EN ISO 1854:1999
(Main)Whey cheese - Determination of fat content - Gravimetric method (Reference method) (ISO 1854:1999)
Whey cheese - Determination of fat content - Gravimetric method (Reference method) (ISO 1854:1999)
Migrated from Progress Sheet (TC Comment) (2000-07-10): shall be // at formal vote level glg/98_02_06
Molkenkäse - Bestimmung des Fettgehaltes - Gravimetrisches Verfahren (Referenzverfahren) (ISO 1854:1999)
Diese Internationale Norm legt das Referenzverfahren für die Bestimmung des Fettgehaltes von Molkenkäse fest. Anmerkung: Falls sich der Molkenkäse nicht vollständig in der Ammoniaklösung auflöst oder in sigifikanter Menge freie Fettsäuren enthält (nur in Ausnahmefällen und dann am ausgeprägten Geruch erkennbar), fällt das Bestimmungsergebnis zu niedrig aus. Bei derartigen Produkten sollte ein Verfahren angewandt werden, das nach dem Weibull-Berntrop-Prinzip arbeitet (siehe ISO 8262-3).
Fromage de sérum - Détermination de la teneur en matière grasse - Méthode gravimétrique (Méthode de référence) (ISO 1854:1999)
Siri iz sirotke - Določevanje maščobe - Gravimetrijska metoda (Referenčna metoda) (ISO 1854:1999)
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST EN ISO 1854:2000
01-maj-2000
6LULL]VLURWNH'RORþHYDQMHPDãþREH*UDYLPHWULMVNDPHWRGD 5HIHUHQþQD
PHWRGD ,62
Whey cheese - Determination of fat content - Gravimetric method (Reference method)
(ISO 1854:1999)
Molkenkäse - Bestimmung des Fettgehaltes - Gravimetrisches Verfahren
(Referenzverfahren) (ISO 1854:1999)
Fromage de sérum - Détermination de la teneur en matiere grasse - Méthode
gravimétrique (Méthode de référence) (ISO 1854:1999)
Ta slovenski standard je istoveten z: EN ISO 1854:1999
ICS:
67.100.30 Sir Cheese
SIST EN ISO 1854:2000 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST EN ISO 1854:2000
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SIST EN ISO 1854:2000
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SIST EN ISO 1854:2000
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SIST EN ISO 1854:2000
INTERNATIONAL ISO
STANDARD 1854
Third edition
1999-10-01
Whey cheese — Determination of fat
content — Gravimetric method (Reference
method)
Fromage de sérum — Détermination de la teneur en matière grasse —
Méthode gravimétrique (Méthode de référence)
A
Reference number
ISO 1854:1999(E)
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SIST EN ISO 1854:2000
ISO 1854:1999(E)
Contents
1 Scope .1
2 Normative reference .1
3 Term and definition .1
4 Principle.1
5 Reagents.2
6 Apparatus .2
7 Sampling.3
8 Preparation of test sample.3
9 Procedure .4
9.1 Test portion .4
9.2 Blank tests.4
9.3 Preparation of fat-collecting vessel .4
9.4 Determination.5
10 Calculation and expression of results.7
10.1 Calculation.7
10.2 Expression of results .7
11 Precision.7
11.1 Interlaboratory test .7
11.2 Repeatability.7
11.3 Reproducibility.8
12 Test report .8
Annex A (informative) Notes on procedures .9
Annex B (informative) Alternative procedure using fat-extraction tubes with siphon or wash-bottle fittings 11
Bibliography.14
© ISO 1999
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 iso@iso.ch
Printed in Switzerland
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ISO 1854:1999(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3.
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 1854 was prepared by Technical Committee ISO/TC 34, Agricultural food products,
Subcommittee SC 5, Milk and milk products, in collaboration with the International Dairy Federation (IDF) and
AOAC International, and will also be published by these organizations.
This third edition cancels and replaces the second edition (ISO 1854:1987), which has been technically revised.
Annexes A and B of this International Standard are for information only.
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SIST EN ISO 1854:2000
INTERNATIONAL STANDARD © ISO ISO 1854:1999(E)
Whey cheese — Determination of fat content — Gravimetric
method (Reference method)
WARNING: The use of this International Standard may involve hazardous materials, operations
and equipment. This standard does not purport to address all the safety problems associated
with its use. It is the responsibility of the user of this standard to establish safety and health
practices and determine the applicability of regulatory limitations prior to use.
1 Scope
This International Standard specifies the reference method for the determination of fat content of whey cheese.
NOTE If the whey cheese does not dissolve completely in the ammonia or if it contains free fatty acids in significant
quantities (only in exceptional cases and then noticeable by a distinct smell), the result of the determination will be too low.
With such products recourse should be made to a method utilizing the Weibull-Berntrop principle (see ISO 8262-3).
2 Normative reference
The following normative document contains provisions which, through reference in this text, constitute provisions of
this International Standard. For dated references, subsequent amendments to, or revisions of, this publications do
not apply. However, parties to agreement based on this International Standard are encouraged to investigate the
possibility of applying the most recent edition of the normative document indicated below. For undated references,
the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of
currently valid International Standards.
ISO 3889, Milk and milk products — Determination of fat content — Mojonnier-type fat extraction flasks.
3 Term and definition
For the purposes of this International Standard, the following term and definition apply.
3.1
fat content of whey cheese
mass fraction of substances determined by the procedure specified in this International Standard.
NOTE The fat content is expressed as a mass fraction, in percent [formerly given as % (m/m)].
4 Principle
An ammoniacal ethanolic solution of a test portion is extracted with diethyl ether and light petroleum. The solvents
are removed by distillation or evaporation. The mass of the substances extracted is determined.
NOTE This is usually known as the Röse-Gottlieb principle.
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5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified, and distilled or demineralized water or
water of equivalent purity.
The reagents shall leave no appreciable residue when the determination is carried out by the method specified (see
9.2.2).
5.1 Ammonia solution, containing a mass fraction of NH of approximately 25 % (r = 910 g/l).
3 20
NOTE If ammonia solution of this concentration is not available, a more concentrated solution of known concentration may
be used (see 9.4.3).
5.2 Ethanol (C H OH), or ethanol denatured by methanol, containing a volume fraction of ethanol of at least 94 %.
2 5
(See A.5.)
5.3 Congo red solution
Dissolve 1 g of Congo red in water in a 100 ml one-mark volumetric flask (6.14). Dilute to the mark with water.
NOTE The use of this solution, which allows the interface between the solvent and aqueous layers to be seen more
clearly, is optional (see 9.4.4). Other aqueous colour solutions may be used provided that they do not affect the result of the
determination.
5.4 Diethyl ether (C H OC H ), free from peroxides (see A.3), containing no more than 2 mg/kg of antioxidants,
2 5 2 5
and complying with the requirements for the blank test (see 9.2.2, A.1 and A.4).
NOTE The use of diethyl ether could lead to hazardous situations. Due to expected changes in safety regulations studies
are ongoing to replace diethyl ether by another reagent provided that it does not affect the end result of the determination.
5.5 Light petroleum, with any boiling range between 30 °C and 60 °C or, as equivalent, pentane (CH [CH ] CH )
3 2 3 3
with a boiling point of 36 °C and complying with the requirements for the blank test (see 9.2.2, A.1 and A.4).
NOTE The use of pentane is recommended because of its higher purity and constant quality.
5.6 Mixed solvent
Shortly before use, mix equal volumes of diethyl ether (5.4) and light petroleum (5.5).
6 Apparatus
WARNING: Since the determination involves the use of volatile flammable solvents, all electrical
apparatus employed shall comply with legislation relating to the hazards in using such solvents.
Usual laboratory equipment and, in particular, the following.
6.1 Analytical balance, capable of weighing to the nearest 1 mg, with a readability of 0,1 mg.
6.2 Centrifuge, capable of holding the fat-extraction flasks or tubes (6.6) and capable of spinning at a rotational
–1 –1
frequency of 500 min to 600 min to produce a radial acceleration of 80 g to 90 g at the outer end of the flasks or
tubes.
NOTE The use of the centrifuge is optional but recommended (see 9.4.7).
6.3 Distillation or evaporation apparatus, for distilling the solvents and ethanol from the boiling or conical flasks,
or evaporating from beakers and dishes (see 9.4.14) at a temperature not exceeding 100 °C.
6.4 Drying oven, electrically heated, with ventilation port(s) fully open, capable of being maintained at a
temperature of 102 °C ± 2 °C throughout its working space.
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The oven shall be fitted with a suitable thermometer.
6.5 Water bath, capable of boiling water.
6.6 Mojonnier-type fat extraction flasks, as specified in ISO 3889.
NOTE It is also possible to use fat-extraction tubes, with siphon or wash-bottle fittings, but then the procedure is different.
The alternative procedure is given in annex B.
The fat-extraction flasks shall be provided with good quality bark corks or stoppers of other material [e.g. silicone
rubber or polytetrafluoroethylene (PTFE)] unaffected by the reagents used. Bark corks shall be extracted with the
diethyl ether (5.4), kept in water at a temperature of 60 °C or more for at least 15 min, and shall then be allowed to
cool in the water so that they are saturated when used.
6.7 Rack, for holding the fat-extraction flasks (or tubes) (6.6).
6.8 Wash bottle, suitable for use with the mixed solvent (5.6).
A plastics wash bottle shall not be used.
6.9 Fat-collecting vessels, such as boiling flasks (flat-bottomed), of capacities 125 ml to 250 ml, conical flasks, of
capacity 250 ml, or metal dishes.
If metal dishes are used, they shall be of stainless steel, flat-bottomed with a diameter of 80 mm to 100 mm and a
height of approximately 50 mm.
6.10 Boiling aids, fat-free, of non-porous porcelain or silicon carbide (optional when metal dishes are used).
6.11 Measuring cylinders, of capacities 5 ml and 25 ml.
6.12 Pipettes, graduated, of capacity 10 ml.
6.13 Tongs, made of metal, for holding flasks, beakers or dishes.
6.14 Appropriate grinding device.
, one-mark, of capacity 100 ml.
6.15 Volumetric flasks
7 Sampling
Sampling is not part of the method specified in this International Standard. A recommended sampling method is
given in ISO 707.
It is important that the laboratory receive a sample which is truly representative and has not been damaged or
changed during transport or storage.
8 Preparation of test sample
Prepare the test sample using an appropriate device (6.14). Quickly mix the ground or grated mass and, if possible,
grind it a second time. Again mix thoroughly. Clean the device after preparing each test sample.
If the test sample cannot be ground or grated, mix it thoroughly by intensive kneading, for example with a pestle in a
mortar. The danger of moisture loss during grinding or grating of the sample should be avoided as far as practically
possible.
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Keep the prepared test sample in an airtight sample container until the time of analysis, which should be carried out
on the same day. If delay is unavoidable, take every precaution to ensure proper storage of the test sample. When
refrigerated, ensure that any condensation of moisture on the inside surface of the container is thoroughly and
uniformly reincorporated into the test sample.
9 Procedure
NOTE 1 If it is required to check whether the repeatability limit (11.2) is met, carry out two single determinations in
accordance with 9.1 to 9.4
NOTE 2 An alternative procedure using fat-extraction tubes with siphon or wash-bottle fittings (see note in 6.6) is given in
annex B.
9.1 Test portion
Mix the test sample (clause 8) by gently stirring or rotating and inverting the sample container several times.
Immediately weigh to the nearest 1 mg, about 3 g of the prepared test sample, directly or by difference, in a fat-
extraction flask (6.6).
Transfer the test portion as completely as possible into the lower (small) bulb of the extraction flask.
9.2 Blank tests
9.2.1 Blank test for method
Carry out a blank test simultaneously with the determination using the same procedure and same reagents, but
replacing the dissolved test portion in 9.4.1 by 10 ml of water (see A.2).
If the value obtained in the blank test regularly exceeds 1,0 mg, check the reagents if this has not been recently
done (9.2.2).
Corrections of more than 2,5 mg should be mentioned in the test report.
9.2.2 Blank test for reagents
To test the quality of the reagents, carry out a blank test as specified in 9.2.1. Additionally use an empty fat-
collecting vessel, prepared as specified in 9.3, for mass control purposes. The reagents shall leave no residue
greater than 1,0 mg (see A.1).
If the residue of the complete reagent blank test is greater than 1,0 mg, determine the residue of the solvents
separately by distilling 100 ml of the diethyl ether and light petroleum, respectively. Use an empty fat-collecting
vessel, prepared for control purposes as described above, to obtain the real mass of residue which shall not exceed
1,0 mg.
Very occasionally, the solvents may contain volatile matter which is strongly retained in fat. If there are indications of
the presence of such substances, carry out blank tests on all the reagents and for each solvent using a fat-
collecting vessel with about 1 g of anhydrous butterfat. If necessary, redistil solvents in the presence of 1 g of
anhydrous butterfat per 100 ml of solvent. Use the solvents only shortly after the redistillation.
Replace unsatisfactory reagents or solvents, or redistil the solvents.
9.3 Preparation of fat-collecting vessel
Dry a fat-collecting vessel (6.9) with a few boiling aids (6.10) in the oven (6.4) set at 102 °C for 1 h.
NOTE 1 Boiling aids are desirable to promote gentle boiling during the subsequent removal of solvents, especially when
using glass fat-collecting vessels; their use is optional with metal dishes.
Protect the fat-collecting vessel from dust and allow it to cool to the temperature of the weighing room (glass fat-
collecting vessel for at least 1 h, metal dish for at least 30 min).
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NOTE 2 To avoid insufficient cooling or unduly long cooling times, the fat-collecting vessel should not be placed in a
desiccator.
Use tongs to place the fat-collecting vessel on the balance. Weigh the fat-collecting vessel to the nearest 1,0 mg.
NOTE 3 Tongs should preferably be used to avoid, in particular, temperature variations.
9.4 Determination
9.4.1 Carry out the determination without delay.
Add 10 ml of pre-heated water at a temperature of 65 °C æ 5 °C to the test portion in the fat-extraction flask (9.1) to
obtain a total volume of 10 ml to 11 ml. Use the water to wash the test portion completely into the small bulb of the
fat-extraction flask. Mix thoroughly with the test portion in the small bulb.
9.4.2 Heat the contents of the fat-extraction flask in the boiling water bath (6.5). Shake gently occasionally until the
test portion is completely dispersed. Leave the flask for 20 min in the boiling water bath. Then cool the flask in
running water to room temperature.
9.4.3 Add 2 ml of ammonia solution (5.1) or an equivalent volume of a more concentrated ammonia solution (see
note in 5.1) to the contents of the fat-extraction flask. Mix thoroughly with the test portion in the small bulb of the
flask.
9.4.4 Add 10 ml of ethanol (5.2). Mix gently but thoroughly by allowing the contents of the fat-extraction flask to
flow backwards and forwards between the small and large bulb. Avoid bringing the liquid too near to the neck of the
flask. If desired, add 2 drops of the Congo red solution (5.3). If necessary, cool the flask in running water to room
temperature.
Add 25
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