1、March 2013 Translation by DIN-Sprachendienst.English price group 15No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS
2、13.060.45!$v“1948396www.din.deDDIN ISO 11352Water quality Estimation of measurement uncertainty based on validation and qualitycontrol data (ISO 11352:2012),English translation of DIN ISO 11352:2013-03Wasserbeschaffenheit Abschtzung der Messunsicherheit beruhend auf Validierungs- und Kontrolldaten(I
3、SO 11352:2012),Englische bersetzung von DIN ISO 11352:2013-03Qualit de leau Estimation de lincertitude de mesure base sur des donnes de validation et de contrlequalit (ISO 11352:2012),Traduction anglaise de DIN ISO 11352:2013-03www.beuth.deDocument comprises 33 pagesIn case of doubt, the German-lang
4、uage original shall be considered authoritative.02.13 DIN ISO 11352:2013-03 A comma is used as the decimal marker. Contents PageForeword . 3Introduction 51 Scope 82 Normative references . 83 Terms and definitions . 84 Symbols .115 Principle .126 Procedure 137 Preparative considerations for the estim
5、ation of measurement uncertainty .137.1 Specification of the measurement 137.2 Specification of the parametric form in which the measurement uncertainty is reported 138 Evaluation of available precision and bias data .148.1 Approach and criteria .148.2 Within-laboratory reproducibility 158.3 Method
6、and laboratory bias 179 Calculation of the combined standard uncertainty 2110 Calculation of the expanded uncertainty 2211 Estimation of measurement uncertainty from reproducibility standard deviation .2212 Report .22Annex A (normative)E stimation of the standard uncertainty from range control chart
7、s 23Annex B (informative) Examples of the estimation of measurement uncertainty 24Bibliography .332DIN ISO 11352:2013-03 National foreword This document (ISO 11352:2012) has been prepared by Technical Committee ISO/TC 147 “Water quality” (Secretariat: DIN, Germany). The responsible German body invol
8、ved in its preparation was the Normenausschuss Wasserwesen (Water Practice Standards Committee), Working Committee NA 119-01-03-06-03 AK Messunsicherheit of NA 119-01-03 AA Wasseruntersuchung. Attention is drawn to the possibility that some of the elements of this document may be the subject of pate
9、nt rights. DIN and/or DKE shall not be held responsible for identifying any or all such patent rights. Designation of method A 0-4: Estimation of measurement uncertainty based on validation and quality control data (A 0-4): Method DIN ISO 11352 A 0-4 The DIN Standards corresponding to the Internatio
10、nal Standards referred to in this document are as follows: ISO 3534-2 E DIN ISO 3534-2 ISO 5725-2 DIN ISO 5725-2 ISO 10304-1 DIN EN ISO 10304-1 ISO 13528 DIN ISO 13528 3DIN ISO 11352:2013-03 Expert assistance and specialized laboratories will be required to perform the analyses described in this sta
11、ndard. Existing safety requirements are to be observed. Depending on the objective of the analysis, a check shall be made on a case-by-case basis as to whether and to what extent additional conditions will have to be specified. This standard has been prepared by the Normenausschuss Wasserwesen (Wate
12、r Practice Standards Committee) in collaboration with the Wasserchemische Gesellschaft - Fachgruppe in der Gesellschaft Deutscher Chemiker (Water Chemistry Society - Division of the German Chemical Society). It is part of the series Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammunters
13、uchung (German standard methods for the examination of water, waste water and sludge and describes method A 0-4: Estimation of measurement uncertainty based on validation and quality control data (A 0-4) Standard methods published as DIN Standards are obtainable from Beuth Verlag GmbH, either indivi
14、dually or grouped in volumes. The standard methods included in the loose-leaf publication entitled Deutsche Einheitsverfahren zur Wasser-, Abwasser- und Schlammuntersuchung will continue to be published by Wiley-VCH Verlag GmbH Eurolab TR 19gives an overview of the main approaches.This International
15、 Standard specifies a set of procedures to enable laboratories to estimate the measurement uncertainty of their results, using an approach based on quality control results and validation data. It is structured in a way that is applicable to analysts that do not have a thorough understanding of metro
16、logy or statistics.NEN 77798and Nordtest TR 53710have been used as a basis for developing this International Standard. The approach taken is “top-down”, contrary to the mainly “bottom-up” strategy adopted in ISO/IEC Guide 98-3.It is statistically acceptable to combine a precision estimate and the un
17、certainty associated with the bias into one uncertainty measure. The sources of data for this approach are method validation and analytical quality control. The experimental approach specified in this International Standard enables a greater coverage of the sources of variation observed during routi
18、ne use of the analytical method.DIN ISO 11352:2013-03 7Water quality Estimation of measurement uncertainty based on validation and qualitycontrol data 1 ScopeThis International Standard specifies methods for the estimation of measurement uncertainty of chemical and physicochemical methods in single
19、laboratories based on validation data and analytical quality control results obtained within the field of water analysis.NOTE 1 The principles of the estimation of uncertainty specified in this International Standard are consistent with the principles described in ISO/IEC Guide 98-3.In this Internat
20、ional Standard, the quantification of measurement uncertainty relies on performance characteristics of a measurement procedure obtained from validation and the results of internal and external quality control.NOTE 2 The approaches specified in this International Standard are mainly based on QUAM11,
21、NEN 77798, Nordtest TR 53710, and Eurolab TR 19.NOTE 3 This International Standard only addresses the evaluation of measurement uncertainty for results obtained from quantitative measurement procedures. The uncertainties associated with results obtained from qualitative procedures are not considered
22、.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO/IEC Guide 98-3:2008, Un
23、certainty of measurement Part 3: Guide to the expression of uncertainty in measurement (GUM:1995)3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.NOTE 1 The terms and definitions listed are generally reproduced without the Notes which are associated
24、 with the terms and definitions in the respective references.NOTE 2 The terms concerning precision data from interlaboratory trials are taken from ISO 3534-2:20061because the definitions in ISO/IEC Guide 99:20077are wider than those in ISO 3534-2:2006 as they include different measurement procedures
25、, which is not appropriate for this International Standard.3.1truenesscloseness of agreement between the average of an infinite number of replicate measured quantity values and a reference quantity valueISO/IEC Guide 99:20077, 2.143.2precisioncloseness of agreement between indications or measured qu
26、antity values obtained by replicate measurements on the same or similar objects under specified conditionsISO/IEC Guide 99:20077,2.15DIN ISO 11352:2013-03 83.3errormeasurement errormeasured quantity value minus a reference quantity valueISO/IEC Guide 99:20077, 2.163.4systematic errorsystematic measu
27、rement errorcomponent of measurement error that in replicate measurements remains constant or varies in a predictable mannerISO/IEC Guide 99:20077, 2.173.5biasmeasurement biasestimate of a systematic measurement errorISO/IEC Guide 99:20077, 2.183.6random errorrandom measurement errorcomponent of mea
28、surement error that in replicate measurements varies in an unpredictable mannerISO/IEC Guide 99:20077, 2.193.7repeatability conditionsobservation conditions where independent test/measurement results are obtained with the same method on identical test/measurement items in the same test or measuring
29、facility by the same operator using the same equipment within short intervals of timeISO 3534-2:20061, 3.3.63.8repeatabilityprecision under repeatability conditionsISO 3534-2:20061, 3.3.53.9batchseries of measurements made under repeatability conditions3.10intermediate precision conditionsconditions
30、 where test results or measurement results are obtained with the same method, on identical test/measurement items in the same test or measurement facility, under some different operating conditionNOTE There are four elements to the operating condition: time, calibration, operator and equipment.ISO 3
31、534-2:20061, 3.3.163.11intermediate precisionprecision under intermediate precision conditionsISO 3534-2:20061, 3.3.15DIN ISO 11352:2013-03 93.12within-laboratory reproducibilityintermediate measurement precision where variations within one laboratory alone are included3.13reproducibility conditions
32、observation conditions where independent test/measurement results are obtained with the same method on identical test/measurement items in different test or measurement facilities with different operators using different equipmentISO 3534-2:20061, 3.3.113.14reproducibilityprecision under reproducibi
33、lity conditionsISO 3534-2:20061, 3.3.103.15uncertaintymeasurement uncertaintynon-negative parameter characterizing the dispersion of the quantity values being attributed to a measurand, based on the information usedISO/IEC Guide 99:20077, 2.263.16standard uncertaintystandard measurement uncertaintym
34、easurement uncertainty expressed as a standard deviationISO/IEC Guide 99:20077, 2.303.17combined standard uncertaintycombined standard measurement uncertaintystandard measurement uncertainty that is obtained using the individual standard measurement uncertainties associated with the input quantities
35、 in a measurement modelISO/IEC Guide 99:20077, 2.313.18relative standard measurement uncertaintystandard measurement uncertainty divided by the absolute value of the measured quantity valueISO/IEC Guide 99:20077, 2.323.19target measurement uncertaintymeasurement uncertainty specified as an upper lim
36、it and decided on the basis of the intended use of measurement resultsISO/IEC Guide 99:20077, 2.343.20expanded uncertaintyexpanded measurement uncertaintyproduct of a combined standard measurement uncertainty and a factor larger than the number oneNOTE The term “factor” in this definition refers to
37、a coverage factor.ISO/IEC Guide 99:20077, 2.35DIN ISO 11352:2013-03 103.21coverage factornumber larger than one by which a combined standard measurement uncertainty is multiplied to obtain an expanded measurement uncertaintyISO/IEC Guide 99:20077, 2.384 Symbolsb bias estimated as the difference betw
38、een mean measured value and an accepted reference valuebibias of the ith reference material respectively deviation from the complete recovery (100 %) of the ith recovery experimentbrmsroot mean square of individual bias values respectively of the deviations from recovery experimentsDidifference betw
39、een the measurement result and the assigned value of the ith sample of the interlaboratory comparisonDrmsroot mean square of the differencesd2 factor for the calculation of the standard deviation from the mean range Ri variable related to an observation of a seriesj variable related to a source of u
40、ncertaintyJ total number of sources of uncertaintyk coverage factornilcnumber of analysed interlaboratory comparison samplesnMnumber of measurementsnp,inumber of participating laboratories for sample inrnumber of reference materialsnnumber of recovery experimentsRmean ranges standard deviationsbstan
41、dard deviation of the measured values of the reference materialsR,ireproducibility standard deviation from the interlaboratory comparison for sample isRwstandard deviation of the quality control resultsU expanded uncertaintyUrelrelative expanded uncertaintyuccombined standard uncertaintyuc,relcombin
42、ed relative standard uncertaintyujstandard uncertainties from different sources jDIN ISO 11352:2013-03 11uj,relrelative standard uncertainties from different sources juaddstandard uncertainty in the concentration of the analyte addedubstandard uncertainty component associated with method and laborat
43、ory biasuconcstandard uncertainty of the concentration of the addition solutionuCrefmean standard uncertainty of the reference values or mean standard uncertainty of the assigned values of the interlaboratory comparison samplesuCrefstandard uncertainty of the reference value uCiref,standard uncertai
44、nty of the assigned value of the interlaboratory sample iuRwstandard uncertainty component for the within-laboratory reproducibilityur,rangestandard uncertainty component from the range control chart (obtained under repeatability conditions)uRwbat,standard uncertainty component resulting from variat
45、ions between batchesuRwstand,standard uncertainty component of the results from the standard solution which is used as quality control sampleuVstandard uncertainty component of the volume addeduV,bsystematic standard uncertainty component of the volume addeduV,reprandom standard uncertainty componen
46、t of the volume added (obtained under repeatability conditions)eV,maxmaximum deviation of the volume from the specified value (producer information) recovery5 PrincipleA measurement result of a laboratory is an estimate of the value of the measurand. The quality of this estimate depends on the inevi
47、table uncertainty that is inherent to the measurement result. In principle, the measurement uncertainty is a property of individual measurement results. The estimation of the measurement uncertainty for each individual measurement result is usually not necessary, if the measurement result originates
48、 from a controlled measurement process. In this International Standard, the measurement uncertainty is, therefore, determined for a set of similar measurement results. Generally, it is assumed that the set of measurement results obtained with a specific analytical method is obtained under controlled conditions. The estimation of the measurement uncertainty applies to all of the measurement results within the set, independently of, for example, sample matrix
