1、BRITISH STANDARDBS EN 14666:2005Surface active Agents Determination of tetraacetyl ethylene diamine (TAED) content in TAED granules Gas chromatographicmethodThe European Standard EN 14666:2005 has the status of a British StandardICS 71.100.40g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g
2、54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58BS EN 14666:2005This British Standard was published under the authority of the Standards Policy and Strategy Committee on 19 August 2005 BSI 19 August 2005ISB
3、N 0 580 46360 5National forewordThis British Standard is the official English language version of EN 14666:2005.The UK participation in its preparation was entrusted to Technical Committee CII/34, Methods of test for surface active agents, which has the responsibility to:A list of organizations repr
4、esented on this committee can be obtained on request to its secretary.Cross-referencesThe British Standards which implement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”,
5、 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 contract. Users are responsible for its correct application.Compliance with a British Standard does not of itself confer im
6、munity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate th
7、em in the UK.Summary of pagesThis document comprises a front cover, an inside front cover, the EN title page, pages 2 to 10, an inside back cover and a back cover.The BSI copyright notice displayed in this document indicates when the document was last issued.Amendments issued since publicationAmd. N
8、o. Date CommentsEUROPEAN STANDARDNORME EUROPENNEEUROPISCHE NORMEN 14666June 2005ICS 71.100.40English versionSurface active Agents - Determination of tetraacetyl ethylenediamine (TAED) content in TAED granules - Gaschromatographic methodAgents de surface - Dtermination de la teneur en ttra-actyl-thyl
9、ne diamine (TAED) dans les granuls deTAED - Mthode par chromatographie en phase gazeuseGrenzflchenaktive Stoffe - Bestimmung desTetraacetylethylendiamin (TAED)-Gehalts in TAED-Granulaten - Gaschromatographisches VerfahrenThis European Standard was approved by CEN on 19 May 2005.CEN members are bound
10、 to comply with the CEN/CENELEC Internal Regulations which stipulate 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 Centr
11、al Secretariat or to any CEN member.This European Standard exists in 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
12、 officialversions.CEN members are the national standards bodies of Austria, 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, Swe
13、den, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT 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
14、. No. EN 14666:2005: EEN 14666:2005 (E) 2ContentsPage Foreword 31 Scope .42 Normative references .43 Principle.44 Reagents45 Apparatus 46 Sampling and preparation of the sample 57 Procedure 58 Calculation and expression of results.69 Precision610 Test report .7Annex A (informative) Typical gas chrom
15、atogram.8Annex B (informative) Results of interlaboratory test .10EN 14666:2005 (E) 3Foreword This document (EN 14666:2005) has been prepared by Technical Committee CEN/TC 276 “Surface active agents”, the secretariat of which is held by AFNOR. This European Standard shall be given the status of a na
16、tional standard, either by publication of an identical text or by endorsement, at the latest by December 2005, and conflicting national standards shall be withdrawn at the latest by December 2005. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followin
17、g countries are bound to implement this European Standard: Austria, 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, S
18、witzerland and United Kingdom. EN 14666:2005 (E) 41 Scope This European Standard specifies a method for the determination of tetraacetyl ethylene diamine (TAED) content greater than or equal to 25 g/100 g in granules. 2 Normative references The following referenced documents are indispensable for th
19、e application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 607, Surface active agents and detergents Methods of sample division.3 Principle The TAED granules are d
20、issolved in acetonitrile, the internal standard is added to this solution and finally it is injected to a gas chromatograph. A flame ionisation detector is used for detection. The results are calculated from the peak areas taking into account the response factors that are determined previously. 4 Re
21、agents During the analysis, unless otherwise specified, use only reagents of recognized analytical grade that have been checked in advance as not interfering with the analytical results. 4.1 Acetonitrile, C2H3N. 4.2 Stearic acid methyl ester, C19H38O2, 99 % (m/m). 4.3 TAED, C10H16O4N2, 99 % (m/m). 4
22、.4 Internal standard solutionWeigh into a 100 ml volumetric flask 250 mg of the stearic acid methyl ester (4.2) to the nearest 0,1 mg and make up to the mark with acetonitrile (4.1). 4.5 Carrier gas, for gas chromatography. 4.6 Auxiliary gases, for gas chromatography. 5 Apparatus Normal laboratory a
23、pparatus and the following: 5.1 Gas chromatograph, with split/splitless injector, flame ionisation detector and integrator or computer. 5.2 Fused silica capillary column, capable of the separation characteristics shown in Figure A1. NOTE A 25 m length, 0,25 mm internal diameter and 0,25 m film thick
24、ness fused silica capillary column with 100% crosslinked dimethyl-polisiloxane stationary phase is advisable. EN 14666:2005 (E) 55.3 Syringe, capacity 5 l.5.4 Filter, porosity 0,45 m. 6 Sampling and preparation of the sample The laboratory sample shall be prepared and stored in accordance with ISO 6
25、07. Granules shall be ground for 1 min in an analytic mill or in a mortar to reach homogeneity. 7 Procedure 7.1 Calibration Weigh into sample vials 25 mg, 50 mg, 75 mg and 100 mg of TAED (4.3) to the nearest 0,1 mg. NOTE It is not required to perform the calibration before each series of samples. Ho
26、wever a standard of 50 mg of TAED in 20 ml of the internal standard solution (4.4) should be analysed before each measurement. The value of response factor should not differ by more than 0,5 % from the average value of the calibration. Add 20 ml of the internal standard solution (4.4) and dissolve t
27、he samples. Inject each calibration solution three times into the gas chromatograph (5.1). An example of a calibration chromatogram is given in Figure A.1. Record the peak areas of TAED and internal standard for each chromatogram and carry out a linear regression analysis of (AIS/AI) versus (mIS/mI)
28、. The response factor of TAED referring to the internal standard is the slope of the calculated calibration curve. If a correlation factor of less than 0,98 is obtained prepare new calibration solution and re-inject. If a data acquisition system is not available, calculate the response factor RFifor
29、 each chromatogram according to the following formula: ISIIISimAmARF= (1) where AIthe peak area of TAED in the chromatogram i of calibration solution; AISthe peak area of the stearic acid methyl ester (4.2) in the chromatogram i of calibration solution; mIthe mass of TAED in the calibration solution
30、 of the chromatogram i, in milligrams; mISthe mass of the stearic acid methyl ester in the calibration solution of the chromatogram i, in milligrams. The response factor RF of TAED referring to the internal standard is the mean value of all RFi. If the relative standard deviation of RF is higher tha
31、n 3 % repeat the calibration procedure and re inject. EN 14666:2005 (E) 67.2 Determination Immediately after grinding or crushing the sample (see Clause 6), weigh approximately 500 mg of the sample (m)to the nearest 0,1 mg into a 100 ml volumetric flask. Add about 250 mg stearic acid methyl ester (4
32、.2) to the nearest 0,1 mg and make up to the mark with acetonitrile (4.1). Insert a stirring rod into the flask and stir for 20 min on a magnetic stirrer at room temperature. Inject the clear solution directly into the gas chromatograph (5.1). If the solution is cloudy, filter it through the filter
33、(5.4) and only then inject it into the gas chromatograph. Set up the gas chromatograph to give results similar to the example chromatogram in Figure A.1. 8 Calculation and expression of results The content of TAED, w(C10H16O4N2), in the sample, expressed in grams per 100 g, is calculated by the equa
34、tion (2): ISSIS241610100)NOHC(AmAmRFw= (2) where RF the response factor of TAED relating to the stearic acid methyl ester (4.2), (see 7.1); mISthe mass of the stearic acid methyl ester, in milligrams (see 7.2); m the mass of the sample, in milligrams (see 7.2); AISthe peak area of the stearic acid m
35、ethyl ester in the chromatogram of the sample solution; ASthe peak area of TAED in the chromatogram of the sample solution. 9 Precision 9.1 Repeatability limit The absolute difference between two independent single test results, obtained using the same method on identical test material in the same l
36、aboratory by the same operator using the same equipment within a short interval of time, will not exceed the repeatability limit, r, in more than 5 % of cases. Precision data are given in Annex B. 9.2 Reproducibility limit The absolute difference between two independent single test results, obtained
37、 using the same method on identical test material in different laboratories by different operators using different equipment, will not exceed the reproducibility limit, R, in more than 5 % of the cases. Precision data are given in Annex B. EN 14666:2005 (E) 710 Test report The test report shall incl
38、ude the following information: a) all information necessary for the complete identification of the sample; b) method used (a reference to this document); c) test results; d) details of any operation not specified in this document or in the European Standards to which reference is made, and any opera
39、tions regarded as optional, as well as any incidents like to have affected the results. EN 14666:2005 (E) 8Annex A (informative)Typical gas chromatogram Key1 TAED 2 stearic acid methyl ester (internal standard) 3 voltage, in millivolts 4 time, in minutes Figure A1 Gas chromatogram of a calibration s
40、olution with 50 mg of TAED EN 14666:2005 (E) 9An example of a suitable set of conditions is: Carrier gas: hydrogen or helium; Column head pressure: 150 kPa (1,5 bar); Split: 50 ml/min; Injection volume: 1,5 l; Injector temperature: 250 C; Detector temperature: 300 C; Temperature programme: 150 C to
41、220 C with 10 C/min; 220C to 300C with 15 C/min. EN 14666:2005 (E) 10 Annex B (informative)Results of inter-laboratory test The inter-laboratory test was carried out in 1999 by the German “Common Committee for Analysis of Surfactants” (GAT). The test sample was a commercial TAED granule. The results
42、 of the inter-laboratory test were evaluated in accordance with ISO 5725-2. Table B1 Results of inter-laboratory test Designation Precision dataNumbers of laboratories participating 6 Numbers of laboratories not eliminated 6 Number of individual test results of all laboratories 18 Mean value, m, in
43、g/100 g 86,19 Repeatability standard deviation sr, in g/100 g 0,304 Repeatability limit r (srx 2,8), in g/100 g 0,850 Reproducibility standard deviation sR, in g/100 g 0,452 Reproducibility limit R (sRx 2,8), in g/100 g 1,266 Repeatability coefficient of variation, in % 0,352 Reproducibility coeffic
44、ient of variation, in % 0,524 blankBS EN 14666:2005BSI389 Chiswick High RoadLondonW4 4ALBSI British Standards InstitutionBSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated
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