BS EN ISO 10565-1998 Oilseeds - Simultaneous determination of oil and water contents - Methods using pulsed nuclear magnetic resonance spectrometry《油料种子 油和水分含量的同时测定 脉冲核磁共振光谱测定法》.pdf

1、BRITISH STANDARD BS EN ISO 10565:1998 BS4289-11: 1998 Oilseeds Simultaneous determination of oil and water contents Method using pulsed nuclear magnetic resonance spectrometry The European Standard EN ISO10565:1998 has the status of a British Standard ICS 67.200.20BSENISO 10565:1998 This British Sta

2、ndard, having been prepared under the directionof the Consumer Products and Services Sector Board, was published under theauthority of the Standards Board and comes into effecton 15November1998 BSI05-1999 ISBN 0 580 30424 8 National foreword This British Standard is the English language version of E

3、N ISO10565:1998. It is identical with ISO10565:1998. It supersedes BS EN ISO10565:1997 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/2, Oilseeds and residues, which has the responsibility to: aid enquirers to understand the text; present to the r

4、esponsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained o

5、n request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement these internationa

6、l or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of

7、a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, pages i and ii, theEN ISO title page, pag

8、e2, the ISO title page, page ii, pages1to7 and abackcover. This standard has been updated (see copyright date) and may have had amendments incorporated. This will be indicated in the amendment table on the inside front cover. Amendments issued since publication Amd. No. Date CommentsBSENISO10565:199

9、8 BSI 05-1999 i Contents Page National foreword Inside front cover Foreword 2 Foreword ii 1 Scope 1 2 Normative references 1 3 Principle 1 4 Calibration samples 1 5 Apparatus 1 6 Sampling 2 7 Preparation of test sample 2 8 Calibration procedure 2 9 Procedure 4 10 Expression of results 5 11 Precision

10、 5 12 Test report 5 Annex A (informative) Results of interlaboratory tests 6 Annex B (informative) Bibliography 7 Annex ZA (normative) Normative references to international publicationswiththeir relevant European publications 7 Table A.1 Interlaboratory test on oil content 6 Table A.2 Interlaborator

11、y test on water content 6ii blankEUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO10565 August1998 ICS67.200 Supersedes EN ISO10565:1997 Descriptors: See ISO document English version Oilseeds Simultaneous determination of oil and water contents Method using pulsed nuclear magnetic resonance s

12、pectrometry (ISO10565:1998) Graines olagineuses Dtermination simultane de la teneur en huile et en eau Mthode par spectromtrie par rsonance magntique nuclaire pulse (ISO10565:1998) lsamen Gleichzeitige Bestimmung des l- und Wassergehaltes Verfahren mit gepulster Kemresonanzspektroskopie (ISO10565:19

13、98) This European Standard was approved by CEN on15August1998. 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 ref

14、erences concerning such national standards may be obtained on application to the Central Secretariat 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

15、into its own language and notified to the Central Secretariat has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal

16、, Spain, Sweden, Switzerland and United Kingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Komitee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for C

17、EN national Members. Ref. No. EN ISO10565:1998EENISO10565:1998 BSI 05-1999 2 Foreword The text of the International Standard ISO10565:1998 has been prepared by Technical Committee ISO/TC34 “Agricultural food products” in collaboration with Technical Committee CEN/TC307 “Oilseeds, vegetable and anima

18、l fats and oils and their by-products Methods of sampling and analysis”, the secretariat of which is held by AFNOR. This European Standard supersedes EN ISO10565:1997. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsemen

19、t, at the latest by February1999, and conflicting national standards shall be withdrawn at the latest by February1999. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, C

20、zech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard ISO10565:1998 was approved by CEN as a European Standard without

21、any modification. NOTENormative references to International Standards are listed in Annex ZA (normative).ENISO10565:1998 ii BSI 05-1999 Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing

22、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 liais

23、on 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

24、 as an International Standard requires approval by at least75% of the member bodies casting a vote. International Standard ISO10565 was prepared by Technical Committee ISO/TC34, Agricultural food products, Subcommittee SC2, Oleaginous seeds and fruits. This second edition cancels and replaces the fi

25、rst edition (ISO10565:1993), which has been technically revised. Annex A and Annex B of this International Standard are for information only. Descriptors: Agricultural products, plant products, oilseeds, tests, determination of content, oils, water, nuclear magnetic resonance method.ENISO10565:1998

26、BSI 05-1999 1 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 than1

27、0%. For seeds with higher water contents, drying is necessary before the oil content can be determined by pulsed NMR. NOTE 1This 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

28、liquid at the temperature of measurement. NOTE 2The reproducibility values are generally higher than those obtained by the drying method (ISO665). 2 Normative references The following standards contain provisions which through reference in this text, constitute provisions of this International Stand

29、ard. 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 IE

30、C and ISO maintain registers of currently valid International Standards. ISO659:1988, Oilseeds Determination of hexane extract (or light petroleum extract), called “oil content”. ISO664:1990, Oilseeds Reduction of laboratory sample to test sample. ISO665:1977, Oilseeds Determination of moisture and

31、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 intense90 radiofrequency (RF) pulse which excites all the hydrogen nuclei. Recording of the free induction dec

32、ay (FID) following the90 pulse. The maximum amplitude of this signal is proportional to the total number of protons from the water and oil phases of the sample. Application of the second RF pulse, a so-called180 pulse, to produce a spin-echo signal when only the signal from the oil phase contributes

33、 to the FID. NOTE 1The 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 prop

34、ortional to the water content. Automatic conversion of the measured signals, after suitable calibration of the apparatus, into percentages of oil or water. NOTE 2Simultaneous indications of the oil and water contents can be given by some spectrometers equipped with a minicomputer and a specific prog

35、ram. 4 Calibration samples Calibration samples shall be homogeneous and free from impurities. A definition of impurities is given in ISO658 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 sa

36、mples be less than10% for all seeds. The water content of seeds can vary depending on storage conditions. Water content shall therefore be determined in accordance with ISO665 just prior to calibration. 4.2 Samples for oil-content calibration Samples of oilseeds shall be of the same species as the t

37、est 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 ISO659. 5 Apparatus Usual laboratory apparatus and,

38、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 of11.2 and11.3. The instruments parameters shall be in accordance with the instructions/specifications from the

39、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 0,01g. This equipment may be linked to the NMR spectrometer

40、 so that the sample mass is recorded directly by the NMR, or linked to a minicomputer (see NOTE2 in clause3). 5.4 Drying oven, capable of being maintained at103 C 2 C. 5.5 Dishes, made of glass or metal, of diameter7cm to10cm, and provided with lids. 5.6 Desiccator, containing an efficient desiccant

41、.ENISO10565:1998 2 BSI 05-1999 6 Sampling Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO542 2. It is important that the laboratory receive a sample which is truly representative and has not been damaged or changed during tra

42、nsport or storage. 7 Preparation of test sample Prepare the test sample in accordance with ISO664. 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 Gener

43、al 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 users manual. Ensure that all operations during calibration and measurement are carried out under the sa

44、me 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 th

45、e NMR spectrometer, following the manufacturers recommendations, and specify a code number under which the calibration curve is to be stored. The total measurement time shall be a minimum of16s. 8.1.3 Set the apparatus to the calibration mode. 8.1.4 Introduce a portion of the first calibration sampl

46、e 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. NOTEA manual feed of the mass ot the calibration sample into the NMR spectrometer is also possible. 8.1.5 Enter, as applicable, the

47、 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.

48、1.7 Repeat steps8.1.4 to8.1.6 for the two (ormore) other calibration samples. 8.1.8 Calculate automatically or manually the calibration parameters of the calibration curve using the results obtained in8.1.6 and8.1.7. The correlation coefficient shall normally be greater than0,95. If this is not the

49、case, check the values obtained using the reference methods specified in ISO659 and ISO665 respectively, or repeat the calibration procedure using three (or more) other calibration samples. Store the calibration curve under the code number chosen in step8.1.2. 8.1.9 Complete the oil-content calibration curve by using an empty tube and by repeating steps8.1.4 to8.1.6. This part of the method is not applicable to the water content calibration curve. 8.2 Calibration procedure for the determination of water conte