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    Analyse van fluoride, formiaat en fosfaat met capillaire zone elektroforese

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    Authors
    Hoop MAGT van den
    Staden JJ van
    Type
    Report
    Language
    nl
    
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    Title
    Analyse van fluoride, formiaat en fosfaat met capillaire zone elektroforese
    Translated Title
    Determination of fluoride, formate and phosphate with capillary zone electrophoresis
    Publiekssamenvatting
    Voor een standaardoplossing van 25 mumol l-1 fluoride, formiaat en fosfaat is met capillaire zone-elektroforese systematisch de invloed van verschillende experimentele parameters op het elektroferogram bestudeerd. Onderzocht zijn variaties in: (i) de opgelegde potentiaal, (ii) de bufferconcentratie, (iii) de pH, (iv) de osmotische flow modifierconcentratie, (v) de injectiemethodiek, (vi) matrixinvloeden en (vi) de temperatuur. Op basis van de resultaten is voor fluoride en fosfaat een meetprocedure ontwikkeld, waarvoor lineaire kalibratiecurves werden verkregen over het concentratiegebied van 1 tot 10 mumol l-1 met een aantoonbaarheidsgrens van 0.59 mumol l-1 voor fluoride en 0.45 mumol l-1 voor fosfaat. Een aantal prestatiekenmerken van deze methode is onderzocht. Formiaat is in dit geheel buiten beschouwing gebleven wegens conserveringsproblemen. De meetprocedure is toegepast op een set van 42 regenwaters, die na toevoeging van het decomplexerende reagens Tiron geanalyseerd zijn op het fluoridegehalte. De resultaten komen goed overeen met de resultaten van de ion-selektieve potentiometrie. De CE-methode geeft significant lagere resultaten dan de ionchromato-grafische methode, waarschijnlijk t.g.v. het niet volledig vrijmaken van gecomplexeerd fluoride door Tiron.
    The present report describes the results of a study into the analysis of fluoride, formate and phosphate in solution using capillary zone electrophoresis (CZE). A series of different experimental parameters, such as applied voltage, buffer composition and concentration, pH, and injection method, have been systematically varied in order to establish their influence on peak resolution and detection limits. Experimental results were in good agreement with theoretical predictions. On the basis of these results a CZE methodology was developed for the analysis of fluoride and phosphate in aqueous solutions. Detection limits were found to be 0.59 mumol l-1 fluoride and 0.45 mumol l-1 phosphate using hydrodynamic injection. For the studied concentration range of 1 to 10 mumol l-1, linear calibration curves were obtained. The CZE-method was applied to a set of 42 rainwater samples in order to quantify their fluoride concentration. Tyron was added to the original sample to liberate complexed fluoride. The results are in excellent agreement with the results obtained using an ion-selective electrode potentiometric method. In comparison with an ion chromatographic method, fluoride concentrations obtained by CZE were significantly lower, most likely due to partially decomplexation of fluoride by Tyron.
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    URI
    http://hdl.handle.net/10029/261959
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