Standard Test Method for Analysis of Organic Compound Vapors Collected by the Activated Charcoal Tube Adsorption Method

SIGNIFICANCE AND USE
5.1 Promulgations by the U.S. Federal Occupational Safety and Health Administration (OSHA) in 29 CFR 1910 designate that certain organic compounds must not be present in workplace atmospheres at concentrations above specified values.  
5.2 This test method, when used in conjunction with Practice D3686, will promote needed accuracy and precision in the determination of airborne concentrations of many of the organic chemicals including but not limited to 29 CFR 1910, CDC-99-74-45, NIOSH Manual of Analytical Methods, OSHA Sampling and Analytical Methods, and HSE Methods for the Determination of Hazardous Substances. It can be used to determine worker exposures to these chemicals, provided appropriate sampling periods are used.  
5.3 Most laboratories are equipped with apparatus similar to that described in Section 7. Other apparatus can be used when analytical procedures suitable for that equipment are employed. The analytical techniques (or variations thereof) described in Sections 9 – 11 are in general use to analyze volatile organic compounds extracted from charcoal. Other procedures can be used when appropriate and validated as being suitable for the intended use.
SCOPE
1.1 This test method describes the extraction and gas chromatographic determination of organic vapors that have been adsorbed from air in sampling tubes packed with activated charcoal.  
1.2 This test method is complementary to Practice D3686.  
1.3 This test method is applicable for analysis of samples taken from workplace or other atmospheres provided that the contaminant adsorbs onto charcoal, that it can be adequately extracted from the charcoal, and that it can be analyzed by gas chromatography (GC). Other adsorbents and other extraction techniques are described in Practice D6196.  
1.4 Organic compounds of multicomponent samples may mutually interfere during analysis. Methods to resolve interferences are given in Section 6.  
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautions are given in 8.5, 9.2, and in X1.2.3.  
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

Status
Published
Publication Date
31-Jul-2019
Technical Committee
D22 - Air Quality

Relations

Effective Date
01-Sep-2020
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15-Mar-2020
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Overview

ASTM D3687-19, "Standard Test Method for Analysis of Organic Compound Vapors Collected by the Activated Charcoal Tube Adsorption Method," provides a widely recognized procedure for extracting and analyzing organic vapors captured from the air using activated charcoal sampling tubes. This standard, published by ASTM International, establishes a robust framework for workplace and environmental air monitoring by specifying methods for collection, extraction, and gas chromatographic determination of volatile organic compounds (VOCs).

The method is frequently referenced for occupational exposure assessments, supporting compliance with regulations from agencies such as OSHA (Occupational Safety and Health Administration) and NIOSH (National Institute for Occupational Safety and Health). It also enables laboratories and industrial hygienists to accurately quantify air concentrations of hazardous organic compounds, ensuring workplace safety and regulatory compliance.

Key Topics

  • Activated Charcoal Tube Adsorption: The standard outlines the use of activated charcoal tubes for collecting air samples containing organic vapors. The method is effective for a variety of volatile and semi-volatile organic compounds that adsorb onto charcoal.
  • Sample Extraction & Gas Chromatography (GC): After sampling, organic vapors are extracted from the charcoal using an appropriate solvent (commonly carbon disulfide) and analyzed via gas chromatography, typically with a flame ionization detector (FID).
  • Interference and Calibration: The standard addresses possible chemical interferences, especially in multi-component samples, and specifies techniques for identification and resolution (such as selective solvent stripping and alternate GC parameters). Calibration procedures ensure analytical accuracy.
  • Quality Control and Assurance: ASTM D3687-19 emphasizes laboratory quality practices, including determination of extraction efficiency, use of internal standards, and regular calibration curves, to ensure data reliability and regulatory compliance.
  • Regulatory Relevance: The method is referenced in OSHA (29 CFR 1910), NIOSH Manual of Analytical Methods, CDC, and UK Health and Safety Executive (HSE) protocols.

Applications

ASTM D3687-19 serves crucial roles in a variety of settings:

  • Occupational Air Monitoring: Supports compliance with legal exposure limits for hazardous organic vapors in workplace atmospheres.
  • Industrial Hygiene: Enables accurate assessment of worker exposure to solvents, hydrocarbons, and other volatile chemicals, facilitating risk management and health protection programs.
  • Environmental Health & Safety: Used in the evaluation of indoor and ambient air for VOC contamination, supporting air quality investigations in industrial, laboratory, or building environments.
  • Laboratory Analysis: Standardizes extraction and GC analysis, making results comparable and meeting quality criteria required by accreditation bodies.
  • Regulatory Documentation: Provides documentation and methods required for regulatory submissions, audits, and environmental reporting.

Related Standards

The test method is often implemented alongside or referenced by complementary standards and guides, including:

  • ASTM D3686: Practice for Sampling Atmospheres to Collect Organic Compound Vapors (Activated Charcoal Tube Adsorption Method)
  • ASTM D6196: Practice for Choosing Sorbents, Sampling Parameters, and Thermal Desorption Analytical Conditions for Monitoring Volatile Organic Chemicals in Air
  • ASTM E355: Practice for Gas Chromatography Terms and Relationships
  • ASTM D1356: Terminology Relating to Sampling and Analysis of Atmospheres
  • NIOSH NMAM: National Institute for Occupational Safety and Health Manual of Analytical Methods
  • OSHA Sampling and Analytical Methods: Validated procedures used for regulatory workplace compliance
  • HSE MDHS: UK Health and Safety Executive Methods for the Determination of Hazardous Substances

Conclusion

ASTM D3687-19 provides a reliable, validated protocol for quantifying organic vapor concentrations in workplace and ambient atmospheres using activated charcoal tube adsorption and gas chromatographic analysis. The method supports occupational safety, regulatory compliance, and environmental health by enabling accurate detection of hazardous organic compounds in air. Compliance with this standard ensures that laboratories and organizations can confidently assess airborne exposures and safeguard health in accordance with best practices and regulatory requirements.

Keywords: ASTM D3687-19, activated charcoal tube, air monitoring, organic vapors, gas chromatography, workplace atmospheres, volatile organic compounds, OSHA, NIOSH, occupational exposure.

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Frequently Asked Questions

ASTM D3687-19 is a standard published by ASTM International. Its full title is "Standard Test Method for Analysis of Organic Compound Vapors Collected by the Activated Charcoal Tube Adsorption Method". This standard covers: SIGNIFICANCE AND USE 5.1 Promulgations by the U.S. Federal Occupational Safety and Health Administration (OSHA) in 29 CFR 1910 designate that certain organic compounds must not be present in workplace atmospheres at concentrations above specified values. 5.2 This test method, when used in conjunction with Practice D3686, will promote needed accuracy and precision in the determination of airborne concentrations of many of the organic chemicals including but not limited to 29 CFR 1910, CDC-99-74-45, NIOSH Manual of Analytical Methods, OSHA Sampling and Analytical Methods, and HSE Methods for the Determination of Hazardous Substances. It can be used to determine worker exposures to these chemicals, provided appropriate sampling periods are used. 5.3 Most laboratories are equipped with apparatus similar to that described in Section 7. Other apparatus can be used when analytical procedures suitable for that equipment are employed. The analytical techniques (or variations thereof) described in Sections 9 – 11 are in general use to analyze volatile organic compounds extracted from charcoal. Other procedures can be used when appropriate and validated as being suitable for the intended use. SCOPE 1.1 This test method describes the extraction and gas chromatographic determination of organic vapors that have been adsorbed from air in sampling tubes packed with activated charcoal. 1.2 This test method is complementary to Practice D3686. 1.3 This test method is applicable for analysis of samples taken from workplace or other atmospheres provided that the contaminant adsorbs onto charcoal, that it can be adequately extracted from the charcoal, and that it can be analyzed by gas chromatography (GC). Other adsorbents and other extraction techniques are described in Practice D6196. 1.4 Organic compounds of multicomponent samples may mutually interfere during analysis. Methods to resolve interferences are given in Section 6. 1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard. 1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautions are given in 8.5, 9.2, and in X1.2.3. 1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

SIGNIFICANCE AND USE 5.1 Promulgations by the U.S. Federal Occupational Safety and Health Administration (OSHA) in 29 CFR 1910 designate that certain organic compounds must not be present in workplace atmospheres at concentrations above specified values. 5.2 This test method, when used in conjunction with Practice D3686, will promote needed accuracy and precision in the determination of airborne concentrations of many of the organic chemicals including but not limited to 29 CFR 1910, CDC-99-74-45, NIOSH Manual of Analytical Methods, OSHA Sampling and Analytical Methods, and HSE Methods for the Determination of Hazardous Substances. It can be used to determine worker exposures to these chemicals, provided appropriate sampling periods are used. 5.3 Most laboratories are equipped with apparatus similar to that described in Section 7. Other apparatus can be used when analytical procedures suitable for that equipment are employed. The analytical techniques (or variations thereof) described in Sections 9 – 11 are in general use to analyze volatile organic compounds extracted from charcoal. Other procedures can be used when appropriate and validated as being suitable for the intended use. SCOPE 1.1 This test method describes the extraction and gas chromatographic determination of organic vapors that have been adsorbed from air in sampling tubes packed with activated charcoal. 1.2 This test method is complementary to Practice D3686. 1.3 This test method is applicable for analysis of samples taken from workplace or other atmospheres provided that the contaminant adsorbs onto charcoal, that it can be adequately extracted from the charcoal, and that it can be analyzed by gas chromatography (GC). Other adsorbents and other extraction techniques are described in Practice D6196. 1.4 Organic compounds of multicomponent samples may mutually interfere during analysis. Methods to resolve interferences are given in Section 6. 1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard. 1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific precautions are given in 8.5, 9.2, and in X1.2.3. 1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

ASTM D3687-19 is classified under the following ICS (International Classification for Standards) categories: 13.040.20 - Ambient atmospheres. The ICS classification helps identify the subject area and facilitates finding related standards.

ASTM D3687-19 has the following relationships with other standards: It is inter standard links to ASTM D1356-20a, ASTM D1356-20, ASTM D3686-20, ASTM D6196-15, ASTM D1356-15a, ASTM D1356-15, ASTM D1356-14b, ASTM D1356-14a, ASTM D1356-14, ASTM D3686-13, ASTM D1356-05(2010), ASTM D6196-03(2009), ASTM D3686-08, ASTM E355-96(2007), ASTM D1356-05. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

ASTM D3687-19 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.

Standards Content (Sample)


This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D3687 − 19
Standard Test Method for
Analysis of Organic Compound Vapors Collected by the
Activated Charcoal Tube Adsorption Method
This standard is issued under the fixed designation D3687; 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
1.1 This test method describes the extraction and gas 2.1 ASTM Standards:
chromatographic determination of organic vapors that have D1356Terminology Relating to Sampling and Analysis of
been adsorbed from air in sampling tubes packed with acti- Atmospheres
vated charcoal. D3686Practice for Sampling Atmospheres to Collect Or-
ganic Compound Vapors (Activated Charcoal Tube Ad-
1.2 This test method is complementary to Practice D3686.
sorption Method)
1.3 This test method is applicable for analysis of samples
D6196Practice for Choosing Sorbents, Sampling Param-
taken from workplace or other atmospheres provided that the
eters and Thermal Desorption Analytical Conditions for
contaminant adsorbs onto charcoal, that it can be adequately
Monitoring Volatile Organic Chemicals in Air
extracted from the charcoal, and that it can be analyzed by gas
E355PracticeforGasChromatographyTermsandRelation-
chromatography (GC). Other adsorbents and other extraction
ships
techniques are described in Practice D6196.
2.2 ISO Standards:
1.4 Organic compounds of multicomponent samples may
ISO/IEC 17025General Requirements for the Competence
mutually interfere during analysis. Methods to resolve inter-
of Testing and Calibration Laboratories
ferences are given in Section 6.
2.3 National Institute for Occupational Safety and Health
1.5 The values stated in SI units are to be regarded as
(NIOSH) Documents:
standard. The values given in parentheses after SI units are CDC-99-74-45Documentation of NIOSH Validation Tests
providedforinformationonlyandarenotconsideredstandard.
NIOSH Manual of Analytical Methods (NMAM)
1.6 This standard does not purport to address all of the
2.4 Occupational Safety and HealthAdministration (OSHA)
safety concerns, if any, associated with its use. It is the Standards:
responsibility of the user of this standard to establish appro-
29 CFR 1910Code of Federal Regulations, Regulations
priate safety, health, and environmental practices and deter- Relating to Labor, Occupational Safety and Health
mine the applicability of regulatory limitations prior to use.
Administration, Department of Labor
Specific precautions are given in 8.5, 9.2, and in X1.2.3.
1.7 This international standard was developed in accor-
dance with internationally recognized principles on standard-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ization established in the Decision on Principles for the
Standards volume information, refer to the standard’s Document Summary page on
Development of International Standards, Guides and Recom-
the ASTM website.
mendations issued by the World Trade Organization Technical 3
Available from International Organization for Standardization (ISO), ISO
Barriers to Trade (TBT) Committee. Central Secretariat, BIBC II, Chemin de Blandonnet 8, CP 401, 1214 Vernier,
Geneva, Switzerland, http://www.iso.org.
Available from the U.S. Department of Commerce, National Technical Infor-
This test method is under the jurisdiction of ASTM Committee D22 on Air mation Service, 5301 Shawnee Road,Alexandria, VA22312, https://www.ntis.gov.
Quality and is the direct responsibility of Subcommittees D22.04 on WorkplaceAir Available from the Centers for Disease Control and Prevention (CDC),
Quality. https://www.cdc.gov/niosh/nmam.
Current edition approved Aug. 1, 2019. Published September 2019. Originally Available from U.S. Government Printing Office, Superintendent of
approved in 1978. Last previous edition approved in 2012 as D3687–07 (2012). Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
DOI: 10.1520/D3687-19. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3687 − 19
OSHA Sampling and Analytical Methods ployed. The analytical techniques (or variations thereof) de-
scribedinSections9–11areingeneralusetoanalyzevolatile
2.5 UK Health and Safety Executive (HSE) Documents:
organic compounds extracted from charcoal. Other procedures
Methods for the Determination of Hazardous Substances
can be used when appropriate and validated as being suitable
(MDHS)
for the intended use.
3. Terminology
6. Interferences
3.1 Definitions:
6.1 Any chemical that produces an FID response and has a
3.1.1 For definitions of terms used in this test method, refer
similar retention time as the analyte is a potential interference.
to the terminology specified in Terminology D1356 and Prac-
Ifpotentialinterferenceswerereportedwhenthesampleswere
tice E355.
received, they should be considered before the samples are
4. Summary of Test Method extracted. Generally, gas chromatographic conditions such as
the type of GC column (phase) or operating parameters can be
4.1 Organic vapors that have been collected on activated
changed to resolve interferences.
charcoal are extracted with carbon disulfide or another appro-
priate solvent and are determined by GC using a flame 6.2 Selective solvent stripping techniques have been used
ionizationdetector(FID).Carbondisulfideisarelativelysmall successfully to make clean and fast separations of polar,
molecule that can penetrate the “ink-bottle” shaped pores of nonpolar and oxygenated compounds. A general guideline is
activatedcharcoal,ithasahighheatofadsorptiononactivated giveninX1.1anddetailedproceduresaregiveninRefs (1 and
charcoal which helps in displacing other adsorbed molecules, 2).
and it is a reasonably good solvent for most, especially
6.3 Whennecessary,theidentityorpurityofananalytepeak
non-polar, organic molecules. Polar modifiers (such as N,N-
can be confirmed by GC/MS.
dimethylformamide) are frequently added to enhance the re-
6.4 The presence of co-adsorbed chemicals can affect the
coveryofpolarorganiccompounds.Otheradvantagestousing
recovery (extraction efficiency) of a particular analyte. Sus-
carbon disulfide include an early elution time on most GC
pectedeffectscanbetestedbyspikingtheanalytesoncharcoal
columns and a small FID response.
as in Section 11.
4.2 Interferences resulting from the analytes having similar
retention times during GC analysis are resolved by changing
7. Apparatus
the GC column, by changing the operating parameters, or by
7.1 Gas chromatograph, equipped with a flame ionization
fractionating the sample using solvent extraction as described
detector (FID), a temperature-programmable oven, and an
in Section X1.1.
automaticsampleinjector(autosampler).Sampleinjectionmay
4.3 Peak purity and identity can be confirmed using tech-
be performed manually if necessary. Other detectors (such as
niques such as gas chromatography/mass spectrometry (GC/
electron capture, flame photometric, nitrogen phosphorous
MS).
detectors) can be used when appropriate but the extraction
solvent may have to be modified.
5. Significance and Use
7.2 Electronicdatasystem,orothersuitablemeanstorecord
5.1 Promulgations by the U.S. Federal Occupational Safety
and measure detector response, to prepare calibration curves,
and HealthAdministration (OSHA) in 29 CFR 1910 designate
and to process sample results.
that certain organic compounds must not be present in work-
7.3 GC columns, required to separate the complex mixture
place atmospheres at concentrations above specified values.
of possible organic chemicals. Examples of the most common
5.2 This test method, when used in conjunction with Prac-
and useful GC columns are 60-m long, 0.32-mm i.d. fused
tice D3686, will promote needed accuracy and precision in the
silica capillary GC columns with 0.1 to 1-µm thick (df) phases
determination of airborne concentrations of many of the
such as 100% dimethyl polysiloxane, 95% dimethyl-5%
organic chemicals including but not limited to 29 CFR 1910,
diphenyl polysiloxane, and polyethylene glycol.
CDC-99-74-45,NIOSHManualofAnalyticalMethods,OSHA
7.4 Laboratory glassware, calibrated syringes, calibrated
Sampling and Analytical Methods, and HSE Methods for the
solvent dispensers, assorted Class A pipets and volumetric
Determination of Hazardous Substances. It can be used to
flasks and glass automatic sample injector (autosampler) vials
determine worker exposures to these chemicals, provided
with PTFE septum caps to contain analytical standards and
appropriate sampling periods are used.
samples.
5.3 Mostlaboratoriesareequippedwithapparatussimilarto
that described in Section 7. Other apparatus can be used when
8. Reagents
analytical procedures suitable for that equipment are em-
8.1 Purity of Reagents—Reagent grade chemicals shall be
usedinalltests.Allreagentsshallconformtothespecifications
7 of the Committee on Analytical Reagents of the American
Available from Occupational Safety and Health Administration (OSHA), 200
Constitution Ave., NW, Washington, DC 20210, https://www.osha.gov/dts/sltc/
methods/index.html.
8 9
Available from Health and Safety Executive (HSE), Redgrave Court, Merton Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
Road,Bootle,Merseyside,L207HS,http://www.hse.gov.uk/pubns/mdhs/index.htm. this standard.
D3687 − 19
Chemical Society where such specifications are available. usefultocreateanin-house“columnmap”foreachGCcolumn
Other grades may be used, provided it is first ascertained that listing retention times for each analyte determined using a
the reagent is of sufficiently high purity to permit its use standard temperature program and a standard carrier gas linear
without lessening the accuracy of the determination. velocity.
8.2 Analytical standards, reagent grade or better, typically
9.6 Prepare analytical standards that bracket the expected
97–99+%.
range of sample results for each of the analytes by injection of
microlitre amounts of the analytes into the extraction solution.
8.3 Carbon disulfide, reagent grade or better, typically
Forexample:iftherequestedanalyteistoluene,theairvolume
99.9% with low benzene content.
sampled with a charcoal tube is 12 L, the density of toluene is
8.4 Internal standard, reagent grade or better, typically
0.866 g/mL, the purity of the analytical standard is 99%, and
99+%, p-cymene and 1-phenyl hexane are often used. Other
the exposure limit (target concentration) is 200 ppm (753
internal standard reagents can be used providing that they not
mg/m ). Calculate the mass of toluene equivalent to the target
appear in air samples and that they are fully tested.
concentrationbymultiplyingtheexposurelimitbythecharcoal
3 3
8.5 Extraction solvent, usually consists of 0.25 µL of
sample air volume (753 mg/m ×0.012 m =9.04 mg per
internal standard per millilitre of carbon disulfide. Other
sample). Prepare a standard at approximately the target con-
extraction solvents can be used provided they are fully tested.
centration by diluting 10.00 µL of toluene to 1.00 mL with
(Warning—Carbon disulfide is toxic and extremely
extraction solvent. This standard will contain 8.57 mg/mL
flammable, as are many of the organic chemicals to be
toluene (10.00 µL×0.866 mg⁄µL×0.99 pure /1.00 mL).
analyzed.Work with these chemicals in a properly functioning
Prepare additional analytical standards at the reporting limit,
laboratory hood.)
0.25×, 0.5×, 1.5×, and 2.0× the target concentration. Standards
for other analytes can be prepared similarly to toluene using
9. Calibration
theirrespectiveexposurelimits,densities,puritiesofanalytical
standards, and sample air volume (or average air volume for
9.1 In general, follow the manufacturer’s manual and safety
multiple samples). Different analytes can be prepared in the
instructions to set up the gas chromatograph.Always use high
same solution if applicable. Prepare independent analytical
purity gases and high quality gas purifiers.
standardswithmaterialobtainedfromaseparatevendortotest
9.2 Install the selected GC column and set the linear
the purity of the source material and the accuracy of the
velocity of the carrier gas following manufacturer’s instruc-
standard preparation.
tions. Set the injector split ratio at 10:1 or at some other
9.7 Analyze the standards using the same temperature
appropriate ratio. The most commonly used capillary GC
programusedin9.5.Comparethechromatogramstobecertain
carriergasishydrogenbutheliumisalsoused.Settheinjector,
the analytes are resolved. Generally, chromatographic condi-
detector, and column oven temperatures appropriate for the
tions can be altered to separate interferences.
selected GC column. It is often useful to heat the GC column
at 10–20°C below the expected maximum operating tempera-
9.8 Use an internal standard (ISTD) calibration method for
ture of the column for about two hours before any analysis is
most organic compounds. An internal standard calibration
performed. Before analyzing standards or samples, place a
function is incorporated with most electronic data systems.
fresh septum into the injection port of the chromatograph.
Calibration curves for each analyte can be constructed by
Replace the septum daily or when necessary. Septum failure is
plotting detector response of standards (y axis) against mass
a frequent cause of inconsistent FID response and changes in
per standard (x axis). FID response is usually linear; therefore,
chromatography. (Warning—Hydrogen gas is explosive and
linearregressionisgenerallyappropriatetofindtheequationof
extremely flammable. It is absolutely essential that the gas
the best-fit line for the calibration curve. Program the data
chromatograph be leak free.)
system to calculate results in terms of micrograms per sample.
9.3 Makesurethattheelectronicdatasystemisproperlyset This is appropriate because both standards and samples are
to collect analytical data.
preparedin1.00mLofextractionsolvent.Typically,resultsfor
standards (other than for the reporting limit) calculated from
9.4 Prepare separate solutions containing 1 mL of each
the calibration curve will deviate from their theoretical
analyte per 1 mL of extraction solvent. These solutions are
amounts by not more than 610%. Usually, deviation for the
used to determine GC column retention time of the analytes.
reporting limit is no more than 625%. Prepare and analyze
9.5 Analyze these solutions and a reagent blank (without
fresh standards as necessary.Analyze a fresh set of calibration
charcoal) using an appropriate GC column and an appropriate
standards with each sample set, or with a day’s sequence of
oven temperature program to determine GC column retention
sample sets.
times for each analyte and for the internal standard. It may be
10. Sample Preparation
10.1 Consider potential analytical interferences that were
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
reported when the samples were received. Make certain that
listed by the American Chemical Society, see Analar Standards for Laboratory
the extraction efficiency (also called desorption efficiency) for
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
all requested analyses has been determined (as described in
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
MD. Section 11) before extracting the samples.
D3687 − 19
10.2 Most charcoal tubes have two sections and each 10.12 Perform replicate injections as necessary.
section is quantitively transferred to a separate labeled au-
11. Extraction Efficiency
tosampler vial. Some charcoal tubes have three sections and
11.1 Each analytical laboratory must determine its own
each of the three sections should be similarly transferred to a
extraction efficiencies because techniques and reagents can
separate labeled autosampler vial.
vary from one laboratory to another. Extraction efficiency can
10.3 Remove the plastic cap from end of the charcoal with
usually be considered constant for each laboratory, but it
the back-up section(s) of the sampling tube.
shouldbeconfirmedwheneverthesampleextractionprocessis
10.4 Remove the plug that holds the back-up section in
significantly changed. Perform preliminary tests to determine
place and transfer the charcoal to an appropriately labeled vial
theminimumamountoftimerequiredtocompletelyextractthe
and close the vial. Similarly transfer the second back-up
analytefromthecharcoal,andalsoifsomeformofmechanical
section(ifpresent)toaseparatelabeledvialandclosethevial.
agitation or other action is necessary. Extraction efficiency
(Asmall crochet hook is a convenient device for removing the
should be determined separately for each analyte. Other
plugsfromthesamplers,orahookcanbefashionedfromafine
extractionsolventsandinternalstandardsthanlistedinthistest
(18 to 20-gauge) steel wire or a 76-mm (3-in.) No. 20
method can be used provided they are tested. Confirm that
hypodermic needle.)
recovery of the internal standard from charcoal is sufficiently
high (at least 95%) by analyzing charcoal tube and reagent
10.5 Remove the plug and transfer the front section of
blanks. Select another chemical to be used as the internal
charcoal to an appropriately labeled vial and close the vial.
standard if recovery of the internal standard is not at least
Checktheplugstomakesurethatnocharcoaladherestothem.
95%. Low internal standard recovery will cause extraction
Discard the plugs and empty glass tube.
efficiency results
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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.
Designation: D3687 − 07 (Reapproved 2012) D3687 − 19
Standard Practice Test Method for
Analysis of Organic Compound Vapors Collected by the
Activated Charcoal Tube Adsorption Method
This standard is issued under the fixed designation D3687; 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. Scope
1.1 This practice covers the applications of methods for the extraction and gas chromatographic determination of organic vapors
that have been adsorbed from air in sampling tubes packed with activated charcoal.
1.2 This practice is complementary to Practice D3686.
1.3 This practice is applicable for analysis of samples taken from workplace or other atmospheres provided that the contaminant
adsorbs onto charcoal, that it can be adequately extracted from the charcoal, and that it can be analyzed by gas chromatography
(GC). Other adsorbents and other extraction techniques are described in Practice D6196.
1.4 Organic compounds of multicomponent samples may mutually interfere during analysis. Methods to resolve interferences
are given in Section 6.
1.5 The values stated in SI units are to be regarded as the standard.
1.6 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. Specific precautions are given in 8.4, 9.2, and in A1.2.3.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D3686 Practice for Sampling Atmospheres to Collect Organic Compound Vapors (Activated Charcoal Tube Adsorption Method)
D6196 Practice for Choosing Sorbents, Sampling Parameters and Thermal Desorption Analytical Conditions for Monitoring
Volatile Organic Chemicals in Air
E355 Practice for Gas Chromatography Terms and Relationships
2.2 NIOSH Standards:
CDC-99-74-45 Documentation of NIOSH Validation Tests
th 4
NIOSH Manual of Analytical Methods, 4 Ed.
2.3 OSHA Standards:
29 CFR 1910 Code of Federal Regulations, Regulations Relating to Labor, Occupational Safety and Health Administration,
Department of Labor
This practice test method is under the jurisdiction of ASTM Committee D22 on Air Quality and is the direct responsibility of Subcommittees D22.04 on Workplace Air
Quality.
Current edition approved April 1, 2012Aug. 1, 2019. Published July 2012September 2019. Originally approved in 1978. Last previous edition approved in 20072012 as
D3687 – 07.D3687 – 07 (2012). DOI: 10.1520/D3687-07R12.10.1520/D3687-19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Available from the U.S. Department of Commerce, National Technical Information Service, Port Royal5301 Shawnee Road, Springfield,Alexandria, VA 22161.22312,
https://www.ntis.gov.
NIOSH Manual of Analytical Methods (NMAM), http://www.cdc.gov/niosh/nmam (accessed 1/2007).Available from the Centers for Disease Control and Prevention
(CDC), https://www.cdc.gov/niosh/nmam.
Available from Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.Superintendent of Documents, 732 N. Capitol St., NW,
Washington, DC 20401-0001, http://www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D3687 − 19
OSHA Sampling and Analytical Methods
2.4 UK Health and Safety Executive (HSE):
Methods for the Determination of Hazardous Substances (MDHS)
2.5 Berufsgenossenschaftliches Institut für Arbeitsschulz (BGIA):
GESTIS Analytical Methods
3. Terminology
3.1 Definitions:
3.1.1 For definitions of terms used in this practice, refer to the terminology specified in D1356 and E355.
4. Summary of Practice
4.1 Organic vapors that have been collected on activated charcoal are extracted with carbon disulfide or another appropriate
solvent and are determined by GC using a flame ionization detector (FID). Carbon disulfide is a relatively small molecule that can
penetrate the “ink-bottle” shaped pores of activated charcoal, it has a high heat of adsorption on activated charcoal which helps
in displacing other adsorbed molecules, and it is a reasonably good solvent for most, especially non-polar, organic molecules. Polar
modifiers (such as N,N-dimethylformamide) are frequently added to enhance the recovery of polar organic compounds. Other
advantages to using carbon disulfide include an early elution time on most GC columns and a small FID response.
4.2 Interferences resulting from the analytes having similar retention times during GC analysis are resolved by changing the GC
column, by changing the operating parameters, or by fractionating the sample using solvent extraction as described in Section
A1.1.
4.3 Peak purity and identity can be confirmed using techniques such as GC/MS.
5. Significance and Use
5.1 Promulgations by the Federal Occupational Safety and Health Administration (OSHA) in 29 CFR 1910 designate that
certain organic compounds must not be present in workplace atmospheres at concentrations above specified values.
5.2 This practice, when used in conjunction with Practice D3686, will promote needed accuracy and precision in the
determination of airborne concentrations of many of the organic chemicals given in 29 CFR 1910, CDC-99-74-45, NIOSH Manual
of Analytical Methods, OSHA Sampling and Analytical Methods, HSE Methods for the Determination of Hazardous Substances,
and BGIA GESTIS Analytical Methods. It can be used to determine worker exposures to these chemicals, provided appropriate
sampling periods are used.
5.3 Most laboratories are equipped with apparatus similar to that described in Section 7. Other apparatus can be used when
analytical procedures suitable for that equipment are employed. The analytical techniques (or variations thereof) described in
Sections 9 – 11 are in general use to analyze volatile organic compounds extracted from charcoal. Other procedures can be used
when appropriate.
6. Interferences
6.1 Any chemical that produces an FID response and has a similar retention time as the analyte is a potential interference. If
potential interferences were reported when the samples were received they should be considered before the samples are extracted.
Generally, gas chromatographic conditions such as the type of GC column (phase) or operating parameters can be changed to
resolve interferences.
6.2 Selective solvent stripping techniques have been used successfully to make clean and fast separations of polar, nonpolar and
oxygenated compounds. A general guideline is given in A1.1 and detailed procedures are given in Refs (1 and 2).
6.3 When necessary, the identity or purity of an analyte peak can be confirmed by GC/mass spectrometry.
6.4 The presence of co-adsorbed chemicals can affect the recovery (extraction efficiency) of a particular analyte. Suspected
effects can be tested by spiking the analytes on charcoal as in Section 11.
7. Apparatus
7.1 Gas chromatograph, equipped with a flame ionization detector (FID), a temperature-programmable oven, and an automatic
sample injector (autosampler). Sample injection may be performed manually if necessary. Other detectors (such as electron
capture, flame photometric, nitrogen phosphorous detectors) can be used when appropriate but the extraction solvent may have to
be modified.
OSHA Sampling and Analytical Methods, http://www.osha.gov/dts/sltc/methods/index.html (accessed 1/2007).Available from Occupational Safety and Health
Administration (OSHA), 200 Constitution Ave., NW, Washington, DC 20210, https://www.osha.gov/dts/sltc/methods/index.html.
HSE Methods for the Determination of Hazardous Substances (MDHS), http://www.hse.gov.uk/pubns/mdhs/index.htm# (accessed 1/2007).
GESTIS Analytical Methods, http://www.hvbg.de/e/bia/gestis/analytical_methods/index.html (accessed 1/2007).Available from Health and Safety Executive (HSE),
Redgrave Court, Merton Road, Bootle, Merseyside, L20 7HS, http://www.hse.gov.uk/pubns/mdhs/index.htm.
The boldface numbers in parentheses refer to the list of references at the end of this standard.
D3687 − 19
7.2 Electronic data system, or other suitable means to record and measure detector response, to prepare calibration curves, and
to process sample results.
7.3 GC columns, required to separate the complex mixture of possible organic chemicals. Examples of the most common and
useful GC columns are 60-m long, 0.32-mm i.d. fused silica capillary GC columns with 0.1 to 1-μm thick (df) phases such as
100 % dimethyl polysiloxane, 95 % dimethyl-5% diphenyl polysiloxane, and polyethylene glycol.
7.4 Laboratory glassware, calibrated syringes, calibrated solvent dispensers, assorted Class A pipets and volumetric flasks and
glass automatic sample injector (autosampler) vials with PTFE septum caps to contain analytical standards and samples.
8. Reagents
8.1 Analytical standards, reagent grade or better, typically 97-99+%.
8.2 Carbon disulfide, reagent grade or better, typically 99.9 % with low benzene content.
8.3 Internal standard, reagent grade or better, typically 99+%, p-cymene and 1-phenyl hexane are often used. Other internal
standard reagents can be used providing that they not appear in air samples and that they are fully tested.
8.4 Extraction solvent, usually consists of 0.25 microlitres of internal standard per milliliter of carbon disulfide. Other extraction
solvents can be used provided they are fully tested. (Warning—Carbon disulfide is toxic and extremely flammable, as are many
of the organic chemicals to be analyzed. Work with these chemicals in a properly functioning laboratory hood.)
9. Calibration
9.1 In general, follow the manufacturer’s manual and safety instructions to set up the gas chromatograph. Always use high
purity gases and high quality gas purifiers.
9.2 Install the selected GC column and set the linear velocity of the carrier gas following manufacturer’s instructions. Set the
injector split ratio at 10:1 or at some other appropriate ratio. The most commonly used capillary GC carrier gas is hydrogen. Set
the injector, detector, and column oven temperatures appropriate for the selected GC column. It is often useful to heat the GC
column at 10-20°C below the expected maximum operating temperature of the column for about two hours before any analysis
is performed. Before analyzing standards or samples, place a fresh septum into the injection port of the chromatograph. Replace
the septum daily or when necessary. Septum failure is a frequent cause of inconsistent FID response and changes in
chromatography. (Warning—Hydrogen gas is explosive and extremely flammable. It is absolutely essential that the gas
chromatograph be leak free.)
9.3 Make sure that the electronic data system is properly set to collect analytical data.
9.4 Prepare separate solutions containing 1 mL of each analyte per 1 mL of extraction solvent. These solutions are used to
determine GC column retention time of the analytes.
9.5 Analyze these solutions and a reagent blank (without charcoal) using an appropriate GC column and an appropriate oven
temperature program to determine GC column retention times for each analyte and for the internal standard. It may be useful to
create an in-house “column map” for each GC column listing retention times for each analyte determined using a standard
temperature program and a standard carrier gas linear velocity.
9.6 Prepare analytical standards that bracket the expected range of sample results for each of the analytes by injection of
microliter amounts of the analytes into the extraction solution. For example: if the requested analyte is toluene, the air volume
sampled with a charcoal tube is 12 L, the density of toluene is 0.866 g/mL, the purity of the analytical standard is 99 %, and the
exposure limit (target concentration) is 200 ppm (753 mg/m ). Calculate the mass of toluene equivalent to the target concentration
3 3
by multiplying the exposure limit by the charcoal sample air volume (753 mg/m × 0.012 m = 9.04 mg per sample). Prepare a
standard at approximately the target concentration by diluting 10.00 μL of toluene to 1.00 mL with extraction solvent. This standard
will contain 8.57 mg/mL toluene (10.00 μL × 0.866 mg ⁄μL × 0.99 pure /1.00 mL). Prepare additional analytical standards at the
reporting limit, 0.25×, 0.5×, 1.5×, and 2.0× the target concentration. Standards for other analytes can be prepared similarly to
toluene using their respective exposure limits, densities, purities of analytical standards, and sample air volume (or average air
volume for multiple samples). Different analytes can be prepared in the same solution if applicable. Prepare independent analytical
standards with material obtained from a separate vendor to test the purity of the source material and the accuracy of the standard
preparation.
9.7 Analyze the standards using the same temperature program used in 9.5. Compare the chromatograms to be certain the
analytes are resolved. Generally, chromatographic conditions can be altered to separate interferences.
9.8 Use an internal standard (ISTD) calibration method for most organic compounds. An internal standard calibration function
is incorporated with most electronic data systems. Calibration curves for each analyte can be constructed by plotting detector
response of standards (y axis) against mass per standard (x axis). FID response is usually linear; therefore, linear regression is
generally appropriate to find the equation of the best-fit line for the calibration curve. Program the data system to calculate results
in terms of micrograms per sample. This is appropriate because both standards and samples are prepared in 1.00 mL of extraction
D3687 − 19
solvent. Typically, results for standards (other than for the reporting limit) calculated from the calibration curve will deviate from
their theoretical amounts by not more than 610 %. Usually, deviation for the reporting limit is no more than 625 %. Prepare and
analyze fresh standards as necessary. Analyze a fresh set of calibration standards with each sample set, or with a day’s sequence
of sample sets.
10. Sample Preparation
10.1 Consider potential analytical interferences that were reported when the samples were received. Make certain that the
extraction efficiency (also called desorption efficiency) for all requested analyses has been determined (as described in Section 11)
before extracting the samples.
10.2 Most charcoal tubes have two sections and each section is quantitively transferred to a separate labeled autosampler vial.
Some charcoal tubes have three sections and each of the three sections should be similarly transferred to a separate labeled
autosampler vial.
10.3 Remove the plastic cap from end of the charcoal with the back-up section(s) of the sampling tube.
10.4 Remove the plug that holds the back-up section in place and transfer the charcoal to an appropriately labeled vial and close
the vial. Similarly transfer the second back-up section (if present) to a separate labeled vial and close the vial. (A small crochet
hook is a convenient device for removing the plugs from the samplers, or a hook can be fashioned from a fine (18 to 20-gauge)
steel wire or a 3-in. (76-mm) No. 20 hypodermic needle.)
10.5 Remove the plug and transfer the front section of charcoal to an appropriately labeled vial and close the vial. Check the
plugs to make sure that no charcoal adheres to them. Discard the plugs and empty glass tube.
10.6 Continue this process until all of the samples have been transferred appropriately to vials. Prepare laboratory media blanks
for analysis in addition to the field media blanks. Laboratory media is identical to field media except that these charcoal tubes have
been set aside for use in the laboratory.
10.7 For some highly volatile compounds such as methylene chloride, it may be useful to refrigerate the vials containing the
charcoal sections before addition of the extraction solvent. Loss can occur due to heat generated by addition of the extraction
solvent. Use a calibrated 1.00-mL solvent dispenser or a 1.00-mL Class A volumetric pipet to transfer the extraction solvent to the
sample vials. It is sometimes necessary to use a larger volume of extraction solvent to adequately extract samples. Prepare
analytical standards with the same volume of extraction solvent used to extract samples.
10.8 With this dispenser or pipet, transfer 1.00 mL of extraction solvent to each of the vials, taking care to seal them securely
after the solvent has been added.
10.9 From time to time (at approximately 5 min intervals), agitate the samples. Let the extraction process continue for at least
30 min, however, some analytes require longer times (3). Use of a mechanical shaker or other device to agitate the samples may
enhance extraction.
10.10 Ensure that the electronic data system is properly set to collect analytical data.
10.11 Analyze the samples using the same temperature program as used for the standards in Section 9. Place autosampler vials
containing reagent blanks between samples and standards when “carry-over” from a previous injection is suspected.
10.12 Perform replicate injections as necessary.
11. Extraction Efficiency
11.1 Each analytical laboratory must determine its own extraction efficiencies because techniques and reagents can vary from
one laboratory to another. Extraction efficiency can usually be considered constant for each laboratory, but it should be confirmed
whenever the sample extraction process is significantly changed. Perform preliminary tests to determine the minimum amount of
time required to completely extract the analyte from the charcoal, and also if some form of mechanical agitation or other action
is necessary. Extraction efficiency should be determined separately for each analyte. Other extraction solvents and internal
standards than listed in this practice can be used provided they are tested. Confirm that recovery of the internal standard from
charcoal is sufficiently high (at least 95 %) by analyzing charcoal tube and reagent blanks. Select another chemical to be used as
the internal standard if recovery of the internal standard is not at least 95 %. Low internal standard recovery will cause extraction
efficiency results to be artificially high.
11.2 Determine extraction efficiency for four samples at each of the following levels: the reporting limit, 0.25×, 0.5×, 1×, 1.5×
and 2.0× times the target concentration masses as determined in Section 9. Perform a test at 1× the target concentration with wet
samplers that were prepared by spiking the charcoal with 50 μL of water a day before spiking the analyte. A 100-mg section of
activated charcoal is saturated after collecting approximately 50 mg of water. The “wet test” is performed to determine if the
The 1.00-mL volume of CS is used when analyzing 150-mg charcoal tubes. If larger charcoal tubes are being analyzed, a proportionately larger volume of CS should
2 2
be used.
D3687 − 19
analyte partitions in the water phase resulting from extraction of wet samples collected in humid atmospheres. This undesirable
situation can sometimes be resolved by using drying reagents such as magnesium sulfate or by using alternative extraction solvents.
11.3 Transfer a sufficient number of front sections of charcoal tubes to autosampler vials and securely seal the vials. If the
back-up section contains half the amount in the front section then two back-up sections can be combined in the same vial to prepare
the equivalent of a front section. Charcoal used as received from the manufacturer is knows as “dry” media.
11.4 Spike each vial with the appropriate amount of analyte and allow the vials to stand at room temperature overnight.
11.5 Extract the vials by removing the caps and adding 1.00 mL (or larger volume if necessary) of extraction solvent as in
Section 10. Agitate the samples manually as in Section 10, or mechanically agitate the samples if it is determined to be necessary
in preliminary tests. Allow the samples to extract for the amount of time determined in the preliminary tests.
11.6 Analyze the four extracted samples at each level plus three separate analytical standards prepared at each level. The
standards should be prepared from the same solution used to spike the samples.
11.7 Calculate results for each level separately after using one of the three standards to perform a single point ISTD calibration.
Average the results for the standards and divide each sample result by that average and multiply by 100 to calculate the extraction
efficiency. The average of the results is the extraction efficiency at that level.
11.8 Repeat the process in 11.6 for each level performing a new single point ISTD calibration at each level.
11.9 The extraction efficiency should be high and constant at all levels. An alternative extraction solvent and technique should
be considered if the extraction efficiency is less than 75 % or if it is not constant. Average the extraction efficiencies for the six
levels providing they are constant (less than 65 % difference between levels). Repeat the test for any level that appears to be an
outlier and be wary of discarding results. Do not include results from the “wet test” in the average because this would bias the
average.
11.10 Low or inconsistent extraction efficiencies can often be resolved by use of a different extraction solvent or by using
mechanical agitation.
11.11 Determine if extracted samples are stable by reanalyzing the dry 1× times target concentration samples about 24 hours
after they were extracted. Use fresh analytical standards.
11.12 Sometimes it is necessary to use low or non-constant extraction efficiencies if they are determined to be reproducible and
if they are greater than 75 %. This situation should be avoided if possible.
12. Sample Results
12.1 Any chemical that produces an FID response and has a similar retention time as the analyte is a potential interference. If
potential interferences were reported they should be considered before the samples are extracted. Alternative GC columns may help
resolve interferences. When necessary, the identity or purity of an analyte peak can be confirmed by GC/mass spectrometry.
12.2 Obtain analytical results in terms of micrograms per sample with the electronic data system that was programmed to
produce calibration curves that were prepared using analytical data from the analytical standards prepared and analyzed as in
Section 9. Dilute the samples with extraction solvent or analyze additional standards if sample results are not within the range of
prepared standards.
12.3 Determine if field media blank samples were contaminated by comparison of analytical results with results from laboratory
media blanks. Do not subtract laboratory media blank media results from field sample results. If the field media blank sample has
been severely contaminated then it is possible that the field samples have been similarly contaminated. Do not perform blank
subtractions using severely contaminated field media blanks, but report analytical results in terms of mass per sample for the field
media blank along with results for the field samples and then qualify all results as “possibly contaminated”. Do not calculate air
concentration for these samples, but allow the person performing sampling to make such calculations.
12.4 Calculate total micrograms of an analyte per sample by adding results for the charcoal tube front section and results for
the back-up section(s) together. Correct this total amount by subtracting the total amount of analyte (if any) found on the field
media blank sample. If the sample back-up section contains more than 10 % of the analyte mass found on the front section, report
this fact along with sample results. Divide the total blank-corrected result by the decimal equivalent of the extraction efficiency
(that is, 98.5 % = 0.985) to calculate corrected μg per sample.
12.5 Calculate air concentrations as follows:
corrected μg per sample
mg/m 5 (1)
litres of air sampled
mg/m
ppm 5 24.47 3 (2)
molecular weight of analyte
D3687 − 19
13. Quality Assurance
13.1 Analytical laboratory accreditation (such as American Industrial Hygiene Association Laboratory Quality Assurance
Programs) and laboratory proficiency testing programs can help establish and maintain high standards of laboratory performance
quality.
13.2 It is beyond the scope of this practice to prescribe how a quality assurance program should be organized and function. The
overall purpose of quality assurance is to ensure that reported laboratory results are sufficiently accurate and precise for their
intended purpose. To this end, most laboratories have a quality assurance program to estimate combined sampling and analytical
uncertainty. Sampling uncertainty, often estimated from sampling pump uncertainty, is usually assumed to be 65 %. Analytical
uncertainty is generally estimated from the results of spiked quality control samples that are analyzed along with field samples.
Analytical uncertainty is then statistically combined with sampling uncertainty to estimate overall sampling and analytical
uncertainty. The generally accepted limit for sampling and analytical uncertainty is no more than 625 %.
14. Keywords
14.1 activated charcoal tube; air monitoring; charcoal tube; organic vapors; sampling and analysis; workplace atmospheres
ANNEX
(Mandatory Information)
A1. SELECTIVE SOLVENT-STRIPPING TECHNIQUES
A1.1 Organic compounds are soluble, or react with a number of solvents in a selective manner. Advantage of these phenomena
may be taken in the analysis of solvent systems in carbon disulfide when there is peak overlap (1).
A1.2 The following criteria are generally useful:
A1.2.1 Certain amines and amides are water soluble. Dimethylformamide is rapidly extracted from carbon disulfide with one wash
of laboratory grade water.
A1.2.2 Oxygenated hydrocarbons such as esters, ketones, alcohols, and ethers are extracted by a solution consisting of 2 parts by
volume of concentrated sulfuric acid and one of phosphoric acid (85 %). A volume of 0.5 to 1 mL of this solution is sufficient to
effect a quantitative extraction of an oxygenated hydrocarbon compound from carbon disulfide (1).
A1.2.3 Dimethyl sulfate will extract nitrated aromatic compound from a mixture of aromatics and alkyl hydrocarbon solvents in
carbon disulfide. (Warning—Dimethyl sulfate is a suspected carcinogen and is extremely corrosive.)
A1.2.4 A saturated solution of sodium metabisulfite will extract selectively acetone and methyl ethyl ketone from a mixture of
oxygenated and other carbon compounds in carbon disulfide with one wash.
A1.2.5 A10 % solution of hydroxylamine hydrochloride will extract selectively acetone, methyl ethyl ketone, isobutyl ketone,
methyl propyl ketone and methyl butyl ketone from solution in carbon disulfide in three separate washes.
A1.3 The usual semimicrochemical techniques and precautions should be taken when such manipulations of the carbon disulfide
eluate are undertaken, and it should be recognized that carbon disulfide is highly toxic, volatile, and flammable.
D3687 − 19
REFERENCES
(1) Levadie, B., and MacAskill, S. M., “Analysis of Organic Solvents Taken on Charcoal Tube Samplers by a Simplified Technique,” Analytical
Chemistry, Vol 48, No. 1, 1976, pp. 76–78.
(2) Levadie, B., and MacAskill, S. M., addendum to Ref (1), Vol 48, No. 11, p. 1656.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
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1. Scope
1.1 This test method describes the extraction and gas chromatographic determination of organic vapors that have been adsorbed
from air in sampling tubes packed with activated charcoal.
1.2 This test method is complementary to Practice D3686.
1.3 This test method is applicable for analysis of samples taken from workplace or other atmospheres provided that the
contaminant adsorbs onto charcoal, that it can be adequately extracted from the charcoal, and that it can be analyzed by gas
chromatography (GC). Other adsorbents and other extraction techniques are described in Practice D6196.
1.4 Organic compounds of multicomponent samples may mutually interfere during analysis. Methods to resolve interferences
are given in Section 6.
1.5 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for
information only and are not considered standard.
1.6 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, health, and environmental practices and determine the applicability of
regulatory limitations prior to use. Specific precautions are given in 8.5, 9.2, and in X1.2.3.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1356 Terminology Relating to Sampling and Analysis of Atmospheres
D3686 Practice for Sampling Atmospheres to Collect Organic Compound Vapors (Activated Charcoal Tube Adsorption Method)
D6196 Practice for Choosing Sorbents, Sampling Parameters and Thermal Desorption Analytical Conditions for Monitoring
Volatile Organic Chemicals in Air
E355 Practice for Gas Chromatography Terms and R
...

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