1、Designation: D 596 01 (Reapproved 2006)Standard Guide forReporting Results of Analysis of Water1This standard is issued under the fixed designation D 596; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、 number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 inorgan
3、icand 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 qual
4、ifiers 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 lev
5、el data, potential errors (TypeI and Type II), and reporting data that are below the calculatedmethod detection limit and above the analyte.2. Referenced Documents2.1 ASTM Standards:2D 933 Practice for Reporting Results of Examination andAnalysis of Water-Formed DepositsD 1129 Terminology Relating t
6、o WaterD 2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD 3856 Guide for Good Laboratory Practices in Laborato-ries Engaged in Sampling and Analysis of WaterD 4210 Practice for Intralaboratory Quality Control Proce-dures and a Discussion on R
7、eporting Low-Level Data3D 4460 Practice for Calculating Precision Limits WhereValues are Calculated from Other Test MethodsD 4840 Guide for Sample Chain-of-Custody ProceduresD 5792 Practice for Generation of Environmental DataRelated to Waste Management Activities: Development ofData Quality Objecti
8、vesD 6091 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 DefinitionsFor definitions of terms used in this prac-ti
9、ce, refer to Terminology D 1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 surrogatescompounds that are similar to analytes ofinterest in chemical composition and behavior, separation, andmeasurements, but that are not normally found in environmen-tal samples.NOTE 1These compounds are
10、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 presentwhen it is not.3.2.3 Type II errora statement that a substance was notpresent (was not found) when the substance wa
11、s 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 analysis, precision and bias of the measure-ments, and related quality ass
12、urance 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 supporting infor-mation that documents sampling and analysis procedures.4.3 This guide contains some of the common data qual
13、ifiersor “flags” commonly used 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) for1This guide is under the jurisdiction of ASTM Committee D19 on Wa
14、ter and isthe direct responsibility of Subcommittee D19.02 on General Specifications,Technical Resources, and Statistical Methods.Current edition approved Aug. 15, 2006. Published August 2006. Originallyapproved in 1940. Last previous edition approved in 2001 as D 596 01.2For referenced ASTM standar
15、ds, 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.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consho
16、hocken, PA 19428-2959, United States.analyzed for but not detected, and (B) for analyte was found 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 D 933 is a compre
17、hensive practice for reportingwater-formed constituents such as metal oxides, acid anhy-drides, and 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.
18、1.1 Laboratory performing analysis,5.1.2 Name and address of organization or person request-ing analysis,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 preservatio
19、n.5.2 In addition to the information in 5.1, the followinginformation should be included as appropriate: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 o
20、f sampling logs with signatures,5.2.5 Chain-of-custody forms with signatures (see GuideD 4840),5.2.6 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 t
21、o provide direct unabridgedlinks to underlying documents (such as chain-of-custodyrecords and field logs) and information (such as name ofsampler, lot numbers of the sample bottles, and preservatives).6. Analysis Documentation6.1 The laboratory system shall provide enough informationto the user or r
22、eviewer so that all of the events that couldinfluence the quality of the data can be reconstructed. 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
23、 processes were controlled so that they meet industryand government standards for performance.6.2 As described in Guide D 3856, 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 te
24、st method should be provided tothe requestor of the analytical services.6.3 The report should note 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
25、 test method should be disclosed as part of either the testmethod or the analytical report. Consult Guide D 3856 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 inPrac
26、tice D 2777 for guidance. The procedure used to derive thedetection limit should be identified along with any specificdefinitions associated with the derivation. Practice D 4210 isone of many sources for computing single laboratory methoddetection limits. Practice D 6091 provides an estimate of thed
27、etection level achievable by multiple laboratories on singlesample.6.5 The date and time on which each 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
28、the form inwhich multi-atomic analytes, such as nitrate and orthophos-phate, are reported.6.7 If a sample 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 rep
29、ort should clearly presentthe deviation and the reason why the deviation was required.6.8 If a sample 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 sampl
30、e analysis may have different quality needsbased on the use of the data or the Data Quality Objectives (SeePractice D 5792). This information should be determinedbefore sampling and analysis. Based on the information, ananalytical report may include the following information, asappropriate:7.1.1 Amo
31、unt recovered and percent recovery of any surro-gate compounds with laboratory control limits,7.1.2 Results 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 lab
32、oratorycontrol limits,7.1.4 Recoveries of any matrix spikes (and matrix spikeduplicates) with laboratory 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
33、 or charts.8. Reporting Data8.1 Report data in accordance with the customer and labo-ratory agreement. In the absence of a specific agreement, reportthe data in accordance with laboratory policy or governmentmandated requirements, if appropriate.8.2 Compound specific analysis may require tentative i
34、den-tification without verification. The criteria for identificationand a copy of the 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.D 596 01 (2006)28.4 Any deviation from the es
35、tablished method or standardoperating procedure (SOP), must be reported to the customer.Reasons for the 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 contr
36、act or agreed uponprocedure, then reference to the document may be sufficient.8.6 In cases where the customer 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 withlab
37、oratory policy, established procedures, or regulatory re-quirement. These polices and procedures must 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 inSecti
38、on 10.NOTE 3Some commercial laboratories establish their detection limitsbased on what their average laboratory 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 f
39、rom the equipment. Blanks should not be subtracted fromthe sample results unless required by the test 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 berepo
40、rted by recording all digits that are known plus one thatmay be subject to change on repeated analysis. 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 determination
41、s are made. Whenreplicate results are obtained, useful information is now avail-able that is lost if the 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
42、this purpose, a number of issues andoptions should be evaluated.8.10.1 Replicate TypesReplication may 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.D
43、ifferent types of replicates may be handled differently andshould not be mixed. The type of replicate 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
44、.2.1 DocumentationThe data users should knowwhen the reported results is an average of replicates. Averagesof 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 averages
45、hould 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 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 a
46、nalytical method. Although the dilution step produces avalue that is not a true replicate, the added value 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
47、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
48、a limit of detection and a limit of quantitationwhere the analyte can be said to be present with a preset 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 t
49、he 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 followed:(1) Select and average only replicates that fall within thequantitation range of the analytical method. If none exist, then,(2) Select and average only replicates that fall above thequantitat
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