(ISO 6463 International Standard Animal and vegetable fats and oils Determination of butylhydroxyanisole (BHA) and butylhydroxytoluene (BHT) - Gas-liquid chromatographic method Corps gras d'origines animale et vegetale - Dosage du butylhydroxyanisol (BHA) et du butylhydroxytoluene (BHT) - Methode par chromatographie en phase gazeuse First edition - 1982-09-01 ISO 6463-1982 (E) UDC 664.3 : 543.544.45 : 547.53 Ref. No. 1SO 6463-1982 (E) Descriptors : agricultural products, animal fats, vegetable fats, determination, antioxidants, gas chromatographic analysis. Price based on 3 pages oronto by Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationof national standards institutes (Iso member bodies). The work of developing Inter- national Standards is carried out through IsO technical committees. Every member bodyinterestedinasubjectforwhichatechnicalcommitteehasbeensetuphasthe and non-governmental, in liaison with iso, also take part in the work. Draft International Standards adopted by the technical committees are circulated to the member bodies for approval before their acceptance as International Standards by the iso Council. International Standard ISO 6463 was developed by Technical Committee ISO/TC 34 Agricultural food products, and was circulated to the member bodies in March 1981. It has been approved by the member bodies of the following countries : india Romania Austraiia Austria Iran South Africa, Rep. of Canada Iraq Sri Lanka Chile Israel Tanzania Italy Thailand Czechoslovakia Dominican Republic Kenya United Kingdom Egypt, Arab Rep. of Korea, Rep. of USA Ethiopia Mexico USSR France Netherlands Yugoslavia Germany, F. R. New Zealand Portugal Hungary No member body expressed disapproval of the document. This International Standard has also been approved by the International Union of Pure and Applied Chemistry (IUPAC). Internationai Organization for Standardization, 1982 Printed in Switzerland INTERNATIONAL STANDARD ISO 6463-1982 (E) Animal and vegetable fats and oils - Determination of butylhydroxyanisole (BHA) and butylhydroxytoluene (BHT) Gas-liguid chromatographic method 1 Scope and field of application 4.3 Dichloromethane or, failing this, carbon disulphide, containing no impurities which could interfere with the deter- This International mination of BHA or BHT by gas chromatography. Standard specifies gas-liquid chromatographic method for the determination of butyl- hydroxyanisole (tert-butyl-4-methoxyphenol) (BHA）and WARNiNG- Dichloromethane andcarbon disulphide butylhydroxytoluene (2,6-di-tert-butyl-4-methylphenol) (BHT), are toxic. In addition, carbon disulphide is very volatile used as antioxidants, in animal and vegetable fats and oils. and explosive and particular care must be exercised in using it. NOTE Themethodalsopermitsquantitativedeterminationofter tiobutylhydroquinone (TBHQ). 4.4 Methyl undecanoate, minimum purity 99 %. 4.5 Butylhydroxyanisole, minimum purity 98 %. 2 Reference Iso 5558, Animal and vegetable fats and oils -- Detection and 4.6 Butylhydroxytoluene, minimum purity 98 %. identification of antioxidants - Thin-layer chromatographic method. 5 Apparatus 3Principle Usual laboratory equipment, and in particular : Dissolution of the fat or oil in a suitable solvent, direct injection into a gas chromatograph, and use of the internal standard 5.1 Gas chromatograph, with a flame ionization detec- tor and recorder, comprising : method of calibration. 5.1.1 Injection device, together with one of the following Reagents systems to retain the non-volatile fats and oils : 4.1 Carrier gas : an inert gas (such as nitrogen, helium or a) a pre-column packed with siliconized glass wool or argon), carefully dried and containing less than 10 mg of glass beads; oxygen per kilogram. b) a sleeve lined with siliconized glass wool placed in the 4.2Auxiliary gases : injector (only in the case of a horizontal injector). 5.1.2 Column, made of stainless steel or glass, permitting hydrogen, mini