SIST EN 13405:2003
(Main)Surface active agents - Determination of dialkyl-tetralins content in linear alkylbenzene by high performance liquid chromatography (HPLC)
Surface active agents - Determination of dialkyl-tetralins content in linear alkylbenzene by high performance liquid chromatography (HPLC)
This European Standard specifies a method for the determination of dialkyl-tetralins (DAT), being 1,4-dialkyl-2,3-dihydro-naphthalene in linear alkylbenzene (LAB) in the range of the mass fraction of 0,5 % to 10 %.
Grenzflächenaktive Stoffe - Bestimmung des Gehaltes von Dialkyltetralin in linearem Alkylbenzol mittels Hochleistungs-Flüssigchromatographie (HPLC)
Diese Norm legt ein Verfahren zur Bestimmung von DAT (Dialkyltetralin/1,4-Dialkyl-2,3-dihydronaphthalin) in linearem Alkylbenzol (LAB) im Bereich von 0,5% bis 10% Massenanteile fest.
Agents de surface - Détermination de la teneur en dialkyltétralines dans les alkylbenzenes linéaires par chromatographie liquide a haute performance (CLHP)
La présente Norme européenne spécifie une méthode de détermination de la teneur en dialkyltétralines (DAT) (1,4 dialkyl 2,3 dihydronaphtalene) des alkylbenzenes linéaires (LAB), pour des concentrations en fraction massique comprises entre 0,5 % et 10 %.
Površinsko aktivne snovi - Določevanje dialkil-tetralinov v linearnem alkilbenzenu s tekočinsko kromatografijo visoke ločljivosti (HPLC)
General Information
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Grenzflächenaktive Stoffe - Bestimmung des Gehaltes von Dialkyltetralin in linearem Alkylbenzol mittels Hochleistungs-Flüssigchromatographie (HPLC)Agents de surface - Détermination de la teneur en dialkyltétralines dans les alkylbenzenes linéaires par chromatographie liquide a haute performance (CLHP)Surface active agents - Determination of dialkyl-tetralins content in linear alkylbenzene by high performance liquid chromatography (HPLC)71.100.40Površinsko aktivna sredstvaSurface active agentsICS:Ta slovenski standard je istoveten z:EN 13405:2002SIST EN 13405:2003en01-februar-2003SIST EN 13405:2003SLOVENSKI
STANDARD
SIST EN 13405:2003
EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 13405December 2002ICS 71.100.40English versionSurface active agents - Determination of dialkyl-tetralins contentin linear alkylbenzene by high performance liquidchromatography (HPLC)Agents de surface - Détermination de la teneur endialkyltétralines dans les alkylbenzènes linéaires parchromatographie liquide à haute performance (CLHP)Grenzflächenaktive Stoffe - Bestimmung des Gehaltes vonDialkyltetralin in linearem Alkylbenzol mittelsHochleistungs-Flüssigchromatographie (HPLC)This 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 13405:2002 ESIST EN 13405:2003
EN 13405:2002 (E)2ContentspageForeword.31Scope.42Normative reference.43Principle.44Reagents.45Apparatus.46Procedure.56.1Preliminary test.56.2Calibration.56.3Determination.67Calculation.88Precision.88.1General.88.2Repeatibility limit.88.3Reproducibility limit.89Test report.9Annex A (informative)
Method of determination of the carbon number distribution of the LAB sample(UOP
Method 673-88).11A.1General.11A.2Principle.11A.3Reagents.11A.4Apparatus.11A.5Procedure.12A.5.1Chromatographic conditions.12A.5.2Determination.13A.5.3Time for analysis.14A.6Calculations.15A.7Precision.15A.7.1Repeatability.15A.7.2Reproducibility.16Bibliography.17SIST EN 13405:2003
EN 13405:2002 (E)3ForewordThis document (EN 13405:2002) 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.Annex A is 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 13405:2003
EN 13405:2002 (E)41 ScopeThis European Standard specifies a method for the determination of dialkyl-tetralins (DAT), being1,4-dialkyl-2,3-dihydro-naphthalene in linear alkylbenzene (LAB) in the range of the mass fraction of 0,5 % to 10 %.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).EN ISO 3696:1995, Water for analytical laboratory use - Specification and test methods (ISO 3696:1987).3 PrincipleThe sample is analysed by isocratic high performance liquid chromatography (HPLC) using a micro-particulatesilica stationary phase, 2,2,4-methylpentane mobile phase and ultra-violet absorbance detection at 254 nm.Quantification is made by using a "modified" external standard technique. Pure standard dialkyl-tetralins (DAT) arenot available, therefore the molar response of DAT is assumed to be the same as the commercially availabletetrahydronaphthalene (THN) used as external standard.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.4.1Water, complying with grade 3 as defined in EN ISO 3696:1995.4.22,2,4-trimethylpentane (iso-octane), C8H18, HPLC grade, with a water content less than 100 mg/kg.NOTECare should be taken when using iso-octane, which is highly flammable.4.3Tetrahydronaphthalene (THN), C10H12, minimum purity 96 % (determination by gas chromatography areastandard technique).NOTECare should be taken when using tetrahydronaphthalene which can be irritating to eyes and skin.4.4Hexane, C6H14.4.5Toluene, C7H8.5 ApparatusOrdinary laboratory apparatus and glassware together with the following.5.1High performance liquid chromatograph, suitable for analysis according to the operating instructionsgiven in Table 1.SIST EN 13405:2003
EN 13405:2002 (E)55.2Chromatographic column, normal phase, 250 mm length, 4 mm internal diameter containingmicro-particulate silica.5.3Suitable means, for determining peak area, e.g. integrator or computer.5.4Disposable filter, 0,5 mm pore diameter.6 Procedure6.1 Preliminary testThe column length (1 column or 2 columns in series) and the flow rate shall be arranged in order to optimise theefficiency and resolution (see Table 2 for column details). One way to test this is to run an HPLC chromatogramusing a standard solution containing approximately 100 mg of toluene (4.5) and 10 mg of tetrahydronaphthalene(4.3) (THN) in 100 ml of hexane (4.4). An example of a chromatogram is given in Figure 1.Do not wash the columns with any polar solvent otherwise the original separation factor is not to be restored anymore.From this chromatogram determine the net retention time (t') and the capacity factor (k') of both THN and tolueneand calculate the relative separation factor (a).NOTETypical values for two Lichrosorb Si 60 columns and 1 ml/min flow rate are shown in Table 1.Table 1 - Net retention time and capacity factor for toluene and THN for two Lichrosorb Si60 columns and a flow rate of 1 ml/minReagentNet retention time (min)Capacity factorottt-='ottotk-='Toluene4,80,94THN6,31,24NOTEto is the duration of elution at the dead volume. A typical value of to for n-hexane is5,1 min.The calculated separation factor, ''12kk=a, is:321,''==ToluèneTHNkkaA reproducible and correct DAT analysis in LAB samples requires that the HPLC conditions are set up so that a isgreater than or equal to 1,20.6.2 CalibrationPrepare a solution of 0,1 g/l of THN in 2,2,4-trimethylpentane (4.2) by weighing 100 mg of thetetrahydronaphthalene (4.3) to the nearest 0,1 mg and making up to volume in an 1 l volumetric flask or by dilutionof a more con
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