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ASTM D5241-92(2011)

(Practice)

Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water

Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water

SIGNIFICANCE AND USE
This practice provides a general procedure for the solvent extraction of volatile and semi-volatile organic compounds from a water matrix. Solvent extraction is used as the initial step in the solvent extraction of organic constituents for the purpose of quantifying extractable organic compounds.
Typical detection limits that can be achieved using micro-extraction techniques with gas chromatography (GC) with flame ionization detector (FID), electron capture detector (ECD), or with a mass spectrometer (GC/MS) range from milligrams per litre (mg/L) to nanograms per litre (ng/L). The detection limit, linear concentration range, and sensitivity of the test method for a specific organic compound will depend upon the sample clean-up, injection volume, solvent to sample ratio, solvent concentration methods used, and the determinative technique employed.
Micro-extraction has the advantage of speed, simple extraction devices, and the use of small amounts of sample and solvents.
Selectivity can be improved by the choice of solvent (usually hexane or pentane) or mixed solvents, extraction time and temperature, and ionic strength of the solution.
Extraction devices can vary from the sample container itself to commercial devices specifically designed for micro-extraction. See 7.1 and 7.2.
SCOPE
1.1 This practice covers standard procedures for extraction of volatile and semi-volatile organic compounds from water using small volumes of solvents.
1.2 The compounds of interest must have a greater solubility in the organic solvent than the water phase.
1.3 Not all of the solvents that can be used in micro extraction are addressed in this practice. The applicability of a solvent to extract the compound(s) of interest must be demonstrated before use.
1.4 This practice provides sample extracts suitable for any technique amenable to solvent injection such as gas chromatography or high performance liquid chromatography (HPLC).
1.5 The values stated in SI units are to be regarded as the standard.
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 9.

General Information

Status
Historical
Publication Date
30-Apr-2011
ICS
13.060.45 - Examination of water in general
Technical Committee
D19 - Water
Drafting Committee
D19.06 - Methods for Analysis for Organic Substances in Water
Current Stage
Ref Project

Relations

Replaces
ASTM D5241-92(2004) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water
Effective Date
01-May-2011
Replaced By
ASTM D5241-92(2017) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water
Effective Date
15-Dec-2017
Referred By
ASTM E3373-23 - Standard Test Method for Scour of Hydrodynamic Separators and Settling Devices
Effective Date
01-May-2011

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ASTM D5241-92(2011) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in WaterASTM D5241-92(2011) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water
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ASTM D5241-92(2011) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water
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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: D5241 − 92 (Reapproved 2011)
Standard Practice for
Micro-Extraction of Water for Analysis of Volatile and Semi-
1
Volatile Organic Compounds in Water
This standard is issued under the fixed designation D5241; 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 D3694 Practices for Preparation of Sample Containers and
for Preservation of Organic Constituents
1.1 This practice covers standard procedures for extraction
D3856 Guide for Management Systems in Laboratories
of volatile and semi-volatile organic compounds from water
Engaged in Analysis of Water
using small volumes of solvents.
D3973 TestMethodforLow-MolecularWeightHalogenated
1.2 The compounds of interest must have a greater solubil-
Hydrocarbons in Water
ity in the organic solvent than the water phase.
D4210 Practice for Intralaboratory Quality Control Proce-
dures and a Discussion on Reporting Low-Level Data
1.3 Not all of the solvents that can be used in micro
3
extraction are addressed in this practice. The applicability of a (Withdrawn 2002)
D4448 Guide for Sampling Ground-Water MonitoringWells
solvent to extract the compound(s) of interest must be demon-
strated before use. D5175 Test Method for Organohalide Pesticides and Poly-
chlorinated Biphenyls in Water by Microextraction and
1.4 This practice provides sample extracts suitable for any
Gas Chromatography
technique amenable to solvent injection such as gas chroma-
tography or high performance liquid chromatography (HPLC).
3. Summary of Practice
1.5 The values stated in SI units are to be regarded as the
3.1 This practice employs liquid/liquid extraction to isolate
standard.
compounds of interest. The sample is added to an extraction
1.6 The values stated in SI units are to be regarded as device.Thesolventmaybeaddedtothesamplecontaineroran
extraction device and extracted for a period of 5 min. The
standard. No other units of measurement are included in this
standard. solvent is then ready for analysis. If required, the pH may be
adjusted and salt may be added prior to extraction to increase
1.7 This standard does not purport to address all of the
the extraction specificity and efficiency.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.2 The solvent extract may be further processed using
priate safety and health practices and determine the applica- sample clean-up and concentration techniques. The analytes in
bility of regulatory limitations prior to use. For specific hazard
the solvent may be analyzed using instrumental methods for
statements, see Section 9. specific volatile or semivolatile organic compounds. This
practice does not include sample extract clean-up methods.
2. Referenced Documents
4. Significance and Use
2
2.1 ASTM Standards:
4.1 This practice provides a general procedure for the
D1129 Terminology Relating to Water
solvent extraction of volatile and semi-volatile organic com-
D1193 Specification for Reagent Water
pounds from a water matrix. Solvent extraction is used as the
D3370 Practices for Sampling Water from Closed Conduits
initial step in the solvent extraction of organic constituents for
the purpose of quantifying extractable organic compounds.
1
4.2 Typical detection limits that can be achieved using
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
micro-extraction techniques with gas chromatography (GC)
Organic Substances in Water.
with flame ionization detector (FID), electron capture detector
Current edition approved May 1, 2011. Published June 2011. Originally
(ECD), or with a mass spectrometer (GC/MS) range from
approved in 1992. Last previous edition approved in 2004 as D5241 – 92 (2004).
DOI: 10.1520/D5241-92R11. milligrams per litre (mg/L) to nanograms per litre (ng/L). The
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 ----------------------
D5241 − 92 (2011)
detection limit, linear concentration range, and sensitivity of 5.1.3 Afield blank prepared from water and carried through
the test method for a specific organic compound wi
...

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SCOPE
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5.1 In order to be certain that the end user of analytical results obtained from using an ASTM Committee D19 test method can be confident that the values have been obtained through a competent application of the test method, a demonstration of the proficiency of the analytical system shall be performed. Appropriate proficiency is demonstrated by achievement of performance criteria derived from results of the test method collaborative study. The QC measures specified in this practice shall be included in each ASTM test method, as applicable, to ensure the quality of measurements.  
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SCOPE
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SCOPE
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SCOPE
1.1 This practice establishes a standard for computing the measurement uncertainty for applicable test methods in Committee D19 on Water. The practice does not provide a single-point estimate for the entire working range, but rather relates the uncertainty to concentration. The statistical technique of regression is employed during data analysis.  
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1.3 Calculation of the measurement uncertainty involves the analysis of data collected to help characterize the analytical method over an appropriate concentration range. Example sources of data include: (1) calibration studies (which may or may not be conducted in pure solvent), (2) recovery studies (which typically are conducted in matrix and include all sample-preparation steps), and (3) collections of data obtained as part of the method’s ongoing Quality Control program. Use of multiple instruments, multiple operators, or both, and field-sampling protocols may or may not be reflected in the data.  
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1.7 It is assumed that the user has access to a statistical software package for performing regression. A statistician should be consulted if assistance is needed in selecting such a program.  
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Standard Practice for Development and Use (Preparation) of Samples for Collaborative Testing of Methods for Analysis of Sediments

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5.1 The objective of this practice is to provide guidelines for the preparation of samples for use in collaborative tests, to evaluate methods during their development, and for the evaluation of the precision and bias of proposed test methods.  
5.2 Statements of the precision and bias are a mandatory part of ASTM test methods. Such an evaluation is necessary to provide guidance to the user as to the reliability of measurements that can be expected by its use. The statements are developed on the basis of user experience (ordinarily collaborative tests) with the test method.  
5.3 The availability of test samples is a key requirement for collaborative evaluation of test methods.
SCOPE
1.1 This practice establishes uniform general procedures for the development (preparation) and use of samples in the collaborative testing of methods for chemical analysis of sediments and similar materials.  
1.2 The principles of this practice are applicable to aqueous samples with suitable technical modifications.  
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Standard Practice for Certificates of Reference Materials for Water Analysis

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4.1 This practice is designed to assist suppliers and users of reference materials by identifying the information necessary on the certificate of analysis of materials designated for use in ASTM test methods. This practice is specifically designed to ensure that materials suitable for use as either calibration or quality control standards are available. This practice does not define a specific certification protocol, but rather provides guidance in the development of adequate data to support the use of the material as either a calibration or quality control standard. Suppliers are referred to ISO Guide 35 for guidelines on acceptable certification protocols. End users are referred to ISO Guide 31 for a more complete description of the elements of typical certificates of analysis.
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Note 1: A certified reference material traceable to SI units is a certified reference material whose value can be related with a stated uncertainty through an unbroken change of comparisons to stated references (usually national or international standards) in SI units, such as a primary measurement made in SI units or a national standard certified in SI units.
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SIGNIFICANCE AND USE
4.1 The proper use of analytical data requires adequate documentation of all inputs, that is, the source and history of the sample, laboratory performing the analysis, method of analysis, date of analysis, precision and bias of the measurements, and related quality assurance information.  
4.2 In order to have defensible data, the report must be complete and accurate, providing adequate information to evaluate the quality of the data and contain supporting information that documents sampling and analysis procedures.  
4.3 This guide contains some of the common data qualifiers or “flags” commonly used by laboratories following the good laboratory practices, the government contract program, or found in the commercial laboratories. Examples of these qualifiers are the use of (E) for estimated value, (U) for analyzed for but not detected, and (B) for analyte was found in the blank (see 8.11). The qualifiers included in this guide should help the laboratory and its customers to better understand each other by using standardized qualifiers.  
4.4 Practice D933 is a comprehensive practice for reporting water-formed constituents such as metal oxides, acid anhydrides, and others.
SCOPE
1.1 This guide provides guidelines for reporting inorganic and organic results of analyses of drinking water, waste water, process water, ground water, and surface water, and so forth, to laboratory clients in a complete and systematic fashion.  
1.2 The reporting of bacterial and radiological data are not addressed in this guide.  
1.3 The commonly used data qualifiers for reviewing and reporting information are listed and defined. Client and laboratory specific requirements may make use of other qualifiers. This guide does not preclude the use of other data qualifiers.  
1.4 This guide discusses procedures for and specific problems in the reporting of low level data, potential errors (Type I and Type II), and reporting data that are below the calculated method detection limit and above the analyte.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 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.

  • Guide
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