四酸敞口溶解-电感耦合等离子体发射光谱法测定土壤中的硫
| 1. | 河北省地质实验测试中心, 河北 保定 071051 |
| 2. | 中国人民大学环境学院, 北京 100872 |
Determination of Sulfur in Soil by Inductively Coupled Plasma-Optical Emission Spectrometry with Four Acids Open Dissolution
| 1. | Hebei Research Center for Geoanalysis, Baoding 071051, China |
| 2. | School of Environment & Natural Resources, Renmin University of China, Beijing 100872, China |
摘要：当前土壤中硫元素的测定方法主要是X射线荧光光谱法和燃烧法，上述两种方法分析速度慢，对高、低含量样品的分析精度较差，难以满足大批量样品快速、准确分析的要求。为提高分析速度和结果的准确度，本文建立了用盐酸-硝酸-氢氟酸-高氯酸（四酸）溶解土壤样品，电感耦合离子体发射光谱法测定硫的方法。通过考察王水消解、王水水浴消解和四酸消解的溶样效果，测定结果表明采用四酸能更好地溶解土壤样品中的硫。方法检出限为10 μg/g，测量范围为33.3~50000 μg/g，相对标准偏差为0.47%~4.05%。本方法简单快速，准确度高，已经过数千件实际样品验证，在不增加分析成本的情况下，一份溶液还可以同时测定钾钠钙镁铁锰铍锂镧铈钪钒钴镍钛等元素，适合在地质行业推广应用。
Determination of Sulfur in Soil by Inductively Coupled Plasma-Optical Emission Spectrometry with Four Acids Open Dissolution
ABSTRACT At present, sulfur in soil is mainly determined by X-ray Fluorescence Spectrometry and tube furnace combustion iodine methods. The analysis speed of these two methods is slow, and the analysis accuracy is poor for both high and low content samples, difficult to meet the requirements of accurate and rapid determination of many samples. In order to improve the speed and accuracy of analysis, a new method for the determination of sulfur in soil samples by Inductively Coupled Plasma-Optical Emission Spectrometry combined with four acids digestion was developed. In this paper the digestion effect of aqua regia, aqua hot water bath and HCl-HNO3-HF-HClO4 is compared. The four acids digestion method was proven to better dissolve sulfur in soil samples. The method is simple, rapid and accurate with a low detection limit of 10 μg/g, analysis range between 33.3 μg/g and 50000 μg/g, and relative standard deviation between 0.47% and 4.05%. Many elements such as potassium, sodium, calcium, magnesium, iron, manganese, beryllium, lithium, lanthanum, cerium, scandium, vanadium, cobalt, nickel, and titanium can be determined simultaneously in a solution without increasing analysis cost. The method, which has been verified with actual samples, is suitable for application in the geological industry.
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