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目的建立地下水中无机砷(iAs3+、iAs5+)的高效液相色谱-氢化物发生-原子荧光(HPLC-HG-AFS)测定法。方法以磷酸氢二铵为流动相,在HamiltonPRP-X100阴离子交换柱上有效分离出水中iAs3+和iAs5+,通过氢化物发生-原子荧光光谱仪测定iAs3+和iAs5+的含量。结果在2～150μg/L线性范围内,iAs3+的线性回归方程为y=159280x-9515.9,r=0.9998,检出限为0.22μg/L;iAs5+的线性回归方程为y=78901x+53737,r=0.9992,检出限为0.75μg/L。该方法所得iAs3+的平均回收率为100.49%～102.05%,RSD为1.59%～3.69%;iAs5+的平均回收率为99.08%～101.06%,RSD为1.83%～4.12%。该方法和氢化物发生-冷阱捕获-原子吸收法(HG-coldtrap-AAS)测定地下水无机砷含量的结果比较,差异无统计学意义(P>0.05)。结论该方法线性范围宽、精密度高、稳定性好,适用于地下水样品中无机砷的测定。
Objective To establish a high performance liquid chromatography-hydride generation-atomic fluorescence spectrometry (HPLC-HG-AFS) method for the determination of inorganic arsenic (iAs3 +, iAs5 +) in groundwater. Methods iAs3 + and iAs5 + were separated from the aqueous solution of Hamilton PRP-X100 anion exchange column using diammonium hydrogen phosphate as mobile phase. The contents of iAs3 + and iAs5 + were determined by hydride generation-atomic fluorescence spectrometry. Results The linear regression equation of iAs3 + was y = 159280x-9515.9, r = 0.9998 with a detection limit of 0.22μg / L in the linear range of 2 ~ 150μg / L. The linear regression equation of iAs5 + was y = 78901x + 53737, 0.9992, the detection limit was 0.75μg / L. The average recoveries of iAs3 + from 100.49% to 102.05% and RSD from 1.59% to 3.69%, respectively. The average recoveries of iAs5 + ranged from 99.08% to 101.06% with RSDs ranging from 1.83% to 4.12%. There was no significant difference between this method and HG-cold trap-AAS in the determination of inorganic arsenic in groundwater (P> 0.05). Conclusion The method has wide linear range, high precision and good stability. It is suitable for the determination of inorganic arsenic in groundwater samples.