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Development of Appropriate Acid Digestion Method used for the Determination of Total Uranium in Soil by Inductively Coupled Plasma-Mass Spectrometer (ICP-MS)

유도결합플라즈마-질량분석기(ICP-MS)를 이용한 토양의 총 우라늄 정량에 요구되는 적정 산분해 전처리 방법 개발

  • 신건환 (서울대학교 농업생명과학대학 농생명과학공동기기원) ;
  • 이군택 (서울대학교 농업생명과학대학 농생명과학공동기기원) ;
  • 강지영 (서울대학교 농업생명과학대학 농생명과학공동기기원) ;
  • 윤정기 (국립환경과학원 토양지하수연구과) ;
  • 김현구 (국립환경과학원 토양지하수연구과) ;
  • 노회정 (국립환경과학원 토양지하수연구과) ;
  • 김지인 (국립환경과학원 토양지하수연구과) ;
  • 김계훈 (서울시립대학교 환경원예학과)
  • Received : 2018.11.06
  • Accepted : 2018.11.30
  • Published : 2018.12.31

Abstract

Inductively coupled plasma-mass spectrometry (ICP-MS), one of the most commonly used instruments for metal analysis, was used to determine total uranium in soil. The method was named as "Modified ASTM C1345-96". When comparing with ASTM C1345-96, digestion time (2~3 days) was shorten to 7 hours and the treatment in furnace was eliminated. In analyses of 26 field soil samples, there was a significant difference in the average concentration of total uranium between modified ASTM C1345-96 and ASTM C1345-96 (F : 6.22 > Fc : 4.03, significance level : 0.05, n=26). The average concentration of modified ASTM C1345-96 was 1.8 times larger than that of ASTM C1345-96. In addition, modified ASTM C1345-96 was compared with other acid digestion methods for soil including ISO 11466, Modified ISO 11466, US EPA-3051, US EPA-3051A and US EPA-3052 using a certificated reference material (SRM 2711a, NIST) and field soil samples with different level of organic matter content (1.6%, 5.8%, 10.6%). Modified ASTM C1345-96 showed the best accuracy of 93.01% for SRM 2711a. Also, modified ASTM C1345-96 showed the higher extraction rates than other digestion methods by 11~45%.

Keywords

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Fig. 1. Schematical diagram of digestion methods for the determination of uranium content in soil (validation test level 1).

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Fig. 2. Comparison of analytical results of total uranium in soil according to the various digestion method using SRM 2711a and field soil having different organic content (soil-a: 1.6%, soil-b: 5.8%, soil-c: 10.6%).

Table 1. Physicochemical characteristics of soil used in validation test (level 2)

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Table 2. Analytical conditions of ICP-MS measurement

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Table 3. Summary of each digestion method for the determination of total uranium in soil (validation test level 1)

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Table 4. Summary of each digestion method for the determination of total uranium in soil (validation test level 2)

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Table 5. Analytical results of total uranium content in soil according to the various pre-treatment methods

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Table 6. Statistical results of one-way ANOVA test

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Table 7. Comparison of total uranium content and precision according to the various digestion methods

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Table 8. Comparison of total uranium content according to microwave digestion time

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