1、Designation: D5847 02 (Reapproved 2012)Standard Practice forWriting Quality Control Specifications for Standard TestMethods for Water Analysis1This standard is issued under the fixed designation D5847; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 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 practice provides specific, mandatory requirementsfor incorporating quality contro
3、l (QC) procedures into all testmethods under the jurisdiction of Committee D-19.1.2 ASTM has adopted the following:Policy on implementation of requirements for a quality controlsection in standard test methods generated by Committee D-19on Water.GENERALBy July 29, 1998, or at the next reapproval or
4、revision,whichever is later, every D-19 Standard Test Method shall contain aQC section that is in full compliance with the requirements of thispractice.NEW COLLABORATIVE TESTINGAs of July 29, 1998, each col-laborative study design shall include a QC section as part of themethod to be tested. Prior t
5、o approval of the study design, the Re-sults Advisor shall ascertain the appropriateness of the QC section inmeeting the requirements of this Practice and Practice D2777, andshall advise the designer of the study of any changes needed to ful-fill the requirements of these practices. Before a collabo
6、rative studymay be conducted, approval of the study design by the Results Advi-sor must be obtained.OLDER VALIDATED METHODSStandard test methods that werevalidated using D-2777-77, D-2777-86, or D-2777-94, when ballottedfor reapproval or revision, shall contain a QC section based upon thebest inform
7、ation from the historical record. Where appropriate, infor-mation derived from the record of the collaborative study shall beutilized for this purpose. The introduction of the QC section intothese standard test methods shall not be construed as a requirementfor a new collaborative study, though the
8、Subcommittee may opt forsuch a study. Any information available regarding QC or precision/bias testing shall be included in the appropriate sections of the pub-lished method.1.3 Required QC sections in all applicable test methods areintended to achieve two goals. First, users of Committee D-19test m
9、ethods will be able to demonstrate a minimum compe-tency in the performance of these test methods by comparisonwith collaborative study data. Second, all users of test methodswill be required to perform a minimum level of QC as part ofproper implementation of these test methods to ensure ongoingcomp
10、etency.1.4 This practice contains the primary requirements for QCof a specific test method. In many cases, it may be desirable toimplement additional QC requirements to assure the desiredquality of data.1.5 The specific requirements in this practice may not beapplicable to all test methods. These re
11、quirements may varydepending on the type of test method used as well as theanalyte being determined and the sample matrix being ana-lyzed. See Explanation 1 in Appendix X1.1.5.1 If there are compelling reasons why any of the specificQC requirements listed in this practice are not applicable to aspec
12、ific test method, these reasons must be documented in theQC section of the test method.1.5.2 With the approval of Committee D-19 on the recom-mendation of the D-19 Results Advisor and the TechnicalOperations section of the Executive Subcommittee, a statementgiving the compelling reasons why complian
13、ce with all orspecific points of this practice cannot be achieved will meet therequirements of both ASTM and this practice.1.5.3 Test Methods developed prior to the approval of thispractice with a QC Section that meet the requirements ofSpecification D5789 are considered in compliance with thisPract
14、ice.1.6 This practice is for use with quantitative methods andmay not be applicable to qualitative test methods.1.7 Presently, this practice is applicable primarily to chemi-cal test methods. It is intended that, in future revisions, thepractice will be expanded to include other methods such asmicro
15、biological methods.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3648 Practices for the Measurement of Radioactivity1This pr
16、actice is under the jurisdiction of ASTM Committee D19 on Water andis the direct responsibility of Subcommittee D19.02 on Quality Systems, Specifi-cation, and Statistics.Current edition approved June 15, 2012. Published June 2012. Originallyapproved in 1999. Last previous edition approved in 2012 as
17、 D5847 02(2007).DOI: 10.1520/D5847-02R12.2For 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.1Copyright ASTM Inte
18、rnational, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4375 Practice for Basic Statistics in Committee D19 onWaterD5789 Practice for Writing Quality Control Specificationsfor Standa
19、rd Test Methods for Organic Constituents3D5810 Guide for Spiking into Aqueous Samples3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this practice, refer toTerminology D1129 and Terminology D4375.3.2 Definitions of Terms Specific to This Standard:3.2.1 batcha set (group) of samp
20、les analyzed such thatresults of analysis of the QC samples (laboratory controlsample, method blank, matrix spike, and duplicate or matrixspike duplicate) analyzed with the batch are indicative of thequality of the results of analysis of samples in the batch. Thenumber of samples in the batch is def
21、ined by the task groupresponsible for the method. See 6.4 and Explanation 2 inAppendix X1.3.2.1.1 DiscussionWhen results from tests of any of theQC samples associated with batch the fail to meet the perfor-mance criteria, the test method should define the appropriatecorrective action. To make such a
22、 response valid, the batchmust be constructed in such a way as to assure that all variablesaffecting the batch will affect all samples in the batch in astatistically equivalent manner.3.2.2 calibration standarda solution containing the ana-lyte of interest at a known concentration either purchased f
23、roman external source or prepared in-house from materials ofknown purity or concentration, or both, and used to calibratethe measurement system.3.2.3 detection limitthe minimum concentration oramount of a substance that can be detected with a knowndegree of confidence.3.2.4 independent reference mat
24、erial (IRM)a material ofknown purity and concentration obtained either from theNational Institute of Standards and Technology (NIST) or otherreputable supplier. The IRM shall be obtained from a differentlot of material than is used for calibration.3.2.5 laboratory control sample (LCS)a sample of kno
25、wnconcentration and composition that is taken through the entiretest method to determine whether the analytical system is incontrol. The LCS must be prepared in the appropriate ASTM-grade water from a material that sufficiently challenges the test.See Explanation 3 in Appendix X1. The LCS can be an
26、IRMobtained from an outside source or prepared in-house frommaterials of known purity and concentration. Alternatively, theLCS may be a real sample of the matrix that is typicallyanalyzed and which has been fully characterized.3.2.5.1 DiscussionThe LCS may also be commonlyknown as a “quality control
27、 sample” or an “ongoing precisionand recovery sample” (OPR).3.2.6 matrix spike (MS)addition of a known concentrationof analyte to a routine sample representing a specific matrix forthe purpose of evaluating interference from matrix compo-nents. (See Guide D5810.)3.2.7 method blank (blank)reagent wat
28、er (see Specifica-tion D1193) either known to be free of the constituent(s) ofinterest or containing only a low, known concentration of theconstituent(s) of interest not exceeding five times the estimateddetection limit.3.2.7.1 DiscussionThe purpose of analysis of the methodblank is to confirm that
29、the reagents or analytical system, orboth, do not contribute a measurable amount of the constitu-ent(s) of interest during analysis of routine samples or, if theydo, to determine what the contribution is.3.2.8 quantitation limitthe minimum concentration oramount of a substance that can be measured w
30、ith a knowndegree of confidence.3.2.9 sample pretreatment (pretreatment)any handling,manipulation or treatment of a sample prior to subjecting thesample to the analysis. Examples are filtration, digestion,dilution, pH adjustment and extraction.4. Summary of Practice4.1 This practice provides the wri
31、ter of a test method inCommittee D19 specific steps to be included in the QC sectionof the test method. A QC section is required in all applicablestandard test methods that mandates use of the following QCmeasures:4.1.1 Periodic calibration or verification of calibration of themeasurement system,4.1
32、.2 Initial demonstration of laboratory capability,4.1.3 Analysis of at least one blank per batch,4.1.4 Analysis of at least one LCS per batch,4.1.5 Analysis of at least one MS per batch, where appli-cable, and4.1.6 Periodic analysis of an IRM.4.2 Duplicate analysis of at least one sample per batch i
33、ssuggested. The duplicate analysis may be of a sample or of amatrix spike (matrix spike duplicate; MSD). See Explanation 4in Appendix X1.4.3 If there are valid reasons why any of the above QCrequirements are inapplicable to a specific test method (seeSection 1.), these reasons must be documented in
34、the QCsection of the test method. See 1.5 and Explanation 1 inAppendix X1.5. Significance and Use5.1 In order to be certain that the end user of analyticalresults obtained from using an ASTM Committee D-19 testmethod can be confident that the values have been obtainedthrough a competent application
35、of the test method, a demon-stration of the proficiency of the analytical system must beperformed. Appropriate proficiency is demonstrated byachievement of performance criteria derived from results of thetest method collaborative study. The QC measures specified inthis practice must be included in e
36、ach ASTM test method, asapplicable, to ensure the quality of measurements.5.2 In order for users of D-19 test methods to achieveconsistently valid results, a minimum level of QC must beperformed. This minimum level of QC is stipulated in thispractice and by the taskgroups developing D-19 test method
37、s.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.D5847 02 (2012)2If the specific requirements outlined in this practice are notapplicable to the test method, alternative QC must be defined inthe test method.6. Requirements for QC Specifications in Test
38、 Methods6.1 Every test method must have a quality control (QC)section. Listed below are requirements applicable to nearly allchemical test methods and that must be followed to ensure thatthe test method is in control and to validate the accuracy of datagenerated for a specific matrix.6.1.1 The measu
39、res that must be specified in the QC sectionof test methods and the reasons for these measures are asfollows:6.1.1.1 Calibration and calibration verification are necessaryto ensure that the analytical system is properly calibratedduring the period that the analysis is performed.6.1.1.2 An initial de
40、monstration of laboratory capability isnecessary to prevent errors as a result of unfamiliarity with thetest.6.1.1.3 Analysis of a blank with each batch may indicatethat analytes in a test sample are the result of contamination.6.1.1.4 An LCS is run with each batch to determine that themeasurement s
41、ystem is in control at the time samples are beinganalyzed.6.1.1.5 An MS (recovery check) provides information onthe bias of the test method in a specific matrix.6.1.1.6 A duplicate analysis (Dup) or duplicate of the MS(matrix spike duplicate; MSD) indicates the repeatability of themethod for a speci
42、fic matrix.6.1.1.7 An IRM is analyzed periodically to validate theaccuracy of the test system and standards used for calibration.6.1.2 In addition to the QC measures required above, eachtest method should contain a detection limit and a quantitationlimit so that there is an indication of the lowest
43、level at whichthe substance(s) determined by the test method can be detectedand measured.6.1.3 Statistical tests should be done at a significance levelof 0.01, that is, 99 % confidence level. If other levels arespecified, the reason for deviation should be delineated in themethod.6.1.4 The operation
44、al principles and characteristics of de-tectors used for radioactivity measurements are somewhatdifferent from those of instruments used for measurements ofchemical and physical properties. Therefore, authors of ASTMtest methods for radioactivity measurements should providespecific guidance within e
45、ach test method, practice or guiderelative to applicable QC program requirements. Guidance onthe preparation and use of instrument tolerance and controlcharts can be found in Practices D3648 and D3856, and inASTM MNL 7.46.2 Calibration and Calibration VerificationFor testmethods requiring calibratio
46、n of instrumentation, an appropri-ate number of calibration standards must be analyzed duringday that an analysis is performed to confirm that the instrumentis properly set up and required sensitivity is being obtained.The actual number of standards required will depend on therequirements of the tes
47、t method. For tests run infrequently,analysis of a single calibration standard to verify an existingcalibration curve may suffice. For tests run frequently, it maybe necessary to intersperse verification standards with testsamples. Under these circumstances, it is recommended that adifferent standar
48、d concentration be used each time calibrationis verified. Raw data (absorbance, intensity, etc.) should becompared to data generated in the past under the sameconditions and should fall within three standard deviations ofthe mean value found in the past based on the pooled singleoperator precision.
49、Alternatively, data should be compared tothe calibration limits stated in the test method or should bedeveloped from collaborative study data. Refer to GuideD3856 and Practice D3648 for further information on calibra-tion checks.6.2.1 For titrimetric test methods, titrants must be standard-ized on a scheduled basis against a standard solution of knownconcentration in duplicate or triplicate. The average normality/molarity is then used for calculation. The frequency of stan-dardization is left to the judgment of the writer of the testmethod and should be based on
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