【引用本文】 杜宝华, 盛迪波, 罗志翔, 等. 低压密闭消解-电感耦合等离子体发射光谱法测定地质样品中的硼[J]. 岩矿测试, 2020, 39(5): 687-695. doi: 10.15898/j.cnki.11-2131/td.201909250139
DU Bao-hua , SHENG Di-bo , LUO Zhi-xiang , et al. Determination of Boron in Geological Samples by ICP-OES with Low-pressure Closed Digestion[J]. Rock and Mineral Analysis, 2020, 39(5): 687-695. doi: 10.15898/j.cnki.11-2131/td.201909250139

低压密闭消解-电感耦合等离子体发射光谱法测定地质样品中的硼

湖南省核工业中心实验室, 湖南 长沙 410100

收稿日期: 2019-09-25  修回日期: 2020-01-01 

作者简介: 杜宝华,高级工程师,从事地质实验测试、电感耦合等离子体光谱/质谱等应用技术研究。E-mail:aabhdu@163.com。。

Determination of Boron in Geological Samples by ICP-OES with Low-pressure Closed Digestion

Hunan Nuclear Central Laboratory, Changsha 410100, China

Received Date: 2019-09-25
Revised Date: 2020-01-01

摘要:采用酸溶-电感耦合等离子体发射光谱法(ICP-OES)测定地质样品中的全硼量,关键环节在于如何防止样品消解过程中硼元素的损失,降低测量过程中的基体干扰、光谱干扰和记忆效应。基于以上问题,本文采用氢氟酸-硝酸-高氯酸-磷酸在低压密闭溶样罐中消解样品,溶出的硼元素与少量磷酸充分络合,防止硼的挥发损失;以基体及主成分浓度与样品相类似的地质类固体标准物质绘制标准曲线做线性校准,有效匹配和降低样品的基体干扰;采用仪器自带的操作软件,观察分析谱线附近是否存在其他元素的干扰,来确定背景扣除最佳的位置及宽度,降低ICP-OES测量中的光谱干扰;以10%的王水作为进样系统的冲洗液,有效消减测量过程中的记忆效应。当稀释因子为200时,方法的检出限(3SD)为1.2μg/g,定量限(10SD)为4.0μg/g;用岩石、土壤及水系沉积物国家一级标准物质对精密度及准确度进行分析验证,11次测定相对标准偏差为1.8%~7.9%,相对误差为-3.6%~6.3%;与外检分析结果对照,对硼含量在定量限以上的样品测定,相对偏差为-4.9%~5.9%。

关键词: 电感耦合等离子体发射光谱法, 低压密闭消解, 标准物质校准, 地质样品, , 记忆效应

Determination of Boron in Geological Samples by ICP-OES with Low-pressure Closed Digestion

KEY WORDS: inductively coupled plasma-optical emission spectrometry, low-pressure closed digestion, calibration of reference materials, geological samples, boron, memory effect

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低压密闭消解-电感耦合等离子体发射光谱法测定地质样品中的硼

杜宝华, 盛迪波, 罗志翔, 王全