ASTM D5810-96
(Guide)Standard Guide for Spiking into Aqueous Samples
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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NOTICE: This standard has either been superseded and replaced by a new version or
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Designation: D 5810 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope microbiological preparations if the homogeneity of the suspen-
sion can be adequately maintained throughout the course of the
1.1 This guide covers the general technique of “spiking” a
analysis, for example, by mechanical agitation or stirring.
broad range of materials into aqueous media. This guide will
1.5 Matrix spiking may be performed in the field or in the
serve the analyst in preparing spiked samples for quality
laboratory, depending on which part of the analytical process is
control purposes. Guidance is also provided to aid the analyst
to be tested. Field spiking tests the recovery of the overall
in calculating recoveries and interpreting results. It is the
process, including preservation and shipping of the sample.
responsibility of the analyst to determine whether the proce-
Laboratory spiking tests the laboratory process only. Spiking of
dures and materials described here are appropriate to the task
sample extracts, concentrates, or dilutions will test only that
at hand.
portion of the process subsequent to addition of the spike.
1.2 The procedures in this guide are focused on “matrix
1.6 The values stated in SI units are to be regarded as the
spike” preparation, analysis, and interpretation of results. The
standard.
applicability of these procedures to the preparation of calibra-
1.7 This standard does not purport to address all of the
tion standards, calibration check standards, laboratory control
safety concerns, if any, associated with its use. It is the
standards, reference materials, and other quality control mate-
responsibility of the user of this standard to establish appro-
rials by spiking is incidental. A sample (the matrix) is fortified
priate safety and health practices and determine the applica-
(spiked) with the analyte of interest for a variety of analytical
bility of regulatory limitations prior to use.
and quality control purposes. While the spiking of multiple
2. Referenced Documents
sample portions is discussed, the method of standard additions
is not covered.
2.1 ASTM Standards:
2
1.3 This guide is intended for use in conjunction with the D 1129 Terminology Relating to Water
2
individual analytical test method that provides procedures for D 1193 Specification for Reagent Water
analysis of the analyte or component of interest. The test D 3694 Practices for Preparation of Sample Containers and
3
method is used to determine an analyte or component’s for Preservation of Organic Constituents
background level and, again after spiking, its now elevated D 3856 Guide for Good Laboratory Practices in Laborato-
2
level. Each test method typically provides procedures not only ries Engaged in Sampling and Analysis of Water
for samples, but also for calibration standards or analytical D 4375 Terminology for Basic Statistics in Committee
2
control solutions, or both. These procedures include prepara- D-19 on Water
tion, handling, storage, preservation, and analysis techniques.
E 200 Practice for Preparation, Standardization, and Stor-
These procedures are applicable by extension, using the age of Standard and Reagent Solutions for Chemical
2
analyst’s judgement on a case-by-case basis, to spiking solu-
Analysis
tions, and are not reiterated in this guide. See also Practice
3. Terminology
E 200 for preparation and storage information.
3.1 Definitions—For definitions of terms used in this guide,
1.4 These procedures apply only to analytes that are soluble
refer to Terminology D 1129.
in water at the concentration of the spike plus any background
3.2 Definitions of Terms Specific to This Standard:
material, or to analytes soluble in a solvent that is itself
3.2.1 matrix spike, n—the quantity (mass) of a component
water-soluble. The system used in the later case must result in
(analyte) of interest that is added to a sample (matrix) in order
a homogeneous solution of analyte and sample. Meaningful
to test the bias as measured by recovery (of that component
recovery data cannot be obtained if an aqueous solution or
under specific analytical conditions) and reported as percent
homogenous suspension of the analyte of interest in the sample
recovery (P).
cannot be attained. These procedures may be applicable to
3.2.2 spike, v—the addition of a known a
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