1、BRITISH STANDARD BS EN 13560:2001 Incorporating Corrigendum No. 1 Surface active agents Determination of amide nitrogen content Potentiometric titration The European Standard EN 13560:2001 has the status of a British Standard ICS 71.100.40 BS EN 13560:2001 This British Standard, having been prepared
2、 under the direction of the Materials and Chemicals Sector Policy 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 languag
3、e version of EN 13560:2001, including Corrigendum December 2002. 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 r
4、equest 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 Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BS
5、I 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 immunity from legal obligations. aid enquire
6、rs 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 them in the UK. Summary of pages This docume
7、nt 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 date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 14371 Corrigendum No.
8、1 10 April 2003 Change to 4.4 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 - Potentiometric titration Agents de surface - Dtermination de
9、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 bound to comply with the CEN/CENELEC Internal Regulations
10、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 the Management Centre or to any CEN member. This European St
11、andard 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 as the official versions. CEN members are the national stan
12、dards 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 STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR
13、 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 EEN 13560:2001 (E) 2 Contents page Foreword3 1 Scope4 2 Normative references4 3 Principle4 4 Reagents.4
14、 5 Apparatus.4 6 Sampling.4 7 Procedure.5 8 Expression of results5 9 Precision.6 10 Test report7 Annex A (informative) Instrument settings.8 Annex B (informative) Typical titration curves.9 Annex C (informative) Results of the interlaboratory test 10 EN 13560:2001 (E) 3 Foreword This European Standa
15、rd 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 conflictin
16、g national 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, G
17、reece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. The annexes A, B and C are informative. EN 13560:2001 (E) 4 1 Scope This European Standard specifies a method for the determination of amide nitrogen content in surface activ
18、e agents by potentiometric titration. It is not applicable to other basic substances. 2 Normative reference 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 publi
19、cations 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 amendment or revision. For undated references the latest edition of the publication referred to applies (including am
20、endments). 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 potentiometric titration of the test sample, dissolved in acetic acid anhydride, with standard trifluoromethane sulfonic aci
21、d 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 sulfonic acid standard volumetric solution. From the difference between the two titrations, the amide nitrogen content in g
22、rams 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 interfere with the analytical results. 4.1 Glacial acetic acid, purity 100 %. 4.2 Acetic acid anhydride, purity 98,5 %
23、 (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 glacial acetic acid can also be used. 4.4 Tris(hydroxymethyl)aminomethane (titrimetric standard), dried at (105 2) C, puri
24、ty 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 ml plunger burette and a stirrer. NOTE An example of instrument settings is given in annex A. 5.2 Beaker, capacity
25、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. EN 13560:2001 (E) 5 7 Procedure 7.1 Factor of the trifluoromethane sulfonic acid standard volumetric solution Weigh approximately
26、120 mg (m 1 ) of tris(hydroxymethyl)aminomethane (4.4) to the nearest 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 equival
27、ent (inflection) point (volume V 1 ) ; (see annex B). Calculate the 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 gr
28、ams ; M is the molar mass of tris(hydroxymethyl)aminomethane (4.4), 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 mole
29、s per litre. 7.2 Titration of the amide nitrogen Weigh from the sample 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. Imm
30、erse the electrode, stir and titrate with trifluoromethane sulfonic 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
31、contains about 0,5 mmol to 1 mmol of total base nitrogen to the nearest 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.
32、3). Record the consumption at the equivalent (inflection) point (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) EN 13560
33、: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), in moles per litre ; f is the factor of the trifluorome
34、thane 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 according to 7.3, in grams per 100 g. The result shall be
35、 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 trifluoromethane sulfonic acid standard volumetric solut
36、ion (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 (4.3) determined according to 7.1 ; M is the molar mas
37、s 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, obtained using the same method on identical test material i
38、n 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 Reproductibility limit The absolute difference between
39、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. Typical precision data obtained in a ring test are given
40、 in annex C. EN 13560:2001 (E) 7 10 Test report The test report shall include the following information : a) all information necessary 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 s
41、pecified in this European Standard or in the European Standards to which reference is made, and any operations regarded as optional, as well as any incidents likely to have affected the results. EN 13560:2001 (E) 8 Annex A (informative) Instrument settings Data given are settings for the Metrohm Tit
42、roprocessor 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
43、by Metrohm 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. EN 13560:2001 (E) 9 Annex B (informative) Typical titration curves Key 1 Equivalent point 2 Consumpt
44、ion 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 Titration of the total base nitrogen EN 13560:2001 (E) 10 Annex C (informative) Results of the interlaboratory te
45、st 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 laboratories participating 12 Number of laboratories not eliminated 1
46、2 Number of individual test results of all laboratories on each sample 36 Mean value, w an , in g/100 g 4,18 Repeatability standard deviation, s r ,in g/100 g 0,056 Repeatability limit r, (r = s r 2,8), in g/100 g 0,16 Reproducibility standard deviation, s R , in g/100 g 0,074 Reproducibility limit
47、R, (R = s R 2,8), in g/100 g 0,21 Repeatability coefficient of variation, in % 1,3 Reproducibility coefficient of variation, in % 1,8 blankBS EN 13560:2001 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing Britis
48、h Standards. It presents the UK view on standards in Europe and at the international level. It is incorporated by Royal Charter. Revisions British Standards are updated by amendment or revision. Users of British Standards should make sure that they possess the latest amendments or editions. It is th
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