Standard Test Method for Determining Concentration of Airborne Single-Crystal Ceramic Whiskers in the Workplace Environment by Scanning Electron Microscopy (Withdrawn 2020)

SIGNIFICANCE AND USE
The SCCW may be present in the workplace atmosphere where these materials are manufactured, processed, transported, or used. This test method can be used to monitor airborne concentrations of SCCW fibers in these environments. It may be employed as part of a personal or area monitoring strategy.
This test method is based on morphology and elemental composition. The analysis technique has the ability to identify SCCW.
Note 1—This test method assumes that the analyst is familiar with the operation of SEM/EDS instrumentation and the interpretation of data obtained using these techniques.
This test method is not appropriate for measurement of fibers with diameters ≤0.10 to 0.25 μm due to visibility limitations associated with SEM. The TEM method may be used to provide additional size information of SCCW if needed (see Practice D6058 for additional information on the use of this test method).
Results from the use of this test method shall be reported along with 95 % confidence limits for the samples being studied. Individual laboratories shall determine their intralaboratory coefficient of variation and use it for reporting 95 % confidence limits (1,3,4).
SCOPE
1.1 This test method covers the sampling methods and analysis techniques used to assess the airborne concentration and size distribution of single-crystal ceramic whiskers (SCCW), such as silicon carbide and silicon nitride, which may occur in and around the workplace where these materials are manufactured, processed, transported, or used. This test method is based on the collection of fibers by filtration of a known quantity of air through a filter. The filter is subsequently evaluated with a scanning electron microscope (SEM) for the number of fibers meeting appropriately selected morphological and compositional criteria. This test method has the ability to distinguish among many different types of fibers based on energy dispersive X-ray spectroscopy (EDS) analysis. This test method may be appropriate for other man-made mineral fibers (MMMF).
1.2 This test method is applicable to the quantitation of fibers on a collection filter that are greater than 5 μm in length, less than 3 μm in width, and have an aspect ratio equal to or greater than 5:1. The data are directly convertible to a statement of concentration per unit volume of air sampled. This test method is limited by the diameter of the fibers visible by SEM (typically greater than 0.10 to 0.25 μm in width as determined in 12.1.5) and the amount of coincident interference particles.  
1.3 A more definitive analysis may be necessary to confirm the presence of fibers with diameters ≤0.10 to 0.25 μm in width. For this purpose, a transmission electron microscope (TEM) is appropriate. The use of the TEM method for the identification and size measurement of SCCW is described in Practice D6058 and Test Method D6056.
1.4 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.  
1.5 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.
WITHDRAWN RATIONALE
This test method covers the sampling methods and analysis techniques used to assess the airborne concentration and size distribution of single-crystal ceramic whiskers (SCCW), such as silicon carbide and silicon nitride, which may occur in and around the workplace where these materials are manufactured, processed, transported, or used.
Formerly under the jurisdiction of Committee D22 on Air Quality, this test method was withdrawn in January 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approv...

General Information

Status
Withdrawn
Publication Date
30-Sep-2011
Withdrawal Date
08-Jan-2020
Current Stage
Ref Project

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ASTM D6059-96(2011) - Standard Test Method for Determining Concentration of Airborne Single-Crystal Ceramic Whiskers in the Workplace Environment by Scanning Electron Microscopy (Withdrawn 2020)
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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: D6059 − 96 (Reapproved 2011)
Standard Test Method for
Determining Concentration of Airborne Single-Crystal
Ceramic Whiskers in the Workplace Environment by
Scanning Electron Microscopy
This standard is issued under the fixed designation D6059; 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 1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method covers the sampling methods and
responsibility of the user of this standard to establish appro-
analysis techniques used to assess the airborne concentration
priate safety and health practices and determine the applica-
and size distribution of single-crystal ceramic whiskers
bility of regulatory limitations prior to use.
(SCCW),suchassiliconcarbideandsiliconnitride,whichmay
occur in and around the workplace where these materials are
2. Referenced Documents
manufactured, processed, transported, or used. This test
2.1 ASTM Standards:
method is based on the collection of fibers by filtration of a
D1193Specification for Reagent Water
knownquantityofairthroughafilter.Thefilterissubsequently
D1356Terminology Relating to Sampling and Analysis of
evaluated with a scanning electron microscope (SEM) for the
Atmospheres
numberoffibersmeetingappropriatelyselectedmorphological
D4532Test Method for Respirable Dust in Workplace At-
and compositional criteria. This test method has the ability to
mospheres Using Cyclone Samplers
distinguish among many different types of fibers based on
D6056Test Method for Determining Concentration of Air-
energydispersiveX-rayspectroscopy(EDS)analysis.Thistest
borne Single-Crystal Ceramic Whiskers in the Workplace
method may be appropriate for other man-made mineral fibers
Environment by Transmission Electron Microscopy
(MMMF).
D6057Test Method for Determining Concentration of Air-
1.2 This test method is applicable to the quantitation of
borne Single-Crystal Ceramic Whiskers in the Workplace
fibers on a collection filter that are greater than 5 µm in length,
Environment by Phase Contrast Microscopy
less than 3 µm in width, and have an aspect ratio equal to or
D6058Practice for Determining Concentration of Airborne
greater than 5:1. The data are directly convertible to a
Single-Crystal Ceramic Whiskers in the Workplace Envi-
statementofconcentrationperunitvolumeofairsampled.This
ronment
test method is limited by the diameter of the fibers visible by
E691Practice for Conducting an Interlaboratory Study to
SEM (typically greater than 0.10 to 0.25 µm in width as
Determine the Precision of a Test Method
determined in 12.1.5) and the amount of coincident interfer-
E766Practice for Calibrating the Magnification of a Scan-
ence particles.
ning Electron Microscope
1.3 Amore definitive analysis may be necessary to confirm
the presence of fibers with diameters ≤0.10 to 0.25 µm in 3. Terminology
width. For this purpose, a transmission electron microscope
3.1 Definitions:
(TEM) is appropriate. The use of the TEM method for the
3.1.1 analytical sensitivity, n—airborne fiber concentration
identification and size measurement of SCCW is described in
represented by a single fiber counted in the SEM.
Practice D6058 and Test Method D6056.
3.1.1.1 Discussion—Although the terms fiber and whisker
1.4 The values stated in SI units are to be regarded as the are, for convenience, used interchangeably in this test method,
standard. The values given in parentheses are for information whisker is correctly applied only to single-crystal fibers
whereas a “fiber” may be single- or poly-crystalline or may be
only.
noncrystalline.
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 and
Analysis of Asbestos. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Oct. 1, 2011. Published October 2011. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1996. Last previous edition approved in 2006 as D6059–96 (2006). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D6059-96R11. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6059 − 96 (2011)
3.1.2 aspect ratio, n—the ratio of the length of a fiber to its ratory coefficient of variation and use it for reporting 95%
width. confidence limits (1,3,4).
3.1.3 fiber, n—for the purpose of this test method,an
6. Interferences
elongated particle having a length greater than 5 µm, a width
6.1 This test method has been designed to filter air for the
less than 3 µm, and an aspect ratio equal to or greater than 5:1.
determination of SCCW concentration. However, filtration of
3.1.4 fibrous, adj—composed of parallel, radiating, or inter-
air also involves collection of extraneous particles and other
lacedaggregatesoffibers,fromwhichthefibersaresometimes
fibers that may not be of interest. Extraneous particles may
separable. That is, the aggregate may be referred to as fibrous
obscure the fibers by overlay or by overloading of the filter.
even if it is not composed of separable fibers, but has that
This situation can be managed by regulating the air volume
distinct appearance. The term fibrous is used in a general
sampled and thus the filter loading. Fibers should appear
mineralogical way to describe aggregates.
separated from other particles to ensure an adequate opportu-
3.1.5 man-made mineral fiber, n—any inorganic fibrous
nity for their recognition as separate entities in the SEM and
material produced by chemical or physical processes.
accurate counting. Some coincident particle agglomeration
does occur even with these guidelines. Analyze an alternate
3.1.6 single-crystal ceramic whiskers, n—a man-made min-
filterwithareducedloadingiftheobscuringconditionappears
eral fiber that has a single-crystal structure.
to exceed 15% of the filter area (5). Redeposition of a portion
3.2 For definitions of other terms used in this test method,
of an overloaded filter is permitted only in circumstances
see Terminology D1356.
whereanalternatefilterisnotavailableandcannotbeobtained
through resampling (see 10.1.5).
4. Summary of Test Method
4.1 The sample is collected on a mixed cellulose ester
7. Apparatus and Reagents
(MCE) filter by drawing air, using a sampling pump, through
7.1 Sampling Cassette—Use a 25-mm electrically conduc-
an open-face 25-mm electrically conductive sampling cassette
tive cassette assembly such as a three-piece cassette with an
assembly (1, 2). AsectionofthefilteristransferredtoanSEM
extension cowl or retainer ring containing a 0.45-µm pore-size
stub and the fibers are identified, sized, and counted at a
MCE filter and a support pad. Seal the cassette assembly with
magnificationof2000×intheSEMusingthecriteriadiscussed
shrink tape. Reloading of used cassettes is not permitted.
inSection11.Resultsareexpressedasafiberconcentrationper
7.2 Personal Sampling Pump—Use a portable battery-
unitvolumeofairandafiberloadingperunitareaoffilter.The
operated pump for personal sampling. Each pump must be
airborne concentration is expressed as fiber per millilitre
capable of operating within the range from 0.5 to 4 L/min and
(f/mL) and fiber loading is expressed as fibers per square
continuously over the chosen sampling period (1). The flow
millimetre (f/mm ).
mustbefreefrompulsation.Allpumpsshallbecalibratedprior
5. Significance and Use to use (6).
5.1 TheSCCWmaybepresentintheworkplaceatmosphere
7.3 Area Sampling Pump—Use a personal sampling pump
where these materials are manufactured, processed, or a non-portable high-volume pump for area sampling. Each
transported, or used. This test method can be used to monitor
pump shall be capable of operating within the range from 0.5
airborneconcentrationsofSCCWfibersintheseenvironments. to 16 L/min and continuously over the chosen sampling period
It may be employed as part of a personal or area monitoring
(1). The flow shall be free from pulsation. All pumps shall be
strategy. calibrated prior to use (6).
5.2 This test method is based on morphology and elemental
7.4 Vinyl tubing or equivalent.
composition. The analysis technique has the ability to identify
7.5 Scanning Electron Microscope, a SEM capable of op-
SCCW.
erating using an accelerating voltage of at least 15 kV. The
SEM must be capable of performing EDS analysis. A light
NOTE 1—This test method assumes that the analyst is familiar with the
operation of SEM/EDS instrumentation and the interpretation of data
element X-ray analyzer capable of detecting carbon, nitrogen,
obtained using these techniques.
and oxygen is recommended.
5.3 This test method is not appropriate for measurement of
7.6 Vacuum Evaporator—For vapor deposition of conduc-
fibers with diameters ≤0.10 to 0.25 µm due to visibility
tive layers of carbon.
limitations associated with SEM. The TEM method may be
NOTE 2—Sputter coaters and carbonaceous fiber coaters are not
usedtoprovideadditionalsizeinformationofSCCWifneeded
appropriate.
(see Practice D6058 for additional information on the use of
7.7 SEM Sample Preparation Stubs—Stubs made of carbon
this test method).
are suitable. (Acarbon planchet disk glued to a metal holder is
5.4 Resultsfromtheuseofthistestmethodshallbereported
also acceptable.)
along with 95% confidence limits for the samples being
7.8 Conducting DAG, (colloidal graphite) type adhesive
studied. Individual laboratories shall determine their intralabo-
paint or double-sided conductive carbon tape.
7.9 NIST SEM Magnification Standard, SRM 484 (see
The boldface numbers in parentheses refer to a list of references at the end of
this test method. Practice E766).
D6059 − 96 (2011)
7.10 Sample Preparation Area, consisting of either a clean 8.5.1 For personal sampling, fasten the sampling cassette to
room facility or a room containing a laminar flow hood. the worker’s lapel in the worker’s breathing zone and orient it
face down. Adjust the calibrated flow rate to a value between
7.11 Specification D1193 Type II Water, (particle-free).
0.5and4L/min (1).Typically,asamplingratebetween0.5and
7.12 Tweezers.
2.5 L/min is selected (2-4,6,7). Also see Test Method D4532.
7.13 Scalpel Blades. 8.5.2 Placeareasamplesonanextensionrodfacingdownat
a 45° angle.Adjust the calibrated flow rate to a value between
7.14 MCE Filters, 25 mm, 0.45 and 0.22-µm.
0.5and16L/min (1).Typically,asamplingratebetween1and
7.15 Funnel/Filter Assembly, 25-mm.
10 L/min is selected (8).
8.5.3 Set the sampling flow rate and time to produce an
7.16 Miscellaneous Supplies.
optimum fiber loading between 100 to 1300 f/mm (1,2). The
NOTE 3—If the alternate sample preparation method discussed in 10.4
time of sampling can be estimated by using the following
is utilized, the following additional apparatus and reagents will be
equation:
necessary:
A F
7.16.1 Oven, capable of operating at 65°C is required to ~ !~ !
c L
t 5 (1)
~Q!~C ! 10
collapse the filter. A hot plate capable of maintaining the
e
required temperature is an acceptable alternative to the oven.
where:
7.16.2 Plasma Asher, a low-temperature asher (LTA) is
A = active filter collection area (;385 mm for 25-mm
c
required to plasma-etch the collapsed MCE filter. A nominal
filter),
100-W unit is suitable.
t = time, min,
7.16.3 Oxygen, used as a bleed gas in the plasma asher.
F = fiber loading, f/mm ,
L
7.16.4 Micro-syringe or Pipette,adevicecapableofconsis-
Q = sampling flow rate, L/min,
tently delivering a solution volume of 100 µL is required.
C = estimated concentration of SCCW, f/mL, and
e
7.16.5 Dimethyl Formamide (DMF).
10 = conversion factor.
7.16.6 Glacial Acetic Acid.
8.5.4 At a minimum, check the flow rate before and after
7.16.7 Purity of Reagents—Reagent grade chemicals shall
sampling. If the difference is greater than 10% from the initial
be used in all tests. Unless otherwise indicated, it is intended
flow rate, the sample shall be rejected. Also see Test Method
thatallreagentsconformtothespecificationsoftheCommittee
D4532.
on Analytical Reagents of the American Chemical Society
4,5
8.6 Carefullyremovethecassettefromthetubingattheend
wheresuchspecificationsareavailable. Othergradesmaybe
of the sampling period (ensure that the cassette is positioned
used, provided it is first ascertained that the reagent is of
upright before interrupting pump flow). Replace the inlet cap
sufficiently high purity to permit its use without lessening the
and inlet and outlet plugs, and store the cassette.
accuracy of the determination.
NOTE 4—Deactivate the sampling pump prior to disconnecting the
8. Sample Collection
cassette from the tubing.
8.1 CollectsamplesofairborneSCCWonMCEfiltersusing
8.7 Submit at least one field blank (or a number equal to
sampling cassettes and pumps as noted in Section 7.
10% of the total samples, whichever is greater) for each set of
samples. Remove the cap of the field blank briefly (approxi-
8.2 Remove the outlet plug from the sampling cassette and
mately 30 s) at the sampling site, then replace it. The field
connect it to a sampling pump by means of flexible,
blank is used to monitor field sampling procedures. Field
constriction-proof tubing.
blanks shall be representative of filters used in sample collec-
8.3 Perform a leak check of the sampling system by
tion (for example, same filter lot number).
activating the pump with the closed cassette and rotameter (or
8.8 Submit at least one unused and unopened sealed blank
other flow measurement device) in line. Any flow indicates a
which is used to monitor the supplies purchased as well as
leak that must be eliminated before starting the sampling
procedures used in the laboratory. The sealed blank shall be
operation.
representativeoffiltersusedinsamplecollection(forexample,
8.4 Remove the inlet plug from the sampling cassette to
same filter lot number).
eliminate any vacuum that may have accumulated during the
leak test, then remove the entire inlet cap.
9. Transport of Samples
8.5 Conduct personal and area sampling as follows:
9.1 Ship the samples in a rigid container with sufficient
packing material to prevent jostling or damage. Care shall be
taken to minimize vibrations and cassette movement.
Reagent Chemicals, American Chemical Society Specifications, American
NOTE 5—Do not use shipping material that may develop electrostatic
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American C
...

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