Bozsai G, Schlemmer G, Grobenski Z
National Institute of Hygiene, H-1966 Budapest, Hungary.
Talanta. 1990 Jun;37(6):545-53. doi: 10.1016/0039-9140(90)80195-l.
A graphite-furnace AAS method using the stabilized-temperature platform furnace (STPF) concept, mixed palladium and magnesium nitrates as chemical modifier and Zeeman background correction has been applied to the direct determination of As, Cd, Pb and Se in highly mineralized waters used for medicinal purposes. These contain 20-40 g/l. concentrations of salts, mainly sodium and magnesium chlorides, bicarbonates and sulphates. The use of a pre-atomization cool-down step to 20 degrees in the graphite-furnace programme reduced the background absorption. Increasing the mass of magnesium nitrate modifier to 5 times that originally proposed improved the analyte peak shape. Under these conditions, no interference was found in analysis of the chloride/bicarbonate type of water, but the sodium and magnesium sulphate type of water had to be diluted, and even then an interference remained. Calibration with matrix-free standard solutions was used, but use of spike recovery is strongly recommended for testing the accuracy. The limits of determination (4.65sigma) of the proposed method for undiluted samples are 2.0 mug/l. for As, 0.05 mug/l. for Cd, 1.0 mug/l. for Pb and 1.5 mug/l. for Se.
一种采用稳定温度平台炉(STPF)概念、以混合钯和硝酸镁作为化学改进剂并结合塞曼背景校正的石墨炉原子吸收光谱法,已被应用于直接测定药用高矿化水中的砷、镉、铅和硒。这些水中盐浓度为20 - 40 g/l,主要为氯化钠、氯化镁、碳酸氢盐和硫酸盐。在石墨炉程序中采用预原子化冷却至20摄氏度的步骤降低了背景吸收。将硝酸镁改进剂的用量增加至原建议用量的5倍改善了分析物的峰形。在此条件下,分析氯化物/碳酸氢盐类型的水时未发现干扰,但硫酸钠和硫酸镁类型的水必须稀释,即便如此仍存在干扰。采用无基体标准溶液进行校准,但强烈建议使用加标回收率来检验准确性。该方法对未稀释样品的测定限(4.65σ)为:砷2.0 μg/l、镉0.05 μg/l、铅1.0 μg/l、硒1.5 μg/l。