1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI Standards PublicationBS EN ISO 12099:2010Animal feeding stuffs, cerealsand milled cereal products Guidelines for the applicationof near infrared spectrometry(ISO 12099:2010)BS EN ISO 12099:2010 BRITI
2、SH STANDARDNational forewordThis British Standard is the UK implementation of EN ISO12099:2010.The UK participation in its preparation was entrusted to TechnicalCommittee AW/10, Animal feeding stuffs.A list of organizations represented on this committee can beobtained on request to its secretary.Thi
3、s publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. BSI 2010ISBN 978 0 580 64447 4ICS 65.120Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the
4、 authority of theStandards Policy and Strategy Committee on 31 July 2010Amendments issued since publicationDate Text affectedEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 12099 June 2010 ICS 65.120 English Version Animal feeding stuffs, cereals and milled cereal products - Guidelines for
5、the application of near infrared spectrometry (ISO 12099:2010) Aliments des animaux, crales et produits de mouture des crales - Lignes directrices pour lapplication de la spectromtrie dans le proche infrarouge (ISO 12099:2010)Futtermittel, Getreide und gemahlene Getreideerzeugnisse - Anleitung fr di
6、e Anwendung von Nahinfrarot-Spektrometrie (ISO 12099:2010) This European Standard was approved by CEN on 12 June 2010. 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
7、any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language mad
8、e by translation under the responsibility of a CEN member into its own language and notified to the CEN 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, Finl
9、and, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES K
10、OMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 12099:2010: EBS EN ISO 12099:2010EN ISO 12099:2010 (E) 3 Foreword This document (EN ISO 12099:2010) has
11、 been prepared by Technical Committee CEN/TC 327 “Animal feeding stuffs - Methods of sampling and analysis” the secretariat of which is held by NEN, in collaboration with Technical Committee ISO/TC 34 “Food products“. This European Standard shall be given the status of a national standard, either by
12、 publication of an identical text or by endorsement, at the latest by December 2010, and conflicting national standards shall be withdrawn at the latest by December 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or
13、CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Re
14、public, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN ISO 12099:2010ISO 12099:2010(E) ISO 2010 Al
15、l rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Terms and definitions .1 3 Principle2 4 Apparatus.2 5 Calibration and initial validation 2 6 Statistics for performance measurement .4 7 Sampling.11 8 Procedure.11 9 Checking instrument stability 12 10 Running performance check
16、 of calibration 12 11 Precision and accuracy 14 12 Test report14 Annex A (informative) Guidelines for specific NIR standards15 Annex B (informative) Examples of figures16 Annex C (informative) Supplementary terms and definitions 22 Bibliography29 BS EN ISO 12099:2010ISO 12099:2010(E) iv ISO 2010 All
17、 rights reservedForeword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subje
18、ct for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC
19、) on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committe
20、es are circulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be h
21、eld responsible for identifying any or all such patent rights. ISO 12099 was prepared by the European Committee for Standardization (CEN) Technical committee TC 327, Animal feeding stuffs Methods of sampling and analysis, in collaboration with ISO Technical Committee TC 34, Food products, Subcommitt
22、ee SC 10, Animal feeding stuffs, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna agreement). BS EN ISO 12099:2010ISO 12099:2010(E) ISO 2010 All rights reserved vIntroduction This International Standard has been drafted using, as a basis, ISO 21543IDF 20115, prep
23、ared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products, and the International Dairy Federation (IDF). BS EN ISO 12099:2010BS EN ISO 12099:2010INTERNATIONAL STANDARD ISO 12099:2010(E) ISO 2010 All rights reserved 1Animal feeding stuffs, cereals and milled cere
24、al products Guidelines for the application of near infrared spectrometry 1 Scope This International Standard gives guidelines for the determination by near infrared spectroscopy of constituents such as moisture, fat, protein, starch, and crude fibre as well as parameters such as digestibility in ani
25、mal feeding stuffs, cereals and milled cereal products. The determinations are based on spectrometric measurement in the near infrared spectral region. 2 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 2.1 near infrared instrument NIR
26、 instrument apparatus which, when used under specified conditions, predicts constituent contents (2.3) and technological parameters (2.4) in a matrix through relationships to absorptions in the near infrared range NOTE In the context of this International Standard, the matrices are animal feeding st
27、uffs, cereals and milled cereal products. 2.2 animal feeding stuff any substance or product, including additives, whether processed, partially processed or unprocessed, intended to be used for oral feeding to animals EXAMPLES Raw materials, fodder, animal flour, mixed feed and other end products, an
28、d pet food. 2.3 constituent content mass fraction of substances determined using the appropriate, standardized or validated chemical method NOTE 1 The mass fraction is often expressed as a percentage. NOTE 2 Examples of constituents determined include moisture, fat, protein, crude fibre, neutral det
29、ergent fibre, and acid detergent fibre. For appropriate methods, see, e.g., References 1 to 16. 2.4 technological parameter property or functionality of a matrix that can be determined using the appropriate standardized or validated method(s) EXAMPLE Digestibility. NOTE 1 In the context of this Inte
30、rnational Standard, the matrices are animal feeding stuffs, cereals and milled cereal products. BS EN ISO 12099:2010ISO 12099:2010(E) 2 ISO 2010 All rights reservedNOTE 2 It is possible to develop and validate NIR methods for other parameters and matrices than listed, as long as the procedure from t
31、his International Standard is observed. The measuring units of the parameters determined have to follow the units used in the reference methods. 3 Principle Spectral data in the near infrared (NIR) region are collected and transformed to constituent or parameter concentrations by calibration models
32、developed on representative samples of the products concerned. 4 Apparatus 4.1 Near-infrared instruments, based on diffuse reflectance or transmittance measurement covering the NIR wavelength region, 770 nm to 2 500 nm (12 900 cm1to 4 000 cm1), or segments of this or at selected wavelengths or waven
33、umbers. The optical principle may be dispersive (e.g. grating monochromators), interferometric or non-thermal (e.g. light-emitting diodes, laser diodes, and lasers). The instrument should be provided with a diagnostic test system for testing photometric noise and reproducibility, wavelength or waven
34、umber accuracy and wavelength or wavenumber precision (for scanning spectrophotometers). The instrument should measure a sufficiently large sample volume or surface to eliminate any significant influence of inhomogeneity derived from chemical composition or physical properties of the test sample. Th
35、e sample pathlength (sample thickness) in transmittance measurements should be optimized according to the manufacturers recommendation with respect to signal intensity for obtaining linearity and maximum signal/noise ratio. In reflectance measurements, a quartz window or other appropriate material t
36、o eliminate drying effects should preferably cover the interacting sample surface layer. 4.2 Appropriate milling or grinding device, for preparing the sample (if needed). NOTE Changes in grinding or milling conditions can influence NIR measurements. 5 Calibration and initial validation 5.1 General T
37、he instrument has to be calibrated before use. Because a number of different calibration systems can be applied with NIR instruments, no specific procedure can be given for calibration. For an explanation of methods for calibration development see, for example, Reference 17 and appropriate manufactu
38、rers manuals. For the validation, it is important to have a sufficient number of representative samples, covering variations such as: a) combinations and composition ranges of major and minor sample components; b) seasonal, geographic and genetic effects on forages, feed raw materials and cereals; c
39、) processing techniques and conditions; d) storage conditions; e) sample and instrument temperature; f) instrument variations (differences between instruments). NOTE For a solid validation at least 20 samples are needed. BS EN ISO 12099:2010ISO 12099:2010(E) ISO 2010 All rights reserved 35.2 Referen
40、ce methods Internationally accepted reference methods for determination of moisture, fat, protein, and other constituents and parameters should be used. See References 1 to 16 for examples. The reference method used for calibration should be in statistical control, i.e. for any sample, the variabili
41、ty should consist of random variations of a reproducible system. It is essential to know the precision of the reference method. 5.3 Outliers In many situations, statistical outliers are observed during calibration and validation. Outliers may be related to NIR data (spectral outliers, hereafter refe
42、rred to as x-outliers) or errors in reference data or samples with a different relationship between reference data and NIR data (hereafter referred to as y-outliers) (see Figures B.1 to B.5). For the purpose of validation, samples are not to be regarded as outliers if: a) they are within the working
43、 range of the constituents/parameters in the calibration(s); b) they are within the spectral variation of the calibration samples, e.g. as estimated by Mahalanobis distance; c) the spectral residual is below a limit defined by the calibration process; d) the prediction residual is below a limit defi
44、ned by the calibration process. If a sample appears as an outlier then it should be checked initially to see if it is an x-outlier. If it exceeds the x-outlier limits defined for the calibration it should be removed. If it is not an x-outlier, then both the reference value and the NIR predicted valu
45、e should be checked. If these confirm the original values then the sample should not be deleted and the validation statistics should include this sample. If the repeat values show that either the original reference values or the NIR predicted ones were in error then the new values should be used. 5.
46、4 Validation of calibration models 5.4.1 General Before use, calibration equations shall be validated locally on an independent test set that is representative of the sample population to be analysed. For the determination of bias, at least 10 samples are needed; for the determination of standard er
47、ror of prediction (SEP, see 6.5) at least 20 samples are needed. Validation shall be carried out for each sample type, constituent or parameter, and temperature. The calibration is valid only for the variations, i.e. sample types, range and temperature, used in the validation. Results obtained on th
48、e independent test set are plotted, reference against NIR, and residuals against reference results, to give a visual impression of the performance of the calibration. The SEP is calculated (see 6.5) and the residual plot of data corrected for mean systematic error (bias) is examined for outliers, i.
49、e. samples with a residual exceeding 3sSEP. If the validation process shows that the model cannot produce acceptable statistics, then it should not be used. NOTE What is acceptable depends on such criteria as the performance of the reference method, the range covered, and the purpose of the analysis and is up to the parties involved to decide. The next step is to fit NIR data, yNIR, and reference data, yref, by linear regression (yref= byNIR+ a) to produce statistics that describe the validation results. BS EN ISO 12099:2010ISO
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