SIST-TP CEN/TR 16324:2012

SLOVENSKI STANDARD
01-oktober-2012
7HKQLþQRSRURþLORRPHGODERUDWRULMVNLãWXGLML]DXJRWDYOMDQMHSULPHVLYSãHQLFLUåL
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Technical report of the interlaboratory study for the determination of Besatz in common
wheat, rye and durum wheat
Technischer Bericht über Ringversuchsergebnisse zur Bestimmung von Besatz in
Weizen, Roggen und Hartweizen
Rapport technique relatif à l'essai interlaboratoire portant sur la détermination du
pourcentage d'impuretés dans le blé tendre, le seigle et le blé dur
Ta slovenski standard je istoveten z: CEN/TR 16324:2012
ICS:
67.060 äLWDVWURþQLFHLQSURL]YRGLL] Cereals, pulses and derived
QMLK products
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL REPORT
CEN/TR 16324
RAPPORT TECHNIQUE
TECHNISCHER BERICHT
August 2012
ICS 67.060
English Version
Technical report of the interlaboratory study for the
determination of Besatz in common wheat, rye and durum wheat
Rapport technique relatif à l'essai interlaboratoire portant Technischer Bericht des Ringversuchs zur Bestimmung
sur la détermination du pourcentage d'impuretés dans le von Besatz in Weizen, Roggen und Hartweizen
blé tendre, le seigle et le blé dur

This Technical Report was approved by CEN on 7 February 2012. 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, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TR 16324:2012: E
worldwide for CEN national Members.

Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Design of the study.5
3 Statistical evaluation .6
4 Results of the determination of "broken grains" .8
5 Results of the determination of "shrivelled grains" . 11
6 Results of the determination of "other cereals" . 14
7 Results of the determination of "grains damaged by pests" . 17
8 Results of the determination of "grains in which the germ is discoloured, mottled grains" . 20
9 Results of the determination of "sprouted grains" . 23
10 Results of the determination of "extraneous seeds" . 26
11 Results of the determination of "unsound grains" . 29
12 Results of the determination of "extraneous matter" . 32
13 Results of the determination of "husks" . 35
14 Results of the determination of "ergot" . 38
15 Results of the determination of "grain impurities" . 41
16 Results of the determination of "miscellaneous impurities" . 44
17 Results of the determination of "total Besatz" . 47
18 Precision data of sample set A . 50
19 Results of sample set A and B . 54
Annex A (informative) Participants . 59
Bibliography . 60

Foreword
This document (CEN/TR 16324:2012) has been prepared by Technical Committee CEN/TC 338 “Cereal and
cereal products”, the secretariat of which is held by AFNOR.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN shall not be held responsible for identifying any or all such patent rights.
Introduction
The term “Besatz” applies to all components of a grain sample that differ from the normal basic cereal. The
principle of the determination of Besatz is to separate all the groups of Besatz from the normal basic cereal
grains of unimpaired quality by sieving and manual selection out of a subsample and to quantify them. The
amount of Besatz and its constituent groups is important for health, cleaning, milling and further processing
aspects. For these reasons Besatz is a part of contracts in grain trade and also of the grain intervention
system of the EU. At present a European Standard for the determination of Besatz (EN 15587) has been
developed.
An international interlaboratory test for the determination of Besatz, according to EN 15587 and involving 15
laboratories in 11 countries, was carried out with two common wheat, two rye and two durum wheat samples.
Statistical analysis was possible for all Besatz fractions with the exception of grains overheated during drying,
bunted grains, and impurities of animal origin.
Very high interlaboratory variation was found for the fractions mottled grains (including grains in which the
germ is discoloured), unsound grains, and grains damaged by pests.
The lowest interlaboratory variation was found for the fractions extraneous matter, extraneous seeds, and
ergot.
The coefficient of variability in most cases depended clearly on the amount of the respective Besatz group,
whereby the amount of the respective Besatz group was in a normal range. As a result the coefficient of
intralaboratory variability for the total Besatz was not higher than 10 %. The coefficient of interlaboratory
variability for the total Besatz was not higher than 20 %, provided the amount of mottled grains or unsound
grains or insect-damaged grain is not higher than 1 % (w/w).
1 Scope
The term "Besatz" applies to all components of a grain sample that differ from the normal basic cereal. It
includes the following groups: broken grains, shrivelled grains, other cereals, grains damaged by pests, grains
with discoloured germ, grains overheated during drying, sprouted grains, extraneous seeds, unsound grains,
ergot, bunted grains, extraneous matter, husks and impurities of animal origin. The amount of Besatz and its
constituent groups is important for health, cleaning, milling and further processing aspects. For these reasons
Besatz is a component of contracts in grain trade and also of the grain intervention system of EU. The
principle of the determination of Besatz is to separate all the groups of Besatz from the normal basic cereal
grains of unimpaired quality by sieving and manual selection out of a subsample and to quantify them. There
are various problems in the determination of Besatz: Firstly, the identification of the different groups of Besatz
depends strongly on the experience and the knowledge of the investigator. Also experienced investigators can
differ in their characterization of grains. Finally, one is faced with the fact that grain, even after mixing, is rarely
homogenous. In other words, if a sample was divided by a sample divider into a number of portions, the
amount of a specific group of Besatz in each portion could be different, even if absolutely no human or
machine error occurred in each determination. These problems will result in variation of the results of the
determination.
An international interlaboratory trial for the determination of Besatz in common wheat, durum wheat and rye
was accomplished with 15 laboratories in order to get information on the intra- and interlaboratory variability of
the determination of Besatz.
The Technical Report here describes the preparation and evaluation of the results of this interlaboratory test.

2 Design of the study
Each laboratory received two kinds of sample sets.
The sample set A consisted of six samples which had a mass of not less than 50g. The participants received
two samples of common wheat, rye and durum wheat. The sample set A was prepared from basic cereal of
1)
unimpaired quality. Certain amounts of the 14 different Besatz groups were added to each sample of the set
A, in the way that the two samples of the same cereal had the same composition. The composition of the
spiked samples was chosen to ensure that i) laboratories obtaining outlying results would be identified and ii)
the influence of sample division on the precision of the method would be recognizable.

1) The added material of the various Besatz groups comes from numerous Besatz-investigations of our own laboratory.
The material was reviewed independently by three persons with regard to the unique assignment to a Besatz group.
The sample set B consisted of six samples which had a mass of not less than 1kg. The participants received
two samples of common wheat, rye and durum wheat, resp. The sample set B was prepared from clean basic
2)
cereal, which contained small amounts of Besatz . One bulk sample of slightly more than 40kg of each
cereal (wheat, rye, and durum) was used. After careful mixing to make the bulk sample as homogeneous as
possible it was divided using a sample divider to obtain 40 samples. Twenty of them were directly sealed in
moisture proof plastic bags. The other 20 samples were spiked with certain Besatz groups, individually mixed
and the sealed in moisture proof plastic bags. In this way we achieved different concentration levels of the
various Besatz groups. The concentration levels were selected to represent the range of Besatz commonly
found in grain samples. The results obtained for the sample set B were used for the calculation of the
precision data given in Annex D of EN 15587:2008.
The participants were instructed to analyse the samples of set A only once and the samples of set B in
duplicate. They had to divide the samples of set B to obtain the required size, before testing.
We sent the sample to 20 laboratories and after six weeks we received results of 15 laboratories for each
sample.
The laboratories were instructed to report the weights of the analysed samples as well as of the separated
Besatz groups. In addition, participants should calculate the results in terms of percentage weight. The
obtained results of sample set B showed that the method of calculation was not described clearly enough in
the draft standard. Many laboratories have not taken into account that extraneous matter was removed (by
sieving) before testing the two sub-samples. Only five laboratories performed the calculations in the correct
manner. The results of the other laboratories were recalculated before beginning the statistical evaluation.
3 Statistical evaluation
The statistical evaluation was performed according to ISO 5725-2. This requires the examination of data with
the Cochran and Mandel‘s k test for non homogeneity of variances (5 % and 1 % level) and the examination of
the data with the Grubbs and Mandel‘s h test for deviations of laboratory mean values (5 % and 1 % level).
So, the analysis of the results for consistency and outliers was done by:
 numerical outlier tests (Cochran’s test, Grubbs’ test); and
 graphical consistency technique (Mandel’s statistics, k and h).
The results obtained for the sample set B are presented in Clause 4 to 17. These results were used for the
calculation of the precision data given in EN 15587. The single results of the duplicate determination and the
calculated precision data (after outlier elimination) are always presented in a table and a figure. The results of
the Mandel’s statistic are presented in a separate figure. Abnormal values can be identified by the comparison
with the critical values which are drawn as lines in the figure.
A value which was straggling (abnormal) according to one of these four statistical tests was removed only if
the following two conditions were met:
a) the precision data without this abnormal values differed significantly from the precision data including it,
so that its elimination gave significantly better values for precision;
b) the elimination of this abnormal value does not have the consequence that the ratio r / R
(repeatability/Reproducibility) reaches the value 1.

2) The use of basic cereal of unimpaired quality was impossible, because the cleaning of 120 kg of grain material by
manual selection was not realisable.
Only if both conditions were met, an abnormal value was eliminated. Therefore, there may be cases in which
an abnormal value was not removed, because the precision data were not significantly improved or the ratio
r/R reached the value 1.
The table which contains the collation of the test results and the calculated precision data shows also the
eliminated outliers, which are underlined.
The results obtained for the sample set A were statistically evaluated in the same manner as described above,
but the collation of test results and precision data are not presented as detailed as above. The precision data
of the sample set A are presented in Clause 18 and shown together with those of the sample set B in Clause
19.
No statistical evaluation could be done for three fractions: grains overheated during drying, smutty grains and
impurities of animal origin. In the first two cases we did not have enough material to spike the grain samples.
In the case of impurities of animal origin there was a problem with the insufficient description in
EN 15587. It was not clear how to handle the insects which fall through the 1 mm sieve. Some laboratories
had counted these insects, others had not.
4 Results of the determination of "broken grains"
Table 1 — Collation of test results, outliers and precision data on the determination of "broken grains"
Determination of "broken grains"
Mean of duplicate determination
Single results of the dupliacte determination (results given in [w/w%])
(results given i n [w/w%])
Sample: A A B B CCD DE E F F A B C D E F
Lab.No
1 1.676 1.517 2.935 2.498 1.202 1.269 5.512 5.639 0.120 0.630 2.158 1.690 1.60 2.72 1.24 5.58 0.38 1.92
2 1.917 1.616 3.813 2.932 1.133 1.370 5.500 6.042 0.222 0.019 1.519 1.488 1.77 3.37 1.25 5.77 0.12 1.50
3 1.985 1.446 2.858 2.538 1.430 1.727 6.278 6.512 0.319 0.788 1.626 2.006 1.72 2.70 1.58 6.40 0.55 1.82
4 0.265 0.732 2.270 2.365 1.235 1.614 6.332 4.915 0.561 0.503 1.673 1.144 0.50 2.32 1.42 5.62 0.53 1.41
5 0.363 0.336 2.574 2.301 1.025 1.023 5.636 5.093 0.338 0.138 1.572 1.367 0.35 2.44 1.02 5.36 0.24 1.47
8 0.588 0.785 2.656 1.858 1.788 1.048 5.121 6.387 0.342 0.257 1.439 1.144 0.69 2.26 1.42 5.75 0.30 1.29
9 1.872 1.702 2.913 2.856 1.014 1.372 5.605 5.350 0.175 0.167 1.688 1.085 1.79 2.88 1.19 5.48 0.17 1.39
11 0.996 1.639 3.456 2.770 1.334 1.536 5.748 5.076 0.774 0.953 1.156 1.531 1.32 3.11 1.44 5.41 0.86 1.34
12 2.064 1.279 3.280 3.167 1.612 1.451 5.735 5.709 -- -- -- -- 1.67 3.22 1.53 5.72 -- --
13 1.491 1.491 3.004 2.873 0.940 1.217 5.517 6.087 0.050 0.054 0.422 0.590 1.49 2.94 1.08 5.80 0.05 0.51
14 0.578 0.512 2.039 1.942 1.597 1.396 5.665 5.871 0.472 0.229 1.311 1.698 0.55 1.99 1.50 5.77 0.35 1.50
16 0.432 0.448 2.766 3.467 1.550 1.879 3.551 5.519 0.660 0.993 2.692 2.424 0.44 3.12 1.71 4.54 0.83 2.56 g
17 1.281 1.111 2.619 2.694 1.055 1.285 5.688 5.707 0.200 0.180 1.349 0.864 1.20 2.66 1.17 5.70 0.19 1.11
18 0.318 0.149 2.116 2.442 1.327 1.212 5.191 4.840 0.285 0.212 1.518 1.547 0.23 2.28 1.27 5.02 0.25 1.53
19 -- -- -- -- -- -- -- -- 0.172 0.100 1.454 1.141 -- -- -- -- 0.14 1.30
20 0.351 0.312 2.005 2.412 1.008 1.524 5.555 5.658 0.149 0.181 1.723 1.254 0.33 2.21 1.27 5.61 0.17 1.49
average ##### ##### ##### ##### ##### #####
Outliers alle Datenalle Datenalle Datenalle Datenalle Datenohne L16
Sample Sample AB CD EF
A = common wheat Mean of test results 1.04 2.68 1.34 5.57 0.34 1.40
Number of laboratories
B = common wheat 15 15 15 15 15 14
C = rye Repeatability standard deviation s 0.24 0.32 0.23 0.55 0.16 0.27
r
D = rye Variation coefficient of repeatability 23 % 12 % 17 % 10 % 47 % 19 %
0.68 0.90 0.65 1.55 0.45 0.75
E = durum wheat Repeatability r
F = durum wheat Reproducibility standard deviation s 0.63 0.48 0.25 0.57 0.27 0.38
R
Variation coefficient of reproducibility 61 % 18 % 19 % 10 % 80 % 27 %
1.77 1.34 0.71 1.58 0.77 1.06
Reproducibility R
0.38 0.67 0.91 0.98 0.59 0.71
Ratio (r/R)
Abbreviations: g Grubbs outlier, 5%, data eliminated

Key
X mean value of "broken grains" [w/w%]
Y standard deviation [w/w%]
Figure 1 — Relationship between the standard deviation (s , s ) and the mean value of "broken
r R
grains"
Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y broken gains [% W/W]
Figure 2 — Single results of the duplicate determination of "broken grains" including the overall
mean, standard deviation of repeatability (s ) and reproducibility (s ) for the six test samples A to F
r R
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 3 — Determination of "broken grains": (a) Mandel’s within-laboratory statistic, k, and (b)
Mandel’s between laboratory consistency statistic, h, each grouped by laboratories
5 Results of the determination of "shrivelled grains"
Table 2 — Collation of test results, outliers and precision data on the determination
of "shrivelled grains"
Determination of "shrivelled grains"
Mean of duplicate determination
Single results of the dupliacte determination (results given in [w/w%])
(results given in [w/w%])
Sample: AABBC C D D E E F F A B C D E F
Lab.No
1 0.904 1.244 2.601 2.201 0.501 0.174 1.322 1.040 0.000 0.000 0.183 0.116 1.07 2.40 0.34 1.18 0.00 0.15
2 1.316 1.339 4.821 4.134 2.605 3.215 2.451 3.442 3.521 2.770 3.275 2.476 1.33 4.48 G 2.91 c 2.95 c 3.15 C 2.88 C
3 1.085 1.190 2.502 2.114 0.322 0.315 0.656 0.896 0.000 0.000 0.293 0.167 1.14 2.31 0.32 0.78 0.00 0.23
4 1.287 1.281 2.093 2.063 0.469 0.521 1.143 0.811 0.000 0.000 0.085 0.213 1.28 2.08 0.50 0.98 0.00 0.15
5 1.428 0.969 2.485 1.929 0.236 0.192 1.202 0.653 0.053 0.039 0.068 0.388 1.20 k 2.21 0.21 0.93 0.05 0.23
8 1.192 1.208 2.676 2.583 0.237 0.266 0.664 0.703 0.098 0.066 0.294 0.217 1.20 2.63 0.25 0.68 0.08 0.26
9 1.054 1.139 2.500 1.579 0.567 0.463 0.927 0.979 0.000 0.000 0.167 0.136 1.10 2.04 k 0.52 0.95 0.00 0.15
11 1.129 1.429 2.580 2.555 0.543 0.462 0.807 1.056 0.000 0.000 0.234 0.269 1.28 2.57 0.50 0.93 0.00 0.25
12 0.860 1.321 2.624 2.628 0.360 0.548 1.211 1.200 -- -- -- -- 1.09 k 2.63 0.45 1.21 -- --
13 0.832 0.832 1.161 1.280 0.687 0.459 0.912 1.402 0.005 0.007 0.114 0.149 0.83 1.22 0.57 1.16 0.01 0.13
g C
14 1.035 1.316 2.596 2.936 0.450 0.655 1.645 2.045 0.056 0.526 1.009 1.252 1.18 2.77 0.55 1.85 0.29 1.13
16 1.111 1.241 2.130 2.127 0.246 0.490 0.564 0.711 0.000 0.000 0.217 0.152 1.18 2.13 0.37 0.64 0.00 0.18
17 1.201 1.111 2.234 2.773 0.227 0.159 0.769 0.710 0.000 0.000 0.159 0.157 1.16 2.50 0.19 0.74 0.00 0.16
18 1.345 1.094 2.133 1.637 0.172 0.299 0.859 0.772 0.000 0.000 0.195 0.230 1.22 1.89 0.24 0.82 0.00 0.21
19 -- -- -- -- -- -- -- -- 0.000 0.000 0.148 0.151 -- -- -- -- 0.00 0.15
20 0.864 0.833 1.412 2.233 0.000 0.000 0.390 0.243 0.000 0.021 0.215 0.181 0.85 1.82 0.00 0.32 0.01 0.20
average ##### ##### ##### ##### ##### #####
Outliers ohne L5 &ohne L2 &ohne L2 &ohne L2 &ohne L2 &ohne L2
Sample
Sample A BCDE F
Mean of test results 1.14 2.24 0.36 0.87 0.01 0.26
A = common wheat
B = common wheat Number of laboratories 13 13 14 13 13 14
C = rye Repeatability standard deviation s 0.12 0.28 0.11 0.19 0.01 0.09
r
Variation coefficient of repeatability
D = rye 11 % 12 % 31 % 22 % 72 % 34 %
E = durum wheat Repeatability r 0.34 0.77 0.31 0.52 0.02 0.24
F = durum wheat Reproducibility standard deviation s 0.17 0.47 0.18 0.28 0.03 0.26
R
Variation coefficient of reproducibility 15 % 21 % 51 % 32 % 229 % 103 %
Reproducibility R 0.49 1.31 0.52 0.79 0.07 0.74
0.70 0.59 0.60 0.66 0.31 0.33
Ratio (r/R)
Abbreviations: C Cochtran's outlier, 1%, d ata eliminated G Grubbs ou tlier, 1%, data el iminated
c Cochrans outlier, 5%, data eliminated g Grubbs ou tlier, 5%, data el iminated
k Mandel's statistic,k, outlier, 5%, data eliminated

Key
X mean value of "shrivelled grains" [W/W%]
Y standard deviation [W/W%]
Figure 4 — Relationship between the standard deviation (s , s ) and the mean value
r R
of "shrivelled grains"
Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y shrivelled grains [W/W%]
Figure 5 — Single results of the duplicate determination of "shrivelled grains" including the overall
mean, standard deviation of repeatability (s ) and reproducibility (s ) for the six test samples A to F
r R
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 6 — Determination of "shrivelled grains": (a) Mandel’s within-laboratory statistic, k, and (b)
Mandel’s between laboratory consistency statistic, h, each grouped by laboratories
6 Results of the determination of "other cereals"
Table 3 — Collation of test results, outliers and precision data on the determination
of "other cereals"
Determination of "other cereals"
Mean of duplicate determination
Single results of the dupliacte determination (results given in [w/w%])
(results given in [w/w%])
Sample: A A B B CCD DE E F F A B C D E F
Lab.No
1 0.000 0.000 1.805 1.010 1.199 1.873 0.510 0.985 1.305 1.165 3.556 2.847 0.00 1.41 1.54 0.75 1.24 3.20
2 0.223 0.126 2.003 2.389 2.407 1.727 1.083 1.356 1.328 0.950 3.484 3.849 0.17 2.20 2.07 1.22 1.14 3.67
3 0.000 0.000 2.740 1.570 1.864 1.683 0.233 1.033 0.485 1.254 3.697 3.996 0.00 2.16 1.77 0.63 0.87 3.85
4 0.110 0.219 1.946 2.674 1.547 1.692 0.486 1.582 0.499 0.742 3.989 3.853 0.16 2.31 1.62 1.03 k 0.62 3.92
5 0.012 0.142 0.442 0.423 0.686 0.790 0.571 0.284 0.588 0.360 1.646 2.606 0.08 0.43 0.74 0.43 0.47 2.13
8 0.000 0.000 0.333 2.007 1.413 3.468 0.776 0.830 0.493 0.704 3.323 3.444 0.00 1.17 2.44 0.80 0.60 3.38
c
9 0.000 0.211 4.260 0.734 1.085 1.171 1.201 0.836 0.841 0.620 3.841 2.923 0.11 2.50 C 1.13 1.02 0.73 3.38
11 0.205 0.112 1.069 1.170 2.174 1.670 0.293 1.211 0.570 0.758 2.488 2.088 0.16 1.12 1.92 0.75 0.66 2.29
12 0.000 0.189 0.867 0.882 1.583 0.983 0.060 0.909 -- -- -- -- 0.09 0.87 1.28 0.48 -- --
13 0.043 0.043 0.520 0.522 1.265 1.177 0.302 0.751 0.303 0.157 0.000 0.000 0.04 0.52 1.22 0.53 0.23 0.00 G
14 0.128 0.000 0.396 0.713 1.331 1.607 0.584 0.715 0.693 0.470 2.539 3.767 0.06 0.55 1.47 0.65 0.58 3.15
16 0.146 0.099 1.544 0.969 1.210 1.544 0.328 0.120 0.590 0.355 2.211 2.311 0.12 1.26 1.38 0.22 0.47 2.26
17 0.160 0.261 1.171 1.743 1.948 1.317 0.497 0.262 0.845 2.176 2.190 2.436 0.21 1.46 1.63 0.38 1.51 c 2.31
18 0.139 0.148 1.525 1.292 1.680 1.660 0.749 0.842 0.575 0.936 4.620 4.243 0.14 1.41 1.67 0.80 0.76 4.43
19 -- -- -- -- -- -- -- -- 0.840 1.159 3.428 3.269 -- -- -- -- 1.00 3.35
20 0.126 0.053 1.175 0.867 1.059 2.250 0.743 0.537 0.769 1.100 2.784 3.427 0.09 1.02 1.65 0.64 0.93 3.11
average
Outliers alle Datenalle Datenalle Datenalle Datenalle Datenohne L16
Sample Sample ABC D EF
A = common wheat Mean of test results 0.10 1.28 1.51 0.66 0.74 3.17
B = common wheat Number of laboratories 15 14 14 14 14 14
C = rye Repeatability standard deviation s 0.07 0.48 0.36 0.33 0.23 0.42
r
Variation coefficient of repeatability
D = rye 76 % 37 % 24 % 50 % 31 % 13 %
E = durum wheat Repeatability r 0.21 1.34 1.01 0.93 0.64 1.16
F = durum wheat Reproducibility standard deviation s 0.08 0.70 0.43 0.35 0.32 0.76
R
Variation coefficient of reproducibility 88 % 55 % 28 % 53 % 44 % 24 %
Reproducibility R 0.24 1.95 1.19 0.98 0.90 2.13
Ratio (r/R) 0.87 0.69 0.84 0.95 0.71 0.55
Abbreviations: C Cochtran's outlier, 1%, data eliminated G Grubbs outlier, 1%, data eliminated
c Cochrans outlier, 5%, data eliminated
k Mandel's statistic,k, outlier, 5%, data eliminated

Key
X mean value of "other cereals" [W/W%]
Y standard deviation [W/W%]
Figure 7 — Relationship between the standard deviation (s , s ) and the mean value
r R
of "other cereals"
Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y other cereals [% W/W]
Figure 8 — Single results of the duplicate determination of "other cereals" including the overall mean,
standard deviation of repeatability (s ) and reproducibility (s ) for the six test samples A to F
r R
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 9 — Determination of "other cereals": (a) Mandel’s within-laboratory statistic, k, and (b)
Mandel’s between laboratory consistency statistic, h, each grouped by laboratories
7 Results of the determination of "grains damaged by pests"
Table 4 — Collation of test results, outliers and precision data on the determination of "grains
damaged by pests"
Determination of "grains damaged by pests"
Mean of duplicate determination
Single results of the dupliacte determination (results given in [w/w%])
(results given in [w/w%])
Sample: A A B B CCD DE E F F A B C D E F
Lab.No
1 0.487 0.272 0.404 0.276 0.043 0.000 0.000 0.072 0.051 0.086 0.000 0.000 0.38 0.34 0.02 0.04 0.07 0.00
2 0.342 0.431 0.241 0.090 0.101 0.089 0.000 0.053 0.074 0.137 0.000 0.095 0.39 0.17 0.10 0.03 0.11 0.05
3 0.253 0.401 0.147 0.440 0.069 0.000 0.086 0.150 0.063 0.046 0.046 0.063 0.33 0.29 0.03 0.12 0.05 0.05
4 2.019 1.296 1.056 0.889 0.624 0.164 0.346 0.548 0.000 0.000 0.000 0.091 1.66 0.97 0.39 C 0.45 0.00 0.05
5 0.427 0.655 0.232 0.129 0.000 0.000 0.288 0.200 0.000 0.000 0.000 0.000 0.54 0.18 0.00 0.24 0.00 0.00
8 1.529 1.474 1.625 0.619 0.186 0.232 1.100 0.499 0.412 0.154 0.078 0.080 1.50 1.12 C 0.21 0.80 c 0.28 0.08
9 0.347 0.456 0.084 0.121 0.064 0.070 0.059 0.196 0.000 0.146 0.000 0.289 0.40 0.10 0.07 0.13 0.07 0.14
11 0.604 0.400 0.222 0.041 0.039 0.015 0.042 0.223 0.000 0.000 0.000 0.000 0.50 0.13 0.03 0.13 0.00 0.00
12 0.569 0.666 0.113 0.056 0.000 0.000 0.145 0.109 -- -- -- -- 0.62 0.08 0.00 0.13 -- --
13 0.245 0.245 0.204 0.204 0.310 0.270 0.129 0.434 0.000 0.000 0.000 0.000 0.25 0.20 0.29 0.28 0.00 0.00
14 1.170 1.618 0.815 0.873 0.195 0.187 0.440 0.159 0.000 0.077 0.058 0.162 1.39 0.84 0.19 0.30 0.04 0.11
16 1.882 2.515 0.810 0.714 0.000 0.094 0.097 0.191 0.064 0.337 0.089 0.328 2.20 0.76 0.05 0.14 0.20 0.21
17 0.256 0.163 0.154 0.158 0.081 0.000 0.032 0.062 0.069 0.000 0.000 0.000 0.21 0.16 0.04 0.05 0.03 0.00
18 1.255 1.798 0.570 1.197 0.097 0.164 0.059 0.110 0.000 0.000 0.154 0.086 1.53 0.88 0.13 0.08 0.00 0.12
19 -- -- -- -- -- -- -- -- 0.310 0.098 0.456 0.235 -- -- -- -- 0.20 0.35
G G C
20 1.621 2.600 1.121 1.170 1.037 0.862 0.771 0.696 1.228 0.832 3.767 2.402 2.11 1.15 0.95 0.73 1.03 3.08
average ##### ##### ##### ##### ##### #####
Outliers alle Datenalle Datenalle Datenalle Datenalle Datenohne L16
Sample
Sample AB CD E F
A = common wheat Mean of test results 0.93 0.45 0.09 0.20 0.08 0.08
B = common wheat Number of laboratories 15 14 13 14 14 14
Repeatability standard deviation s
C = rye r 0.29 0.15 0.03 0.10 0.09 0.09
D = rye Variation coefficient of repeatability 31 % 33 % 39 % 51 % 118 % 108 %
Repeatability r
E = durum wheat 0.82 0.41 0.10 0.29 0.25 0.25
F = durum wheat Reproducibility standard deviation s 0.74 0.40 0.09 0.21 0.11 0.12
R
Variation coefficient of reproducibility 79 % 88 % 106 % 101 % 146 % 143 %
Reproducibility R
2.08 1.11 0.26 0.58 0.31 0.33
0.40 0.37 0.37 0.50 0.81 0.76
Ratio (r/R)
Abbreviations: C Cochtran's outlier, 1%, data eliminated G Grubbs outlier, 1%, data eliminated
c Cochrans outlier, 5%, data eliminated

Key
X mean value of "grains damaged by pests" [W/W%]
Y standard deviation [W/W%]
Figure 10 — Relationship between the standard deviation (s , s ) and the mean value
r R
of "grains damaged by pests"
Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y grains damaged by pests [% W/W]
Figure 11 — Single results of the duplicate determination of "grains damaged by pests" including the
overall mean, standard deviation of repeatability (s ) and reproducibility (s ) for the six test samples A
r R
to F
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 12 — Determination of "grains damaged by pests": (a) Mandel’s within-laboratory statistic, k,
and (b) Mandel’s between laboratory consistency statistic, h, each grouped by laboratories
8 Results of the determination of "grains in which the germ is discoloured, mottled
grains"
Table 5 — Collation of test results, outliers and precision data on the determination
of "mottled grains"
Determination of "mottled grains, grains in which the germ is discoloured"
Single results of the dupliacte determination                Mean of duplicate d eter mination
(results given in [w/w%]) (results given in [w/w%])
Sample: AABB E E F F A B E F
Lab.No
1 0.000 0.000 0.490 0.379 1.474 1.422 3.5 05 3 .440 0.00 0 .43 1.45 3.47
2 0.000 0.072 0.951 1.302 6.649 4.721 5.7 97 5 .341 0.04 1 .13 5.69 5.57
3 0.175 0.000 0.704 0.635 20.056 19.632 21.462 21.633 0.09 0.67 19.84 21.55 g
4 0.008 0.000 0.564 0.246 12.208 11.570 10.446 8.318 0.00 0.41 11.89 9.38
5 0.000 0.000 0.000 0.000 1.708 2.864 3.5 91 3 .880 0.00 0 .00 2.29 3.74
8 0.000 0.000 0.530 0.390 2.781 2.895 2.5 12 2 .239 0.00 0 .46 2.84 2.38
9 0.000 0.000 0.613 0.377 2.073 2.150 2.8 11 2 .631 0.00 0 .50 2.11 2.72
11 0.164 0.249 0.530 0.412 16.240 16.112 14.033 16.053 0.21 0.47 16.18 15.04
12 0.470 0.365 0.418 0.464 -- -- -- -- 0.42 0.44 -- --
13 0.000 0.000 0.000 0.000 0.000 0.000 0.0 00 0 .000 0.00 0 .00 0.00 0.00
14 0.212 0.000 0.301 0.698 3.264 3.104 5.2 09 3 .775 0.11 0 .50 3.18 4.49
16 0.000 0.000 0.199 0.486 5.582 6.731 4.1 10 4 .360 0.00 0 .34 6.16 4.24
17 0.000 0.065 0.616 0.238 4.684 4.083 2.4 59 3 .159 0.03 0 .43 4.38 2.81
18 0.180 0.000 0.436 0.270 0.000 0.000 0.8 42 1 .800 0.09 0 .35 0.00 1.32
19 -- -- -- -- 15.504 15.055 14.120 14.351 -- -- 15.28 14.24
C
20 0.000 0.518 0.317 0.206 5.578 6.489 8.691 7.338 0.26 0.26 6.03 8.01
##### ##### ##### #####
alle Datenalle Datenalle Datenohne L16
Sample
Sample AB EF
A = common wheat Mean of test results 0.07 0.43 6.49 5.53
B = common wheat Number of laboratories 14 15 15 14
C = rye Repeatability standard deviation s 0.07 0.16 0.53 0.72
r
Variation coefficient of repeatability
D = rye 99 % 37 % 8 % 13 %
E = duru m wheat Repeatability r 0.19 0.44 1.48 2.01
F = duru m wheat Reproducibility standard deviation s 0.13 0.29 6.31 4.59
R
Variation coefficient of reproducibility
181 % 67 % 97 % 83 %
Reproducibility R 0.36 0.80 17.66 12.86
Ratio (r/R) 0.55 0.56 0.08 0.16
Abbreviations: C Cochtran's outlier, 1%, data eliminated g Grubb s outlier, 5%, data e liminated

Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y grains in which the germ is discoloured, mottled grains [% W/W]
Figure 13 — Single results of the duplicate determination of "grains in which the germ is discoloured,
mottled grains" including the overall mean, standard deviation of repeatability (s ) and reproducibility
r
(s ) for the six test samples A, B, E and F
R
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 14 — Determination of "grains in which the germ is discoloured, mottled grains": (a) Mandel’s
within-laboratory statistic, k, and (b) Mandel’s between laboratory consistency statistic, h, each
grouped by laboratories
9 Results of the determination of "sprouted grains"
Table 6 — Collation of test results, outliers and precision data on the determination of "sprouted
grains"
Determination of "sprouted grains"
Mean of duplicate deter mination
Single results of the dupliacte determination (results given in [w/w%])
(results given i n [w/w%])
Sample: A ABBC C D D E E F F A B C D E F
Lab.No
1 0.581 0.868 0.192 0.391 0.000 0.064 2.257 1.834 0.162 0.214 0.902 1.194 0.72 0.29 0.03 2.05 0.19 1.05
2 0.941 1.066 0.524 0.322 0.158 0.200 1.580 1.238 0.080 0.111 1.464 1.324 1.00 0.42 0.18 1.41 0.10 1.39
3 1.146 0.750 0.415 0.329 0.205 0.135 2.492 2.392 0.779 0.487 1.832 1.514 0.95 0.37 0.17 2.44 0.63 1.67
4 0.761 0.910 0.378 0.353 0.370 0.189 2.013 2.823 0.485 0.673 1.454 2.023 0.84 0.37 0.28 2.42 0.58 1.74
5 1.389 0.902 0.115 0.248 0.000 0.000 1.938 1.849 0.000 0.527 0.764 0.597 1.15 0.18 0.00 1.89 0.26 0.68
8 0.751 1.135 0.689 0.446 0.000 0.000 2.371 1.916 0.000 0.000 0.511 0.781 0.94 0.57 0.00 2.14 0.00 0.65
9 0.986 0.775 0.195 0.549 0.192 0.108 1.960 1.828 0.151 0.303 0.637 0.827 0.88 0.37 0.15 1.89 0.23 0.73
11 0.762 1.078 0.338 0.401 0.200 0.523 2.342 1.591 0.987 1.093 0.834 0.766 0.92 0.37 0.36 1.97 1.04 0.80
12 0.598 0.424 0.328 0.396 0.052 0.049 1.832 1.931 -- -- -- -- 0.51 0.36 0.05 1.88 -- --
13 0.669 0.669 0.523 0.491 0.121 0.426 2.082 1.515 0.000 0.249 0.240 0.339 0.67 0.51 0.27 1.80 0.12 0.29
14 1.126 1.646 0.673 0.316 0.076 0.104 1.720 1.923 0.000 0.000 0.854 1.154 1.39 0.49 0.09 1.82 0.00 1.00
16 1.748 0.770 0.551 0.855 0.138 0.296 2.827 2.095 0.839 0.457 1.100 0.826 1.26 K 0.70 0.22 2.46 0.65 0.96
17 0.801 0.898 0.231 0.238 0.000 0.032 1.698 1.774 0.230 0.603 0.063 0.141 0.85 0.23 0.02 1.74 0.42 0.10
18 1.325 1.061 0.442 0.430 0.050 0.000 1.973 2.361 0.550 0.283 0.371 0.740 1.19 0.44 0.03 2.17 0.42 0.56
19 -- -- -- -- -- -- -- -- 0.307 0.280 0.078 0.579 -- -- -- -- 0.29 0.33
20 0.883 0.939 0.593 0.647 0.123 0.300 2.151 1.706 0.000 0.178 0.610 0.423 0.91 0.62 0.21 1.93 0.09 0.52
average ##### ##### ##### ##### ##### #####
Outliers alle Datenalle Datenalle Datenalle Datenalle Datenohne L16
Sample Sample ABC D EF
A = common wheat Mean of test results 0.92 0.42 0.14 2.00 0.33 0.83
B = common wheat Number of laboratories 14 15 15 15 15 15
Repeatability standard deviation s
C = rye r 0.21 0.13 0.10 0.32 0.17 0.21
Variation coefficient of repeatability
D = rye 22 % 31 % 74 % 16 % 51 % 25 %
E = durum wheat Repeatability r 0.58 0.37 0.28 0.89 0.48 0.58
F = durum wheat Reproducibility standard deviation s R 0.26 0.17 0.14 0.37 0.32 0.50
Variation coefficient of reproducibility
29 % 40 % 100 % 18 % 94 % 61 %
Reproducibility R 0.74 0.47 0.38 1.02 0.88 1.41
Ratio (r/R) 0.78 0.78 0.74 0.87 0.55 0.41
Abbreviations:
Abbreviations: K Mandel's statistic,k, outlier, 1%, data eliminated

Key
X mean value of "sprouted grains" [W/W%]
Y standard deviation [W/W%]
Figure 15 — Relationship between the standard deviation (s , s ) and the mean value of "sprouted
r R
grains"
Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y sprouted grains [% W/W]
Figure 16 — Single results of the duplicate determination of "sprouted grains" including the overall
mean, standard deviation of repeatability (s ) and reproducibility (s ) for the six test samples A to F
r R
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 17 — Determination of "sprouted grains": (a) Mandel’s within-laboratory statistic, k, and (b)
Mandel’s between laboratory consistency statistic, h, each grouped by laboratories
10 Results of the determination of "extraneous seeds"
Table 7 — Collation of test results, outliers and precision data on the determination
of "extraneous seeds"
Determination of "extraneous seeds"
Mean of duplicate determination
Single results of the dupliacte determination (results given in [w/w%])
(results given i n [w/w%])
Sample: A A B B C CD DE E F F A B C D E F
Lab.No
1 0.630 0.884 0.048 0.074 1.490 2.232 0.522 0.575 1.284 1.438 0.085 0.177 0.76 0.06 1.86 K 0.55 1.36 0.13
2 0.758 0.735 0.085 0.038 1.487 1.424 0.403 0.324 1.301 0.887 0.118 0.093 0.75 0.06 1.46 0.36 1.09 0.11
3 0.929 0.951 0.047 0.090 1.666 1.820 0.627 0.551 1.388 1.314 0.196 0.177 0.94 0.07 1.74 0.59 1.35 0.19
4 0.969 0.611 0.088 0.085 1.868 1.914 0.651 0.504 1.446 1.488 0.164 0.133 0.79 0.09 1.89 0.58 1.47 0.15
5 0.773 0.908 0.140 0.103 1.512 1.503 0.541 0.647 1.404 1.572 0.201 0.271 0.84 0.12 1.51 0.59 1.49 0.24
8 0.877 1.068 0.147 0.068 1.552 1.789 0.360 0.514 1.557 1.344 0.139 0.179 0.97 0.11 k 1.67 0.44 1.45 0.16
9 0.793 0.859 0.050 0.074 1.933 1.547 0.403 0.472 1.187 1.277 0.220 0.209 0.83 0.06 1.74 0.44 1.23 0.21
11 0.956 0.874 0.090 0.093 1.823 1.890 0.522 0.450 1.437 1.181 0.264 0.164 0.92 0.09 1.86 0.49 1.31 0.21
12 0.822 0.869 0.127 0.085 1.876 2.076 0.414 0.707 -- -- -- -- 0.85 0.11 1.98 0.56 -- --
13 0.799 0.799 0.112 0.112 1.869 1.602 0.361 0.236 0.307 0.713 0.328 0.329 0.80 0.11 1.74 0.30 0.51 0.33
14 0.358 0.327 0.010 0.010 1.333 1.000 0.179 0.426 0.587 0.922 0.021 0.094 0.34 0.01 1.17 0.30 0.75 0.06
16 0.704 0.804 0.074 0.125 1.630 1.074 0.226 0.449 0.495 0.801 0.248 0.191 0.75 0.10 1.35 0.34 0.65 0.22
17 0.657 0.735 0.077 0.048 1.412 1.587 0.513 0.231 0.845 0.826 0.079 0.079 0.70 0.06 1.50 0.37 0.84 0.08
18 0.894 0.815 0.083 0.086 1.468 1.418 0.327 0.355 1.318 1.323 0.129 0.199 0.85 0.08 1.44 0.34 1.32 0.16
19 -- -- -- -- -- -- -- -- 1.007 1.416 0.141 0.125 -- -- -- -- 1.21 0.13
20 0.546 0.763 0.052 0.086 1.287 1.276 0.369 0.460 1.581 1.469 0.235 0.204 0.65 0.07 1.28 0.41 1.53 0.22
average ##### ##### ##### ##### ##### #####
Outliers alle Datenalle Datenalle Datenalle Datenalle Datenohne L16
Sample Sample AB CDE F
A = common wheat Mean of test results 0.78 0.08 1.59 0.44 1.17 0.17
Number of laboratories
B = common wheat 15 14 14 15 15 15
C = rye Repeatability standard deviation s 0.11 0.02 0.17 0.11 0.17 0.04
r
Variation coefficient of repeatability
D = rye 13 % 28 % 11 % 25 % 15 % 22 %
E = durum wheat Repeatability r 0.29 0.06 0.47 0.32 0.49 0.10
F = durum wheat Reproducibility standard deviation s 0.17 0.03 0.27 0.13 0.35 0.07
R
Variation coefficient of reproducibility
21 % 41 % 17 % 30 % 30 % 43 %
Reproducibility R 0.47 0.09 0.76 0.38 0.98 0.21
Ratio (r/R) 0.63 0.67 0.62 0.84 0.49 0.50
Abbreviations: K Mandel's statistic,k, outlier, 1%, data eliminated
k Mandel's statistic,k, outlier, 5%, data eliminated

Key
X mean value of "extraneous seeds" [W/W%]
Y standard deviation [W/W%]
Figure 18 — Relationship between the standard deviation (s , s ) and the mean value
r R
of "extraneous seeds"
Key
mean s s (values without eliminated outliers (*))
r R
X lab. No.
Y extraneous seeds [% W/W]
Figure 19 — Single results of the duplicate determination of "extraneous seeds" including the overall
mean, standard deviation of repeatability (s ) and reproducibility (s ) for the six test samples A to F
r R
Key
A (wheat)
B (wheat)
C (rye)
D (rye)
E (durum)
F (durum)
X laboratory
Y1 Mandel's statistic, K
Y2 Mandel's statistic, h
Figure 20 — Determination of "extraneous seeds": (a) Mandel’s within-laboratory statistic, k, and (b)
Mandel’s between laboratory consistency statistic, h, each grouped by laboratories
11 Results of the determination of "unsound grains"
Table 8 — Collation of test results, outliers and precision data on the determination
of "unsound grains"
Determination of "unsound grains"
Mean of duplicate deter min ation
Single results of the dupliacte determination (results given in [w/w%])
(results given i n [w/w%])
Sample: A A B B CCD DE E F F A B C D E F
Lab.No
1 0.207 0.191 0.980 0.571 0.661 0.485 0.957 1.193 0.318 0.174 1.381 0.999 0.20 0.78 0.57 1.08 0.25 1.19
2 0.246 0.071 0.012 0.020 0.026 0
...