ASTM D5788-95(2017)
(Guide)Standard Guide for Spiking Organics into Aqueous Samples
Standard Guide for Spiking Organics into Aqueous Samples
SIGNIFICANCE AND USE
5.1 Matrix spiking of samples is commonly used to determine the bias under specific analytical conditions, or the applicability of a test method to a particular sample matrix, by determining the extent to which the added spike is recovered from the sample matrix under these conditions. Reactions or interactions of the analyte or component of interest with the sample matrix may cause a significant positive or negative effect on recovery and may render the chosen analytical, or monitoring, process ineffectual for that sample matrix.
5.2 Matrix spiking of samples can also be used to monitor the performance of a laboratory, individual instrument, or analyst as part of a regular quality assurance program. Changes in spike recoveries from the same or similar matrices over time may indicate variations in the quality of analyses and analytical results.
5.3 Spiking of samples may be performed in the field or in the laboratory, depending on what part of the analytical process is to be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample and may be considered a measure of the stability of the analytes in the matrix. Laboratory spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will be reflective of only that portion of the process subsequent to the addition of the spike.
5.4 Special precautions shall be observed when nonlaboratory personnel perform spiking in the field. It is recommended that all spike preparation work be performed in a laboratory by experienced analysts so that the field operation consists solely of adding a prepared spiking solution to the sample matrix. Training of field personnel and validation of their spiking techniques are necessary to ensure that spikes are added accurately and reproducibly. Consistent and acceptable recoveries from duplicate field spikes can be used to document the reproducibility of sampling and the spiking technique....
SCOPE
1.1 This guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials cited here are compatible with the analytes of interest.
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified (spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample test portions is discussed, the method of standard additions is not covered.
1.3 This guide is intended for use in conjunction with the individual analytical test method that provides procedures for analysis of the analyte or component of interest. The test method is used to determine an analyte or component's background level and, again after spiking, its now elevated level. Each test method typically provides procedures not only for samples, but also for calibration standards or analytical control solutions, or both. These procedures include preparation, handling, storage, preservation, and analysis techniques. These procedures are applicable by extension, using the analyst's judgement on a case-by-case basis, to spiking solutions, ...
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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: D5788 − 95 (Reapproved 2017)
Standard Guide for
1
Spiking Organics into Aqueous Samples
This standard is issued under the fixed designation D5788; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 1.4 Theseproceduresapplyonlytoanalytesthataresoluble
in water at the concentration of the spike plus any background
1.1 This guide covers the general technique of “spiking”
material, or to analytes soluble in a solvent that is itself
aqueous samples with organic analytes or components. It is
water-soluble. The system used in the later case must result in
intended to be applicable to a broad range of organic materials
a homogeneous solution of analyte and sample. Meaningful
in aqueous media. Although the specific details and handling
recovery data cannot be obtained if an aqueous solution or
procedures required for all types of compounds are not
homogeneous suspension of the analyte of interest in the
described,thisgeneralapproachisgiventoserveasaguideline
sample cannot be attained.
to the analyst in accurately preparing spiked samples for
subsequent analysis or comparison. Guidance is also provided 1.5 Matrix spiking may be performed in the field or in the
to aid the analyst in calculating recoveries and interpreting laboratory,dependingonwhichpartoftheanalyticalprocessis
results. It is the responsibility of the analyst to determine to be tested. Field spiking tests the recovery of the overall
whether the methods and materials cited here are compatible process, including preservation and shipping of the sample.
with the analytes of interest. Laboratoryspikingteststhelaboratoryprocessonly.Spikingof
sample extracts, concentrates, or dilutions will test only that
1.2 The procedures in this guide are focused on “matrix
portion of the process subsequent to the addition of the spike.
spike” preparation, analysis, results, and interpretation. The
applicability of these procedures to the preparation of calibra- 1.6 The values stated in SI units are to be regarded as
tion standards, calibration check standards, laboratory control standard. No other units of measurement are included in this
standards, reference materials, and other quality control mate- standard.
rials by spiking is incidental.Asample (the matrix) is fortified
1.7 This standard does not purport to address all of the
(spiked) with the analyte of interest for a variety of analytical
safety concerns, if any, associated with its use. It is the
and quality control purposes. While the spiking of multiple
responsibility of the user of this standard to establish appro-
sample test portions is discussed, the method of standard
priate safety, health, and environmental practices and deter-
additions is not covered.
mine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accor-
1.3 This guide is intended for use in conjunction with the
dance with internationally recognized principles on standard-
individual analytical test method that provides procedures for
ization established in the Decision on Principles for the
analysis of the analyte or component of interest. The test
Development of International Standards, Guides and Recom-
method is used to determine an analyte or component’s
mendations issued by the World Trade Organization Technical
background level and, again after spiking, its now elevated
Barriers to Trade (TBT) Committee.
level. Each test method typically provides procedures not only
for samples, but also for calibration standards or analytical
2. Referenced Documents
control solutions, or both. These procedures include
2
preparation, handling, storage, preservation, and analysis tech-
2.1 ASTM Standards:
niques.Theseproceduresareapplicablebyextension,usingthe
D1129Terminology Relating to Water
analyst’s judgement on a case-by-case basis, to spiking
D1193Specification for Reagent Water
solutions, and are not reiterated in this guide. See also Practice
D3694Practices for Preparation of Sample Containers and
E200 for preparation and storage information.
for Preservation of Organic Constituents
D3856Guide for Management Systems in Laboratories
Engaged in Analysis of Water
1
This guide 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
Curre
...
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: D5788 − 95 (Reapproved 2017)
Standard Guide for
1
Spiking Organics into Aqueous Samples
This standard is issued under the fixed designation D5788; 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 1.4 These procedures apply only to analytes that are soluble
in water at the concentration of the spike plus any background
1.1 This guide covers the general technique of “spiking”
material, or to analytes soluble in a solvent that is itself
aqueous samples with organic analytes or components. It is
water-soluble. The system used in the later case must result in
intended to be applicable to a broad range of organic materials
a homogeneous solution of analyte and sample. Meaningful
in aqueous media. Although the specific details and handling
recovery data cannot be obtained if an aqueous solution or
procedures required for all types of compounds are not
homogeneous suspension of the analyte of interest in the
described, this general approach is given to serve as a guideline
sample cannot be attained.
to the analyst in accurately preparing spiked samples for
subsequent analysis or comparison. Guidance is also provided 1.5 Matrix spiking may be performed in the field or in the
to aid the analyst in calculating recoveries and interpreting laboratory, depending on which part of the analytical process is
results. It is the responsibility of the analyst to determine to be tested. Field spiking tests the recovery of the overall
whether the methods and materials cited here are compatible process, including preservation and shipping of the sample.
with the analytes of interest. Laboratory spiking tests the laboratory process only. Spiking of
sample extracts, concentrates, or dilutions will test only that
1.2 The procedures in this guide are focused on “matrix
portion of the process subsequent to the addition of the spike.
spike” preparation, analysis, results, and interpretation. The
applicability of these procedures to the preparation of calibra- 1.6 The values stated in SI units are to be regarded as
tion standards, calibration check standards, laboratory control standard. No other units of measurement are included in this
standards, reference materials, and other quality control mate- standard.
rials by spiking is incidental. A sample (the matrix) is fortified
1.7 This standard does not purport to address all of the
(spiked) with the analyte of interest for a variety of analytical
safety concerns, if any, associated with its use. It is the
and quality control purposes. While the spiking of multiple
responsibility of the user of this standard to establish appro-
sample test portions is discussed, the method of standard
priate safety, health, and environmental practices and deter-
additions is not covered.
mine the applicability of regulatory limitations prior to use.
1.8 This international standard was developed in accor-
1.3 This guide is intended for use in conjunction with the
dance with internationally recognized principles on standard-
individual analytical test method that provides procedures for
ization established in the Decision on Principles for the
analysis of the analyte or component of interest. The test
Development of International Standards, Guides and Recom-
method is used to determine an analyte or component’s
mendations issued by the World Trade Organization Technical
background level and, again after spiking, its now elevated
Barriers to Trade (TBT) Committee.
level. Each test method typically provides procedures not only
for samples, but also for calibration standards or analytical
2. Referenced Documents
control solutions, or both. These procedures include
2
preparation, handling, storage, preservation, and analysis tech-
2.1 ASTM Standards:
niques. These procedures are applicable by extension, using the
D1129 Terminology Relating to Water
analyst’s judgement on a case-by-case basis, to spiking
D1193 Specification for Reagent Water
solutions, and are not reiterated in this guide. See also Practice
D3694 Practices for Preparation of Sample Containers and
E200 for preparation and storage information.
for Preservation of Organic Constituents
D3856 Guide for Management Systems in Laboratories
Engaged in Analysis of Water
1
This guide is under the jurisdiction of ASTM 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, 2017. Published January 2018. Originally contact ASTM Customer Service
...
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: D5788 − 95 (Reapproved 2011) D5788 − 95 (Reapproved 2017)
Standard Guide for
1
Spiking Organics into Aqueous Samples
This standard is issued under the fixed designation D5788; 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 guide covers the general technique of “spiking” aqueous samples with organic analytes or components. It is intended
to be applicable to a broad range of organic materials in aqueous media. Although the specific details and handling procedures
required for all types of compounds are not described, this general approach is given to serve as a guideline to the analyst in
accurately preparing spiked samples for subsequent analysis or comparison. Guidance is also provided to aid the analyst in
calculating recoveries and interpreting results. It is the responsibility of the analyst to determine whether the methods and materials
cited here are compatible with the analytes of interest.
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, results, and interpretation. The
applicability of these procedures to the preparation of calibration standards, calibration check standards, laboratory control
standards, reference materials, and other quality control materials by spiking is incidental. A sample (the matrix) is fortified
(spiked) with the analyte of interest for a variety of analytical and quality control purposes. While the spiking of multiple sample
test portions is discussed, the method of standard additions is not covered.
1.3 This guide is intended for use in conjunction with the individual analytical test method that provides procedures for analysis
of the analyte or component of interest. The test method is used to determine an analyte or component’s background level and,
again after spiking, its now elevated level. Each test method typically provides procedures not only for samples, but also for
calibration standards or analytical control solutions, or both. These procedures include preparation, handling, storage, preservation,
and analysis techniques. These procedures are applicable by extension, using the analyst’s judgement on a case-by-case basis, to
spiking solutions, and are not reiterated in this guide. See also Practice E200 for preparation and storage information.
1.4 These procedures apply only to analytes that are soluble in water at the concentration of the spike plus any background
material, or to analytes soluble in a solvent that is itself water-soluble. The system used in the later case must result in a
homogeneous solution of analyte and sample. Meaningful recovery data cannot be obtained if an aqueous solution or homogeneous
suspension of the analyte of interest in the sample cannot be attained.
1.5 Matrix spiking may be performed in the field or in the laboratory, depending on which part of the analytical process is to
be tested. Field spiking tests the recovery of the overall process, including preservation and shipping of the sample. Laboratory
spiking tests the laboratory process only. Spiking of sample extracts, concentrates, or dilutions will test only that portion of the
process subsequent to the addition of the spike.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use.
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
1
This guide 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 May 1, 2011Dec. 15, 2017. Published June 2011January 2018. Originall
...
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