1、BS EN 15585:2008ICS 67.060NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBRITISH STANDARDCereals and cerealproducts Durumwheat (T. durum Desf.) Determination ofpercentage of mitadinegrains and calculationof percentage ofvitreous grainsThis British Standardwas published under t
2、heauthority of the StandardsPolicy and StrategyCommittee on 28 February2009 BSI 2009ISBN 978 0 580 57710 9Amendments/corrigenda issued since publicationDate CommentsBS EN 15585:2008National forewordThis British Standard is the UK implementation of EN 15585:2008.The UK participation in its preparatio
3、n was entrusted to TechnicalCommittee AW/4, Cereals and pulses.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisionsof a contract. Users are responsible for its correct application.Co
4、mpliance with a British Standard cannot confer immunityfrom legal obligations.BS EN 15585:2008EUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 15585July 2008ICS 67.060English VersionCereals and cereal products - Durum wheat (T. durum Desf.) -Determination of percentage of mitadine grains and calcul
5、ationof percentage of vitreous grainsCrales et produits craliers - Bl dur (T. durum Desf.) -Dtermination du taux de mitadinage et calcul du taux devitrositGetreide- und Getreideerzeugnisse - Hartweizen (T. DurumDesf.) - Bestimmung des prozentualen Anteils an mehligenKrnern und Berechnung des prozent
6、ualen Anteils anglasigen KrnernThis European Standard was approved by CEN on 21 June 2008.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lis
7、ts and bibliographical references concerning such nationalstandards may be obtained on application to the CEN Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the respon
8、sibility of a CEN member into its own language and notified to the CEN Management Centre has the same status as theofficial versions.CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland,France, Germany, Greece, Hungary, Icelan
9、d, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal,Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassa
10、rt, 36 B-1050 Brussels 2008 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15585:2008: EBS EN 15585:2008EN 15585:2008 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Terms and definitions .4 4 Principle4 5 Apparat
11、us .5 6 Sampling.5 7 Procedure .5 8 Expression of results 6 9 Precision.7 10 Test report 8 ANNEX A (informative).9 Results of interlaboratory tests.9 Bibliography 11 BS EN 15585:2008EN 15585:2008 (E) 3 Foreword This document (EN 15585:2008) has been prepared by Technical Committee CEN/TC 338 “Cereal
12、 and cereal products”, the secretariat of which is held by AFNOR. 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 January 2009, and conflicting national standards shall be withdrawn at the latest
13、by January 2009. Attention is drawn to the possibility that some of the elements of 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 stand
14、ards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Po
15、rtugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 15585:2008EN 15585:2008 (E) 4 1 Scope This European Standard specifies a reference method for the determination of the proportion of mitadine grains, applicable exclusively to durum wheat (Triticum durum De
16、sf.). 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 15587, Cereals an
17、d cereal products - Determination of Besatz in wheat (Triticum aestivum L.), durum wheat (Triticum durum Desf.), rye (Secale cereale L.) and feed barley (Hordeum vulgare L.) EN ISO 6644, Flowing cereals and milled cereal products - Automatic sampling by mechanical means (ISO 6644:2002) EN ISO 13690,
18、 Cereals, pulses and milled products - Sampling of static batches (ISO 13690:1999) prEN ISO 24333, Cereals and cereal products - Sampling (ISO/DIS 24333:2008) ISO 5223, Test sieves for cereals 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 v
19、itreous grain translucent grain, the cut grain having a smooth, shiny surface without any mealy appearance 3.2 mitadine grain durum wheat grain which is not considered to be completely vitreous under the conditions of this European Standard NOTE In some countries, these grains are also called piebal
20、d grains. 3.3 proportion of mitadine grains percentage by mass of mitadine grains in a sample of durum wheat as determined with the method described in this European Standard 3.4 proportion of vitreous grains percentage by mass as calculated with the formula given in 8 4 Principle Removal of any imp
21、urities, including grains of common wheat (Triticum aestivum), by sifting and sorting by hand according to EN 15587, followed by separation of visibly mitadine grains, and verification of the vitreous state of the other grains after cutting with a scalpel. BS EN 15585:2008EN 15585:2008 (E) 5 5 Appar
22、atus 5.1 Sample divider 5.2 Sieve, with perforated plate having slots 1,9 mm x 20,0 mm, complying with the requirements of ISO 5223. 5.3 Scalpel. 5.4 Balance, having an accuracy of 0,1 g. 6 Sampling It is important the laboratory receive a sample which is truly representative and has not been damage
23、d or changed during transport and storage. Sampling is not part of the method specified in this International Standard. Recommended sampling methods are given in EN ISO 6644, EN ISO 13690 and prEN ISO 24333. 7 Procedure 7.1 Preparation of the test sample 7.1.1 Take approximately 50 g of the laborato
24、ry sample using the sample divider (5.1), and weigh it to the nearest 0,1 g (mass m). 7.1.2 Place the test sample on the sieve (5.2) and shake by hand or machine for 30 s, keeping the sieve horizontal and moving it in the direction parallel with the length of the slots. Discard the material passing
25、through the sieve. 7.1.3 Remove by hand any impurities in the sample retained on the sieve. Grains of common wheat (Triticum aestivum L.) shall be considered to be impurities. 7.2 Test portion Weigh the mass of durum wheat grains thus prepared to the nearest 0,1 g. 7.3 Determination 7.3.1 Spread the
26、 test portion (7.2) over a flat surface. Examine each grain individually with the naked eye (corrected, if necessary, for abnormal vision). 7.3.2 Separate out all grains which are visibly mitadine. NOTE Do not confuse mitadine grains with “washed grains”, the external appearance of which is similar
27、to that of completely mealy grains, but which differ in their dull appearance. Washed grains are not necessarily mealy. 7.3.3 Using the scalpel (5.3), cut transversely all the remaining grains through the middle and remove both parts of each grain which, when cut, prove to be mitadine. 7.3.4 Gather
28、and weigh to the nearest 0,1 g: firstly, grains which are visibly mitadine, and both parts of those grains which when cut proved to be mitadine (mass m1); secondly, the parts of the vitreous grains (mass m2). BS EN 15585:2008EN 15585:2008 (E) 6 7.3.1 The determination is considered to be valid if (m
29、1+ m2) does not differ from the mass of the test portion (7.2) by more than 0,5 %. If this is not the case, carry out the determination again on a new test sample. 8 Expression of results 8.1 Methods of calculation and formulae 8.1.1 The proportion of mitadine grains, expressed in percentage regardi
30、ng the raw sample as received (7.1.1) (before sieving and removal of impurities), is equal to: 1001mm(1) where m is the mass, in grams, of the test sample taken in 7.1.1; m1is the mass, in grams, of the mitadine grains (see 7.3). 8.1.2 The proportion of mitadine grains, expressed in percentage regar
31、ding the sieved test sample from which impurities have been removed (7.1.3), is equal to: 100211+ mmm(2) where m1is the mass, in grams, of the mitadine grains (see 7.3); m2 is the mass, in grams, of the vitreous grains (see 7.3). 8.1.3 The proportion of vitreous grains, expressed in percentage regar
32、ding the raw sample as received (7.1.1), is equal to: 1002mm(3) where mis the mass, in grams, of the test sample taken in 7.1.1. m2is the mass, in grams, of the vitreous grains (see 7.3). 8.1.4 The proportion of vitreous grains, expressed in percentage regarding the sieved test sample from which imp
33、urities have been removed (7.1.3), is equal to: 100212+ mmm(4) where m1is the mass, in grams, of the mitadine grains (see 7.3); m2 is the mass, in grams, of the vitreous grains (see 7.3). BS EN 15585:2008EN 15585:2008 (E) 7 8.2 Number of determinations Carry out two determinations on different sampl
34、es taken from the same laboratory sample. If the difference between the two determinations is bigger than the repeatability limit (see 9.1), carry out two new determinations. If with these two other determinations, the difference is bigger than the repeatability limit, take the mean of the four dete
35、rminations as the result. If the difference between the two determinations is lower or equal to the repeatability limit (see 9.1), take the mean of the two determinations as the result. Express the result with one decimal. 9 Precision 9.1 Interlaboratory test Details of an international interlaborat
36、ory test on the precision of the method are summarized in Annex A. The values derived from this test may not be applicable to mitadine concentration ranges and matrices other than those given, namely from 10 % to 55 %. 9.2 Repeatability limit (r) The absolute difference between two independent singl
37、e test results, obtained using the same method on identical test material in the same laboratory by the same operator using the same equipment within a short interval of time will not in more that 5 % of cases be greater than the repeatability limit (r) given hereunder: r = 2,77 x sr= 2,77 x (1,05)
38、= 2,9 (5) where sris the repeatability standard deviation. 9.3 Reproducibility limit (R) The absolute difference between two single test results, obtained using the same method on identical test material in different laboratories with different operators using different equipment, will not in more t
39、hat 5 % of cases be greater than the reproducibility limit (R) given hereunder: R = 2,77 x sR= 2,77 x 3,43 = 9,5 (6) where sRis the reproducibility standard deviation. 9.4 Critical difference (CD) When the difference between two averaged values obtained from two test results under repeatability cond
40、itions is to be assessed, the repeatability limit cannot be used: Critical Difference shall be used. 9.4.1 Comparison of two groups of measurements in one laboratory The critical difference (CD1) between two averaged values obtained in one laboratory from two test results under repeatability conditi
41、ons is equal to: 06,2 96,12177,2 21212,77 211=+=rrrssnnsCD (7) BS EN 15585:2008EN 15585:2008 (E) 8 where sris the standard deviation of repeatability; n1and n2are the number of test results corresponding to each of the averaged values (here, n1= n2= 2). 9.4.2 Comparison of two groups of measurements
42、 in two laboratories The critical difference (CD2) between two averaged values obtained in two different laboratories from two test results under repeatability conditions is equal to: 9,28 5,0 77,2 21211 - 2,77 22212r22=rRRssnnssCD (8) where sris the standard deviation of repeatability; sRis the sta
43、ndard deviation of reproducibility; n1and n2are the number of test results corresponding to each of the averaged values (here, n1= n2= 2). 9.5 Uncertainty (Ue) The measurement uncertainty (Ue) is a parameter representing the distribution of the values that may reasonably be attributed to the result.
44、 This uncertainty is given by a statistical distribution of the results from the interlaboratory test and is characterized by the experimental standard deviation. The uncertainty (Ue) is equal to plus or minus twice the reproducibility standard deviation given in this European Standard: for products
45、 whose mitadine fraction is between 10 % to 55 % (see Table A.1 and Figure A.1): Ue = 2 x sR= 2 x 3,43 = 6,86 (9) where sRis the standard deviation of reproducibility. 10 Test report The test report shall show the method used, the results obtained, and the method of expressing the results. It shall
46、also include all details of the procedure not specified in this European Standard, or regarded as optional, as well as any circumstances that may have influenced the results, of which the number of determination carried out to obtain the result. The test report shall contain all information necessar
47、y for complete identification of the sample. BS EN 15585:2008EN 15585:2008 (E) 9 ANNEX A (informative) Results of interlaboratory tests An international interlaboratory test was carried out on 6 samples of durum wheat. 12 laboratories in 3 countries have participated. This test was organized by the
48、BIPEA in May 2007 with financial support from ONIGC (Office National Interprofessionnel des Grandes Cultures) and ANMAC (Association pour la Normalisation des Mthodes dAnalyses des Crales). The results obtained were subjected to statistical analysis in accordance with the parts 1, 2 and 6 of ISO 572
49、5 to give the precision data shown in table A. Table A.1 - Precision data for mitadine grains fraction Samples Parameters 1 2 3 4 5 6 Number of laboratories after eliminating outliers 9 10 9 10 8 10 Mean value 11,3 34,0 24,1 33,7 11,4 56,8 Repeatability standard deviation, Sr0,9 0,7 0,5 1,8 1,3 1,1 Coefficient of variation of repeatability, %, CVr7,9 2,2 1,9 5,2 11,3 1,9 Repeatability limit r 2,5 2,1 1,3 4,9 3,6 3,0 Reproducibility standard deviation, SR0,9 3,7 7,0 4,8 1,2 3,0 Coefficient of variation of reproducibility, %, CVR8,1
