SIST EN 13717:2003

Surface active agents - Determination of primary, secondary and tertiary amino nitrogen - Potentiometric titration

This European Standard specifies the methods for the determination of primary, secondary and tertiary amino nitrogen content in surface active agents by potentiometric titration.

Grenzflächenaktive Stoffe - Bestimmung des Gehalts an Primär-, Sekundär- und Tertiär-Aminstickstoff - Potentiometrische Titration

Diese Europäische Norm legt ein Prüfverfahren zur Bestimmung des Gehalts an Primär-, Sekundär- und Tertiär-Aminstickstoff in grenzflächenaktiven Stoffen durch potentiometrische Titration fest.

Agents de surface - Détermination de la teneur en azote sous forme amine primaire, secondaire et tertiaire - Titrage potentiométrique

La présente Norme européenne spécifie une méthode de détermination par titrage potentiométrique de la teneur en azote sous forme amine primaire, secondaire et tertiaire dans les agents de surface.

Površinsko aktivne snovi - Določevanje primarnega, sekundarnega in terciarnega amino dušika - Potenciometrijska titracija

General Information

• Status: Published
• Publication Date: 31-Jan-2003
• ICS: 71.100.40 - Surface active agents
• Technical Committee: KDS - Cosmetics, chemical disinfectants and surface active agents
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 01-Feb-2003
• Due Date: 01-Feb-2003
• Completion Date: 01-Feb-2003
• Ref Project: EN 13717:2002 - Surface active agents - Determination of primary, secondary and tertiary amino nitrogen - Potentiometric titration

Standards Content (Sample)

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Grenzflächenaktive Stoffe - Bestimmung des Gehalts an Primär-, Sekundär- und Tertiär-Aminstickstoff - Potentiometrische TitrationAgents de surface - Détermination de la teneur en azote sous forme amine primaire, secondaire et tertiaire - Titrage potentiométriqueSurface active agents - Determination of primary, secondary and tertiary amino nitrogen - Potentiometric titration71.100.40Površinsko aktivna sredstvaSurface active agentsICS:Ta slovenski standard je istoveten z:EN 13717:2002SIST EN 13717:2003en01-februar-2003SIST EN 13717:2003SLOVENSKI
STANDARD



SIST EN 13717:2003



EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13717December 2002ICS 71.100.40English versionSurface active agents - Determination of primary, secondary andtertiary amino nitrogen - Potentiometric titrationAgents de surface - Détermination de la teneur en azotesous forme amine primaire, secondaire et tertiaire - TitragepotentiométriqueGrenzflächenaktive Stoffe - Bestimmung des Gehalts anPrimär-, Sekundär- und Tertiär-Aminstickstoff -Potentiometrische TitrationThis European Standard was approved by CEN on 23 October 2002.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-date lists and bibliographical references concerning such nationalstandards 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 translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36
B-1050 Brussels© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 13717:2002 ESIST EN 13717:2003



EN 13717:2002 (E)2ContentspageForeword.31Scope.42Normative reference.43Principle.44Reagents.45Apparatus.56Sampling and preparation of the sample.57Procedure.58Expression of results.69Precision.810Test report.8Annex A (informative)
Instrument settings.9Annex B (informative)
Typical titration curves.10Annex C (informative)
Results of interlaboratory test.11Bibliography.13SIST EN 13717:2003



EN 13717:2002 (E)3ForewordThis document (EN 13717:2002) has been prepared by Technical Committee CEN /TC 276, "Surface activeagents" 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 orby endorsement, at the latest by June 2003, and conflicting national standards shall be withdrawn at the latest byJune 2003.The annexes A, B and C are informative.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries 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.SIST EN 13717:2003



EN 13717:2002 (E)41 ScopeThis European Standard specifies the methods for the determination of primary, secondary and tertiary aminonitrogen content in surface active agents by potentiometric titration.2 Normative referenceThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).ISO 607, Surface active agents and detergents – Methods of sample division3 Principle3.1 The sum of primary and secondary amino nitrogenAfter reaction of the primary and secondary amino nitrogen with carbon disulfide, the resulting dithiocarbamic acidsare titrated with sodium hydroxide standard volumetric solution (see also NOTE in 7.1).3.2 The sum of secondary and tertiary amino nitrogenAfter reaction of the primary amino nitrogen with salicylaldehyde to give a Schiff’s base, the sum of secondary andtertiary amino nitrogen is determined by potentiometric titration with hydrochloric acid standard volumetric solution.3.3 Tertiary amino nitrogenAfter reaction of the primary and secondary amino nitrogen with acetic acid anhydride, the tertiary amino nitrogen isdetermined by titration with standard trifluoromethane sulfonic acid solution.NOTEAlternatively, a reaction with phenylisothiocyanate and a subsequent titration with hydrochloric acid standardvolumetric solution can be carried out.4 ReagentsDuring the analysis, unless otherwise specified, use only reagents of recognized analytical grade and have beenchecked in advance as to not interfere with the analytical results.4.1Sodium hydroxide standard volumetric solution, c (NaOH) = 0,1 mol/l.4.2Carbon disulfide, purity 99,7 % (minimum).WARNINGThis substance is highly flammable and toxic. It causes serious damage to health byprolongated exposure through inhalation and is a possible risk of impaired fertility as well as harm to theunborn child. This substance irritates to eyes and skin.4.32-Propanol, purity 99,5 % (minimum).4.4Hydrochloric acid standard volumetric solution, c (HCl) = 0,1 mol/l, in 2-propanol.SIST EN 13717:2003



EN 13717:2002 (E)54.5Salicylaldehyde, purity 99 % (minimum).4.6Acetic acid anhydride, purity 98,5 % (minimum).4.7Trifluoromethane sulfonic acid standard volumetric solution, c (HSO3CF3) = 0,1 mol/l, in glacial aceticacid.NOTEPerchloric acid, c (HClO4) = 0,1 mol/l, in glacial acetic acid can also be used.4.8Glacial acetic acid, purity 100 %.4.9Phenolphthalein solution, r = 1 g/100 ml, in ethanol, as indicator.4.10Phenylisothiocyanate, purity 98 % (minimum).5 ApparatusOrdinary laboratory apparatus and the following.5.1Potentiometric titrating apparatus, comprising a titrator with a combined pH glass electrode, a 20 ml plungerburette and a stirrer.NOTEAn example of instrument settings is given in Annex A.5.2Beaker, capacity 150 ml.5.3Analytical balance, reading to the nearest 0,1 mg.5.4Magnetic stirrer, with hot plate.5.5Oven.5.6Pressure bottles, encased in plastics, capacity 250 ml, with plastics screw caps and polytetrafluoroethylene(PTFE) seal.5.7Fume cupboard.6 Sampling and preparation of the sampleThe laboratory sample of surface active agent shall be prepared and stored in accordance with ISO 607.7 Procedure7.1 Titration of the primary and secondary amino nitrogenWeigh into the beaker (5.2) a quantity of the sample (m1) to be tested which contains about 0,5 mmol to 1 mmol oftotal base nitrogen to the nearest 0,1 mg. Dissolve the sample in 50 ml of 2-propanol (4.3). Add a few drops ofphenolphthalein solution (4.9). Then add sodium hydroxide standard volumetric solution (4.1) until the colourchanges to faint pink.Add 5 ml of carbon disulfide (4.2) and stir for 1 min at room temperature (work in a fume cupboard).Immerse the electrode,
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