ASTM D5197-09e1
(Test Method)Standard Test Method for Determination of Formaldehyde and Other Carbonyl Compounds in Air (Active Sampler Methodology)
Standard Test Method for Determination of Formaldehyde and Other Carbonyl Compounds in Air (Active Sampler Methodology)
SIGNIFICANCE AND USE
This test method provides an analytical procedure for measuring formaldehyde and other carbonyl compounds in indoor or outdoor air.
SCOPE
1.1 This test method covers a procedure for the determination of formaldehyde (HCHO) and other carbonyl compounds (aldehydes and ketones) in air. Other carbonyl compounds that have been validated for determination by this method include acetaldehyde, acetone, propanal (propionaldehyde), methacrolein, 2-butanone (methyl ethyl ketone), butyraldehyde, benzaldehyde, isovaleraldehyde, valeraldehyde, o-tolualdehyde, m-tolualdehyde, p-tolualdehyde, hexanal, and 2,5-dimethylbenzaldehyde. Acrolein and crotonaldehyde can not be determined quantitatively using the analytical procedure described in 10.2 due to the formation of multiple derivative peaks and the instability of the peak ratios . However, the procedure described in the Annex A has been used by the U. S. Environmental Protection Agency to estimate acrolein and crotonaldehyde concentrations in standard atmospheres following special precautions.
1.2 This test method involves drawing air through a cartridge containing silica gel coated with 2,4-dinitrophenylhydrazine (DNPH) reagent. Carbonyl compounds readily form stable derivatives with the DNPH reagent. The DNPH derivatives are analyzed for parent aldehydes and ketones utilizing high performance liquid chromatography (HPLC). The sampling procedure is a modification of U.S. EPA Method TO-11A (see 2.2).
1.3 This test method is based on the specific reaction of carbonyl compounds with DNPH in the presence of an acid to form stable derivatives according to the reaction shown in Fig. 1, (where: both R and R1 are alkyl or aromatic groups (ketones), or both, or either R or R1 is a hydrogen atom (aldehydes)). The determination of formaldehyde and other carbonyl compounds, as DNPH derivatives, is similar to that of U.S. EPA Method TO-11A in that it utilizes HPLC with UV detection as the analytical finish. The detection limits have been extended to other carbonyl compounds that can be determined as outlined in Section 10.2.4. This test method is suitable for determination of formaldehyde and other carbonyl compounds in the concentration range from approximately 10 ppb to 1 ppm (v/v).
1.4 The sampling method gives a time-weighted average (TWA) sample. It can be used for long-term (1 to 24 h) or short-term (5 to 60 min) sampling of air for formaldehyde.
1.5 This test method instructs the user on how to prepare sampling cartridges from commercially available chromatographic grade silica gel cartridges by the application of acidified DNPH to each cartridge.
1.6 The sampling flow rate, as described in this test method, has been validated for sampling rates up to 1.5 L/min. This flow rate limitation is principally due to the high pressure drop (>8 kPa at 1.0 L/min) across the user prepared silica gel cartridges which have a particle size of 55 to 105 μm. These cartridges are not generally compatible with battery-powered pumps used in personal sampling equipment (for example, those used by industrial hygienists.
1.7 Alternatively, pre-coated DNPH silica gel cartridges are also commercially available and may be substituted provided they can be demonstrated to perform equivalently. Some of these use silica gel of a larger particle size that results in a lower pressure drop across the cartridge. These low pressure drop cartridges may be more suitable for sampling air using battery-powered personal sampling pumps.
1.8 The values stated in SI units are to be regarded as the standard.
1.9 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
Relations
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
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Designation: D5197 − 09
Standard Test Method for
Determination of Formaldehyde and Other Carbonyl
1
Compounds in Air (Active Sampler Methodology)
This standard is issued under the fixed designation D5197; 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.
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ε NOTE—Added research report information to Section 13 editorially in September 2010.
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1. Scope (ketones), or both, or either R or R is a hydrogen atom
(aldehydes)). The determination of formaldehyde and other
1.1 This test method covers a procedure for the determina-
carbonylcompounds,asDNPHderivatives,issimilartothatof
tion of formaldehyde (HCHO) and other carbonyl compounds
U.S. EPA Method TO-11A in that it utilizes HPLC with UV
(aldehydes and ketones) in air. Other carbonyl compounds that
detection as the analytical finish. The detection limits have
have been validated for determination by this method include
been extended to other carbonyl compounds that can be
acetaldehyde, acetone, propanal (propionaldehyde),
determined as outlined in Section 10.2.4. This test method is
methacrolein, 2-butanone (methyl ethyl ketone),
suitable for determination of formaldehyde and other carbonyl
butyraldehyde, benzaldehyde, isovaleraldehyde,
compounds in the concentration range from approximately 10
valeraldehyde, o-tolualdehyde, m-tolualdehyde,
ppb to 1 ppm (v/v).
p-tolualdehyde,hexanal,and2,5-dimethylbenzaldehyde.Acro-
lein and crotonaldehyde can not be determined quantitatively 1.4 The sampling method gives a time-weighted average
using the analytical procedure described in 10.2 due to the
(TWA) sample. It can be used for long-term (1 to 24 h) or
formationofmultiplederivativepeaksandtheinstabilityofthe short-term (5 to 60 min) sampling of air for formaldehyde.
2,3
peak ratios . However, the procedure described in theAnnex
1.5 This test method instructs the user on how to prepare
AhasbeenusedbytheU.S.EnvironmentalProtectionAgency
sampling cartridges from commercially available chromato-
to estimate acrolein and crotonaldehyde concentrations in
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graphic grade silica gel cartridges by the application of
standard atmospheres following special precautions.
acidified DNPH to each cartridge.
1.2 This test method involves drawing air through a car-
1.6 Thesamplingflowrate,asdescribedinthistestmethod,
tridge containing silica gel coated with 2,4-
has been validated for sampling rates up to 1.5 L/min. This
dinitrophenylhydrazine(DNPH)reagent.Carbonylcompounds
flowratelimitationisprincipallyduetothehighpressuredrop
readily form stable derivatives with the DNPH reagent. The
(>8 kPa at 1.0 L/min) across the user prepared silica gel
DNPH derivatives are analyzed for parent aldehydes and
cartridges which have a particle size of 55 to 105 µm. These
ketones utilizing high performance liquid chromatography
cartridges are not generally compatible with battery-powered
(HPLC). The sampling procedure is a modification of U.S.
pumps used in personal sampling equipment (for example,
EPA Method TO-11A (see 2.2).
those used by industrial hygienists.
1.3 This test method is based on the specific reaction of
1.7 Alternatively, pre-coated DNPH silica gel cartridges are
carbonyl compounds with DNPH in the presence of an acid to
also commercially available and may be substituted provided
form stable derivatives according to the reaction shown in Fig.
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they can be demonstrated to perform equivalently. Some of
1
1, (where: both R and R are alkyl or aromatic groups
these use silica gel of a larger particle size that results in a
lower pressure drop across the cartridge. These low pressure
1
This test method is under the jurisdiction of ASTM Committee D22 on Air
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Current edition approved Nov. 1, 2009. Published December 2009. Originally
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approved in 1991. Last previous edition approved in 2003 as D5197–03. DOI: The cartridge used in the development and performance evaluation of this test
10.1520/D5197-09E01. method was the Sep-Pak Plus Silica cartridge. The sole source of supply of the
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Levin, J. O., and Lindahl, R., “Aldehyde Measuring Methods Using DNPH- cartridgeknowntothecommitteeatthistimeisWatersAssociates,34MapleStreet,
coated Filters—Summary and Conclusions,” Proceedings of the Workshop “Sam- Milford, MA 01757. If you are aware of alternative suppliers, please provide this
pling Project”, Mol, Belgium, June 27–28, 1986. information toASTM Headquarters. Your comments will receive careful consider-
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Clark, W. L., Biller, W. F., Tejada, S. B., Siegl, W. O., Rosenhamer, D., ation at a meeting of the responsi
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