1、BRITISH STANDARD BS EN ISO 18609:2001 BS 684-2.51:2001 Incorporating Corrigendum No. 1 Animal and vegetable fats and oils Determination of unsaponifiable matter Method using hexane extraction The European Standard EN ISO 18609:2000 has the status of a British Standard ICS 67.200.10 NO COPYING WITHOU
2、T BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN ISO 18609:2001 This British Standard, having been prepared under the direction of the Consumer products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 October 2001 BSI
3、24 January 2002 ISBN 0 580 38046 7 National foreword This British Standard is the official English language version of EN ISO 18609:2001. It is identical with ISO 18609:2000. It supersedes BS EN ISO 3596-2:2000 which is withdrawn. The UK participation in its preparation was entrusted to Technical Co
4、mmittee AW/11, Animal and vegetable fats and oils, which 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 doc
5、ument may be found in the BSI Standards Catalogue under 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
6、British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or pro
7、posals for change, and keep the UK interests informed; monitor related 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 a
8、nd iii, a blank page, pages 1 to 8, the Annex ZA page and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 13637 Incorporating Corrigendum No. 1 24 January 2002 Replaced the EN ISO
9、foreword and inserted the Annex ZA page.EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO18609 August2001 ICS67.200.10 SupersedesENISO35962:2000 Englishversion AnimalandvegetablefatsandoilsDeterminationof unsaponifiablematterMethodusinghexaneextraction(ISO 18609:2000) Corpsgrasdoriginesanimaleetv
10、gtaleDtermination delateneurenmatiresinsaponifiablesMthodepar extractionlhexane(ISO18609:2000) TierischeundpflanzlicheFetteundleBestimmungder unverseifbarenBestandteileVerfahrenmitHexan Extraktion(ISO18609:2000) ThisEuropeanStandardwasapprovedbyCENon21June2001. CENmembersareboundtocomplywiththeCEN/C
11、ENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsint
12、hreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland
13、,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationina
14、nyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO18609:2001ECORRECTED20011205 Foreword ThetextoftheInternationalStandardfromTechnicalCommitteeISO/TC34“Agriculturalfood products“oftheInternationalOrganizationforStandardization(ISO)hasbeentakenoverasan EuropeanStandardbyTechnica
15、lCommitteeCEN/TC307“Oilseeds,vegetableandanimalfats andoilsandtheirbyproductsMethodsofsamplingandanalysis“,thesecretariatofwhichis heldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyFebruary2002,andconflictingna
16、tional standardsshallbewithdrawnatthelatestbyFebruary2002. ThisEuropeanStandardreplacesENISO35962:2000. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,
17、Germany,Greece,Iceland,Ireland,Italy,Luxembourg, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO18609:2000hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodification. NOTE:NormativereferencestoInternationalStandardsar
18、elistedinannexZA(normative). ENISO18609:2001 Reference number ISO 18609:2000(E) INTERNATIONAL STANDARD ISO 18609 First edition 2000-08-15 Animal and vegetable fats and oils Determination of unsaponifiable matter Method using hexane extraction Corps gras dorigines animale et vgtale Dtermination de la
19、 teneur en matires insaponifiables Mthode par extraction lhexane ENISO18609:2001 ii ENISO18609:2001 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 norma
20、lly carried out through ISO technical committees. Each member body interested in a subject 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 th
21、e work. ISO collaborates closely with the International Electrotechnical Commission (IEC) 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 technic
22、al committees are circulated to the member bodies 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 r
23、ights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 18609 was prepared by Technical Committee ISO/TC 34, Agricultural food products, Subcommittee SC 11, Animal and vegetable fats and oils. This first edition of ISO 18609 cancels and repl
24、aces ISO 3596-2:1988 and its Amendment 1:1999, of which it constitutes a minor revision. Annex A of this International Standard is for information only. ENISO18609:2001 ENISO18609:2001 INTENRATIONAL TSANDADR ISO 90681:(0002)E1 Animal and vegetable fats and oils Determination of unsaponifiable matter
25、 Method using hexane extraction 1 Scope This International Standard specifies a method using three hexane extractions for the determination of the unsaponifiable matter content of animal and vegetable fats and oils. The method is applicable to all fats and oils but not to waxes. CAUTION In compariso
26、n with the method given in ISO 3596, however, the present method gives results which are systematically low. 2 Normative reference The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, s
27、ubsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this International Standard are encouraged to investigate the possibility of applying the most recent edition of the normative document indicated below. For undated references, t
28、he latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 661, Animal and vegetable fats and oils Preparation of test sample. 3 Terms and definitions For the purposes of this International Standard, the
29、following term and definition applies. 3.1 unsaponifiable matter all the substances present in the product which, after saponification of the latter by potassium hydroxide and extraction by hexane, are not volatile under the specified operating conditions. NOTE The unsaponifiable matter includes lip
30、ids of natural origin such as sterols, higher hydrocarbons and alcohols, aliphatic and terpenic alcohols, as well as any foreign organic matter extracted by the solvent and not volatile at 103 C( e . g . mineral oils) that may be present. 4P r i n c i p l e The fat or oil is saponified by boiling un
31、der reflux with an ethanolic potassium hydroxide solution. The unsaponifiable matter is extracted from the soap solution by hexane or, failing this, light petroleum. The solvent is evaporated and the residue is weighed after drying. ENISO18609:2001 2 5 Reagents Use only reagents of recognized analyt
32、ical grade, and distilled or deionized water or water of equivalent purity. 5.1 n-Hexane or, failing this, light petroleum, distilling between 40 C and 60 C, bromine number less than 1. Both solvents shall be free from residue. 5.2 Ethanol, 10 % (by volume) solution. 5.3 Phenolphthalein, 10 g/l solu
33、tion in 95 % (by volume) ethanol. 5.4 Potassium hydroxide, ethanolic solution, c(KOH) 1mol/l . Dissolve 60 g of potassium hydroxide in 50 ml of water and dilute to 1 000 ml with 95 % (by volume) ethanol. The solution should be colourless or straw-yellow. 6 Apparatus Usual laboratory equipment and, i
34、n particular, the following. 6.1 Round-bottomed flasks, of 250 ml capacity, with ground neck. 6.2 Reflux condenser, with ground joint to fit the flasks (6.1). 6.3 Separating funnels, of 250 ml capacity, with stopcocks and stoppers made of polytetrafluoroethylene. 6.4 Boiling water bath. 6.5 Oven, ca
35、pable of being maintained at 103 C 2 C, or apparatus for drying under vacuum,e . g .r o t a r y evaporator or similar apparatus. 7 Sampling Sampling is not part of the method specified in this International Standard. A recommended sampling method is given in ISO 5555 2. It is important the laborator
36、y receive a sample which is truly representative and has not been damaged or changed during transport or storage. 8 Preparation of test sample Prepare the test sample in accordance with ISO 661. 9 Procedure 9.1 Test portion Weigh, to the nearest 0,01 g, about 5 g of the test sample (clause 8) into a
37、 250 ml flask (6.1). ENISO18609:2001 3 9.2 Saponification Add 50 ml of the potassium hydroxide solution (5.4) and some anti-bumping granules. Attach the reflux condenser (6.2) to the flask and boil the contents gently for 1 h. Stop heating. Add 50 ml of water through the top of the condenser and swi
38、rl. 9.3 Extraction of unsaponifiable matter After cooling, transfer the solution to a 250 ml separating funnel (6.3). Rinse the flask and the anti-bumping granules several times with the hexane (5.1), using 50 ml in all, and pour these rinsings into the separating funnel. Stopper and shake vigorousl
39、y for 1 min, periodically releasing pressure by inverting the separating funnel and cautiously opening the stopcock. Allow to stand until there is complete separation of the two phases. Then run off the lower layer as completely as possible into a second separating funnel. If an emulsion is formed,
40、destroy it by adding small quantities of ethanol or concentrated potassium hydroxide or sodium chloride solution. Extract the aqueous ethanolic soap solution twice more, each time in the same way with 50 ml of the hexane. Collect the three hexane extracts in one separating funnel. 9.4 Washing of hex
41、ane extract Wash the combined extracts three times with 25 ml portions of the ethanol solution (5.2), shaking vigorously and drawing off the aqueous ethanolic solution after each wash. Draw off each washing solution leaving 2 ml, then rotate the separating funnel around its axis. Wait some minutes t
42、o allow the remaining aqueous ethanolic layer to collect. Draw this off, closing the stopcock when the hexane solution reaches the bore of the stopcock. Continue to wash with the ethanol solution until the washings no longer give a pink colour on the addition of a drop of the phenolphthalein solutio
43、n (5.3). 9.5 Evaporation of solvent Transfer the hexane solution quantitatively, a little at a time if necessary, through the top of the separating funnel into a 250 ml flask (6.1) previously dried at 103 C in the oven (6.5), then cooled and weighed to the nearest 0,1 mg. Evaporate the solvent on a
44、boiling water bath (6.4). 9.6 Drying the residue and determination 9.6.1 Dry the residue for 15 min in the oven (6.5) set at 103 C, with the flask in an almost horizontal position. Allow to cool in a desiccator and weigh to the nearest 0,1 mg. Alternatively, attach the flask to the apparatus for dry
45、ing under vacuum (6.5) and dry on the boiling water bath under the maximum vacuum of the water pump for about 15 min. Allow to cool to room temperature under the maximum vacuum of the water pump, carefully wipe the flask, and weigh to the nearest 0,1 mg. Repeat the drying for successive 15 min perio
46、ds until the loss of mass between two successive weighings is less than 1,5 mg. If constant mass is not obtained after three periods of drying, the unsaponifiable matter is probably contaminated and the determination shall be repeated. 9.6.2 If a correction for free fatty acids is considered necessa
47、ry, after weighing the residue dissolve it in 4 ml of the hexane (5.1) and then add 20 ml of ethanol previously neutralized to a faint pink colour in the presence of the phenolphthalein (5.3) as indicator. Titrate with standard volumetric ethanolic potassium hydroxide solution, c(KOH) = 0,1 mol/l, t
48、o the same final colour. Calculate the mass of free fatty acids as oleic acid and correct the mass of the residue accordingly (see clause 10). ENISO18609:2001 4 9.7 Number of determinations Carry out two determinations on the same test sample. 9.8 Blank test Carry out a blank test, using the same procedure and the same quantities of all the reagents, but omitting the test portion. If the residue ex
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