石墨管涂覆-塞曼效应石墨炉原子吸收法测定土壤和沉积物中钡

样品使用硝酸-氢氟酸-高氯酸湿法消解,在0.015 mol·L-1硝酸介质中,采用自制涂钨石墨管,塞曼效应背景校正技术石墨炉原子吸收法测定了土壤和沉积物中的钡.经涂钨处理的石墨管表面形成了稳定的碳化钨层,有效避免了在原子化过程中待测元素钡与石墨管直接接触形成难熔碳化物,大幅度提高了检测的灵敏度和精密度,显著延长了石墨管使用寿命.碳化钨为间充型碳化物,在高温下可以产生较强的还原性氛围,可在一定程度上避免土壤和沉积物中常见的高浓度基体成分在原子化阶段生成难熔的氧化物而干扰钡的测定.氢氧化钙分子带背景干扰可以通过稀释法消除.该法测定土壤和沉积物中钡操作简便,快速;检出限为4.2×10-10 g·g-1.环境样品中钡测定的相对标准偏差范围为2.0%～6.5%,测定标准土壤的相对偏差均小于5%.

Determination of Trace Barium in Soil and Sediment by Zeeman Graphite AAS with Coated Graphite Tube

The sample was decomposed by HNO3-HF-HClO4. Using a tungsten-coated graphite tube, trace barium in soil and sediment was determined by Zeeman graphite AAS. To avoid producing carbide, the graphite tube was coated with tungsten. Tungsten and carbon in the surface layer of graphite tube became tungsten carbide. Tungsten carbide prevented barium and carbon from forming barium carbide, which in turn not only led to a long service life for the tube, but also increased greatly the sensitivity and precision of the determination Ba. Tungsten carbide belongs to internal filled type and can give reduction environment. To some extent, the common interfering elements co-existing in the soil and sediment had little chance to form oxides to interfere the determination of Ba in the atomization period. The method was easy and sensitive. The detection limit of Ba was 4.2 x 10(-10) g x g(-1). The relative standard deviation (RSD) was in the range of 2.0%-6.5% (n = 4). The relative deviations from the certificated values of standard soils were under 5%.