ASTM D596-2001(2011) Standard Guide for Reporting Results of Analysis of Water《水分析结果报告的标准指南》.pdf

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1、Designation: D596 01 (Reapproved 2011)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.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This guide provides guidelines for reporting inorganica

3、nd organic results of analyses of drinking water, waste water,process water, ground 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 qualifi

4、ers for reviewing andreporting information are listed and defined. Client and labo-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

5、data, potential errors (TypeI and Type II), and reporting data that are below the calculatedmethod detection limit and above the analyte.1.4.1 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.2. Referenced Documents2.1 ASTM Stand

6、ards:2D933 Practice for Reporting Results of Examination andAnalysis 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 Good Laboratory Practices in Laborato-ries Engaged

7、 in Sampling and Analysis of WaterD4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on Reporting Low-Level Data3D4460 Practice for Calculating Precision Limits WhereValues are Calculated from Other Test MethodsD4840 Guide for Sample Chain-of-Custody ProceduresD5792 Prac

8、tice for Generation of Environmental Data Re-lated to Waste Management 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 t

9、oDetermine Conformance with Specifications3. Terminology3.1 DefinitionsFor definitions of terms used in this prac-tice, refer to Terminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 surrogatescompounds that are similar to analytes ofinterest in chemical composition and behavior

10、, separation, andmeasurements, but that are not normally found in environmen-tal samples.NOTE 1These compounds are added to blanks, standards, samples, orspiked samples prior to analysis to confirm the proper operation of theanalytical system.3.2.2 Type I errora statement that a substance is present

11、when it is not.3.2.3 Type II errora statement 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

12、the analysis, method ofanalysis, date of analysis, precision and bias of the measure-ments, and related quality assurance information.4.2 In order to have defensible data, the report must becomplete and accurate, providing adequate information toevaluate the quality of the data and contain supportin

13、g infor-mation that documents sampling and analysis procedures.4.3 This guide contains some of the common data qualifiersor “flags” commonly used by laboratories following the GoodLaboratory Practices, the Government Contract program, or1This guide is under the jurisdiction of ASTM Committee D19 on

14、Water and isthe direct responsibility of Subcommittee D19.02 on Quality Systems, Specification,and Statistics.Current edition approved May 1, 2011. Published June 2011. Originallyapproved in 1940. Last previous edition approved in 2006 as D596 01(2006).DOI: 10.1520/D0596-01R11.2For referenced ASTM s

15、tandards, 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.3Withdrawn. The last approved version of this historical standard is referencedon w

16、ww.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.found 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

17、 inthe blank (see 8.11). The qualifiers 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, acid anhy-drides, an

18、d others.5. Sample Documentation5.1 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 an

19、alysis,5.1.3 Specific location of sampling 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 approp

20、riate:5.2.1 Identification of sampling 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.

21、6 Results of field measurements, and5.2.7 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 fie

22、ld logs) and information (such as name 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 reconstructe

23、d. The usermay not need to have the 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

24、 As described in Guide D3856, the test 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

25、 any deviation from the specifiedtest 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. Consul

26、t Guide D3856 for thequality control 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

27、 with any specificdefinitions associated 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

28、 determination isperformed should be 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 and orthophos-phate, are reported.6.7 If a sam

29、ple is prepared for analysis in a nonstandardmanner 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

30、is diluted prior to analysis, the sampledilution 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

31、 (SeePractice D5792). This information 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 R

32、esults of corresponding check samples 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 laborat

33、ory control limits,7.1.5 Results of all blanks,7.1.6 Results of any reference samples run during sampleanalysis with laboratory control limits,7.1.7 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

34、. In the absence of a specific agreement, reportthe data in accordance with laboratory policy or governmentmandated requirements, if appropriate.D596 01 (2011)28.2 Compound specific analysis may require tentative iden-tification without verification. The criteria for identificationand a copy of the

35、chromatogram or other instrument outputshould 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 th

36、e deviation and the expected impact on the datashould be given.8.5 The procedures, method, or SOP used to report theanalytical values shall be specified.NOTE 2If there is no deviation from the contract or agreed uponprocedure, then reference to the document may be sufficient.8.6 In cases where the c

37、ustomer desires a summary of thedata 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

38、be clearlyidentified and understood by all personnel reporting the analy-sis. Results reported below laboratory established detectionlimits may be reported upon customer request as discussed inSection 10.NOTE 3Some commercial laboratories establish their detection limitsbased on what their average l

39、aboratory can achieve over an extendedperiod 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

40、method. Thecustomer should determine, with advisement form the labora-tory, if blank subtraction is necessary or required. (See Section10).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

41、. When calcu-lating results from test data, 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 t

42、he results of these replicates are not 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

43、be performed atdifferent levels. Replication may occur at the point of sam-pling, 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

44、should be madeclear to the user.8.10.2 Reporting 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 knowwhen the reported results is an average of replicates. Ave

45、ragesof different numbers or replicates have different quality (pre-cision) 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 a

46、result is part of a replicate set. For example, 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 v

47、alue of reportingan average of these values 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.

48、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 pre

49、set limitof confidence but the concentration value does not meet apreset criteria.(3) Between a limit of quantitation and the upper limit of thequantitation range of the analytical method. This is the quan-titation range of the analytical method. This is typically thehighest calibration standard used.(4) Above the quantitation range of the analytical method.8.10.2.4 It is important to first establish which of the rangesfound in 8.10.2 is applicable to each replicate. Replicatesshould not be averaged across ranges. The following selectioncriteria for averaging should be f