过氧化钠熔融ICP-OES法测定地矿样品中的硼  

Determination of boron in geological and mineral samples by sodium peroxide melting ICP-OES

作　　者：方宏树 何媛媛 鲁海妍 FANG Hong-shu;HE Yuan-yuan;LU Hai-yan(Qinghai Province Geology Ore Testing and Application Center,Xining 810000,China)

机构地区：[1]青海省地质矿产测试应用中心,青海西宁810000

出　　处：《化学工程师》2023年第1期24-28,共5页Chemical Engineer

基　　金：四川省科技厅科技计划项目(No.22QYCX0061)。

摘　　要：地矿样品中硼的测定难点在于既要将样品完全分解还不能造成硼的损失,本文选择强碱过氧化钠(Na_(2)O_(2))作为熔剂能够完全有效地分解样品。碱熔带入试液中大量的钠会影响仪器测定,采用强酸性阳离子交换树脂,在振荡器上交换吸附溶液中Na+,降低试液含盐量,减小Ca^(2+)、Mg^(2+)、Al^(3+)、Fe^(3+)、K^(+)等阳离子的干扰,同时也可以降低溶液的pH值到中性。使用柠檬酸溶液络合试液中的重金属离子,进一步降低基体干扰。使用电感耦合等离子体发射光谱仪(ICP-OES)进行测定。通过实验,选择出合适的分析谱线,确定最佳的树脂用量和交换吸附时间。对国家标准物质和地矿样品进行测定,确定方法的检出限为50μg·g^(-1),相对标准偏差(RSD,n=7)为1.90%~8.36%,相对误差为-1.67%~5.20%。与其他测试方法进行比对,测定结果没有明显偏差。The difficulty in the determination of boron in geological and mineral samples is that the samples must be completely decomposed without causing boron loss.In this paper,strong alkali sodium peroxide is selected as the flux to decompose the sample completely and effectively.A large amount of sodium brought into the test solution by alkali melting will affect the determination of the instrument.Strong acid cation exchange resin is used,exchange sodium ions in the adsorption solution on an oscillator.It can reduce the salt content of the solution and reduce the interference of cations,such as calcium,magnesium,aluminum,iron and potassium.At the same time,the pH value of the solution can be reduced to neutral.Citric acid solution is used to complex the heavy metal ions in the solution to further reduce matrix interference.The determination was performed using an inductively coupled plasma emission spectrometer(ICP-OES).Through experiments,the appropriate analytical spectrum was selected,the optimum resin dosage and exchange adsorption time were determined.The national reference materials,geological and mineral samples were determined.The detection limit of the method is 50μg·g^(-1).The relative standard deviations(RSD,n=7)were between 1.90%and 8.36%.The relative error were between-1.67%and 5.20%.Compared with other test methods,there is no obvious deviation in the results.

关 键 词：过氧化钠 电感耦合等离子体发射光谱法 地矿 硼 

分 类 号：O657.3[理学—分析化学]