ASTM D5197-09
(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.
FIG. 1 Reaction of Carbonyl Compounds
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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.
1. Scope (aldehydes)). The determination of formaldehyde and other
carbonylcompounds,asDNPHderivatives,issimilartothatof
1.1 This test method covers a procedure for the determina-
U.S. EPA Method TO-11A in that it utilizes HPLC with UV
tion of formaldehyde (HCHO) and other carbonyl compounds
detection as the analytical finish. The detection limits have
(aldehydes and ketones) in air. Other carbonyl compounds that
been extended to other carbonyl compounds that can be
have been validated for determination by this method include
determined as outlined in Section 10.2.4. This test method is
acetaldehyde, acetone, propanal (propionaldehyde), methac-
suitable for determination of formaldehyde and other carbonyl
rolein, 2-butanone (methyl ethyl ketone), butyraldehyde, ben-
compounds in the concentration range from approximately 10
zaldehyde, isovaleraldehyde, valeraldehyde, o-tolualdehyde,
ppb to 1 ppm (v/v).
m-tolualdehyde, p-tolualdehyde, hexanal, and 2,5-
1.4 The sampling method gives a time-weighted average
dimethylbenzaldehyde. Acrolein and crotonaldehyde can not
(TWA) sample. It can be used for long-term (1 to 24 h) or
be determined quantitatively using the analytical procedure
short-term (5 to 60 min) sampling of air for formaldehyde.
described in 10.2 due to the formation of multiple derivative
,
2 3
1.5 This test method instructs the user on how to prepare
peaks and the instability of the peak ratios . However, the
sampling cartridges from commercially available chromato-
proceduredescribedintheAnnexAhasbeenusedbytheU.S.
4
graphic grade silica gel cartridges by the application of
Environmental Protection Agency to estimate acrolein and
acidified DNPH to each cartridge.
crotonaldehyde concentrations in standard atmospheres fol-
1.6 Thesamplingflowrate,asdescribedinthistestmethod,
lowing special precautions.
has been validated for sampling rates up to 1.5 L/min. This
1.2 This test method involves drawing air through a car-
flow rate limitation is principally due to the high pressure drop
tridge containing silica gel coated with 2,4-
(>8 kPa at 1.0 L/min) across the user prepared silica gel
dinitrophenylhydrazine(DNPH)reagent.Carbonylcompounds
cartridges which have a particle size of 55 to 105 µm. These
readily form stable derivatives with the DNPH reagent. The
cartridges are not generally compatible with battery-powered
DNPH derivatives are analyzed for parent aldehydes and
pumps used in personal sampling equipment (for example,
ketones utilizing high performance liquid chromatography
those used by industrial hygienists.
(HPLC). The sampling procedure is a modification of U.S.
1.7 Alternatively, pre-coated DNPH silica gel cartridges are
EPA Method TO-11A (see 2.2).
also commercially available and may be substituted provided
1.3 This test method is based on the specific reaction of
5
they can be demonstrated to perform equivalently. Some of
carbonyl compounds with DNPH in the presence of an acid to
these use silica gel of a larger particle size that results in a
form stable derivatives according to the reaction shown in Fig.
1
lower pressure drop across the cartridge. These low pressure
1, (where: both R and R are alkyl or aromatic groups
1
drop cartridges may be more suitable for sampling air using
(ketones), or both, or either R or R is a hydrogen atom
battery-powered personal sampling pumps.
1.8 The values stated in SI units are to be regarded as the
1
This test method is under the jurisdiction of ASTM Committee D22 on Air standard.
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
Current edition approved Nov. 1, 2009. Published December 2009. Originally
4
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/D5197-09. method was the Sep-Pak Plus Silica cartridge. The sole source of supply of the
2
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-
3 1
Cl
...
This document is not anASTM standard and is intended only to provide the user of anASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately,ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation:D5197–03 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.
1. Scope
1.1This 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(methylethylketone),butyraldehyde,benzaldehyde,
isovaleraldehyde, valeraldehyde, o-tolualdehyde, m-tolualdehyde, p-tolualdehyde, hexanal, and 2,5-dimethylbenzaldehyde.
Acrolein and crotonaldehyde may be quantified with good accuracy following special precautions (see 10.2.5).
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(methylethylketone),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
,
2 3
formation of multiple derivative peaks and the instability of the peak ratios . However, the procedure described in theAnnexA
has been used by the U. S. Environmental ProtectionAgency 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
1
stablederivativesaccordingtothereactionshowninFig.1,(where:both Rand R arealkyloraromaticgroups(ketones),orboth,
1
or either R or R is a hydrogen atom (aldehydes)).The determination of formaldehyde and other carbonyl compounds, as DNPH
derivatives, is similar to that of U.S. EPAMethodTO-11Ain that it utilizes HPLC with UVdetection 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
4
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
ratelimitationisprincipallyduetothehighpressuredrop(>8kPaat1.0L/min)acrosstheuserpreparedsilicagelcartridgeswhich
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.
CurrenteditionapprovedApril10,2003.PublishedJuly2003.Originallyapprovedin1991.Lastpreviouseditionapprovedin1997asD5197–97.DOI:10.1520/D5197-03.
Current edition approved Nov. 1, 2009. Published December 2009. Originally approved in 1991. Last previous edition approved in 2003 as D5197–03. DOI:
10.1520/D5197-09.
2
The cartridge used in the development and performance evaluation of this test method was the Sep-Pak Plus Silica cartridge. The sole source of supply of the cartridge
known to the committee at this time is Waters Associates, 34 Maple Street, Milford, MA 01757. If you are aware of alte
...
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