1、October 2016 English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 67.200.20!%*“2579907www.din.deDIN
2、 EN ISO 14244Oilseed meals Determination of soluble proteins in potassium hydroxide solution (ISO 14244:2014);English version EN ISO 14244:2016,English translation of DIN EN ISO 14244:2016-10lsamenschrote Bestimmung der in Kaliumhydroxidlsung lslichen Proteine (ISO 14244:2014);Englische Fassung EN I
3、SO 14244:2016,Englische bersetzung von DIN EN ISO 14244:2016-10Tourteaux de graines olagineuses Dtermination de la teneur en protines solubles en solution dhydroxyde de potassium (ISO 14244:2014);Version anglaise EN ISO 14244:2016,Traduction anglaise de DIN EN ISO 14244:2016-10www.beuth.deDocument c
4、omprises 12 pagesDTranslation by DIN-Sprachendienst.In case of doubt, the German-language original shall be considered authoritative.10.16 DIN EN ISO 14244:2016-10 2 A comma is used as the decimal marker. National foreword The text of ISO 14244:2014 has been prepared by Technical Committee ISO/TC 34
5、 “Food products” (Secretariat: AFNOR, France), Subcommittee SC 2 “Oleaginous seeds and fruits and oilseed meals” (Secretariat: AFNOR, France) and has been taken over as EN ISO 14244:2016 by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products Methods of
6、sampling and analysis” (Secretariat: AFNOR, France). The responsible German bodies involved in its preparation were DIN-Normenausschuss Lebensmittel und landwirtschaftliche Produkte (DIN Standards Committee Food and Agricultural Products) and the Deutsche Gesellschaft fr Fettwissenschaft (German Fat
7、 Research Society), Joint Working Committee NA 057-05-05 AA Gemeinschaftsausschuss fr die Analytik von Fetten, len, Fettprodukten, verwandten Stoffen und Rohstoffen. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 565 DIN ISO 565 ISO 57
8、25-1 DIN ISO 5725-1 ISO 5725-2 DIN ISO 5725-2 ISO 5983-1 DIN EN ISO 5983-1 ISO 5983-2 DIN EN ISO 5983-2 National Annex NA (informative) Bibliography DIN EN ISO 5983-1, Animal feeding stuffs Determination of nitrogen content and calculation of crude protein content Part 1: Kjeldahl method DIN EN ISO
9、5983-2, Animal feeding stuffs Determination of nitrogen content and calculation of crude protein content Part 2: Block digestion and steam distillation method DIN ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openings DIN ISO 5725-1, Accuracy
10、(trueness and precision) of measurement methods and results Part 1: General principles and definitions DIN ISO 5725-2, Accuracy (trueness and precision) of measurement methods and results Part 2: Basic method for the determination of repeatability and reproducibility of a standard measurement method
11、 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 14244 August 2016 ICS 67.200.20 English Version Oilseed meals - Determination of soluble proteins in potassium hydroxide solution (ISO 14244:2014) Tourteaux de graines olagineuses - Dtermination de la teneur en protines solubles en solution d
12、hydroxyde de potassium (ISO 14244:2014) lsamenschrote - Bestimmung der in Kaliumhydroxidlsung lslichen Proteine (ISO 14244:2014) This European Standard was approved by CEN on 15 July 2016. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for gi
13、ving 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 of
14、ficial 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
15、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
16、, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels 2016 CEN All rights of exploitation in any form and by any means reserved worldwide
17、for CEN national Members. Ref. No. EN ISO 14244:2016 EContents PageEuropean foreword .31 Scope . 52 Normative references 53 Principle 54 Reagents 55 Apparatus . 66 Sampling 67 Preparation of test sample . 78 Procedure. 79 Expression of results 710 Precision . 810.1 Interlaboratory test. 810.2 Repeat
18、ability . 810.3 Reproducibility . 811 Test report . 8Annex A (informative) Results of interlaboratory tests 9Bibliography . 10DIN EN ISO 14244:2016-10 EN ISO 14244:2016 (E)2Foreword .4European foreword The text of ISO 14244:2014 has been prepared by Technical Committee ISO/TC 34 “Food products” of t
19、he International Organization for Standardization (ISO) and has been taken over as EN ISO 14244:2016 by Technical Committee CEN/TC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling and analysis” the secretariat of which is held by DIN. This European Standa
20、rd shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by February 2017, and conflicting national standards shall be withdrawn at the latest by February 2017. Attention is drawn to the possibility that some of the elements of
21、this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. According to the CEN-CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European S
22、tandard: 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,
23、 Spain, Sweden, Switzerland, Turkey and the United Kingdom. Endorsement notice The text of ISO 14244:2014 has been approved by CEN as EN ISO 14244:2016 without any modification. DIN EN ISO 14244:2016-10 EN ISO 14244:2016 (E) 3 ForewordISO (the International Organization for Standardization) is a wor
24、ldwide 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
25、 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 d
26、ocument 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 Direc
27、tives, 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 develo
28、pment 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 meaning of ISO s
29、pecific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 34, Food product
30、s, Subcommittee SC 2, Oleaginous seeds and fruits and oilseed meals.DIN EN ISO 14244:2016-10 EN ISO 14244:2016 (E)4 1 ScopeThis International Standard specifies a method for the determination of soluble proteins in potassium hydroxide solution in soya meals, rapeseed meals and sunflower pellets, whi
31、ch are then assayed using the Kjeldahl method as specified in ISO 5983-1 and ISO 5983-2.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cited applies. For
32、 undated references, the latest edition of the referenced document (including any amendments) applies.ISO 565, Test sieves Metal wire cloth, perforated metal plate and electroformed sheet Nominal sizes of openingsISO 5500, Oilseed residues SamplingISO 5502, Oilseed residues Preparation of test sampl
33、esISO 5983-1, Animal feeding stuffs Determination of nitrogen content and calculation of crude protein content Part 1: Kjeldahl methodISO 5983-2, Animal feeding stuffs Determination of nitrogen content and calculation of crude protein content Part 2: Block digestion and steam distillation method3 Pr
34、incipleThe sample is dispersed in a solution of potassium hydroxide of approximately 12,5 pH, stirred and centrifuged. Then, the nitrogen content of the clarified liquid is determined by the Kjeldahl method for crude protein and compared with the value of crude protein of the original sample.NOTE Th
35、e Kjeldahl method is described in ISO 5983-1 and ISO 5983-2.4 ReagentsWARNING 1 The tests, according to this International Standard, involve risks for persons and the possibility of releasing substances which might cause damage to the environment. For this reason, appropriate measures shall be taken
36、 to prevent risk, protect personnel, and avoid the release of the substances involved.WARNING 2 Attention shall be paid to preserving the environment in all phases of this activity. For further information, it is recommended to make reference to ASTM D4447, which describes the classification of the
37、kind of residues and pretreatment methods for their recovery or disposal.Use only reagents of recognized analytical grade.4.1 Potassium hydroxide.4.2 Potassium hydroxide solution, c(KOH) = 0,036 mol/l.Preparation: Dissolve 2,4 g of potassium hydroxide (mass fraction w = 85 g/100 g) in 1 000 ml of di
38、stilled water.DIN EN ISO 14244:2016-10 EN ISO 14244:2016 (E) 5 4.3 n-hexane or hexane mixed isomers or petroleum ether.5 ApparatusUsual laboratory apparatus and, in particular, the following.5.1 Sieve, 500 m for sunflower pellets and 250 m for soya and rapeseed meals (as specified in ISO 565).5.2 An
39、alytical balance, capable of weighting to the nearest 0,001 g.5.3 Stirrers vessels, of 150 ml capacity.5.4 Magnetic stirrer with revolutions per minute (r/min) indicator or mechanical rotary stirrer, composed of an axis, and allowing the centrifuge tubes to invert totally as the axis rotates.5.5 Gri
40、nder.5.5.1 Cutting mill, type of coffee grinder or grinder equipped with a grid or equivalent.5.5.2 Cyclone mill, or similar.5.6 Centrifuge, allowing reaching a relative acceleration of 800 g 100 g.The value of the rotational frequency, v, is calculated using Formula (1):vFd=423c(1)wherev is the rot
41、ational frequency, in revolutions per minute;d is the spinning diameter, in centimetres, measured between the ends of the opposite tubes, in rotation position;Fcis the relative centrifugal acceleration (in this case, 800 g).5.7 One-mark volumetric pipettes, of 25 ml capacity.5.8 Burette, of 100 ml c
42、apacity.5.9 Centrifuge tube or centrifugation ampoule.5.10 Filter paper, nitrogen free or glass pot, with a filter plate.6 SamplingSampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 5500.It is important that the laboratory recei
43、ves a sample which is truly representative and has not been damaged or changed during transport or storage.DIN EN ISO 14244:2016-10 EN ISO 14244:2016 (E)6 7 Preparation of test samplePrepare the test sample in accordance with ISO 5502.If the fat content of the sample is higher than 5 %, it shall be
44、defatted by cold extraction using n-hexane.8 Procedure8.1 Carry out the determination in duplicate.8.2 Grind the sample with a grinder or with any other apparatus which does not cause warming until it totally passes through a 250 m sieve for soya and rapeseed meals and through a 500 m sieve for sunf
45、lower pellets.Particle size greatly affects the final result of the analysis; therefore, it is recommended to carry out the milling with care.8.3 Weigh 1,5 g of the meal prepared as in 8.2, and place it in a 150 ml stirrers vessel. If a mechanical rotator stirrer is employed, the stirrers recipient
46、should be used instead of the stirrers vessel.8.4 Add 75 ml (5.8) of potassium hydroxide solution (4.2) and stir at minimum speed for 20 min to maintain all the solids in suspension. If a stirrer is utilized, use the centrifuge tube with the stirring sets at minimum speed.8.5 Transfer the totality o
47、f the liquid to a centrifugal tube or centrifugation ampoule and centrifuge for 10 min at a relative acceleration of 800 g.8.6 If some particles are still in suspension, filter the clarified liquid through filter paper or a glass pot to prevent the possible transfer of particles.8.7 Take 25 ml (5.7)
48、 aliquots of filtrate and determine the nitrogen content by the Kjeldhal method as described in ISO 5983-1 or ISO 5983-2.NOTE According to this procedure, each aliquot corresponds to 0,5 g of the original milled sample.8.8 The nitrogen content of the original milled sample shall be determined in duplicate using the Kjeldahl method as described in ISO 5983-1 or ISO 5983-2.9 Expression of resultsThe content of soluble
