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Ultra-trace determination of thallium by electrochemical hydride generation using efficient tungsten electrodes followed by in situ trapping on a graphite tube and detection by electrothermal atomic absorption spectrometry
Journal of Analytical Atomic Spectrometry ( IF 3.4 ) Pub Date : 2017-08-08 00:00:00 , DOI: 10.1039/c7ja00145b
Alireza Shams 1, 2, 3, 4, 5 , Narges Ashraf 1, 2, 3, 4, 5 , Mohammad Hossein Arbab-Zavar 1, 2, 3, 4, 5 , Mahboubeh Masrournia 1, 4, 5, 6, 7
Affiliation  

A novel and extremely efficient cathode material, namely, tungsten-inert gas welding electrode, along with Pd(II) as an enhancement reagent has been introduced for electrochemical hydride generation of thallium (Tl). In situ trapping of the volatile species on a graphite tube along with electrothermal atomic absorption spectrometry was used for preconcentration and detection of Tl in order to provide high sensitivity. The volatile species were transferred to the graphite tube by the flow of argon gas and trapped there for a time period of 170 s. To optimize the performance of the proposed analytical method, effects of several effective experimental parameters, such as the graphite tube modifier, argon gas flow rate, trapping temperature and period, atomization temperature, concentration of the catholyte, and also electrolysis duration were investigated and discussed. Under optimum operating conditions, the calibration curve was plotted which was linear in the concentration range of 28 to 300 ng L−1 of Tl. The limit of detection (LOD) and the limit of quantification (LOQ) of the method were obtained to be 8 ng L−1 and 28 ng L−1, based on 3sb/m and 10sb/m criteria, respectively. The relative standard deviation (RSD%) of the method was found to be 2% for seven replicate measurements at a concentration level of 150 ng L−1 of Tl. The effects of several potential chemical interferents were studied and discussed. The accuracy and the analytical applicability of the proposed method were checked through the analysis of commercial certified reference materials, namely, contaminated unalloyed zinc (ERM®-EB325) and also drinking water containing trace metals (CRM-TMDW). As this method was insensitive towards the oxidation state of Tl, it is suitable for the determination of the total Tl in real analytical samples.

中文翻译:

使用高效钨电极通过电化学氢化物生成,然后石墨管上原位捕集并通过电热原子吸收光谱法进行检测,以超痕量测定determination

已经引入了一种新型且极其有效的阴极材料,即钨极惰性气体保护焊条,以及作为增强试剂的Pd(II),用于electrochemical(Tl)的电化学氢化物生成。原位为了提供高灵敏度,将石墨管上的挥发性物质捕集与电热原子吸收光谱一起用于T1的预浓缩和检测。挥发性物质通过氩气流被转移到石墨管中,并在其中捕获了170 s的时间。为了优化所提出的分析方法的性能,研究并讨论了石墨管改性剂,氩气流速,捕集温度和周期,雾化温度,阴极电解液的浓度以及电解时间等几个有效实验参数的影响。 。在最佳操作条件下,绘制了校准曲线,该校准曲线在28至300 ng L -1的浓度范围内呈线性Tl。根据3 s b / m和10 s b / m的标准,该方法的检测限(LOD)和定量限(LOQ)分别为8 ng L -1和28 ng L -1。。对于浓度为150 ng L -1的七次重复测量,发现该方法的相对标准偏差(RSD%)为2%Tl。研究和讨论了几种潜在的化学干扰物的作用。通过分析经商业认证的参考材料,即污染的非合金锌(ERM®-EB325)和含微量金属的饮用水(CRM-TMDW),检查了所提出方法的准确性和分析适用性。由于该方法对T1的氧化态不敏感,因此适用于测定实际分析样品中的总T1。
更新日期:2017-09-07
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