DIN EN ISO 2871-2-2010 Surface active agents - Detergents - Determination of cationic-active matter content - Part 2 Cationic-active matter of low molecular mass (between 200 and 5.pdf

1、June 2010 Translation by DIN-Sprachendienst.English price group 8No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS 71

2、.100.40!$i8“1700421www.din.deDDIN EN ISO 2871-2Surface active agents Detergents Determination of cationic-active matter content Part 2: Cationic-activematteroflowmolecularmass(between 200 and 500) (ISO 2871-2:2010)English translation of DIN EN ISO 2871-2:2010-06Tenside Waschmittel Bestimmung des Geh

3、altes der kationaktiven Substanz Teil 2: Kationaktive Substanz niedriger Molmasse (zwischen 200 und 500) (ISO 2871-2:2010)Englische bersetzung von DIN EN ISO 2871-2:2010-06Agents de surface Dtergents Dtermination de la teneur en matire active cationique Partie 2: Matire activecationique faible masse

4、 molculaire (entre 200 et 500) (ISO 2871-2:2010)Traduction anglaise de DIN EN ISO 2871-2:2010-06SupersedesDIN EN ISO 2871-2:1994-12www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.05.1011DIN EN ISO 2871-2:2010-06 A comma is used as

5、the decimal marker. National foreword This standard has been prepared by Technical Committee CEN/TC 276 “Surface active agents” (Secretariat: AFNOR, France) in collaboration with Technical Committee ISO/TC 91 “Surface active agents” (Secretariat: ISIRI, Iran). The responsible German body involved in

6、 its preparation was the Normenausschuss Materialprfung (Materials Testing Standards Committee), Working Committee NA 062-05-62 AA Analytik von Tensiden. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 385 DIN EN ISO 385 ISO 607 DIN ISO

7、 607 ISO 1042 DIN EN ISO 1042 ISO 2271 DIN ISO 2271 Amendments This standard differs from DIN EN ISO 2871-2:1994-12 as follows: a) Normative references have been updated. b) Structural formulae have been corrected. c) The standard has been editorially revised. Previous editions DIN EN ISO 2871-2: 19

8、94-12 National Annex NA (informative) Bibliography DIN EN ISO 385, Laboratory glassware Burettes DIN EN ISO 1042, Laboratory glassware One-mark volumetric flasks DIN ISO 607, Surface active agents and detergents Methods of sample division DIN ISO 2271, Surface active agents Detergents Determination

9、of anionic-active matter (direct two-phase titration procedure) 2 EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 2871-2 February 2010 ICS 71.100.40 Supersedes EN ISO 2871-2:1994English Version Surface active agents Detergents Determination of cationic-active matter content Part 2: Cationic

10、-active matter of low molecular mass (between 200 and 500) (ISO 2871-2:2010) Agents de surface Dtergents Dtermination de la teneur en matire active cationique Partie 2: Matire active cationique faible masse molculaire (entre 200 et 500) (ISO 2871-2:2010) Tenside Waschmittel Bestimmung des Gehaltes d

11、er kationaktiven Substanz Teil 2: Kationaktive Substanz niedriger Molmasse (zwischen 200 und 500) (ISO 2871-2:2010) This European Standard was approved by CEN on 11 February 2010. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

12、 EuropeanStandard 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 CEN Management Centre or to any CEN member. This European Standard exists in three official versions (E

13、nglish, 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 CEN Management Centre has the same status as theofficial versions. CEN members are the national standards bodies of Austria, Belgium, Bulgar

14、ia, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR ST

15、ANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: Avenue Marnix 17, B-1000 Brussels 2010 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 2871-2:2010: E2DIN EN ISO 2871-2:2010-06 EN I

16、SO 2871-2:2010 (E) Contents Page Foreword .3 1 Scope.4 2 Normative references.4 3 Principle 4 4 Reagents .5 5 Apparatus7 6 Sampling .7 7 Procedure7 7.1 Test portion.7 7.2 Determination .8 8 Expression of results.8 8.1 Calcualtion 8 8.2 Precision .8 9 Test report.9 3Foreword This document (EN ISO 287

17、1-2:2010) has been prepared by Technical Committee ISO/TC 91 Surface active agents in collaboration with 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

18、 an identical text or by endorsement, at the latest by August 2010, and conflicting national standards shall be withdrawn at the latest by August 2010. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not b

19、e held responsible for identifying any or all such patent rights. This document supersedes EN ISO 2871-2:1994. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

20、 Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The

21、text of ISO 2871-2:2010 has been approved by CEN as a EN ISO 2871-2:2010 without any modification. “”DIN EN ISO 2871-2:2010-06 EN ISO 2871-2:2010 (E) 1 Scope This part of ISO 2871 specifies a method for the determination of low-molecular-mass cationic-active materials such as monoamines, amine oxide

22、s, quaternary ammonium compounds and alkylpyridinium salts which have a main chain of 10 to 22 carbon atoms and not more than 6 other carbon atoms in the cation. The method is also suitable for other cationic-active materials. The method is applicable to solids or to aqueous solutions of the active

23、material when the relative molecular mass of the cationic-active matter is known or when it has been previously determined if its content is expressed as a percentage by mass. If more than one type of cationic-active material is present, an estimate of average relative molecular mass may be used. Th

24、e method is not applicable if anionic and/or amphoteric surface active agents are present. 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 editio

25、n of the referenced document (including any amendments) applies. ISO 385, Laboratory glassware Burettes ISO 607, Surface active agents and detergents Methods of sample division ISO 1042, Laboratory glassware One-mark volumetric flasks ISO 2271:1989, Surface active agents Detergents Determination of

26、anionic-active matter by manual or mechanical direct two-phase titration procedure ISO 3696, Water for analytical laboratory use Specification and test methods 3 Principle The cationic-active matter in a sample is titrated in a two-phase (aqueous chloroform) system against a standard anionic surface

27、 active agent in the presence of an indicator consisting of mixed anionic and cationic dyes. The cationic surface active agent present in the sample initially reacts with the anionic dye to form a salt which dissolves in the chloroform layer, imparting a blue colour to this layer. During the titrati

28、on, the anionic surface active agent displaces the anionic dye and, at the end point, forms a salt with the cationic dye, imparting a greyish-pink colour to the chloroform layer. 4DIN EN ISO 2871-2:2010-06 EN ISO 2871-2:2010 (E) 4 Reagents During the analysis, use only reagents of recognized analyti

29、cal grade and only distilled water or water of at least equivalent purity complying with the specifications for grade 3 of ISO 3696. 4.1 Chloroform, 20= 1,48 g/ml, distilling between 59,5 C and 61,5 C. 4.2 Sodium lauryl sulfate (sodium dodecyl sulfate) CH3(CH2)11OSO3Na, standard volumetric solution,

30、 c(C12H25NaO4S) = 0,004 mol/l. While preparing the standard volumetric solution as described in 4.2.2, check the purity of the solid sodium lauryl sulfate used as described in 4.2.1. 4.2.1 Determination of purity of sodium lauryl sulfate. Weigh, to the nearest 1 mg, 5 g 0,2 g of the solid product in

31、to a 250 ml round-bottomed flask with ground-glass neck. Add exactly 25 ml of a standard volumetric sulfuric acid solution, c(H2SO4) = 1 mol/l, and reflux using a water condenser. During the first 5 min to 10 min, the solution will thicken and tend to foam strongly; control this by removing the sour

32、ce of heat and swirling the contents of the flask. In order to avoid excessive foaming, instead of refluxing, the solution may be left on a boiling water bath for 60 min. After a further 10 min, the solution will become clear and foaming will cease. Reflux for a further 90 min. Remove the source of

33、heat, cool the flask and carefully rinse the condenser with 30 ml of ethanol followed by water. Add a few drops of ethanolic phenolphthalein solution (concentration 10 g/l), and titrate the solution with sodium hydroxide solution c(NaOH) = 1 mol/l. Carry out a blank test by titrating 25 ml of the 1

34、mol/l sulfuric acid solution with the 1 mol/l sodium hydroxide solution. Calculate the purity, , expressed as a percentage by mass, of the sodium lauryl sulfate using the formula ()100128,84 VVcmwhere V0is the volume, in millilitres, of the 1 mol/l sodium hydroxide solution used for the blank test;

35、V1is the volume, in millilitres, of the 1 mol/l sodium hydroxide solution used for the test portion of sodium lauryl sulfate taken; c0is the exact concentration, expressed in moles of NaOH per litre, of the sodium hydroxide solution used; m1is the mass, in grams, of the test portion of sodium lauryl

36、 sulfate taken. 4.2.2 Preparation of standard volumetric sodium lauryl sulfate solution. Weigh, to the nearest 1 mg, between 1,14 g and 1,16 g of sodium lauryl sulfate and dissolve in 200 ml of water. Transfer the solution quantitatively to a 1 000 ml one-mark volumetric flask (5.3) fitted with a gr

37、ound-glass stopper, and dilute to the mark with water. 5DIN EN ISO 2871-2:2010-06 EN ISO 2871-2:2010 (E) Calculate the exact concentration c2, expressed in moles of C12H25NaO4S per litre, of the solution thus obtained, using the formula 2288,4 100m where m2is the mass, in grams, of sodium Iauryl sul

38、fate used to prepare the solution; has the same meaning as in 4.2.1. 4.3 Mixed indicator solution1). 4.3.1 Stock solution. This solution shall be prepared from acid blue 1 and dimidium bromide. 4.3.1.1 Acid blue 12)(Colour Index 42045) (Hydrogen 4-4-(diethylamino)-2,4-disulfonatobenzhydrylidenecyclo

39、hexa-2,5-dien-1-ylidenediethylammonium, sodium salt). N + N SS OOOOO O Na +4.3.1.2 Dimidium bromide (3,8-diamino-5-methyl-6-phenylphenanthridinium bromide). N+N H 2 NH2Br 1) This mixed indicator is available commercially in the form of a basic solution, which should be acidified and diluted before u

40、se. 2) Acid blue 1, also known as disulfine blue VN 150, is an example of a suitable product available commercially. This information is given for the convenience of users of this part of ISO 2871 and does not constitute an endorsement by ISO of this product. 6DIN EN ISO 2871-2:2010-06 EN ISO 2871-2

41、:2010 (E) 4.3.1.3 Preparation of the stock solution. Weigh, to the nearest 1 mg, 0,5 g 0,005 g of dimidium bromide (4.3.1.2) into a 50 ml beaker, and 0,25 g 0,005 g of acid blue 1 (4.3.1.1) into a second 50 ml beaker. Add between 20 ml and 30 ml of hot 10 % (volume fraction) ethanol to each beaker.

42、Stir until dissolved and transfer the solutions to a 250 ml one-mark volumetric flask. Rinse the beakers into the volumetric flask with the ethanol and dilute to the mark with the ethanol. 4.3.2 Acid solution. Add 200 ml of water to 20 ml of the stock solution (4.3.1) in a 500 ml one-mark volumetric

43、 flask. Add 20 ml of approximately 245 g/l sulfuric acid solution, mix and dilute to the mark with water. Store in the dark. 5 Apparatus Ordinary laboratory apparatus and the following: 5.1 Flask or measuring cylinder, 250 ml capacity, with ground-glass stopper. 5.2 Burette, 25 ml capacity, complyin

44、g with the specifications for class A of ISO 385. 5.3 One-mark volumetric flask, 1 000 ml capacity, with ground-glass stopper, complying with class A of ISO 1042. 6 Sampling The laboratory sample of the detergent shall be prepared and stored in accordance with instructions given in ISO 607. 7 Proced

45、ure 7.1 Test portion Weigh, to the nearest 0,5 mg, a sufficient amount of the laboratory sample to contain between 0,002 mol and 0,003 mol of cationic-active matter. Table 1, which has been calculated on the basis of a relative molecular mass of 360, may be used as a rough guide. Table 1 Guide to ma

46、ss of test portion Expected cationic-active % (mass fraction) Mass of test portion g 10 10 20 5 100 1 Possible interferences: 7DIN EN ISO 2871-2:2010-06 EN ISO 2871-2:2010 (E) Low relative molecular mass sulfonates of toluene and xylene present as hydrotropes do not interfere when present in concent

47、rations up to and including 15 % (mass fraction) with respect to the active material. At higher levels, their influence should be evaluated in each particular case. Non-ionic surface active agents, soap, urea and the salts of (ethylenedinitrilo)tetraacetic acid do not interfere. Typical inorganic co

48、mponents of detergent formulations, such as sodium chloride, sulfate, borate, tripolyphosphate, perborate, silicate, etc., do not interfere, but bleaching agents other than perborate shall be destroyed before the analysis, and the sample shall be completely soluble in water. 7.2 Determination Dissol

49、ve the test portion (7.1) in water and transfer to the 1 000 ml one-mark volumetric flask (5.3). Dilute to the mark with water and mix well. By means of a pipette, transfer 25 ml of this solution to the 250 ml flask or measuring cylinder (5.1). Using measuring cylinders, add 10 ml of the mixed indicator solution (4.3), 15 ml of chloroform (4.1) and 25 ml of water. Mix well. Fill the burette (5.2) with the sodium lauryl sulfate solution (4.2) and titrate; stopper the flask or me