1、STD-BSI BS EN IS0 LOSbS-ENGL 1998 W Lb24bb9 0731824 757 W BRITISH STANDARD Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed nuclear magnetic resonance spectrometry The European Standard EN IS0 10565:1998 has the status of a British Standard ICs 67.200.20 BS EN IS
2、0 10565: 1998 BS 4289-11:1998 - nimi NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW %sa STD*BSI BS EN IS0 1OSbS-ENGL 1998 E Lb24bb9 0733825 b73 W Amd. No. Date BS EN IS0 10666:1998 Text affected National foreword This British Standard is the English language version of EN IS0
3、 10561998. It is identical with IS0 10565A998. It supersedes BS EN IS0 10565:1997 which is withdrawn. The UK participation in its prepamtion was entrusted to Technid Committee AWE, Oilseeds and residues, which has the responsibfity to: - aid enquirers to understand the text; - present to the respons
4、ible internatio - monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secrem. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normally include an
5、annex which lists normative references to international publications with their corresponding European publications. The British Standards which implement these international or European publications may be found in the BSI Standards Catalogue under the section entitled “International Standards Corr
6、espondence Index”, or by using the ”Find” facility of the BSI Standards Elecronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their corred application. Compliance with a British Standard does not
7、 of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the EN IS0 title page, the EN IS0 foreword page, the IS0 titie page, page ii, pages 1 to 12, the annex ZA page and a back cover. This British Standard, having been prepar
8、ed under the direction of the Consumer Products and Services Sector Board, was published under the authority of the Standards Board and comes into effect on 15 November 1998 O BSI 1998 ISBN O 680 30424 8 STD-BSI BS EN IS0 LOSbS-ENGL L998 W Lb24bb7 073L82b 52T W EUROPEAN STANDARD NORME EUROPENNE EURO
9、PISCHE NORM EN IS0 10565 ICs 67,200 Descriptors: see IS0 document Supersedes EN IS0 10565:1997 English version Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed nuclear magnetic resonance spectrometry (IS0 10565: 1998) Graines olagineuses - Dtermination simultane
10、de la teneur en huile et en eau - Mthode par spectromtrie par rsonance magntique nud8aire pulSee (IS0 10565:1998) 6isamen - Gleichzeitige Bestimmung des oi- und Wassergehaites - Verfahren mit gepulster Kernresonanzspektroskopie (IS0 1056!5:1998) This European Standard was approved by CEN on 15 Augus
11、t 1998. CEN members are bound to compiy with the CEWCENELEC 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 bibliographicai references concerning such national standards may be obtain
12、ed 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 into its own language and notified to the Central Secret
13、ariat has the same status as the offlcial 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, Spain, Sweden, Switzerland and United Kingdom. ENROPEA
14、N COMMITEE FOR STANDARDIZATION EUROPISCHES KOMITEE FUR NORMUNG COMITE EUROPBEN DE NORMALISATION 0 1998 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN IS0 10565:1998 E STD-BSI BS EN IS0 LD5bS-ENGL 1998 II Lb24bb7 0733827 4bb = EN I
15、S0 10565:1998 Foreword The text of the International Standard IS0 105651998 has been prepared by Technical Committee ISOTTC 34 “Agricultural food products“ in collaboration with Technical Committee CENTC 307 “Oilseeds, vegetable and animal fats and oils and their by-products - Methods of sampling an
16、d analysis“, the secretariat of which is held by AFNOR. This European Standard supersedes EN IS0 10565:1997. 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 February 1999, and conflicting national
17、 standards shall be withdrawn at the latest by February 1999. According to the CENKENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
18、Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of the International Standard IS0 10565:1998 was approved by CEN as a European Standard without any modification. NOTE: Normative references to Internati
19、onal Standards are listed in annex ZA (normative). INTERNATIONAL STANDARD IS0 10565 Second edition 1998-08-1 5 Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed nuclear magnetic resonance spectrometry Graines olagineuses - Dtermination simultane de ia teneur en hu
20、ile et en eau - Mthode par spectromtrie par rsonance magntique nuclaire pulse Reference number IS0 10565: 1998(E) STD.BS1 BS EN IS0 LSbS-ENGL 3778 Lb24bb9 0733829 237 a EN IS0 10565:1998 Foreword IS0 (the International Organization for Standardization) is a worldwide federation of national standards
21、 bodies (IS0 member bodies). The work of preparing International Standards is normally carried out through IS0 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 organiza
22、tions, governmental and non- governmental, in liaison with ISO, also take part in the work. IS0 collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. Draft International Standards adopted by the technical committees are circ
23、ulated to the member bodies for voting. Publication as an International Standard requires approval by at least 75 Oh of the member bodies casting a vote. International Standard IS0 10565 was prepared by Technical Committee ISOTTC 34, Agricultural food products, Subcommittee SC 2, Oleaginous seeds an
24、d fruits. This second edition cancels and replaces the first edition (IS0 10565:1993), which has been technically revised. Annexes A and 6 of this Intemational Standard are for information only. Descriptors: agricultural products, plant products, oilseeds, tests, determination of content, oils, wate
25、r, nuclear magnetic resonance method. ii STD.BSI BS EN IS0 105b5-ENGL 1998 Lb24bb9 073L83O T50 EN IS0 10565:1998 Oilseeds - Simultaneous determination of oil and water contents - Method using pulsed nuclear magnetic resonance spectrometry 1 Scope This Intemational Standard specifies a rapid method f
26、or the determination of the oil and water contents of commercial oilseeds using pulsed nuclear magnetic resonance (NMR). - i It is applicable to rapeseeds, soya beans, linseeds and sunflower seeds with a water content less than 10 *h. For seeds with higher water contents, drying is necessary before
27、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
28、 values are generally higher than those obtained by the drying method (IS0 665). - i - VI - * * 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 indic
29、ated were valid. All standards are subject to revision, and parties to agreements based on this Intemational Standard are encouraged to investigate the possibility of applying the most recent editims of the standards indicated below. Members of IEC and IS0 maintain registers of currently valid Inter
30、national Standards. IS0 659:1988, Oilseeds - Determination of hexane extract (or light petroleum extracf), called “oil content“. IS0 664:1990, Oilseeds - Reduction of laboratory sample to fest sample. IS0 665:1977, Oilseeds - Determination of moisture and volatile matter content. 3 Principle Inserti
31、on 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 maxi
32、mum amplitude of this signal is proportional to the total number of protons from the water and oil phases of the sample. 1 STD.BSI BS EN IS0 1OSbS-ENGL 1998 Lb24bb9 0731831 997 0 EN IS0 10565:1998 Application of the second RF pulse, a so-called 180“ pulse, to produce a spin-echo signal when only the
33、 signal from the oil phase contributes to the FID. NOTE 1 The maximum amplitude of this echo signal is proporional 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 bet
34、ween 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
35、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 IS0 658 l. 4.1 Samples for moisturecontent calibration In order to obtain a reliable calibration curve, it is recommended that t
36、he 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 IS0 665 just prior to calibration. 4.2 Samples for oil-content calibration Samples of oils
37、eeds 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 IS0 659. 5
38、 Apparatus Usual laboratory apparatus and, in particular, the following. 5.1 oilseeds, and meeting the precision requirements of 11.2 and 11.3. Pulsed low-resolution NMR spectrometer, suitable for measurement of the oil content and water content of The instruments parameters shall be in accordance w
39、ith the instnictionslspecifications 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 H,O1 g. This
40、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 OC i 2 OC. 5.5 Dishes, made of glass or metal, of diameter 7 cm to 10 cm, and provided wi
41、th lids. 2 STD. BSI BS EN IS0 LSbS-ENGL EN IS0 10565:1998 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 IS0 542 2. It is important that the laboratory receive a samp
42、le 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 IS0 664. Remove from the prepared test sample all metallic objects (e.g. staples, needles, etc.). Whole seeds shall be homogeneous
43、 and, as far as possible, free from impuiiies. 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 users manual. Ensure tha
44、t all operations during calibration and measurement are carried out under the same conditions and, in particular, at the same temperature (12 OC). - e - E - i i A minimum of three calibration samples is necessary, although more than three samples may be used. * * m 8.1.2 Enter the parameters for the
45、 measurements (pulse sequence, attenuation, etc.) of the oil or water content (as applicable) into the 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 of 16 s. 8.
46、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 ma
47、ss 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 sa
48、mple 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 obt
49、ained 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 IS0 659 and IS0 665 respectively, or repeat the calibration procedure using three (or more) other calibration samples. 3 STD.BSI BS EN IS0 10565-ENGL 1778 6 1624bb7 0731833 7bT EN IS0 10565:1998 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.
