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优化了微波消解沉积物样品前处理方法,选择了HNO3-HF体系。以沉积物标准物质(GBW07436)为参照对象,选用HNO3-HF微波消解提取重金属全量,采用BCR三步法提取重金属形态,建立了石墨炉原子吸收光谱法(GFAAS)测定As,Cd,Pb,Cr,Cu,Mn,Zn,Ni,Co 9种重金属全量及形态的方法。结果表明,重金属全量测定结果误差为-4.58%~7.33%,BCR形态结果误差为-7.9%~11.6%,符合质控误差范围要求。各重金属形态之和提取率为88.96%~109.36%。对于含多种重金属的沉积物样品,微波消解-GFAAS分析可作为其重金属形态与总量研究的一种分析手段。
The microwave digestion sediment sample pretreatment method was optimized, and the HNO3-HF system was selected. The total amount of heavy metals was extracted by HNO3-HF microwave digestion and the heavy metals were extracted by BCR three-step method. The determination of As, Cd, Pb and Cr by graphite furnace atomic absorption spectrometry (GFAAS) , Cu, Mn, Zn, Ni, Co total amount of heavy metals and morphology of the method. The results showed that the error of total heavy metal determination was -4.58% -7.33%, and the error of BCR morphology was -7.9% ~ 11.6%, which accorded with the requirement of quality control error range. The sum of the heavy metal forms and the extraction rate of 88.96% ~ 109.36%. For sediment samples containing multiple heavy metals, microwave digestion-GFAAS analysis can be used as an analytical tool for the study of their heavy metals morphology and total amount.