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LIU Xiang-lei,SUN Wen-jun,WEN Tian-yao,LI Yong-xin,WANG Teng-fei,LIU Xue-li,YAN Yu,LI Huai-chao.Determination of 23 Metal Elements in Detailed Soil Survey Samples by Inductively Coupled Plasma-Mass Spectrometry with Three Acid Stepwise Digestion[J].Rock and Mineral Analysis,2020,39(5):793-800
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Determination of 23 Metal Elements in Detailed Soil Survey Samples by Inductively Coupled Plasma-Mass Spectrometry with Three Acid Stepwise Digestion
Received:February 27, 2019  Revised:September 30, 2019
DOI:10.15898/j.cnki.11-2131/td.201902270026
Key words: detailed soil survey samples|metal elements|nitric acid-hydrofluoric acid-perchloric acid digestion|inductively coupled plasma-mass spectrometry
Author NameAffiliation
LIU Xiang-lei The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China
Ecology and Exploration Geochemistry Application Engineering Technology Center of Henan Province, Luoyang 471023, China 
SUN Wen-jun The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China
Ecology and Exploration Geochemistry Application Engineering Technology Center of Henan Province, Luoyang 471023, China 
WEN Tian-yao The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China
Ecology and Exploration Geochemistry Application Engineering Technology Center of Henan Province, Luoyang 471023, China 
LI Yong-xin The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China 
WANG Teng-fei The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China 
LIU Xue-li The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China 
YAN Yu The First Institute of Geological and Mineral Resources Survey, Henan Province Geological Exploration Bureau, Luoyang 471023, China 
LI Huai-chao Luanchuan County Environmental Protection Monitoring Station of Henan Province, Luanchuan 471500, China 
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Abstract:
      BACKGROUND: The soil detailed survey samples have the characteristics of large quantity, complex matrix, and high organic matter content. The traditional digestion method using a variety of mixed acid systems not only leads to incomplete digestion of organic matter, but also leaves black carbon in the solution after digestion. Because the sample is only extracted with dilute nitric acid, some insoluble oxides, sulfates, and fluorides are difficult to form soluble salts, resulting in incomplete extraction. If the reverse aqua regia is used during extraction, it is easy to introduce a large amount of chloride ions and cause the interference problem of chlorine multi-atomic ion mass spectrometry.
OBJECTIVES: In order to accurately determine 23 metal elements in soil. The analysis efficiency and quality can be improved by making full use of the different characteristics of nitric acid, hydrofluoric acid and perchloric acid in sample digestion.
METHODS: Soil samples were digested on electric heating plate, by stepwise addition of nitric acid, hydrofluoric acid and perchloric acid. For the digested samples, nitric acid-hydrochloric acid (20:1, V/V) mixed solution was used as the extractant, effectively reducing the interference of chlorine polyatomic ion mass spectrum and extracting elements thoroughly. Twenty-three metal elements in the soil were simultaneously determined by inductively coupled plasma-mass spectrometry (ICP-MS).
RESULTS: This method can effectively digest organic matter and silicate components in soil. It has the advantages of less reagent consumption,less mass spectrum interference of chlorine, simple operation process, high working efficiency, and lower detection limit (0.0008-0.90mg/kg, 3s). This method was applied to the national level standard substance such as dark brown soil, limestone soil, yellow brown soil samples for the determination of 23 elements, and the measurement result was superior to the traditional digestion method. The precision (RSD, n=6) was 0.022%-5.83% and relative error was -8.33% to 9.17%. The results are consistent with the certified values, indicating that the method is applicable and reliable.
CONCLUSIONS: The method for the simultaneous determination of 23 elements in soil samples by ICP-MS with three acid stepwise digestion has high applicability and reliability.