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Investigations on extraction procedures for Pt species from spiked road dust samples using HPLC-ICP-MS detection

机译:使用HPLC-ICP-MS检测从加标道路扬尘样品中提取Pt物种的程序

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For the optimisation of the extraction procedures PtCl_4~(2-) and PtCl_6~(2-) were used as model species for extractable Pt(II)-and Pt(IV)-compounds in road dust.A previously developed ion exchange chromatography-ICP-MS method was applied for the quantification of the Pt species in the extracts.A concept in three steps was realised.First,the stability of the model species in several extractants like HC1,methionine,EDTA and thiourea was studied under variation of the concentrations of the extracting agents,the pH and the supply of energy (refluxing,exposure to microwaves,sonication).Second,spiked road dust samples were extracted with those solvents that provided good results in the first step.The results from samples spiked with a mixture of both model species were compared to analogous extractions from dust samples which were spiked with only one of the chloroplatinates.Moreover,the extractant-to-dust-ratio was optimised.Third,the optimised procedures from the second step were applied to unspiked dust samples originating from two different road tunnels in order to characterise the extractable Pt species.The results of the optimisation proved that the model species are fairly stable in the extractants in the absence of the dust matrix.However,the recoveries of PtCl_4~(2-) from the spiked dust samples were significantly lower and PtCl_6~(2-) could not be recovered without transformation at all.The extraction efficiencies for total Pt from the unspiked samples were below 5%.The concentrations of the model species in the extracts of these samples were below the limit of detection of the applied HPLC-ICP-MS method.For quality control mass balances of total Pt were established for all extractions.
机译:为了优化提取程序,将PtCl_4〜(2-)和PtCl_6〜(2-)用作路尘中可提取Pt(II)和Pt(IV)化合物的模型物种。以前开发的离子交换色谱- ICP-MS方法用于提取物中Pt种类的定量分析,实现了三个步骤的概念。首先,研究了在HCl,蛋氨酸,EDTA和硫脲等几种萃取剂中模型种类的稳定性。萃取剂的浓度,pH值和能量的供应(回流,暴露于微波,超声处理)。第二步掺加的道路扬尘样品在第一步中获得了良好的分离效果。将两种模型物种的混合物与仅添加了一种氯铂酸盐的粉尘样品的类似提取物进行了比较。此外,优化了萃取剂与粉尘的比率。第三,应用了第二步的优化程序对来自两个不同道路隧道的未掺粉尘样品进行了表征,以表征可萃取的Pt物种。优化结果证明,在没有粉尘基质的情况下,模型物种在萃取剂中相当稳定。但是,PtCl_4〜加标粉尘样品中的(2-)明显降低,完全不转化就无法回收PtCl_6〜(2-)。未加标样品中总Pt的提取效率低于5%。这些样品的提取物均低于所用HPLC-ICP-MS方法的检测极限。为进行质量控制,所有提取物均建立了总Pt的质量平衡。

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