1、BRITISH STANDARD BS EN ISO 15301:2001 Incorporating corrigendum no. 1 Animal and vegetable fats and oils Determination of sediment in crude fats and oils Centrifuge method The European Standard EN ISO 15301:2001 has the status of a British Standard ICS 67.200.10 BS EN ISO 15301:2001 This British Sta
2、ndard was published under the authority of the Standards Policy and Strategy Committee on 15 October 2001 BSI 2007 ISBN 978 0 580 59659 9 National foreword This British Standard is the UK implementation of EN ISO 15301:2001, incorporating corrigendum June 2007. It is identical with ISO 15301:2001, i
3、ncorporating corrigendum March 2007. The start and finish of text introduced or altered by corrigendum is indicated in the text by tags . Text altered by ISO corrigendum March 2007 is indicated in the text by . The UK participation in its preparation was entrusted to Technical Committee AW/11, Anima
4、l and vegetable fats and oils. A list of organizations represented on this committee can be obtained on request to its secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Stan
5、dard cannot confer immunity from legal obligations. Amendments issued since publication Amd. No. Date Comments 17267 Corrigendum No. 1 31 August 2007 See national forewordEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO15301 September2001 ICS67.200.10 Englishversion Animalandvegetablefatsandoils
6、Determinationofsediment incrudefatsandoilsCentrifugemethod(ISO15301:2001) CorpsgrasdoriginesanimaleetvgetaleDtermination delateneurensdimentdansdescorpsgrasbruts Mthodeparcentrifugation(ISO15301:2001) TierischeundpflanzlicheFetteundleBestimmungdes SedimentgehaltesinrohenFettenundlen Zentrifugenverfa
7、hren(ISO15301:2001) ThisEuropeanStandardwasapprovedbyCENon1September2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uch
8、national standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatu
9、sasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATI
10、ON EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO15301:2001E IncorporatingcorrigendumJune2007Foreword ThetextoftheInternationalStandardISO15301:2001hasbeenpreparedby
11、Technical CommitteeISO/TC34“Agriculturalfoodproducts“incollaborationwithTechnicalCommittee CEN/TC307“Oilseeds,vegetableandanimalfatsandoilsandtheirbyproductsMethodsof samplingandanalysis“,thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublica
12、tion ofanidenticaltextorbyendorsement,atthelatestbyMarch2002,andconflictingnational standardsshallbewithdrawnatthelatestbyMarch2002. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRep
13、ublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnited Kingdom. NOTEFROMCMC TheforewordissusceptibletobeamendedonreceptionoftheGerman languageversion.Theconfirmedoramendedforeword,andwhenappropriate,thenormative
14、annexZAforthereferencestointernationalpublicationswiththeirrelevantEuropean publicationswillbecirculatedwiththeGermanversion. Endorsementnotice ThetextoftheInternationalStandardISO15301:2001wasapprovedbyCENasaEuropean Standardwithoutanymodification. EN ISO 15301:2001INTERNATIONAL STANDARD ISO 15301
15、First edition 2001-09-01 Reference number ISO 15301:2001(E) Animal and vegetable fats and oils Determination of sediment in crude fats and oils Centrifuge method Corps gras dorigines animale et vgtale Dtermination de la teneur en sdiment dans des corps gras bruts Mthode par centrifugation EN ISO 153
16、01:2001ii iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing International Standards is normally carried out through ISO technical committees. Each member body interested in a subject
17、 for which a technical committee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC)
18、on all matters of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Internatio
19、nal Standard requires approval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. In
20、ternational Standard ISO 15301 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. Annexes A and B of this International Standard are for information only. EN ISO 15301:2001blankAnimal and vegetable fats and oils Determination of sedi
21、ment in crud efat sandoilsC en t rifu gem et h od 1 Scope This International Standard specifies a method for the determination in crude fats or oils of that sediment which can be separated by centrifugal force. obtained by means of extraction and/or crushing. The method is not applicable to fats whi
22、ch are not liquid at a temperature of . 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publica- tions
23、 do not apply. However, parties to agreements based on this International Standard are encouraged to investi- gate the possibility of applying the most recent edition of the normative document indicated below. For undated references, the latest edition of the normative document referred to applies.
24、Members of ISO and IEC maintain reg- isters of currently valid International Standards. ISO 661:1989, Animal and vegetable fats and oils Preparation of test sample 3 Term and definition For the purposes of this International Standard, the following term and definition applies. 3.1 sediment that part
25、 of the insoluble matter in a crude fat or oil which can be centrifugally separated and is the total amount of the unclear layer of components collected at the bottom of the measuring tube after centrifuging NOTE The sediment contains, for example, phospholipids, impurities, dirt, etc. dispersed in
26、a water-containing phase, and can be quantified according to this International Standard. Any white crystalline components deposited on top of and within the dark layer of insoluble materials are regarded as part of the sediment. 4 Principle A homogenized test sample is subjected to centrifuging as
27、specified. The amount of separated material, called sediment, is volumetrically measured in a calibrated centrifuge tube. 5A p p a r a t u s Usual laboratory apparatus and, in particular, the following. 20 C 1 EN ISO 15301:2001 Themethodisapplicabletocrudeoilsandtooilswithasedimentcontentof0,1mlper1
28、00gto15mlper100g,2 ISO 1002 All rithgs rreseved 5.1 Centrifuge tubes, of capacity , pear- or cone-shaped, made from thoroughly annealed glass and fitted w i thas t op p er( se eF i g ur es1a nd2 ) . NOTE Reading the volume of the unclear layer may be more difficult in a cone-shaped tube than in a pe
29、ar-shaped tube. 5.2 Buckets, for centrifuge tubes (5.1), resistant to fats and oils. 5.3 Centrifuge, suitable for the centrifuge tubes (5.1) placed in the buckets (5.2), capable of controlling the rotational frequency so as to give a radial acceleration at the narrow part of the tubes of 700 to 800
30、times the acceleration of free fall. See annex A for the calculation of the rotational frequency of the centrifuge. In rooms which are not air-conditioned, use a centrifuge capable of maintaining its temperature between and . 5.4 Balance, capable of weighing to the nearest . 6 Sampling It is importa
31、nt that the laboratory receive a sample which is truly representative and has not been damaged or changed during transport or storage. Sampling is not a part of the method specified in this International Standard. A recommended sampling method is given in ISO 5555 1. Store samples in glass or polyet
32、hylene terephthalate (PET) bottles. 7 Preparation of test sample Prepare the test sample in accordance with ISO 661. Bring the test sample, if necessary, to a temperature of between and . Redisperse any sediment in the oil from the bottom of the sample bottle to ensure a sufficiently homogeneous and
33、 representative sample. Immediately proceed in accordance with clause 8. 8 Procedure Weigh two centrifuge tubes (5.1) to the nearest . Transfer of the prepared test sample (clause 7) to each of the centrifuge tubes. Weigh the tubes and place them in the buckets (5.2) in the centrifuge (5.3). Adjust
34、the rotational frequency so as to give a radial acceleration at the narrow part of tubes of 700 to 800 times the acceleration of free fall. Centrifuge for . Read sediment volumes up to and including to the nearest . Read sediment volumes greater than to the nearest . When using a cone-shaped tube, i
35、t may be more difficult to read the volume of the unclear layer; read the sediment v ol um e sa sa ccu r a t el ya sp os sib le . If in a pear-shaped tube the separation is not complete (clear layer in the neck of the narrow tube section of the tube), the sediment reading should be corrected for thi
36、s volume. Record the relative radial acceleration or the swing diameter and the rotational frequency of the centrifuge. Record the temperature before and after centrifuging. 100 ml 20 C 25 C 0,1 g 20 C2 5 C 0,1 g 100 ml 1h 5s 1,5 ml 0,03 ml 1,5 ml 0,5 ml 2 EN ISO 15301:20019 Expression of results Ca
37、lculate the sediment content of the test sample using the equation: where is the numerical value of the sediment content of the test sample, in millilitres per ; is the numerical value of the sediment volume, in millilitres; is the numerical value of the mass of the centrifuge tube with the test por
38、tion, in grams; is the numerical value of the mass of the centrifuge tube, in grams. Calculate the mean of the results for the two tubes and report the results to the nearest 10 Precision 10.1 Interlaboratory test Details of interlaboratory tests on the precision of the method are given in annex B.
39、The values derived from these tests may not be applicable to concentration ranges and matrices other than those given. 10.2 Repeatability The absolute difference between two independent single test results, obtained using the same method on identical test material in the same laboratory by the same
40、operator using the same equipment within a short interval of time, will in not more than of cases exceed the repeatability limit given in or derived from Table 1. 10.3 Reproducibility The absolute difference between two single test results, obtained using the same method on identical test material i
41、n different laboratories by different operators using different equipment, will in not more than of cases exceed the reproducibility limit given in or derived from Table 1. 11 Test report The test report shall specify: all information necessary for the complete identification of the sample; the samp
42、ling method used, if known; the test method used, with reference to this International Standard; the relative radial acceleration or the swing diameter and the rotational frequency; Table 1 Repeatability limit ( ) and reproducibility limit ( ) Sediment content ml per ml per ml per 0,1 0,7 1to3 0 ,2
43、1,0 w = V 100 (m 1 m 2 ) w 100 g V m 1 m 2 5% r rR rR 100 g 100 g 100 g 1 5% R 3 0,1 ml per 100 g. EN ISO 15301:2001 4 ISO 1002 All rithgs rreseved the temperature before and after centrifuging; all operating details not specified in this International Standard, or regarded as optional, together wit
44、h details of any incidents which may have influenced the test result(s); the test result obtained, or the two test results obtained if the repeatability has been checked. Dimensions in millimetres Figure 1 Pear-shaped sediment tube 4 EN ISO 15301:2001 ISO 1002 All rithgs rreseved 5 Dimensions in mil
45、limetres Figure 2 Cone-shaped sediment tube 5 EN ISO 15301:20016 ISO 1002 All rithgs rreseved Annex A (informative) Calculation of the rotational frequency of a centrifuge The rotational frequency of the centrifuge may be calculated by the equation: where is the numerical value of the rotational fre
46、quency, in ; is the relative radial acceleration (for example or ); is the numerical value of the diameter of swing, measured between the tips of opposite tubes when tubes are in a rotating position, in millimetres. n = 1 337 r a r d n min 1 a r a r = 700 a r = 800 d 6 EN ISO 15301:2001 ISO 1002 All
47、 rithgs rreseved 7 Annex B (informative) Results of interlaboratory tests B.1 Statistical results of interlaboratory tests The precision of the method was established by two interlaboratory tests organized by the Netherlands Oils, Fats and Oilseeds Trade Association (NOFOTA) in cooperation with the Federation of Oils, Seeds and Fats Associations (FOSFA International) in 1996 and 1997/1998 and carried out in accordance with ISO 5725-2 3. In the first test 12 laboratories participated. Six (spiked) samples of crude sunflowerseed oil were investig
