent) of asbestos. The limits of detection will,
in general, be improved if matrix absorption effects are minimized, and
if the sample particle size is reduced to the optimal 1 to 10 [mu]m
range, provided that the crystal lattice is not degraded in the milling
process. Therefore, in those instances where confirmation of the
presence of an asbestiform mineral at very low levels is required, or
where a negative result from initial screening of the bulk material by
XRD (see Section 2.7.2.2.1) is in conflict with previous PLM results, it
may be desirable to prepare the sample as described for quantitative
analysis (see Section 2.7.2.3) and step-scan over appropriate
2[thetas] ranges of selected diagnostic peaks (Table 2-2).
Accurate transfer of the sample to the silver membrane filter is not
necessary unless subsequent quantitative analysis is to be performed.
2.7.2.3 Quantitative Analysis
The proposed method for quantitation of asbestos in bulk samples is
a modification of the NIOSH-recommended thin-layer method for chrysotile
in air. \5\ A thick-layer or bulk method involving pelletizing the
sample may be used for semiquantitative analysis; \7,8\ however, this
method requires the addition of an internal standard, use of a specially
fabricated sample press, and relatively large amounts of standard
reference materials. Additional research is required to evaluate the
comparability of thin- and thick-layer methods for quantitative asbestos
analysis.
For quantitative analysis by thin-layer methods, the following
procedure is recommended:
1. Mill and size all or a substantial representative portion of the
sample as outlined in Section 2.7.2.1.1.
2. Dry at 100 [deg]C for 2 hr; cool in a desiccator.
3. Weigh accurately to the nearest 0.01 mg.
4. Samples shown by PLM to contain large amounts of cellulosic or
other organic materials, gypsum, or carbonates, should be submitted to
appropriate matrix reduction procedures described in Sections 2.7.2.1.2
and 2.7.2.1.3. After ashing and/or acid treatment, repeat the drying and
weighing procedures described above, and determine the percent weight
loss; L.
5. Quantitatively transfer an accurately weighed amount (50-100 mg)
of the sample to a 1-L volumetric flask with approximately 200 mL
isopropanol to which 3 to 4 drops of surfactant have been added.
6. Ultrasonicate for 10 min at a power density of approximately 0.1
W/mL, to disperse the sample material.
7. Dilute to volume with isopropanol.
8. Place flask on a magnetic stirring plate. Stir.
9. Place a silver membrane filter on the filtration apparatus, apply
a vacuum, and attach the reservoir. Release the vacuum and add several
milliliters of isopropanol to the reservoir. Vigorously hand shake the
asbestos suspension and immediately withdraw an aliquot from the center
of the suspension so that total sample weight, WT, on the
filter will be approximately 1 mg. Do not adjust the volume in the pipet
by expelling part of the suspension; if more than the desired aliquot is
withdrawn, discard the aliquot and resume the procedure with a clean
pipet. Transfer the aliquot to the reservoir. Filter rapidly under
vacuum. Do not wash the reservoir walls. Leave the filter apparatus
under vacuum until dry. Remove the reservoir, release the vacuum, and
remove the filter with forceps. (Note: Water-soluble matrix
interferences such as gypsum may be removed at this time by careful
washing of the filtrate with distilled water. Extreme care should be
taken not to disturb the sample.)
10. Attach the filter to a flat holder with a suitable adhesive and
place on the diffractometer. Use of a sample spinner is recommended.
11. For each asbestos mineral to be quantitated select a reflection
(or reflections) that has been shown to be free from interferences by
prior PLM or qualitative XRD analysis and that can be used unambiguously
as an index of the amount of material present in the sample (see Table
2-2).
12. Analyze the selected diagnostic reflection(s) by step scanning
in increments of 0.02[deg] 2[thetas] for an appropriate fixed
time and integrating the counts. (A fixed count scan may be used
alternatively; however, the method chosen should be used consistently
for all samples and standards.) An appropriate scanning interval should
be selected for each peak, and background corrections made. For a fixed
time scan, measure the background on each side of the peak for one-
[[Page 819]]
half the peak-scanning time. The net intensity, Ia, is the
difference between the peak integrated count and the total background
count.
13. Determine the net count, IAg, of the filter 2.36 A
silver peak following the procedure in step 12. Remove the filter from
the holder, reverse it, and reattach it to the holder. Determine the net
count for the unattenuated silver peak, IA.7g. Scan times may
be less for measurement of silver peaks than for sample peaks; however,
they should be constant throughout the analysis.
14. Normalize all raw, net intensities (to correct for instrument
instabilities) by referencing them to an external standard (e.g., the
3.34 A peak of an [alpha]-quartz reference crystal). After each unknown
is scanned, determine the net count, Irr.7:
[GRAPHIC] [TIFF OMITTED] TC01AP92.018
2.8 Calibration
2.8.1 Preparation of Calibration Standards
1. Mill and size standard asbestos materials according to the
procedure outlined in Section 2.7.2.1.1. Equivalent, standardized matrix
reduction and sizing techniques should be used for both standard and
sample materials.
2. Dry at 100 [deg]C for 2 hr; cool in a desiccator.
3. Prepare two suspensions of each standard in isopropanol by
weighing approximately 10 and 50 mg of the dry material to the nearest
0.01 mg. Quantitatively transfer each to a 1-L volumetric flask with
approximately 200 mL isopropanol to which a few drops of surfactant have
been added.
4. Ultrasonicate for 10 min at a power density of approximately 0.1
W/mL, to disperse the asbestos material.
5. Dilute to volume with isopropanol.
6. Place the flask on a magnetic stirring plate. Stir.
7. Prepare, in triplicate, a series of at least five standard
filters to cover the desired analytical range, using appropriate
aliquots of the 10 and 50 mg/L suspensions and the following procedure.
Mount a silver membrane filter on the filtration apparatus. Place a
few milliliters of isopropanol in the reservoir. Vigorously hand shake
the asbestos suspension and immediately withdraw an aliquot from the
center of the suspension. Do not adjust the volume in the pipet by
expelling part of the suspension; if more than the desired aliquot is
withdrawn, discard the aliquot and resume the procedure with a clean
pipet. Transfer the aliquot to the reservoir. Keep the tip of the pipet
near the surface of the isopropanol. Filter rapidly under vacuum. Do not
wash the sides of the reservoir. Leave the vacuum on for a time
sufficient to dry the filter. Release the vacuum and remove the filter
with forceps.
2.8.2 Analysis of Calibration Standards
1. Mount each filter on a flat holder. Perform step scans on
selected diagnostic reflections of the standards and reference specimen
using the procedure outlined in Section 2.7.2.3, step 12, and the same
conditions as those used for the samples.
2. Determine the normalized intensity for each peak measured,
Is.7td, as outlined in Section 2.7.2.3, step 14.
2.9 Calculations
For each asbestos reference material, calculate the exact weight
deposited on each standard filter from the concentrations of the
standard suspensions and aliquot volumes. Record the weight, w, of each
standard. Prepare a calibration curve by regressing I2s.7td
on w. Poor reproducibility (15 percent RSD) at any
given level indicates problems in the sample preparation technique, and
a need for new standards. The data should fit a straight line equation.
Determine the slope, m, of the calibration curve in counts/
microgram. The intercept, b, of the line with the Is.7td axis
should be approximately zero. A large negative intercept indicates an
error in determining the background. This may arise from incorrectly
measuring the baseline or from interference by another phase at the
angle of background measurement. A large positive intercept indicates an
error in determining the baseline or that an impurity is included in the
measured peak.
Using the normalized intensity, IAg, for the attenuated
silver peak of a sample, and the corresponding normalized intensity from
the unattenuated silver peak, IA.7g, of the sample filter,
calculate the transmittance, T, for each sample as follows:\26\ \27\
[GRAPHIC] [TIFF OMITTED] TC01AP92.019
Determine the correction factor, f(T), for each sample according to
the formula:
...... -R (ln T)
f (T) --------
=
...... l-TR
where
[[Page 820]]
..... sin [Theta]Ag
R = --------
..... sin [Theta]a
[thetas]Ag=angular position of the measured silver peak (from
Bragg's Law), and
[thetas]a=angular position of the diagnostic asbestos peak.
Calculate the weight, Wa, in micrograms, of the asbestos
material analyzed for in each sample, using the appropriate calibration
data and absorption corrections:
[GRAPHIC] [TIFF OMITTED] TC01AP92.020
Calculate the percent composition, Pa, of each asbestos
mineral analyzed for in the parent material, from the total sample
weight, WT, on the filter:
..... Wa(1-.01L)
Pa = ---------- x 100
..... WT
where
Pa=percent asbestos mineral in parent material;
Wa=mass of asbestos mineral on filter, in [mu]g;
WT=total sample weight on filter, in [mu]g;
L=percent weight loss of parent material on ashing and/or acid treatment
(see Section 2.7.2.3).
2.10 References
1. H. P. Klug and L. E. Alexander, X-ray Diffraction Procedures for
Polycrystalline and Amorphous Materials, 2nd ed., New York: John Wiley
and Sons, 1979.
2. L. V. Azaroff and M. J. Buerger, The Powder Method of X-ray
Crystallography, New York: McGraw-Hill, 1958.
3. JCPDS-International Center for Diffraction Data Powder
Diffraction File, U.S. Department of Commerce, National Bureau of
Standards, and Joint Committee on Powder Diffraction Studies,
Swarthmore, PA.
4. W. J. Campbell, C. W. Huggins, and A. G. Wylie, Chemical and
Physical Characterization of Amosite, Chrysotile, Crocidolite, and
Nonfibrous Tremolite for National Institute of Environmental Health
Sciences Oral Ingestion Studies, U.S. Bureau of Mines Report of
Investigation RI8452, 1980.
5. B. A. Lange and J. C. Haartz, Determination of microgram
quantities of asbestos by X-ray diffraction: Chrysotile in thin dust
layers of matrix material, Anal. Chem., 51(4):520-525, 1979.
6. NIOSH Manual of Analytical Methods, Volume 5, U.S. Dept. HEW,
August 1979, pp. 309-1 to 309-9.
7. H. Dunn and J. H. Stewart, Jr., Quantitative determination of
chrysotile in building materials, The Microscope, 29(1), 1981.
8. M. Taylor, Methods for the quantitative determination of asbestos
and quartz in bulk samples using X-ray diffraction, The Analyst,
103(1231):1009-1020, 1978.
9. L. Birks, M. Fatemi, J. V. Gilfrich, and E. T. Johnson,
Quantitative Analysis of Airborne Asbestos by X-ray Diffraction, Naval
Research Laboratory Report 7879, Naval Research Laboratory, Washington,
DC, 1975.
10. U.S. Environmental Protection Agency, Asbestos-Containing
Materials in School Buildings: A Guidance Document, Parts 1 and 2, EPA/
OPPT No. C00090, March 1979.
11. J. B. Krause and W. H. Ashton, Misidentification of asbestos in
talc, pp. 339-353, in: Proceedings of Workshop on Asbestos: Definitions
and Measurement Methods (NBS Special Publication 506), C. C. Gravatt, P.
D. LaFleur, and K. F. Heinrich (eds.), Washington, DC: National
Measurement Laboratory, National Bureau of Standards, 1977 (issued
1978).
12. H. D. Stanley, The detection and identification of asbestos and
asbesti-form minerals in talc, pp. 325-337, in Proceedings of Workshop
on Asbestos: Definitions and Measurement Methods (NBS Special
Publication 506), C. C. Gravatt, P. D. LaFleur, and K. F. Heinrich
(eds.), Washington, DC, National Measurement Laboratory, National Bureau
of Standards, 1977 (issued 1978).
13. A. L. Rickards, Estimation of trace amounts of chrysotile
asbestos by X-ray diffraction, Anal. Chem., 44(11):1872-3, 1972.
14. P. M. Cook, P. L. Smith, and D. G. Wilson, Amphibole fiber
concentration and determination for a series of community air samples:
use of X-ray diffraction to supplement electron microscope analysis, in:
Electron Microscopy and X-ray Applications to Environmental and
Occupation Health Analysis, P. A. Russell and A. E. Hutchings (eds.),
Ann Arbor: Ann Arbor Science Publications, 1977.
15. A. N. Rohl and A. M. Langer, Identification and quantitation of
asbestos in talc, Environ. Health Perspectives, 9:95-109, 1974.
16. J. L. Graf, P. K. Ase, and R. G. Draftz, Preparation and
Characterization of Analytical Reference Minerals, DHEW (NIOSH)
Publication No. 79-139, June 1979.
17. J. C. Haartz, B. A. Lange, R. G. Draftz, and R. F. Scholl,
Selection and characterization of fibrous and nonfibrous amphiboles for
analytical methods development, pp. 295-312, in: Proceedings of Workshop
on Asbestos: Definitions and Measurement Methods (NBS Special
Publication 506), C. C. Gravatt, P. D. LaFleur, and K. F. Heinrich
(eds.), Washington, DC: National Measurement Laboratory, National Bureau
of Standards, 1977 (issued 1978).
18. Personal communication, A. M. Langer, Environmental Sciences
Laboratory, Mount
[[Page 821]]
Sinai School of Medicine of the City University of New York, New York,
New York.
19. A. M. Langer, M. S. Wolff, A. N. Rohl, and I. J. Selikoff,
Variation of properties of chrysotile asbestos subjected to milling, J.
Toxicol. and Environ. Health, 4:173-188, 1978.
20. A. M. Langer, A. D. Mackler, and F. D. Pooley, Electron
microscopical investigation of asbestos fibers, Environ. Health
Perspect., 9:63-80, 1974.
21. E. Occella and G. Maddalon, X-ray diffraction characteristics of
some types of asbestos in relation to different techniques of
comminution, Med. Lavoro, 54(10):628-636, 1963.
22. K. R. Spurny, W. Stober, H. Opiela, and and G. Weiss, On the
problem of milling and ultrasonic treatment of asbestos and glass fibers
in biological and analytical applications, Am. Ind. Hyg. Assoc. J.,
41:198-203, 1980.
23. L. G. Berry and B. Mason, Mineralogy, San Francisco: W. H.
Greeman & Co., 1959.
24. J. P. Schelz, The detection of chrysotile asbestos at low levels
in talc by differential thermal analysis, Thermochimica Acta, 8:197-204,
1974.
25. Reference 1, pp. 372-374.
26. J. Leroux, Staub-Reinhalt Luft, 29:26 (English), 1969.
27. J. A. Leroux, B. C. Davey, and A. Paillard, Am. Ind. Hyg. Assoc.
J., 34:409, 1973.
[47 FR 23369, May 27, 1982; 47 FR 38535, Sept. 1, 1982; Redesignated at
60 FR 31922, June 19, 1995]
Subpart F [Reserved]