首页> 外文期刊>Journal of the Brazilian Chemical Society >Cadmium and Lead Cloud Point Preconcentration and Determination in Tobacco Samples by Thermospray Flame Furnace Atomic Absorption Spectrometry
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Cadmium and Lead Cloud Point Preconcentration and Determination in Tobacco Samples by Thermospray Flame Furnace Atomic Absorption Spectrometry

机译:热喷雾火焰炉原子吸收光谱法测定烟草样品中镉和铅的浊点浓度

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A thermospray flame furnace atomic absorption spectrometer (TS-FF-AAS) was employed to determine Cd and Pb in different Brazilian tobacco samples. Sample pretreatment consisted of acid decomposition and cloud point (CP) preconcentration optimized by Doehlert design. To promote phase separation in the cloud point procedure, polyoxyethylene(8) isooctylphenyl ether (Triton (R) X-114) and 2-(bromo-2-pyridylazo)-5-diethyl-amino-phenol (Br-PADAP) were used as a nonionic surfactant and a complexing agent, respectively. The variables of the cloud point preconcentration procedure optimized by Doehlert design were: complexing agent volume, Triton X-114 volume, and pH. A response surface maximum point was obtained for Cd and Pb. For TS-FF-AAS, a sample volume of 50 mu L was introduced into the hot Ni tube using air carrier at a flow rate of 0.4 mL min(-1). The limits of detection and relative standard deviations obtained for Cd and Pb when CP and TS-FF-AAS were associated were 4.0 and 13 mu g kg(-1), and 3.1 and 0.7%, respectively. Accuracy was checked by addition-recovery experiments, as well as by using two certified reference materials (tea and peach leaves). Cadmium and lead recoveries ranged from 93 to 103 and 93 to 107%, respectively. All results obtained for reference materials were in agreement with certified values at 95 or 99% confidence levels by t-Student test.
机译:使用热喷雾火焰炉原子吸收光谱仪(TS-FF-AAS)测定巴西不同烟草样品中的Cd和Pb。样品的预处理由酸分解和通过Doehlert设计优化的浊点(CP)预浓缩组成。为了促进浊点法中的相分离,使用了聚氧乙烯(8)异辛基苯基醚(Triton(R)X-114)和2-(溴-2-吡啶基偶氮)-5-二乙基氨基苯酚(Br-PADAP)作为非离子表面活性剂和络合剂。通过Doehlert设计优化的浊点预浓缩程序的变量为:络合剂体积,Triton X-114体积和pH。获得了Cd和Pb的响应面最大值。对于TS-FF-AAS,使用空气载体以0.4 mL min(-1)的流速将50μL的样品体积引入热镍管中。当CP和TS-FF-AAS结合时,镉和铅的检出限和相对标准偏差分别为4.0和13μg kg(-1),分别为3.1和0.7%。通过加样回收实验以及使用两种认证的参考物质(茶和桃叶)检查准确性。镉和铅的回收率分别为93至103和93至107%。通过t-Student测试,所有参考材料的结果均与95%或99%置信水平下的认证值相符。

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