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1、BRITISH STANDARD BS EN 13320:2002 Surface active agents Gas chromatographic trace determination of free ethylene oxide in ethoxylates The European Standard EN 13320:2002 has the status of a British Standard ICS 71.100.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Licensed
2、 Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS EN 13320:2002 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards
3、Policy and Strategy Committee on 28 March 2002 BSI 28 March 2002 ISBN 0 580 39315 1 National foreword This British Standard is the official English language version of EN 13320:2002. The UK participation in its preparation was entrusted to Technical Committee CII/34, Methods of test for surface acti
4、ve agents, 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 document may be found in the BSI Standards
5、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 British Standards are responsible for th
6、eir 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 European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed;
7、 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 title page, pages 2 to 12, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates
8、when the document was last issued. Amendments issued since publication Amd. No. DateComments Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13320 February 2002 ICS 71.100.40 English versi
9、on Surface active agents - Gas chromatographic trace determination of free ethylene oxide in ethoxylates Agents de surface - Dtermination de traces doxyde dthylne libre dans les thoxylats par chromatographie en phase gazeuse Grenzflchenaktive Stoffe - Gaschromatographische Spurenbestimmung von freie
10、m Ethylenoxid in Ethoxylaten This European Standard was approved by CEN on 16 November 2001. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date
11、 lists and bibliographical references concerning such national standards may be obtained on application to the Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the res
12、ponsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Mal
13、ta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2002 CENAll rights of exploitation in any form and by any mean
14、s reserved worldwide for CEN national Members. Ref. No. EN 13320:2002 E Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13320:2002 (E) 2 Contents page Foreword3 1Scope 4 2Normative references 4 3Principle4 4Reagents.4 5Apparatus .4 6Sampl
15、ing and preparation of the test sample.5 7Procedure .5 8Calculation and expression of results.7 9Precision.7 10Test report 8 Annex A (informative) Ring test results9 Annex B (informative) Titration of ethylene oxide stock solution11 Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT
16、+00:00 2006, Uncontrolled Copy, (c) BSI EN 13320:2002 (E) 3 Foreword This document EN 13320 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 national standard, either by publi
17、cation of an identical text or by endorsement, at the latest by August 2002, and conflicting national standards shall be withdrawn at the latest by August 2002. The annexes A and B are informative. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followi
18、ng countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Licensed Copy: sheffieldun sheffieldu
19、n, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13320:2002 (E) 4 1 Scope This European Standard specifies a test method for the determination of the content of free ethylene oxide in the range from 1 mg/kg to 100 mg/kg in polyglycols, ethoxylates of alcohols and alkylphenols
20、 and in fatty acid polyglycol esters. 2 Normative references This European Standard incorporates by dated or undated reference, provisions from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated referen
21、ces, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). EN ISO 3696, Water for analytical la
22、boratory use Specification and test methods (ISO 3696:1987). ISO 607, Surface active agents and detergents Test methods of sample division. 3 Principle The ethoxylates are, after addition of water, analyzed by gas chromatography using a head-space sampling accessory. The free ethylene oxide content
23、is determined by the standard addition test method. 4 Reagents During the analysis, unless otherwise specified, use only reagents of recognized analytical grade and have been checked in advance as to not interfere with the analytical results. 4.1Water complying with grade 1 as defined in EN ISO 3696
24、. 4.2Ethylene oxide, C2H4O, w(C2H4O) ? 99,5 %. 4.3Ethylene oxide, C2H4O, dissolved in dichloromethane, vials containing 50 mg of ethylene oxide dissolved in 1 ml of dichloromethane. 4.4N,N-dimethylformamide, C3H7NO. 5 Apparatus Ordinary laboratory apparatus and the following. 5.1 Capillary gas chrom
25、atograph, with flame ionisation detector (FID) and head-space sampling accessory. The apparatus shall be equipped with a split system. The head-space sampling accessory shall be designed such that each head-space bottle can be thermostated for a defined time. NOTESince ethylene oxide is easily decom
26、posed by traces of impurities such as acids and transition metals, (catalysed decomposition), a meticulously clean sampling accessory is necessary. 5.2Fused silica capillary column, coating: crosslinked dimethylpolysiloxanes, column length 30 m, internal diameter 0,25 mm, film thickness 1,0 ?. 5.3Vi
27、als, closable by means of a septum, 20 ml, suitable for head-space sampling accessory. 5.4Septums and aluminium caps, lined with aluminium or polytetrafluoroethylene (PTFE) for closing the vials. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) B
28、SI EN 13320:2002 (E) 5 5.5Sealing pliers, for sealing the caps onto the vials. 5.6 Integrator or computer, with appropriate evaluation programme. 5.7 Analytical balance, accurate to 0,1 mg. 6 Sampling and preparation of the test sample 6.1 Sampling The laboratory samples shall be prepared and stored
29、 in accordance with ISO 607. 6.2 Test sample NOTE 1The test samples can be in liquid, paste or solid form. For paste-like products, liquefy and homogenize the laboratory samples by gentle warming. NOTE 2If the test sample is heated above 50 C, low results will be obtained. Do not melt solid products
30、 above 50 C. 7 Procedure 7.1 Preparation of calibration solutions 7.1.1 Standard solutions Prepare a stock solution of ethylene oxide (EO) (4.2) either by : a) Difference weighing Weigh a 200 ml volumetric flask containing about 100 ml of water. Pass about 500 mg of ethylene oxide (4.2) into the wat
31、er and reweigh. Make up the solution to 200 ml with water. In place of difference weighing, the addition of ethylene oxide (4.2) can be carried out by weighing-in using a cooled syringe, or b) Using a vial Dissolve the contents of a vial of ethylene oxide (4.3) in 250 ml of N,N-dimethylformamide (4.
32、4). NOTEA method of titration of the ethylene oxide stock solution is given in annex B. Prepare standard solutions with concentrations of ?(C2H4O) = 0,1 g/100 ml and ?(C2H4O) = 0,01 g/100 ml by multistage dilutions with water from the stock solution. Store the standard solutions in a refrigerator. 7
33、.1.2 Calibration solutions Prepare calibration solution A as follows : Place 2 ml of ethylene oxide standard solution with a concentration of ?(C2H4O) = 0,01 g/100 ml in a 100 ml volumetric flask and make up to the mark with water. 1 ml of this solution contains 2 ? Licensed Copy: sheffieldun sheffi
34、eldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13320:2002 (E) 6 Prepare calibration solution B as follows : Place 1 ml of ethylene oxide standard solution with a concentration of ?(C2H4O) = 0,1 g/100 ml in a 100 ml volumetric flask and make up to the mark with water. 1
35、ml of this solution contains 10 ? 7.2 Determination Weigh about 1 g of the test sample (6.2), to the nearest 0,1 mg into each of two vials and add 1 ml of water to each. Close the vials and make sure that they are pressure-tight. Weigh about 1 g of the test sample (6.2) to the nearest 0,1 mg into ea
36、ch of two further vials and add 1 ml of calibration solution A or B to each. Close the vials and make sure that they are pressure-tight. For products with a low degree of ethoxylation, solubility problems can be encountered in pure water. In this case, the determination can be carried out using a di
37、fferent solvent such as toluene or N,N-dimethylformamide, provided that it has been shown to give comparable results. The solvent used shall be reported under e) of the test report (see clause 10). Equilibrate the solutions for 45 min at (70 ? 1) C. Inject the solutions and perform the analysis usin
38、g the following gas chromatographic conditions : ? temperature of the transfer line :150 C ; ? thermostating temperature :70 C ; ? pressure build-up time :3 s ; ? injection time :6 s ; ? analysis time :45 min. NOTE 1GC conditions deviating from those given above may be used provided that a correspon
39、ding separation performance is demonstrated. a) Temperature ? oven :50 ?C isothermal for 5 min, then from 50 C to 180 C at 5 C/min ; ? detector (FID) :250 ?C. b) Carrier gas ? helium :about 1 ml/min ; ? column pressure :about 70 kPa (0,7 bar) ; ? split :about 1 : 40. c) Hydrogen and airOptimized for
40、 FID ; d) Evaluation Using an electronic integrator or computer, with appropriate evaluation programme. NOTE 2Unknown constituents of the test sample which are eluted at the same retention time as ethylene oxide can cause systematic errors. Compounds that commonly occur in ethoxylates such as methan
41、ol, ethanol, acetaldehyde and 1,4-dioxane are separated from ethylene oxide under the given separation conditions. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13320:2002 (E) 7 8 Calculation and expression of results The ethylene oxide
42、 content, wj, in micrograms per gram of the test sample, is calculated using the following equations : m A = A j j 2 1 ? 2 1=j (1) ? ? ? ? 2 1 kk kk 2 1 k mC AmB f / )/( _ (2) fm A w j j j= (3) where Ais the mean peak area of ethylene oxide per unit mass of the original test sample, in millivolts se
43、conds per gram ; Aiis the peak area of ethylene oxide in the original test sample in the jth individual determination, in millivolts seconds ; mjis the mass of the original test sample weighed-in for the jth individual determination, in grams ; jis the index of the individual determination ; fis the
44、 mean headspace response factor out of two standard additions, in millivolts seconds per microgram ; Bkis the peak area of ethylene oxide in the test sample with the kth standard addition, in millivolts seconds ; Ckis the mass of ethylene oxide added to the test sample, in micrograms ; mkis the mass
45、 of the original test sample weighed-in for the kth standard addition, in grams ; kis the index for the standard addition. Calculate the result as the mean of w1 and w2 to the nearest 0,1 ? 9 Precision 9.1 Repeatability limit The absolute difference between two independent single test results, obtai
46、ned using the same method on identical test material in the same laboratory 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. Typical precision data obtained in a ring test are given in annex A. 9.2 R
47、eproducibility limit The absolute difference between two single test results, obtained 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 cases. Licensed Copy:
48、sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy, (c) BSI EN 13320:2002 (E) 8 Typical precision data obtained in a ring test are given in annex A. 10 Test report The information shall include the following information : a) all information necessary for the complete
49、identification of the sample ; b) a reference to this European Standard ; c) the GC conditions used if deviating from those given in 7.2 ; d) the results calculated according to clause 8 and the test method chosen for evaluation of the results ; e) details of any operation not specified in this European Standard and any operation regarded as optional as well as any incidents likely to have affected the results. Licensed Copy: sheffieldun sheffieldun, na, Mon Oct 30 02:14:21 GMT+00:00 2006, Uncontrolled Copy