ASTM D5197-16
(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
5.1 This test method provides an analytical procedure for measuring formaldehyde and other carbonyl compounds in indoor, workplace, outdoor air or for emission testing.
SCOPE
1.1 This test method presents a procedure for the determination of formaldehyde (HCHO) and other carbonyl compounds (aldehydes and ketones) in air. Other carbonyl compounds that have been successfully quantified by this method include acetaldehyde, acetone, propanal (propionaldehyde), 2-butanone (methyl ethyl ketone), butyraldehyde, benzaldehyde, isovaleraldehyde, valeraldehyde, o-tolualdehyde, m-tolualdehyde, p-tolualdehyde, hexanal, and 2,5-dimethylbenzaldehyde.
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 either, or both 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 applicability of this test method is extended beyond the stated applicability of TO-11A to include other carbonyl compounds that can be determined as stated in 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). Lower concentrations may be determined with careful control of contamination, appropriate selection of flow rate and sampling duration.
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. Shorter sampling times or low flow rates will result in higher detection limits and may result in greater variation in co-located sampler results. Tests should be performed over a duration and a flow rate that allows the data quality objective of the project to be achieved. Sample times for other carbonyls, such as acetaldehyde, may be limited to short term (1).2 The data provides total concentrations of carbonyl compounds from which time weighted average concentrations can be calculated.
1.5 This test method instructs the user on how to prepare sampling cartridges from commercially available chromatographic grade silica gel cartridges3 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 for formaldehyde. 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 (2). 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 standard. No other units of measurement are included in this standard.
1.9 This standard ...
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Designation: D5197 − 16
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 1.4 The sampling method gives a time-weighted average
(TWA) sample. It can be used for long-term (1 to 24 h) or
1.1 This test method presents a procedure for the determi-
short-term (5 to 60 min) sampling of air for formaldehyde.
nation of formaldehyde (HCHO) and other carbonyl com-
Shorter sampling times or low flow rates will result in higher
pounds (aldehydes and ketones) in air. Other carbonyl com-
detection limits and may result in greater variation in co-
pounds that have been successfully quantified by this method
located sampler results. Tests should be performed over a
include acetaldehyde, acetone, propanal (propionaldehyde),
duration and a flow rate that allows the data quality objective
2-butanone (methyl ethyl ketone), butyraldehyde,
oftheprojecttobeachieved.Sampletimesforothercarbonyls,
benzaldehyde, isovaleraldehyde, valeraldehyde,
2
such as acetaldehyde, may be limited to short term (1). The
o-tolualdehyde, m-tolualdehyde, p-tolualdehyde, hexanal, and
dataprovidestotalconcentrationsofcarbonylcompoundsfrom
2,5-dimethylbenzaldehyde.
whichtimeweightedaverageconcentrationscanbecalculated.
1.2 This test method involves drawing air through a car-
1.5 This test method instructs the user on how to prepare
tridge containing silica gel coated with 2,4-
sampling cartridges from commercially available chromato-
dinitrophenylhydrazine(DNPH)reagent.Carbonylcompounds
3
graphic grade silica gel cartridges by the application of
readily form stable derivatives with the DNPH reagent. The
acidified DNPH to each cartridge.
DNPH derivatives are analyzed for parent aldehydes and
1.6 Thesamplingflowrate,asdescribedinthistestmethod,
ketones utilizing high performance liquid chromatography
has been validated for sampling rates up to 1.5 L/min for
(HPLC). The sampling procedure is a modification of U.S.
formaldehyde.Thisflowratelimitationisprincipallyduetothe
EPA Method TO-11A (see 2.2).
high pressure drop (>8 kPa at 1.0 L/min) across the user
1.3 This test method is based on the specific reaction of
prepared silica gel cartridges which have a particle size of 55
carbonyl compounds with DNPH in the presence of an acid to
to 105 µm. These cartridges are not generally compatible with
form stable derivatives according to the reaction shown in Fig.
battery-powered pumps used in personal sampling equipment
1
1, (where: both R and R are alkyl or aromatic groups
(for example, those used by industrial hygienists).
1
(ketones), or either, or both R or R is a hydrogen atom
1.7 Alternatively, pre-coated DNPH silica gel cartridges are
(aldehydes)). The determination of formaldehyde and other
also commercially available and may be substituted provided
carbonylcompounds,asDNPHderivatives,issimilartothatof
theycanbedemonstratedtoperformequivalently (2).Someof
U.S. EPA Method TO-11A in that it utilizes HPLC with UV
these use silica gel of a larger particle size that results in a
detection as the analytical finish. The applicability of this test
lower pressure drop across the cartridge. These low pressure
method is extended beyond the stated applicability of TO-11A
drop cartridges may be more suitable for sampling air using
toincludeothercarbonylcompoundsthatcanbedeterminedas
battery-powered personal sampling pumps.
stated in 10.2.4. This test method is suitable for determination
offormaldehydeandothercarbonylcompoundsintheconcen- 1.8 The values stated in SI units are to be regarded as
trationrangefromapproximately10ppbto1ppm(v/v).Lower standard. No other units of measurement are included in this
concentrations may be determined with careful control of standard.
contamination, appropriate selection of flow rate and sampling
1.9 This standard does not purport to address all of the
duration.
safety concerns, if any, associated with its use. It is the
1 2
This test method is under the jurisdiction of ASTM Committee D22 on Air The boldface numbers in parentheses refer to a list of references at the end of
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air. this standard.
3
Current edition approved Oct. 1, 2016. Published November 2016. Originally The cartridge used in the development and performance evaluation of this test
ɛ1
approved in 1991. Last previous edition approved in 2009 as D5197–09 . DOI: method was the Sep-Pak Plus Silica cartridge. Other manufac
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM 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.
´1
Designation: D5197 − 09 D5197 − 16
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1
ε NOTE—Added research report information to Section 13 editorially in September 2010.
1. Scope
1.1 This test method coverspresents 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 successfully quantified 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
2,3
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
1
stable derivatives according to the reaction shown in Fig. 1, (where: both R and R are alkyl or aromatic groups (ketones), or
1
both,either, or eitherboth 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. EPA Method TO-11A in that it utilizes HPLC with UV detection as
the analytical finish. The detection limits have been extended to applicability of this test method is extended beyond the stated
applicability of TO-11A to include other carbonyl compounds that can be determined as outlinedstated 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). Lower concentrations may be determined with careful control of contamination, appropriate
selection of flow rate and sampling duration.
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. Shorter sampling times or low flow rates will result in higher detection limits and
may result in greater variation in co-located sampler results. Tests should be performed over a duration and a flow rate that allows
the data quality objective of the project to be achieved. Sample times for other carbonyls, such as acetaldehyde, may be limited
2
to short term (1). The data provides total concentrations of carbonyl compounds from which time weighted average concentrations
can be calculated.
1.5 This test method instructs the user on how to prepare sampling cartridges from commercially available chromatographic
3
grade silica gel cartridges by the application of acidified DNPH to each cartridge.
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, 2009Oct. 1, 2016. Published December 2009November 2016. Originally approved in 1991. Last previous edition approved in 20032009
ɛ1
as D5197 – 03.D5197 – 09 . DOI: 10.1520/D5197-09E01.10.1520/D5197-16.
2
Levin, J. O., and Lindahl, R., “Aldehyde Measuring Methods Using DNPH-coated Filters—Summary and Conclusions,” Proceedings of the Workshop “Sampling
Project”, Mol, Belgium, June 27–28, 1986.The boldface numbers in parentheses refer to a list of references at the end of this standard.
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