1、 - STD.BSI BS EN IS0 5511-ENGL 1777 = Lb24bb9 Ob58338 TL5 BRITISH STANDARD Oilseeds - Determination of oil content - Method using continuous-wave low-resolution nuclear magnetic resonance spectrometry (Rapid method) The European standard EN IS0 5511 : 1996 has the status of a British standard ICs 67
2、.200.20 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW BS EN IS0 5511 : 1997 Incqmting Amendment No. 1 BS EN IS0 8811 : 1997 Issue 2, November 1997 9642 The foliowing BSI references relate to the work on this standard: Committee reference AWE2 Draft for comment 9i52786 DC - I
3、SBN O 680 27010 6 Committees responsible for this British Standard November 1997 Indicated by a sideline in the margin The preparation of this British Standard was entrusted to Technical Committee AWD, oilseeds, upon which the following bodies were represented: Depariment of We and Industry (Laborat
4、ory of the Government Chemist) FOSFA International Grain and Feed li-ade 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 Tbpicai Growers Associa
5、tion United Kingdom Agricultural Supply li-ade Association Ltd. This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Board, was pubiished under the auhoriy of the Standards Board and comes into effect on 15 January 1997 O BSI 1997 Amendments is
6、sued since publication Amd No. ID is the mass, In grams, of the test portion before drying (9.3); is the mass, in grams, ofcrude oil corre- sponding to the response R, read from the callbration line of the instrument (9.2); is the mean value of the responses of the instrument for the test portion, d
7、etermined in 9.5; is the response of the instrument corre- sponding to the mass % of crude oil, read from the calibration line of the instrument (9.2). 10.2 Calculate lhe response factor of the residue using the formula Tx-x100% w, = - where Wr m, is the response factor, expressed as a per- centage
8、by mass, of the residue; is !he mass, in grams, of the dried oilseed residue from which the oil has been ex- tracted, used in 9.6; STD-BSI BS EN IS0 5511-ENGL L997 1b24bb9 b58348 Yb4 Page 6 EN IS0 5511 : 1996 Issue 2, November 1997 7 is the mean value of the responses of the Express the result to th
9、e nearest 0,l YO (mlm). instrument for the mass m, of dried oilseed residue from which the oil has been ex- NOTE 7 For a given type of seed, the respmse of the tracted, determined in 9.6; residue is generally independent of the samples. For ex- ample, in the case of rapeds (see note 6 in 9.6), the o
10、il content of the seeds is approximately equal to % and Rx have the same meanings as in 10.1. 10.3 Calculate the oil content of the seeds using the formula W= w- where W is the oil content of the seeds, ex- pressed as a percentage by mass; is the moisture content of the seeds, expressed as a percent
11、age by mass, determined in accordance with IS0 665; w, and IV, have the same meanings as in 10.1 and 10.2 respectively. Take as the result the arithmetic mean of the results of the two determinations (9.7), provided that their difference does not exceed 0.4 YO (m/m). if their dif- WH w = w, - 0,30 ?
12、O (m/m) 11 Repeatability The difference between two cingle test results (see 3.2) obtained under repeatability conditions (see 3.3) shall not exceed 0,6 YO (mim). Reject both results if their absolute difference ex- ceeds 0,6 YO (m/m) and carry out two new single determinations (each time according
13、to clauses 9 and IO). 12 Test report The test report shall specify the method used, the results obtained, the name and type of NMR spec- trometer used and, if applicable, all adjustments made. It shall also mention all operating details not specified in this International Standard, or regarded as op
14、tional, together with details of any incidents which may have influenced the results. ference does exceed 0.4 % (m/m)i discard the re- sults of the two determinations and repeat the procedure (clause 9). The test report shall include all information necess- ary for the complete identification of the
15、 sample. 0 BSI 1997 STD.BSI BS EN IS0 5511-ENGL 1997 1bilqbbS Ob583L19 ATO Page 7 EN IS0 6611 : 1996 Annex A (informative) Bibliography l IS0 542:199. Oilseeds - Sampling. 2 IS0 57251986, Precision of test methods - Determination of repeatability and reproducibility for a stan- dard test method by i
16、nter-laboratory tests. STD.BSI BS EN IS0 55LL-ENGL 1997 = Lb24bb Ob58350 512 Page 8 EN IS0 6611 : 1996 Annex ZA (normative) Normative references to international publications with their relevant European publications This European Standard incorporates by dated or undated reference, provisions from
17、other publications. These normative references are cited at the appropriate piaces in the text and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment
18、 or revision. For undated references the latest edition of the publication referred to applies. Publication Year Itie EN Year IS0 664 1990 Weeds - Reduction of laboratory sample to EN IS0 664 1995 Is0 665 1977 Oilseeds - Determination of moisture and EN IS0 665 1995 test sampk volatile mutter conten
19、t O ES1 1997 STD-BSI BS EN IS0 551L-ENGL 1997 D Lb24bb9 Ob58351 459 D BS EN IS0 5511 : 1997 List of references See national foreword O BSI 1997 BS EN IS0 5511 : 1997 BSI 389 Chiswick High Road London w4 4AL BSI - British Standards Institution BSI is the independent Monal body responsible for prepari
20、ng British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Contract requirements A British Standard does not purport to include all the necessary provisions of a contract, Users of British Stan- are responsible for their
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28、lude the free use, in the course of implementing the standard, of necessary detaiis such as symbols, and size, type or grade designations. If these details are to be used for any other purpose than implementation then the prior written permission of BSI must be obtained If permisSion is granted, the
29、 tem may include royalty payments or a licensing agreement. Details and advice can be obtained from the Copyright Manager, BSI, 389 Chiswick High Road, London W4 4AL STDmBSI BS EN IS0 5511-ENGL 1997 = 1b24bb9 Ob58353 221 AMD 9642 Amendment No. 1 published and effective from 15 November 1997 to BS EN
30、 IS0 5511 : 1997 Oilseeds - Determination of oil content - Method using continuous-wave low-resolution nuclear magnetic resonance spectrometry (Rapid method) Instructions for replacement of pages Where ony one of the two pages on each sheet has been updated, the other page has been reprinted Front c
31、over and inside front cover Replace the pages aandb Insert the pages immediately after the inside front cover 6and6 Replace the pages You may wish to retain the superseded pages, e.g. for reference purposes, if so please mark them Superseded by issue X, where X is the appropriate issue number. If yo
32、u do not wish to retain the superseded pages, please destroy them. - STD-BSI BS EN IS0 5511-ENGL 1777 Lb24bb7 0b.58354 Lb8 BRITISH STANDARD Oilseeds - Determination of oil content - Method using continuous-wave low-resolution nuclear magnetic resonance spectrometry (Rapid method) The European Standa
33、rd EN IS0 5511 : 1996 has the status of a British standard ICs 67.200.20 NO COPPING W“0UT BSI PERMISSION EXCEPT AS PERMlTED BY COPYRIGHT LAW BS EN IS0 5511 : 1997 BS EN IS0 5511 : 1997 he 2, November 1997 AmdNo. Date 9642 November 1997 Comm Britisl Text affected Indicated by a sideline in the margin
34、 ttees responsible for this Standard “he preparation of this British Standasd was entrusted to Technical Committee AWB, Oilseeds, upon which the following bodies were represented: Department of li-ade and Industry (Laboraitory of the Government Chemist) FOSFA International Grain and Feed We Associat
35、ion Leatherhead Food Research Association Ministsy of Agriculture, Fisheries and Food National Farmers Union Nd0na.l Institute of Agricultural Botany Seed Cmhers and Oil Processors Association li-opical Growers Association United Kingdom Agricultural Supply li-ade Association Ltd. This British Stand
36、ard, having been prepared under the direction of the Consumer Products and Services Sector Board, was published under the authoriq of the Standards Board and comes into effect on 16 January 1997 Q BSI 1997 The foliowing BSI references relate to the work on this standard Committee reference AW/2 Draf
37、t for cornerf QU52786 DC ISBN O 580 27010 6 STD-BSI BS EN IS0 5511-ENGL 1777 1b24bb7 Ob5835b T30 he 1, November 1997 BS EN IS0 6611 : 1997 Issue Onginal Original Original Original Origind I original 2 Summary of pages The foliowing table identifies the current issue of each page. issue 1 indicates t
38、hat a page has been introduced for the first time by amendment. Subsequent issue numbers indicate an updated page. Vertical sidelining on repiacement pages indicates the most recent changes (amendment, addition, deletion). Front cover hide front cover a b 1 2 3 Issue II Page 2 2 1 blank Original Ori
39、ginal Originai 4 5 6 7 8 Inside back cover Back cover * u2 * O BSI 1997 a STD-BSI BS EN IS0 55LL-ENGL 1997 D Lb2LIbbS Ob58357 977 D 9.3 lest portlon Weigh, to the nearest 0,Ol g. a sufficient quantity of the prepared test sample (clause 8), but at least 20 g, to fill the effective part of a measurin
40、g tube (6.3). NOTE3 The effective part corresponds to the tube height included in the magnet airgap (approximately 20 g of seeds) but some instruments cannot accommodate 20 g of me species of seed. If less than 20 g of seed is used, the test portion is less representative and, in this case, several
41、successive measurements shouid be taken. 9.4 Drying Dry the test portion and determine its moisture con- tent in accordance with the method specified in IS0 665. Place the desiccator (6.4) containing the dried seeds in immediate proximity to the NMR spectrometer (6.2) in a room in which the temperat
42、ure (generally about 20 “C) does not show sudden variations and leave for at least 3 h before carrying out the deter- mination so that the seed and the apparatus are at the same temperature. = NOTE 4 If possible, use a temperature-controlled room. - m - II 9.5 Measurement E * * rn Quantitatively and
43、 rapidly transfer the dry seeds into a measuring tube (6.3) identical to that used for the calibration. If possible, close the tube to prevent absorption of moisture. Without altering the adjustment of the inarument, measure the response for the tube. Let R be the mean value of this response for fiv
44、e readings of the integrator using the integration time chosen pre- viously. 9.6 Correction for oilseed residue 9.6.1 Into a measuring tube (6.3) identical to that used for the calibration, weigh, to the nearest 0,Ol g, a sufficient quantity (mass ni,) of dried oil- seed residue from which the oil h
45、as been extracted (5.2) to fill the effective part of the tube. Keep it at room temperature. NOTES Just before use, dry the residue at 103 “C f 2 “C in accordance with the method specified in IS0 771, and cool in the desiccator (6.4). 9.6.2 Without altering the adjustment of the instru- ment, measur
46、e the response-r the tube and take as the result the mean value, R, of this response for five readings of the integrator using the integration time chosen previously. Page 6 EN IS0 6611 : 1996 9.8.3 Repeat successively the operations described in 9.6.1 and 9.6.2 a further five to ten times, using th
47、e samemass ni, of the dried oilseed residue (9.6.1). Take 7 as the mean value of the mean responses obtained. This value needs to be determined only about once per month. NOTE6 As a guide, rapeseed data have shown that, without correction, this method gives higher results than the reference method s
48、pecified in IS0659 by approxi- mately, on average, 030 % (m/m). 9.7 Number of determinations Carry out a minimum of two determinations on test portions taken from the same test sample, particu- larly if the sample is heterogeneous. 10 Expression of results 10.1 Calculate the apparent seeds using the
49、 formula RX+X loo % Rxxm, wa = where oil content of the wa is the apparent oil content, expressed as a percentage by mass, of the seeds; n is the mass, in grams, of the test portion before drying (9.3); m, is the mass, in grams, ofcrude oil corre- sponding to the response is the mean value of the responses of the instrument for the test portion, determined in 9.5; 71, is the response of the instrument corre- sponding to the mass * of crude oil, read from the calibration line of the instrument (9.2). R 10.2 Calculate lhe response factor of the re
