1、Designation: D 5847 02 (Reapproved 2007)Standard Practice forWriting Quality Control Specifications for Standard TestMethods for Water Analysis1This standard is issued under the fixed designation D 5847; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice provides specific, mandatory requirementsfor incorporating quality con
3、trol (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
4、or 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. Prio
5、r to 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 D 2777, andshall advise the designer of the study of any changes needed to ful-fill the requirements of these practices. Before a col
6、laborative 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 in
7、formation 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
8、the 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-19te
9、st methods 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 ongoing
10、competency.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. Thes
11、e requirements 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 a
12、specific 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 comp
13、liance 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 D 5789 are considered in compliance with this
14、Practice.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 as
15、microbiological methods.2. Referenced Documents2.1 ASTM Standards:2D 1129 Terminology Relating to WaterD 1193 Specification for Reagent WaterD 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on Water1This practice is under the jurisdiction of ASTM Com
16、mittee D19 on Water andis the direct responsibility of Subcommittee D19.02 on General Specifications,Technical Resources, and Statistical Methods.Current edition approved April 15, 2007. Published April 2007. Originallyapproved in 1999. Last previous edition approved in 2002 as D 5847 02.2For refere
17、nced 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 International, 100 Barr Harbor Drive, PO Box C700, West
18、Conshohocken, PA 19428-2959, United States.D 3648 Practices for the Measurement of RadioactivityD 3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD 4375 Practice for Basic Statistics in Committee D19 onWaterD 5789 Practice for Writing Quality Contro
19、l Specificationsfor Standard Test Methods for Organic Constituents3D 5810 Guide for Spiking into Aqueous Samples3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this practice, refer toTerminology D 1129 and Terminology D 4375.3.2 Definitions of Terms Specific to This Standard:3.2
20、.1 batcha set (group) of samples 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 o
21、f samples in the batch is defined 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 appropriatecorr
22、ective action. To make such a 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 con
23、centration either purchased froman 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.
24、2.4 independent reference material (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 contro
25、l sample (LCS)a sample of knownconcentration 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 Ap
26、pendix X1. The LCS can be an 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 common
27、lyknown as a “quality control 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 D 5810.)3.2.7 m
28、ethod blank (blank)reagent water (see Specifica-tion D 1193) 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
29、methodblank is to confirm that 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 s
30、ubstance that can be measured with 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
31、 This practice provides the writer 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 calibrati
32、on of themeasurement system,4.1.2 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
33、at least one sample per batch issuggested. 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
34、 reasons must be documented in 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 obtainedt
35、hrough a competent application 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
36、 practice must be included in each 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 be3Withdrawn.D 5847 02 (2007)2performed. This minimum level of QC is stipulated in thi
37、spractice and by the taskgroups developing D-19 test methods.If 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 Methods6.1 Every test method must have a quality co
38、ntrol (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 measures that must be specified in the QC sectionof test
39、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 demonstration of laboratory capability isnecessary to
40、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 system is in control at the time samples are beingana
41、lyzed.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 specific matrix.6.1.1.7 An IRM is analyzed periodically t
42、o 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 level at whichthe substance(s) determined by the tes
43、t method can be detectedand measured.6.1.3 Statistical tests should be done at a significance levelof a # 0.01, that is, $ 99 % confidence level. If other levelsare specified, the reason for deviation should be delineated inthe method.6.1.4 The operational principles and characteristics of de-tector
44、s 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 each test method, practice or guiderelative to
45、applicable QC program requirements. Guidance onthe preparation and use of instrument tolerance and controlcharts can be found in Practices D 3648 and D 3856, and inASTM MNL 7.46.2 Calibration and Calibration VerificationFor testmethods requiring calibration of instrumentation, an appropri-ate number
46、 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 test method. For tests run infrequently,analysi
47、s 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 standard concentration be used each time calibratio
48、nis 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. Alternatively, data should be compared tothe
49、 calibration limits stated in the test method or should bedeveloped from collaborative study data. Refer to GuideD 3856 and Practice D 3648 for further information on cali-bration 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 the stability of the titrant.6.2.2 An alternate
