微波消解-电感耦合等离子体原子发射光谱法测定土壤和水系沉积物中15种组分

建立了微波消解-电感耦合等离子体原子发射光谱法测定土壤、水系沉积物中的As、Co、Cr、Cu、Fe₂O₃、K₂O、Li、Mn、Mo、Na₂O、Ni、Pb、Ti、V、Zn 15种组分的方法。对每种元素的多条测定谱线进行了对比分析,选择强度大、峰形好和干扰小的谱线作为分析线;对经微波处理和蒸发的盐类溶解酸、ICP-AES仪器测定参数(载气流量、观测方向)进行了研究,结果表明,样品采用王水-HF混酸消解后,以5%(V/V)HCl溶解试液经蒸发得到盐类,选择RF功率为1 150 W,载气流量为0.6 L/min,采用轴向观测方式测定,可获得较为满意的结果。各组分的检出限在0.06~49 μg/g范围。方法用于土壤、水系沉积物标准物质的测定,各组分的相对标准偏差小于10%,测定值与认定值的平均对数误差小于0.05,符合《地质矿产实验室测试质量管理规范》要求。

Determination of fifteen components in soil and stream sediment byinductively coupled plasma atomic emission spectrometry after microwave digestion

The determination method of fifteen components (As, Co, Cr, Cu, Fe₂O₃, K₂O, Li, Mn, Mo, Na₂O, Ni, Pb, Ti, V and Zn) in soil and stream sediment by inductively coupled plasma atomic emission spectrometry after microwave digestion was established. Several analysis lines of each element were compared and analyzed. The spectral lines with high intensity, good shape and little interference were selected as the analysis lines. The effect of acid for the dissolution of salts after microwave treatment and evaporation as well as the instrumental operation parameters of ICP-AES (such as carries gas flow and observation method) was studied. The researches indicated that the satisfactory results could be obtained under the following conditions: the sample was dissolved with mixed aqua regia and hydrofluoric acid; after solution evaporation, the salts were dissolved in 5 % (V/V) HCl; the RF power was 1 150 W; the flow rate of carrier gas was 0.6 L/min; the axial observation mode was adopted. The detection limits were between 0.06 μg/g and 49 μg/g. The proposed method was applied to the determination of certified reference materials of soil and stream sediment. The relative standard deviations (RSD) were less than 10%. The mean log errors between found results and certified values were less than 0.05, which could meet the requirements of .