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首页> 外文期刊>Spectrochimica Acta, Part B. Atomic Spectroscopy >Development of an on-line procedure for the indirect determination of iodide by flow-injection cold-vapor atomic absorption spectrometry
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Development of an on-line procedure for the indirect determination of iodide by flow-injection cold-vapor atomic absorption spectrometry

机译：流动注射冷蒸气原子吸收光谱法间接测定碘化物的在线方法的开发

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A commercially available mercury-analyzer based on flow-injection cold-vapor atomic absorption spectrometry (FI-CVAAS) was modified so as enable an indirect determination of iodide. The technique makes use of the interference caused by iodide in the determination of Hg by FI-CVAAS and allows it to obtain a calibration curve with a negative slope. An on-line technique was realized by providing an additional loop for a Hg solution introduced in the FI-CV system. The loop was provided by installing a further magnetic valve and by using the fourth channel of the peristaltic pump. Software methods for filling and operating the system were developed. The concentrations of the reducing agent SnCl_2 and of the HNO_3 were optimized with regard to the analytical figures of merit. A linear calibration curve (R~2=0.9959) for 13 solutions with differnet concentrations of iodide between 0 and 60 ng/ml and a detection limit of 3.6 ng/ml were obtained. the analytical precision in terms of the R.S.D. is at the 1% level. The method developed could be successfully applied to the determination of iodide in a brine sample at the 2-ng/ml level. Efforts to improve the power of detection by using preconcentration by gold amalgamation at the optimum concentration of Hg wer ehampered by the higher standard deviations for the blank values which could not be compensated by the increase in sensitivity. This resulted in a detection limit of 9.6 ng/ml. The procedure with preconcentrastion was found to lead to the same results as the procedure without preconcentrtion for the same analysis brine sample.
机译：修改了基于流动注射冷蒸气原子吸收光谱法（FI-CVAAS）的市售汞分析仪，以便能够间接测定碘。该技术在FI-CVAAS测定Hg中利用了碘化物引起的干扰，并获得了具有负斜率的校准曲线。通过为FI-CV系统中引入的Hg解决方案提供额外的回路来实现在线技术。通过安装另一个电磁阀并使用蠕动泵的第四通道来提供回路。开发了用于填充和操作系统的软件方法。相对于品质因数优化了还原剂SnCl_2和HNO_3的浓度。获得了13种溶液的线性校准曲线（R〜2 = 0.9959），其中碘化物的净浓度在0至60 ng / ml之间，检出限为3.6 ng / ml。相对于R.S.D.的分析精度处于1％的水平。所开发的方法可以成功地用于2-ng / ml浓度的盐水样品中碘的测定。通过在最佳汞浓度下使用金汞齐预富集来提高检测能力的努力，空白浓度的较高标准偏差阻碍了灵敏度的提高，而汞的最佳标准偏差阻碍了汞的最佳标准偏差。结果检测限为9.6 ng / ml。发现对于相同的分析盐水样品，采用预浓缩的方法可得到与不进行预浓缩的方法相同的结果。

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