SIST EN 15948:2012
(Main)Cereals - Determination of moisture and protein - Method using Near-Infrared-Spectroscopy in whole kernels
Cereals - Determination of moisture and protein - Method using Near-Infrared-Spectroscopy in whole kernels
This European Standard defines a routine method for the determination of moisture and protein in whole kernels of barley and wheat using a near-infrared spectrophotometer in the constituent ranges: for wheat: - moisture content minimum range from 8 % to 22 %; - protein content minimum range from 7 % to 20 %. for barley: - moisture content minimum range from 8 % to 22 %; - protein content minimum range from 7 % to 16 %. This European Standard describes the modalities to be implemented by the supplier (5.3 and 5.4) and the user of the method.
Getreide - Bestimmung der Feuchte und des Proteins - Verfahren der Nahinfrarot-Spektroskopie bei ganzen Körnern
Diese Europäische Norm legt ein routinemäßiges Verfahren für die Bestimmung der Feuchte und des Proteins in ganzen Gersten und Weizenkörnern unter Anwendung eines Nahinfrarot-Spektrophotometers in den folgenden Bestandteilbereichen fest:
Für Weizen:
- Feuchtegehalt mindestens von 8 % bis 22 %;
- Proteingehalt mindestens von 7 % bis 20 %.
Für Gerste:
- Feuchtegehalt mindestens von 8 % bis 22 %;
- Proteingehalt mindestens von 7 % bis 16 %.
In der vorliegenden Europäischen Norm sind die Modalitäten beschrieben, die vom Lieferanten (5.3 und 5.4) und vom Anwender des Verfahrens umzusetzen sind.
Céréales - Détermination de la teneur en eau et en protéines - Méthode utilisant la spectroscopie dans le proche infrarouge sur des grains entiers
La présente norme spécifie une méthode de routine pour la détermination simultanée de la teneur en eau et en protéines dans des grains entiers d'orge et de blé à l'aide d’un spectrophotomètre dans le proche infrarouge en combinaison avec un modèle de prédiction basé sur un réseau neuronal artificiel et une base de données associées.
Žito - Določanje vlage in beljakovin - Metoda z uporabo bližnje infrardeče spektroskopije v celih zrnih
Ta evropski standard določa rutinsko metodo za določanje vlage in beljakovin v celih zrnih ječmena in pšenice z bližnjim infrardečim spektrometrom v razponu sestavin, in sicer za pšenico: – minimalni obseg vsebnosti vlage od 8 % do 22 %, – minimalni obseg vsebnosti beljakovin od 7 % do 20 %; za ječmen: – minimalni obseg vsebnosti vlage od 8 % do 22 %, – minimalni obseg vsebnosti beljakovin od 7 % do 16 %. Ta evropski standard opisuje modalitete, ki jih morata izvesti dobavitelj (točki 5.3 in 5.4) in uporabnik metode.
General Information
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Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.QIUDUGHþHGetreide - Bestimmung der Feuchte und des Proteins - Verfahren der Nahinfrarot-Spektroskopie bei ganzen KörnernCéréales - Détermination de la teneur en eau et en protéines - Méthode utilisant la spectroscopie dans le proche infrarouge sur des grains entiersCereals - Determination of moisture and protein - Method using Near-Infrared-Spectroscopy in whole kernels67.060QMLKCereals, pulses and derived productsICS:Ta slovenski standard je istoveten z:EN 15948:2012SIST EN 15948:2012en,fr,de01-september-2012SIST EN 15948:2012SLOVENSKI
STANDARD
SIST EN 15948:2012
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 15948
March 2012 ICS 67.060 English Version
Cereals - Determination of moisture and protein - Method using Near-Infrared-Spectroscopy in whole kernels
Céréales - Détermination de la teneur en eau et en protéines - Méthode utilisant la spectroscopie dans le proche infrarouge sur des grains entiers
Getreide - Bestimmung der Feuchte und des Proteins - Verfahren der Nahinfrarot-Spektroskopie bei ganzen Körnern This European Standard was approved by CEN on 28 January 2012.
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-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 translation 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, Finland, 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
COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre:
Avenue Marnix 17,
B-1000 Brussels © 2012 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 15948:2012: ESIST EN 15948:2012
EN 15948:2012 (E) 2 Contents Page Foreword .31Scope .42Normative references .43Terms and definitions .44Principle .45Method of analysis.45.1General .45.2Near Infrared Instrument .55.3Prediction models .55.4Initial validation of the model .55.5Update of calibration model and validation of new model .66Sampling .67Procedure .67.1Preparation of the test sample .67.2Measurement .67.3Local validation of the method .67.4Periodical adjustment of the instrument .77.5Checking instrument stability .77.6Follow up of method performance .78Calculation and expression of results .79Accuracy and precision of the method .89.1Accuracy .89.2Precision .810Test Report . 10Annex A (informative)
Results of an example of interlaboratory test . 11Annex B (informative)
Validation of ANN prediction model WB003034 . 16Bibliography . 20 SIST EN 15948:2012
EN 15948:2012 (E) 3 Foreword This document (EN 15948:2012) has been prepared by Technical Committee CEN/TC 338 “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 September 2012, and conflicting national standards shall be withdrawn at the latest by September 2012. 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. 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 Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 15948:2012
EN 15948:2012 (E) 4 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-infrared spectrophotometer in the constituent ranges: for wheat: moisture content minimum range from 8 % to 22 %; protein content minimum range from 7 % to 20 %. for barley: moisture content minimum range from 8 % to 22 %; protein content minimum range from 7 % to 16 %. This European Standard 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 edition 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 (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 Principle 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 nonlinear regression modelling is used to relate NIR spectra to moisture or protein concentrations determined by officially 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. SIST EN 15948:2012
EN 15948:2012 (E) 5 5.2 Near Infrared Instrument Based on diffuse reflectance or transmittance measurement covering the wavelength region of 700 nm–2500 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 grain 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 model 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 technique, 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 EN ISO standards previously cited (Clause 2). The purpose of validation is to determine the root mean square error 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 initial 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 samples 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 effects over at least a three year period, temperature effects, instrument variation and the variability of reference data shall be included in the set. SIST EN 15948:2012
EN 15948:2012 (E) 6 5.4.3 Initial validation performances The results of the initial validation shall at least fulfil the specifications 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 data set Min 8,0 % 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 robustness 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 introduced 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 (5.3) 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 [2]. It is important that the sample analyzed in routine is truly representative for the batch and has not been damaged or modified. 7 Procedure 7.1 Preparation of the test sample No specific sample preparation is required. 7.2 Measurement Follow the instructions of the instrument manufacturer. 7.3 Local validation of the method Before use, the method shall be validated on an independent test set that is representative of the sample population to be analyzed. For the determination of bias, at least 10 samples are needed; for the determination of Standard Error of Prediction (SEP, see EN ISO 12099:2010, Clause 6.5) at least 20 samples SIST EN 15948:2012
EN 15948:2012 (E) 7 are needed. Validation shall be carried out for each sample type, constituent/ parameter and temperature (see EN ISO 12099:2010, Clause 5.4). Bias or inherent systematic error, as described in EN ISO 12099:2010 (Clause 6), is exhibited when the predicted results of a specific sample group or product show a mean offset value when compared to their reference values. This may occur with unique sample types. The bias (i.e. mean difference between the chemical analysis results and the predicted results) may or may not be statistically significant. Based on the procedure described in EN ISO 12099, a bias confidence limit can be calculated. When this limit is exceeded, a bias is implemented in the instrument software and the validation process repeated. Refer to the manufacturer instructions and to EN ISO 12099 for procedure. 7.4 Periodical adjustment of the instrument To ensure its accuracy, each instrument shall be checked at least annually, against the reference method, either directly or through a master instrument. The execution of this check shall be performed on samples covering
a range as wide as possible, taking into account seasonal, geographic and genetic variations. The number of samples for the adjustment should be sufficient for the statistics used to check the performance. For the determination of the bias, at least 10 samples are needed, for the determination of standard error of prediction (SEP) and for the slope adjustment, at least 20 samples are needed. 7.5 Checking instrument stability See Clause 9 of EN ISO 12099:2010. 7.6 Follow up of method performance Performance of the method shall be checked at least annually, against reference methods to secure the constant adequacy of the model with the requirements of this standard (see 5.3.2). This performance test shall be
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SLOVENSKI STANDARD
oSIST prEN 15948:2011
01-marec-2011
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Cereals - Determination of moisture and protein - Method using Near-Infrared-
Transmittance in Method using Near-Infrared-Spectroscopy in whole kernels
Getreide - Bestimmung der Feuchte und des Proteins - Verfahren der Ganzkorn-
Nahinfrarot-Transmission bei einer Nahinfrarot-Spektroskopie-Methode
Céréales - Détermination de la teneur en eau et en protéines - Méthode utilisant la
transmission dans le proche infrarouge issue de la méthode utilisant la spectroscopie
dans le proche infrarouge sur des grains entiers
Ta slovenski standard je istoveten z: prEN 15948
ICS:
67.060 äLWDVWURþQLFHLQSURL]YRGLL] Cereals, pulses and derived
QMLK products
oSIST prEN 15948:2011 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 15948:2011
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oSIST prEN 15948:2011
EUROPEAN STANDARD
DRAFT
prEN 15948
NORME EUROPÉENNE
EUROPÄISCHE NORM
January 2011
ICS 67.060
English Version
Cereals - Determination of moisture and protein - Method using
Near-Infrared-Transmittance in Method using Near-Infrared-
Spectroscopy in whole kernels
Céréales - Détermination de la teneur en eau et en Getreide - Bestimmung der Feuchte und des Proteins -
protéines - Méthode utilisant la transmission dans le proche Verfahren der Ganzkorn-Nahinfrarot-Transmission bei einer
infrarouge issue de la méthode utilisant la spectroscopie Nahinfrarot-Spektroskopie-Methode
dans le proche infrarouge sur des grains entiers
This draft European Standard is submitted to CEN members for second enquiry. It has been drawn up by the Technical Committee
CEN/TC 338.
If this draft becomes a European Standard, 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.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other language
made by translation 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,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are aware and to
provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without notice and
shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2011 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 15948:2011: E
worldwide for CEN national Members.
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oSIST prEN 15948:2011
prEN 15948:2011 (E)
Contents Page
Foreword .3
1 Scope .3
2 Normative references .3
3 Terms and definitions .3
4 Principle .3
5 Principle .4
5.1 Near Infrared Instrument .4
5.2 Prediction model .4
6 Sampling .4
7 Procedure .4
7.1 Preparation of the test sample .4
7.2 Determination .4
7.3 Performance check of calibration .4
8 Calculation and expression of results .4
9 Validation .5
9.1 Initial validation .5
9.1.1 Validation sample set .5
9.1.2 Initial validation performances .5
9.2 Local validation .5
9.3 Validation during use .6
10 Update of calibration model and validation of new model .6
11 Accuracy and precision .6
11.1 Accuracy .6
11.2 Precision .6
11.3 Repeatability .7
11.4 Reproducibility .7
11.5 Critical difference.7
11.5.1 Comparison of two groups of measurements in one laboratory .7
11.5.2 Comparison of two groups of measurements in two laboratories .7
12 Test Report .8
Annex A (informative) Results of an example of interlaboratory test .9
Annex B (informativ) Validation of ANN prediction model WB003034 . 13
Bibliography . 16
2
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oSIST prEN 15948:2011
prEN 15948:2011 (E)
Foreword
This document (prEN 15948:2011) has been prepared by Technical Committee CEN/TC 338 “Cereal and
cereal products”, the secretariat of which is held by AFNOR.
This document is currently submitted to the second CEN Enquiry.
1 Scope
This standard specifies a routine method for the determination of moisture and protein in whole kernels of
barley and wheat in the constituent ranges of 8 -28% moisture and 7-22% protein using a near-infrared
spectrophotometer.
2 Normative references
The following 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.
EN ISO 712 Cereals and cereal products -- Determination of moisture content -- Routine reference method
EN ISO 5983-2 Animal feeding stuffs -- Determination of nitrogen content and calculation of crude protein
content -- Part 2: Block digestion/steam distillation method
EN ISO 12099 Animal feeding stuff, cereals and milled cereal products — Guidance for the application of near
infrared spectrometry
EN ISO TS 16634-2 Food products - Determination of the total nitrogen content by combustion according to
the Dumas principle and calculation of the crude protein content -- Part 2: Cereals, pulses and milled cereal
products
EN ISO 20483 Cereals and pulses -- Determination of the nitrogen content and calculation of the crude
protein content -- Kjeldahl method
ISO 5725-2 Application of statistics- Accuracy (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
See terms and definitions (Annex C) in EN ISO 12099
4 Principle
The method is based on Near-Infrared (NIR) spectroscopy, a secondary, correlative technique to predict the
concentration of various constituents in organic samples. Linear and nonlinear regression modeling is used to
relate NIR spectra to moisture or protein concentrations determined by officially approved standard methods
(e.g. artificial neural network-ANN, Partial Least Square Regression –PLS,…)
3
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oSIST prEN 15948:2011
prEN 15948:2011 (E)
5 Principle
5.1 Near Infrared Instrument
Based on diffuse reflectance or transmittance measurement covering the wavelength region of 700–2500 nm
or segments of this or at selected wavelengths.
5.2 Prediction model
The model for the prediction of protein and moisture contents in whole grain of wheat and barley is defined by:
the number of samples used for the calibration development
the constituent ranges covered in the model for moisture and protein
the calibration file name associated to each parameter
the seasonal, geographic and genetic varieties covered.
6 Sampling
Sampling is not part of the method specified in this standard. A recommended sampling procedure is given in
EN ISO 24333.
It is important that the sample analyzed is truly representative for the lot and has not been damaged or
changed.
7 Procedure
7.1 Preparation of the test sample
No specific sample preparation is required.
7.2 Determination
Follow the instructions of the instrument manufacturer.
Check the instrument stability as described in EN ISO 12099
7.3 Performance check of calibration
Regularly run a performance check of the calibration model according to EN ISO 12099.
In situations where several instruments have been standardized against each other and are operated in a
network it is sufficient to run the performance check of the calibration on just one instrument.
8 Calculation and expression of results
The software of the instrument calculates the results for moisture and protein and displays them in e.g. % w/w
(g/100g) to 2 decimal places.
If multiple measurements are made on the same sample, calculate the arithmetic mean.
4
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oSIST prEN 15948:2011
prEN 15948:2011 (E)
Express final results to one decimal place.
9 Validation
Since NIR analysis is a secondary, correlative technique, the results must be validated against chemical
analysis reference methods. It is important that the reference methods used are officially approved such as
the EN ISO standards previously cited (clause 2). The purpose of validation is two-fold; determine the overall
correlation of predicted results to the chemical analysis and to evaluate any bias.
2
The linear correlation (R ) between chemical analysis methods and predictions can be compared to calibration
performance specifications and/or historical performance.
9.1 Initial validation
9.1.1 Validation sample set
The initial validation of a calibration model must 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 300 samples coming from 15 countries (20 representative samples min/country) distributed
homogeneously over the entire range,
the part of the range without any reference sample cannot exceed 0.3 % ,
different scans from one sample cannot be considered as different samples,
seasonal and temperature effects, instrument variation must be included in the set
9.1.2 Initial validation performances
The results of the initial validation must fulfill the specifications given in table 1.
Table 1 — NIR performances for the determination of moisture and protein (see Annex B)
Moisture Protein
Overall accuracy expressed as SEP as 0,24 0,27
constituent % w/w
Constituent concentration in Min 8,0 % 7 % d.m.
the independent validation
data set
Max 28 % 22 % d.m.
9.2 Local validation
Before use, the calibration model shall be validated on an independent test set that is representative of the sample
population to be analyzed. For the determination of bias, at least 10 samples are needed; for the determination of
Standard Error of Prediction (SEP, see EN ISO 12099, Clause 6.5) at least 20 samples are neede
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