1、BRITISH STANDARD BS EN ISO 10539:2002 Incorporating Corrigendum No. 1 Animal and vegetable fats and oils Determination of alkalinity The European Standard EN ISO 10539:2002 has the status of a British Standard ICS 67.200.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN
2、ISO 10539:2002 This British Standard, having been prepared under the direction of the Consumer Products and Services Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 16 April 2002 BSI 15 May 2002 ISBN 0 580 39434 4 National for
3、eword This British Standard is the official English language version of EN ISO 10539:2002. It is identical with ISO 10539:2002. It supersedes BS 684-2.5:1989 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee AW/11, Animal and vegetable fats and oils, wh
4、ich has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue und
5、er the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct a
6、pplication. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor rela
7、ted international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iii, pages 1 to 6, the Annex ZA page and a back cover. The BSI co
8、pyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 13912 Corr. No. 1 15 May 2002 Incorporating Annex ZA and correction to EN ISO foreword pageEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO10539 March20
9、02 ICS67.200.10 Englishversion AnimalandvegetablefatsandoilsDeterminationofalkalinity (ISO10539:2002) CorpsgrasdoriginesanimaleetvgtaleDtermination delalcalinit(ISO10539:2002) TierischeundpflanzlicheFetteundleBestimmungder Alkalitt(ISO10539:2002) ThisEuropeanStandardwasapprovedbyCENon6March2002. CEN
10、membersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENme
11、mber. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Be
12、lgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Br
13、ussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO10539:2002EINESO01:9352002(E) 2 CORRECTED20020417 Foreword Thisdocument(ISO10539:2002)hasbeenpreparedbyTechnicalCommitteeISO/TC34 “Agriculturalfoodproducts“incollaborationwithTechnicalCom
14、mitteeCEN/TC307“Oilseeds, vegetableandanimalfatsandoilsandtheirbyproductsMethodsofsamplingandanalysis“, thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbySeptember2002,andconflicting nati
15、onalstandardsshallbewithdrawnatthelatestbySeptember2002. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembour
16、g,Malta,Netherlands,Norway,Portugal,Spain,Sweden,Switzerlandandthe UnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO10539:2002hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO10539:
17、200251 Reference number ISO 10539:2002(E) ISO2002 INTERNATIONAL STANDARD ISO 10539 First edition 2002-03-15 Animal and vegetable fats and oils Determination of alkalinity Corps gras dorigines animale et vgtale Dtermination de lalcalinit 5egaP ENISO10539:2002ii ISO 10539:2002(E) iiiForeword ISO (the
18、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 for which a technical committee
19、 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) on all matters of electrotechnic
20、al standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bo
21、dies for voting. Publication as an International 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
22、identifying any or all such patent rights. ISO 10539 was prepared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. Annex A of this International Standard is for information only. 2egaP ENISO10539:2002blank 3egaP ENISO10539:2002INTENRATIONALS TA
23、NDA DR IS:93501 O2002(E)1Animal and vegetable fats and oils Determination of alkalinity 1 Scope This International Standard specifies a method for the determination of the alkalinity of animal and vegetable fats and oils without distinguishing between the various constituents. The method is not appl
24、icable to dry melted animal fats, nor to oils and fats with an acidity greater than 60 % (mass fraction) as determined in accordance with ISO 660. NOTE Fats and oils can contain alkaline constituents either naturally (e.g. calcium soaps from bones) or accidentally (e.g. sodium soaps in imperfectly r
25、efined fats and oils). 2 Normative references The following normative documents contain 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 publications do not apply. How
26、ever, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent editions of the normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and
27、 IEC maintain registers of currently valid International Standards. ISO 660:1996, Animal and vegetable fats and oils Determination of acid value and acidity ISO 661:1989, Animal and vegetable fats and oils Preparation of test sample ISO 3696:1987, Water for analytical laboratory use Specification an
28、d test methods 3 Term and definition For the purposes of this International Standard, the following term and definition apply. 3.1 alkalinity proportion of alkali in a fat or oil determined by titration with hydrochloric acid, in accordance with the method specified in this International Standard 4
29、Principle A test portion is dissolved in warm aqueous acetone and titrated with hydrochloric acid. 5 Reagents Use only reagents of recognized analytical grade, unless otherwise stated. 5.1 Water, conforming to grade 3 of ISO 3696. 5.2 Aqueous acetone Mix 970 ml of acetone, 20 ml of water and 10 ml o
30、f bromophenol blue solution (2 g/l in acetone). Add sodium hydroxide solution c(NaOH) = 0,1 mol/l to give a blue colour, then add hydrochloric acid c(HCl) = 0,1 mol/l until a yellowish green colour appears. 4egaP ENISO10539:2002ISO 10539:2002(E) 2 5.3 Hydrochloric acid standard volumetric solution,
31、c(HCl) = 0,01 mol/l, standardized not more than 7 days before use. 6 Apparatus Usual laboratory apparatus and, in particular, the following. 6.1 Borosilicate glass apparatus, for aqueous acetone (5.2). 6.2 Conical flasks, with wide necks, and of capacities 400 ml to 500 ml. 7 Sampling It is importan
32、t that the laboratory receive a sample which is truly representative and has not been damaged or changed during transport or storage. Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 5555. 8 Preparation of test sample Prepare
33、the test sample in accordance with ISO 661. 9 Procedure 9.1 Preparation of the apparatus Rinse each conical flask (6.2) and stirrer to be used with successive 20 ml amounts of aqueous acetone (5.2) until the aqueous acetone does not change colour. Allow the flasks and stirrer to dry. 9.2 Test portio
34、n From the test sample (clause 8) weigh, to the nearest 0,1 g, a test portion of up to 40 g (see Table 1) according to the expected result and colour of the sample. Melt a solid test portion at below the boiling point of acetone. Add 100 ml of the acetone (5.2) at 40 C and stir. Allow to settle unti
35、l the solution splits in two layers; in the presence of soap, the upper layer is blue-coloured. Table 1 Mass of test portion Expected result Mass Colour of sample mg sodium oleate/kg of sample g Light up to 500 40 Light over 500 to 1 000 10 Light over 1 000 4 Dark not relevant 2 Very dark not releva
36、nt 1 For test portions of less than 10 g, take replicate portions totalling at least 5 g for titration and sum the masses and titres to give the result for one determination. 5egaP ENISO10539:2002ISO 10539:2002(E) 39.3 Determination Titrate the warm (30 C to 40 C) solution with the hydrochloric acid
37、 (5.3) while stirring until the colour of the indicator changes from blue (or blue green) to the yellowish green of the acetone (5.2) added. Allow the mixture to settle in order to observe the colour clearly. NOTE An explosion-resistant hotplate with magnetic stirrer and burette support is particula
38、rly useful. 9.4 Number of determinations Carry out two determinations on the same test sample, treating the replications for small test portions as one determination (see Table 1). 10 Expression of results Alkalinity may be expressed as a mass, in milligrams, of sodium oleate per kilogram of fat or
39、oil, or as a percentage (mass fraction) of sodium hydroxide: a) the alkalinity in terms of sodium hydroxide is given by the expression 4Vc A m = b) the alkalinity in terms of sodium oleate is given by the expression 304 000 Vc S m = where A is the alkalinity expressed as a percentage (mass fraction)
40、 of sodium hydroxide; S is the alkalinity expressed as milligrams of sodium oleate per kilogram of sample; m is the mass of the test portion, in grams; c is the exact concentration of the standard volumetric hydrochloric acid solution used, in moles per litre; V is the volume of hydrochloric acid st
41、andard volumetric solution used to titrate the test portion, in millilitres. Take as the result the mean of two determinations, provided that the requirement for repeatability (see 11.2) is met. 11 Precision 11.1 Interlaboratory test Details of an interlaboratory test are summarized in annex A. The
42、values derived from this interlaboratory test may not be applicable to concentration ranges other than those given. 11.2 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 ope
43、rator using the same equipment within a short interval of time, will in not more than 5 % of cases exceed the repeatability limit r given in Table A.1 for the relevant level of the mean value determined. 6egaP ENISO10539:2002ISO 10539:2002(E) 4 11.3 Reproducibility The absolute difference between tw
44、o single test results, obtained using the same method on identical test material in different laboratories by different operators using different equipment, will in not more than 5 % of cases exceed the reproducibilty limit R given in Table A.1 for the relevant level of the mean value determined. 12
45、 Test report The test report shall specify: all information necessary for the complete identification of the sample; the sampling method used, if known; the test method used, with reference to this International Standard; all operating conditions not specified in this International Standard, or rega
46、rded as optional, together with details of any incidents which may have influenced the test results; the test results obtained or, if the repeatability has been checked, the final result obtained. 7egaP ENISO10539:2002ISO 10539:2002(E) 5Annex A (informative) Results of an interlaboratory trial An in
47、ternational collaborative test has been carried out on the method given in this International Standard. The test, involving fifteen laboratories in six countries, was organized by AFNOR and the results obtained were subjected to statistical analysis in accordance with ISO 5725-2 to give the precisio
48、n data reported in Table A.1. Table A.1 Precision data Sample D Sample E Sample H Number of laboratories 15 15 15 Number of laboratories retained after eliminating outliers 14 11 12 Mean alkalinity (mg/kg) 8,3 216,3 12,5 Repeatability standard deviation, s r(mg/kg) 0,7 0,6 0,5 Repeatability coefficient of variation (%) 8,1 0,3 3,6 Repeatability limit, r (mg/kg) 1,9 1,8 1,3 Reproducibility standard deviation, s R(mg/kg) 2
