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ASTM D5810-96(2021)

(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

Status
Published
Publication Date
30-Jun-2021
ICS
19.020 - Test conditions and procedures in general
Technical Committee
D19 - Water
Drafting Committee
D19.02 - Quality Systems, Specification, and Statistics
Current Stage
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ASTM D5810-96(2021) - Standard Guide for Spiking into Aqueous Samples
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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: D5810 − 96 (Reapproved 2021)
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, health, and environmental practices and deter-
individual analytical test method that provides procedures for
mine the applicability of regulatory limitations prior to use.
analysis of the analyte or component of interest. The test
1.8 This international standard was developed in accor-
method is used to determine an analyte or component’s
dance with internationally recognized principles on standard-
background level and, again after spiking, its now elevated
ization established in the Decision on Principles for the
level. Each test method typically provides procedures not only
Development of International Standards, Guides and Recom-
for samples, but also for calibration standards or analytical
mendations issued by the World Trade Organization Technical
control solutions, or both. These procedures include
Barriers to Trade (TBT) Committee.
preparation, handling, storage, preservation, and analysis tech-
niques.Theseproceduresareapplicablebyextension,usingthe
2. Referenced Documents
analyst’s judgement on a case-by-case basis, to spiking
2
solutions, and are not reiterated in this guide. See also Practice
2.1 ASTM Standards:
E200 for preparation and storage information.
D1129Terminology Relating to Water
D1193Specification for Reagent Water
1.4 Theseproceduresapplyonlytoanalytesthataresoluble
D3694Practices for Preparation of Sample Containers and
in water at the concentration of the spike plus any background
for Preservation of Organic Constituents
material, or to analytes soluble in a solvent that is itself
D3856Guide for Management Systems in Laboratories
water-soluble. The system used in the later case must result in
Engaged in Analysis of Water
D4375Practice for Basic Statistics in Committee D19 on
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
CurrenteditionapprovedJuly1,2021
...

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Standard Practice for Determination of Soluble Residual Contaminants in Materials by Ultrasonic Extraction

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5.1 Background—In a single laboratory, the limit of quantitation, LOQ, equal to ten times the standard deviation obtained under repeatability conditions extrapolated to zero concentration (s0) based on samples with close to zero concentrations has been recommended.3 A test result at this LOQ has an uncertainty of ±30 % at the 99 % confidence level.  
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The purpose of this guide is to provide guidelines for identifying the elements that comprise the test result of a test method and to illustrate how these elements combine into the test result. It covers the types of measurement scales used for expressing observations and test results. This guide provides information on the construction of test results from more elemental measurements.
SIGNIFICANCE AND USE
4.1 All test methods have an output in the form of a test result. This guide provides information on the construction of test results from more elemental measurements.  
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4.2.1 Form and Style for ASTM Standards,2 Section A21, requires that every test method shall contain a statement regarding its precision, preferably as a result of an interlaboratory test program. Reporting of such studies is described in Practice E177, which illustrates the development of test results from observations and test determinations.  
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ASTM E1488-12(2023)(Guide)
Standard Guide for Statistical Procedures to Use in Developing and Applying Test Methods

ABSTRACT
This guide identifies statistical procedures for use in developing new test methods or revising or evaluating existing test methods, or both. It also cites statistical procedures especially useful in the application of test methods. This standard recommends what approaches may be taken and indicates which standards may be used to perform such assessments.
SIGNIFICANCE AND USE
4.1 The creation of a standardized test method generally follows a series of steps from inception to approval and ongoing use. In all such stages there are questions of how well the test method performs.  
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FIG. 1 Sequence of Steps  
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ABSTRACT
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SCOPE
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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.
Note 1: There is no known ISO equivalent to this standard.  
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SCOPE
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