Abstract：Electronic pure reagents (high purity hydrochloric acid) were key materials in the field of electronic chemical technology. The establishment of determination method of trace sulfate ion in high purity hydrochloric acid for electronic industry by ion chromatography was of great significance for the development of microelectronic technology. The sample was fully evaporated and concentrated at high temperature to remove the hydrogen chloride and water. The chloride and metal ions were removed by solid phase extraction (SPE) silver column and sodium column, respectively. Ultra-low pressure enrichment column was used for on-line pre-enrichment, and the high-capacity anion column was used as for separation and analysis. Consequently, the determination of trace sulfate ion in high purity hydrochloric acid for electronic industry was realized by ion chromatography. The experiments showed that the pH of filtrate was about 6.0-7.0 after treatment with solid phase extraction of silver column and sodium column, which could meet the testing conditions of the instrument. The contents of metal ions, including Li, Ba, Cu, Ca, Ga, Fe, Zn, As, Al, Ni, Cd, Pb, Mn, Sr and Zr, in the solution after solid phase extraction treatment were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). The results showed that the mass concentrations of these metal ions in the solution were all lower than 0.001 mg/L, which indicated that the metal ions in sample solution had no interference with the determination after solid phase extraction treatment. Under the optimal conditions the mass concentration of sulfate ion in range of 1.0-7.0 mg/L had a good linear relationship with correlation coefficients of 0.999 99. The proposed method was applied for the determination of trace sulfate ion in high purity hydrochloric acid for electronic industry. The result was 1.49 mg/L, which was converted to the mass fraction of sulfate in hydrochloric acid, i.e., 4.17×10-6%. The standard deviation (SD) was 2.6%, the relative standard deviation (RSD) was 1.8%, and the recoveries were between 93% and 105%.
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ZHAO Yan, XIE Yanyan, GAO Yan, XU Suoping, BAI Xiaoyan, XU Qing. Determination of trace sulfate ion in high purity hydrochloric acid for electronic industry by ion chromatography. , 2021, 41(3): 86-90.
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