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BS EN 15948:2015

BS EN 15948:2015

$189.07

Cereals. Determination of moisture and protein. Method using Near-Infrared-Spectroscopy in whole kernels

Published By Publication Date Number of Pages
BSI 2015 50
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This European Standard defines a routine method for the determination of moisture and protein in whole kernels of barley and wheat using a near-infrared spectrophotometer in the constituent ranges:

  1. for wheat:

    1. moisture content minimum range from 8 % to 22 %;

    2. protein content minimum range from 7 % to 20 %.

  2. for barley:

    1. moisture content minimum range from 8 % to 22 %;

    2. protein content minimum range from 7 % to 16 %.

This European Standard describes the modalities to be implemented by the supplier ( 5.3 and 5.4) and the user of the method.

PDF Catalog

PDF Pages PDF Title
6 Foreword
7 1 Scope
2 Normative references
3 Terms and definitions
4 Principle
5 Method of analysis
5.1 General
8 5.2 Near Infrared Instrument
5.3 Prediction models
5.4 Initial validation of the model
5.4.1 General
5.4.2 Initial validation sample set
9 5.4.3 Initial validation performances
Table 1 — NIR performances for the determination of moisture and protein (see also Annex B)
5.5 Update of calibration model and validation of new model
6 Sampling
7 Procedure
7.1 Preparation of the test sample
7.2 Measurement
7.3 Local validation of the method
10 7.4 Periodical adjustment of the instrument
7.5 Checking instrument stability
7.6 Follow up of method performance
8 Calculation and expression of results
11 9 Accuracy and precision of the method
9.1 Accuracy
9.2 Precision
9.2.1 General
9.2.2 Repeatability
9.2.3 Reproducibility
12 9.2.4 Critical difference
9.2.4.1 General
9.2.4.2 Comparison of two groups of measurements in one laboratory
9.2.4.3 Comparison of two groups of measurements in two laboratories
13 10 Test Report
14 Annex A (informative) Results of examples of interlaboratory test
A.1 FOSS interlaboratory test
Table A.1 — Samples for the interlaboratory study
15 Table A.2 — Results of statistical analysis for the determination of the protein content in wheat by the ANN model WB003034
Table A.3 — Results of statistical analysis for the determination of the protein content in barley by the ANN model WB003034
16 Table A.4 — Results of statistical analysis for the determination of the moisture content in wheat by ANN model WB003034
Table A.5 — Results of statistical analysis for the determination of the moisture content in barley by ANN model WB003034
17 Figure A.1 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the protein content
18 Figure A.2 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the moisture content
19 A.2 PERTEN interlaboratory test
Table A.6 — Samples for the interlaboratory study
Table A.7 — Results of statistical analysis for the determination of the protein content in wheat by Inframatic 9500 Wheat Calibrations Version 5, March 19, 2013
20 Table A.8— Results of statistical analysis for the determination of the protein content in barley by Inframatic 9500 Barley Calibrations Version 6, March 19, 2013
Table A.9 — Results of statistical analysis for the determination of the moisture content in wheat by Inframatic 9500 Wheat Calibrations Version 5, March 19, 2013
21 Table A.10 — Results of statistical analysis for the determination of the moisture content in barley by Inframatic 9500 Barley Calibrations Version 6, March 19, 2013
Figure A.3 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the protein content
22 Figure A.4 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the moisture content
23 A.3 CHOPIN Technologies interlaboratory test
Table A.11 — Wheat Samples for the interlaboratory study
24 Table A.12 — Barley Samples for the interlaboratory study
25 Table A.13 a) — Results of statistical analysis for the determination of the protein content in wheat by Infraneo PLS model bl-pro03.cal
Table A.13 b) — Results of statistical analysis for the determination of the protein content in wheat by Infraneo PLS model bl-pro03.cal
26 Table A.14 a) — Results of statistical analysis for the determination of the protein content in barley by Infraneo PLS model or-pro03.cal
Table A.14 b) — Results of statistical analysis for the determination of the protein content in barley by Infraneo PLS model or-pro03.cal
27 Table A.15 a) — Results of statistical analysis for the determination of the moisture content in wheat by Infraneo PLS model bl-hum05.cal
Table A.15 b) — Results of statistical analysis for the determination of the moisture content in wheat by Infraneo PLS model bl-hum05.cal
28 Table A.16 a) — Results of statistical analysis for the determination of the moisture content in barley by Infraneo PLS model or-hum05.cal
Table A.16 b) — Results of statistical analysis for the determination of the moisture content in barley by Infraneo PLS model or-hum05.cal
29 Figure A.5 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the protein content on wheat samples
Figure A.6 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the protein content on barley samples
30 Figure A.7 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the moisture content on wheat samples
Figure A.8 — Standard deviations for the repeatability, sr, and reproducibility, sR, as a function of the moisture content on barley samples
31 Annex B (informative) Validation of ANN prediction model WB003034
B.1 ANN prediction model WB003034 with associated database
Table B.1 — ANN prediction model WB003034
B.2 Results of validation according to EN ISO 12099
Table B.2 — ANN model WB003034 validation summary
32 Table B.3 — Origin of samples used for the validation of the ANN model WB003034
Figure B.1 — Plot of reference vs. predicted moisture results using the ANN model WB003034 (bias 0,01, slope 1,00)
33 Figure B.2 — Plot of reference vs. predicted protein results using the ANN model WB003034 (bias 0,01; slope 1,00)
B.3 Stability and robustness
34 Figure B.3 — Average deviation of protein values predicted by the model WB003034 from the best estimate of the true value as established by the mean value of the master labs of European networks (border lines : +/- 2 standard deviations of reproducibi…
Figure B.4 — Average deviation of moisture values predicted by the model WB003034 from the best estimate of the true value as established by the mean value of the master labs of European networks (border lines : +/- 2 standard deviations of reproducib…
35 Annex C (informative) Validation of Inframatic 9500 prediction models
C.1 Perten Inframatic 9500 prediction models
Table C.1 — Inframatic 9500 Wheat Calibrations Version 5, March 19, 2013
Table C.2 — Inframatic 9500 Barley Calibrations Version 6, March 19, 2013
C.2 Results of validations according to EN ISO 12099
36 Table C.3 — Validation summary for Perten Inframatic 9500 calibrations
Figure C.1 — Histogram of samples used for the validation of the prediction model – Inframatic 9500 Barley Calibrations Version 6, March 19, 2013 – for the moisture content in barley samples (no of samples vs. % moisture)
37 Figure C.2 — Histogram of samples used for the validation of the prediction model – Inframatic 9500 Barley Calibrations Version 6, March 19, 2013 – for the protein content of barley samples (no of samples vs. % protein d.m.)
Figure C.3 — Histogram of samples used for the validation of the prediction model – Inframatic 9500 Wheat Calibrations Version 5, March 19, 2013 – for the moisture content in wheat samples (no of samples vs. % moisture)
38 Figure C.4 — Histogram of samples used for the validation of the prediction model – Inframatic 9500 Wheat Calibrations Version 5, March 19, 2013 – for the protein content of wheat samples (no of samples vs. % protein d.m.)
Figure C.5 — Validation of the Inframatic 9500 Barley Calibrations Version 6 from March 19, 2013: Plot of reference vs. predicted moisture results.
39 Figure C.6 — Validation of the Inframatic 9500 Barley Calibrations Version 6 from March 19, 2013: Plot of reference vs. predicted protein results.
Figure C.7 — Validation of the Inframatic 9500 Wheat Calibrations Version 5 from March 19, 2013: Plot of reference vs. predicted moisture results.
40 Figure C.8 — Validation of the Inframatic 9500 Wheat Calibrations Version 5 from March 19, 2013: Plot of reference vs. predicted protein results.
41 Annex D (informative) Validation of Infraneo prediction models
D.1 CHOPIN Technologies Infraneo prediction models
Table D.1 — Infraneo Calibration models
D.2 Results of validation according to EN ISO 12099
42 Table D.2 — Infraneo prediction models validation summary
Figure D.1 — Distribution of samples used for the validation of the Infraneo prediction model or-hum05.cal for moisture content on barley.
43 Figure D.2 — Distribution of samples used for the validation of the Infraneo prediction model or-pro03.cal for protein content on barley.
Figure D.3 — Distribution of samples used for the validation of the Infraneo prediction model bl-hum05.cal for moisture content on wheat.
44 Figure D.4 — Distribution of samples used for the validation of the Infraneo prediction model bl-pro03.cal for protein content on wheat.
Figure D.5 — Reference values vs. predicted results for moisture on barley
45 Figure D.6 — Reference values vs. predicted results for protein on barley
Figure D.7 — Reference values vs. predicted results for moisture on wheat
46 Figure D.8 — Reference values vs. predicted results for protein on wheat
47 Bibliography

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BS EN 15948:2015
$189.07