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Determination of Aromatic Arsines in Environmental Solids by Direct Thermal Desorption Gas Chromatography

机译:直接热解吸气相色谱法测定环境固体中的芳香族胂

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To quantify aromatic arsines in the environment, such as World War I era chemical warfare agents and degradation products of arsenicals used in agriculture, a sensitive, selective, and direct method is needed. We describe the development and optimization of a method for the measurement of trace levels of triphenylarsine used as a model aromatic arsenic compound. Triphenylarsine was determined at low mu g/g levels in sand, soil, and lake sediment by thermal desorption before gas-liquid chromatography (GC) with mass spectrometric and pulsed flame photometric detection. The dithiol derivative of phenylarsonic acid was used as an internal standard, thereby significantly improving the precision of the method. The desorption conditions were studied and found to be optimal at 350 degrees C for 15min. Significant improvement in precision was realized by preparing the solid samples as slurries in acetone and by inserting a small (approximate to 100mg) quartz wool plug into the sample vial. The method was applied to determine triphenylarsine in authentic soil and sediment samples that had been fortified with triphenylarsine and aged for at least 15 days. Recoveries for soil samples ranged from 84.3 +/- 2.3 to 87.7 +/- 1.3%, while lower recoveries were obtained for sediment samples (75.1 +/- 3.0%). The detection limit for triphenylarsine in soil was 3.14ng with a precision of 7.10% (n=4). Using these optimized conditions, the performance of the direct thermal desorption GC method for sample introduction was greatly improved compared to methods that have been reported in the literature.
机译:为了量化环境中的芳香毒液,如第二次世界大战的ERA化学战和农业中使用的砷的降解产物,需要一种敏感,选择性和直接方法。我们描述了用作型芳族砷化合物的痕量三苯甲串测定痕量水平的方法的开发和优化。通过在气液色谱(GC)之前的热解吸以质量光谱和脉冲火焰光度检测,在砂,土壤和湖泊沉积物中以低mm g / g水平测定三苯基arsine。苯胂酸的二硫醇衍生物用作内标,从而显着提高了该方法的精度。研究了解吸条件,发现在350℃下最佳15分钟。通过将固体样品作为丙酮中的浆料制备固体样品并通过将小(近似100mg)石英羊毛插入样品瓶中的小(近似约100mg)石英羊毛塞来实现显着改善。该方法用于确定正宗土壤和沉积物样品中的三苯基arsine,该样品被三烯基arsine强化,衰减至少15天。土壤样品的回收率范围为84.3 +/- 2.3至87.7 +/- 1.3%,而沉积物样品获得较低的回收率(75.1 +/- 3.0%)。土壤中三苯基胂的检测限为3.14,精度为7.10%(n = 4)。使用这些优化的条件,与文献中报道的方法相比,对样品引入的直接热解吸GC方法的性能大大提高。

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