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ASTM D3871-84(2003)

(Test Method)

Standard Test Method for Purgeable Organic Compounds in Water Using Headspace Sampling

Standard Test Method for Purgeable Organic Compounds in Water Using Headspace Sampling

SIGNIFICANCE AND USE
Purgeable organic compounds, including organohalides, have been identified as contaminants in raw and drinking water. These contaminants may be harmful to the environment and man. Dynamic headspace sampling is a generally applicable method for concentrating these components prior to gas chromatographic analysis (1 to 5).5 This test method can be used to quantitatively determine purgeable organic compounds in raw source water, drinking water, and treated effluent water.
SCOPE
1.1 This test method covers the determination of most purgeable organic compounds that boil below 200°C and are less than 2 % soluble in water. It covers the low μg/L to low mg/L concentration range (see Section 15 and Appendix X1).
1.2 This test method was developed for the analysis of drinking water. It is also applicable to many environmental and waste waters when validation, consisting of recovering known concentrations of compounds of interest added to representative matrices, is included.
1.3 Volatile organic compounds in water at concentrations above 1000 μg/L may be determined by direct aqueous injection in accordance with Practice D 2908.
1.4 It is the user's responsibility to assure the validity of the test method for untested matrices.
1.5 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 precautionary statements are given in 8.5.5.1.

General Information

Status
Historical
Publication Date
09-Jan-2003
ICS
13.060.50 - Examination of water for chemical substances
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Replaces
ASTM D3871-84(1995)e1 - Standard Test Method for Purgeable Organic Compounds in Water Using Headspace Sampling
Effective Date
10-Jan-2003
Replaced By
ASTM D3871-84(2011) - Standard Test Method for Purgeable Organic Compounds in Water Using Headspace Sampling
Effective Date
01-May-2011
Referred By
ASTM D5790-18 - Standard Test Method for Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas Chromatography/Mass Spectrometry
Effective Date
10-Jan-2003
Referred By
ASTM D3973-85(2017) - Standard Test Method for Low-Molecular Weight Halogenated Hydrocarbons in Water
Effective Date
10-Jan-2003
Referred By
ASTM D3694-96(2017) - Standard Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
Effective Date
10-Jan-2003
Referred By
ASTM D4128-18 - Standard Guide for Identification and Quantitation of Organic Compounds in Water by Combined Gas Chromatography and Electron Impact Mass Spectrometry
Effective Date
10-Jan-2003

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ASTM D3871-84(2003) - Standard Test Method for Purgeable Organic Compounds in Water Using Headspace SamplingASTM D3871-84(2003) - Standard Test Method for Purgeable Organic Compounds in Water Using Headspace Sampling
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ASTM D3871-84(2003) - Standard Test Method for Purgeable Organic Compounds in Water Using Headspace Sampling
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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:D3871–84 (Reapproved 2003)
Standard Test Method for
Purgeable Organic Compounds in Water Using Headspace
1
Sampling
This standard is issued under the fixed designation D3871; 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 3.2 Description of Term Specific to This Standard:
3.2.1 purgeable organic—any organic material that is re-
1.1 This test method covers the determination of most
moved from aqueous solution under the purging conditions
purgeable organic compounds that boil below 200°C and are
described in this test method (10.1.1).
less than 2 % soluble in water. It covers the low µg/L to low
mg/L concentration range (see Section 15 and Appendix X1).
4. Summary of Test Method
1.2 This test method was developed for the analysis of
4.1 An inert gas is bubbled through the sample to purge
drinking water. It is also applicable to many environmental and
volatilecompoundsfromtheaqueousphase.Thesecompounds
waste waters when validation, consisting of recovering known
are then trapped in a column containing a suitable sorbent.
concentrations of compounds of interest added to representa-
After purging is complete, trapped components are thermally
tive matrices, is included.
desorbed onto the head of a gas chromatographic column for
1.3 Volatile organic compounds in water at concentrations
separation and analysis. Measurement is accomplished with an
above 1000 µg/L may be determined by direct aqueous
appropriate detector.
injection in accordance with Practice D2908.
1.4 It is the user’s responsibility to assure the validity of the
5. Significance and Use
test method for untested matrices.
5.1 Purgeable organic compounds, including organohalides,
1.5 This standard does not purport to address all of the
have been identified as contaminants in raw and drinking
safety concerns, if any, associated with its use. It is the
water. These contaminants may be harmful to the environment
responsibility of the user of this standard to establish appro-
and man. Dynamic headspace sampling is a generally appli-
priate safety and health practices and determine the applica-
cable method for concentrating these components prior to gas
bility of regulatory limitations prior to use. Specific precau-
3
chromatographic analysis (1 to 5). This test method can be
tionary statements are given in 8.5.5.1.
used to quantitatively determine purgeable organic compounds
in raw source water, drinking water, and treated effluent water.
2. Referenced Documents
2
2.1 ASTM Standards:
6. Interferences
D1129 Terminology Relating to Water
6.1 Purgeable compounds that coelute with components of
D1193 Specification for Reagent Water
interest and respond to the detector will interfere with the
D2908 Practice for Measuring Volatile Organic Matter in
chromatographicmeasurement.Likelihoodofinterferencemay
Water by Aqueous-Injection Gas Chromatography
be decreased by using dissimilar columns or a more selective
E355 Practice for Gas Chromatography Terms and Rela-
detector for the chromatographic step.
tionships
7. Apparatus
3. Terminology
7.1 Purging Device—Commercial devices are available for
3.1 Definitions—For definitions of terms used in this test
this analysis. Either commercial apparatus or the equipment
method, refer to Terminology D1129 and Practice E355.
described below may be used for this analysis. Devices used
shall be capable of meeting the precision and bias statements
1
This test method is under the jurisdiction of ASTM Committee D19 on Water
given in 15.1.
andisthedirectresponsibilityofSubcommitteeD19.06onMethodsforAnalysisfor
7.1.1 Glass Purging Device having a capacity of 5 mL is
Organic Substances in Water.
shown in Fig. A1.1. Construction details are given in Annex
Current edition approved Jan. 10, 2003. Published January 2003. Originally
´1
approved in 1979. Last previous edition approved in 1995 as D3871 – 84 (1995) .
A1. A glass frit is installed at the base of the sample reservoir
DOI: 10.1520/D3871-84R03.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on The boldface numbers in parentheses refer to the references at the end of this
the ASTM website. test method.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
D3871–84 (2003)
toallowfinelydividedgasbubblestopassthroughtheaqueous 7.3.2.2 The flow controller, PTFE tubi
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1.3 A reporting limit check sample (RLCS) is analyzed during every batch to ensure that if an analyte was present in a sample at or near the reporting limit it would be positively identified and accurately quantitated within set quality control limits. A method detection limit (MDL) study was not done for this method, the method detection limits would be much lower than the reporting limits in this method and would be irrelevant. A RLCS was determined to be more applicable for this standard. If this method is adapted to report much lower or near the MDL then a MDL study would be warranted.  
1.4 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.5 The Reporting Range for the target analytes are listed in Table 1.  
1.5.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 6 after taking into account an 8 mL water sample volume and a final diluted sample volume of 10 mL (80 % water/20 % methanol).  
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Standard Test Method for Determination of Nonylphenol, p-tert-Octylphenol, Nonylphenol Monoethoxylate and Nonylphenol Diethoxylate in Environmental Waters by Liquid Chromatography/Tandem Mass Spectrometry

SIGNIFICANCE AND USE
5.1 NP and OP have been shown to have toxic effects in aquatic organisms. The source of NP and OP is prominently from the use of common commercial surfactants. The most widely used surfactant is nonylphenol ethoxylate (NPEO) which has an average ethoxylate chain length of nine. The ethoxylate chain is readily biodegraded to form NP1EO, NP2EO, nonylphenol carboxylate (NPEC) and, under anaerobic conditions, NP. NP will also biodegrade, but may be released into environmental waters directly at trace levels. This method has been investigated and is applicable for environmental waters, including seawater.
SCOPE
1.1 This test method covers the determination of nonylphenol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), and octylphenol (OP), extracted from water utilizing solid phase extraction (SPE), separated using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS). These compounds are qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting limit (RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.    
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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.  
1.5 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.

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