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研究了新型吸附材料铬蓝黑R(钙试剂)负载改性的活性炭对样品中Cr(Ⅲ)和P b(Ⅱ)的固相萃取(SPE)并用电感耦合等离子体-原子发射光谱法(ICP-AES)进行检测。优化了pH值、吸附剂用量、流速等条件以达到定量吸附(≥95%),同时研究了洗脱剂的最佳洗脱条件以及共存离子干扰等问题。本法测定Cr(Ⅲ)和Pb(Ⅱ)的检出限分别为0.91ng·mL-1和0.65ng·mL-1,将其应用于土壤沉积物、猪肝、黄河水中的Cr(Ⅲ)和P b(Ⅱ)含量的测定,加标回收率在98%—101%之间;用于测定标准物质中Cr(Ⅲ)和P b(Ⅱ)的含量,结果与标准物参照值一致。
The solid phase extraction (SPE) of Cr (Ⅲ) and P b (Ⅱ) in Cr (Ⅲ) and P b (Ⅱ) samples with activated carbon loaded with chrome blue black R (calcium reagent) was studied and the results of ICP-AES were studied by inductively coupled plasma atomic emission spectrometry -AES) for testing. The conditions of pH value, adsorbent dosage and flow rate were optimized to achieve the quantitative adsorption (≥95%). The optimum elution conditions of eluents and coexisting ion interference were also studied. The detection limits of Cr (Ⅲ) and Pb (Ⅱ) by this method were 0.91ng · mL-1 and 0.65ng · mL-1, respectively, which were applied to Cr (Ⅲ) And P b (Ⅱ). The recoveries were between 98% and 101%. The contents of Cr (Ⅲ) and P b (Ⅱ) in the reference materials were determined. The results were in good agreement with the standard values.