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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Flow analysis-hydride generation-Fourier transform infrared spectrometry. A new analytical technique for the simultaneous determination of antimony, arsenic and tin
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Flow analysis-hydride generation-Fourier transform infrared spectrometry. A new analytical technique for the simultaneous determination of antimony, arsenic and tin

机译:流动分析-氢化物发生-傅立叶变换红外光谱法。同时测定锑,砷和锡的新分析技术

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The combination of flow analysis (FA), hybride generation (HG) and Fourier transform infrared (FTIR) spectrometry is proposed as a novel and powerful analytical technique for the individual and simultaneous determination of antimony, arsenic and tin in aqueous samples. The analytes were transformed into the volatile hydride form by on-line reaction with sodium tetrahydroborate in acidic medium The gaseous analyte hydrides [M_nH_m(g)] generated, were transported by means of a carrier gas stream inside the IR gas cell and the corresponding FTIR spectrum was acquired in a continuous mode. The 1893, 1904 and 2115 cm~(-1) bands of the SbH_3, SnH_4, and AsH_3 were selected for the determination of antimony, tin and arsenic, respectively. The limit of detection (3#signa#) obtained by using a short-path (10 cm) IR gas cell were 0.25, 0.30 and 1.2 mg l~(-1) for the determination of antimony, tin and arsenic, respectively; while the precision (relative standard deviation, RSD, n = 5) found from a standard solution containing 50 mg l~(-) of each element was, in all cases, less than 0.3%. However, the use of a long-path (7.25 m) IR gas cell improved the figures of merirt (sensitivity, limits of detection and quantification) nearly 60-fold. The effect of the main experimental and instrumental variables, such as acidic media, sodium tetraborohydrate concentration, nitrogen flow rate, nominal resolution and the scan accumulation on the analytical signals of the antimony, tin and arsenic hydrides, were studied. Further, the potential of the proposed technique for the simultaneous determination of these elements was tested, analyzing synthetic samples containing different amounts of Sb, Sn and As.
机译:流动分析(FA),杂种生成(HG)和傅立叶变换红外光谱(FTIR)光谱的结合被提出作为一种新颖而强大的分析技术,可用于同时测定水性样品中的锑,砷和锡。通过与四氢硼酸钠在酸性介质中在线反应,将分析物转化为挥发性氢化物形式。生成的气态分析物氢化物[M_nH_m(g)]通过载气气流在IR气室和相应的FTIR中传输连续采集光谱。选择了SbH_3,SnH_4和AsH_3的1893、1904和2115 cm〜(-1)谱带分别测定锑,锡和砷。使用短路径(10厘米)红外气室获得的锑,锡和砷的检测极限分别为0.25、0.30和1.2 mg l〜(-1)(3#signa#);而在每种情况下,从每个元素含50 mg l〜(-)的标准溶液中测得的精度(相对标准偏差,RSD,n = 5)均小于0.3%。但是,使用长距离(7.25 m)红外气室可将测量值(灵敏度,检测和定量限)提高近60倍。研究了主要的实验和仪器变量,如酸性介质,四硼酸钠的浓度,氮气流速,标称分辨率和扫描累积量对锑,锡和氢化砷的分析信号的影响。此外,通过分析包含不同量的Sb,Sn和As的合成样品,测试了同时测定这些元素的提议技术的潜力。

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