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ICP-OES标准加入法准确测定海水中的硼
孙玲玲1, 宋金明1, 于 颖1, 孙 萱1, 温廷宇1
中国科学院海洋研究所 分析测试中心
摘要:
硼作为海水中的重要组分, 其准确测定对海洋环境生物地球化学过程研究具有重要意义。海水中硼的常用测定方法具有前处理步骤繁琐、耗时长、样品易被污染、灵敏度低等缺点, 不适于大批量海水样品的准确测定。为剔除海水高盐基体效应及干扰, 本文运用电感耦合等离子体发射光谱法(ICP-OES), 将海水样品进行稀释, 采用标准加入法建立工作曲线, 对海水中硼含量进行准确测定。正交实验显示, ICP-OES最佳工作条件为射频功率 1400 W, 雾化气流量 0.7 L/min, 观测高度14 mm,进样泵速1.5 mL/min。标准加入法标准曲线相关系数大于0.999, 相对标准偏差为0.76%~1.27%, 加标回收率为94.6%~101.8%, 方法检出限为1.073 μg/L。实际的海水样品分析表明, 该方法可消除海水基体干扰, 减少测定误差, 并且前处理操作简单快速, 化学试剂用量少, 回收率高, 精密度好, 灵敏度高, 可用于海水及其它高盐样品中硼含量的准确测定。
关键词:    标准加入法  海水  电感耦合等离子体发射光谱法
DOI:10.11759/hykx20140705001
分类号:
基金项目:中国科学院仪器设备功能开发创新项目(ghy201701)
Accurate determination of boron in seawater by ICP-OES standard addition method
SUN Ling-ling,SONG Jin-ming,YU Ying,SUN Xuan,WEN Ting-yu
Abstract:
As an important component of seawater, the accurate determination of boron has important significance in the study of marine environmental biogeochemistry. The traditional method for detecting boron in seawater has many disadvantages, including the need for tedious pretreatment, being time consuming and easily polluted, and having low sensitivity, making it unsuitable for analyzing numerous seawater samples. In this paper, we accurately determine the boron content in seawater by applying inductively coupled plasma–optical emission spectroscopy (ICP-OES), coupled with the dilution and standard addition methods, to solve the high salt matrix effect and interference problem. The optimum operating parameters of ICP-OES, which we determined using an orthogonal array design, are an RF power of 1400 W, a nebulizer gas flow of 0.7 L/min, a viewing height of 14 mm, and a sample introduction rate of 1.5 mL/min. The correlation coefficient of the linear regression equation was above 0.999. We achieved recovery rates for this method of 94.6%–101.8% and relative standard deviations of 0.76%–1.27%. The detection limit of this method was 1.073 μg/L. Our analysis of actual seawater samples demonstrated this method to be simple, rapid, sensitive, and precise, and able to effectively correct the matrix interference as well as reduce the measurement error. This method could be used to accurately determine boron in seawater and other samples with high salt contents.
Key words:  Boron  Standard addition method  Seawater  ICP-OES
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