ASTM D6520-06
(Practice)Standard Practice for the Solid Phase Micro Extraction (SPME) of Water and its Headspace for the Analysis of Volatile and Semi-Volatile Organic Compounds
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
This practice provides a general procedure for the solid-phase microextraction 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.
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.
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. The numbers in parentheses refer to references at the end of this standard.
Volatile Organic Compounds (1,2,3) 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 microextraction (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.
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. For specific hazard statements, see Section .
General Information
Relations
Buy Standard
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: D6520 − 06
StandardPractice 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 D1193 Specification for Reagent Water
D3370 Practices for Sampling Water from Closed Conduits
1.1 This practice covers procedures for the extraction of
D3694 Practices for Preparation of Sample Containers and
volatile and semi-volatile organic compounds from water and
for Preservation of Organic Constituents
its headspace using solid-phase microextraction (SPME).
D3856 Guide for Management Systems in Laboratories
1.2 The compounds of interest must have a greater affinity
Engaged in Analysis of Water
for the SPME-absorbent polymer or adsorbent or combinations
D4210 Practice for Intralaboratory Quality Control Proce-
of these than the water or headspace phase in which they
dures and a Discussion on Reporting Low-Level Data
reside. 3
(Withdrawn 2002)
D4448 Guide for Sampling Ground-Water MonitoringWells
1.3 Not all of the analytes that can be determined by SPME
are addressed in this practice. The applicability of the absor-
3. Terminology
bent polymer, adsorbent, or combination thereof, to extract the
compound(s) of interest must be demonstrated before use.
3.1 Definitions—For definitions of terms used in this
practice, refer to Terminology D1129.
1.4 This practice provides sample extracts suitable for
quantitative or qualitative analysis by gas chromatography
4. Summary of Practice
(GC) or gas chromatography-mass spectrometry (GC-MS).
4.1 This practice employs adsorbent/liquid or adsorbent/gas
1.5 Whereused,itistheresponsibilityoftheusertovalidate
extractiontoisolatecompoundsofinterest.Anaqueoussample
the application of SPME to the analysis of interest.
is added to a septum-sealed vial. The aqueous phase or its
1.6 The values stated in SI units are to be regarded as the
headspace is then exposed to an adsorbent coated on a fused
standard.
silica fiber.The fiber is desorbed in the heated injection port of
a GC or GC-MS or the injector of an HPLC.
1.7 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4.2 The desorbed organic analytes may be analyzed using
responsibility of the user of this standard to establish appro-
instrumental methods for specific volatile or semi-volatile
priate safety and health practices and determine the applica-
organic compounds. This practice does not include sample
bility of regulatory limitations prior to use. For specific hazard
extract clean-up procedures.
statements, see Section 10.
5. Significance and Use
2. Referenced Documents
5.1 This practice provides a general procedure for the
2
2.1 ASTM Standards:
solid-phase microextraction of volatile and semi-volatile or-
D1129 Terminology Relating to Water
ganic 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 quantify-
1
This practice is under the jurisdiction ofASTM Committee D19 on Water and
ing or screening for extractable organic compounds.
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
5.2 Typical detection limits that can be achieved using
CurrenteditionapprovedJuly1,2006.PublishedJuly2006.Originallyapproved
SPME techniques with gas chromatography with flame ioniza-
in 2000. Last previous edition approved in 2000 as D6520 – 00. DOI: 10.1520/
tion detector (FID), electron capture detector (ECD), or with a
D6520-06.
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 last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
D6520 − 06
mass spectrometer (MS) range from mg/L to µg/L. The required when the analysis requires levels of µg/L or below.
detection limit, linear concentration range, and sensitivity of Once the glassware has been cleaned, it should be used
the test method for a specific organic compound will depend immediately or stored wrapped in aluminum foil (shiny side
upon the aqueous matrix, the fiber
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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.
An American National Standard Designation: D 6520 – 06
Designation:D6520–00
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 D 6520; 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 (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.
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 and health practices and determine the applicability of regulatory
limitations prior to use. For specific hazard statements, see Section 910.
2. Referenced Documents
2
2.1 ASTM Standards:
D 1129 Terminology Relating to Water
D 1193 Specification for Reagent Water
D 3370 Practices for Sampling Water from Closed Conduits
D 3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
3
D 3856 Practice for Evaluating Laboratories Engaged in Sampling and Analysis of Water and Wastewater Guide for Good
Laboratory Practices in Laboratories Engaged in Sampling and Analysis of Water
D 4210 Practice for Intralaboratory Quality Control Procedures and a Discussion on Reporting Low-Level Data
D 4448 Guide for Sampling Groundw-Water Monitoring Wells
3. Summary of Practice
3.1This 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.
3.2The 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. Terminology
3.1 Definitions—For definitions of terms used in this practice, refer to Terminology D 1129.
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.
1
This practice is under the jurisdiction of ASTM Committee D-19 D19 on Water and is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water.
Current edition approved Jan. 10, 2000. Published May 2000.
Current edition approved July 1, 2006. Published July 2006. Originally approved in 2000. Last previous edition approved in 2000 as D 6520 – 00.
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
, Vol 11.01.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 ----------------------
D6520–06
The fiber is desorbed in the heated injection port of a GC or GC-MS or the injector of an HPLC.
4.2 The desorbed organic analytes may be analyzed using instrumental methods for specific volatile or semi-volatile organic
compounds. This pract
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.