摘要
土壤的全磷和全钾常使用电感耦合等离子体发射光谱(ICP-OES)检测,而其他常规的金属元素则多采用电感耦合等离子体质谱(ICP-MS)检测。在使用ICP-MS分析土壤金属元素的基础上,同时进行全磷和全钾的分析,能大大节省样品分析时间,提高检测效率。基于土壤金属元素的硝酸-盐酸-氢氟酸-过氧化氢消解体系,采用微波消解法,建立ICP-MS测定土壤中全磷和全钾的方法,并对ICP-MS法和传统的ICP-OES法开展方法比对。结果表明,磷和钾的测定存在质谱干扰,使用氦气碰撞池模式能有效降低质谱干扰;以103铑作为内标元素,标准曲线线性相关系数均大于0.999;磷的方法检出限为0.014 g/kg,钾为0.015 g/kg;对数偏差在0.014~0.067,相对标准偏差(RSD,n=6)在1.1%~6.8%,准确度及精密度满足《地球化学普查规范(1∶50000)》(DZ/T 0011—2015)的要求。方法比对采用不确定度评定、单因素方差分析及事后多重比较两种方法进行评价,结果均表明,ICP-MS与ICP-OES法对土壤全磷、全钾的检测不存在显著差异。相比于ICP-OES法,ICP-MS法可以同时兼顾全磷、全钾及多种痕量金属元素的检测,大大提高检测效率,在面对检测项目多、样品量大的土壤普查项目时,ICP-MS法的优势能得到更好体现。
Total phosphorus and total potassium in soil are typically detected using inductively coupled plasma-optical emission spectrometry(ICP-OES),while other metal elements are detected using inductively coupled-plasma mass spectrometry(ICP-MS).The simultaneous analysis of total phosphorus and total potassium based on the analysis of metal elements in soil using ICP-MS can greatly reduce the sample analysis time and improve overall efficiency.Based on the nitric acid-hydrochloric acid-hydrofluoric acid-hydrogen peroxide digestion system for soil metal elements,a microwave digestion method was established for the determination of total phosphorus and total potassium in soil by ICP-MS,and a method comparison between the ICP-MS method and the traditional ICP-OES method was carried out.The findings revealed that mass spectral interferences affected the determination of phosphorus and potassium,and these interferences could be effectively reduced by using the He collision cell mode.The standard curve linear correlation coefficients for both elements exceeded 0.999 using 103Rhodium as the internal standard element,with limits of detection for phosphorus and potassium of 0.014 and 0.015 g/kg,respectively.The logarithm deviation ranged from 0.014 to 0.067,and the relative standard deviations(RSD,n=6)ranged from 1.1%to 6.8%,which satisfied the requirements of accuracy and precision in the Specification of Geochemical Reconnaissance Survey(1∶50000)(DZ/T 0011—2015).The method comparison was evaluated by uncertainty assessment and multiple comparison tests following one-way ANOVA,and the results both showed that there was no significant difference between the ICP-MS method and the ICP-OES method for the detection of total phosphorus and total potassium in soil.Compared with ICP-OES method,ICP-MS method greatly improved detection efficiency by simultaneously detecting total phosphorus,total potassium and a variety of trace metal elements in soil.The advantages of the ICP-MS method can be better demonstrated when facing the soil survey project with a large number of samples and test items.
作者
林健辉
卢嘉慧
梁诗捷
邓豪健
周少锋
许玫英
LIN Jian-hui;LU Jia-hui;LIANG Shi-jie;DENG Hao-jian;ZHOU Shao-feng;XU Mei-ying(Institute of Microbiology,Guangdong Academy of Sciences,Guangzhou Guangdong 510070;Guangdong Detection Center of Microbiology,Guangzhou Guangdong 510070;State Key Laboratory of Applied Microbiology Southern China,Guangzhou Guangdong 510070;Guangdong Provincial Key Laboratory of Microbial Culture Collection and Application,Guangzhou Guangdong 510070)
出处
《中国土壤与肥料》
北大核心
2025年第7期258-266,共9页
Soil and Fertilizer Sciences in China
基金
广东省科学院打造综合产业技术创新中心行动资金项目(2022GDASZH-2022010203-001)
广东省科学院青年人才专项(2024GDASQNRC-0201)
广东省科学院发展专项资金项目(2024GDASZH-2024010102)
“广东特支计划”杰出人才项目(2023JC07L096)。
关键词
土壤全磷、全钾
电感耦合等离子体质谱法
电感耦合等离子体发射光谱法
方法比对
不确定度
方差分析
total phosphorus and total potassium in soil
inductively coupled plasma-mass spectrometry
inductively coupled plasma-optical emission spectrometry
method comparison
uncertainty
analysis of variance
作者简介
林健辉(1984-),硕士,工程师,主要从事环境污染物监测与分析方法研究。E-mail:linjh@gddcm.cn;通讯作者:周少锋,E-mail:zhoushaofeng@gdim.cn。
