Determination of thirty-one trace impurities in guarantee reagent nitric acid by inductively coupled plasma mass spectrometry with standard addition method
LIU Ting, LI Jian, LI Zhenqian, LU Fan, FENG Jing, LUO Ce
Abstract：The guarantee reagent nitric acid is often used for sample decomposition or as an acidity regulator in the process of sample preparation. Therefore, it is of great significance to monitor the contents of related impurity elements accurately and reliably in guarantee reagent nitric acid. Firstly, the calibration curve method was used for semi-quantitative determination. Then the standard addition amount of each element was determined according to the concentration range of 0.5-fold, 1.0-fold, and 2.0-fold of the content of each element. The method for direct determination of silver, aluminum, arsenic, barium, bismuth, calcium, chromium, cesium, copper, iron, indium, magnesium, manganese, sodium, nickel, lead, rubidium, palladium, tin, strontium, thallium, uranium, vanadium, zinc, boron, hafnium, niobium, tantalum, titanium, tungsten, zirconium content in guarantee reagent nitric acid by ordinary resolution inductively coupled plasma mass spectrometry (ICP-MS) with standard addition was established. The isotopes to be measured were selected through the analysis of mass spectrum interference and the isotopic abundance. The dynamic reaction technology (DRC) was used to determine five elements including calcium, chromium, iron, manganese, and vanadium. Moreover, the measurement conditions of each element were optimized. Other elements were determined at the standard mode. The interference correction equation was used to overcome the interference of nuclear isobar of 115In from 115Sn. Under the optimized conditions, the calibration curve of standard addition method was established for each element. In addition, the working curve with the "external standard method" mode was set using the instrument software. The subsequent detections of other guarantee reagent nitric acid samples could be conducted directly under this working curve without the need of standard addition for every sample. The linear correlation coefficients (r) of working curves for elements were all not less than 0.999. The limits of detection were between 0.000 3 and 0.114 ng/mL, and the limits of quantification were between 0.001 0 and 0.38 ng/mL. The proposed method was applied for the determination of 31 trace impurity elements in guarantee reagent nitric acid samples. The results showed that the mass concentration of calcium and sodium exceeded 75 ng/mL, the mass concentration of boron, iron, magnesium and zinc were between 5.0 and 11.0 ng/mL, and the mass concentration of other elements were all less than 5.0 ng/mL. The relative standard deviations (RSD, n=7) of the determination results were between 0.89% and 5.9%, and the recoveries were between 90% and 110%. The proposed method not only solved the problem of too high detection cost of high-resolution ICP-MS, but also used the standard addition method after dissolving the sample, which avoided the relatively low efficiency of sample pretreatment method of evaporation and enrichment, and the risk of sample contamination.
刘婷, 李剑, 李震乾, 卢凡, 冯婧, 罗策. 电感耦合等离子体质谱标准加入法测定优级纯硝酸中31种痕量杂质元素[J]. 冶金分析, 2022, 42(7): 54-61.
LIU Ting, LI Jian, LI Zhenqian, LU Fan, FENG Jing, LUO Ce. Determination of thirty-one trace impurities in guarantee reagent nitric acid by inductively coupled plasma mass spectrometry with standard addition method. , 2022, 42(7): 54-61.
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