ASTM D5756-02(2008)
(Test Method)Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Mass Surface Loading (Withdrawn 2017)
Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Mass Surface Loading (Withdrawn 2017)
SIGNIFICANCE AND USE
This microvacuum sampling and indirect analysis method is used for the general testing of non-airborne dust samples for asbestos. It is used to assist in the evaluation of dust that may be found on surfaces in buildings, such as ceiling tiles, shelving, electrical components, duct work, carpet, etc. This test method provides an estimate of the mass surface loading of asbestos in the dust reported as either the mass of asbestos per unit area or as the mass of asbestos per mass of sampled dust as derived from a quantitative TEM analysis.
This test method does not describe procedures or techniques required to evaluate the safety or habitability of buildings with asbestos-containing materials, or compliance with federal, state, or local regulations or statutes. It is the user's responsibility to make these determinations.
At present, no relationship has been established between asbestos-containing dust as measured by this test method and potential human exposure to airborne asbestos. Accordingly, the users should consider other available information in their interpretation of the data obtained from this test method.
This definition of dust accepts all particles small enough to pass through a 1 mm screen. Thus, a single, large asbestos-containing particle(s) (from the large end of the particle size distribution) disassembled during sample preparation may result in anomalously large asbestos surface loading results in the TEM analyses of that sample. Conversely, failure to disaggregate large particles may result in anomalously low asbestos mass surface loadings. It is, therefore, recommended that multiple independent samples be secured from the same area, and that a minimum of three samples be analyzed by the entire procedure.
SCOPE
1.1 This test method covers a procedure to (a) identify asbestos in dust and (b) provide an estimate of the surface loading 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 D 5755.
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 surface loading of asbestos starting from approximately 0.24 pg of asbestos per square centimetre (assuming a minimum fiber dimension of 0.5 μm by 0.025 μm, 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 not destroys asbestos, but it may alter the physical form of the m...
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D5756 − 02 (Reapproved 2008)
Standard Test Method for
Microvacuum Sampling and Indirect Analysis of Dust by
Transmission Electron Microscopy for Asbestos Mass
Surface Loading
This standard is issued under the fixed designation D5756; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope can be more accurately identified, counted, and sized by
transmission electron microscopy. However, as with all indi-
1.1 This test method covers a procedure to (a) identify
rect sample preparation techniques, the asbestos observed for
asbestos in dust and (b) provide an estimate of the surface
quantitation may not represent the physical form of the
loading of asbestos in the sampled dust, reported as either the
asbestos as sampled. More specifically, the procedure de-
mass of asbestos per unit area of sampled surface or as the
scribed neither creates not destroys asbestos, but it may alter
mass of asbestos per mass of sampled dust.
the physical form of the mineral fibers.
1.1.1 If an estimate of asbestos structure counts is to be
determined, the user is referred to Test Method D5755. 1.5 The values stated in SI units are to be regarded as the
standard.
1.2 This test method describes the equipment and proce-
1.6 This standard does not purport to address all of the
dures necessary for sampling, by a microvacuum technique,
safety concerns, if any, associated with its use. It is the
non-airborne dust for levels of asbestos. The non-airborne
responsibility of the user of this standard to establish appro-
sample is collected inside a standard filter membrane cassette
priate safety and health practices and determine the applica-
fromthesamplingofasurfaceareafordustwhichmaycontain
bility of regulatory limitations prior to use.
asbestos.
1.2.1 Thisprocedureusesamicrovacuumingsamplingtech-
2. Referenced Documents
nique. The collection efficiency of this technique is unknown.
2.1 ASTM Standards:
Variability of collection efficiency for any particular substrate
D1193Specification for Reagent Water
and across different types of substrates is also unknown. The
D3195Practice for Rotameter Calibration
effectsofsamplingefficiencydifferencesandvariabilityonthe
D5755TestMethodforMicrovacuumSamplingandIndirect
interpretation of dust sampling measurements have not been
Analysis of Dust by Transmission Electron Microscopy
determined.
for Asbestos Structure Number Surface Loading
1.3 Asbestosidentifiedbytransmissionelectronmicroscopy
D6620Practice for Asbestos Detection Limit Based on
(TEM) is based on morphology, selected area electron diffrac-
Counts
tion (SAED), and energy dispersive X-ray analysis (EDXA).
E832Specification for Laboratory Filter Papers
Some information about structure size is also determined.
2.2 ISO Standards:
1.4 This test method is generally applicable for an estimate
ISO/10312Ambient Air: Determination of Asbestos Fibers;
of the surface loading of asbestos starting from approximately
DirectTransferTransmission Electron Microscopy Proce-
0.24 pg of asbestos per square centimetre (assuming a mini-
dure
mum fiber dimension of 0.5 µm by 0.025 µm, see 17.8), but
ISO/CD13794Ambient Air: Determination of Asbestos Fi-
will vary with the analytical parameters noted in 17.8.
bres; Indirect-TransferTransmission Electron Microscopy
1.4.1 Theprocedureoutlinedinthistestmethodemploysan
Procedure
indirect sample preparation technique. It is intended to disag-
3. Terminology
gregate and disperse asbestos into fibrils and fiber bundles that
3.1 Definitions:
1 2
This test method is under the jurisdiction of ASTM Committee D22 on Air For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Quality and is the direct responsibility of Subcommittee D22.07 on Sampling and contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Analysis of Asbestos. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved April 15, 2008. Published July 2008. Originally the ASTM website.
approved in 1995. Last previous edition approved in 2002 as D5756–02. DOI: Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
10.1520/D5756-02R08. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5756 − 02 (2008)
3.1.1 asbestiform—a special type of fibrous habit in which 3.2.7 fibrous mineral—a mineral that is composed of
the fibers are separable into thinner fibers and ultimately into parallel, radiating, or interlaced aggregates of fibers, from
fibrils. This habit accounts for greater flexibility and higher which the fibers are sometimes separable.
tensilestrengththanotherhabitsofthesamemineral.Formore 3.2.7.1 Discussion—The crystalline aggregate may be re-
information on asbestiform mineralogy, see references (1), (2)
ferred to as fibrous even if it is not composed of separable
and (3). fibers,buthasthatdistinctappearance.Thetermfibrousisused
inageneralmineralogicalwaytodescribeaggregatesofgrains
3.1.2 asbestos—a collective term that describes a group of
that crystallize in a needle-like habit and appear to be com-
naturally occurring, inorganic, highly fibrous silicate minerals,
posedoffibers.Fibroushasamuchmoregeneralmeaningthan
which are easily separated into long, thin, flexible fibers when
asbestos. While it is correct that all asbestos minerals are
crushed or processed.
fibrous, not all minerals having fibrous habits are asbestos.
3.1.2.1 Discussion—Included in the definition are the as-
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(tremoliteasbestos);andactinolite(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 nomenclature of the International Mineralogi-
fiber bundles, touch, are attached to, or partially concealed by
cal Association (3).
a single particle or connected group of non-fibrous particles.
Chemical Abstract Service
The exposed fiber must meet the fiber definition (see section
Asbestos
No.
3.2.6). Matrices occur as two varieties—disperse matrices and
Chrysotile 12001-29-5
Crocidolite 12001-28-4
compact matrices.
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
Actinolite Asbestos 77536-66-4
seen either within the structure or projecting from it, such that
3.1.3 fibril—a single fiber that cannot be separated into
the dimensions of individual fibers and bundles cannot be
smaller components without losing its fibrous properties or
unambiguously determined.
appearance.
3.2.9.2 disperse matrix—a structure consisting of a particle
orlinkedgroupofparticles,withoverlappingorattachedfibers
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
oriented 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
preparedandtransferredtoaTEMgridusingthedirecttransfer
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.
3.2.6 fiber—a structure having a minimum length of 0.5µ m
5. Significance and Use
with an aspect ratio of 5 to 1 or greater and substantially
5.1 This microvacuum sampling and indirect analysis
parallel sides (4). Fibers are assumed to have a cylindrical
method is used for the general testing of non-airborne dust
shape (5).
samples for asbestos. It is used to assist in the evaluation of
dustthatmaybefoundonsurfacesinbuildings,suchasceiling
The boldface numbers refer to the list of references at the end of the test
tiles, shelving, electrical components, duct work, carpet, etc.
method.
This test method provides an estimate of the mass surface
Thenon-asbestiformvariationsofthemineralsindicatedin3.1.2havedifferent
Chemical Abstract Service (CAS) numbers. loading of asbestos in the dust reported as either the mass of
D5756 − 02 (2008)
asbestos per unit area or as the mass of asbestos per mass of 7.4 High Effıciency Particulate Air (HEPA), filtered nega-
sampled dust as derived from a quantitative TEM analysis. tive flow hood.
5.1.1 This test method does not describe procedures or
7.5 Exhaust or Fume Hood.
techniques required to evaluate the safety or habitability of
7.6 Particle-Free Water (ASTM Type II, see Specification
buildings with asbestos-containing materials, or compliance
D1193).
with federal, state, or local regulations or statutes. It is the
user’s responsibility to make these determinations. 7.7 Glass Beakers, 50 mL.
5.1.2 At present, no relationship has been established be-
7.8 Glass Sample Containers, with wide mouth screw cap
tweenasbestos-containingdustasmeasuredbythistestmethod
(200 mL), or equivalent sealable container (height of the glass
and potential human exposure to airborne asbestos.
samplecontainershouldbeapproximately13cmhighby6cm
Accordingly, the users should consider other available infor-
wide).
mationintheirinterpretationofthedataobtainedfromthistest
7.9 Waterproof Markers.
method.
7.10 Forceps (tweezers).
5.2 Thisdefinitionofdustacceptsallparticlessmallenough
to pass througha1mm screen. Thus, a single, large asbestos- 7.11 Ultrasonic Bath,tabletopmodel(100W,approximate,
see 22.5).
containing particle(s) (from the large end of the particle size
distribution) disassembled during sample preparation may
7.12 Graduated Pipettes, 1, 5, and 10 mL sizes, glass or
result in anomalously large asbestos surface loading results in
plastic.
the TEM analyses of that sample. Conversely, failure to
7.13 Filter Funnel, 25 mm or 47 mm (either glass or
disaggregate large particles may result in anomalously low
disposable).Filterfunnelassemblies,eitherglassordisposable
asbestos mass surface loadings. It is, therefore, recommended
plastic, and using either a 25 mm or 47 mm diameter filter.
that multiple independent samples be secured from the same
area, and that a minimum of three samples be analyzed by the 7.14 Side Arm Filter Flask, 1000 mL.
entire procedure.
7.15 Mixed Cellulose Ester (MCE) Membrane Filters,25or
47 mm diameter, ≤0.22 µm and 5 µm pore size.
6. Interferences
7.16 Polycarbonate (PC) Filters, 25 or 47 mm diameter,≤
6.1 The following minerals have properties (that is, chemi-
0.2 µm pore size.
cal or crystalline structure) which are very similar to asbestos
7.17 Storage Containers, for the 25 or 47 mm filters (for
minerals and may interfere with the analysis by causing false
archiving).
positives to be recorded during the test. Therefore, literature
references for these materials must be maintained in the 7.18 Glass Slides.
laboratory for comparison to asbestos minerals so that they are
7.19 Scalpel Blades.
not misidentified as asbestos minerals.
7.20 Cabinet-type Desiccator, or low temperature drying
6.1.1 Antigorite.
oven.
6.1.2 Palygorskite (Attapulgite).
6.1.3 Halloysite.
8. Reagents and Materials
6.1.4 Pyroxenes.
8.1 Purity of Reagents—Reagent grade chemicals shall be
6.1.5 Sepiolite.
used in all tests. Unless otherwise indicated, it is intended that
6.1.6 Vermiculite scrolls.
all reagents conform to the specifications of the Committee on
6.1.7 Fibrous talc.
Analytical Reagents of theAmerican Chemical Society where
6.1.8 Hornblende and other amphiboles not listed in 5.1.3. 6
such specifications are available. Other grades may be used,
6.2 Collection of any dust particles greater than 1 mm in provided it is first ascertained that the reagent is of sufficiently
size in this test method may cause an interference and, high purity to permit its use without lessening the accuracy of
therefore, should be avoided.
the determination.
8.2 Acetone.
7. Apparatus
8.3 Dimethylformamide (DMF).
7.1 Transmission Electron Microscope (TEM), an 80 to 120
8.4 Chloroform.
kV TEM, capable of performing electron diffraction, with a
fluorescent screen inscribed with calibrated gradations, is 8.5 1-methyl-2-pyrrolidone.
required. The TEM must be equipped with energy dispersive
8.6 Glacial Acetic Acid.
X-ray spectroscopy (EDXA) and it must have a scanning
transmission electron microscopy (STEM) attachment or be
Reagent Chemicals, American Chemical Society Specifications , American
capable of producing a spot size of less than 250 nm in
Chemical Society, Washington, DC. For suggestions on
...
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