EN ISO 16035-2005 en Animal and vegetable fats and oils Determination of low-boiling halogenated hydrocarbons in edible oils《动物和植物脂肪和油 食用油中低沸点卤代烃的测定 (ISO 16035)-2003》.pdf

1、BRITISH STANDARDBS EN ISO 16035:2005Incorporating Amendment No. 1 to BS ISO 16035:2003 (renumbers BS ISO as BS EN ISO 16035:2005)Animal and vegetable fats and oils Determination of low-boiling halogenated hydrocarbons in edible oilsThe European Standard EN ISO 16035:2005 has the status of a British

2、StandardICS 67.200.10g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN ISO 16035:2005This British Standard was published under the authority of

3、the Standards Policy and Strategy Committee on 25 June 2003 BSI 16 February 2006ISBN 0 580 42121 XNational forewordThis British Standard is the English language version of EN ISO 16035:2005. It is identical with ISO 16035:2003.The UK participation in its preparation was entrusted to Technical Commit

4、tee AW/307, Oil seeds 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-referencesThe British Standards which implement international or European publications referred to in thi

5、s document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online.This publication does not purport to include all the necessary provisions of a cont

6、ract. Users are responsible for its 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 proposals f

7、or change, and keep UK interests informed; monitor related international and European developments and promulgate them in the UK.Summary of pagesThis 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 iv, pages 1

8、to 12, an inside back cover and a back cover.The BSI copyright date displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. No. Date Comments15854 February 2006 Renumbers BS ISO 16035:2003 as BS EN ISO 16035:2005EUROPEAN STANDARDNORME EUROPENNEE

9、UROPISCHE NORMEN ISO 16035August 2005ICS 67.200.10English VersionAnimal and vegetable fats and oils Determination of low-boilinghalogenated hydrocarbons in edible oils (ISO 16035:2003)Corps gras dorigines animale et vgtale Dosage deshydrocarbures halogns bas point dbullition dans leshuiles comestibl

10、es (ISO 16035:2003)Tierische und pflanzliche Fette und le Bestimmung vonniedrig siedenden halogenierten Kohlenwasserstoffen inSpeiselen (ISO 16035:2003)This European Standard was approved by CEN on 28 July 2005.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate

11、 the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central Secretariat or to any CEN member.This European Standard exists in

12、 three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of A

13、ustria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDI

14、ZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36 B-1050 Brussels 2005 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN ISO 16035:2005: EForeword The text of ISO 16035:2003 has be

15、en prepared by Technical Committee ISO/TC 34, Agricultural food products, of the International Organization for Standardization (ISO) and has been taken over as EN ISO 16035:2005 by Technical Committee CEN/TC 307, Oilseeds, vegetable and animal fats and oils and their by-products Methods of sampling

16、 and analysis, 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 February 2006, and conflicting national standards shall be withdrawn at the latest by Febr

17、uary 2006. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy,

18、 Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. Endorsement notice The text of ISO 16035:2003 has been approved by CEN as EN ISO 16035:2005 without any modifications. EN ISO 16035:2005Reference numberISO

19、 16035:2003(E)INTERNATIONAL STANDARD ISO16035First edition2003-04-15Animal and vegetable fats and oils Determination of low-boiling halogenated hydrocarbons in edible oils Corps gras dorigines animale et vgtale Dosage des hydrocarbures halogns bas point dbullition dans les huiles comestibles EN ISO

20、16035:2005ii iiiContents Page Foreword iv 1 Scope 1 2 Normative references . 1 3 Terms and definitions. 1 4 Principle . 1 5 Reagents and materials 1 6 Apparatus. 3 7 Sampling 4 8 Preparation of samples 5 8.1 General. 5 8.2 Test solutions 5 8.3 Calibration solutions 5 8.4 Blank sample . 5 9 Procedure

21、. 5 9.1 Gas chromatography conditions. 5 9.2 Gas chromatography 6 10 Calculation and expression of results 7 10.1 Determination of the ratios from the measurement for the sample and internal standard. 7 10.2 Calculation of regression from calibration solutions . 7 10.3 Calculation of the content of

22、halogenated hydrocarbons 7 11 Precision 8 11.1 Results of interlaboratory test. 8 11.2 Repeatability 8 11.3 Reproducibility 8 12 Test report 8 Annex A (informative) Results of interlaboratory test 9 Bibliography . 12 EN ISO 16035:2005iv Foreword ISO (the International Organization for Standardizatio

23、n) 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 has been established has the right to be rep

24、resented 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 electrotechnical standardization. International Standards a

25、re drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an Internatio

26、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 document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 16035 was pr

27、epared by Technical Committee ISO/TC 34, Food products, Subcommittee SC 11, Animal and vegetable fats and oils. EN ISO 16035:2005INTENRATIONAL TSANDADR I SO 3002 All irhgts seredevr 1Animal and vegetable fats and oils Determination of low-boiling halogenated hydrocarbons in edible oils 1 Scope This

28、International Standard specifies a method for the determination of low-boiling halogenated hydrocarbons by means of static headspace gas chromatography. Halogenated hydrocarbon solvents are ubiquitously distributed toxic compounds. The method is applicable to all edible fats and oils to determine th

29、ese compounds in the range 0,01 mg/kg to 0,2 mg/kg. 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

30、 any amendments) applies. ISO 661:1989, Animal and vegetable fats and oils Preparation of test sample 3 Terms and definitions For the purposes of this document, the following terms and definitions apply. 3.1 halogenated hydrocarbons content content of low-boiling halogenated hydrocarbons in the prod

31、ucts determined by the method specified in this International Standard NOTE 1 The halogenated hydrocarbons content is expressed in milligrams per kilogram. NOTE 2 For the purposes of this International Standard, the term low-boiling halogenated hydrocarbons covers those specified in 5.1. 4 Principle

32、 The contents of halogenated hydrocarbons in the test sample are determined by manual or automatic static headspace gas chromatography of a sample drawn from the vapour space above the heated test sample. A capillary column is used for separation, and detection is carried out by means of an electron

33、 capture detector (ECD). An internal standard is used to obtain a quantitative evaluation. For the purpose of calibration, calibration curves are obtained by the addition of various halogenated hydrocarbon calibration solutions to a blank sample. 5 Reagents and materials WARNING Attention is drawn t

34、o the regulations which prescribe the handling of dangerous matter. Technical, organizational and personal safety measurements shall be followed. Use only reagents of recognized analytical grade unless otherwise stated. 1EN ISO 16035:20052 I SO 3002 All irhgts seredevr5.1 Standard substances, of app

35、ropriate purity as required by the nature and number of components to be determined, for example, the following. 5.1.1 1,1,1-Trichloroethane, density = 1,34 g/ml. 5.1.2 Tetrachloromethane, density = 1,59 g/ml. 5.1.3 1,1,2-Trichloroethene, density = 1,46 g/ml. 5.1.4 Tetrachloroethene, density = 1,63

36、g/ml. 5.1.5 2-Bromo-1-chloropropane (internal standard), density = 1,54 g/ml. 5.1.6 Dichloromethane (methylene chloride), density = 1,32 g/ml. 5.1.7 Trichloromethane (chloroform), density = 1,47 g/ml. 5.1.8 Bromodichloromethane, density = 1,98 g/ml. 5.1.9 Dibromochloromethane, density = 2,45 g/ml. 5

37、.1.10 Tribromomethane (bromoform), density = 2,89 g/ml. 5.1.11 1,1,2-Trichloro-1,2,2-trifluoroethane, density = 1,57 g/ml. 5.2 Isooctane, suitable for haloform analysis. Check the isooctane for its halogenated hydrocarbons content. 5.3 Nitrogen (extra purified), helium or hydrogen, as carrier gas. 5

38、.4 Argon/methane or nitrogen, as purge gas for the ECD. Use in accordance with the manufacturers instructions. 5.5 Halogenated hydrocarbons stock solutions Add 10 l of each of the standard substances (5.1) to be determined to a 100 ml volumetric flask that contains 40 ml of isooctane, using an injec

39、tion syringe and make up to the mark. However, only add 5 l of tetrachloromethane since its detection sensitivity is very high, but add 500 l of dichloromethane since its detection sensitivity is very low. These stock solutions contain: 1,1,1-trichloroethane: 13,40 mg/100 ml; tetrachloromethane: 7,9

40、5 mg/100 ml; 1,1,2-trichloroethene: 14,60 mg/100 ml; tetrachloroethene: 16,30 mg/100 ml; dichloromethane: 660,00 mg/100 ml; trichloromethane: 14,70 mg/100 ml; bromodichloromethane: 19,80 mg/100 ml; dibromochloromethane: 24,50 mg/100 ml; tribromomethane: 28,90 mg/100 ml; 1,1,2-trichloro-1,2,2-trifluo

41、roethane: 15,70 mg/100 ml. 2EN ISO 16035:20055.6 Halogenated hydrocarbons standard solutions I, II, III and IV Use the stock solution (5.5) to prepare standard solutions (I, II, III, IV) of appropriate concentrations by adding, for example, 200 l, 400 l, 1 000 l and 2 000 l of the stock solution to

42、10 ml volumetric flasks that contain a little isooctane, and make up to the mark with isooctane. The internal standard (5.7) may also be added to the halogenated hydrocarbon standard solutions. 5.7 Internal standard solution (2-bromo-1-chloropropane solution). Add 200 l 2-bromo-1-chloropropane to a

43、little isooctane in a 50 ml volumetric flask using an injection syringe and make up to the mark with isooctane (concentration by mass = 308 mg/50 ml). In order to obtain a suitable dilution, add 400 l of the above solution to a little isooctane in a 10 ml volumetric flask and make up to the mark wit

44、h isooctane. The concentration by mass of this solution is 2,464 mg/10 ml. 5.8 Blank solution Use an oil which is as free as possible from the halogenated hydrocarbons. 6 Apparatus 6.1 Gas chromatograph, suitable for use with a capillary column and fitted with an electron capture detector (ECD) and,

45、 if available, an automatic headspace sampler. The conditioning apparatus used for the injection vials shall have a temperature range of at least 80 C. It is advantageous to have a facility for heating up to 110 C in determining the halogenated hydrocarbon contents of fats and oils since higher sens

46、itivities can be achieved. It is also advisable to use an apparatus which makes it possible to establish a constant conditioning time for all the samples. 6.2 Low-polarity glass or quartz capillary column, whose separation efficiency shall be high enough to make it possible to separate all the subst

47、ances shown in the chromatogram in Figure 1. NOTE A fused silica column of length 50 m and internal diameter 0,32 mm, coated with cross-linked SE 54, film thickness 1 m, has been found to be suitable. 6.3 Injection vials, of capacities 10 ml or 25 ml, with gas-tight closures and PTFE-faced septa. Ch

48、eck whether the injection vials and closures emit any halogenated hydrocarbons and store them in a sealed container. Special attention shall be paid to leak tightness if tempering times are long. Leaks are indicated by variations of the peak areas of the internal standard. 6.4 Microsyringes, of capa

49、cities 10 l, 50 l and 100 l. 6.5 Gas-tight injection syringe, of capacity 2,5 ml, with needle of wide diameter with lateral orifice for manual injections from the headspace. 6.6 Heating bath or aluminium block, with clamps for holding injection vials (6.3), thermostatically maintained at 80 C. Glycerol is recommended as heating fluid for continuous operation in a heating bath. EN ISO 16035:200534 I SO 3002 All irhgts seredevrPeak identification 1 dichloromethane 2 1,1,2-trichloro-1,2,2-trifluo