Determination of Sulfur in High-sulfur Bauxite by Alkali Fusion-Inductively Coupled Plasma-Optical Emission Spectrometry
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摘要: 应用电感耦合等离子体发射光谱法（ICP-OES）测定高硫铝土矿（硫含量≤8%）中的硫时，由于硫存在-2、+4和+6等多种价态，常用的酸溶法和碱熔法处理高硫铝土矿时往往无法完全氧化硫而导致硫测定结果偏低。本文用过氧化钠熔融、热水浸取和盐酸酸化提取高硫铝土矿中的硫，使用基体匹配法绘制校准曲线补偿铝和钠对硫测定的光谱干扰，以S182.034 nm（184 nm）作为分析谱线，采用ICP-OES对硫进行测定。结果表明：3 g过氧化钠在700℃下熔融10 min，可以较好地氧化高硫铝土矿中的硫；校准曲线的线性相关系数为0.9999，方法检出限为0.025 μg/mL，相对标准偏差（RSD，n=6）小于5%；与碳硫仪的测定结果相比较，两种方法无显著性差异。本方法溶样彻底，无样品损失，为今后实现应用ICP-OES同时测定高硫铝土矿中的硫和其他元素奠定了基础。
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关键词:
- 铝土矿 /
- 硫 /
- 过氧化钠碱熔 /
- 电感耦合等离子体发射光谱法
Abstract: When Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) is used to analyze the sulfur content of high-sulfur (S≤8%) bauxite, commonly used acid dissolving and alkali fusion methods cannot oxidize sulfur completely, leading to a false (lower) result of sulfur due to multiple valences of sulfur (-2, +4, +6). In this study, high-sulfur bauxite samples were fused with sodium hydroxide and leached out by hot water and hydrochloric acid, and the calibration curve was plotted through a matrix matching method to compensate for the spectral interferences of aluminum and sodium on sulfur. S182.034 nm (184 nm) was selected as the analytical line, and sulfur was analyzed by ICP-OES. Results show that sulfur in high-sulfur bauxite samples is completely oxidized with 3 g sodium peroxide at 700℃ for 10 min. The linear correlation coefficient of the calibration curve was 0.9999, the detection limit was 0.025 μg/mL, and the relative standard deviation (RSD, n=6) was less than 5%. Compared with the results of carbon sulfur analysis, there are no significant differences between the two methods. This method has the advantage of completely decomposing the samples without any loss, which will lay the foundations for the simultaneous determination of sulfur and other elements in high-sulfur bauxite by ICP-OES. -
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表 1 不同溶样方法的比较
Table 1. Comparison of analytical results of sulfur with different dissolution methods
溶样方法 溶解状况 硫含量ICP-OES测定结果 样品1 样品2 样品3 平均值 (%) 绝对误差 (%) 平均值 (%) 绝对误差 (%) 平均值 (%) 绝对误差 (%) 盐酸+硝酸+氢氟酸+高氯酸 未溶清 0.50 -0.07 1.48 -0.20 2.00 -0.28 氢氧化钠 溶清 0.49 -0.08 1.46 -0.22 1.98 -0.30 氢氧化钠+过氧化钠 溶清 0.52 -0.05 1.55 -0.13 2.10 -0.18 过氧化钠 溶清 0.55 -0.02 1.64 -0.04 2.22 0.06 碳硫仪测定结果 0.57 - 1.68 - 2.28 - 注：绝对误差=ICP-OES测定值-碳硫仪测定值。 
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