ASTM D5810-96(2015)
(Guide)Standard Guide for Spiking into Aqueous Samples
Standard Guide for Spiking into Aqueous Samples 
SIGNIFICANCE AND USE
5.1 Matrix spiking is commonly used to determine the bias under specific analytical conditions, or the applicability of a test method to a particular sample matrix in that context, by determining the extent to which the spiked analyte or component 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 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 or recovery limits from the same or similar matrices over time may indicate variations in the quality of analytical results.
5.3 Spiking can be used to compare the recoveries of like spikes from reagent water samples and natural matrix samples (measured with and without spike) to distinguish between (1) unusual interference and (2) inherent method recovery and instability effects. This guide does not attempt to deal with the statistical significance of differences in spike recoveries from different matrices.
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. Duplicate field spikes can be used to document the reproducibility of the technique. When environmentally labile compounds are used as spikes, the spiking solution shall be protected up to the point of use by appropriate means such as chilling, protection from sunlight and o...
SCOPE
1.1 This guide covers the general technique of “spiking” a broad range of materials into aqueous media. This guide will serve the analyst in preparing spiked samples for quality control purposes. 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 procedures and materials described here are appropriate to the task at hand.
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, and interpretation of results. 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 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...
General Information
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: D5810 − 96 (Reapproved 2015)
Standard Guide for
1
Spiking into Aqueous Samples
This standard is issued under the fixed designation D5810; 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 a homogeneous solution of analyte and sample. Meaningful
recovery data cannot be obtained if an aqueous solution or
1.1 This guide covers the general technique of “spiking” a
homogenoussuspensionoftheanalyteofinterestinthesample
broad range of materials into aqueous media. This guide will
cannot be attained. These procedures may be applicable to
serve the analyst in preparing spiked samples for quality
microbiologicalpreparationsifthehomogeneityofthesuspen-
control purposes. Guidance is also provided to aid the analyst
sioncanbeadequatelymaintainedthroughoutthecourseofthe
in calculating recoveries and interpreting results. It is the
analysis, for example, by mechanical agitation or stirring.
responsibility of the analyst to determine whether the proce-
dures and materials described here are appropriate to the task 1.5 Matrix spiking may be performed in the field or in the
at hand. laboratory,dependingonwhichpartoftheanalyticalprocessis
to be tested. Field spiking tests the recovery of the overall
1.2 The procedures in this guide are focused on “matrix
process, including preservation and shipping of the sample.
spike” preparation, analysis, and interpretation of results. The
Laboratoryspikingteststhelaboratoryprocessonly.Spikingof
applicability of these procedures to the preparation of calibra-
sample extracts, concentrates, or dilutions will test only that
tion standards, calibration check standards, laboratory control
portion of the process subsequent to addition of the spike.
standards, reference materials, and other quality control mate-
rials by spiking is incidental.Asample (the matrix) is fortified 1.6 The values stated in SI units are to be regarded as
(spiked) with the analyte of interest for a variety of analytical standard. No other units of measurement are included in this
and quality control purposes. While the spiking of multiple standard.
sample portions is discussed, the method of standard additions
1.7 This standard does not purport to address all of the
is not covered.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
1.3 This guide is intended for use in conjunction with the
priate safety and health practices and determine the applica-
individual analytical test method that provides procedures for
bility of regulatory limitations prior to use.
analysis of the analyte or component of interest. The test
method is used to determine an analyte or component’s
2. Referenced Documents
background level and, again after spiking, its now elevated
2
2.1 ASTM Standards:
level. Each test method typically provides procedures not only
D1129Terminology Relating to Water
for samples, but also for calibration standards or analytical
D1193Specification for Reagent Water
control solutions, or both. These procedures include
D3694Practices for Preparation of Sample Containers and
preparation, handling, storage, preservation, and analysis tech-
for Preservation of Organic Constituents
niques.Theseproceduresareapplicablebyextension,usingthe
D3856Guide for Management Systems in Laboratories
analyst’s judgement on a case-by-case basis, to spiking
Engaged in Analysis of Water
solutions, and are not reiterated in this guide. See also Practice
D4375Practice for Basic Statistics in Committee D19 on
E200 for preparation and storage information.
Water
1.4 Theseproceduresapplyonlytoanalytesthataresoluble
E200Practice for Preparation, Standardization, and Storage
in water at the concentration of the spike plus any background
of Standard and Reagent Solutions for ChemicalAnalysis
material, or to analytes soluble in a solvent that is itself
water-soluble. The system used in the later case must result in
3. Terminology
3.1 Definitions—For definitions of terms used in this guide,
refer to Terminology D1129.
1
This guide is under the jurisdiction ofASTM Committee D19 on Water and is
thedirectresponsibilityofSubcommitteeD19.02onQualitySystems,Specification,
2
and Statistics. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 15, 2015. Published December 2015. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1996. Last previous edition approved in 2011 as D5810–96 (2011). Standards volume information, refer to the standard’s Document Summary page on
DOI:
...
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: D5810 − 96 (Reapproved 2011) D5810 − 96 (Reapproved 2015)
Standard Guide for
1
Spiking into Aqueous Samples
This standard is issued under the fixed designation D5810; 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” a broad range of materials into aqueous media. This guide will serve
the analyst in preparing spiked samples for quality control purposes. 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 procedures and materials
described here are appropriate to the task at hand.
1.2 The procedures in this guide are focused on “matrix spike” preparation, analysis, and interpretation of results. 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
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 homogenous
suspension of the analyte of interest in the sample cannot be attained. These procedures may be applicable to microbiological
preparations if the homogeneity of the suspension can be adequately maintained throughout the course of the analysis, for example,
by mechanical agitation or stirring.
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 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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
D1129 Terminology Relating to Water
D1193 Specification for Reagent Water
D3694 Practices for Preparation of Sample Containers and for Preservation of Organic Constituents
1
This guide is under the jurisdiction of ASTM Committee D19 on Water and is the direct responsibility of Subcommittee D19.02 on Quality Systems, Specification, and
Statistics.
Current edition approved May 1, 2011Dec. 15, 2015. Published June 2011December 2015. Originally approved in 1996. Last previous edition approved in 20062011 as
D5810 – 96 (2006).(2011). DOI: 10.1520/D5810-96R11.10.1520/D5810-96R15.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.