CEN/TR 17474:2020

Cereals (wheat and barley) - Technical Report of the interlaboratory studies for the determination of moisture and protein in whole kernels by near infrared spectroscopy

This document defines the repeatability and the reproducibility of a method using near infrared spectroscopy in whole kernels for the determination of moisture and protein on wheat and barley. The performance of the method (accuracy) is found in EN 15948.
The values derived from the report are applicable to the following concentration ranges:
-  for wheat:
-   moisture content range from 9,5 % - 15,7 %;
-   protein content range from 10,0 % DM to 18,6 % DM;
-  for barley:
-   moisture content range from 10,6 % - 15,9 %;
-   protein content range from 9,2 % DM - 15,4 % DM.

Getreide - Technischer Bericht des Ringtestversuchs zur Bestimmung des Feuchte- und Proteingehalts von ganzen Körnern mittels Nahinfrarotspektroskopie

Céréales (blé et orge) - Rapport technique des essais interlaboratoires pour la détermination de la teneur en eau et en protéines par spectroscopie proche infrarouge sur des grains entiers

Le présent document définit la répétabilité et la reproductibilité d’une méthode utilisant la spectroscopie proche infrarouge sur des grains entiers pour la détermination de la teneur en eau et en protéines du blé et de l’orge. Les performances de la méthode (exactitude) sont présentées dans l’EN 15948.
Les valeurs dérivées du rapport sont applicables dans les plages de concentration suivantes :
- pour le blé :
- teneur en eau comprise dans une plage de 9,5 % à 15,7 % ;
- teneur en protéines comprise dans une plage de 10,0 % MS à 18,6 % MS ;
- pour l'orge :
- teneur en eau comprise dans une plage de 10,6 % à 15,9 % ;
- teneur en protéines comprise dans une plage de 9,2 % MS à 15,4 % MS.

Žito (pšenica in ječmen) - Tehnično poročilo medlaboratorijskih študij o ugotavljanju vlage in proteinov v celih zrnih z uporabo bližnje infrardeče spektroskopije

General Information

• Status: Published
• Publication Date: 08-Dec-2020
• ICS: 67.060 - Cereals, pulses and derived products
• Technical Committee: CEN/TC 338 - Cereal and cereal products
• Drafting Committee: CEN/TC 338 - Cereal and cereal products
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 09-Dec-2020
• Due Date: 24-Dec-2020
• Completion Date: 09-Dec-2020
• Ref Project: SIST-TP CEN/TR 17474:2021 - Cereals (wheat and barley) - Technical Report of the interlaboratory studies for the determination of moisture and protein in whole kernels by near infrared spectroscopy

Standards Content (Sample)

SLOVENSKI STANDARD
01-februar-2020
Žito (pšenica in ječmen) - Tehnično poročilo medlaboratorijskih študij o
ugotavljanju vlage in proteinov v celih zrnih z uporabo bližnje infrardeče
spektroskopije
Cereals (wheat and barley) - Technical Report of the interlaboratory studies for the
determination of moisture and protein in whole kernels by near infrared spectroscopy
Getreide - Technischer Bericht des Ringtestversuchs zur Bestimmung des Feuchte- und
Proteingehalts von ganzen Körnern
Céréales (blé et orge) - Rapport technique des essais interlaboratoires pour la
détermination de la teneur en eau et en protéines par spectroscopie proche infrarouge
sur des grains entiers
Ta slovenski standard je istoveten z: CEN/TR 17474:2020
ICS:
67.060 Žita, stročnice in proizvodi iz Cereals, pulses and derived
njih products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

CEN/TR 17474
TECHNICAL REPORT
RAPPORT TECHNIQUE
December 2020
TECHNISCHER BERICHT
ICS 67.060
English Version
Cereals (wheat and barley) - Technical Report of the
interlaboratory studies for the determination of moisture
and protein in whole kernels by near infrared
spectroscopy
Céréales (blé et orge) - Rapport technique des essais Getreide - Technischer Bericht des Ringtestversuchs
interlaboratoires pour la détermination de la teneur en zur Bestimmung des Feuchte- und Proteingehalts von
eau et en protéines par spectroscopie proche ganzen Körnern mittels Nahinfrarotspektroskopie
infrarouge sur des grains entiers

This Technical Report was approved by CEN on 2 March 2020. It has been drawn up by the Technical Committee CEN/TC 338.

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, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 17474:2020 E
worldwide for CEN national Members.

Contents Page
European foreword . 3
Introduction . 4
1 Scope . 5
2 Normative references . 5
3 Terms and Definitions. 5
4 Interlaboratory tests . 5
4.1 FOSS . 5
4.2 CHOPIN Technologies . 10
4.3 PERTEN Instruments AB. 18
5 Global treatment . 22
5.1 General. 22
5.2 Precision Data for protein . 22
5.2.1 Wheat . 22
5.2.2 Barley . 23
5.3 Precision Data for moisture . 25
5.3.1 Wheat . 25
5.3.2 Barley . 26
Annex A (informative) Validation of ANN prediction model WB003034 . 28
Annex B  . 32
(informative) Validation of Infraneo prediction models
Annex C (informative) Validation of Inframatic 9500 prediction models . 38
Bibliography . 45
European foreword
This document (CEN/TR 17474:2020) has been prepared by Technical Committee CEN/TC 338 “Cereal
and cereal products”, the secretariat of which is held by AFNOR.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Introduction
The determination of moisture and protein content in whole kernels of barley and wheat can be done
using a near infrared spectrometer.
This document presents the results of 3 interlaboratory tests implementing this routine method and
their overall statistical treatment.
The outcomes have been used to fix the precision (repeatability and reproducibility) of EN 15948,
“Cereals — Determination of moisture and protein - Method using near infrared spectroscopy in whole
kernels”.
The 3 interlaboratory tests have been managed by FOSS Analytical AB (Sweden) in 2008, by CHOPIN
Technologies (France) in 2012 and by PERTEN Instruments AB (Sweden), a PerkinElmer company, in
2013 in accordance with ISO 5725-2.
1 Scope
This document defines the repeatability and the reproducibility of a method using near infrared
spectroscopy in whole kernels for the determination of moisture and protein on wheat and barley. The
performance of the method (accuracy) is found in EN 15948.
The values derived from the report are applicable to the following concentration ranges:
— for wheat:
— moisture content range from 9,5 % – 15,7 %;
— protein content range from 10,0 % DM to 18,6 % DM;
— for barley:
— moisture content range from 10,6 % – 15,9 %;
— protein content range from 9,2 % DM – 15,4 % DM.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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 15948, Cereals - Determination of moisture and protein - Method using Near-Infrared Spectroscopy in
whole kernels
ISO 5725-1, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
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
EN ISO 12099, Animal feeding stuffs, cereals and milled cereal products - Guidelines for the application of
near infrared spectrometry (ISO 12099)
3 Terms and Definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— IEC Electropedia: available at http://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp
4 Interlaboratory tests
4.1 FOSS
An interlaboratory test, organized by the FOSS Analytical AB (Sweden) company in 2008, involving 20
participants from 12 countries was carried out on 6 wheat and 4 barley samples from the 2007 harvest,
containing protein and moisture in various concentrations. The participants were the master
laboratories of European grain networks. The grain networks did also assist in the collection of the
samples (Table 1).
Table 1 — Samples for the interlaboratory study organized by FOSS Analytical
Sample Description Country of origin
B1 Spring barley (2-row, malting barley) UK
B2 Spring barley (2-row, feed barley) Denmark
B3 Spring barley (2-row, malting barley) Denmark
B4 Winter barley (6-row, malting barley) France
W1 Spring wheat (hard) Germany
W2 Spring wheat (hard) France
W3 Winter wheat (hard) UK
W4 Spring wheat (soft) Germany
W5 Winter wheat (hard) Italy
W6 Durum wheat Italy
The prediction model used for the interlaboratory test is WB003034.
This ANN prediction model for the simultaneous prediction of protein and moisture contents in whole
grain of wheat and barley is based on thousands of samples and has been validated according to
EN ISO 12099 by FOSS Analytical AB (Sweden) using independent test sets of wheat and barley
samples, originating from different parts of the world and analysed by different laboratories using the
reference methods given in bibliography. The performance (accuracy) is in accordance with EN 15948,
all the details about the prediction model are given in Annex A.
The results of the interlaboratory test were subjected to statistical analysis in accordance with
ISO 5725-1 and ISO 5725-2 to calculate the precision data shown in Tables 2 to 5 and Figures 1 and 2.
Table 2 — Results of statistical analysis for the determination of the protein content in wheat by
the ANN model WB003034
Sample WG 1 WG 2 WG 3 WG 4 WG 5 WG 6
Number of laboratories 20 20 20 20 20 20
Mean predicted protein content (%DM) 16,883 11,789 13,047 10,876 14,985 14,173
Repeatability standard deviation s (%DM) a
0,159a 0,113a 0,099 0,106 0,087
r 0,109
Repeatability relative stand. dev. s (%)
0,943 0,958 0,76 0,979 0,583 0,771
r
Repeatability limit r [ r = 2,77 × s ] (%DM)
0,440 0,313 0,274 0,294 0,241 0,302
r
Reproducibility stand. dev. s (%DM)
0,159 0,113 0,107 0,143 0,125 0,109
R
Reproducibility relative stand. dev. s (%)
0,943 0,958 0,819 1,317 0,834 0,771
R
Reproducibility limit R [R = 2,77x s ] (%DM)
0,440 0,313 0,296 0,396 0,346 0,302
R
b
16,88 11,75 13,08 10,86 14,93 14,50
Best estimate of true protein value (%DM)
Critical difference (n = 2), reference methods 0,31 0,22 0,22 0,34 0,30 0,21
Deviation predicted - true value (%DM) 0,01 0,04 0,03 0,01 0,06 0,33
a
s > s , s set to be equal s .
r R R r
b
Average protein value (after elimination of outliers) generated by 17 Master laboratories of the European grain
networks, using Kjeldahl (EN ISO 20483 or EN ISO 5983-2) and Dumas (EN ISO 16634-2) methods.
Table 3 — Results of statistical analysis for the determination of the protein content in barley by
the ANN model WB003034
Sample B 1 B 2 B 3 B 4
Number of laboratories 20 20 20 20
Mean predicted protein content (%DM) 10,964 13,05 11,15 12,772
Repeatability standard deviation s (%DM) a
0,198a 0,169a 0,123
r 0,343
Repeatability relative stand. dev. s (%)
1,804 1,292 1,105 2,682
r
Repeatability limit r [ r = 2,77 × s ] (%DM)
0,548 0,468 0,341 0,95
r
Reproducibility stand. dev. s (% DM)
0,198 0,169 0,151 0,343
R
Reproducibility relative stand. dev. s (%)
1,804 1,292 1,352 2,682
R
Reproducibility limit R [R = 2,77 x s ]
R
0,548 0,468 0,418 0,950
(%DM)
Best estimate of true protein value
10,66 13,11 11,27 12,97
b
(%DM)
Critical difference (n = 2), reference
0,39 0,33 0,34 0,67
methods
Deviation predicted - true value (%DM) 0,30 −0,06 −0,12 −0,20
a
s > s , s set to be equal s .
r R R r
b
Average protein value (after elimination of outliers) generated by 17 Master laboratories of the European
grain networks, using Kjeldahl (EN ISO 20483 or EN ISO 5983-2) and Dumas (EN ISO 16634-2) methods.
Key
X protein content (%DM)
Y s (%DM)
1 s
r
2 S
R
3 Linear (s )
r
4 Linear (s )
R
Figure 1 — Standard deviations for the repeatability, s , and reproducibility, s , as a function of
r R
the protein content (wheat and barley)
Table 4 — Results of statistical analysis for the determination of the moisture content in wheat
by the ANN model WB003034
Sample WG 1 WG 2 WG 3 WG 4 WG 5 WG 6
Number of laboratories 20 20 20 20 20 20
Mean predicted moisture content (%) 14,125 13,415 13,978 13,764 11,102 11,074
Repeatability standard dev s (%)
0,024 0,025 0,030 0,016 0,015 0,019
r
Repeatability relative stand. dev. s (%)
0,170 0,187 0,215 0,116 0,138 0,167
r
Repeatability limit r [r = 2,77 × s ] (%)
0,066 0,069 0,083 0,044 0,042 0,053
r
Reproducibility stand. dev. s (%)
0,077 0,07 0,090 0,079 0,045 0,047
R
Reproducibility relative stand. dev. s (%)
0,546 0,523 0,642 0,573 0,405 0,422
R
Reproducibility limit R [R
...