ASTM D5755-95
(Test Method)Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Structure Number Concentrations
Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Structure Number Concentrations
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 the number of asbestos structures per unit area of sampled surface.
1.1.1 If an estimate of the asbestos mass is to be determined, the user is referred to Test Method D5756.
1.2 This test method describes the equipment and procedures necessary for sampling, by a microvacuum technique, non-airborne dust for levels of asbestos structures. 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 and will vary among substrates. Properties influencing collection efficiency include surface texture, adhesiveness, electrostatic properties and other factors.
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 structures starting from approximately 1000 asbestos structures per square centimetre.
1.4.1 The procedure outlined in this test method employs an indirect sample preparation technique. It is intended to disperse aggregated asbestos into fundamental fibrils, fiber bundles, clusters, or matrices that can be more accurately quantified by transmission electron microscopy. However, as with all indirect sample preparation techniques, the asbestos observed for quantification 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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Designation: D 5755 – 95
Standard Test Method for
Microvacuum Sampling and Indirect Analysis of Dust by
Transmission Electron Microscopy for Asbestos Structure
Number Concentrations
This standard is issued under the fixed designation D 5755; 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 standard. The values given in parentheses are for information
only.
1.1 This test method covers a procedure to ( a) identify
1.6 This standard does not purport to address all of the
asbestos in dust and (b) provide an estimate of the concentra-
safety concerns, if any, associated with its use. It is the
tion of asbestos in the sampled dust reported as the number of
responsibility of the user of this standard to establish appro-
asbestos structures per unit area of sampled surface.
priate safety and health practices and determine the applica-
1.1.1 If an estimate of the asbestos mass is to be determined,
bility of regulatory limitations prior to use.
the user is referred to Test Method D 5756.
1.2 This test method describes the equipment and proce-
2. Referenced Documents
dures necessary for sampling, by a microvacuum technique,
2.1 ASTM Standards:
non-airborne dust for levels of asbestos structures. The non-
D 1193 Specification for Reagent Water
airborne sample is collected inside a standard filter membrane
D 1739 Test Method for the Collection and Measurement of
cassette from the sampling of a surface area for dust which may
Dustfall (Settleable Particulate Matter)
contain asbestos.
D 3195 Practice for Rotameter Calibration
1.2.1 This procedure uses a microvacuuming sampling tech-
D 3670 Guide for Determination of Precision and Bias of
nique. The collection efficiency of this technique is unknown
Methods of Committee D-22
and will vary among substrates. Properties influencing collec-
D 5756 Test Method for Microvacuum Sampling and Indi-
tion efficiency include surface texture, adhesiveness, electro-
rect Analysis of Dust by Transmission Electron Micros-
static properties and other factors.
copy for Asbestos Mass Concentration
1.3 Asbestos identified by transmission electron microscopy
(TEM) is based on morphology, selected area electron diffrac-
3. Terminology
tion (SAED), and energy dispersive X-ray analysis (EDXA).
3.1 Definitions:
Some information about structure size is also determined.
3.1.1 asbestiform—a special type of fibrous habit in which
1.4 This test method is generally applicable for an estimate
the fibers are separable into thinner fibers and ultimately into
of the concentration of asbestos structures starting from ap-
fibrils. This habit accounts for greater flexibility and higher
proximately 1000 asbestos structures per square centimetre.
tensile strength than other habits of the same mineral. For more
1.4.1 The procedure outlined in this test method employs an
information on asbestiform mineralogy, see Refs (1), (2) and
indirect sample preparation technique. It is intended to disperse
(3).
aggregated asbestos into fundamental fibrils, fiber bundles,
3.1.2 asbestos—a collective term that describes a group of
clusters, or matrices that can be more accurately quantified by
naturally occurring, inorganic, highly fibrous, silicate domi-
transmission electron microscopy. However, as with all indi-
nated minerals, which are easily separated into long, thin,
rect sample preparation techniques, the asbestos observed for
flexible fibers when crushed or processed.
quantification may not represent the physical form of the
3.1.2.1 Discussion—Included in the definition are the as-
asbestos as sampled. More specifically, the procedure de-
bestiform varieties of: serpentine (chrysotile); riebeckite (cro-
scribed neither creates nor destroys asbestos, but it may alter
cidolite); grunerite (grunerite asbestos); anthophyllite (antho-
the physical form of the mineral fibers.
phyllite asbestos); tremolite (tremolite asbestos); and actinolite
1.5 The values stated in SI units are to be regarded as the
(actinolite asbestos). The amphibole mineral compositions are
1 2
This test method is under the jurisdiction of ASTM Committee D-22 on Annual Book of ASTM Standards, Vol 11.01.
Sampling and Analysis of Atmospheresand is the direct responsibility of Subcom- Annual Book of ASTM Standards, Vol 11.03.
mittee D22.07on Sampling and Analysis of Asbestos. The boldface numbers in parentheses refer to the list of references at the end of
Current edition approved August 15, 1995. Published October 1995. this test method.
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 5755
defined according to nomenclature of the International Miner- 4. Summary of Test Method
alogical Association (3).
4.1 The sample is collected by vacuuming a known surface
Asbestos Chemical Abstract Service No.
area with a standard 25 or 37 mm air sampling cassette using
Chrysotile 12001-29-5
a plastic tube that is attached to the inlet orifice which acts as
Crocidolite 12001-28-4
a nozzle. The sample is transferred from inside the cassette to
Grunerite Asbestos 12172-73-5
Anthophyllite Asbestos 77536-67-5
an aqueous solution of known volume. Aliquots of the suspen-
Tremolite Asbestos 77536-68-6
sion are then filtered through a membrane. A section of the
Actinolite Asbestos 77536-66-4
membrane is prepared and transferred to a TEM grid using the
3.1.3 fibril—a single fiber that cannot be separated into
direct transfer method. The asbestiform structures are identi-
smaller components without losing its fibrous properties or
fied, sized, and counted by TEM, using SAED and EDXA at a
appearance.
magnification of 15 000 to 20 000X.
3.2 Definitions of Terms Specific to This Standard:
5. Significance and Use
3.2.1 aspect ratio—the ratio of the length of a fibrous
particle to its average width. 5.1 This microvacuum sampling and indirect analysis
method is used for the general testing of non-airborne dust
3.2.2 bundle—a structure composed of three or more fibers
samples for asbestos. It is used to assist in the evaluation of
in a parallel arrangement with the fibers closer than one fiber
dust that may be found on surfaces in buildings such as ceiling
diameter to each other.
tiles, shelving, electrical components, duct work, carpet, etc.
3.2.3 cluster—a structure with fibers in a random arrange-
This test method provides an index of the concentration of
ment such that all fibers are intermixed and no single fiber is
asbestos structures in the dust per unit area analyzed as derived
isolated from the group; groupings of fibers must have more
from a quantitative TEM analysis.
than two points touching.
5.1.1 This test method does not describe procedures or
3.2.4 debris—materials that are of an amount and size
techniques required to evaluate the safety or habitability of
(particles greater than 1 mm in diameter) that can be visually
buildings with asbestos-containing materials, or compliance
identified as to their source.
with federal, state, or local regulations or statutes. It is the
3.2.5 dust—any material composed of particles in a size
user’s responsibility to make these determinations.
range of #1 mm and large enough to settle by virtue of their
5.1.2 At present, a single direct relationship between
weight from the ambient air (see definition for settleable
asbestos-containing dust and potential human exposure does
particulate matter in Test Method D 1739).
not exist. Accordingly, the user should consider these data in
3.2.6 fiber—a structure having a minimum length of 0.5 μm,
relationship to other available information in their evaluation.
an aspect ratio of 5:1 or greater, and substantially parallel sides
5.2 This test method uses the definition, settleable particu-
(4).
late material, found in Test Method D 1739 as the definition of
3.2.7 fibrous—of a mineral composed of parallel, radiating,
dust. This definition accepts all particles small enough to pass
or interlaced aggregates of fibers, from which the fibers are
througha1mm (No. 18) screen. Thus, a single, large asbestos
sometimes separable. That is, the crystalline aggregate may be
containing particle(s) (from the large end of the particle size
referred to as fibrous even if it is not composed of separable
distribution) dispersed during sample preparation may result in
fibers, but has that distinct appearance. The term fibrous is used
anomalously large asbestos concentration results in the TEM
in a general mineralogical way to describe aggregates of grains
analyses of that sample. It is, therefore, recommended that
that crystallize in a needle-like habit and appear to be com-
multiple independent samples are secured from the same area,
posed of fibers. Fibrous has a much more general meaning than
and a minimum of three samples analyzed by the entire
asbestos. While it is correct that all asbestos minerals are
procedure.
fibrous, not all minerals having fibrous habits are asbestos.
3.2.8 indirect preparation—a method in which a sample
6. Interferences
passes through one or more intermediate steps prior to final
6.1 The following minerals have properties (that is, chemi-
filtration.
cal or crystalline structure) which are very similar to asbestos
3.2.9 matrix—a structure in which one or more fibers, or
minerals and may interfere with the analysis by causing a false
fiber bundles that are touching, are attached to, or partially
positive to be recorded during the test. Therefore, literature
concealed by a single particle or connected group of non-
references for these materials must be maintained in the
fibrous particles. The exposed fiber must meet the fiber
laboratory for comparison to asbestos minerals so that they are
definition (see 3.2.6).
not misidentified as asbestos minerals.
3.2.10 structures—a term that is used to categorize all the
6.1.1 Antigorite.
types of asbestos particles which are recorded during the
6.1.2 Palygorskite (Attapulgite).
analysis (such as fibers, bundles, clusters, and matrices). Final
6.1.3 Halloysite.
results of the test are always expressed in asbestos structures
6.1.4 Pyroxenes.
per square centimetre.
6.1.5 Sepiolite.
6.1.6 Vermiculite scrolls.
6.1.7 Fibrous talc.
5 6.1.8 Hornblende and other amphiboles other than those
The non-asbestiform variations of the minerals indicated in 5.1.3 have different
Chemical Abstract Service (CAS) numbers. listed in 3.1.2.
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 5755
6.2 Collecting any dust particles greater than 1 mm in size 7.22 Chloroform, reagent grade.
in this test method may cause an interference and, therefore, 7.23 Acetone, reagent grade.
must be avoided. 7.24 Dimethylformamide (DMF).
7.25 Glacial Acetic Acid.
7. Materials and Equipment
7.26 1-methyl-2-pyrrolidone.
7.27 Plasma Asher, low temperature.
7.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that 7.28 pH Paper.
7.29 Air Sampling Pump, low volume personal-type, ca-
all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society, where pable of achieving a flow rate of 1 to 5 L/min.
7.30 Rotameter.
such specifications are available. Other grades may be used,
provided it is first ascertained that the reagent is of sufficiently 7.31 Air Sampling Cassettes, 25 mm or 37 mm, containing
high purity to permit its use without lessening the accuracy of 0.8μ m or smaller pore size MCE or PC filters.
the determination. 7.32 Cork Borer, 7 mm.
7.2 Transmission Electron Microscope (TEM),an80to120 7.33 Non-Asbestos Mineral, references as outlined in 6.1.
kV TEM, capable of performing electron diffraction, with a 7.34 Asbestos Standards, as outlined in 3.1.2.
fluorescent screen inscribed with calibrated gradations, is 7.35 Tygon Tubing, or equivalent.
required. The TEM must be equipped with energy dispersive 7.36 Small Vacuum Pump, that can maintain a pressure of 92
X-ray spectroscopy (EDXA) and it must have a scanning kPa.
transmission electron microscopy (STEM) attachment or be 7.37 Petri Dishes, large glass, approximately 90 mm in
capable of producing a spot size of less than 250 nm in diameter.
7.38 Jaffe Washer, stainless steel or aluminum mesh screen,
diameter in crossover.
7.3 Energy Dispersive X-ray System (EDXA). 30 to 40 mesh, and approximately 75 mm by 50 mm in size.
7.39 Copper TEM Finder Grids, 200 mesh.
7.4 High Vacuum Carbon Evaporator, with rotating stage.
7.5 High Effıciency Particulate Air (HEPA), filtered nega- 7.40 Carbon Evaporator Rods.
7.41 Lens Tissue.
tive flow hood.
7.6 Exhaust or Fume Hood. 7.42 Ashless Filter Paper Filters, 90 mm diameter.
7.43 Gummed Paper Reinforcement Rings.
7.7 Particle-free Water (ASTM Type II, see Specification
D 1193). 7.44 Wash Bottles, plastic.
7.45 Reagent Alcohol, HPLC Grade (Fisher A995 or equiva-
7.8 Glass Beakers (50 mL).
7.9 Glass Sample Containers, with wide mouth screw cap lent).
7.46 Opening Mesh Screen, plastic, 1.0 by 1.0 mm,
(200 mL) or equivalent sealable container (height of the glass
sample container should be approximately 13 cm high by 6 cm (Spectra-Mesh #146410 or equivalent).
wide). 7.47 Diffraction Grating Replica.
7.10 Waterproof Markers.
8. Sampling Procedure for Microvacuum Technique
7.11 Forceps (tweezers).
7.12 Ultrasonic Bath, table top model (100 W). 8.1 For sampling asbestos-containing dust in either indoor
7.13 Graduated Pipettes (1, 5, 10 mL sizes), glass or or outdoor environments, commercially available cassettes
plastic. must be used. Air monitoring cassettes containing 25 mm or 37
7.14 Filter Funnel, either 25 mm or 47 mm, glass or mm diameter mixed cellulose ester (MCE) or polycarbonate
(PC) filter membranes with a pore size less than or equal to 0.8
disposable. Filter funnel assemblies, either glass or disposable
plastic, and using either a 25 mm or 47 mm diameter filter. μm are required (7.31). The number of samples collected
depends upon the specific circumstances of the study.
7.15 Side Arm Filter Flask, 1000 mL.
7.16 Mixed Cellulose Ester (MCE) Membrane Filters,25or 8.2 Maintain a log of all pertinent sampling information and
sampling locations.
47 mm diameter, #0.22 μm and 5 μm pore size.
7.17 Polycarbonate (PC) Filters, 25 or 47 mm diameter, 8.3 Sampling
...
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