ASTM D6520-18

Standard Practice for the Solid Phase Micro Extraction (SPME) of Water and its Headspace for the Analysis of Volatile and Semi-Volatile Organic Compounds

SIGNIFICANCE AND USE
5.1 This practice provides a general procedure for the solid phase micro extraction of volatile and semi-volatile organic compounds from an aqueous matrix or its headspace. Solid sorbent extraction is used as the initial step in the extraction of organic constituents for the purpose of quantifying or screening for extractable organic compounds.  
5.2 Typical detection limits that can be achieved using SPME techniques with gas chromatography with flame ionization detector (FID), electron capture detector (ECD), or with a mass spectrometer (MS) range from mg/L to μg/L. The detection limit, linear concentration range, and sensitivity of the test method for a specific organic compound will depend upon the aqueous matrix, the fiber phase, the sample temperature, sample volume, sample mixing, and the determinative technique employed.  
5.3 SPME has the advantages of speed, no desorption solvent, simple extraction device, and the use of small amounts of sample.  
5.3.1 Extraction devices vary from a manual SPME fiber holder to automated commercial device specifically designed for SPME.  
5.3.2 Listed below are examples of organic compounds that can be determined by this practice. This list includes both high and low boiling compounds.
Volatile Organic Compounds (1-3)3
Pesticides, General (4, 5)
Organochlorine Pesticides (6)
Organophosphorous Pesticides (7, 8)
Polyaromatic Hydrocarbons (9, 10)
Polychlorinated Biphenyls (10)
Phenols (11)
Nitrophenols (12)
Amines (13)  
5.3.3 SPME may be used to screen water samples prior to purge and trap extraction to determine if dilution is necessary, thereby eliminating the possibility of trap overload.
SCOPE
1.1 This practice covers procedures for the extraction of volatile and semi-volatile organic compounds from water and its headspace using solid phase micro extraction (SPME).  
1.2 The compounds of interest must have a greater affinity for the SPME-absorbent polymer or adsorbent or combinations of these than the water or headspace phase in which they reside.  
1.3 Not all of the analytes that can be determined by SPME are addressed in this practice. The applicability of the absorbent polymer, adsorbent, or combination thereof, to extract the compound(s) of interest must be demonstrated before use.  
1.4 This practice provides sample extracts suitable for quantitative or qualitative analysis by gas chromatography (GC) or gas chromatography-mass spectrometry (GC-MS).  
1.5 Where used, it is the responsibility of the user to validate the application of SPME to the analysis of interest.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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. For specific hazard statements, see Section 12.  
1.8 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: 14-Dec-2018
• 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

Relations

• Refers: ASTM D4448-01(2019) - Standard Guide for Sampling Ground-Water Monitoring Wells
• Effective Date: 01-Feb-2019
• Referred By: ASTM D6889-03(2017) - Standard Practice for Fast Screening for Volatile Organic Compounds in Water Using Solid Phase Microextraction (SPME)
• Effective Date: 15-Dec-2018

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: D6520 − 18
Standard Practice for
the Solid Phase Micro Extraction (SPME) of Water and its
Headspace for the Analysis of Volatile and Semi-Volatile
1
Organic Compounds
This standard is issued under the fixed designation D6520; 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 2. Referenced Documents
2
1.1 This practice covers procedures for the extraction of 2.1 ASTM Standards:
volatile and semi-volatile organic compounds from water and D1129 Terminology Relating to Water
its headspace using solid phase micro extraction (SPME). D1193 Specification for Reagent Water
D3370 Practices for Sampling Water from Closed Conduits
1.2 The compounds of interest must have a greater affinity
D3694 Practices for Preparation of Sample Containers and
for the SPME-absorbent polymer or adsorbent or combinations
for Preservation of Organic Constituents
of these than the water or headspace phase in which they
D3856 Guide for Management Systems in Laboratories
reside.
Engaged in Analysis of Water
1.3 Not all of the analytes that can be determined by SPME
D4448 Guide for Sampling Ground-Water MonitoringWells
are addressed in this practice. The applicability of the absor-
bent polymer, adsorbent, or combination thereof, to extract the 3. Terminology
compound(s) of interest must be demonstrated before use.
3.1 Definitions:
1.4 This practice provides sample extracts suitable for 3.1.1 For definitions of terms used in this standard, refer to
quantitative or qualitative analysis by gas chromatography Terminology D1129.
(GC) or gas chromatography-mass spectrometry (GC-MS).
4. Summary of Practice
1.5 Whereused,itistheresponsibilityoftheusertovalidate
4.1 This practice employs adsorbent/liquid or adsorbent/gas
the application of SPME to the analysis of interest.
extractiontoisolatecompoundsofinterest.Anaqueoussample
1.6 The values stated in SI units are to be regarded as
is added to a septum-sealed vial. The aqueous phase or its
standard. No other units of measurement are included in this
headspace is then exposed to an adsorbent coated on a fused
standard.
silica fiber. The fiber is desorbed in the heated injection port of
1.7 This standard does not purport to address all of the
a GC or GC-MS or the injector of an high-performance liquid
safety concerns, if any, associated with its use. It is the
chromatography (HPLC).
responsibility of the user of this standard to establish appro-
4.2 The desorbed organic analytes may be analyzed using
priate safety, health, and environmental practices and deter-
instrumental methods for specific volatile or semi-volatile
mine the applicability of regulatory limitations prior to use.
organic compounds. This practice does not include sample
For specific hazard statements, see Section 12.
extract clean-up procedures.
1.8 This international standard was developed in accor-
dance with internationally recognized principles on standard-
5. Significance and Use
ization established in the Decision on Principles for the
5.1 This practice provides a general procedure for the solid
Development of International Standards, Guides and Recom-
phase micro extraction of volatile and semi-volatile organic
mendations issued by the World Trade Organization Technical
compounds from an aqueous matrix or its headspace. Solid
Barriers to Trade (TBT) Committee.
sorbent extraction is used as the initial step in the extraction of
organicconstituentsforthepurposeofquantifyingorscreening
for extractable organic compounds.
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
2
Organic Substances in Water. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 15, 2018. Published January 2019. Originally contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
approved in 2000. Last previous edition approved in 2012 as D6520 – 06 (2012). Standards volume information, refer to the standard’s Document Summary page on
DOI: 10.1520/D6520-18. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6520 − 18
5.2 Typical detection limits that can be achieved using 7. Interferences
SPME techniques with gas chromatography with flame ioniza-
7.1 Reagents, glassware, se
...

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: D6520 − 06 (Reapproved 2012) D6520 − 18
Standard Practice for
the Solid Phase Micro Extraction (SPME) of Water and its
Headspace for the Analysis of Volatile and Semi-Volatile
1
Organic Compounds
This standard is issued under the fixed designation D6520; 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 procedures for the extraction of volatile and semi-volatile organic compounds from water and its
headspace using solid-phase microextraction solid phase micro extraction (SPME).
1.2 The compounds of interest must have a greater affinity for the SPME-absorbent polymer or adsorbent or combinations of
these than the water or headspace phase in which they reside.
1.3 Not all of the analytes that can be determined by SPME are addressed in this practice. The applicability of the absorbent
polymer, adsorbent, or combination thereof, to extract the compound(s) of interest must be demonstrated before use.
1.4 This practice provides sample extracts suitable for quantitative or qualitative analysis by gas chromatography (GC) or gas
chromatography-mass spectrometry (GC-MS).
1.5 Where used, it is the responsibility of the user to validate the application of SPME to the analysis of interest.
1.6 The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.
1.7 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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazard statements, see Section 1012.
1.8 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
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D3370 Practices for Sampling Water from Closed Conduits
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
D3856 Guide for Management Systems in Laboratories Engaged in Analysis of Water
D4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data (Withdrawn
3
2002)
D4448 Guide for Sampling Ground-Water Monitoring Wells
3. Terminology
3.1 Definitions—For definitions of terms used in this practice, refer to Terminology D1129.
3.1 Definitions:
3.1.1 For definitions of terms used in this standard, refer to Terminology D1129.
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for Organic
Substances in Water.
Current edition approved June 15, 2012Dec. 15, 2018. Published June 2012January 2019. Originally approved in 2000. Last previous edition approved in 2012 as
D6520 – 06.D6520 – 06 (2012). DOI: 10.1520/D6520-06R12.10.1520/D6520-18.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
D6520 − 18
4. Summary of Practice
4.1 This practice employs adsorbent/liquid or adsorbent/gas extraction to isolate compounds of interest. An aqueous sample is
added to a septum-sealed vial. The aqueous phase or its headspace is then exposed to an adsorbent coated on a fused silica fiber.
The fiber is desorbed in the heated injection port of a GC or GC-MS or the injector of an HPLC.high-performance liquid
chromatography (HPLC).
4.2 The desorbed organic analytes may be analyzed using instrumental methods for specific volatile or semi-volatile organic
compounds. This practice does not include sample extract clean-up procedures.
5. Significance and Use
5.1 This practice
...