液相色谱-原子荧光联用测定作业场所空气中的无机砷

匡必玲; 唐磊; 王林

doi:10.16369/j.oher.issn.1007-1326.2021.01.020

液相色谱-原子荧光联用测定作业场所空气中的无机砷

Determination of airborne inorganic arsenic in workplaces by liquid chromatographyatomic fluorescence

摘要

摘要:
目的建立液相色谱-原子荧光光谱法测量作业场所空气中亚砷酸盐As（III）与砷酸盐As（Ⅴ）含量的方法。
方法样品经0.15 mol/L硝酸90℃浸提1 h后，以15 mmol/L磷酸氢二铵为流动相，CNWSep AX（250 mm×4.0 mm×10 μm）（LAEQ-4025G7）色谱柱分离，分析检测空气样品中As（Ⅲ）与As（Ⅴ）。
结果 As（Ⅲ）与As（Ⅴ）在0~100 μg/L时，As（Ⅲ）与As（Ⅴ）线性相关系数（r）：0.999 9和0.999 8，检出限为0.14 μg/L和0.38 μg/L；洗脱效率：As（Ⅲ）为96.77%~98.66%，As（Ⅴ）为95.27%~98.39%；加标回收率：As（Ⅲ）为90.67%~95.60%，As（Ⅴ）为91.82%~95.84%；相对标准偏差（n=6）：As（Ⅲ）为0.47%~1.44%，As（Ⅴ）为0.48%~1.34%。
结论该前处理方法能有效避免无机砷形态的转化，对两种无机砷形态分离效果好，且灵敏度和准确度较高，适用于作业场所中无机砷的测定。

Abstract:
Objective To establish a method for determination of As (Ⅲ) and As (Ⅴ) in the air of workplaces by liquid chromatography -atomic fluorescence spectrometry.
Methods The samples were extracted by 0.15 mol/L HNO₃ solution at 90℃ for 1 h, then As (Ⅲ) and As (V) were separated and analyzed with the mobile phase of 15 mmol/L diammonium hydrogen phosphate, using CNWSep AX(250 mm×4.0 mm×10 μm)(LAEQ-4025G7) column.
Results In the range of 0 -100 g/L, the linear correlation coefficients (r) of As (Ⅲ) and As (V)were 0.999 9 and 0.999 8, respectively. The detection limits of As (Ⅲ) and As (V) were 0.14 g/L and 0.38 g/L, and the elution efficiencies were 96.77% 98.66%, 96.77% 98.66% respectively. The recoveries of As (Ⅲ) and As (V) were 90.67% 95.60%, 91.82% 95.84%, and the relative standard deviations were 0.47% 1.44% and 0.48% 1.34% respectively.
Conclusions This pretreatment method can avoid morphological changes of inorganic arsenic species. The method has good separation effect on two inorganic arsenic species, and has high sensitivity and accuracy, and is suitable for the determination of inorganic arsenic in the air of workplaces.

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