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采用动态反应池(Dynamic Reaction Cell,DRC)消除环境样品中碳和氯对铬ICP-MS测定的干扰,实验结果表明O2比CH4能更加有效地消除基体干扰,52Cr更适宜作为铬形态分析的同位素。在优化的DRC条件下2.284μg/L、4.886μg/L和10.579μg/L 3个加标浓度下均具有理想的回收率。进一步采用Pecosphere C8分析柱(3×3),深入研究了流动相组成、pH值及流速对铬形态分离的影响,在1.0 mmol/L四丁基氢氧化铵(TBAH)+0.5 mmol/L乙二胺四乙酸二钠(EDTA)+1%甲醇流动相组成,pH 6.9和流速1.2 mL/min的色谱条件下可以得到最为理想的分离效果,在10～100μg/L标准浓度范围内,Cr(Ⅲ)和Cr(Ⅵ)的线性相关系数均大于0.999 7,建立的方法对Cr(Ⅲ)和Cr(Ⅵ)具有较好的重复性。最后尝试性地对模拟填埋场和地下水环境下市政污泥在脱水、干化和热解过程中铬形态的环境迁移性进行了研究,为更加准确评价铬元素对生态环境的潜在危害提供参考依据。
The dynamic reaction cell (DRC) is used to eliminate the interference of the determination of carbon and chlorine in environmental samples by ICP-MS. The experimental results show that O2 can eliminate matrix interference more effectively than CH4, and 52Cr is more suitable as isotope of chromium speciation . The results showed that the optimal recoveries were obtained at the three spiked concentrations of 2.284μg / L, 4.886μg / L and 10.579μg / L under the optimal conditions of DRC. The effects of mobile phase composition, pH value and flow rate on the separation of chromium species were further studied by using Pecosphere C8 analytical column (3 × 3) The optimum separation conditions were obtained under the conditions of a mobile phase of EDTA + 1% methanol, pH 6.9 and a flow rate of 1.2 mL / min. Under the standard concentration range of 10 ~ 100μg / L, Cr (Ⅲ) And Cr (Ⅵ) were all above 0.999 7. The established method has good repeatability for Cr (Ⅲ) and Cr (Ⅵ). In the end, the environmental migration of chromium form in municipal sludge under landfill and groundwater environment was simulated tentatively to provide a reference for more accurate assessment of the potential hazard of chromium to the ecological environment in accordance with.