Simple Speciation Technique for Arsenic and Antimony in Waste Material Recycling Processes

高效液相-氢化物发生原子荧光光谱分析是生物样品中砷的形态分析方法之一，对分析方法中样品的前处理进行了研究。利用各种标准物质，考察了前处理的最佳条件(特别是萃取剂的选择)。用常规方法测定时，除甜菜碱(ASB)外，其余形态砷的回收率均不高。用磷酸溶液作萃取剂，不仅对ASB，而且对无机砷(As(III)和As(V))、单甲基化砷(MMA)和二甲基化砷(DMA)都有满意的回收率。还尝试了另一种砷形态分析方法--冷冻捕集-氢化物发生原子吸收光谱分析(CV-HGAAS)，其结果与高效液相-氢化物发生原子吸收光谱分析(HGAFS)结果基本一致。到目前为止，关于COM…的研究还很少CT法和高效液相色谱法之间有更多的相似之处。在本研究中，我们阐明了这两种方法的特点，并证明了CT方法在操作简单方面具有优势，而该方法可以提供与HPLC方法相同的结果。为了测定样品中的总砷，尝试了微波辅助酸消解，并建立了测定砷和锑的最佳条件(该结果已提交给《Talanta》杂志，并被接受)。在甲烷发酵污泥中加入二甲基砷酸(DMA)或ASB，在发酵过程中对污泥中砷的形态进行分析。随着发酵的进行，DMA甲基化生成ASB，再转化为三甲基砷，再转移到气相。对于Sb的形态，用CT-HGAAS进行了三甲基形态和无机形态的分离测定。较少

HPLC-hydride generation atomic fluorescence spectrometry (HPLC-HGAFS) is one of the arsenic speciation methods for biological samples, and the pretreatment of samples for the analytical method was studied. By use of various certified reference materials, the optimum conditions for the pretreatment (especially for the selection of extraction solvent) were examined. When the conventional method was used, the recovery of arsenic species except for arsenobetaine (AsB) was not good. The use of phosphoric acid solution as an extraction solvent resulted in the satisfactory recovery for not only AsB but also inorganic arsenicals (As(III) and As(V)), monomethylated arsenicals (MMA), and dimethylated arsenicals (DMA). Cryo trap-hydride generation atomic absorption spectrometry (CV-HGAAS), which is another method of arsenic speciation, was also tried, and it was found that CV-HGAAS gave about the same result that was obtained by HPLC-HGAFS. So far, there have been only a few studies about the com … More parison between the CT method and the HPLC method. In this study, we clarified the characteristics of both methods, and it is proved that the CT method has an advantage in the simplicity of operation, whereas the method can provide the same result that the HPLC method does. For the determination of total arsenic in the samples, microwave-assisted acid digestion was attempted, and the optimum conditions for the determination of arsenic and antimony were established (This result was submitted to a journal, Talanta, and accepted.) When dimethylarsenic acid (as a DMA) or AsB was added in a methane fermentation sludge, and the speciation of arsenic in the sludge was performed during the fermentation process. As the fermentation proceeded, DMA was methylated into AsB, and it was further transformed into trimethylarsine, which was transferred to gas phase. For the speciation of antimony, the fractional determination of trimethyl species and inorganic species was favorably carried out by use of CT-HGAAS. Less