Ihnat M
J Assoc Off Anal Chem. 1976 Jul;59(4):911-22.
The performance of hydrogen selenide generation- and carbon furnace atomization-atomic absorption spectrometry, with a semiautomated trace metal accessory and a carbon rod atomizer, respectively, was evaluated for the determination of selenium in foods. Samples were digested with nitric, perchloric, and sulfuric acids for both procedures. Hydrogen selenide was generated with stannous chloride/potassium iodide/zinc from 20 ml aliquots in a hydrochloric-sulfuric acid medium and directed into an argon-hydrogen-entrained air flame. Sample matrix interferences in the carbon furnace technique were minimized by isolating selenium by precipitation with ascorbic acid and redissolution in nitric-perchloric acid prior to taking 5 mul aliquots for estimation; precision was significantly improved by incorporating 5000 mug nickel/ml into analytical solutions. For the hydrogen selenide and carbon furnace techniques, respectively, the following data were obtained for untreated standard solutions: sensitivity, 0.13 and 10.0 ng/ml; absolute sensitivity, 2.6 and 0.05 ng; detection limit, 0.4 and 90 ng/ml; absolute detection limit, 7 and 0.45 ng. The detection limit and absolute detection limit for samples were 2.5 ng/ml and 50 ng, respectively, for the hydrogen selenide method, and 25 ng/ml and 0.13 ng, respectively, for the carbon furnace method. Taking into consideration these figures and the practical aspects of both methods, the overall performance of the hydrogen selenide method was superior.
分别使用半自动化痕量金属附件和碳棒原子化器,对硒化氢发生-碳炉原子化-原子吸收光谱法测定食品中硒的性能进行了评估。两种方法的样品均用硝酸、高氯酸和硫酸进行消化。在盐酸-硫酸介质中,用氯化亚锡/碘化钾/锌从20毫升等分试样中生成硒化氢,并导入氩-氢夹带空气火焰中。通过在抗坏血酸沉淀分离硒并在硝酸-高氯酸中重新溶解后取5微升等分试样进行测定,可将碳炉技术中的样品基体干扰降至最低;通过在分析溶液中加入5000微克/毫升镍,精密度得到显著提高。对于硒化氢法和碳炉法,未处理标准溶液分别获得以下数据:灵敏度,0.13和10.0纳克/毫升;绝对灵敏度,2.6和0.05纳克;检测限,0.4和90纳克/毫升;绝对检测限,7和0.45纳克。硒化氢法测定样品的检测限和绝对检测限分别为2.5纳克/毫升和50纳克,碳炉法分别为25纳克/毫升和0.13纳克。考虑到这些数据以及两种方法的实际情况,硒化氢法的整体性能更优。