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Precision attainable in the determination of silver by flame atomic absorption spectrometry Analysis of thermoelectric silver-doped tellurides

机译:火焰原子吸收光谱法测定银中的精密度热电掺杂银的碲化物分析

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摘要

Effect of the presence of mineral acids and varied matrix composition were investigated to assess the reliability of flame atomic absorption spectrometric determination of Ag in milligram samples of bismuth antimony telluride monocrystals with thermoelectric properties. For optimum conditions, i.e. hydrogen ion concentration of about 1 mol l~(-1) in a mixture of HNO_3, HCl and tartaric acid, a linear calibration between 0.1 and 3 #mu#g ml~(-1) of Ag was obtained. In order to achieve a high precision of absorbance readings, it was necessary to minimize the time delay (about 2 h for 1 mol l~(-1) of H~+) between the preparation of solutions and the measurements. Under such conditions, a long-run reproducibility of the slope values and reliable determinations of 100-900 #mu#g g~(-1) of Ag in 10-25 mg samples were achieved with relative standard deviation of 1-3%. The 3#sigma# detection limit was estimated to be about 0.050 #mu#g ml~(-1). A modified version of the standard additions technique with three steps was applied to confirm the results close to the limit of determination.
机译:考察了存在无机酸和改变基质组成的影响,以评估火焰原子吸收光谱法测定具有热电特性的碲化铋锑碲单晶毫克样品中的银的可靠性。对于最佳条件,即在HNO_3,HCl和酒石酸的混合物中氢离子浓度约为1 mol l〜(-1),可以在0.1和3#mu#g ml〜(-1)之间获得线性校准的Ag 。为了获得高精度的吸光度读数,必须最小化溶液制备和测量之间的时间延迟(对于1 mol l〜(-1)的H〜+,大约需要2个小时)。在这种条件下,可以实现斜率值的长期再现性,并能可靠地测定10-25 mg样品中100-900#mu#g g〜(-1)的Ag,相对标准偏差为1-3%。估计3#sigma#的检出限为约0.050#mu#g ml·(-1)。使用标准添加技术的修改版本(包括三个步骤)来确认结果接近测定极限。

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