摘要
针对盐碱地高盐分、高pH值环境下有效硒检测的技术瓶颈,建立了基于电感耦合等离子体质谱法的高灵敏度、高精度分析方法。通过优化浸提液种类、液固比、pH值、振荡时间、仪器条件和内标选择并且与原子荧光光谱法在准确性、精密度及抗干扰能力等方面进行了对比。结果表明,用磷酸盐-EDTA作为浸提剂,在pH=5.5、液固比10∶1、振荡时间2 h条件下,RF功率1600 W、载气流速1.10 L/min、He模式流速5.0 mL/min,选用锗为内标能够准确测定盐碱地有效硒。方法学验证表明,有效硒检出限0.002 mg/kg、定量限0.005 mg/kg,相对误差在1.39%~2.59%,加标回收率为95.8%~98.5%,精密度为2.,8%~3.8%,并且对第三次全国土壤普查样品进行了检测分析揭示盐碱土有效硒含量普遍偏低,但局部存在富集现象,为硒资源分区管理与富硒农业开发提供科学依据,为盐碱地生态修复与可持续利用提供了高效可靠的技术支撑,具有显著的环境与农业应用价值。
Aiming at the technical bottleneck of effective selenium detection caused by the high salinity and high pH environment of saline soils in China,this study systematically constructed a new detection method based on inductively coupled plasma mass spectrometry(ICP-MS).Through multi-dimensional technology optimization and strict methodological validation,the technical difficulties of the traditional detection method,such as insufficient sensitivity and serious interference in complex matrix environment,were overcome,providing scientific support for the efficient use of selenium resources in saline-alkaline land.The type of leachate,liquid-solid ratio,pH value,oscillation time,instrumental conditions and internal standard selection were optimized,and comparisons were made with the atomic fluorescence method in terms of accuracy,precision and anti-interference ability.The results showed that the selenium determination using phosphate and phosphate solids method is very sensitive.It was found that the effective analysis of selenium in saline soil could be achieved by using phosphate-EDTA as leaching agent under the conditions of pH 5.5,liquid-solid ratio of 10∶1 and oscillation time of 2 h.The instrumental conditions of RF power of 1600 W,carrier gas flow rate of 1.10 L/min,He-mode flow rate of 5.0 mL/min with germanium chosen as the internal standard could be used to accurately determine the effective selenium in saline soils.Methodological validation showed that the detection limit of effective selenium was 0.002 mg/kg,the quantification limit was 0.005 mg/kg,the relative error was 1.39%-2.59%,the spiked recoveries were 95.8%-98.5%,and the precision was 2.8%-3.8%.The samples of the Third National Soil Survey were tested and analyzed and the content of effective selenium in 100 soil samples was in the range of 0.01-0.11 mg/kg.The average value of overall effective selenium content was 0.065 mg/kg,indicating a low level with most samples concentrated in the range of 0.04-0.08 mg/kg.According to the distribution of effective selenium content,it is necessary to apply selenium-containing fertilizers such as sodium selenite,plant selenium-enriched crops or improve soil governance.This can provide a scientific basis for the zoned management of selenium resources and the development of selenium-enriched agriculture.This method offers efficient and reliable technical support for the ecological restoration and sustainable utilization of saline-alkaline land,and has significant environmental and agricultural application value.
作者
贾雷
左修源
周文辉
孙兆楠
薄海军
JIA Lei;ZUO Xiuyuan;ZHOU Wenhui;SUN Zhaonan;BO Haijun(Hohhot General Survey of National Resources Center,China Geological Survey,Hohhot,Inner Mongolia 010010,China;Liaoning Key Laboratory of Chemical Additive Synthesis and Separation,Yingkou Institute of Technology,Yingkou,Liaoning 115014,China)
出处
《中国无机分析化学》
北大核心
2025年第10期1617-1626,共10页
Chinese Journal of Inorganic Analytical Chemistry
基金
全国金等战略性矿产实验测试技术支撑与服务(呼和浩特中心)项目(DD20251130)
国家重点研发计划项目(2022YFE0196700)
辽宁省教育厅基本科研项目(JYTQN2023016)。
关键词
电感耦合等离子体质谱
有效硒
方法优化
仪器对比
inductively coupled plasma mass spectrometry
available selenium
method optimization
instrument comparison
作者简介
贾雷,男,工程师,主要从事离子色谱的分析与应用研究。E-mail:1308412159@qq.com;通信作者:薄海军,男,高级工程师,主要从事地质矿产分析研究。E-mail:bohaijun1985@163.com。
