Tracy M L, Littlefield E S, Moller G
University of California, California Veterinary Diagnostic Laboratory System, Davis 95616.
J Assoc Off Anal Chem. 1991 May-Jun;74(3):516-21.
Total arsenic is determined by inductively coupled plasma atomic emission using hydride vapor generation. A 1 g sample is wet washed in a 16 x 150 mm 10 mL volumetric test tube on a programmed heating block with nitric, sulfuric, and perchloric acids at up to 310 degrees C. After treatment with hydrochloric acid and potassium iodide, arsenic is reduced by sodium borohydride to arsine in a simplified continuous flow manifold. A standard pneumatic nebulizer affects the gas-liquid separation of AsH3, which is quantified by ICP atomic emission at 193.756 nm. The instrument detection limit for the method has been determined to be 0.4 microgram/L. For a 10:1 dilution of a nominal 1 g sample, the detection limit is 4 micrograms/kg and the linear range is up to 4 mg/kg. Recoveries from 3 matrixes were 99-104%, with a typical RSD of 2%. The method has demonstrated statistical control for samples of biological interest and is especially well suited to analysis of small samples.
采用氢化物发生-电感耦合等离子体原子发射光谱法测定总砷。称取1g样品于16×150mm的10mL容量试管中,在程序升温加热块上,加入硝酸、硫酸和高氯酸,在高达310℃的温度下进行湿消解。用盐酸和碘化钾处理后,在简化的连续流动装置中,硼氢化钠将砷还原为砷化氢。标准气动雾化器实现AsH₃的气液分离,通过ICP原子发射光谱法在193.756nm处对其进行定量。该方法的仪器检测限已确定为0.4μg/L。对于标称1g样品10:1的稀释液,检测限为4μg/kg,线性范围高达4mg/kg。三种基质的回收率为99 - 104%,典型相对标准偏差为2%。该方法已证明对生物样品具有统计控制能力,特别适合于小样品的分析。