ASTM_D_5810_-_96_2015.pdf

Designation:D581096(Reapproved 2015)Standard Guide forSpiking into Aqueous Samples1This standard is issued under the fixed designation D5810;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This guide covers the general technique of“spiking”abroad range of materials into aqueous media.This guide willserve the analyst in preparing spiked samples for qualitycontrol purposes.Guidance is also provided to aid the analystin calculating recoveries and interpreting results.It is theresponsibility of the analyst to determine whether the proce-dures and materials described here are appropriate to the taskat hand.1.2 The procedures in this guide are focused on“matrixspike”preparation,analysis,and interpretation of results.Theapplicability of these procedures to the preparation of calibra-tion standards,calibration check standards,laboratory controlstandards,reference materials,and other quality control mate-rials by spiking is incidental.A sample(the matrix)is fortified(spiked)with the analyte of interest for a variety of analyticaland quality control purposes.While the spiking of multiplesample portions is discussed,the method of standard additionsis not covered.1.3 This guide is intended for use in conjunction with theindividual analytical test method that provides procedures foranalysis of the analyte or component of interest.The testmethod is used to determine an analyte or componentsbackground level and,again after spiking,its now elevatedlevel.Each test method typically provides procedures not onlyfor samples,but also for calibration standards or analyticalcontrol solutions,or both.These procedures includepreparation,handling,storage,preservation,and analysis tech-niques.These procedures are applicable by extension,using theanalysts judgement on a case-by-case basis,to spikingsolutions,and are not reiterated in this guide.See also PracticeE200 for preparation and storage information.1.4 These procedures apply only to analytes that are solublein water at the concentration of the spike plus any backgroundmaterial,or to analytes soluble in a solvent that is itselfwater-soluble.The system used in the later case must result ina homogeneous solution of analyte and sample.Meaningfulrecovery data cannot be obtained if an aqueous solution orhomogenous suspension of the analyte of interest in the samplecannot be attained.These procedures may be applicable tomicrobiological preparations if the homogeneity of the suspen-sion can be adequately maintained throughout the course of theanalysis,for example,by mechanical agitation or stirring.1.5 Matrix spiking may be performed in the field or in thelaboratory,depending on which part of the analytical process isto be tested.Field spiking tests the recovery of the overallprocess,including preservation and shipping of the sample.Laboratory spiking tests the laboratory process only.Spiking ofsample extracts,concentrates,or dilutions will test only thatportion of the process subsequent to addition of the spike.1.6 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.7 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4375 Practice for Basic Statistics in Committee D19 onWaterE200 Practice for Preparation,Standardization,and Storageof Standard and Reagent Solutions for Chemical Analysis3.Terminology3.1 DefinitionsFor definitions of terms used in this guide,refer to Terminology D1129.1This guide is under the jurisdiction of ASTM Committee D19 on Water and isthe direct responsibility of Subcommittee D19.02 on Quality Systems,Specification,and Statistics.Current edition approved Dec.15,2015.Published December 2015.Originallyapproved in 1996.Last previous edition approved in 2011 as D5810 96(2011).DOI:10.1520/D5810-96R15.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.2 Definitions:3.2.1 matrix spike,nthe quantity(mass)of a component(analyte)of interest that is added to a