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

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 Rapport technique 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) doivent être conformes à
l’EN 15948.
Les valeurs dérivées du rapport sont applicables aux plages de concentration suivantes :
— pour le blé :
¾ teneur en eau comprise dans une plage de 9,5 % à 15,7 % ;
¾ teneur en protéines comprise dans une plage de 10,0 %MS à 18,6 %MS ;
— pour l’orge :
¾ teneur en eau comprise dans une plage de 10,6 % à 15,9 % ;
¾ 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
Public Enquiry End Date
19-Jan-2020
Publication Date
21-Jan-2021
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
18-Dec-2020
Due Date
22-Feb-2021
Completion Date
22-Jan-2021

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Standards Content (Sample)

SLOVENSKI STANDARD
SIST-TP CEN/TR 17474:2021
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
SIST-TP CEN/TR 17474:2021 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TP CEN/TR 17474:2021


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.

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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
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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.
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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.
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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).
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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.
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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.
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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)
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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 = 2,77 × s ] (%)
0,213 0,194 0,249 0,219 0,125 0,130
R
a
14,24 13,61 14,08 13,93 11,35 11,23
Best estimate of true moisture value (%)
Critical difference (n = 2), reference
0,20 0,28 0,26 0,34 0,27 0,56
methods
Deviation predicted - true value (%) −0,11 −0,20 −0,10 −0,17 −0,25 −0,15
a
Average moisture value (after elimination of outliers) generated by 17 Master laboratories of the European
grain networks, using EN ISO 712 method.
Table 5 — Results of statistical analysis for the determination of the moisture content in barley
by the ANN model WB003034
Sample B1 B2 B3 B4
Number of laboratories 20 20 20 20
Mean predicted moisture content (%) 12,417 13,731 14,299 12,986
Repeatability standard dev s (%)
0,103 0,053 0,054 0,213
r
Repeatability relative stand. dev. s (%)
0,827 0,384 0,377 1,639
r
Repeatability limit r [r = 2,77 × s ] (%)
0,285 0,147 0,150 0,590
r
Reproducibility stand. dev. s (%)
0,111 0,071 0,087 0,238
R
Reproducibility relative stand. dev. s (%)
0,896 0,517 0,611 1,836
R
Reproducibility limit R [R = 2,77 × s ] (%)
0,307 0,197 0,241 0,659
R
a
12,51 13,79 14,37 12,83
Best estimate of true moisture value (%)
Critical difference (n = 2), reference
0,14 0,29 0,30 0,16
methods
Deviation predicted - true value (%) −0,09 −0,06 −0,07 0,16
a
Average moisture value (after elimination of outliers) generated by 17 Master laboratories of the European
grain networks, using EN ISO 712 method.
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Key
X moisture (%)
Y s (%)
1 s
r
2 S
R
3 Linear (s )
r
4 Linear (s )
R
Figure 2 — Standard deviations for the repeatability, s , and reproducibility, s , as a function of
r R
the moisture content (wheat and barley)
4.2 CHOPIN Technologies
An interlaboratory test, organized by the CHOPIN Technologies (France) company in 2012, involving 13
participants from 7 countries was carried out on 16 wheat and 15 barley samples from the 2011
harvest, containing protein and moisture in various concentrations. The participants did assist in the
collection of the samples (Table 6 and Table 7).
Table 6 — Wheat Samples for the interlaboratory study organized by CHOPIN
Country of
Sample Description
origin
W1 Common wheat France
W2 Common wheat France
W3 Common wheat France
W4 Common wheat France
W5 Common wheat France
W6 Durum wheat Italy
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Country of
Sample Description
origin
W7 Common wheat Turkey
W8 Common wheat France
W9 Common wheat France
W10 Common wheat France
W11 Durum wheat France
W12 Durum wheat France
W13 Common wheat France
W14 Common wheat France
W15 Common wheat France
W16 Common wheat Argentine
Table 7 — Barley Samples for the interlaboratory study organized by CHOPIN
Country of
Sample Description
origin
B1 Barley France
B2 Spring barley France
B3 Winter barley France
B4 Barley France
B5 Barley France
B6 Barley France
B7 Barley France
B8 Barley France
B9 Barley France
B10 Winter Barley France
B11 Spring barley France
B12 Spring barley France
B13 Barley France
B14 Winter barley Germany
B15 Spring barley Argentine
The Infraneo prediction models for the determination of protein and moisture contents on whole grain
of wheat and barley have been developed on samples worldwide collected and coming from crop year
2006 to 2011.They have been validated according to EN ISO 12099 by CHOPIN Technologies (France)
using independent test sets of wheat and barley samples, originating from different parts of the world,
and analysed on different Infraneo using the reference methods given in bibliography. The performance
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(accuracy) is in accordance with EN 15948, all the details about the four prediction models are given in
Annex B.
The results obtained were subjected to statistical analysis in accordance with ISO 5725-1 and
ISO 5725-2 to calculate the precision data shown in Tables 8 to 16 and Figures 3 to 6.
Table 8 — Results of statistical analysis for the determination of the protein content in wheat by
Infraneo PLS model bl-pro03.cal
Sample W1 W2 W3 W4 W5 W6 W7 W8
Number of laboratories 11 12 11 11 11 11 11 11
Mean predicted protein content (%DM) 10,97 15,45 11,27 12,01 16,55 14,18 10,97 10,99
Repeatability standard deviation s (%DM)
0,064 0,106 0,055 0,079 0,088 0,063 0,091 0,125
r
Repeatability relative stand. dev. s (%)
0,555 0,685 0,492 0,660 0,532 0,443 0,828 1,139
r
Repeatability limit r [r = 2,77 × s ] (%DM)
0,178 0,296 0,155 0,222 0,247 0,176 0,254 0,350
r
Reproducibility stand. dev. s (%DM)
0,115 0,168 0,130 0,130 0,123 0,084 0,133 0,132
R
Reproducibility relative stand. dev. s (%)
1,005 1,086 1,150 1,083 0,742 0,592 1,209 1,203
R
Reproducibility limit R [R = 2,77x s ] (%DM)
0,323 0,470 0,363 0,364 0,344 0,235 0,371 0,370
R
a
11,05 15,10 11,50 11,90 16,35 14,10 11,20 10,85
True protein value (%DM)
Deviation predicted - true value (%DM) −0,08 0,35 −0,23 0,11 0,20 0,08 −0,23 0,14
a
Protein value obtained by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483) method.
Table 9 — Results of statistical analysis for the determination of the protein content in wheat by
Infraneo PLS model bl-pro03.cal
Sample W9 W10 W11 W12 W13 W14 W15 W16
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted protein content (% DM) 9,97 11,92 11,91 13,29 16,34 14,82 13,53 18,55
Repeatability standard deviation s (%DM)
0,101 0,085 0,060 0,080 0,088 0,070 0,101 0,088
r
Repeatability relative stand. dev. s (%)
1,012 0,716 0,502 0,601 0,541 0,469 0,744 0,474
r
Repeatability limit r [r = 2,77 × s ] (%DM)
0,283 0,239 0,168 0,223 0,247 0,195 0,282 0,246
r
Reproducibility stand. dev. s (%DM)
0,136 0,131 0,113 0,119 0,166 0,127 0,118 0,152
R
Reproducibility relative stand. dev. s (%) 1,365 1,100 0,949 0,892 1,018 0,857 0,875 0,820
R
Reproducibility limit R [R = 2,77 × s ] (%DM) 0,381 0,367 0,317 0,332 0,466 0,355 0,332 0,426
R
a
9,95 12,00 12,20 13,45 16,45 15,20 13,45 18,30
True protein value (%DM)
Deviation predicted - true value (%DM) 0,02 −0,08 −0,29 −0,16 −0,11 −0,38 0,08 0,25
a
Protein value obtained by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483) method.
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Key
X protein (%DM)
Y standard deviation (%DM)
1 s
r
2 s
R
3 Linear (s )
r
4 Linear (s )
R
Figure 3 — Standard deviations for the repeatability, s , and reproducibility, s , as a function of
r R
the protein content on wheat samples
Table 10— Results of statistical analysis for the determination of the protein content in barley
by Infraneo PLS model or-pro03.cal
Sample B1 B2 B3 B4 B5 B6 B7 B8
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted protein content (%DM) 10,93 11,80 12,08 10,41 11,74 11,85 10,09 12,52
Repeatability standard deviation s
r
0,096 0,090 0,104 0,086 0,134 0,106 0,119 0,141
(%DM)
Repeatability relative stand. dev. s (%)
0,874 0,762 0,859 0,830 1,139 0,897 1,175 1,127
r
Repeatability limit r [r = 2,77 × s ], (%)
0,267 0,252 0,290 0,242 0,375 0,298 0,332 0,395
r
Reproducibility stand. dev. s (% DM)
0,121 0,101 0,134 0,086 0,162 0,123 0,148 0,208
R
Reproducibility relative stand. dev. s
R
1,104 0,859 1,110 0,830 1,383 1,035 1,469 1,661
(%)
Reproducibility limit R [R = 2,77 × s ]
R
0,338 0,221 0,375 0,242 0,455 0,343 0,415 0,582
(%)
a
11,15 11,70 11,90 10,55 11,75 11,75 10,20 12,30
True protein value (%DM)
Deviation predicted - true value (%DM) −0,22 0,10 0,18 −0,14 −0,01 0,10 −0,11 0,22
a
Protein value obtained by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483) method.
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Table 11 — Results of statistical analysis for the determination of the protein content in barley
by Infraneo PLS model or-pro03.cal
Sample B9 B10 B11 B12 B13 B14 B15
Number of laboratories 11 11 11 11 11 11 11
Mean predicted protein content (% DM) 15,32 10,40 12,73 15,36 11,33 10,79 10,72
Repeatability standard deviation s (%
r
0,095 0,097 0,183 0,156 0,073 0,113 0,105
DM)
Repeatability relative stand. dev. s (%)
0,618 0,883 1,438 1,014 0,648 1,050 0,977
r
Repeatability limit r [r = 2,77 × s ]
r
0,265 0,257 0,513 0,513 0,206 0,317 0,293
(%DM)
Reproducibility stand. dev. s (% DM)
0,256 0,119 0,183 0,183 0,155 0,190 0,147
R
Reproducibility relative stand. dev. s
R
1,674 1,147 1,438 1,192 1,364 1,759 1,371
(%)
Reproducibility limit R [R = 2,77 × s ]
R
0,718 0,337 0,513 0,651 0,433 0,532 0,411
(%DM)
a
15,05 10,40 12,65 15,50 11,65 10,95 10,70
True protein value (%DM)
Deviation predicted - true value (%DM) 0,27 −0,00 0,08 −0,14 −0,32 −0,16 0,02
a
Protein value obtained by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483)
method.

Key
X protein (%DM)
Y standard deviation (%DM)
1 s
r
2 s
R
3 Linear (s )
r
4 Linear (s )
R
Figure 4 — Standard deviations for the repeatability, s , and reproducibility, s , as a function of
r R
the protein content on barley samples
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Table 12 — Results of statistical analysis for the determination of the moisture content in wheat
by Infraneo PLS model bl-hum05.cal
Sample W1 W2 W3 W4 W5 W6 W7 W8
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted moisture content (%) 13,49 12,79 15,47 13,65 13,10 13,61 10,63 14,26
Repeatability standard deviation s
r
0,059 0,033 0,030 0,037 0,035 0,046 0,051 0,060
(%)
Repeatability relative stand. dev. s
r
0,434 0,258 0,195 0,270 0,269 0,341 0,478 0,423
(%)
Repeatability limit r [ r = 2,77 × s ]
r
0,164 0,092 0,084 0,103 0,099 0,130 0,142 0,169
(%)
Reproducibility stand. dev. s (%)
0,096 0,103 0,099 0,075 0,106 0,092 0,085 0,091
R
Reproducibility relative stand. dev. s
R
0,715 0,807 0,641 0,547 0,811 0,680 0,804 0,639
(%)
Reproducibility limit R [R = 2,77 × s ]
R
0,270 0,289 0,278 0,209 0,297 0,259 0,239 0,255
(%)
a
13,80 13,00 15,70 13,70 13,00 13,30 10,70 14,20
True moisture value (%)
Deviation predicted - true value (%) −0,31 −0,16 −0,23 0,00 0,15 0,31 −0,07 0,06
a
Moisture value obtained by 1 Master lab of the European grain networks using ISO 712 method.
Table 13 — Results of statistical analysis for the determination of the moisture content in wheat
by Infraneo PLS model bl-hum05.cal
Sample W9 W10 W11 W12 W13 W14 W15 W16
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted moisture content (%) 12,24 12,49 12,88 10,89 11,21 15,74 13,67 12,16
Repeatability standard deviation s (%)
0,056 0,036 0,047 0,050 0,018 0,035 0,039 0,036
r
Repeatability relative stand. dev. s (%)
0,456 0,287 0,367 0,456 0,161 0,221 0,285 0,300
r
Repeatability limit r [ r = 2,77 × s ] (%) 0,156 0,100 0,132 0,132 0,051 0,097 0,109 0,102
r
Reproducibility stand. dev. s (%) 0,087 0,092 0,082 0,088 0,118 0,108 0,092 0,120
R
Reproducibility relative stand. dev. s 0,707 0,734 0,636 0,811 1,049 0,687 0,674 0,989
R

Reproducibility limit R [R = 2,77 × s ] 0,242 0,257 0,229 0,247 0,330 0,303 0,258 0,337
R

a
12,60 12,50 12,70 11,00 11,00 15,80 13,60 12,05
True moisture value (%)
Deviation predicted - true value (%) −0,31 −0,01 0,23 −0,06 0,26 −0,06 0,12 0,11
a
Moisture value obtained by 1 Master lab of the European grain networks using ISO 712 method.
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Key
X moisture (%)
Y standard deviation (%)
1 s
r
2 s
R
3 Linear (s )
r
4 Linear (s )
R
Figure 5 — Standard deviations for the repeatability, s , and reproducibility, s , as a function of
r R
the moisture content on wheat samples
Table 14 — Results of statistical analysis for the determination of the moisture content in barley
by Infraneo PLS model or-hum05.cal
Sample B1 B2 B3 B4 B5 B6 B7 B8
Number of laboratories 11 11 11 12 11 11 11 11
Mean predicted moisture content (%) 13,30 14,06 13,80 11,89 11,94 14,14 10,60 15,90
Repeatability standard deviation s
r
0,042 0,041 0,046 0,050 0,050 0,041 0,058 0,046
(%)
Repeatability relative stand. dev. s
r
0,312 0,289 0,335 0,422 0,419 0,288 0,547 0,290
(%)
Repeatability limit r [ r = 2,77 × s ]
r
0,116 0,114 0,130 0,140 0,140 0,114 0,162 0,129
(%)
Reproducibility stand. dev. s (%)
0,099 0,079 0,061 0,088 0,064 0,067 0,140 0,127
R
Reproducibility relative stand. dev. s
R
0,747 0,559 0,441 0,737 0,536 0,476 1,323 0,800
(%)
Reproducibility limit R [R = 2,77 × s ]
R
0,278 0,220 0,170 0,245 0,179 0,189 0,393 0,356
(%)
a
13,40 14,10 13,70 12,00 12,10 14,10 10,80 16,00
True moisture value (%)
Deviation predicted - true value (%) −0,10 0,01 0,10 −0,06 −0,16 0,09 −0,15 −0,05
a
Moisture value obtained by 1 Master lab of the European grain networks using ISO 712 method.
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Table 15 — Results of statistical analysis for the determination of the moisture content in barley
by Infraneo PLS model or-hum05.cal
Sample B9 B10 B11 B12 B13 B14 B15
Number of laboratories 11 12 11 11 11 11 11
Mean predicted moisture content (%) 12,50 12,72 13,89 15,70 13,49 11,68 11,13
Repeatability standard deviation s (%)
0,062 0,036 0,052 0,053 0,035 0,049 0,056
r
Repeatability relative stand. dev. s (%)
0,500 0,279 0,377 0,339 0,258 0,419 0,505
r
Repeatability limit r [ r = 2,77 × s ] (%)
0,175 0,099 0,146 0,146 0,098 0,137 0,157
r
Reproducibility stand. dev. s (%)
0,157 0,055 0,069 0,069 0,074 0,080 0,111
R
Reproducibility relative stand. dev. s
R
1,258 0,433 0,499 0,442 0,549 0,688 0,996
(%)
Reproducibility limit R [R = 2,77 × s ]
R
0,440 0,154 0,194 0,384 0,207 0,225 0,310
(%)
a
12,50 12,70 13,60 15,80 13,30 11,80 11,20
True moisture value (%)
Deviation predicted - true value (%) 0,00 0,07 0,29 −0,10 0,19 −0,12 −0,07
a
Moisture value obtained by 1 Master lab of the European grain networks using ISO 712 method.

Key
X moisture (%)
Y standard deviation (%)
1 s
r
2 s
R
3 Linear (s )
r
4 Linear (s )
R
Figure 6 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
the moisture content on barley samples
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4.3 PERTEN Instruments AB
An interlaboratory test, organized by the Perten Instruments AB (Sweden) company in 2013, involving
8 participants from 6 countries was carried out on 6 wheat and 4 barley samples from the 2012 harvest,
containing protein and moisture in various
...

SLOVENSKI STANDARD
kSIST-TP FprCEN/TR 17474:2020
01-januar-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: FprCEN/TR 17474
ICS:
67.060 Žita, stročnice in proizvodi iz Cereals, pulses and derived
njih products
kSIST-TP FprCEN/TR 17474:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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kSIST-TP FprCEN/TR 17474:2020

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kSIST-TP FprCEN/TR 17474:2020


FINAL DRAFT
TECHNICAL REPORT
FprCEN/TR 17474
RAPPORT TECHNIQUE

TECHNISCHER BERICHT

November 2019
ICS
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
infrarouge sur des grains entiers


This draft Technical Report is submitted to CEN members for Vote. 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.

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 Technical Report. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a Technical Report.


EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TR 17474:2019 E
worldwide for CEN national Members.

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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. 17
5 Global treatment . 21
5.1 General. 21
5.2 Precision Data for protein . 21
5.2.1 Wheat . 21
5.2.2 Barley . 22
5.3 Precision Data for moisture . 24
5.3.1 Wheat . 24
5.3.2 Barley . 25
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

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European foreword

This document (FprCEN/TR 17474:2019) 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 Vote on TR.
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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) in 2013 in accordance with
ISO 5725-2.
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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 http://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).
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Table 1 — Samples for the interlaboratory study organized by FOSS Analytical
Country of
Sample Description
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
a
Repeatability standard deviation sr (%DM) 0,159a 0,113a 0,099 0,106 0,087
0,109
Repeatability relative stand. dev. sr (%) 0,943 0,958 0,76 0,979 0,583 0,771
Repeatability limit r [ r = 2,77 × sr ] (%DM) 0,440 0,313 0,274 0,294 0,241 0,302
Reproducibility stand. dev. sR (%DM) 0,159 0,113 0,107 0,143 0,125 0,109
Reproducibility relative stand. dev. sR (%) 0,943 0,958 0,819 1,317 0,834 0,771
Reproducibility limit R [R = 2,77x sR] (%DM) 0,440 0,313 0,296 0,396 0,346 0,302
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
sr > sR, sR set to be equal sr.
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.
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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
a
Repeatability standard deviation sr (%DM) 0,198a 0,169a 0,123
0,343
Repeatability relative stand. dev. sr (%) 1,804 1,292 1,105 2,682
Repeatability limit r [ r = 2,77 × sr ] (%DM) 0,548 0,468 0,341 0,95
Reproducibility stand. dev. sR (% DM) 0,198 0,169 0,151 0,343
Reproducibility relative stand. dev. sR (%) 1,804 1,292 1,352 2,682
Reproducibility limit R [R = 2,77x sR]
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
sr > sR, sR set to be equal sr.
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.
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Key
X protein content (%DM)
Y s (%DM)
1 sr
2 SR
3 Linear (sr)
4 Linear (sR)
Figure 1 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
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 sr (%) 0,024 0,025 0,030 0,016 0,015 0,019
Repeatability relative stand. dev. sr
0,170 0,187 0,215 0,116 0,138 0,167
(%)
Repeatability limit r [r = 2,77 × sr ] (%) 0,066 0,069 0,083 0,044 0,042 0,053
Reproducibility stand. dev. sR (%) 0,077 0,07 0,090 0,079 0,045 0,047
Reproducibility relative stand. dev. sR
0,546 0,523 0,642 0,573 0,405 0,422
(%)
Reproducibility limit R [R = 2,77 × sR]
0,213 0,194 0,249 0,219 0,125 0,130
(%)
Best estimate of true moisture value
14,24 13,61 14,08 13,93 11,35 11,23
a
(%)
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Sample WG 1 WG 2 WG 3 WG 4 WG 5 WG 6
Critical difference (n = 2), reference
0,20 0,28 0,26 0,34 0,27 0,56
methods
Deviation predicted - true value (%) −0,11 −0,20 −0,10 −0,17 −0,25 −0,15
a
Average moisture value (after elimination of outliers) generated by 17 Master laboratories of the European
grain networks, using EN ISO 712 method.
Table 5 — Results of statistical analysis for the determination of the moisture content in barley
by the ANN model WB003034
Sample B1 B2 B3 B4
Number of laboratories 20 20 20 20
Mean predicted moisture content (%) 12,417 13,731 14,299 12,986
Repeatability standard dev sr (%) 0,103 0,053 0,054 0,213
Repeatability relative stand. dev. sr (%) 0,827 0,384 0,377 1,639
Repeatability limit r [r = 2,77 × sr ] (%) 0,285 0,147 0,150 0,590
Reproducibility stand. dev. sR (%) 0,111 0,071 0,087 0,238
Reproducibility relative stand. dev. sR
0,896 0,517 0,611 1,836
(%)
Reproducibility limit R [R = 2,77 × sR]
0,307 0,197 0,241 0,659
(%)
Best estimate of true moisture value
12,51 13,79 14,37 12,83
a
(%)
Critical difference (n = 2), reference
0,14 0,29 0,30 0,16
methods
Deviation predicted - true value (%) −0,09 −0,06 −0,07 0,16
a
Average moisture value (after elimination of outliers) generated by 17 Master laboratories of the European
grain networks, using EN ISO 712 method.
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Key
X moisture (%)
Y s (%)
1 sr
2 SR
3 Linear (sr)
4 Linear (sR)
Figure 2 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
the moisture content (wheat and barley)
4.2 CHOPIN Technologies
An interlaboratory test, organized by the CHOPIN Technologies (France) company in 2012, involving 13
participants from 7 countries was carried out on 16 wheat and 15 barley samples from the 2011
harvest, containing protein and moisture in various concentrations. The participants did assist in the
collection of the samples (Table 6 and Table 7).
Table 6 — Wheat Samples for the interlaboratory study organized by CHOPIN
Country of
Sample Description
origin
W1 Common wheat France
W2 Common wheat France
W3 Common wheat France
W4 Common wheat France
W5 Common wheat France
W6 Durum wheat Italy
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Country of
Sample Description
origin
W7 Common wheat Turquey
W8 Common wheat France
W9 Common wheat France
W10 Common wheat France
W11 Durum wheat France
W12 Durum wheat France
W13 Common wheat France
W14 Common wheat France
W15 Common wheat France
W16 Common wheat Argentine
Table 7 — Barley Samples for the interlaboratory study organized by CHOPIN
Country of
Sample Description
origin
B1 Barley France
B2 Spring barley France
B3 Winter barley France
B4 Barley France
B5 Barley France
B6 Barley France
B7 Barley France
B8 Barley France
B9 Barley France
B10 Winter Barley France
B11 Spring barley France
B12 Spring barley France
B13 Barley France
B14 Winter barley Germany
B15 Spring barley Argentine
The Infraneo prediction models for the determination of protein and moisture contents on whole grain
of wheat and barley have been developed on samples worldwide collected and coming from crop year
2006 to 2011.They have been validated according to EN ISO 12099 by CHOPIN Technologies (France)
using independent test sets of wheat and barley samples, originating from different parts of the world,
and analysed on different Infraneo using the reference methods given in bibliography. The performance
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(accuracy) is in accordance with EN 15948, all the details about the four prediction models are given in
Annex B.
The results obtained were subjected to statistical analysis in accordance with ISO 5725-1 and
ISO 5725-2 to calculate the precision data shown in Tables 8 to 16 and Figures 3 to 6.
Table 8 — Results of statistical analysis for the determination of the protein content in wheat by
Infraneo PLS model bl-pro03.cal
Sample W1 W2 W3 W4 W5 W6 W7 W8
Number of laboratories 11 12 11 11 11 11 11 11
Mean predicted protein content (%DM) 10,97 15,45 11,27 12,01 16,55 14,18 10,97 10,99
Repeatability standard deviation sr (%DM) 0,064 0,106 0,055 0,079 0,088 0,063 0,091 0,125
Repeatability relative stand. dev. sr (%) 0,555 0,685 0,492 0,660 0,532 0,443 0,828 1,139
Repeatability limit r [r = 2,77 × sr ] (%DM) 0,178 0,296 0,155 0,222 0,247 0,176 0,254 0,350
Reproducibility stand. dev. sR (%DM) 0,115 0,168 0,130 0,130 0,123 0,084 0,133 0,132
Reproducibility relative stand. dev. sR (%) 1,005 1,086 1,150 1,083 0,742 0,592 1,209 1,203
Reproducibility limit R [R = 2,77x sR] (%DM) 0,323 0,470 0,363 0,364 0,344 0,235 0,371 0,370
a
11,05 15,10 11,50 11,90 16,35 14,10 11,20 10,85
True protein value (%DM)
Deviation predicted - true value (%DM) −0,08 0,35 −0,23 0,11 0,20 0,08 −0,23 0,14
a
Protein value obtain by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483) method.
Table 9 — Results of statistical analysis for the determination of the protein content in wheat by
Infraneo PLS model bl-pro03.cal
Sample W9 W10 W11 W12 W13 W14 W15 W16
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted protein content (% DM) 9,97 11,92 11,91 13,29 16,34 14,82 13,53 18,55
Repeatability standard deviation sr (%DM) 0,101 0,085 0,060 0,080 0,088 0,070 0,101 0,088
Repeatability relative stand. dev. sr (%) 1,012 0,716 0,502 0,601 0,541 0,469 0,744 0,474
Repeatability limit r [r = 2,77 × sr ] (%DM) 0,283 0,239 0,168 0,223 0,247 0,195 0,282 0,246
Reproducibility stand. dev. sR (%DM) 0,136 0,131 0,113 0,119 0,166 0,127 0,118 0,152
Reproducibility relative stand. dev. sR (%) 1,365 1,100 0,949 0,892 1,018 0,857 0,875 0,820
Reproducibility limit R [R = 2,77 × sR] (%DM) 0,381 0,367 0,317 0,332 0,466 0,355 0,332 0,426
a
9,95 12,00 12,20 13,45 16,45 15,20 13,45 18,30
True protein value (%DM)
Deviation predicted - true value (%DM) 0,02 −0,08 −0,29 −0,16 −0,11 −0,38 0,08 0,25
a
Protein value obtain by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483) method.
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Key
X protein (%DM)
Y standard deviation (%DM)
Figure 3 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
the protein content on wheat samples
Table 10— Results of statistical analysis for the determination of the protein content in barley
by Infraneo PLS model or-pro03.cal
Sample B1 B2 B3 B4 B5 B6 B7 B8
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted protein content (%DM) 10,93 11,80 12,08 10,41 11,74 11,85 10,09 12,52
Repeatability standard deviation sr
0,096 0,090 0,104 0,086 0,134 0,106 0,119 0,141
(%DM)
Repeatability relative stand. dev. sr (%) 0,874 0,762 0,859 0,830 1,139 0,897 1,175 1,127
Repeatability limit r [r = 2,77 × sr ], (%) 0,267 0,252 0,290 0,242 0,375 0,298 0,332 0,395
Reproducibility stand. dev. sR (% DM) 0,121 0,101 0,134 0,086 0,162 0,123 0,148 0,208
Reproducibility relative stand. dev. sR
1,104 0,859 1,110 0,830 1,383 1,035 1,469 1,661
(%)
Reproducibility limit R [R = 2,77 × sR]
0,338 0,221 0,375 0,242 0,455 0,343 0,415 0,582
(%)
a
11,15 11,70 11,90 10,55 11,75 11,75 10,20 12,30
True protein value (%DM)
Deviation predicted - true value (%DM) −0,22 0,10 0,18 −0,14 −0,01 0,10 −0,11 0,22
a
Protein value obtain by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483) method.
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kSIST-TP FprCEN/TR 17474:2020
FprCEN/TR 17474:2019 (E)
Table 11 — Results of statistical analysis for the determination of the protein content in barley
by Infraneo PLS model or-pro03.cal
Sample B9 B10 B11 B12 B13 B14 B15
Number of laboratories 11 11 11 11 11 11 11
Mean predicted protein content (% DM) 15,32 10,40 12,73 15,36 11,33 10,79 10,72
Repeatability standard deviation sr (%
0,095 0,097 0,183 0,156 0,073 0,113 0,105
DM)
Repeatability relative stand. dev. sr (%) 0,618 0,883 1,438 1,014 0,648 1,050 0,977
Repeatability limit r [r = 2,77 × sr ]
0,265 0,257 0,513 0,513 0,206 0,317 0,293
(%DM)
Reproducibility stand. dev. sR (% DM) 0,256 0,119 0,183 0,183 0,155 0,190 0,147
Reproducibility relative stand. dev. sR
1,674 1,147 1,438 1,192 1,364 1,759 1,371
(%)
Reproducibility limit R [R = 2,77 × sR]
0,718 0,337 0,513 0,651 0,433 0,532 0,411
(%DM)
a
15,05 10,40 12,65 15,50 11,65 10,95 10,70
True protein value (%DM)
Deviation predicted - true value (%DM) 0,27 −0,00 0,08 −0,14 −0,32 −0,16 0,02
a
Protein value obtain by 1 Master lab of the European grain networks, using Kjeldahl (EN ISO 20483)
method.

Key
X protein (%DM)
Y standard deviation (%DM)
Figure 4 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
the protein content on barley samples
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kSIST-TP FprCEN/TR 17474:2020
FprCEN/TR 17474:2019 (E)
Table 12 — Results of statistical analysis for the determination of the moisture content in wheat
by Infraneo PLS model bl-hum05.cal
Sample W1 W2 W3 W4 W5 W6 W7 W8
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted moisture content (%) 13,49 12,79 15,47 13,65 13,10 13,61 10,63 14,26
Repeatability standard deviation sr
0,059 0,033 0,030 0,037 0,035 0,046 0,051 0,060
(%)
Repeatability relative stand. dev. sr
0,434 0,258 0,195 0,270 0,269 0,341 0,478 0,423
(%)
Repeatability limit r [ r = 2,77 × sr ]
0,164 0,092 0,084 0,103 0,099 0,130 0,142 0,169
(%)
Reproducibility stand. dev. sR(%) 0,096 0,103 0,099 0,075 0,106 0,092 0,085 0,091
Reproducibility relative stand. dev. sR
0,715 0,807 0,641 0,547 0,811 0,680 0,804 0,639
(%)
Reproducibility limit R [R = 2,77 × sR]
0,270 0,289 0,278 0,209 0,297 0,259 0,239 0,255
(%)
a
13,80 13,00 15,70 13,70 13,00 13,30 10,70 14,20
True moisture value (%)
Deviation predicted - true value (%) −0,31 −0,16 −0,23 0,00 0,15 0,31 −0,07 0,06
a
Moisture value obtain by 1 Master lab of the European grain networks using ISO 712 method.
Table 13 — Results of statistical analysis for the determination of the moisture content in wheat
by Infraneo PLS model bl-hum05.cal
Sample W9 W10 W11 W12 W13 W14 W15 W16
Number of laboratories 11 11 11 11 11 11 11 11
Mean predicted moisture content (%) 12,24 12,4 12,88 10,89 11,21 15,74 13,67 12,16
9
0,03
Repeatability standard deviation sr (%) 0,056 0,047 0,050 0,018 0,035 0,039 0,036
6
0,28
Repeatability relative stand. dev. sr (%) 0,456 0,367 0,456 0,161 0,221 0,285 0,300
7
Repeatability limit r [ r = 2,77 × sr ] (%) 0,156 0,10 0,132 0,132 0,051 0,097 0,109 0,102
0
Reproducibility stand. dev. sR(%) 0,087 0,09 0,082 0,088 0,118 0,108 0,092 0,120
2
Reproducibility relative stand. dev. sR 0,707 0,73 0,636 0,811 1,049 0,687 0,674 0,989
(%) 4
Reproducibility limit R [R = 2,77 × sR] 0,242 0,25 0,229 0,247 0,330 0,303 0,258 0,337
(%)
a 12,5
12,60 12,70 11,00 11,00 15,80 13,60 12,05
True moisture value (%)
0
Deviation predicted - true value (%) −0,31 −0,0 0,23 −0,06 0,26 −0,06 0,12 0,11
1
a
Moisture value obtain by 1 Master lab of the European grain networks using ISO 712 method.
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kSIST-TP FprCEN/TR 17474:2020
FprCEN/TR 17474:2019 (E)

Key
X moisture (%)
Y standard deviation (%)
Figure 5 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
the moisture content on wheat samples
Table 14 — Results of statistical analysis for the determination of the moisture content in barley
by Infraneo PLS model or-hum05.cal
Sample B1 B2 B3 B4 B5 B6 B7 B8
Number of laboratories 11 11 11 12 11 11 11 11
Mean predicted moisture content (%) 13,30 14,06 13,80 11,89 11,94 14,14 10,60 15,90
Repeatability standard deviation sr
0,042 0,041 0,046 0,050 0,050 0,041 0,058 0,046
(%)
Repeatability relative stand. dev. sr
0,312 0,289 0,335 0,422 0,419 0,288 0,547 0,290
(%)
Repeatability limit r [ r = 2,77 × sr ]
0,116 0,114 0,130 0,140 0,140 0,114 0,162 0,129
(%)
Reproducibility stand. dev. sR(%) 0,099 0,079 0,061 0,088 0,064 0,067 0,140 0,127
Reproducibility relative stand. dev. sR
0,747 0,559 0,441 0,737 0,536 0,476 1,323 0,800
(%)
Reproducibility limit R [R = 2,77 × sR]
0,278 0,220 0,170 0,245 0,179 0,189 0,393 0,356
(%)
a
13,40 14,10 13,70 12,00 12,10 14,10 10,80 16,00
True moisture value (%)
Deviation predicted - true value (%) −0,10 0,01 0,10 −0,06 −0,16 0,09 −0,15 −0,05
a
Moisture value obtain by 1 Master lab of the European grain networks using ISO 712 method.
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kSIST-TP FprCEN/TR 17474:2020
FprCEN/TR 17474:2019 (E)
Table 15 — Results of statistical analysis for the determination of the moisture content in barley
by Infraneo PLS model or-hum05.cal
Sample B9 B10 B11 B12 B13 B14 B15
Number of laboratories 11 12 11 11 11 11 11
Mean predicted moisture content (%) 12,50 12,72 13,89 15,70 13,49 11,68 11,13
Repeatability standard deviation sr(%) 0,062 0,036 0,052 0,053 0,035 0,049 0,056
Repeatability relative stand. dev. sr (%) 0,500 0,279 0,377 0,339 0,258 0,419 0,505
Repeatability limit r [ r = 2,77 × sr ] (%) 0,175 0,099 0,146 0,146 0,098 0,137 0,157
Reproducibility stand. dev. sR(%) 0,157 0,055 0,069 0,069 0,074 0,080 0,111
Reproducibility relative stand. dev. sR
1,258 0,433 0,499 0,442 0,549 0,688 0,996
(%)
Reproducibility limit R [R = 2,77 × sR]
0,440 0,154 0,194 0,384 0,207 0,225 0,310
(%)
a
12,50 12,70 13,60 15,80 13,30 11,80 11,20
True moisture value (%)
Deviation predicted - true value (%) 0,00 0,07 0,29 −0,10 0,19 −0,12 −0,07
a
Moisture value obtain by 1 Master lab of the European grain networks using ISO 712 method.

Key
X moisture (%)
Y standard deviation (%)
Figure 6 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of
the moisture content on barley samples
4.3 PERTEN Instruments AB
An interlaboratory test, organized by the Perten Instruments AB (Sweden) company in 2013, involving
8 participants from 6 countries was carried out on 6 wheat and 4 barley samples from the 2012 harvest,
containing protein and moisture in various concentrations. The participants were the master or
reference laboratories of European grain networks. The g
...

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