Sist en 15948 2012

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
iTeh STANDARD PREVIEW

Getreide - Bestimmung der Feuchte und des Proteins - Verfahren der Ganzkorn-
(standards.iteh.ai)
Nahinfrarot-Transmission bei einer Nahinfrarot-Spektroskopie-Methode
Céréales - Détermination de la teneur SISTenENeau et en protéines - Méthode utilisant la

15948:2012
transmission dans le proche infrarouge issue de la méthode utilisant la spectroscopie
https://standards.iteh.ai/catalog/standards/sist/50cbcc9f-713c-4c6f-976e-
dans le proche infrarouge sur des grains entiers
49941244e436/sist-en-15948-2012
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.

(standards.iteh.ai)
SIST EN 15948:2012
49941244e436/sist-en-15948-2012
EUROPEAN STANDARD DRAFT

NORME EUROPÉENNE prEN 15948
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.
(standards.iteh.ai)
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 bodiesSIST ENBelgium,

of Austria, 15948:2012
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.
49941244e436/sist-en-15948-2012
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.
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
9.1.1
Initial validation ......................................................................................................................................5
Validation sample set ............................................................................................................................5
9.1.2
9.2
(standards.iteh.ai)
Initial validation performances .............................................................................................................5
Local validation ......................................................................................................................................5
9.3 Validation during use ............................................................................................................................6
10 SIST EN
Update of calibration model and validation 15948:2012
of new model ................................................................6
11 Accuracy and precision ........................................................................................................................6
11.1 49941244e436/sist-en-15948-2012
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
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
(standards.iteh.ai)
EN ISO 12099 Animal feeding stuff, cereals and milled cereal products — Guidance for the application of near
infrared spectrometry
SIST EN 15948:2012
EN ISO TS https://standards.iteh.ai/catalog/standards/sist/50cbcc9f-713c-4c6f-976e-
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
49941244e436/sist-en-15948-2012
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
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.
(standards.iteh.ai)
7 Procedure
SIST EN 15948:2012
7.1 Preparation of the test sample
49941244e436/sist-en-15948-2012
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
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 % ,
 (standards.iteh.ai)
different scans from one sample cannot be considered as different samples,
 seasonal and temperature effects, instrument variation must be included in the set
SIST EN 15948:2012
9.1.2
Initial validation performances
49941244e436/sist-en-15948-2012
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 needed. Validation must
be carried out for each sample type, constituent/ parameter and temperature (see EN ISO 12099, Clause 5.4).
Bias or inherent systematic error, as described in EN ISO 12099 (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.
5
prEN 15948:2011 (E)
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 (or intercept) is implemented in the instrument software and the validation
process repeated. Refer to the manufacturer instructions and to EN ISO 12099 for procedure.
9.3 Validation during use
See clause 10 in EN ISO 12099.
10 Update of calibration model and validation of new model

The prediction model in accordance with this standard should 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 with the
original validation set including a representative number of samples covering the newly added sample
properties. The new independent test set should include 30% of the new samples, but at least 20 samples.
Annual validation shall be made with samples from an internationally accepted proficieny testing scheme
(PTS) that includes NIRS predicted results and results generated by the reference methods specified in
clause 2.
11 Accuracy and precision iTeh STANDARD PREVIEW

11.1 Accuracy (standards.iteh.ai)
The accuracy of the prediction model is determined by validation in accordance with EN ISO 12099 and
expressed by the Standard Error of PredictionSIST (see EN
table15948:2012
1). The Standard Error of Prediction (SEP) is an
expression of the bias corrected average difference between predicted and reference values predicted by the
model when applied to a set of samples49941244e436/sist-en-15948-2012
not included in the derivation of the model. The values also include
the uncertainty of reference results.
The predicted results will not in more that 5 % of cases deviate more than 1,96 x the above values from the
best estimate of the true value.
NOTE As NIR is an indirect method, the typical standard deviation of reproducibility for the used reference methods
are given here for comparison
 Moisture (EN ISO 712) = 0,16%

 Protein (EN ISO 20483) = 0,20%
 Protein (EN ISO 5983-2) = 0,20%
 Protein (EN ISO/TS 16634-2)= 0,21-0,26%
11.2 Precision
The precision of the prediction model shall be determined from an interlaboratory test organized according to
ISO 5725-2 and at least fulfil the performances of repeatability and reproducibility given below.
Details of an example of interlaboratory test are summarized in Annex A, that is informative.
The figures in Annex A show that the repeatability and the reproducibility are independent of the concentration.
The figures in Annex B show that the dispersion is identical over the validated range. The figures B.1 and B.2
6
prEN 15948:2011 (E)
can therefore be used in the whole validated range, even though the interlaboratory trial covered a smaller
range.
11.3 Repeatability
The absolute difference between two independent single test results, obtained using the same method on
identical test material in the same laboratory by the same operator using the same equipment within a short
interval of time will not in more that 5 % of cases be greater than the repeatability limit r (r=sr*2,8) with:
r (protein) = 0,42
r (moisture) = 0,15
11.4 Reproducibility
The absolute difference between two single test results, obtained using the same method on identical test
material in different laboratories with different operators using different equipment, will not in more that 5 % of
cases be greater than the reproducibility limit R (R=sR*2,8) with:
R (protein) = 0,45
R (moisture) = 0,25
11.5 Critical difference

When the difference between two averaged values obtained from two test results under repeatability or
reproducibility conditions is to be assessed, the repeatability or reproducibility limit cannot be used, one shall
(standards.iteh.ai)
use the Critical Difference (CD)
11.5.1 Comparison of two groups of measurements in one laboratory

SIST EN 15948:2012
The critical https://standards.iteh.ai/catalog/standards/sist/50cbcc9f-713c-4c6f-976e-
difference (CD) between two averaged values obtained from two test results under repeatability
conditions is equal to: 49941244e436/sist-en-15948-2012
where
Sr is the standard deviation of repeatability;
n1 and n2 are the number of test results corresponding to each of the averaged values
CDr (protein) = 0,30
CDr (moisture) = 0,11
11.5.2 Comparison of two groups of measurements in two laboratories
The critical difference (CD) between two averaged values obtained in two different laboratories from two test
results under repeatability conditions is equal to:
7
prEN 15948:2011 (E)
where
Sr is the standard deviation of repeatability;
SR is the standard deviation of reproducibility;
n1 and n2 are the number of test results corresponding to each of the averaged values
CDR (protein) = 0,32
CDR (moisture) = 0,23
12 Test Report
The test report shall specify:
 all information necessary for the complete identification of the sample
 the sampling method used (if known)
 the application model and instrument used with reference to this standard

all operating details not specified in this standard, or regarded as optional, together with details of any
incidents which may have influenced the test result(s)
 the test result(s) obtained (standards.iteh.ai)

SIST EN 15948:2012
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SLOVENSKI STANDARD

oSIST prEN 15948:2011

Cereals - Determination of moisture and protein - Method using Near-Infrared-

iTeh STANDARD PREVIEW

Céréales - Détermination de la teneur SISTenENeau et en protéines - Méthode utilisant la

Ta slovenski standard je istoveten z: prEN 15948

oSIST prEN 15948:2011 en,fr,de

iTeh STANDARD PREVIEW

EUROPEAN STANDARD DRAFT

Cereals - Determination of moisture and protein - Method using

iTeh STANDARD PREVIEW

CEN members are the national standards bodiesSIST ENBelgium,

EUROPEAN COMMITTEE FOR STANDARDIZATION

Management Centre: Avenue Marnix 17, B-1000 Brussels

prEN 15948:2011 (E)

prEN 15948:2011 (E)

This document is currently submitted to the second CEN Enquiry.

iTeh STANDARD PREVIEW

3 Terms and definitions

prEN 15948:2011 (E)

5.1 Near Infrared Instrument

5.2 Prediction model

 the number of samples used for the calibration development

 the calibration file name associated to each parameter

 the seasonal, geographic and genetic varieties covered.

iTeh STANDARD PREVIEW

Follow the instructions of the instrument manufacturer.

Check the instrument stability as described in EN ISO 12099

7.3 Performance check of calibration

8 Calculation and expression of results

prEN 15948:2011 (E)

Express final results to one decimal place.

9.1 Initial validation

9.1.1 Validation sample set

Requirements for the validation sample set are:

Overall accuracy expressed as SEP as 0,24 0,27

Constituent concentration in Min 8,0 % 7 % d.m.

9.2 Local validation

prEN 15948:2011 (E)

9.3 Validation during use

See clause 10 in EN ISO 12099.

10 Update of calibration model and validation of new model

11 Accuracy and precision iTeh STANDARD PREVIEW

 Moisture (EN ISO 712) = 0,16%

Details of an example of interlaboratory test are summarized in Annex A, that is informative.

prEN 15948:2011 (E)

11.5 Critical difference

iTeh STANDARD PREVIEW

11.5.1 Comparison of two groups of measurements in one laboratory

Sr is the standard deviation of repeatability;

CDr (protein) = 0,30

CDr (moisture) = 0,11

11.5.2 Comparison of two groups of measurements in two laboratories

prEN 15948:2011 (E)

Sr is the standard deviation of repeatability;

SR is the standard deviation of reproducibility;

CDR (protein) = 0,32

CDR (moisture) = 0,23

 all information necessary for the complete identification of the sample