SIST EN ISO 10565:1998

Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed nuclear magnetic resonance spectrometry (ISO 10565:1998)

This International Standard specifies a rapid method for the determination of the oil and water contents of commercial oilseeds using pulsed nuclear magnetic resonance (NMR). It is applicable to rapeseeds, soya beans, linseeds and sunflower seeds with a water content less than 10 %. For seeds with higher water contents, drying is necessary before the oil content can be determined by pulsed NMR. NOTE 1 This method has been tested with rapeseeds, soya beans, linseeds and sunflower seeds. This does not, however, preclude its applicability to other commercial seeds whose oil is liquid at the temperature of measurement. NOTE 2 The reproducibility values are generally higher than those obtained by the drying method (ISO 665)

Ölsamen - Gleichzeitige Bestimmung des Öl- und Wassergehaltes - Verfahren mit gepulster Kernresonanzspektroskopie (ISO 10565:1998)

Diese Internationale Norm legt ein Schnellverfahren zur Bestimmung des Öl- und Wassergehalts handelsüblicher Ölsamen mit gepulster Kernresonanzspektrometrie (NMR) fest. Es ist bei Rapssamen, Sojabohnen, Leinsamen und Sonnenblumensamen mit einem Wassergehalt unter 10% anwendbar. Samen mit höherem Wassergehalt müssen getrocknet werden, bevor die Bestimmung des Ölgehaltes mit gepulster NMR durchgeführt wird.

Graines oléagineuses - Détermination simultanée de la teneur en huile et en eau - Méthode par spectrométrie par résonance magnétique nucléaire pulsée (ISO 10565:1998)

La présente Norme internationale spécifie une méthode de détermination rapide de la teneur en huile et en eau dans les graines entières du commerce, par spectrométrie par résonance magnétique nucléaire (RMN) pulsée. Elle est applicable aux graines de colza, de soja, de lin et de tournesol dont la teneur en eau est inférieure à 10 %. Pour des graines ayant des teneurs en eau plus élevées, il est nécessaire de les sécher avant de déterminer leur teneur en huile par RMN pulsée. NOTE 1 Cette méthode a été expérimentée sur les graines de colza, de soja, de lin et de tournesol. Cela n'exclut toutefois pas qu'elle puisse s'appliquer également à d'autres graines oléagineuses du commerce dont l'huile est liquide à la température de mesurage. NOTE 2 Les valeurs de reproductibilité obtenues sont généralement plus élevées que celles obtenues par la méthode par dessiccation (ISO 665).

Oljna semena - Simultano določevanje olja in vode - Spektrometrijska metoda z uporabo pulzne jedrske magnetne resonance (ISO 10565:1998)

General Information

• Status: Published
• Publication Date: 31-Oct-1998
• ICS: 67.200.20 - Oilseeds
• Technical Committee: KŽP - Agricultural food products
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Nov-1998
• Due Date: 01-Nov-1998
• Completion Date: 01-Nov-1998
• Ref Project: EN ISO 10565:1998 - Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed nuclear magnetic resonance spectrometry (ISO 10565:1998)

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 10565:1998
01-november-1998
2OMQDVHPHQD6LPXOWDQRGRORþHYDQMHROMDLQYRGH6SHNWURPHWULMVNDPHWRGD]
XSRUDERSXO]QHMHGUVNHPDJQHWQHUHVRQDQFH,62
Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed
nuclear magnetic resonance spectrometry (ISO 10565:1998)
Ölsamen - Gleichzeitige Bestimmung des Öl- und Wassergehaltes - Verfahren mit
gepulster Kernresonanzspektroskopie (ISO 10565:1998)
Graines oléagineuses - Détermination simultanée de la teneur en huile et en eau -
Méthode par spectrométrie par résonance magnétique nucléaire pulsée (ISO
10565:1998)
Ta slovenski standard je istoveten z: EN ISO 10565:1998
ICS:
67.200.20 Oljnice Oilseeds
SIST EN ISO 10565:1998 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 10565:1998

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SIST EN ISO 10565:1998
INTERNATIONAL ISO
STANDARD 10565
Second edition
1998-08-15
Oilseeds — Simultaneous determination of
oil and water contents — Method using
pulsed nuclear magnetic resonance
spectrometry
Graines oléagineuses — Détermination simultanée de la teneur en huile et
en eau — Méthode par spectrométrie par résonance magnétique nucléaire
pulsée
A
Reference number
ISO 10565:1998(E)

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SIST EN ISO 10565:1998
ISO 10565:1998(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.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 10565 was prepared by Technical Committee
ISO/TC 34, Agricultural food products, Subcommittee SC 2, Oleaginous
seeds and fruits.
This second edition cancels and replaces the first edition
(ISO 10565:1993), which has been technically revised.
Annexes A and B of this International Standard are for information only.
©  ISO 1998
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii

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SIST EN ISO 10565:1998
©
INTERNATIONAL STANDARD  ISO ISO 10565:1998(E)
Oilseeds — Simultaneous determination of oil and water
contents — Method using pulsed nuclear magnetic resonance
spectrometry
1 Scope
This International Standard specifies a rapid method for the determination of the oil and water contents of
commercial oilseeds using pulsed nuclear magnetic resonance (NMR).
It is applicable to rapeseeds, soya beans, linseeds and sunflower seeds with a water content less than 10 %. For
seeds with higher water contents, drying is necessary before the oil content can be determined by pulsed NMR.
NOTE 1 This method has been tested with rapeseeds, soya beans, linseeds and sunflower seeds. This does not, however,
preclude its applicability to other commercial seeds whose oil is liquid at the temperature of measurement.
NOTE 2 The reproducibility values are generally higher than those obtained by the drying method (ISO 665).
2 Normative references
The following standards contain provisions which through reference in this text, constitute provisions of this
International Standard. At the time of publication, the editions indicated were valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent editions of the standards indicated below. Members of IEC and ISO maintain
registers of currently valid International Standards.
ISO 659:1988, Oilseeds — Determination of hexane extract (or light petroleum extract), called "oil content".
ISO 664:1990, Oilseeds — Reduction of laboratory sample to test sample.
ISO 665:1977, Oilseeds — Determination of moisture and volatile matter content.
3 Principle
Insertion of the test sample into the magnetic field of a pulsed NMR spectrometer.
Application of an alternating electromagnetic field in the form of an intense 90° radiofrequency (RF) pulse which
excites all the hydrogen nuclei. Recording of the free induction decay (FID) following the 90° pulse. The maximum
amplitude of this signal is proportional to the total number of protons from the water and oil phases of the sample.
1

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SIST EN ISO 10565:1998
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ISO
ISO 10565:1998(E)
Application of the second RF pulse, a so-called 180° pulse, to produce a spin-echo signal when only the signal from
the oil phase contributes to the FID.
NOTE 1 The maximum amplitude of this echo signal is proportional to the oil content. It varies with the sample temperature
following a complex law. An increase in temperature decreases the measured value of the echo.
Calculation of the difference between the two amplitudes, which is proportional to the water content.
Automatic conversion of the measured signals, after suitable calibration of the apparatus, into percentages of oil or
water.
NOTE 2 Simultaneous indications of the oil and water contents can be given by some spectrometers equipped with a
minicomputer and a specific program.
4 Calibration samples
Calibration samples shall be homogeneous and free from impurities. A definition of impurities is given in
ISO 658 [1].
4.1 Samples for moisture-content calibration
In order to obtain a reliable calibration curve, it is recommended that the water contents of the calibration samples
be less than 10 % for all seeds.
The water content of seeds can vary depending on storage conditions. Water content shall therefore be determined
in accordance with ISO 665 just prior to calibration.
4.2 Samples for oil-content calibration
Samples of oilseeds shall be of the same species as the test samples and of similar fatty acid compositions (for
instance for the analysis of rapeseeds which are rich in erucic acid, or sunflower seeds which are rich in oleic acid).
Oil content shall be determined using the reference method specified in ISO 659.
5 Apparatus
Usual laboratory apparatus and, in particular, the following.
5.1 Pulsed low-resolution NMR spectrometer, suitable for measurement of the oil content and water content of
oilseeds, and meeting the precision requirements of 11.2 and 11.3.
The instrument's parameters shall be in accordance with the instructions/specifications from the manufacturer.
CAUTION — Remove metallic objects from the proximity of the NMR spectrometer.
5.2 Sample tubes, made of glass, suitable for use with the NMR spectrometer.
5.3 Analytical balance, electronic, capable of weighing to an accuracy of ±0,01 g.
This equipment may be linked to the NMR spectrometer so that the sample mass is recorded directly by the NMR,
or linked to a minicomputer (see NOTE 2 in clause 3).
5.4 Drying oven, capable of being maintained at 103 °C ± 2 °C.
5.5 Dishes, made of glass or metal, of diameter 7 cm to 10 cm, and provided with lids.
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SIST EN ISO 10565:1998
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5.6 Desiccator, containing an efficient desiccant.
6 Sampling
Sampling is not part of the method specified in this International Standard. A recommended sampling method is
given in ISO 542 [2].
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changed during transport or storage.
7 Preparation of test sample
Prepare the test sample in accordance with ISO 664.
Remove from the prepared test sample all metallic objects (e.g. staples, needles, etc.). Whole seeds shall be
homogeneous and, as far as possible, free from impurities.
8 Calibration procedure
8.1 General
8.1.1 Use the set-up parameters of the NMR spectrometer (5.1) recommended by the manufacturer and optimize
them by preliminary tests. For all calibration and measurement operations, follow the user's manual. Ensure that all
operations during calibration and measurement are carried out under the same conditions and, in particular, at the
same temperature (±2 °C).
A minimum of three calibration samples is necessary, although more than three samples may be used.
8.1.2 Enter the parameters for the measurements (pulse sequence, attenuation, etc.) of the oil or water content (as
applicable) into the NMR spectrometer, following the manufacturer's recommendations, and specify a code number
under which the calibration curve is to be stored. The total measurement time shall be a minimum of 16 s.
8.1.3 Set the apparatus to the calibration mode.
8.1.4 Introduce a portion of the first calibration sample into a tared sample tube (5.2) up to the optimum height
specified by the manufacturer. Transfer the value of the sample mass from the balance to the NMR spectrometer.
NOTE  A manual feed of the mass ot the calibration sample into the NMR spectrometer is also possible.
8.1.5 Enter, as applicable, the value of either the water content (as a percentage by mass) or the oil content (as a
percentage by mass) into the spectrometer.
8.1.6 Introduce the sample tube containing the first calibration sample into the measuring head. Record
automatically or manually the water or oil values thus obtained.
8.1.7 Repeat steps 8.1.4 to 8.1.6 for the two (or more) other calibration samples.
8.1.8 Calculate automatically or manually the calibration parameters of the calibration curve using the results
obtained in 8.1.6 and 8.1.7.
The correlation coefficient shall normally be greater than 0,95. If this is not the case, check the values obtained
using the reference methods specified in ISO 659 and ISO 665 respectively, or repeat the calibration procedure
using three (or more) other calibration samples.
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Store the calibration curve under the code number chosen in step 8.1.2.
8.1.9  Complete the oil-content calibration curve by using an empty tube and by repeating steps 8.1.4 to 8.1.6. This
part of the method is not applicable to the water content calibration curve.
8.2  Calibration procedure for the determination of water content
8.2.1  Procedure A: Three calibration samples with known water contents
To obtain a reliable calibration graph, it is necessary that the water contents of the calibration samples span the
largest possible range. However, a water content of 0 is not permissible.
Follow the general procedure specified in 8.1.1 to 8.1.8.
8.2.2  Procedure B: One calibration sample with known water content
NOTE In this calibration procedure, the quantity of water detected by the NMR spectrometer is varied by varying the height to
which the sample tubes are filled with the calibration sample.
8.2.2.1  Follow the general procedure specified in 8.1.1 to 8.1.3.
8.2.2.2  Introduce into three tared sample tubes (5.2) portions of the calibration sample with known water content to
approximate heights of 35 mm, 30 mm and 25 mm (20 mm minimum) and weigh them. Note the corresponding
masses, in grams, as m , m and m .
1 2 3
NOTE Three calibration points is the minimum for establishing the calibration curve.
8.2.2.3  Calculate the relative water content, w, as a percentage by mass, of each of the three portions of the
calibration sample as follows:
mW×
1
w=
1
m
1
mW×
2
w=
2
m
1
mW×
3
=
w
3
m
1
where
m , m and m are the masses, in grams, of the three portions of the calibration sample in each of the three
1 2 3
tubes, where m is the largest mass;
1
W is the water content, as a per
...