ASTM D5197-03

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 may be quantified with good accuracy following special precautions (see 10.2.5).
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

• Status: Historical
• Publication Date: 09-Apr-2003
• ICS: 71.080.80 - Aldehydes and ketones
• Technical Committee: D22 - Air Quality
• Drafting Committee: D22.05 - Indoor Air

Relations

• Replaces: ASTM D5197-97 - Standard Test Method for Determination of Formaldehyde and Other Carbonyl Compounds in Air (Active Sampler Methodology)
• Effective Date: 10-Apr-2003
• Replaced By: ASTM D5197-09 - Standard Test Method for Determination of Formaldehyde and Other Carbonyl Compounds in Air (Active Sampler Methodology)
• Effective Date: 01-Nov-2009
• Referred By: ASTM D7911-19 - Standard Guide for Using Reference Material to Characterize Measurement Bias Associated with Volatile Organic Compound Emission Chamber Test
• Effective Date: 10-Apr-2003
• Referred By: ASTM D7339-18 - Standard Test Method for Determination of Volatile Organic Compounds Emitted from Carpet using a Specific Sorbent Tube and Thermal Desorption / Gas Chromatography
• Effective Date: 10-Apr-2003
• Referred By: ASTM D7297-21 - Standard Practice for Evaluating Residential Indoor Air Quality Concerns
• Effective Date: 10-Apr-2003
• Referred By: ASTM D8142-17e1 - Standard Test Method for Determining Chemical Emissions from Spray Polyurethane Foam (SPF) Insulation using Micro-Scale Environmental Test Chambers
• Effective Date: 10-Apr-2003
• Referred By: ASTM D6177-19 - Standard Practice for Determining Emission Profiles of Volatile Organic Chemicals Emitted from Bedding Sets
• Effective Date: 10-Apr-2003
• Referred By: ASTM D8407-21 - Standard Guide for Measurement Techniques for Formaldehyde in Air
• Effective Date: 10-Apr-2003
• Referred By: ASTM D7143-17 - Standard Practice for Emission Cells for the Determination of Volatile Organic Emissions from Indoor Materials/Products
• Effective Date: 10-Apr-2003
• Referred By: ASTM D6399-18 - Standard Guide for Selecting Instruments and Methods for Measuring Air Quality in Aircraft Cabins
• Effective Date: 10-Apr-2003
• Referred By: ASTM D7706-17 - Standard Practice for Rapid Screening of VOC Emissions from Products Using Micro-Scale Chambers
• Effective Date: 10-Apr-2003
• Referred By: ASTM E1333-22 - Standard Test Method for Determining Formaldehyde Concentrations in Air and Emission Rates from Wood Products Using a Large Chamber
• Effective Date: 10-Apr-2003
• Referred By: ASTM D6803-19 - Standard Practice for Testing and Sampling of Volatile Organic Compounds (Including Carbonyl Compounds) Emitted from Architectural Coatings Using Small-Scale Environmental Chambers
• Effective Date: 10-Apr-2003
• Referred By: ASTM D8445-22a - Standard Practice for Measuring Chemical Emissions from Spray Polyurethane Foam (SPF) Insulation Samples in a Large-scale Ventilated Enclosure
• Effective Date: 10-Apr-2003
• Referred By: ASTM D6670-18 - Standard Practice for Full-Scale Chamber Determination of Volatile Organic Emissions from Indoor Materials/Products
• Effective Date: 10-Apr-2003

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.
Designation: D5197 – 03
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 1.5 This test method instructs the user on how to prepare
sampling cartridges from commercially available chromato-
1.1 This test method covers a procedure for the determina-
2
graphic grade silica gel cartridges by the application of
tion of formaldehyde (HCHO) and other carbonyl compounds
acidified DNPH to each cartridge.
(aldehydes and ketones) in air. Other carbonyl compounds that
1.6 Thesamplingflowrate,asdescribedinthistestmethod,
have been validated for determination by this method include
has been validated for sampling rates up to 1.5 L/min. This
acetaldehyde, acetone, propanal (propionaldehyde), methac-
flow rate limitation is principally due to the high pressure drop
rolein, 2-butanone (methyl ethyl ketone), butyraldehyde, ben-
(>8 kPa at 1.0 L/min) across the user prepared silica gel
zaldehyde, isovaleraldehyde, valeraldehyde, o-tolualdehyde,
cartridges which have a particle size of 55 to 105 µm. These
m-tolualdehyde, p-tolualdehyde, hexanal, and 2,5-
cartridges are not generally compatible with battery-powered
dimethylbenzaldehyde. Acrolein and crotonaldehyde may be
pumps used in personal sampling equipment (for example,
quantified with good accuracy following special precautions
those used by industrial hygienists.
(see 10.2.5).
1.7 Alternatively, pre-coated DNPH silica gel cartridges are
1.2 This test method involves drawing air through a car-
also commercially available and may be substituted provided
tridge containing silica gel coated with 2,4-
3
they can be demonstrated to perform equivalently. Some of
dinitrophenylhydrazine(DNPH)reagent.Carbonylcompounds
these use silica gel of a larger particle size that results in a
readily form stable derivatives with the DNPH reagent. The
lower pressure drop across the cartridge. These low pressure
DNPH derivatives are analyzed for parent aldehydes and
drop cartridges may be more suitable for sampling air using
ketones utilizing high performance liquid chromatography
battery-powered personal sampling pumps.
(HPLC). The sampling procedure is a modification of U.S.
1.8 The values stated in SI units are to be regarded as the
EPA Method TO-11A (see 2.2).
standard.
1.3 This test method is based on the specific reaction of
1.9 This standard does not purport to address all of the
carbonyl compounds with DNPH in the presence of an acid to
safety concerns, if any, associated with its use. It is the
form stable derivatives according to the reaction shown in Fig.
1
responsibility of the user of this standard to establish appro-
1, (where: both R and R are alkyl or aromatic groups
1
priate safety and health practices and determine the applica-
(ketones), or both, or either R or R is a hydrogen atom
bility of regulatory limitations prior to use.
(aldehydes)). The determination of formaldehyde and other
carbonylcompounds,asDNPHderivatives,issimilartothatof
2. Referenced Documents
U.S. EPA Method TO-11A in that it utilizes HPLC with UV
4
2.1 ASTM Standards:
detection as the analytical finish. The detection limits have
D1193 Specification for Reagent Water
been extended to other carbonyl compounds that can be
D1356 Terminology Relating to Sampling and Analysis of
determined as outlined in Section 10.2.4. This test method is
Atmospheres
suitable for determination of formaldehyde and other carbonyl
compounds in the concentration range from approximately 10
ppb to 1 ppm (v/v).
2
The cartridge used in the development and performance evaluation of this test
1.4 The sampling method gives a time-weighted average
method was the Sep-Pak Plus Silica cartridge. The sole source of supply of the
(TWA) sample. It can be used for long-term (1 to 24 h) or
cartridgeknowntothecommitteeatthistimeisWatersAssociates,34MapleStreet,
short-term (5 to 60 min) sampling of air for formaldehyde.
Milford, MA 01757. If you are aware of alternative suppliers, please provide this
information toASTM Headquarters. Your comments will receive careful consider-
1
ation at a meeting of the responsible technical committee, which you may attend.
3
Tejada,S.B.,“EvaluationofSilicaGelCartridgesCoatedinsituwithAcidified
1
This test method is under the jurisdiction of ASTM Committee D22 on Air
2,4-Dinitrophenylhydrazine for SamplingAldehydes and Ketones inAir,” Interna-
Quality and is the direct responsibility of Subcommittee D22.05 on Indoor Air.
tional
...