DIN EN 15948-2015 Cereals - Determination of moisture and protein - Method using Near-Infrared-Spectroscopy in whole kernels German version EN 15948 2015《谷类 湿度和蛋白质的测定 整个内核用近红外光谱学法 .pdf

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1、June 2015 Translation by DIN-Sprachendienst.English price group 19No 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 6

2、7.060!%CZh“2325569www.din.deDDIN EN 15948Cereals Determination of moisture and protein Method using Near-Infrared-Spectroscopy in whole kernels;English version EN 15948:2015,English translation of DIN EN 15948:2015-06Getreide Bestimmung der Feuchte und des Proteins Verfahren der Nahinfrarot-Spektros

3、kopie bei ganzen Krnern;Englische Fassung EN 15948:2015,Englische bersetzung von DIN EN 15948:2015-06Crales Dtermination de la teneur en eau et en protines Mthode utilisant la spectroscopie dans le proche infrarouge sur des grains entiers;Version anglaise EN 15948:2015,Traduction anglaise de DIN EN

4、15948:2015-06SupersedesDIN EN 15948:2012-05www.beuth.deDocument comprises 49 pagesIn case of doubt, the German-language original shall be considered authoritative.06.15 DIN EN 15948:2015-06 2 A comma is used as the decimal marker. National foreword This document (EN 15948:2015) has been prepared by

5、Technical Committee CEN/TC 338 “Cereal and cereal products” (Secretariat: AFNOR, France). The responsible German body involved in its preparation was the DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products), Working Committee NA 0

6、57-05-06 AA Getreide und Getreideerzeugnisse. The DIN Standards corresponding to the European and International Standards referred to in this document are as follows: EN ISO 12099 DIN EN ISO 12099 ISO 5725-2 DIN ISO 5725-2 EN ISO 712 DIN EN ISO 712 EN ISO 5983-2 DIN EN ISO 5983-2 CEN ISO/TS 16634-2

7、DIN SPEC 1138 (DIN ISO/TS 16634-2) EN ISO 20483 DIN EN ISO 20483 EN ISO 24333 DIN EN ISO 24333 ISO 5725-1 DIN ISO 5725-1 Amendments This standard differs from DIN EN 15948:2012-05 as follows: a) Annex A “Results of examples of interlaboratory test” has been extended to include, in addition to the FO

8、SS interlaboratory test, results of the PERTEN interlaboratory test and the CHOPIN Technologies interlaboratory test; b) Annex C (informative) “Validation of Inframatic 9500 prediction models” has been added; c) Annex D (informative) “Validation of Infraneo prediction models” has been added; d) the

9、standard has been editorially revised. Previous editions DIN EN 15948: 2012-05 DIN EN 15948:2015-06 3 National Annex NA (informative) Bibliography DIN EN ISO 12099, Animal feeding stuff, cereals and milled cereal products Guidelines for the application of near infrared spectrometry DIN ISO 5725-2, A

10、ccuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method DIN EN ISO 712, Cereals and cereal products Determination of moisture content Reference method DIN EN ISO 5983-2, Anima

11、l feeding stuffs Determination of nitrogen content and calculation of crude protein content Part 2: Block digestion and steam distillation method DIN SPEC 1138 (DIN ISO/TS 16634-2), Food products Determination of the total nitrogen content by combustion according to the Dumas principle and calculati

12、on of the crude protein content Part 2: Cereals, pulses and milled cereal products DIN EN ISO 20483, Cereals and pulses Determination of the nitrogen content and calculation of the crude protein content Kjeldahl method DIN EN ISO 24333, Cereals and cereal products Sampling DIN ISO 5725-1, Accuracy (

13、trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN EN 15948:2015-06 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 15948 March 2015 ICS 67.060 Supersedes EN 15948:2012English Version Cereals - Determinati

14、on of moisture and protein - Method using Near-Infrared-Spectroscopy in whole kernels Crales - Dtermination de la teneur en eau et en protines - Mthode utilisant la spectroscopie dans le proche infrarouge sur des grains entiers Getreide - Bestimmung der Feuchte und des Proteins - Verfahren der Nahin

15、frarot-Spektroskopie bei ganzen Krnern This European Standard was approved by CEN on 5 January 2015. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up

16、-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by trans

17、lation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finlan

18、d, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION

19、 COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15948:2015 EEN 15948:2015 (E) 2 Contents Page Fore

20、word 4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle 5 5 Method of analysis.5 5.1 General 5 5.2 Near Infrared Instrument .6 5.3 Prediction models 6 5.4 Initial validation of the model .6 5.4.1 General 6 5.4.2 Initial validation sample set 6 5.4.3 Initial validation perfor

21、mances .7 5.5 Update of calibration model and validation of new model 7 6 Sampling .7 7 Procedure .7 7.1 Preparation of the test sample .7 7.2 Measurement 7 7.3 Local validation of the method .7 7.4 Periodical adjustment of the instrument .8 7.5 Checking instrument stability 8 7.6 Follow up of metho

22、d performance .8 8 Calculation and expression of results .8 9 Accuracy and precision of the method .9 9.1 Accuracy .9 9.2 Precision .9 9.2.1 General 9 9.2.2 Repeatability .9 9.2.3 Reproducibility .9 9.2.4 Critical difference 10 10 Test Report 11 Annex A (informative) Results of examples of interlabo

23、ratory test 12 A.1 FOSS interlaboratory test 12 A.2 PERTEN interlaboratory test . 17 A.3 CHOPIN Technologies interlaboratory test 21 Annex B (informative) Validation of ANN prediction model WB003034 . 29 B.1 ANN prediction model WB003034 with associated database 29 B.2 Results of validation accordin

24、g to EN ISO 12099 29 B.3 Stability and robustness 31 Annex C (informative) Validation of Inframatic 9500 prediction models 33 C.1 Perten Inframatic 9500 prediction models . 33 C.2 Results of validations according to EN ISO 12099 33 DIN EN 15948:2015-06 EN 15948:2015 (E) 3 Annex D (informative) Valid

25、ation of Infraneo prediction models . 39 D.1 CHOPIN Technologies Infraneo prediction models . 39 D.2 Results of validation according to EN ISO 12099 39 Bibliography 45 DIN EN 15948:2015-06 EN 15948:2015 (E) 4 Foreword This document (EN 15948:2015) has been prepared by Technical Committee CEN/TC 338

26、“Cereal and cereal products”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by October 2015, and conflicting national standards shall be withdrawn at the

27、latest by October 2015. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN 15948:2012. The following modifica

28、tions were made in this new edition: Annexes have been enhanced with information on 2 other NIR instruments based on the results of the interlaboratory tests and the models of prediction. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countri

29、es are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Polan

30、d, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. DIN EN 15948:2015-06 EN 15948:2015 (E) 5 1 Scope This European Standard defines a routine method for the determination of moisture and protein in whole kernels of barley and wheat using a near-infrar

31、ed spectrophotometer in the constituent ranges: a) for wheat: 1) moisture content minimum range from 8 % to 22 %; 2) protein content minimum range from 7 % to 20 %. b) for barley: 1) moisture content minimum range from 8 % to 22 %; 2) protein content minimum range from 7 % to 16 %. This European Sta

32、ndard describes the modalities to be implemented by the supplier (5.3 and 5.4) and the user of the method. 2 Normative references The following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the editio

33、n cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN ISO 12099:2010, Animal feeding stuffs, cereals and milled cereal products Guidelines for the application of near infrared spectrometry (ISO 12099:2010) ISO 5725-2, Accuracy (

34、trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN ISO 12099:2010 apply. 4 Princip

35、le The method is based on Near-Infrared (NIR) spectroscopy, an indirect, correlative technique to predict the concentration of various constituents in organic samples. Linear or non-linear regression modelling is used to relate NIR spectra to moisture or protein concentrations determined by official

36、ly approved standard methods (e.g. artificial neural network - ANN, Partial Least Square Regression - PLS). 5 Method of analysis 5.1 General According to this document, the method of analysis is defined as the association between a NIR instrument and a model of prediction. DIN EN 15948:2015-06 EN 15

37、948:2015 (E) 6 5.2 Near Infrared Instrument Based on diffuse reflectance or transmittance measurement covering the wavelength region of 700 nm to 2 500 nm or segments of this or at selected wavelengths. 5.3 Prediction models Each model for the prediction of protein and moisture contents in whole gra

38、in of wheat and barley is amongst others defined by: the number of samples used for the calibration development; the constituent ranges covered in the model for moisture and protein; the temperature range of the samples; the number and performance of involved reference labs; the stability of the mod

39、el i.e. by number of harvests covered; the calibration file defined by its name and its IT name (for example CHECKSUM) insuring its integrity; the seasonal, geographic and genetic variations covered. 5.4 Initial validation of the model 5.4.1 General Since NIR analysis is an indirect, correlative tec

40、hnique, the results shall be validated against chemical analysis reference methods. It is important that the reference methods used are officially approved such as the methods described in the standards previously cited (Clause 2). The purpose of validation is to determine the root mean square error

41、 of prediction which depends at the same time on the correlation, the bias and the slope. The root mean square error between chemical analysis methods and predictions shall be compared to calibration performance specifications and/or historical performance. 5.4.2 Initial validation sample set The in

42、itial validation of a calibration model shall be done in accordance with EN ISO 12099 using independent test sets of wheat and barley samples, originating from different countries and analyzed by the reference methods given in Clause 2. Requirements for the validation sample set are: at least 200 sa

43、mples coming from 10 countries (20 representative samples min/country) distributed homogeneously over the entire constituent range; the part of the range without any reference sample shall not exceed 0,3 %; different scans from one sample shall not be considered as different samples; seasonal effect

44、s over at least a three year period, temperature effects, instrument variation and the variability of reference data shall be included in the set. DIN EN 15948:2015-06 EN 15948:2015 (E) 7 5.4.3 Initial validation performances The results of the initial validation shall at least fulfil the specificat

45、ions given in Table 1. Table 1 NIR performances for the determination of moisture and protein (see also Annex B) Moisture Wheat and barley Protein Wheat Protein Barley Overall accuracy expressed as SEP as constituent % w/w 0,24 % 0,27 % 0,27 % Constituent concentration in the independent validation

46、data set Min 8 % 7 % d.m. 7 % d.m. Max 22 % 20 % d.m. 16 % d.m. NOTE The minimum performance given in Table 1 includes the variation of reference data as documented by the number of reference labs involved, regional and genetic variations, the number of countries and crop species involved and the ro

47、bustness over the last five years (see also Annex B). 5.5 Update of calibration model and validation of new model The prediction model in accordance with this standard shall be updated by the one issuing the calibration model to ensure inclusion of new climatic crop conditions and new varieties intr

48、oduced on the market. These updates shall be made by keeping the original database with addition of the new samples as needed. The new prediction model shall be updated according to EN ISO 12099. Validation shall be made according to the initial validation (5.4) and include at least 20 new samples. 6 Sampling Sampling is not part of the method specified in this European Standard. A recommended sampling procedure is given in EN ISO 24333 5. It is important that the sample analyzed in r