ASTM D5755-09(2014)e1

Standard Test Method for Microvacuum Sampling and Indirect Analysis of Dust by Transmission Electron Microscopy for Asbestos Structure Number Surface Loading (Withdrawn 2023)

SIGNIFICANCE AND USE
5.1 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 index of the surface loading of asbestos structures in the dust per unit area analyzed as derived from a quantitative TEM analysis.  
5.1.1 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.  
5.1.2 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.  
5.2 This definition of dust accepts all particles small enough to pass through a 1-mm (No. 18) screen. Thus, a single, large asbestos containing particle(s) (from the large end of the particle size distribution) dispersed during sample preparation may result in anomalously large asbestos surface loading results in the TEM analyses of that sample. It is, therefore, recommended that multiple independent samples are 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 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 surface loading 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 limita...

General Information

• Status: Withdrawn
• Publication Date: 31-Mar-2014
• Withdrawal Date: 09-Jul-2023
• ICS: 13.040.20 - Ambient atmospheres
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.07 - Sampling, Analysis, Management of Asbestos, and Other Microscopic Particles

Standards Content (Sample)

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
´1
Designation: D5755 − 09 (Reapproved 2014)
Standard Test Method for
Microvacuum Sampling and Indirect Analysis of Dust by
Transmission Electron Microscopy for Asbestos Structure
Number Surface Loading
This standard is issued under the fixed designation D5755; 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 (´) indicates an editorial change since the last revision or reapproval.
ε NOTE—Warning notes were editorially updated throughout in April 2014.
1. Scope asbestos as sampled. More specifically, the procedure de-
scribed neither creates nor 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 estimate of the surface
loading of asbestos in the sampled dust reported as the number 1.5 The values stated in SI units are to be regarded as the
of asbestos structures per unit area of sampled surface.
standard. The values given in parentheses are for information
1.1.1 If an estimate of the asbestos mass is to be determined, only.
the user is referred to Test Method D5756.
1.6 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.2 This test method describes the equipment and proce-
dures necessary for sampling, by a microvacuum technique, responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
non-airborne dust for levels of asbestos structures. The non-
airborne sample is collected inside a standard filter membrane mine the applicability of regulatory limitations prior to use.
1.7 This international standard was developed in accor-
cassette from the sampling of a surface area for dust which may
contain asbestos. dance with internationally recognized principles on standard-
ization established in the Decision on Principles for the
1.2.1 This procedure uses a microvacuuming sampling tech-
nique. The collection efficiency of this technique is unknown Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
and will vary among substrates. Properties influencing collec-
tion efficiency include surface texture, adhesiveness, electro- Barriers to Trade (TBT) Committee.
static properties and other factors.
2. Referenced Documents
1.3 Asbestos identified by transmission electron microscopy
(TEM) is based on morphology, selected area electron diffrac-
2.1 ASTM Standards:
tion (SAED), and energy dispersive X-ray analysis (EDXA). D1193 Specification for Reagent Water
Some information about structure size is also determined.
D3195 Practice for Rotameter Calibration
D3670 Guide for Determination of Precision and Bias of
1.4 This test method is generally applicable for an estimate
Methods of Committee D22
of the surface loading of asbestos structures starting from
D5756 Test Method for Microvacuum Sampling and Indirect
approximately 1000 asbestos structures per square centimetre.
Analysis of Dust by Transmission Electron Microscopy
1.4.1 The procedure outlined in this test method employs an
for Asbestos Mass Surface Loading
indirect sample preparation technique. It is intended to disperse
D6620 Practice for Asbestos Detection Limit Based on
aggregated asbestos into fundamental fibrils, fiber bundles,
Counts
clusters, or matrices that can be more accurately quantified by
E177 Practice for Use of the Terms Precision and Bias in
transmission electron microscopy. However, as with all indi-
ASTM Test Methods
rect sample preparation techniques, the asbestos observed for
E691 Practice for Conducting an Interlaboratory Study to
quantification may not represent the physical form of the
Determine the Precision of a Test Method
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.07 on Sampling,
Analysis, Management of Asbestos, and Other Microscopic Particles. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved April 1, 2014. Published May 2014. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 1995. Last previous edition approved in 2009 as D5755 – 09. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D5755-09R14E01. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D5755 − 09 (2014)
3. Terminology 3.2.7.1 Discussion—The term fibrous is used in a general
mineralogical way to describe aggregates of grains that crys-
3.1 Definitions:
tallize in a needle-like habit and appear to be composed of
3.1.1 asbestiform—a special type of fibrous habit in which
fibers. Fibrous has a much more general meaning than asbes-
the fibers are separable into thinner fibers and ultimately into
tos. While it is correct that all asbestos minerals are fibrous, not
fibrils. This habit accounts for greater flexibility and higher
all minerals having fibrous habits are asbestos.
tensile strength than other habits of the same mineral. For more
3.2.8 indirect preparation—a method in which a sample
information on asbestiform mineralogy, see Refs (1-3).
passes through one or more intermediate steps prior to final
3.1.2 asbestos—a collective term that describes a group of
filtration.
naturally occurring, inorganic, highly fibrous, silicate domi-
3.2.9 matrix—a structure in which one or more fibers, or
nated minerals, which are easily separated into long, thin,
fiber bundles that are touching, are attached to, or partially
flexible fibers when crushed or processed.
concealed by a single particle or connected group of non-
3.1.2.1 Discussion—Included in the definition are the as-
fibrous particles in which the exposed fiber must meet the fiber
bestiform varieties of: serpentine (chrysotile); riebeckite (cro-
definition (see 3.2.6).
cidolite); grunerite (grunerite asbestos); anthophyllite (an-
3.2.10 structures—a term that is used to categorize all the
thophyllite asbestos); tremolite (tremolite asbestos); and
types of asbestos particles which are recorded during the
actinolite (actinolite asbestos). The amphibole mineral compo-
analysis (such as fibers, bundles, clusters, and matrices).
sitions are defined according to nomenclature of the Interna-
3.2.10.1 Discussion—Final results of the test are always
tional Mineralogical Association (3).
expressed in asbestos structures per square centimetre.
A
Asbestos Chemical Abstract Service No.
Chrysotile 12001-29-5
4. Summary of Test Method
Crocidolite 12001-28-4
Grunerite Asbestos 12172-73-5
4.1 The sample is collected by vacuuming a known surface
Anthophyllite Asbestos 77536-67-5
Tremolite Asbestos 77536-68-6 area with a standard 25 or 37-mm air sampling cassette using
Actinolite Asbestos 77536-66-4
a plastic tube that is attached to the inlet orifice which acts as
a nozzle. The sample is transferred from inside the cassette to
A
The non-asbestiform variations of the minerals indicated in 3.1.2.1 have different
an aqueous suspension of known volume. Aliquots of the
Chemical Abstract Service (CAS) numbers.
suspension are then filtered through a membrane. A section of
3.1.3 fibril—a single fiber that cannot be separated into
the membrane is prepared and transferred to a TEM grid using
smaller components without losing its fibrous properties or
the direct transfer method. The asbestiform structures are
appearance.
identified, sized, and counted by TEM, using SAED and
3.2 Definitions of Terms Specific to This Standard:
EDXA at a magnification of 15 000 to 20 000×.
3.2.1 aspect ratio—the ratio of the length of a fibrous
5. Significance and Use
particle to its average width.
5.1 This microvacuum sampling and indirect analysis
3.2.2 bundle—a structure composed of three or more fibers
in a parallel arrangement with the fibers closer than one fiber method is used for the general testing of non-airborne dust
samples for asbestos. It is used to assist in the evaluation of
diameter to each other.
dust that may be found on surfaces in buildings such as ceiling
3.2.3 cluster—a structure with fibers in a random arrange-
tiles, shelving, electrical components, duct work, carpet, etc.
ment such that all fibers are intermixed and no single fiber is
This test method provides an index of the surface loading of
isolated from the group; groupings of fibers must have more
asbestos structures in the dust per unit area analyzed as derived
than two points touching.
from a quantitative TEM analysis.
3.2.4 debris—materials that are of an amount and size
5.1.1 This test method does not describe procedures or
(particles greater than 1 mm in diameter) that can be visually
techniques required to evaluate the safety or habitability of
identified as to their source.
buildings with asbestos-containing materials, or compliance
3.2.5 dust—any material composed of particles in a size
with federal, state, or local regulations or statutes. It is the
range of <1 mm.
user’s responsibility to make these determinations.
5.1.2 At present, no relationship has been established be-
3.2.6 fiber—a structure having a minimum length of 0.5 µm,
tween asbestos-containing dust as measured by this test method
an aspect ratio of 5:1 or greater, and substantially parallel sides
and potential human exposure to airborne asbestos.
(4).
Accordingly, the users should consider other available infor-
3.2.7 fibrous—of a mineral composed of parallel, radiating,
mation in their interpretation of the data obtained from this test
or interlaced aggregates of fibers, from which the fibers are
method.
sometimes separable: that is, the crystalline aggregate may be
referred to as fibrous even if it is not composed of separable 5.2 This definition of dust accepts all particles small enough
fibers, but has that distinct appearance. to pass through a 1-mm (No. 18) screen. Thus, a single, large
asbestos containing particle(s) (from the large end of the
particle size distribution) dispersed during sample preparation
3 may result in anomalously large asbestos surface loading
The boldface numbers in parentheses refer to a list of references at the end of
this standard. results in the TEM analyses of that sample. It is, therefore,
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D5755 − 09 (2014)
recommended that multiple independent samples are secured 7.8 Glass Beakers (50 mL).
from the same area, and that a minimum of three samples be
7.9 Glass Sample Containers, with wide mouth screw cap
analyzed by the entire procedure.
(200 mL) or equivalent sealable container (height of the glass
sample container should be approximately 13 cm high by 6 cm
6. Interferences
wide).
6.1 The following minerals have properties (that is, chemi-
7.10 Waterproof Markers.
cal or crystalline structure) which are very similar to asbestos
7.11 Forceps (tweezers).
minerals and may interfere with the analysis by causing a false
positive to be recorded during the test. Therefore, literature
7.12 Ultrasonic Bath, table top model (100 W).
references for these materials must be maintained in the
7.13 Graduated Pipettes (1, 5, 10-mL sizes), glass or
laboratory for comparison to asbestos minerals so that they are
plastic.
not misidentified as asbestos minerals.
7.14 Filter Funnel, either 25 mm or 47 mm, glass or
6.1.1 Antigorite.
disposable. Filter funnel assemblies, either glass or disposable
6.1.2 Palygorskite (Attapulgite).
plastic, and using either a 25-mm or 47-mm diameter filter.
6.1.3 Halloysite.
6.1.4 Pyroxenes.
7.15 Side Arm Filter Flask, 1000 mL.
6.1.5 Sepiolite.
7.16 Mixed Cellulose Ester (MCE) Membrane Filters, 25 or
6.1.6 Vermiculite scrolls.
47-mm diameter, ≤0.22-µm and 5-µm pore size.
6.1.7 Fibrous talc.
7.17 Polycarbonate (PC) Filters, 25 or 47-mm diameter,
6.1.8 Hornblende and other amphiboles other than those
≤0.2-µm pore size.
listed in 3.1.2.
7.18 Storage Containers, for the 25 or 47-mm filters (for
6.2 Collecting any dust particles greater than 1 mm in size
archiving).
in this test method may cause an interference and, therefore,
must be avoided.
7.19 Glass Slides, approximately 76 by 25 mm in size.
7.20 Scalpel Blades, No. 10, or equivalent.
7. Materials and Equipment
7.21 Cabinet-type Desiccator, or low temperature drying
7.1 Purity of Reagents—Reagent grade chemicals shall be
oven.
used in all tests. Unless otherwise indicated, it is intended that
all reagents conform to the specifications of the Committee on 7.22 Chloroform, reagent grade.
Analytical Reagents of the American Chemical Society, where
7.23 Acetone, reagent grade.
such specifications are available. Other grades may be used,
7.24 Dimethylformamide (DMF).
provided it is first ascertained that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy of 7.25 Glacial Acetic Acid.
the determination.
7.26 1-methyl-2-pyrrolidone.
7.2 Transmission Electron Microscope (TEM), an 80 to 120
7.27 Plasma Asher, low temperature.
kV TEM, capable of performing electron diffraction, with a
7.28 pH Paper.
fluorescent screen inscribed with calibrated gradations, is
required. The TEM must be equipped with energy dispersive
7.29 Air Sampling Pump, low volume personal-type, ca-
X-ray spectroscopy (EDXA) and it must have a scanning
pable of achieving a flow rate of 1 to 5 L/min.
transmission electron microscopy (STEM) attachment or be
7.30 Rotameter.
capable of producing a spot size of less than 250 nm in
7.31 Air Sampling Cassettes, 25 mm or 37 mm, containing
diameter in crossover.
0.8 µm or smaller pore size MCE or PC filters.
7.3 Energy Dispersive X-ray System (EDXA).
7.32 Cork Borer, 7 mm.
7.4 High Vacuum Carbon Evaporator, with rotating stage.
7.33 Non-Asbestos Mineral, references as outlined in 6.1.
7.5 High Effıciency Particulate Air (HEPA), filtered nega-
7.34 Asbestos Standards, as outlined in 3.1.2.
tive flow hood.
7.35 Tygon Tubing, or equivalent.
7.6 Exhaust or Fume Hood.
7.36 Small Vacuum Pump, that can maintain a pressure of 92
7.7 Particle-free Water (ASTM Type II, see Specification
kPa.
D1193).
7.37 Petri Dishes, large glass, approximately 90 mm in
diameter.
Reagent Chemicals, American Chemical Society Specifications, American
7.38 Jaffe Washer, stainless steel or aluminum mesh screen,
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
30 to 40 mesh, and approximately 75 mm by 50 mm in size.
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemica
...