Standard Guide for Spiking into Aqueous Samples

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 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.

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Publication Date
09-Jun-1996
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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:D 5810–96 (Reapproved 2001)
Standard Guide for
1
Spiking into Aqueous Samples
This standard is issued under the fixed designation D 5810; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope recovery data cannot be obtained if an aqueous solution or
homogenoussuspensionoftheanalyteofinterestinthesample
1.1 This guide covers the general technique of “spiking” a
cannot be attained. These procedures may be applicable to
broad range of materials into aqueous media. This guide will
microbiologicalpreparationsifthehomogeneityofthesuspen-
serve the analyst in preparing spiked samples for quality
sioncanbeadequatelymaintainedthroughoutthecourseofthe
control purposes. Guidance is also provided to aid the analyst
analysis, for example, by mechanical agitation or stirring.
in calculating recoveries and interpreting results. It is the
1.5 Matrix spiking may be performed in the field or in the
responsibility of the analyst to determine whether the proce-
laboratory,dependingonwhichpartoftheanalyticalprocessis
dures and materials described here are appropriate to the task
to be tested. Field spiking tests the recovery of the overall
at hand.
process, including preservation and shipping of the sample.
1.2 The procedures in this guide are focused on “matrix
Laboratoryspikingteststhelaboratoryprocessonly.Spikingof
spike” preparation, analysis, and interpretation of results. The
sample extracts, concentrates, or dilutions will test only that
applicability of these procedures to the preparation of calibra-
portion of the process subsequent to addition of the spike.
tion standards, calibration check standards, laboratory control
1.6 The values stated in SI units are to be regarded as the
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 portions is discussed, the method of standard additions
priate safety and health practices and determine the applica-
is not covered.
bility of regulatory limitations prior to use.
1.3 This guide is intended for use in conjunction with the
individual analytical test method that provides procedures for
2. Referenced Documents
analysis of the analyte or component of interest. The test
2.1 ASTM Standards:
method is used to determine an analyte or component’s
2
D1129 Terminology Relating to Water
background level and, again after spiking, its now elevated
2
D1193 Specification for Reagent Water
level. Each test method typically provides procedures not only
D3694 Practices for Preparation of Sample Containers and
for samples, but also for calibration standards or analytical
3
for Preservation of Organic Constituents
control solutions, or both. These procedures include prepara-
D3856 Guide for Good Laboratory Practices in Laborato-
tion, handling, storage, preservation, and analysis techniques.
2
ries Engaged in Sampling and Analysis of Water
These procedures are applicable by extension, using the
D4375 Practice for Basic Statistics in Committee D19 on
analyst’s judgement on a case-by-case basis, to spiking solu-
2
Water
tions, and are not reiterated in this guide. See also Practice
E200 Practice for Preparation, Standardization, and Stor-
E200 for preparation and storage information.
age of Standard and Reagent Solutions for Chemical
1.4 These procedures apply only to analytes that are soluble
2
Analysis
in water at the concentration of the spike plus any background
material, or to analytes soluble in a solvent that is itself
3. Terminology
water-soluble. The system used in the later case must result in
3.1 Definitions—For definitions of terms used in this guide,
a homogeneous solution of analyte and sample. Meaningful
refer to Terminology D1129.
1
This guide is under the jurisdiction ofASTM Committee D19 on Water and is
the direct responsibility of Subcommittee D19.02 on General Specifications,
2
Technical Resources, and Statistical Methods. Annual Book of ASTM Standards, Vol 11.01.
3
Current edition approved Jan. 10, 1996. Published March 1996. Annual Book of ASTM Standards, Vol 11.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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D 5810–96 (2001)
3.2 Definit
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