ASTM D596-2001(2018) Standard Guide for Reporting Results of Analysis of Water.pdf

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1、Designation: D596 01 (Reapproved 2018)Standard Guide forReporting Results of Analysis of Water1This standard is issued under the fixed designation D596; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A n

2、umber 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 provides guidelines for reporting inorganicand organic results of analyses of drinking water, waste water,process water, grou

3、nd water, and surface water, and so forth, tolaboratory clients in a complete and systematic fashion.1.2 The reporting of bacterial and radiological data are notaddressed in this guide.1.3 The commonly used data qualifiers for reviewing andreporting information are listed and defined. Client and lab

4、o-ratory specific requirements may make use of other qualifiers.This guide does not preclude the use of other data qualifiers.1.4 This guide discusses procedures for and specific prob-lems in the reporting of low level data, potential errors (TypeI and Type II), and reporting data that are below the

5、 calculatedmethod detection limit and above the analyte.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This international standard was developed in accor-dance with internationally recognized principles on standard-izat

6、ion established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D933 Practice for Reporting Results of Examination and

7、Analysis of Water-Formed DepositsD1129 Terminology Relating to WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD4210 Practice for Intralaboratory Quality Contr

8、ol Proce-dures and a Discussion on Reporting Low-Level Data(Withdrawn 2002)3D4460 Practice for Calculating Precision Limits WhereValues are Calculated from Other Test MethodsD4840 Guide for Sample Chain-of-Custody ProceduresD5792 Practice for Generation of Environmental Data Re-lated to Waste Manage

9、ment Activities: Development ofData Quality ObjectivesD6091 Practice for 99 %/95 % Interlaboratory DetectionEstimate (IDE) for Analytical Methods with NegligibleCalibration ErrorE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3. Terminology3.1 Defini

10、tions:3.1.1 For definitions of terms used in this standard, refer toTerminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 surrogates, ncompounds that are similar to analytesof interest in chemical composition and behavior, separation,and measurements, but that are not normally f

11、ound in environ-mental samples.3.2.1.1 DiscussionThese compounds are added to blanks,standards, samples, or spiked samples prior to analysis toconfirm the proper operation of the analytical system.3.2.2 Type I error, na statement that a substance is presentwhen it is not.3.2.3 Type II error, na stat

12、ement that a substance was notpresent (was not found) when the substance was present.4. Significance and Use4.1 The proper use of analytical data requires adequatedocumentation of all inputs, that is, the source and history ofthe sample, laboratory performing the analysis, method ofanalysis, date of

13、 analysis, precision and bias of themeasurements, and related quality assurance information.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 Aug. 1, 20

14、18. Published August 2018. Originallyapproved in 1940. Last previous edition approved in 2011 as D596 01 (2011).DOI: 10.1520/D0596-01R18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume i

15、nformation, refer to the standards Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard

16、 was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.2 In or

17、der to have defensible data, the report must becomplete and accurate, providing adequate information toevaluate the quality of the data and contain supporting infor-mation that documents sampling and analysis procedures.4.3 This guide contains some of the common data qualifiersor “flags” commonly us

18、ed by laboratories following the goodlaboratory practices, the government contract program, orfound in the commercial laboratories. Examples of thesequalifiers are the use of (E) for estimated value, (U) foranalyzed for but not detected, and (B) for analyte was found inthe blank (see 8.11). The qual

19、ifiers included in this guideshould help the laboratory and its customers to better under-stand each other by using standardized qualifiers.4.4 Practice D933 is a comprehensive practice for reportingwater-formed constituents such as metal oxides, acidanhydrides, and others.5. Sample Documentation5.1

20、 Information regarding the source and history of thesample to be included in the analytical report should define thesample and include the following, as appropriate:5.1.1 Laboratory performing analysis;5.1.2 Name and address of organization or person request-ing analysis;5.1.3 Specific location of s

21、ampling and complete identifica-tion of sample;5.1.4 Date and time of sampling;5.1.5 Sample identification number; and5.1.6 Sampling method, treatment, and preservation.5.2 In addition to the information in 5.1, the followinginformation should be included as appropriate:5.2.1 Identification of sampl

22、ing organization and individualsampler;5.2.2 Pressure and temperature of system sampled;5.2.3 Flow rate of water in a stream, outfall, pipe, and soforth;5.2.4 Copies of sampling logs with signatures;5.2.5 Chain-of-custody forms with signatures (see GuideD4840);5.2.6 Results of field measurements; an

23、d5.2.7 Description information (color, odor, and so forth)clearly presented.5.2.8 The information about the sample documented in thereport should be complete enough to provide direct unabridgedlinks to underlying documents (such as chain-of-custody re-cords and field logs) and information (such as n

24、ame of sampler,lot numbers of the sample bottles, and preservatives).6. Analysis Documentation6.1 The laboratory system shall provide enough informationto the user or reviewer so that all of the events that couldinfluence the quality of the data can be reconstructed. The usermay not need to have the

25、 information communicated directly tothem, but it must be available upon request. Such informationshould describe how effectively all procedures were carried outand how processes were controlled so that they meet industryand government standards for performance.6.2 As described in Guide D3856, the t

26、est method ofanalysis should be specified in the analytical report for eachdetermination performed on a sample. A reference of sufficientdefinition or a copy of the test method should be provided tothe requestor of the analytical services.6.3 The report should note any deviation from the specifiedte

27、st method. Whenever a choice is allowed, the rational forselecting a given method should be documented.6.4 The precision, bias, and detection limit of each analyti-cal test method should be disclosed as part of either the testmethod or the analytical report. Consult Guide D3856 for thequality contro

28、l system from which estimates of precision andbias could be made, or review the procedure for determiningsingle-operator precision of a test method as provided inPractice D2777 for guidance. The procedure used to derive thedetection limit should be identified along with any specificdefinitions assoc

29、iated with the derivation. Practice D4210 isone of many sources for computing single laboratory methoddetection limits. Practice D6091 provides an estimate of thedetection level achievable by multiple laboratories on singlesample.6.5 The date and time on which each determination isperformed should b

30、e recorded, as should other time-criticalprocesses such as extractions, storage times, drying times, andso forth.6.6 The analytical reports should clearly specify the form inwhich multi-atomic analytes, such as nitrate andorthophosphate, are reported.6.7 If a sample is prepared for analysis in a non

31、standardmanner or in a manner different from the routine batchprocedures (that is, special cleanup procedures or dilutionrequired prior to analysis) then the report should clearly presentthe deviation and the reason why the deviation was required.6.8 If a sample is diluted prior to analysis, the sam

32、pledilution values should be reported from which the ratios can bedetermined and the reason for the dilution documented.7. Documentation of Quality7.1 Each sample analysis may have different quality needsbased on the use of the data or the data quality objectives (seePractice D5792). This informatio

33、n should be determined be-fore sampling and analysis. Based on the information, ananalytical report may include the following information, asappropriate:7.1.1 Amount recovered and percent recovery of any surro-gate compounds with laboratory control limits,7.1.2 Results of corresponding check samples

34、 or blankspikes with laboratory control limits,7.1.3 Results of analysis of duplicate samples or duplicatematrix spike samples and the percent difference with laboratorycontrol limits,7.1.4 Recoveries of any matrix spikes (and matrix spikeduplicates) with laboratory control limits,7.1.5 Results of a

35、ll blanks,7.1.6 Results of any reference samples run during sampleanalysis with laboratory control limits,D596 01 (2018)27.1.7 Calibration and tuning data, and7.1.8 Chromatogram or charts.8. Reporting Data8.1 Report data in accordance with the customer and labo-ratory agreement. In the absence of a

36、specific agreement, reportthe data in accordance with laboratory policy or governmentmandated requirements, if appropriate.8.2 Compound specific analysis may require tentative iden-tification without verification. The criteria for identificationand a copy of the chromatogram or other instrument outp

37、utshould be included in the report.8.3 Upon request, the quality documentation found in Sec-tion 7 should be included in the report.8.4 Any deviation from the established method or standardoperating procedure (SOP), must be reported to the customer.Reasons for the deviation and the expected impact o

38、n the datashould be given.8.5 The procedures, method, or SOP used to report theanalytical values shall be specified.NOTE 1If there is no deviation from the contract or agreed uponprocedure, then reference to the document may be sufficient.8.6 In cases where the customer desires a summary of thedata

39、to be transmitted to them, the laboratory will keepsufficient records on file to reproduce the data.8.7 Detection limits should be reported in accordance withlaboratory policy, established procedures, or regulatory re-quirement. These polices and procedures must be clearlyidentified and understood b

40、y all personnel reporting the analy-sis. Results reported below laboratory established detectionlimits may be reported upon customer request as discussed inSection 10.NOTE 2Some commercial laboratories establish their detection limitsbased on what their average laboratory can achieve over an extende

41、dperiod of time. A given laboratory may achieve lower compound specificvalues than the average.8.8 Report blank data results and, where appropriate, actualdata from the equipment. Blanks should not be subtracted fromthe sample results unless required by the test method. Thecustomer should determine,

42、 with advisement form thelaboratory, if blank subtraction is necessary or required. (SeeSection 10.)8.9 Recording direct measurement test results should bereported by recording all digits that are known plus one thatmay be subject to change on repeated analysis. When calcu-lating results from test d

43、ata, rounding should be performedonly on the final result, not upon the intermediate valuesemployed in the calculation.8.10 Frequently, replicate determinations are made. Whenreplicate results are obtained, useful information is now avail-able that is lost if the results of these replicates are not

44、reported.It is important that a reporting laboratory establish a consistentprotocol for reporting replicate data. In order to arrive at acoherent protocol for this purpose, a number of issues andoptions should be evaluated.8.10.1 Replicate TypesReplication may be performed atdifferent levels. Replic

45、ation may occur at the point ofsampling, at the sample preparation step, the prepared sampleanalysis step, or at some other point in the analytical process.Different types of replicates may be handled differently andshould not be mixed. The type of replicate should be madeclear to the user.8.10.2 Re

46、porting Replicate AveragesReplicate resultsmay be reported separately or as an average. When averageresults are reported, several factors are considered.8.10.2.1 DocumentationThe data users should know whenthe reported results is an average of replicates. Averages ofdifferent numbers or replicates h

47、ave different quality (preci-sion) leading to different conclusions about data validity. Forthis reason, the number of replicates used in a reported averageshould be reported with the averaged results.8.10.2.2 CriteriaCriteria must be established as to when aresult is part of a replicate set. For ex

48、ample, when a dilution isperformed on a sample prior to analysis, the original result andthe diluted result may both be within the quantitative range ofthe analytical method. Although the dilution step produces avalue that is not a true replicate, the added value of reportingan average of these valu

49、es may be warranted.8.10.2.3 Selection for AveragingAnalytical results may beproduced within four discrete ranges. Each of these ranges isaffected by sample dilution or concentration. Replicates maybe generated within different ranges for the sample analysis.The four discrete ranges are listed as follows in increasingorder of size:(1) Below a limit of detection, where the analyte cannot besaid to be present with confidence above a set level.(2) Between a limit of detection and a limit of quantitationwhere the analyte can be said to be present with a preset limitof confide