Abstract：Chlorine is an important indicator for land quality investigation and evaluation. In the geological industry, the industrial standard method for the analysis of chlorine is X-ray fluorescence spectroscopy (DZ/T 0279.10-2016). The difficulty of the method is that chlorine is easily contaminated,and the measured values are easily affected by some factors such as measurement time,number of measurements, and sample storage conditions. The sample was decomposed at high temperature,and the generated chloride was dried with concentrated sulfuric acid and then transferred into the absorption cell of electrolytic cell of elemental analyzer.The chloride ions (Cl-) generated in absorption process could react with silver ions (Ag+) to form silver chloride precipitation.The elemental analyzer could automatically determine the titration end point according to the equilibrium potential,and meanwhile automatically calculate the chlorine content in the sample.The experiments showed that the addition of excessive acetic acid in electrolyte could effectively inhibit water electrolysis,avoiding the analytical error caused by water electrolysis.The limit of detection of proposed method was 10.4 μg/g. The proposed method was applied for the determination of chlorine in national certified reference materials of soil and stream sediment.The relative standard deviation (RSD, n=12) of determination results was less than 7%,and the relative error (RE) was less than 6%. The relative deviation (RD) between analysis results of actual samples by the experimental method and X-ray fluorescence spectrometry could meet the requirements.The proposed method was suitable to analyze large quantities of samples due to some advantages such as the use of solid sample injection,small usage of sample (0.050 0-0.150 0 g), and no need of curve calibration.
石友昌, 吕振龙, 杨金国, 王志凯, 黎宏新, 杨国军. 元素分析仪测定土壤和水系沉积物中氯[J]. 冶金分析, 2022, 42(5): 37-42.
SHI Youchang, LÜ Zhenlong, YANG Jinguo, WANG Zhikai, LI Hongxin, YANG Guojun. Determination of chlorine in soil and stream sediment by elemental analyzer. , 2022, 42(5): 37-42.
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