碘化钾-甲基异丁基甲酮萃取电感耦合等离子体发射光谱法测定磷酸一铵、磷酸二铵中铊含量

通过对观测方式、测定波长、共存元素干扰等因素进行分析和条件优化，建立了测定磷酸一铵、磷酸二铵中铊含量的碘化钾-甲基异丁基甲酮（KI-MIBK）萃取电感耦合等离子体发射光谱法。实验表明，直接采用电感耦合等离子体发射光谱法进行测定时，磷酸一铵、磷酸二铵中的锰元素对分析结果有正干扰。通过萃取分离，干扰被排除，测定结果准确、可靠。在0～1.0 mg/L范围内，铊的质量浓度与光谱强度呈良好的线性关系，相关系数达1.0000。该方法检出限为0.0072 mg/kg，相对标准偏差为4.28%（n = 10），加标回收率在97.00%～100.5%之间。

Determination of Thallium in monoammonium phosphate and diammonium phosphate by Inductively Coupled Plasma Optical Emission Spectrometry with KI-MIBK Extraction

The method for determination of thallium in monoammonium phosphate and diammonium phosphate by ICP-OES with KI-MIBK extraction was developed on the basis of the analysis and optimization of the factors such as observation mode, wavelength of measurement, interference of coexisting elements, and so on. It was found that the result of direct determination by ICP-OES was positively interfered with Mn in monoammonium phosphate and diammonium phosphate.The interference was eliminated by extraction, and the result was accurate and reliable. In the range of 0 ~1 mg/L, the mass concentration of thallium has a good linear relationship with the spectral intensity (r2=1.0000). The limit of detection was 0.0072 mg/kg, the relative standard deviation was 4.28% (n = 10), and the recoveries were from 97.00% to 100.5%.