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电感耦合等离子体发射光谱法测定硼硅酸盐玻璃中的硼等常见元素

Determination of Boron and Other Common Elements in Borosilicate Glass by Inductively Coupled Plasma-Atomic Emission Spectrometry

  • 摘要: 硼硅酸盐玻璃中的硼、钙、镁、铝、铁、钛、硅等常见元素普遍采用各元素分别测定的方式进行分析, 分析效率很低; 而且硼的测定普遍采用容量法, 当B2O3含量低于1%时, 容量法测定误差较大.本文以KOH熔融的方式消解样品, 采用电感耦合等离子体发射光谱法(ICP-AES)进行分析.通过实验研究了KOH用量和不同称样量对B2O3测定结果的影响.结果表明, KOH用量在3 g以上时有较好的熔样效率和熔样效果, 称样量低于0.4 g对B2O3测定结果无明显影响, 考虑到其他元素的测定, 确定了KOH用量优选3 g, 称样量优选0.1 g.在此条件下, 测定B2O3等常见元素的精密度(RSD, n=6)≤2%, 加标回收率在96.0%~105.6%之间, 除SiO2测定误差较大外, 其他元素的测定结果均令人满意.本方法确定的B2O3的定量限为0.067%, 且对于B2O3最高含量达到16%的测定结果也令人满意, 因此可测定B2O3含量的范围至少为0.067%~16%.当样品中的B2O3含量高于4%时, 方法准确度和精密度与国家标准分析方法(容量法)相当; 当B2O3含量低于1%时, 方法准确度和精密度都优于容量法.与现有报道相比, 本方法显著拓宽了B2O3的测定范围, 并具有良好的准确度, 而且在B2O3准确测定的同时, 也实现了Ca、Mg、Al、Fe、Ti的定量分析和Si的半定量分析, 大大提高了分析效率, 可以实现硼硅酸盐玻璃中B2O3等常见元素的准确快速分析.

     

    Abstract: Boron and other common elements, such as Ca, Mg, Al, Fe, Ti, Si, in borosilicate glass are commonly determined by different methods with low analytical efficiency. The measurement deviation of commonly used volumetric method for boron determination is large when B2O3 content is lower than 1%. B2O3 and other common elements were determined by Inductively Coupled Plasma-Atomic Emission Spectrometry with sample pretreated by molten KOH and are presented in this paper. The influence of KOH dosage and sample weight is also discussed. The results showed that high efficiency and good effect were found with KOH dosage higher than 3 g, and sample weight lower than 0.4 g had no effect on B2O3 results. Considering other determination elements, the optimum selection of KOH dosage was 3 g, and sample weight 0.1 g. Under these conditions, all RSDs(n=6) of tests were less than 2%, the recoveries of each element were from 96.0% to 105.6%, each element had perfect results besides the obvious deviation of SiO2. The limit of quantification of B2O3 was 0.067%. The result was still good when B2O3 content reached 16%. The content range of B2O3 determination was at least 0.067%-16%. The accuracy and precision of this method for B2O3 determination were equivalent to national standard method (Volumetry) when B2O3 content was higher than 4% and better than volumetric method when B2O3 content lower than 1%. Compared with the related results, the content range of B2O3 determination was significantly extended in this method with high accuracy. Quantitative analysis of Ca, Mg, Al, Fe, Ti and semi-quantitative analysis of Si were simultaneously realized with B2O3 accurate determination. This method greatly increased analytical efficiency. Boron and other common elements can be determined quickly and accurately.

     

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