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ASTM D5241-92(2024)

(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
4.1 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.  
4.2 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.  
4.3 Micro-extraction has the advantage of speed, simple extraction devices, and the use of small amounts of sample and solvents.  
4.3.1 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.  
4.3.2 Extraction devices can vary from the sample container itself to commercial devices specifically designed for micro-extraction. See 7.1 and 7.2.  
4.3.3 A list of chlorinated organic compounds that can be determined by this practice includes both high and low boiling compounds or chemicals (see Table 1). (A) Based on the injection of chlorinated compounds in pentane solution, taking into consideration the 100:1 concentration of a water sample by the microextraction technique.
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 standard. No other units of measurement are included in this 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. For specific hazard statements, see Section 9.  
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-Mar-2024
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(2017) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in Water
Effective Date
01-Apr-2024
Refers
ASTM D5175-91(2024) - Standard Test Method for Organohalide Pesticides and Polychlorinated Biphenyls in Water by Microextraction and Gas Chromatography
Effective Date
01-Apr-2024
Refers
ASTM D5175-91(2017)e1 - Standard Test Method for Organohalide Pesticides and Polychlorinated Biphenyls in Water by Microextraction and Gas Chromatography
Effective Date
15-Dec-2017
Referred By
ASTM E3373-24 - Standard Test Method for Scour of Hydrodynamic Separators and Settling Devices
Effective Date
01-Apr-2024

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ASTM D5241-92(2024) - Standard Practice for Micro-Extraction of Water for Analysis of Volatile and Semi-Volatile Organic Compounds in WaterASTM D5241-92(2024) - 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(2024) - 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)

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: D5241 − 92 (Reapproved 2024)
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 D1193 Specification for Reagent Water
D3370 Practices for Sampling Water from Flowing Process
1.1 This practice covers standard procedures for extraction
Streams
of volatile and semi-volatile organic compounds from water
D3694 Practices for Preparation of Sample Containers and
using small volumes of solvents.
for Preservation of Organic Constituents
1.2 The compounds of interest must have a greater solubil-
D3856 Guide for Management Systems in Laboratories
ity in the organic solvent than the water phase. 3
Engaged in Analysis of Water (Withdrawn 2024)
D3973 Test Method for Low-Molecular Weight Halogenated
1.3 Not all of the solvents that can be used in micro
extraction are addressed in this practice. The applicability of a Hydrocarbons in Water
D4210 Practice for Intralaboratory Quality Control Proce-
solvent to extract the compound(s) of interest must be demon-
strated before use. dures and a Discussion on Reporting Low-Level Data
3
(Withdrawn 2002)
1.4 This practice provides sample extracts suitable for any
D4448 Guide for Sampling Ground-Water Monitoring Wells
technique amenable to solvent injection such as gas chroma-
D5175 Test Method for Organohalide Pesticides and Poly-
tography or high performance liquid chromatography (HPLC).
chlorinated Biphenyls in Water by Microextraction and
1.5 The values stated in SI units are to be regarded as
Gas Chromatography
standard. No other units of measurement are included in this
standard. 3. Summary of Practice
1.6 This standard does not purport to address all of the 3.1 This practice employs liquid/liquid extraction to isolate
safety concerns, if any, associated with its use. It is the
compounds of interest. The sample is added to an extraction
responsibility of the user of this standard to establish appro- device. The solvent may be added to the sample container or an
priate safety, health, and environmental practices and deter- extraction device and extracted for a period of 5 min. The
mine the applicability of regulatory limitations prior to use.
solvent is then ready for analysis. If required, the pH may be
For specific hazard statements, see Section 9. adjusted and salt may be added prior to extraction to increase
1.7 This international standard was developed in accor-
the extraction specificity and efficiency.
dance with internationally recognized principles on standard-
3.2 The solvent extract may be further processed using
ization established in the Decision on Principles for the
sample clean-up and concentration techniques. The analytes in
Development of International Standards, Guides and Recom-
the solvent may be analyzed using instrumental methods for
mendations issued by the World Trade Organization Technical
specific volatile or semivolatile organic compounds. This
Barriers to Trade (TBT) Committee.
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-
pounds from a water matrix. Solvent extraction is used as the
1
This practice is under the jurisdiction of ASTM Committee D19 on Water and
initial step in the solvent extraction of organic constituents for
is the direct responsibility of Subcommittee D19.06 on Methods for Analysis for
Organic Substances in Water. the purpose of quantifying extractable organic compounds.
Current edition approved April 1, 2024. Published April 2024. Originally
4.2 Typical detection limits that can be achieved using
approved in 1992. Last previous edition approved in 2017 as D5241 – 92 (2017).
DOI: 10.1520/D5241-92R24. micro-extraction techniques with gas chromatography (GC)
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 C70
...

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1.1 This practice provides specific, mandatory requirements for incorporating quality control (QC) procedures into all test methods under the jurisdiction of Committee D19.  
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Policy on implementation of requirements for a quality control section in standard test methods generated by Committee D19 on Water.  
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NEW COLLABORATIVE TESTING—As of July 29, 1998, each collaborative study design shall include a QC section as part of the method to be tested. Prior to approval of the study design, the Results Advisor or equivalent shall ascertain the appropriateness of the QC section in meeting the requirements of this practice and Practice D2777, and shall advise the designer of the study of any changes needed to fulfill the requirements of these practices. Before a collaborative study may be conducted, approval of the study design by the Results Advisor or equivalent shall be obtained.  
OLDER VALIDATED METHODS—Standard test methods that were validated using Practices D2777 – 77, D2777 – 86, or D2777 – 94, when balloted for reapproval or revision, shall contain a QC section based upon the best information from the historical record. Where appropriate, information derived from the record of the collaborative study shall be utilized for this purpose. The introduction of the QC section into these standard test methods shall not be construed as a requirement for a new collaborative study, though the Subcommittee may opt for such a study. Any information available regarding QC or precision/bias testing shall be included in the appropriate sections of the published test method.  
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5.1 The transport of any suspended solids or corrosion products from the preboiler cycle has been shown to be detrimental to all types of steam generating equipment. Corrosion product transport as low as 10 ppb can have significant impact on steam generators performance.  
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SCOPE
1.1 This practice is applicable for sampling condensed steam or water, such as boiler feedwater, for the collection of suspended solids and (optional) ionic solids using a 0.45-μm membrane filter (suspended solids) and ion exchange media (ionic solids). As the major suspended component found in most boiler feedwaters is some form of corrosion product from the preboiler system, the device used for this practice is commonly called a corrosion product sampler.  
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5.1 Appropriate application of this practice should result in an estimate of the test-method’s uncertainty (at any concentration within the working range), which can be compared with data-quality objectives to see if the uncertainty is acceptable.  
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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.  
1.2 Applicable test methods are those whose results come from regression-based methods and whose data are intra-laboratory (not inter-laboratory data, such as result from round-robin studies). For each analysis conducted using such a method, it is assumed that a fixed, reproducible amount of sample is introduced.  
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.  
1.4 In any designed study whose data are to be used to calculate method uncertainty, the user should think carefully about what the study is trying to accomplish and much variation should be incorporated into the study. General guidance on designing studies (for example, calibration, recovery) is given in Appendix X1. Detailed guidelines on sources of variation are outside the scope of this practice, but general points to consider are included in Appendix X2, which is not intended to be exhaustive. With any study, the user must think carefully about the factors involved with conducting the analysis, and must realize that the computed measurement uncertainty will reflect the quality of the input data.  
1.5 Associated with the measurement uncertainty is a user-chosen level of statistical confidence.  
1.6 At any concentration in the working range, the measurement uncertainty is plus-or-minus the half-width of the prediction interval associated with the regression line.  
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.  
1.8 A statistician also should be consulted if data transformations are being considered.  
1.9 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.  
1.10 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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ASTM D3975-93(2019)(Practice)
Standard Practice for Development and Use (Preparation) of Samples for Collaborative Testing of Methods for Analysis of Sediments

SIGNIFICANCE AND USE
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.  
1.3 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.  
1.4 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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ASTM D6362-98(2018)(Practice)
Standard Practice for Certificates of Reference Materials for Water Analysis

SIGNIFICANCE AND USE
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.
SCOPE
1.1 This practice covers the information that must be provided on certificates of analysis of reference materials designated to support ASTM methods. It provides end users of these materials with a defined set of data that is required to be on a certificate of analysis and provides information to assist the end user in evaluating the independence of the material. Similarly, it provides the suppliers of reference materials with a consistent format for the presentation of certification data.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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.  
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ASTM D6568-00(2018)(Guide)
Standard Guide for Planning, Carrying Out, and Reporting Traceable Chemical Analyses of Water Samples

SIGNIFICANCE AND USE
4.1 This guide establishes basic requirements which should be met by water and environmental laboratories that generate and report test chemical analyses which the laboratory client desires to be traceable to SI units (Note 1) or certified reference materials traceable to SI units. Traceability of chemical analyses is important because it provides a uniform basis for the comparison of results from different measurement systems and because it relates those results to our current knowledge of physical laws (Note 2).
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.
Note 2: Not all chemical analysis results can be traceable to SI units or to certified reference material’s traceable to SI units, such as turbidity and or total suspended solids.  
4.2 Many waters-related laboratories comply with ISO Guide 17025 and participate in Proficiency Testing Programs. Laboratories that are connected to the same accreditation bodies and Proficiency Test providers can be expected to report statistically similar results on the same sample. However, some test methods and some certified reference materials are not supported with data traceable to SI units. Therefore, fully compliant laboratories that are not connected to the same providers may report statistically different chemical analysis results if they used the same nontraceable test method on the same sample. This problem could be minimized if they used test methods, measurement devices, and certified reference materials that are traceable to SI units, where available.  
4.3 Although some standard test methods and certified reference materials provide evidence of traceability to SI units, many others do not. Therefor...
SCOPE
1.1 This guide sets a protocol for generating and reporting chemical analyses that are traceable to SI units or to certified reference materials in laboratories that serve the water and environmental industry.  
1.2 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.  
1.3 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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ASTM
ASTM D596-01(2018)(Guide)
Standard Guide for Reporting Results of Analysis of Water

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.

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