Determination of water soluble sulfate in soil by inductively coupled plasma atomic emission spectrometry
HU Jia-zhen1,2, WANG Lin*1, LIU Jun1,2, SHEN Shuo-guo1, YU Ya-hui1, HAN Zhi-xuan2
1. Henan Province Rock & Mineral Testing Centre, Key Laboratory of Precious Metals Analysis and Exploration Technology Ministry of Land and Resources,Zhengzhou 450012, China; 2.UNESCO,International Center on Global-scale Geochemistry, Langfang 065000, China
Abstract：The content of water soluble sulfate in soil is usually determined by EDTA titration method. However, it has some disadvantages such as complex operation and long analysis period. In order to adapt to analysis of samples in large quantities, the temperature, time and frequency for oscillation leaching were optimized. The soil samples were oscillated and leached by cyclotron oscillation for 10min using the freshly prepared deionized water at room temperature in range of 22-28℃. The solid and liquid could be completely separated through high speed freezing centrifuge. Consequently, a kind of method for the direct analysis method of water soluble sulfate in soil by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. Under the selected testing conditions, the mass concentration of sulfate in range of 0.1-500μg/mL had a linear relationship with the corresponding emission intensity, and the linear correlation coefficient of calibration curve was r=0.9999. The detection limit of method was 0.26μg/g. The content of water soluble sulfate in primary reference materials of available state of soil (including GBW07412a, GBW07414a, GBW07415a, GBW07417a, GBW07459 and GBW07461) was determined according to the experimental method. The relative errors (RE) between found results and certified values were between -4.8% and 4.4%, and the relative standard deviations (RSD, n=12) were all not more than 3.3%, which could meet the analysis quality requirements of Industrial Standard for Geology and Mineral of the People′s Republic of China (Specification of Land Quality Geochemical Assessment, DZ/T 0295-2016). The proposed method was applied for the determination of acid and alkaline soil samples from Xiong′an New Area as well as primary reference materials of available state of soil (GBW07413a, GBW07415a, GBW07416a and GBW07417a). Compared to titration method (NY/T 1121.18-2006) and ion chromatography (GB 8538-2016), the found results by experimental method had no significant difference.
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