1、BRITISH STANDARD BS EN ISO 5511:1997 Incorporating Amendment No.1 Oilseeds Determination of oil content Methodusing continuous-wave low-resolution nuclear magnetic resonance spectrometry (Rapidmethod) The European Standard EN ISO5511:1996 has the status of a BritishStandard ICS 67.200.20BSENISO5511:
2、1997 This BritishStandard, having been prepared under the directionof the Consumer Products and Services Sector Board, was published under theauthority of the Standards Board and comes into effect on 15January1997 BSI 04-2000 The following BSI references relate to the work on this standard: Committe
3、e reference AW/2 Draft for comment91/52786 DC ISBN 0 580 27010 6 Committees responsible for this BritishStandard The preparation of this BritishStandard was entrusted to Technical Committee AW/2, Oilseeds, upon which the following bodies were represented: Department of Trade and Industry (Laboratory
4、 of the Government Chemist) FOSFA International Grain and Feed Trade Association Leatherhead Food Research Association Ministry of Agriculture, Fisheries and Food National Farmers Union National Institute of Agricultural Botany Seed Crushers and Oil Processors Association Tropical Growers Associatio
5、n UnitedKingdom Agricultural Supply Trade Association Ltd. Amendments issued since publication Amd. No. Date Comments 9642 November 1997 Indicated by a sideline in the marginBSENISO5511:1997 BSI 04-2000 i Contents Page Committees responsible Inside front cover National foreword ii Foreword 2 1 Scope
6、 3 2 Normative references 3 3 Definitions 3 4 Principle 3 5 Materials 3 6 Apparatus 3 7 Sampling 4 8 Preparation of the test sample 4 9 Procedure 4 10 Expression of results 5 11 Repeatability 6 12 Test report 6 Annex A (informative) Bibliography 7 Annex ZA (normative) Normative references to interna
7、tional publicationswiththeir relevant European publications 8 List of references Inside back coverBSENISO5511:1997 ii BSI 04-2000 National foreword This BritishStandard has been prepared by Technical Committee AW/2 and is the English language version of EN ISO5511:1996 Oilseeds Determination of oil
8、content Method using continuous-wave low-resolution nuclear magnetic resonance spectrometry (Rapid method), published by the European Committee for Standardization (CEN). This BritishStandard has been published to fulfil BSIs obligation to publish all approved European Standards. It is identical wit
9、h ISO5511:1992 published by the International Organization for Standardization (ISO) and in the preparation of which the UK played a full part. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct appl
10、ication. Compliance with a British Standard does not of itself confer immunity from legal obligations. Cross-references Publication referred to Corresponding BritishStandard ISO542:1990 BS EN ISO542:1995 Oilseeds Sampling ISO659:1988 BS4289 Methods for analysis of oilseeds Part4:1989 Determination o
11、f hexane extract (or light petroleum extract) called “oil content” ISO664:1990 BS EN ISO664:1995 Oilseeds Reduction of laboratory sample to test sample ISO665:1977 BS EN ISO665:1995 Oilseeds Determination of moisture and volatile matter content ISO771:1977 BS4325 Methods for analysis of oilseed resi
12、dues Part1:1978 Determination of moisture and volatile matter content ISO5725:1986 a BS5497 Precision of test methods Part1:1987 Guide for the determination of repeatability and reproducibility for a standard test method by interlaboratory tests a ISO5725:1986, to which informative reference is made
13、 in the text, has been superseded by ISO5725-1:1994, ISO5725-2:1994, ISO5725-3:1994, ISO5725-4:1994 and ISO5725-6:1994 which are identical with BS ISO5725 Accuracy (trueness and precision) of measurement methods and results, BSISO5725-1:1994 General principles and definitions, BSISO5725-2:1994 Basic
14、 methods for the determination of repeatability and reproducibility of a standard measurement method, BSISO5725-3:1994, Intermediate measures of the precision of a standard measurement method, BSISO5725-4:1994 Basic methods for the determination of the trueness of a standard measurement method, and
15、BSISO5725-6:1994 Use in practice of accuracy values. Summary of pages This document comprises a front cover, an inside front cover, pagesi andii, theEN ISO title page, pages2 to8, an inside back cover and a back cover. This standard has been updated (see copyright date) and may have had amendments i
16、ncorporated. This will be indicated in the amendment table on the inside front cover.EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO5511 September 1996 ICS 67.200.20 Descriptors: Agricultural products, oilseeds, chemical analysis, determination of content, oils, nuclear magnetic resonance m
17、ethod, spectrometric method English version Oilseeds Determination of oil content Method using continuous-wave low-resolution nuclear magnetic resonance spectrometry (Rapid method) (ISO5511:1992) Graines olagineuses Dtermination de la teneur en huile Mthode par spectromtrie de rsonance magntique nuc
18、laire basse rsolution et onde continue (Mthode rapide) (ISO5511:1992) lsamen Bestimmung des lgehaltes Kernresonanzspektroskopie mit niedriger Auflsung (Schnellverfahren) (ISO5511:1992) This European Standard was approved by CEN on1995-12-06. CEN members are bound to comply with the CEN/CENELEC Inter
19、nal 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 references concerning such national standards may be obtained on application to the Central Secretariat or to any CEN member
20、. 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 Secretariat has the same status as the official versions. CEN members a
21、re the national standards bodies of Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and UnitedKingdom. CEN European Committee for Standardization Comit Europen de Normalisation Europisches Kom
22、itee fr Normung Central Secretariat: rue de Stassart 36, B-1050 Brussels 1996 Copyright reserved to CEN members Ref.No.ENISO5511:1996EENISO5511:1996 BSI 04-2000 2 Foreword The text of the International Standard from Technical Committee ISO/TC34, Agricultural food products, of the International Organ
23、ization for Standardization (ISO) has been taken over as a European Standard by Technical Committee CEN/TC307, Oilseeds, vegetable and animal fats and oils and their by-products Methods of sampling and analysis, the secretariat of which is held by ANFOR. This European Standard shall be given the sta
24、tus of a national standard, either by publication of an identical text or by endorsement, at the latest by March1997, and conflicting national standards shall be withdrawn at the latest by March1997. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the follo
25、wing countries are bound to implement this European Standard: Austria, Belgium, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the UnitedKingdom. NOTENormative references to International Standards are lis
26、ted in Annex ZA (normative).ENISO5511:1996 BSI 04-2000 3 1 Scope This International Standard specifies a rapid method for the determination of the oil content of oilseeds using continuous-wave low-resolution nuclear magnetic resonance spectrometry. Under normal conditions of use, it does not apply t
27、o oilseeds which do not yield oil which is completely liquid at20 C (e.g.shea, palm, illipe, cocoa, etc.). This method has been successfully tested on the following oilseeds: rapeseed, soya, sunflower seed and groundnuts. NOTE 1The reference method for the determination of the oil content of oilseed
28、s is specified in ISO659. 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 t
29、o 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
30、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. ISO 771:1977, Oilseed residues Determination of moisture and volatile matter content. 3 Defi
31、nitions For the purposes of this International Standard, the following definitions apply. 3.1 oil content the mass fraction of organic substances, which are liquid at the temperature of measurement (in principle20 C) of the oilseeds, determined using the method specified in this InternationalStandar
32、d the oil content is expressed as a percentage by mass 3.2 single test result result obtained by carrying out a specified test method one time according to the prescribed procedure 3.3 repeatability conditions conditions where mutually independent test results are obtained with the same method on id
33、entical test material in the same laboratory by the same operator using the same equipment within short intervals of time ISO5725:1986,3.1.7 4 Principle Determination using continuous-wave low-resolution nuclear magnetic resonance (NMR) spectrometry of the content of liquid components containing hyd
34、rogen which are present in oilseeds which have been previously dried at103 C 2 C, and taking into account the effect of solids (oilseedresidue). 5 Materials 5.1 Calibration oil, crude oil from seeds of the same botanical species and of similar geographical origin and chemical composition to those of
35、 the seeds for analysis, extracted in the laboratory carrying out the analysis, in accordance with the method specified in ISO659, less than1 month previously. Store the oil under dry conditions preventing oxidation. 5.2 Oilseed residue, from seeds of the same botanical species, and of similar geogr
36、aphical origin and chemical composition, to those of the seeds for analysis, from which the oil has been extracted in the laboratory carrying out the analysis, in accordance with the method specified in ISO659, less than1month previously. 6 Apparatus Usual laboratory apparatus and, in particular, th
37、e following. 6.1 Apparatus required for the drying method (seeISO665). 6.2 Continuous-wave low-resolution NMR spectrometer 6.3 Measuring tubes, preferably with closures, suitable for use with the NMR spectrometer(6.2) and of the largest possible capacity, made from a non-conducting non-magnetic mate
38、rial which does not contain hydrogen e.g.glass or polytetrafluoroethylene (PTFE). 6.4 Desiccator, containing an efficient desiccant.ENISO5511:1996 4 BSI 04-2000 7 Sampling It is important that the sample received by the laboratory be truly representative and not damaged or changed during transport a
39、nd storage. Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO542. 8 Preparation of the test sample Prepare the test sample in accordance with ISO664. Then remove any particles of ferrous metals using a magnet. NOTE 2Particles o
40、f ferrous metals will falsify the results. 9 Procedure IMPORTANT Since the effect of temperature variation on the results obtained is very large (theoil response decreases by approximately0,3% per degree Celsius), all operations for calibrating the instrument and all measuring operations shall be ca
41、rried out strictly at the same temperature. It is recommended, if the necessary apparatus is available, to control thermostatically the “effective” part of the instrument and to place the seeds, before measurement, in insulated metal blocks at the measuring temperature. Otherwise, carry out a simpli
42、fied calibration of the apparatus every30min (see9.2.5). 9.1 Check on repeatability (if required) If it is required to establish whether the repeatability requirement (see clause11) is met, carry out two single determinations, each including the two intermediate determinations(9.6), under repeatabil
43、ity conditions (see3.3). 9.2 Calibration of the instrument 9.2.1 Adjust the NMR spectrometer(6.2) in accordance with the manufacturers instructions, then adjust to zero after placing an empty measuring tube(6.3) in the magnetic field. 9.2.2 Into four measuring tubes identical to that used for the ad
44、justment (i.e.also giving a reading of zero when they are placed empty in the magnetic field), weigh, to the nearest0,01g,5g,10g,20g, and, if the apparatus so permits,30g of the calibration oil(5.1), taking care that no oil adheres to the sides of the tubes above the effective part. 9.2.3 Measure th
45、e response of the instrument for each of the four tubes, taking andas the mean values of five readings of the integrator on each of the four tubes, during the integration time giving the best repeatability of measurement, using a level of radiofrequency energy sufficient to obtain a satisfactory sig
46、nal in relation to the background noise, but not producing more than approximately1% saturation. The correct selection of the level of saturation may be carried out by the operator if the relation between the radiofrequency energy and the saturation is known. If not, the correct adjustment of the le
47、vel of saturation shall be obtained from the manufacturer of the instrument. 9.2.4 Draw a straight line representing the values ofas a function of the mass of oil placed in the tubes. This line shall pass through the origin. If it does not, contact the manufacturer to adjust the instrument or make t
48、he necessary adjustment if the instrument so permits. 9.2.5 Check the calibration of the instrument regularly (if possible, once each day). If the instrument and the samples are not thermostatically controlled, check the variation in the gradient of the calibration line by measuring the response of
49、a20g or30g sample every30min. 9.3 Test portion Weigh, to the nearest0,01g, a sufficient quantity of the prepared test sample (clause8), but at least20g, to fill the effective part of a measuring tube(6.3). NOTE 3The effective part corresponds to the tube height included in the magnet airgap (approximately20g of seeds) but some instruments cannot accommodate20g of some species of seed. If less than20g of seed is used, the test portion is less representative and, in this case, several successive measurements should be take
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