ジアルキルジチオリン酸のガスクロマトグラフ法による定量
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概要
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A method was proposed for the gas chromatographic determination of <I>O</I>, <I>O</I>-dimethyl, <I>O</I>, <I>O</I>-diethyl, <I>O</I>, <I>O</I>-diisopropyl-dithiophosphoric acids, which were esterified with trialkylphosphite in nitrogen atmosphere before injection into a gas chromatograph equipped with a thermal conductivity detector.<BR>Dialkyl-dithiophosphoric acids are easily esterified by adding trialkylphosphites, but this reaction must be done in nitrogenous atmosphere to prevent it from the influence of oxygen.<BR>Triethylphosphite is used for esterification of dimethyl dithiophosphoric acid and trimethylphosphite for esterification of diethyl- and diisopropyl dithiophos-phoric acids.<BR>Chromatographic analysis was performed on a 2m×0.3mm stainless steel column containing 80100mesh Celite 545 coated with 20% silicone DC550.<BR>Gaschromatographic conditions in this experiment are as follows.<BR>Dimethyl dithiophosphoric acid : column temperature, 190°C; carrier gas, helium 17m<I>l</I>/min; and internal standard, diethyl adipate. <BR>Diethyl- and diisopropyl dithiophosphoric acid :column temperature, 200°C; carrier gas, helium 18.1m<I>l</I>/min; and internal standard, isoamyl benzoate.
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