Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Mass Concentration

SCOPE
1.1 This test method covers a procedure to ( ) identify asbestos in dust and ( ) provide an estimate of the concentration of asbestos in the sampled dust, reported as either the mass of asbestos per unit area of sampled surface or as the mass of asbestos per mass of sampled dust.  
1.1.1 If an estimate of asbestos structure counts is to be determined, the user is referred to Test Method D5755.  
1.2 This test method describes the equipment and procedures necessary for sampling, by a microvacuum technique, non-airborne dust for levels of asbestos. The non-airborne sample is collected inside a standard filter membrane cassette from the sampling of a surface area for dust which may contain asbestos.  
1.2.1 This procedure uses a microvacuuming sampling technique. The collection efficiency of this technique is unknown. Variability of collection efficiency for any particular substrate and across different types of substrates is also unknown. The effects of sampling efficiency differences and variability on the interpretation of dust sampling measurements have not been determined.  
1.3 Asbestos identified by transmission electron microscopy (TEM) is based on morphology, selected area electron diffraction (SAED), and energy dispersive X-ray analysis (EDXA). Some information about structure size is also determined.  
1.4 This test method is generally applicable for an estimate of the concentration of asbestos starting from approximately 0.24 pg of asbestos per square centimeter (assuming a minimum fiber dimension of 0.5 [mu]m by 0.025 [mu]m, see 17.8), but will vary with the analytical parameters noted in 17.8.  
1.4.1 The procedure outlined in this test method employs an indirect sample preparation technique. It is intended to disaggregate and disperse asbestos into fibrils and fiber bundles that can be more accurately identified, counted, and sized by transmission electron microscopy. However, as with all indirect sample preparation techniques, the asbestos observed for quantitation may not represent the physical form of the asbestos as sampled. More specifically, the procedure described neither creates nor destroys asbestos, but it may alter the physical form of the mineral fibers.  
1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

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ASTM D5756-95 - Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Mass Concentration
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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5756 – 95
Standard Test Method for
Microvacuum Sampling and Indirect Analysis of Dust by
Transmission Electron Microscopy for Asbestos Mass
Concentration
This standard is issued under the fixed designation D 5756; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope asbestos as sampled. More specifically, the procedure de-
scribed nmeither creates not destroys asbestos, but it may alter
1.1 This test method covers a procedure to (a) identify
the physical form of the mineral fibers.
asbestos in dust and (b) provide an extimate of the concentra-
1.5 The values stated in SI units are to be regarded as the
tion of asbestos in the sampled dust, reported as either the mass
standard. The values given in parentheses are for information
of asbestos per unit area of sampled suurface or as the mass of
only.
asbestos per mass of sampled dust.
1.6 This standard does not purport to address all of the
1.1.1 If an estimate of asbestos structure counts is to be
safety concerns, if any, associated with its use. It is the
determined, the user is referred to Test Method D 5755.
responsibility of the user of this standard to establish appro-
1.2 This test method describes the equipment and proce-
priate safety and health practices and determine the applica-
dures necessary for sampling, by a microvacuum technique,
bility of regulatory limitations prior to use.
non-airborne dust for levels of asbestos. The non-airborne
sample is collected inside a standard filter membrane cassette
2. Referenced Documents
from the sampling of a surface area for dust which may contain
2.1 ASTM Standards:
asbestos.
D 1193 Specification for Reagent Water
1.2.1 This procedure uses a microvacuuming sampling tech-
D 1739 Test Methods for Collection and Measurement of
nique. The collection efficiency of this technique is unknown.
Dustfall (Settleable Particulate Matter)
Variability of collection efficiency for any particular substrate
D 3195 Practice for Rotameter Calibration
and across different types of substrates is also unknown. The
D 5755 Test Method for Microvacuum Sampling and Indi-
effects of sampling efficiency differences and variability on the
rect Analysis of Dust by Transmission Electron Micros-
interpretation of dust sampling measurements have not been
copy for Asbestos Structure Number Concentrations
determined.
E 832 Specification for Laboratory Filter Papers
1.3 Asbestos identified by transmission electron microscopy
2.2 ISO Standards:
(TEM) is based on morphology, selected area electron diffrac-
ISO/10312 Ambient Air: Determination of Asbestos Fibers;
tion (SAED), and energy dispersive X-ray analysis (EDXA).
Direct Transfer Transmission Electron Microscopy Proce-
Some information about structure size is also determined.
dure
1.4 This test method is generally applicable for an estimate
ISO/CD13794 Ambient Air: Determination of Asbestos Fi-
of the concentration of asbestos starting from approximately
bres; Indirect-Transfer Transmission Electron Microscopy
0.24 pg of asbestos per square centimeter (assuming a mini-
Procedure
mum fiber dimension of 0.5 μm by 0.025 μm, see 17.8), but
will vary with the analytical parameters noted in 17.8.
3. Terminology
1.4.1 The procedure outlined in this test method employs an
3.1 Definitions:
indirect sample preparation technique. It is intended to disag-
3.1.1 asbestiform—a special type of fibrous habit in which
gregate and disperse asbestos into fibrils and fiber bundles that
the fibers are separable into thinner fibers and ultimately into
can be more accurately identified, counted, and sized by
fibrils. This habit accounts for greater flexibility and higher
transmission electron microscopy. However, as with all indi-
tensile strength than other habits of the same mineral. For more
rect sample preparation techniques, the asbestos observed for
quantitation may not represent the physical form of the
Annual Book of ASTM Standards, Vol 11.01.
1 3
This test method is under the jurisdiction of ASTM Committee D-22 on Annual Book of ASTM Standards, Vol 11.03.
Sampling and Analysis of Atmospheresand is the direct responsibility of Subcom- Annual Book of ASTM Standards, Vol 14.02.
mittee D22.07on Sampling and Analysis of Asbestos. Available from American National Standards Institute, 11 W. 42nd St., 13th
Current edition approved Aug. 15, 1995. Published October 1995. Floor, New York, NY 10036.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5756
information on aasbestiform mineralogy, see references (1), (2) ferred to as fibrous even if it is not composed of separable
and (3). fibers, but has that distinct appearance. The term fibrous is used
3.1.2 asbestos—a collective term that describes a group of in a general mineralogical way to describe aggregates of grains
naturally occurring, inorganic, highly fibrous silicate minerals, that crystallize in a needle-like habit and appear to be com-
which are easily separated into long, thin, flexible fibers when posed of fibers. Fibrous has a much more general meaning than
crushed or processed. asbestos. While it is correct that all asbestos minerals are
3.1.2.1 Discussion—Included in the definition are the as- fibrous, not all minerals having fibrous habits are asbestos.
bestiform varieties of: serpentine (chyrsotile); riebeckite (cro- 3.2.8 indirect preparation—a method in which a sample
cidolite); grunerite (amosite); anthophyllite (anthophyllite as- passes through one or more intermediate steps prior to final
bestos); tremolite (tremolite asbestos); and actinolite (actinolite filtration.
asbestos). The amphibole mineral compositions are defined 3.2.9 matrix—a structure in which one or more fibers, or
according to the nomemclature of the International Mineral- fiber bundles, touch, are attached to, or partially concealed by
ogical Association (3). a single particle or connected group of non-fibrous particles.
The exposed fiber must meet the fiber definition (see section
Chemical Abstract Service
Asbestos
No.
3.2.6). Matrices occur as two varieties—disperse matrices and
Chrysotile 12001-29-5
compact matrices.
Crocidolite 12001-28-4
Grunerite Asbestos (Amosite) 12172-73-5 3.2.9.1 compact matrix—a structure consisting of a particle
Anthophyllite Asbestos 77536-67-5
or linked group of particles, in which fibers or bundles can be
Tremolite Asbestos 77536-68-6
seen either within the structure or projecting from it, such that
Actinolite Asbestos 77536-66-4
the dimensions of individual fibers and bundles cannot be
3.1.3 fibril—a single fiber that cannot be separated into
unambiguously determined.
smaller components without losing its fibrous properties or
3.2.9.2 disperse matrix—a structure consisting of a particle
appearance.
or linked group of particles, with overlapping or attached fibers
3.2 Definitions of Terms Specific to This Standard:
or bundles in which at least one of the individual fibers or
3.2.1 aspect ratio—the ratio of the length of a fibrous
bundles can be separately identified and its dimensions mea-
particle to its average width.
sured.
3.2.2 bundle—a structure composed of three or more fibers
3.2.10 structures—a term that is used to categorize all the
in a parallel arrangement with the fibers closer than one fiber
types of asbestos particles which are recorded during the
diameter to each other.
analysis (such as fibers, bundles, clusters, and matrices).
3.2.3 cluster—an aggregate of two or more randomly ori-
ented fibers, with or without bundles. Clusters occur as two 4. Summary of Test Method
varieties—disperse clusters and compact clusters.
4.1 The sample is collected by vacuuming a known surface
3.2.3.1 compact cluster—a complex and tightly bound net-
area with a standard 25 or 37 mm air sampling cassette using
work in which one or both ends of each individual fiber or
a plastic tube that is attached to the inlet orifice which acts as
bundle are obscured, such that the dimensions of individual
a nozzle. The sample is transferred from inside the cassette to
fibers or bundles cannot be unambiguously measured.
a 50/50 alcohol/water solution and screened through a 1.0 by
3.2.3.2 disperse cluster—a disperse and open network in
1.0 mm screen. The fine dust is filtered onto a membrane filter
which both ends of one of the individual fibers or bundles can
and ashed in a muffle furnace. The ash is mixed with distilled
be separately located and its dimensions measured.
water to a known volume. Aliquots of the suspension are then
3.2.4 debris—materials that are of an amount and size
filtered through a membrane. A section of the membrane is
(particles greater than 1 mm in diameter as defined by a 1.0 by
prepared and transferred to a TEM grid using the direct transfer
1.0 mm screen) that can be visually identified (by color,
method. The asbestiform structures are identified, sized, and
texture, etc.) as to their source.
counted by TEM, using SAED and EDXA at a magnification
3.2.5 dust—any material composed of particles in a size
dependent on the size range of asbestos structures present.
range of #1 mm and large enough to settle by virtue of their
5. Significance and Use
weight from the ambient air. See Test Method D 1739.
3.2.6 fiber—a structure having a minimum length of 0.5μ m
5.1 This microvacuum sampling and indirect analysis
with an aspect ratio of 5 to 1 or greater and substantially
method is used for the general testing of non-airborne dust
parallel sides (4). Fibers are assumed to have a cylindrical
samples for asbestos. It is used to assist in the evaluation of
shape (5).
dust that may be found on surfaces in buildings, such as ceiling
3.2.7 fibrous mineral—a mineral that is composed of paral-
tiles, shelving, electrical components, duct work, carpet, etc.
lel, radiating, or interlaced aggregates of fibers, from which the
This test method provides an estimate of the mass concentra-
fibers are sometimes separable.
tion of asbestos in the dust reported as either the mass of
3.2.7.1 Discussion—The crystalline aggregate may be re-
asbestos per unit area or as the mass of asbestos per mass of
sampled dust as derived from a quantitative TEM analysis.
5.1.1 This test method does not describe procedures or
The boldface numbers refer to the list of references at the end of the test
techniques required to evaluate the safety or habitability of
method.
7 buildings with asbestos-containing materials, or compliance
The non-asbestiform variations of the minerals indicated in 3.1.2 have different
Chemical Abstract Service (CAS) numbers. with federal, state, or local regulations or statutes. It is the
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 5756
user’s responsibility to make these determinations. sample container should be approximately 13 cm high by 6 cm
wide).
5.1.2 At present, a single direct relationship between
asbestos-containing dust and potential human exposure does 7.9 Waterproof Markers.
7.10 Forceps (tweezers).
not exist. Accordingly, the user should consider these data in
relationship to other available information in their evaluation. 7.11 Ultrasonic Bath, table top model (100 W, approximate,
see 22.5).
5.2 This test method uses the definition settleable particu-
late matter found in Test Method D 1739 as the definition of 7.12 Graduated Pipettes, 1, 5, and 10 mL sizes, glass or
plastic.
dust. This definition accepts all particles small enough to pass
througha1mm screen. Thus, a single, large asbestos- 7.13 Filter Funnel, 25 mm or 47 mm (either glass or
disposable). Filter funnel assemblies, either glass or disposable
containing particle(s) (from the large end of the particle size
distribution) disassembled during sample preparation may plastic, and using either a 25 mm or 47 mm diameter filter.
7.14 Side Arm Filter Flask, 1000 mL.
result in anomalously large asbestos concentration results in
the TEM analyses of that sample. Conversely, failure to 7.15 Mixed Cellulose Ester (MCE) Membrane Filters,25or
47 mm diameter, #0.22 μm and 5 μm pore size.
disaggregate large particles may result in anomalously low
asbestos mass concentrations. It is, therefore, recommended 7.16 Polycarbonate (PC) Filters, 25 or 47 mm diameter,#
that multiple independent samples be secured from the same 0.2 μm pore size.
area, and that a minimum of three samples be analyzed by the 7.17 Storage Containers, for the 25 or 47 mm filters (for
entire procedure. archiving).
7.18 Glass Slides.
6. Interferences 7.19 Scalpel Blades.
7.20 Cabinet-type Desiccator, or low temperature drying
6.1 The following minerals have properties (that is, chemi-
oven.
cal or crystalline structure) which are very similar to asbestos
minerals and may interfere with the analysis by causing false
8. Reagents and Materials
positives to be recorded during the test. Therefore, literature
8.1 Purity of Reagents—Reagent grade chemicals shall be
references for these materials must be maintained in the
used in all tests. Unless otherwise indicated, it is intended that
laboratory for comparison to asbestos minerals so that they are
all reagents conform to the specifications of the Committee on
not misidentified as asbestos minerals.
Analytical Reagents of the American Chemical Society where
6.1.1 Antigorite.
such specifications are available. Other grades may be used,
6.1.2 Palygorskite (Attapulgite).
provided it is first ascertained that the reagent is of sufficiently
6.1.3 Halloysite.
high purity to permit its use without lessening the accuracy of
6.1.4 Pyroxenes.
the determination.
6.1.5 Sepiolite.
8.2 Acetone.
6.1.6 Vermiculite scrolls.
8.3 Dimethylformamide (DMF).
6.1.7 Fibrous talc.
8.4 Chloroform.
6.1.8 Hornblende and other amphiboles not listed in 5.1.3.
8.5 1-methyl-2-pyrrolidone.
6.2 Collection of any dust particles greater than 1 mm in
8.6 Glacial Acetic Acid.
size in this test method may cause an interference and,
8.7 Low Temperature Plasma Asher.
therefore, should be avoided.
8.8 pH Paper.
8.9 Air Sampling Pump (low volume personal-type pump).
7. Apparatus
8.10 Rotameter.
7.1 Transmission Electron Microscope (TEM),an80to120
8.11 Air Sampling Cassettes (25 mm or 37 mm), containing
kV TEM, capable of performing electron diffraction, with a
0.8 μm or smalle
...

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