摘要
本研究使用碳酸钠高温碱熔消解试样,通过优化熔融温度、熔融时间、酸溶解条件等实验条件,建立了碱熔-电感耦合等离子体质谱(ICP-MS)法测定土壤中全硼。实验表明,向样品中加入2.0 g Na_(2)CO_(3)于950℃碱熔20 min后,使用HCl水溶液(1:1,V/V)溶解熔块的效果最好。碱熔法可以有效避免硼在HF中易挥发损失的问题。使用有证标准物质和实际样品对方法进行验证,结果表明,该方法测定全硼含量在0~100μg/L浓度范围内的线性关系良好,线性相关系数为0.999 5,方法检出限为0.20 mg/kg,定量限为0.65 mg/kg,方法精密度(RSD,n=6)为1.92%~3.79%,相对误差(RE)为-0.32%~3.69%。实际样品测定的相对标准偏差(RSD,n=6)为0.99%~1.82%。相比于电感耦合等离子体发射光谱(ICP-OES)法,本方法的数据稳定性更好、工作效率更高,适用于土壤中全硼的测定。
The traditional methods of boron determination mainly include spectrophotometry,titration and electrochemical method,etc.These methods are complicated,time-consuming and easy to be affected by external environmental factors.With the development of analytical technology,inductively coupled plasma mass spectrometry(ICP-MS)has gradually become the preferred method for the determination of trace and ultra-trace elements in environmental samples due to its advantages of simple operation,high sensitivity and high selectivity.For ICP-MS analysis,it is very important to choose a appropriate pretreatment method.The commonly used acid hydrolysis method is not only time-consuming,but also has high operational safety risk and environmental pollution,and boron is easy to volatilize in hydrofluoric acid environment,which leads to loss of the analyte.Alkali melting method is very effective for the decomposition and dissolution of insoluble substances.By melting the soil sample with alkaline flux,the boron element in the sample was completely released,and the melt was dissolved with acid,and then analyzed by ICP-MS.This method can effectively avoid the volatilization loss of boron element in the traditional acid solution method,and improve the accuracy and reliability of the determination.In this study,a method of alkali melting and ICP-MS was established for the determination of total boron in soil.The accuracy and reliability of the method were ensured by optimizing the experimental conditions,such as melting temperature,melting time and acid dissolution conditions.The results showed that after adding 2.0 g Na_(2)CO_(3),soil samples were heated at 950℃for 20 min,and then hydrochloric acid solution(1:1,V/V)was used to dissolve the frit,affording the best dissolution effect.With the proposed pretreatment,the linear relationship of total boron concentration in the range of 0-100μg/L is good,and the linear correlation coefficient is 0.9995.The limit of detection and the limit of quantification are 0.20,0.65 mg/kg,respectively.The precision(RSD,n=6)is 1.92%-3.79%,with the relative error(RE)ranging from-0.32%to 3.69%,and the relative standard deviation(RSD,n=6)of the actual sample is 0.99%-1.82%.Compared with inductively coupled plasma-optical emission spectrometer(ICP-OES),the data stability of this method is better,the working efficiency is higher.
作者
陈家舒
熊雄
段锦梅
陈颖麟
江家俊
朱红惠
CHEN Jia-shu;XIONG Xiong;DUAN Jin-mei;CHEN Ying-lin;JIANG Jia-jun;ZHU Hong-hui(Guangdong Provincial Key Laboratory of Microbial Culture Collection and Application,Key Laboratory of Agricultural Microbiome(MARA),Key Laboratory of Agricultural Microbiomics and Precision Application(MARA),State Key Laboratory of Applied Microbiology Southern China,Guangdong Detection Center of Microbiology,Institute of Microbiology,Guangdong Academy of Sciences,Guangzhou 510070,China)
出处
《质谱学报》
北大核心
2025年第3期361-369,共9页
Journal of Chinese Mass Spectrometry Society
基金
广东特支计划项目(2021JC06N628)
广东省科技计划项目(2021B1212050022)。
