Standard Test Method for Measurement of Airborne Metal and Metal Oxide Nanoparticle Surface Area Concentration in Inhalation Exposure Chambers using Krypton Gas Adsorption

SIGNIFICANCE AND USE
5.1 A tiered strategy for characterization of nanoparticle properties is necessary to draw meaningful conclusions concerning dose-response relationships observed during inhalation toxicology experiments. This tiered strategy includes characterization of nanoparticles as produced (that is, measured as the bulk material sold by the supplier) and as administered (that is, measured at the point of delivery to a test subject) (Oberdorster et al., 2005) (6).  
5.2 Test Methods B922 and C1274 and ISO Standards 9277 and 18757 exist for determination of the as produced surface area of bulk metal and metal oxide powders. During the delivery of metal and metal oxide nanoparticles in inhalation exposure chambers, the material properties may undergo change and therefore have properties that differ from the material as produced. This test method describes the determination of the as administered surface area of airborne metal and metal oxide nanoparticles in inhalation exposure chambers for inhalation toxicology studies.
SCOPE
1.1 This test method covers determination of surface area of airborne metal and metal oxide nanoparticles in inhalation exposure chambers for inhalation toxicology studies. Surface area may be measured by gas adsorption methods using adsorbates such as nitrogen, krypton, and argon (Brunauer et al., 1938; Anderson, 1975; Gregg and Sing, 1982) (1, 2, 3)2 or by ion attachment and mobility-based methods (Ku and Maynard, 2005) (4). This test method is specific to the measurement of surface area by gas adsorption by krypton gas adsorption. The test method permits the use of any modern commercial krypton adsorption instruments but strictly defines the sample collection, outgassing, and analysis procedures for metal and metal oxide nanoparticles. Use of krypton is required due to the low overall surface area of particle-laden samples and the need to accurately measure the background surface area of the filter used for sample collection. Instrument-reported values of surface area based on the multipoint Brunauer, Emmett and Teller (BET) equation (Brunauer et al., 1938; Anderson, 1975; Gregg and Sing, 1982) (1, 2, 3) are used to calculate surface area of airborne nanoparticles collected on a filter.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. State all numerical values in terms of SI units unless specific instrumentation software reports surface area using alternate units.  
1.3 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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Status
Historical
Publication Date
31-Aug-2013
Current Stage
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ASTM E2864-13 - Standard Test Method for Measurement of Airborne Metal and Metal Oxide Nanoparticle Surface Area Concentration in Inhalation Exposure Chambers using Krypton Gas Adsorption
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: E2864 − 13
Standard Test Method for
Measurement of Airborne Metal and Metal Oxide
Nanoparticle Surface Area Concentration in Inhalation
1
Exposure Chambers using Krypton Gas Adsorption
This standard is issued under the fixed designation E2864; 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 2. Referenced Documents
3
2.1 ASTM Standards:
1.1 Thistestmethodcoversdeterminationofsurfaceareaof
B922Test Method for Metal Powder Specific Surface Area
airborne metal and metal oxide nanoparticles in inhalation
by Physical Adsorption
exposure chambers for inhalation toxicology studies. Surface
C1274Test Method forAdvanced Ceramic Specific Surface
area may be measured by gas adsorption methods using
Area by Physical Adsorption
adsorbates such as nitrogen, krypton, and argon (Brunauer et
2
E691Practice for Conducting an Interlaboratory Study to
al., 1938;Anderson, 1975; Gregg and Sing, 1982) (1, 2, 3) or
Determine the Precision of a Test Method
by ion attachment and mobility-based methods (Ku and
E2456Terminology Relating to Nanotechnology
Maynard, 2005) (4). This test method is specific to the
4
2.2 ISO Standards:
measurement of surface area by gas adsorption by krypton gas
ISO 9277Determination of the Specific Surface Area of
adsorption. The test method permits the use of any modern
Solids by Gas Adsorption using the BET Method
commercial krypton adsorption instruments but strictly defines
ISO 18757Fine Ceramics (Advanced Ceramics, Advanced
the sample collection, outgassing, and analysis procedures for
Technical Ceramics)—Determination of Specific surface
metalandmetaloxidenanoparticles.Useofkryptonisrequired
Area of Ceramic Powders by Gas Adsorption using the
due to the low overall surface area of particle-laden samples
BET Method
and the need to accurately measure the background surface
area of the filter used for sample collection. Instrument-
3. Terminology
reported values of surface area based on the multipoint
3.1 Definitions—For additional definitions related to
Brunauer, Emmett and Teller (BET) equation (Brunauer et al.,
nanotechnology, see Terminology E2456.
1938;Anderson,1975;GreggandSing,1982) (1, 2, 3)areused
3.1.1 nanoparticles, n—in nanotechnology, a sub-
to calculate surface area of airborne nanoparticles collected on
classification of ultrafine particle with lengths in two or three
a filter.
dimensions greater than 0.001 micrometre (1 nanometre) and
1.2 The values stated in SI units are to be regarded as
smallerthanabout0.1micrometre(100nanometres)andwhich
standard. No other units of measurement are included in this
may or may not exhibit a size-related intensive property.
standard. State all numerical values in terms of SI units unless
E2456
specific instrumentation software reports surface area using
3.1.2 adsorbate, n—material that has been retained by the
alternate units.
process of adsorption. B922
1.3 This standard does not purport to address all of the
3.1.3 adsorbent, n—any solid having the ability to concen-
safety concerns, if any, associated with its use. It is the
trate or collect significant quantities of other substances on its
responsibility of the user of this standard to establish appro-
surface. B922
priate safety and health practices and determine the applica-
3.1.4 adsorption, n—a process in which fluid molecules are
bility of regulatory limitations prior to use.
concentrated or collected on a surface by chemical or physical
forces, or both. B922
1
This test method is under the jurisdiction of ASTM Committee E56 on
3
Nanotechnology and is the direct responsibility of Subcommittee E56.02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Physical and Chemical Characterization. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved Sept. 1, 2013. Published October 2013. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
E2864-13. the ASTM website.
2 4
Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
this standard. 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
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E2864 − 13
3.1.5 BET-constant, n—an indication of the magnitude of instrument pressure tolerance (pressure range that must be
the adsorbent/adsorbate interactions in the first adsorbed layer. maintained within a sample cell to accept a va
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