1、 g49g50g3g38g50g51g60g44g49g42g3g58g44g55g43g50g56g55g3g37g54g44g3g51g40g53g48g44g54g54g44g50g49g3g40g59g38g40g51g55g3g36g54g3g51g40g53g48g44g55g55g40g39g3g37g60g3g38g50g51g60g53g44g42g43g55g3g47g36g58alkylamidopropylbetainesThe European Standard EN 15109:2006 has the status of a British StandardICS
2、 71.100.40Surface active agents Determination of the active matter content of BRITISH STANDARDBS EN 15109:2006BS EN 15109:2006This British Standard was published under the authority of the Standards Policy and Strategy Committee on 29 December 2006 BSI 2006ISBN 0 580 49886 7Amendments issued since p
3、ublicationAmd. No. Date Commentscontract. Users are responsible for its correct application.Compliance with a British Standard cannot confer immunity from legal obligations.National forewordThis British Standard was published by BSI. It is the UK implementation of EN 15109:2006.The UK participation
4、in its preparation was entrusted to Technical Committee CII/34, Methods of test for surface active agents.A list of organizations represented on CII/34 can be obtained on request to its secretary.This publication does not purport to include all the necessary provisions of a EUROPEAN STANDARDNORME EU
5、ROPENNEEUROPISCHE NORMEN 15109November 2006ICS 71.100.40English VersionSurface active agents - Determination of the active mattercontent of alkylamidopropylbetainesAgents de surface - Dtermination de la teneur en matiresactives des alkylamidopropylbtanesGrenzflchenaktive Stoffe - Bestimmung des Akti
6、vgehaltesvon AlkylamidopropylbetainenThis European Standard was approved by CEN on 6 October 2006.CEN members are bound 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-
7、date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Central 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
8、responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,Germany, Greece, Hungary, Iceland, Ire
9、land, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania,Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMIT EUROPEN DE NORMALISATIONEUROPISCHES KOMITEE FR NORMUNGManagement Centre: rue de Stassart, 36
10、 B-1050 Brussels 2006 CEN All rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 15109:2006: EEN 15109:2006 (E) 2 Contents Page Foreword3 1 Scope 4 2 Normative references 4 3 Principle4 4 Reagents.4 5 Apparatus .5 6 Sampling and preparation of
11、the test sample.6 7 Procedure .6 8 Calculation and expression of results.7 9 Precision.8 9.1 Repeatability limit 8 9.2 Reproducibility limit 8 10 Test report 8 Annex A (informative) Titration parameters .9 Annex B (informative) Statistical and other data derived from the results of inter-laboratory
12、tests .10 Annex C (informative) EN 13270 and EN 15109 active matter comparative analysis.11 C.1 General11 C.2 Analysis of alkylamidopropylbetaines 11 C.3 Analysis of alkyldimethylbetaines .12 Bibliography 13 EN 15109:2006 (E) 3 Foreword This document (EN 15109:2006) has been prepared by Technical Co
13、mmittee 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 May 2007, and conflicting national standards shall be withdra
14、wn at the latest by May 2007. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Icela
15、nd, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EN 15109:2006 (E) 4 1 Scope This European Standard specifies a method for the determination of the active matter content of alk
16、ylamidobetaines in commercial surface active agents. 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 edition of the referenced document (includin
17、g any amendments) applies. EN ISO 3696, Water for analytical laboratory use Specification and test methods (ISO 3696:1987) ISO 607, Surface active agents and detergents Methods of sample division 3 Principle The test sample to be analysed is alkalinized by addition of sodium hydroxide. In this way a
18、ll substances present are converted into a defined form, namely: the betaine into its intermolecular salt form; the amidoamine into the free amidoamine; the acids (e.g. hydrochloric acid, fatty acids, chloroacetic acids and glycolic acid) into their sodium salt forms. During the titration with perch
19、loric acid in the non-aqueous medium: the betaine is changed into the protonated form; the amidoamine is changed into the amidoamine perchlorate; the excess sodium hydroxide and sodium salts of the different acids are transformed into weakly dissociated sodium perchlorate. By using a solvent mixture
20、 which enables a good differentiation of varying pK(b) values, it is possible to differenciate the betaine from these accompanying substances. Salts of chloroacetic acids, glycolic acid, fatty acid and amidoamine do not interfere. Short chain betaines are titrated together with long chain betaines.
21、4 Reagents 4.1 General WARNING Your attention is drawn to the regulations covering the handling of hazardous substances. Technical, organisational and personal protection measures should be observed. During the analysis, unless otherwise specified, use only reagents of recognized analytical grade an
22、d have been checked in advance as to not interfere with the analytical results and water complying with grade 1 as defined in EN ISO 3696. 4.2 1,4-dioxane, minimum purity 99 % (CAS number: 123-91-1). EN 15109:2006 (E) 5 WARNING This substance can cause irreversible effects and eye irritation. 4.3 Me
23、thoxyethanol, minimum purity 99 % (CAS number : 32718-54-0). WARNING This substance is considered as mutagenic. 4.4 Methanol, minimum purity 99,5 % (CAS number : 67-56-1). WARNING This substance is considered toxic by ingestion or inhalation. 4.5 Sodium hydroxide, c(NaOH) = 1,0 mol/l (CAS number : 1
24、310-73-2). 4.6 Sodium acetate, minimum purity 99 % (CAS number : 127-09-3). 4.7 Sodium hydroxide/sodium acetate solution Dissolve 80 g of sodium acetate in aqueous sodium hydroxide (c(NaOH) = 1,0 mol/l) into a 1 l volumetric flask. Make up to the volume with the same sodium hydroxide solution. Stopp
25、er and mix. 4.8 Potassium hydrogen phthalate, purity (100 0,1) %, (CAS number : 877-24-7). 4.9 Acetic acid, minimum purity 99,8 % (CAS number : 64-19-7). 4.10 Perchloric acid standard volumetric solution, c(HClO4) = 0,1 mol/l (CAS number: 7601-90-3), in 1,4-dioxane. Fill approximately 500 ml of diox
26、ane in a 1 000 ml volumetric flask. Add the capacity of an ampoule for the preparation of 0,1 mol/l perchloric acid standard volumetric solution. Make up to the volume with 1,4-dioxane. For the determination of the concentration of the perchloric acid standard volumetric solution, weigh about 0,18 g
27、 of dried potassium hydrogen phthalate to the nearest 0,1 mg into the titration beaker and dissolve in about 100 ml of acetic acid. Switch the stirrer on, immerse the electrodes and titrate with the perchloric acid standard volumetric solution beyond the potential jump. Calculate the concentration,
28、fc, of the perchloric acid standard volumetric solution, in moles per litre, using the Equation (1): V Mm= fc10000(1) where m0is the mass of potassium hydrogen phthalate, in grams; M is the molar mass of potassium hydrogen phthalate (M = 204,23 g/mol); V is the volume, in millilitres, of perchloric
29、acid standard volumetric solution consumed to the inflection point. 5 Apparatus Ordinary apparatus and the following. 5.1 Automatic potentiometric titration apparatus, with drift-controlled data acquisition and dynamic titrimetric dosing equipped with a piston burette delivery system of 20 ml capaci
30、ty. EN 15109:2006 (E) 6 5.2 pH glass electrode 5.3 Reference electrode Ag/AgCl The instrument parameters shall be adjusted as to produce a curve similar to that shown in Figure 1. 6 Sampling and preparation of the test sample The test sample shall be prepared and stored in accordance with ISO 607. 7
31、 Procedure WARNING Perform all titrations specified in a well ventilated hood. Weigh 1,3 g of the test sample to the nearest 0,1 mg into the beaker. Add 20 ml of methanol and dissolve. Add 0,5 ml of sodium hydroxide/sodium acetate solution measured with a graduated 1 ml pipette and allow to stand fo
32、r 5 min at room temperature to react. Add further 20 ml of methanol and 80 ml of methoxyethanol, both measured with a 100 ml graduated cylinder. Switch the stirrer on, immerse the electrodes and titrate with the perchloric acid standard volumetric solution beyond the third potential jump. A typical
33、titration curve is shown in Figure 1. NOTE 1 Bad shaped curves can occasionally be obtained because of the following reasons: a) static electricity problems (to prevent these problems, special electronic arrangements (e.g. differential potentiometry) should be used); b) clogging of the electrode dia
34、phragm (remedy by scratching with a needle); c) overaged perchloric acid standard volumetric solution (remedy by preparing a fresh solution). NOTE 2 Typical curves start in the negative potential zone (between -100 mV and -400 mV) and show three distinct potential jumps (see Figure 1). The first jum
35、p corresponds to the protonation of excess alkali. The second jump corresponds to the protonation of 1-hydroxy acetate, chloroacetates, fatty acid salts and free amine (i.e. amidoamine). It occurs at positive potential zone. The third jump corresponds to the protonation of betaines. Short chain beta
36、ines are also titrated at this point. EN 15109:2006 (E) 7 Key 1 first inflection point 2 second inflection point 3 third inflection point 4 voltage, in millivolts 5 volume consumed of perchloric acid standard volumetric solution, in millilitres Figure 1 Typical titration curve (A) and its first deri
37、vative (B) 8 Calculation and expression of results The content of betaine, wB, expressed as grams per 100 g, is calculated by the Equation (2): 10c23Bm f M ) V- V(= w(2) where V3is the volume consumed of the perchloric acid standard volumetric solution until the third inflection point, in millilitre
38、s; V2is the volume consumed of the perchloric acid standard volumetric solution until the second inflection point, in millilitres; M is the molar mass of the betaine in grams per mole; EN 15109:2006 (E) 8 fcis the exact concentration of the perchloric acid standard volumetric solution, in moles per
39、litre; m is the mass of the test sample, in grams. The content of betaine, wBshall be given to one decimal place. 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 laboratory
40、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 Tables B.1 and B.2. 9.2 Reproducibility limit The absolute difference between two independ
41、ent 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 in Tables B
42、.1 and B.2. 10 Test report The test report shall include the following information: a) all information necessary for the identification of the sample tested; b) a reference to this European Standard, i.e. EN 15109; c) the test results; d) details of any operation not specified in this European Stand
43、ard or in the European Standards to which reference is made, and any operations regarded as optional, as well as any incidents like to have affected the results. EN 15109:2006 (E) 9 Annex A (informative) Titration parameters The following parameters are settings for the Metrohm 716 DMS Titrino Titro
44、processor 1)and are intended to act as a guideline only (see Table A.1): Table A.1 Instrument settings Parameter Set point Measuring point density 3 Minimum increment 10 l Titration rate maximum Signal, drift 10 mV/min Equilibration time 52 s Start volt off Pause 0 Measuring input 1 NOTE The designa
45、tions of the parameters correspond to those given by the Metrohm 716 DMS Titrino Titroprocessor. 1) Metrohm 716 DMS Titrino Titroprocessor is an example of suitable apparatus commercially available. This information is given for the convenience of users of this European Standard and does not constit
46、ute an endorsement by CEN of the instruments named. EN 15109:2006 (E) 10 Annex B (informative) Statistical and other data derived from the results of inter-laboratory tests The data for the repeatability and reproducibility limits of this method are the results of inter laboratory tests carried out
47、by GAT (Common Committee for Analysis of Surfactants) in 1996 and CESIO (Comit Europen des agents de Surface et de leurs Intermdiaires Organiques)/AISE (International Association for Soaps, Detergents and Maintenance Products) in 1997. The evaluation of the laboratory test was performed in accordanc
48、e with ISO 5725-2. The alkylamidobetaine (Sample A) was analysed comparatively with samples B, C, and D that were obtained from sample A after addition of fatty acid amidoamine, glycolic acid and respectively fatty acid. Table B.1 GAT interlaboratory test of samples of commercial alkylamidopropylbet
49、aines Designation Sample A Sample B Sample C Sample DNumber of participating laboratories 8 8 8 8 Number of accepted test results 23 23 23 23 Mean value (wB) (g/100 g) 27,65 27,54 27,42 27,43 Repeatability standard deviation (sr) 0,11 0,16 0,14 0,13 Repeatability coefficient of variation 0,4% 0,6% 0,5% 0,5% Repeatability limit, (r) (2,8 sr) 0,32 0,45 0,39 0,36 Standard deviation of reproducibility (sR) 0,17 0,25 0,28 0,31 Reproducibility coefficient of variation 0,6% 0,9% 1,0% 1,1% Reproducibili
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