Animal feeding stuffs, cereals and milled cereal products - Guidelines for the application of near infrared spectrometry (ISO 12099:2017)

ISO 12099:2017 gives guidelines for the determination by near infrared spectroscopy of constituents such as moisture, fat, protein, starch and crude fibre and parameters such as digestibility in animal feeding stuffs, cereals and milled cereal products.
The determinations are based on spectrometric measurement in the near infrared spectral region.

Futtermittel, Getreide und gemahlene Getreideerzeugnisse - Anleitung für die Anwendung von Nahinfrarot-Spektrometrie (ISO 12099:2017)

Diese Internationale Norm stellt eine Anleitung für die Bestimmung von Bestandteilen, wie z. B. Feuchte, Fett, Protein, Stärke und Rohfaser, und von Parametern, wie z. B. Verdaubarkeit des Futtermittels, von Getreide und gemahlenen Getreideerzeugnissen, mit Nahinfrarot-Spektroskopie bereit.
Die Bestimmungen basieren auf einer spektrometrischen Messung im Nahinfrarotbereich.

Aliments des animaux, céréales et produits de mouture des céréales - Lignes directrices pour l'application de la spectrométrie dans le proche infrarouge (ISO 12099:2017)

ISO 12099:2017 fournit des lignes directrices pour la détermination par spectrométrie dans le proche infrarouge de constituants tels que l'eau, les matières grasses, les protéines, l'amidon et la cellulose brute, et des paramètres tels que la digestibilité des aliments pour animaux, des céréales et des produits de mouture des céréales.
Les déterminations sont basées sur des mesurages spectrométriques dans le domaine spectral du proche infrarouge.

Krma, žito in mlevski proizvodi - Smernice za uporabo bližnje infrardeče spektrometrije (ISO 12099:2017)

Ta dokument podaja smernice za določevanje lastnosti, kot so vlažnost, maščoba, beljakovine, škrob in surove vlaknine, ter parametrov, kot je prebavljivost, v krmi, žitu in mlevskih proizvodih z bližnjo infrardečo spektrometrijo.
Določitve temeljijo na spektrometričnih meritvah v bližnjem infrardečem spektralnem območju.

General Information

Status
Published
Publication Date
19-Sep-2017
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Due Date
20-Sep-2017
Completion Date
20-Sep-2017

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SLOVENSKI STANDARD
SIST EN ISO 12099:2017
01-november-2017
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SIST EN ISO 12099:2010
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Animal feeding stuffs, cereals and milled cereal products - Guidelines for the application

of near infrared spectrometry (ISO 12099:2017)
Futtermittel, Getreide und gemahlene Getreideerzeugnisse - Anleitung für die
Anwendung von Nahinfrarot-Spektrometrie (ISO 12099:2017)

Aliments des animaux, céréales et produits de mouture des céréales - Lignes directrices

pour l'application de la spectrométrie dans le proche infrarouge (ISO 12099:2017)

Ta slovenski standard je istoveten z: EN ISO 12099:2017
ICS:
65.120 Krmila Animal feeding stuffs
67.060 äLWDVWURþQLFHLQSURL]YRGLL] Cereals, pulses and derived
QMLK products
SIST EN ISO 12099:2017 en

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 12099:2017
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SIST EN ISO 12099:2017
EN ISO 12099
EUROPEAN STANDARD
NORME EUROPÉENNE
September 2017
EUROPÄISCHE NORM
ICS 65.120 Supersedes EN ISO 12099:2010
English Version
Animal feeding stuffs, cereals and milled cereal products -
Guidelines for the application of near infrared
spectrometry (ISO 12099:2017)

Aliments des animaux, céréales et produits de mouture Futtermittel, Getreide und gemahlene

des céréales - Lignes directrices pour l'application de la Getreideerzeugnisse - Anleitung für die Anwendung

spectrométrie dans le proche infrarouge (ISO von Nahinfrarot-Spektrometrie (ISO 12099:2017)

12099:2017)
This European Standard was approved by CEN on 14 July 2017.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

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, 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: Avenue Marnix 17, B-1000 Brussels

© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 12099:2017 E

worldwide for CEN national Members.
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SIST EN ISO 12099:2017
EN ISO 12099:2017 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 12099:2017
EN ISO 12099:2017 (E)
European foreword

This document (EN ISO 12099:2017) has been prepared by Technical Committee ISO/TC 34 “Food

products" in collaboration with Technical Committee CEN/TC 327 “Animal feeding stuffs - Methods of

sampling and analysis” the secretariat of which is held by NEN.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by March 2018 and conflicting national standards shall be

withdrawn at the latest by March 2018.

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.

This document supersedes EN ISO 12099:2010.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,

Turkey and the United Kingdom.
Endorsement notice

The text of ISO 12099:2017 has been approved by CEN as EN ISO 12099:2017 without any modification.

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SIST EN ISO 12099:2017
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SIST EN ISO 12099:2017
INTERNATIONAL ISO
STANDARD 12099
Second edition
2017-08
Animal feeding stuffs, cereals and
milled cereal products — Guidelines
for the application of near infrared
spectrometry
Aliments des animaux, céréales et produits de mouture des céréales —
Lignes directrices pour l’application de la spectrométrie dans le
proche infrarouge
Reference number
ISO 12099:2017(E)
ISO 2017
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SIST EN ISO 12099:2017
ISO 12099:2017(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2017, Published in Switzerland

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form

or by any means, electronic or mechanical, including photocopying, or posting on the internet or an intranet, without prior

written permission. Permission can be requested from either ISO at the address below or ISO’s member body in the country of

the requester.
ISO copyright office
Ch. de Blandonnet 8 • CP 401
CH-1214 Vernier, Geneva, Switzerland
Tel. +41 22 749 01 11
Fax +41 22 749 09 47
copyright@iso.org
www.iso.org
ii © ISO 2017 – All rights reserved
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SIST EN ISO 12099:2017
ISO 12099:2017(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Apparatus ..................................................................................................................................................................................................................... 2

6 Calibration and initial validation ........................................................................................................................................................ 2

6.1 General ........................................................................................................................................................................................................... 2

6.2 Reference methods .............................................................................................................................................................................. 3

6.3 Outliers .......................................................................................................................................................................................................... 3

6.4 Validation of calibration models .............................................................................................................................................. 3

6.4.1 General...................................................................................................................................................................................... 3

6.4.2 Bias correction ................................................................................................................................................................... 4

6.4.3 Slope adjustment ............................................................................................................................................................. 4

6.4.4 Expansion of calibration set ................................................................................................................................... 4

6.5 Changes in measuring and instrument conditions .................................................................................................. 4

7 Statistics for performance measurement ................................................................................................................................... 5

7.1 General ........................................................................................................................................................................................................... 5

7.2 Plot the results ........................................................................................................................................................................................ 5

7.3 Bias .................................................................................................................................................................................................................... 6

7.4 Root mean square error of prediction (s ) ......................................................................................................... 8

RMSEP

7.5 Standard error of prediction (s ) ....................................................................................................................................... 8

SEP

7.6 Slope ..............................................................................................................................................................................................................10

8 Sampling .....................................................................................................................................................................................................................12

9 Procedure..................................................................................................................................................................................................................12

9.1 Preparation of test sample .........................................................................................................................................................12

9.2 Measurement .........................................................................................................................................................................................12

9.3 Evaluation of result ..........................................................................................................................................................................12

10 Checking instrument stability .............................................................................................................................................................13

10.1 Control sample .....................................................................................................................................................................................13

10.2 Instrument diagnostics .................................................................................................................................................................13

10.3 Instruments in a network ...........................................................................................................................................................13

11 Running performance check of calibration ...........................................................................................................................13

11.1 General ........................................................................................................................................................................................................13

11.2 Control charts using the difference between reference and NIR results ...........................................14

12 Precision and accuracy ...............................................................................................................................................................................15

12.1 Repeatability ..........................................................................................................................................................................................15

12.2 Reproducibility ....................................................................................................................................................................................15

12.3 Accuracy .....................................................................................................................................................................................................15

12.4 Uncertainty ..............................................................................................................................................................................................15

13 Test report ................................................................................................................................................................................................................15

Annex A (informative) Guidelines for specific NIR standards .................................................................................................16

Annex B (informative) Examples of outliers and control charts ..........................................................................................17

Annex C (informative) Supplementary terms and definitions ................................................................................................23

Bibliography .............................................................................................................................................................................................................................28

© ISO 2017 – All rights reserved iii
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SIST EN ISO 12099:2017
ISO 12099:2017(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO’s adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following

URL: w w w . i s o .org/ iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 10,

Animal feeding stuffs.

This second edition cancels and replaces the first edition (ISO 12099:2010), which has been technically

revised.
iv © ISO 2017 – All rights reserved
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SIST EN ISO 12099:2017
ISO 12099:2017(E)
Introduction

This document has been drafted using, as a basis, ISO 21543 | IDF 201, which was prepared by Technical

Committee ISO/TC 34, Food products, Subcommittee SC 5, Milk and milk products, and the International

Dairy Federation (IDF).
© ISO 2017 – All rights reserved v
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SIST EN ISO 12099:2017
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SIST EN ISO 12099:2017
INTERNATIONAL STANDARD ISO 12099:2017(E)
Animal feeding stuffs, cereals and milled cereal
products — Guidelines for the application of near infrared
spectrometry
1 Scope

This document gives guidelines for the determination by near infrared spectroscopy of constituents

such as moisture, fat, protein, starch and crude fibre and parameters such as digestibility in animal

feeding stuffs, cereals and milled cereal products.

The determinations are based on spectrometric measurement in the near infrared spectral region.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

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
3.1
near infrared instrument
NIR instrument

apparatus which, when used under the conditions defined in this document, predicts constituent

contents (3.3) and technological parameters (3.4) in animal feeding stuffs (3.2), cereals and milled cereal

products through relationships to absorptions in the near infrared range
3.2
animal feeding stuffs

substance or product, including additives, whether processed, partially processed or unprocessed,

intended to be used for oral feeding to animals

EXAMPLE Raw materials, fodder, meat and bone meal, mixed feed and other end products, pet food, etc.

3.3
constituent content

mass fraction of substances determined using the appropriate, standardized or validated chemical

method
Note 1 to entry: The mass fraction is often expressed as a percentage.

Note 2 to entry: For examples of appropriate methods, see References [1] to [12].

EXAMPLE Moisture, fat, protein, crude fibre, neutral detergent fibre and acid detergent fibre.

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SIST EN ISO 12099:2017
ISO 12099:2017(E)
3.4
technological parameter

property or functionality of animal feeding stuffs (3.2), cereals and milled cereal products that can be

determined using the appropriate, standardized or validated method(s)

Note 1 to entry: It is possible to develop and validate NIR methods for other parameters and sample types than

listed above, as long as the procedure from this document is observed. The measuring units of the parameters

determined follow the units used in the reference methods.
EXAMPLE Digestibility.
4 Principle

Spectral data in the near infrared region are collected and transformed to constituent or parameter

concentrations by calibration models developed on representative samples of the products concerned.

5 Apparatus
5.1 Near infrared instruments.

Instruments based on diffuse reflectance or transmittance measurement covering the near infrared

−1 −1

wavelength region of 770 nm to 2 500 nm (12 900 cm to 4 000 cm ) or segments of this or at selected

wavelengths or wavenumbers. The optical principle may be dispersive (e.g. grating monochromators),

interferometric or non-thermal (e.g. light emitting diodes, laser diodes and lasers). The instrument

should be provided with a diagnostic test system for testing photometric noise and reproducibility,

wavelength/wavenumber accuracy and wavelength/wavenumber precision (for scanning
spectrophotometers).

The instrument should measure a sufficiently large sample volume or surface to eliminate any

significant influence of inhomogeneity derived from chemical composition or physical properties of

the test sample. The sample path length (sample thickness) in transmittance measurements should

be optimized according to the manufacturer’s recommendation with respect to signal intensity for

obtaining linearity and maximum signal/noise ratio.

5.2 Appropriate milling or grinding device, for preparing the sample (if needed).

NOTE Changes in grinding or milling conditions can influence NIR measurements due, for example, to

heating which can drive off volatile components such as water.
6 Calibration and initial validation
6.1 General

The instrument shall be calibrated before use. Calibration involves the comparison with a reference

and adjustment processes to the instrument. Because a number of different calibration systems can be

applied with NIR instruments, no specific procedure can be given for calibration.

For an explanation of methods for calibration development, see Reference [16] and the respective

manufacturer’s manual. For the validation, it is important to have a sufficient number of representative

samples, covering variations such as the following:
a) combinations and composition ranges of major and minor sample components;

b) seasonal, geographic and genetic effects on forages, feed raw material and cereals;

c) processing techniques and conditions;
d) storage conditions;
2 © ISO 2017 – All rights reserved
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SIST EN ISO 12099:2017
ISO 12099:2017(E)
e) sample and instrument temperature;
f) instrument variations (i.e. differences between instruments).
NOTE For a solid validation, at least 20 samples are needed.
6.2 Reference methods

Internationally accepted reference methods for determination of moisture, fat, protein and other

constituents and parameters should be used. See References [1] to [12] for examples.

The reference method used for calibration should be in statistical control. It is essential to know the

precision of the reference method.

Where possible, references that provide measurement traceability to the SI (International system of

units), such as certified reference materials, should be used.
6.3 Outliers

In many situations, statistical outliers are observed during calibration and validation. Outliers may be

related to NIR data (spectral outliers, hereafter referred to as “x-outliers”) or errors in reference data

or samples with a different relationship between reference data and NIR data (hereafter referred to as

“y-outliers”); see Figures B.1 to B.5 for examples.

For the purpose of validation, samples are not to be regarded as outliers if they fulfil the following

conditions:

a) if they are within the working range of the constituents/parameters in the calibration(s);

b) if they are within the spectral variation of the calibration samples, as, for example, estimated by

Mahalanobis distance;
c) if the spectral residual is below a limit defined by the calibration process;

d) if the prediction residual is below a limit defined by the calibration process.

If a sample appears as an outlier, then it should be checked initially to see if it is an x-outlier. If it exceeds

the x-outlier limits defined for the calibration, it should be removed. If it is not an x-outlier, then both

the reference value and the NIR predicted value should be checked, e.g. by repeated measurements. If

these confirm the original values, then the sample should not be deleted and the validation statistics

should include this sample. If the repeat values show that either the original reference values or the NIR

predicted ones were in error, then the new values should be used.
6.4 Validation of calibration models
6.4.1 General

Before use, calibration equations shall be validated locally on an independent test set that is

representative of the sample population to be analysed. For the determination of bias, slope and for the

determination of standard error of prediction (SEP, see 7.5), at least 20 samples are needed. Validation

shall be carried out for each sample type, constituent/parameter, temperature and other factors known

to affect or expected to have an effect the measurement. The calibration is valid only for the variations,

i.e. sample types, range and temperature, used in the validation.

NOTE 1 Calibration models can only be used in the range they have been validated.

Results obtained on the independent test set are plotted, reference against NIR, and residuals against

reference results, to give a visual impression of the performance of the calibration. The SEP is calculated

(see 7.5) and the residual plot of data corrected for mean systematic error (bias) is examined for

outliers, i.e. samples with a residual exceeding ±3 s .
SEP
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SIST EN ISO 12099:2017
ISO 12099:2017(E)

If the validation process shows that the model cannot produce acceptable statistics, then it should not

be used.

NOTE 2 What will be acceptable will depend, for example, on the performance of the reference method, the

covered range, the purpose of the analysis, etc., and is up to the parties involved to decide.

Where available and suitable, reference materials or certified reference materials can be used as part of

validation of calibration models.

The next step is to fit NIR, y , and reference data, y , by linear regression (y = a + b × y ) to

NIRS ref ref NIRS
produce statistics that describe the validation results.
6.4.2 Bias correction

The data are also examined for a bias between the methods. If the difference between means of the

NIR predicted and reference values is significantly different from zero, then this indicates that the

calibration is biased. A bias may be removed by adjusting the constant term (see 7.3) in the calibration

equation.
6.4.3 Slope adjustment
If the slope, b, is significantly different from 1, the calibration is skewed.

Adjusting the slope/intercept of the calibration is generally not recommended unless the calibration

is applied to new types of samples or instruments. If a reinvestigation of the calibration does not

detect outliers, especially outliers with high leverage, it is preferable to expand the calibration set to

include more samples. However, if the slope is adjusted, the calibration should then be tested on a new

independent test set.
6.4.4 Expansion of calibration set

If the accuracy of the calibration does not meet expectations, the calibration set should be expanded

to include more samples or a new calibration should be made. In all cases when a new calibration

is developed on an expanded calibration set, the validation process should be repeated on a new

validation set. If necessary, expansion of the calibration set should be repeated until acceptable results

are obtained on a validation set.
6.5 Changes in measuring and instrument conditions

Unless additional calibration is performed, a local validation of a NIR method stating the accuracy of

the method can generally not be considered valid if the test conditions are changed.

For example, calibrations developed for a certain population of samples may not be valid for samples

outside this population, although the analyte concentration range is unchanged. A calibration developed

on grass silages from one area may not give the same accuracy on silages from another area if the

genetic, growing and processing parameters are different.

Changes in the sample presentation technique or the measuring conditions, e.g. temperature, not

included in the calibration set may also influence the analytical results.

Calibrations developed on a certain instrument cannot always be transferred directly to an identical

instrument operating under the same principle. It may be necessary to perform bias or slope /

intercept adjustments to calibration equations. In many cases, it will be nec
...

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