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
Repeatability limit r [ r = 2,77 × s ] (%DM)
0,440 0,313 0,274 0,294 0,241 0,302
Reproducibility stand. dev. s (%DM)
0,159 0,113 0,107 0,143 0,125 0,109
Reproducibility relative stand. dev. s (%)
0,943 0,958 0,819 1,317 0,834 0,771
Reproducibility limit R [R = 2,77x s ] (%DM)
0,440 0,313 0,296 0,396 0,346 0,302
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
s > s , s set to be equal s .
r R R r

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
Repeatability limit r [ r = 2,77 × s ] (%DM)
0,548 0,468 0,341 0,95
Reproducibility stand. dev. s (% DM)
0,198 0,169 0,151 0,343
Reproducibility relative stand. dev. s (%)
1,804 1,292 1,352 2,682
Reproducibility limit R [R = 2,77 x s ]
0,548 0,468 0,418 0,950
(%DM)
Best estimate of true protein value
10,66 13,11 11,27 12,97
(%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
s > s , s set to be equal s .
r R R r

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
2 S
3 Linear (s )
4 Linear (s )

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
Repeatability relative stand. dev. s (%)
0,170 0,187 0,215 0,116 0,138 0,167
Repeatability limit r [r = 2,77 × s ] (%)
0,066 0,069 0,083 0,044 0,042 0,053
Reproducibility stand. dev. s (%)
0,077 0,07 0,090 0,079 0,045 0,047
Reproducibility relative stand. dev. s (%)
0,546 0,523 0,642 0,573 0,405 0,422
Reproducibility limit R [R = 2,77 × s ] (%)
0,213 0,194 0,249 0,219 0,125 0,130
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

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
Repeatability relative stand. dev. s (%)
0,827 0,384 0,377 1,639
Repeatability limit r [r = 2,77 × s ] (%)
0,285 0,147 0,150 0,590
Reproducibility stand. dev. s (%)
0,111 0,071 0,087 0,238
Reproducibility relative stand. dev. s (%)
0,896 0,517 0,611 1,836
Reproducibility limit R [R = 2,77 × s ] (%)
0,307 0,197 0,241 0,659
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

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
2 S
3 Linear (s )
4 Linear (s )

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
Repeatability relative stand. dev. s (%)
0,555 0,685 0,492 0,660 0,532 0,443 0,828 1,139
Repeatability limit r [r = 2,77 × s ] (%DM)
0,178 0,296 0,155 0,222 0,247 0,176 0,254 0,350
Reproducibility stand. dev. s (%DM)
0,115 0,168 0,130 0,130 0,123 0,084 0,133 0,132
Reproducibility relative stand. dev. s (%)
1,005 1,086 1,150 1,083 0,742 0,592 1,209 1,203
Reproducibility limit R [R = 2,77x s ] (%DM)
0,323 0,470 0,363 0,364 0,344 0,235 0,371 0,370
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

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
Repeatability relative stand. dev. s (%)
1,012 0,716 0,502 0,601 0,541 0,469 0,744 0,474
Repeatability limit r [r = 2,77 × s ] (%DM)
0,283 0,239 0,168 0,223 0,247 0,195 0,282 0,246
Reproducibility stand. dev. s (%DM)
0,136 0,131 0,113 0,119 0,166 0,127 0,118 0,152

Reproducibility relative stand. dev. s (%) 1,365 1,100 0,949 0,892 1,018 0,857 0,875 0,820

Reproducibility limit R [R = 2,77 × s ] (%DM) 0,381 0,367 0,317 0,332 0,466 0,355 0,332 0,426

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

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
2 s
3 Linear (s )
4 Linear (s )

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
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
Repeatability limit r [r = 2,77 × s ], (%)
0,267 0,252 0,290 0,242 0,375 0,298 0,332 0,395
Reproducibility stand. dev. s (% DM)
0,121 0,101 0,134 0,086 0,162 0,123 0,148 0,208
Reproducibility relative stand. dev. s
1,104 0,859 1,110 0,830 1,383 1,035 1,469 1,661
(%)
Reproducibility limit R [R = 2,77 × s ]
0,338 0,221 0,375 0,242 0,455 0,343 0,415 0,582
(%)
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

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 (%
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
Repeatability limit r [r = 2,77 × s ]
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
Reproducibility relative stand. dev. s
1,674 1,147 1,438 1,192 1,364 1,759 1,371
(%)
Reproducibility limit R [R = 2,77 × s ]
0,718 0,337 0,513 0,651 0,433 0,532 0,411
(%DM)
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

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
2 s
3 Linear (s )
4 Linear (s )

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
0,059 0,033 0,030 0,037 0,035 0,046 0,051 0,060
(%)
Repeatability relative stand. dev. s
0,434 0,258 0,195 0,270 0,269 0,341 0,478 0,423
(%)
Repeatability limit r [ r = 2,77 × s ]
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
Reproducibility relative stand. dev. s
0,715 0,807 0,641 0,547 0,811 0,680 0,804 0,639
(%)
Reproducibility limit R [R = 2,77 × s ]
0,270 0,289 0,278 0,209 0,297 0,259 0,239 0,255
(%)
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

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
Repeatability relative stand. dev. s (%)
0,456 0,287 0,367 0,456 0,161 0,221 0,285 0,300

Repeatability limit r [ r = 2,77 × s ] (%) 0,156 0,100 0,132 0,132 0,051 0,097 0,109 0,102

Reproducibility stand. dev. s (%) 0,087 0,092 0,082 0,088 0,118 0,108 0,092 0,120

Reproducibility relative stand. dev. s 0,707 0,734 0,636 0,811 1,049 0,687 0,674 0,989

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

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

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
2 s
3 Linear (s )
4 Linear (s )

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
0,042 0,041 0,046 0,050 0,050 0,041 0,058 0,046
(%)
Repeatability relative stand. dev. s
0,312 0,289 0,335 0,422 0,419 0,288 0,547 0,290
(%)
Repeatability limit r [ r = 2,77 × s ]
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
Reproducibility relative stand. dev. s
0,747 0,559 0,441 0,737 0,536 0,476 1,323 0,800
(%)
Reproducibility limit R [R = 2,77 × s ]
0,278 0,220 0,170 0,245 0,179 0,189 0,393 0,356
(%)
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

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
Repeatability relative stand. dev. s (%)
0,500 0,279 0,377 0,339 0,258 0,419 0,505
Repeatability limit r [ r = 2,77 × s ] (%)
0,175 0,099 0,146 0,146 0,098 0,137 0,157
Reproducibility stand. dev. s (%)
0,157 0,055 0,069 0,069 0,074 0,080 0,111
Reproducibility relative stand. dev. s
1,258 0,433 0,499 0,442 0,549 0,688 0,996
(%)
Reproducibility limit R [R = 2,77 × s ]
0,440 0,154 0,194 0,384 0,207 0,225 0,310
(%)
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

Moisture value obtained by 1 Master lab of the European grain networks using ISO 712 method.

Key
X moisture (%)
Y standard deviation (%)
1 s
2 s
3 Linear (s )
4 Linear (s )

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
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
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
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
sr > sR, sR set to be equal sr.

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 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
(%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
sr > sR, sR set to be equal sr.

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
(%)
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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

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
(%)
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

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

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

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

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

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
(%)
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

Protein value obtain 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 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)
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

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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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
(%)
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

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

0,03

Repeatability standard deviation sr (%) 0,056 0,047 0,050 0,018 0,035 0,039 0,036

0,28

Repeatability relative stand. dev. sr (%) 0,456 0,367 0,456 0,161 0,221 0,285 0,300

Repeatability limit r [ r = 2,77 × sr ] (%) 0,156 0,10 0,132 0,132 0,051 0,097 0,109 0,102

Reproducibility stand. dev. sR(%) 0,087 0,09 0,082 0,088 0,118 0,108 0,092 0,120

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 (%)
Deviation predicted - true value (%) −0,31 −0,0 0,23 −0,06 0,26 −0,06 0,12 0,11

Moisture value obtain by 1 Master lab of the European grain networks using ISO 712 method.

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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
(%)
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

Moisture value obtain 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 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
(%)
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

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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