微波消解- 电感耦合等离子体质谱法 测定土壤和沉积物中溴和碘
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作者单位:

(1.河南省地矿局第一地质矿产调查院,河南 洛阳 471023;2.河南省国土资源厅生态与勘查地球化学应用工程技术中心,河南 洛阳 471023;3.赛默飞世尔科技,上海 201206)

作者简介:

李永新(1974-),男,河南焦作人,本科,工程师,主要从事土壤和水质分析及分析方法研究,E-mail:635788659@qq.com。

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基金项目:

基金项目:洛阳市硒资源详查项目(洛公交易采购)[2018]053 号)。


LI Yong-xin1,2,REN Yu-zhong1,SUN Wen-jun1,2,LIU Xiang-lei1,2,WEN Tian-yao1,2,SHI Zhi-lu1,WANG Tengfei
Author:
Affiliation:

(1.The First Institute of Geological and Mineral Resources Survey,Henan Province Geological Exploration Bureau,Luoyang Henan 471023;2.Ecology and Exploration Geochemistry Application Engineering Technology Center of Henan Province,Luoyang Henan 471023;3.Thermo Fisher Scientific,Shanghai 201206)

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    摘要:

    传统上采用碳酸钠和氧化锌混合试剂烧结、热水浸取、交换树脂分离基体干扰、电感耦合等离子体质谱法(ICP-MS)测定土壤和沉积物中溴和碘的分析方法,不仅样品处理流程长、效率低,且易造成分析结果的空白值偏高,影响方法的检出限。在现有的研究基础上,采用微波封闭消解技术、12% 稀氨水浸取、碰撞池技术消除多原子离子质谱干扰、ICP-MS 直接测定土壤和沉积物中的溴和碘,实现了高效、高灵敏度的研究目的。结果表明,该方法对溴和碘的检出限分别为0.021 和0.010 mg/kg,精密度(RSD,n=7)分别为4.34% ~ 10.7% 和2.42% ~ 6.81%,准确度(RE,n=7)分别为-1.11% ~ 2.26% 和-2.80% ~ 2.68%。所得结果明显优于传统方法并且与认定值相符,表明此方法对土壤和沉积物中溴和碘的测定具有适用性和可靠性。

    Abstract:

    Traditionally,the use of sodium carbonate and zinc oxide mixed reagent sintering,hot water leaching,exchange resin to separate matrix interference,inductively coupled plasma mass spectrometry( ICP-MS) was developed for the determination of bromine and iodine in soil and sediment analysis method.This method not only has a long sample processing procedure and low efficiency,but also tends to lead to high blank value of the analysis results,which affects the detection limit of the method.Based on the existing research,the ICP-MS was used to directly determine the bromine and iodine in soil and sediment by using microwave closed digestion technology,12% dilute ammonia extraction and collision pool technology to eliminate the interference of polyatomic ion mass spectrometry.It realized efficient and sensitive research purpose.The results showed that the detection limits of this method for bromine and iodine were 0.021 and 0.010 mg/kg,the precision( RSD,n=7) were 4.34%~ 10.7% and 2.42% ~ 6.81%,and the accuracy(RE,n=7) were -1.11%~ 2.26% and -2.80% ~ 2.68%,respectively.The results are better than the traditional method and are consistent with the identified value,which indicates that this method is applicable and reliable for the determination of bromine and iodine in soil and sediment.

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李永新,任彧仲,孙文军,刘向磊,文田耀,时志路,王腾飞,岳涛,陈文华.微波消解- 电感耦合等离子体质谱法 测定土壤和沉积物中溴和碘[J].中国土壤与肥料,2021,(5):346-350.

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  • 收稿日期:2020-10-12
  • 最后修改日期:
  • 录用日期:2020-11-28
  • 在线发布日期: 2021-11-18
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