BS EN 13560-2001 Surface active agents - Determination of amide nitrogen content - Potentiometric titration《表面活性剂 酰胺氮含量的测定 电势滴定法》.pdf

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1、Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIBRITISH STANDARD BS EN 13560:2001 Incorporating Corrigendum No. 1 Surface active agents Determination of amide nitrogen content Potentiometric titration The European Standard EN 135

2、60:2001 has the status of a British Standard ICS 71.100.40 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIBS EN 13560:2001 This British Standard, having been prepared under the direction of the Materials and Chemicals Sector Pol

3、icy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 23 September 2002 BSI 10 April 2003 ISBN 0 580 40453 6 National foreword This British Standard is the official English language version of EN 13560:2001, including Corrigendum December 200

4、2. 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 represented on this committee can be obtained on request to its secretary. Cross-references The British Standard

5、s 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”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This pu

6、blication 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 immunity from legal obligations. aid enquirers to understand the text; present to the responsible internat

7、ional/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 them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN titl

8、e page, pages 2 to 10, 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 publication Amd. No. Date Comments 14371 Corrigendum No. 1 10 April 2003 Change to 4.4 Licensed Copy: Wang Bin, ISO/Exc

9、hange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSI EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN 13560 December 2001 ICS 71.100.40 Incorporating corrigendum December 2002 English version Surface active agents - Determination of amide nitrogen content - Pot

10、entiometric titration Agents de surface - Dtermination de la teneur en azote sous forme amide - Titrage potentiomtrique Grenzflchenaktive Stoffe - Bestimmung des Gehaltes an Amid-Stickstoff - Potentiometrische Titration This European Standard was approved by CEN on 11 November 2001. CEN members are

11、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 lists and bibliographical references concerning such national standards may be obtained on application to th

12、e 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 responsibility of a CEN member into its own language and notified to the Management Centre has the same status a

13、s the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZA

14、TION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: rue de Stassart, 36 B-1050 Brussels 2001 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN 13560:2001 E Licensed Copy: Wang Bin, ISO/Exchange China

15、 Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 2 Contents page Foreword3 1 Scope4 2 Normative references4 3 Principle4 4 Reagents.4 5 Apparatus.4 6 Sampling.4 7 Procedure.5 8 Expression of results5 9 Precision.6 10 Test report7 Annex A (informative) Ins

16、trument settings.8 Annex B (informative) Typical titration curves.9 Annex C (informative) Results of the interlaboratory test 10 Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 3 Foreword This European Standard

17、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 publication of an identical text or by endorsement, at the latest by June 2002, and conflicting n

18、ational standards shall be withdrawn at the latest by June 2002. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Gree

19、ce, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. The annexes A, B and C are informative. Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E)

20、4 1 Scope This European Standard specifies a method for the determination of amide nitrogen content in surface active agents by potentiometric titration. It is not applicable to other basic substances. 2 Normative reference This European Standard incorporates by dated or undated reference, provision

21、s from other publications. These normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to this European Standard only when incorporated in it by a

22、mendment or revision. For undated references the latest edition of the publication referred to applies (including amendments). ISO 607, Surface active agents and detergents Methods of sample division. 3 Principle The sum of amide nitrogen and amine nitrogen as well as soap are determined by potentio

23、metric titration of the test sample, dissolved in acetic acid anhydride, with standard trifluoromethane sulfonic acid solution. The content of amine nitrogen as well as soap are determined by potentiometric titration of the test sample, dissolved in glacial acetic acid, with trifluoromethane sulfoni

24、c acid standard volumetric solution. From the difference between the two titrations, the amide nitrogen content in grams per 100 g is calculated. 4 Reagents During the analysis, unless otherwise specified, use only reagents of recognized analytical grade and have been checked in advance as to not in

25、terfere with the analytical results. 4.1 Glacial acetic acid, purity 100 %. 4.2 Acetic acid anhydride, purity 98,5 % (minimum). 4.3 Trifluoromethane sulfonic acid standard volumetric solution, c (HSO 3 CF 3 ) = 0,1 mol/l, in acetic acid (4.1). NOTE Perchloric acid, c (HClO 4 ) = 0,1 mol/l, in glacia

26、l acetic acid can also be used. 4.4 Tris(hydroxymethyl)aminomethane (titrimetric standard), dried at (105 2) C, purity 99,9 % (minimum). 5 Apparatus Ordinary laboratory apparatus and the following. 5.1 Potentiometric titrating apparatus, comprising a titrator with a combined pH glass electrode, a 20

27、 ml plunger burette and a stirrer. NOTE An example of instrument settings is given in annex A. 5.2 Beaker, capacity 150 ml. 5.3 Analytical balance, accurate to 0,1 mg. 6 Sampling The laboratory sample of the surface active agent shall be prepared and stored in accordance with ISO 607. Licensed Copy:

28、 Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 5 7 Procedure 7.1 Factor of the trifluoromethane sulfonic acid standard volumetric solution Weigh approximately 120 mg (m 1 ) of tris(hydroxymethyl)aminomethane (4.4) to the nea

29、rest 0,1 mg into the beaker (5.2) and dissolve in 80 ml of glacial acetic acid (4.1). Immerse the electrode, stir and titrate with trifluoromethane sulfonic acid standard volumetric solution (4.3). Record the consumption at the equivalent (inflection) point (volume V 1 ) ; (see annex B). Calculate t

30、he factor (f) for this solution from the consumption of trifluoromethane sulfonic acid standard volumetric solution (4.3) by the equation (1) : c V M m f000 1 1 = (1) where m 1is the mass of tris(hydroxymethyl)aminomethane (4.4), in grams ; M is the molar mass of tris(hydroxymethyl)aminomethane (4.4

31、), M = 121,14 g/mol ; V 1is the consumption of trifluoromethane sulfonic acid standard volumetric solution (4.3), in millilitres ; c is the concentration of the trifluoromethane sulfonic acid standard volumetric solution (4.3), in moles per litre. 7.2 Titration of the amide nitrogen Weigh from the s

32、ample to be tested a quantity (m 2 ) which contains about 0,5 mmol to 1 mmol of amide nitrogen to the nearest 0,1 mg into the beaker (5.2). Dissolve the sample in 80 ml of acetic acid anhydride (4.2), under light heating if needed. Immerse the electrode, stir and titrate with trifluoromethane sulfon

33、ic acid standard volumetric solution (4.3). Record the consumption at the equivalent (inflection) point (volume V 2 ) ; (see annex B). 7.3 Titration of the total base nitrogen Weigh from the sample to be tested a quantity (m 3 ) which contains about 0,5 mmol to 1 mmol of total base nitrogen to the n

34、earest 0,1 mg into the beaker (5.2). Dissolve the sample in 80 ml of glacial acetic acid (4.1), under light heating if needed. Immerse the electrode, stir and titrate with trifluoromethane sulfonic acid standard volumetric solution (4.3). Record the consumption at the equivalent (inflection) point (

35、volume V 3 ) ; (see annex B). 8 Expression of results 8.1 Calculation of the amide nitrogen content Calculate the amide nitrogen content, w an , in grams per 100 g, by the equation (2) : tbn an w m M f c V w = 000 1 100 2 2(2) Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre,

36、 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 6 where V 2is the consumption of the trifluoromethane sulfonic acid standard volumetric solution (4.3) according to 7.2, in millliitres ; c is the concentration of the trifluoromethane sulfonic acid standard volumetric solution (4.3), i

37、n moles per litre ; f is the factor of the trifluoromethane sulfonic acid standard volumetric solution (4.3) determined according to 7.1 ; M is the molar mass of nitrogen, M = 14 g/mol ; m 2is the mass of the sample according to 7.2, in grams ; w tbnis the content of total base nitrogen titrated acc

38、ording to 7.3, in grams per 100 g. The result shall be given to two decimal places. 8.2 Calculation of the total base nitrogen content Calculate the total base nitrogen content, w tbn , in grams per 100 g, by the equation (3) : 000 1 100 3 3 = m M f c V w tbn(3) where V 3is the consumption of the tr

39、ifluoromethane sulfonic acid standard volumetric solution (4.3) according to 7.3, in millilitres ; c is the concentration of the trifluoromethane sulfonic acid standard volumetric solution (4.3), in moles per litre ; f is the factor of the trifluoromethane sulfonic acid standard volumetric solution

40、(4.3) determined according to 7.1 ; M is the molar mass of nitrogen, M = 14 g/mol ; m 3is the mass of the sample according to 7.3, in grams. The result shall be given to two decimal places. 9 Precision 9.1 Repeatability limit The absolute difference between two independent single test results, obtai

41、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 C. 9.2 R

42、eproductibility limit The absolute difference between two independent 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. Ty

43、pical precision data obtained in a ring test are given in annex C. Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 7 10 Test report The test report shall include the following information : a) all information ne

44、cessary for the complete identification of the sample ; b) the method used (a reference to this European Standard) ; c) the test results ; d) details of any operations not specified in this European Standard or in the European Standards to which reference is made, and any operations regarded as opti

45、onal, as well as any incidents likely to have affected the results. Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 8 Annex A (informative) Instrument settings Data given are settings for the Metrohm Titroproces

46、sor 682 1)and are intended to act as a guideline, only : Pause 1 : 20 s Electrical input : 1 Titration rate : 1,50 ml/min Anticipation : 40 Stop volume : 15,00 ml Temperature : 25 C Equivalent point (EP) criterion : 1 1) Metrohm Titroprocessor 682 is the trade name of an instrument supplied by Metro

47、hm Ltd. (CH-9101 Herisau, Switzerland). This information is given for the convenience of users of this European Standard and does not constitute an endorsement by CEN of the instrument named. Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Co

48、py, (c) BSIEN 13560:2001 (E) 9 Annex B (informative) Typical titration curves Key 1 Equivalent point 2 Consumption of the standard volumetric solution 3 Voltage Figure B.1 Titration of the amide nitrogen Key 1 Equivalent point 2 Consumption of the standard volumetric solution 3 Voltage Figure B.2 Ti

49、tration of the total base nitrogen Licensed Copy: Wang Bin, ISO/Exchange China Standards Information Centre, 15 September 2003, Uncontrolled Copy, (c) BSIEN 13560:2001 (E) 10 Annex C (informative) Results of the interlaboratory test The interlaboratory test was carried out in 1997 by AISE/CESIO WG “Surfactant Analysis“. The test sample was a commercial product (cocofatty acid diethanolamide). Table C.1 Ring test results Designation Precision data Number of lab