Determination of Sulfate Ion in Ferric Oxide Powder by Ion Chromatography
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摘要:
实验建立了一种抑制电导检测器离子色谱测定三氧化二铁粉中硫酸根含量的方法。实验采用浓盐酸分解样品， 3.2 mmol/L碳酸钠–1.0 mmol/L碳酸氢钠作为淋洗液，流速为0.7 mL/min，柱温35 ℃，进样体积为20 μL。结果表明，硫酸根离子在0.5～100 mg/L浓度范围内线性关系良好，线性方程为y=0.228 9x-0.038 3，线性相关系数R2=0.999 96。样品加标回收率为97.38%～104.42%，RSD为1.01%，检出限为0.002%。该方法操作简单、灵敏度高、重现性好，可作为三氧化二铁粉中硫酸根离子的定量检测方法。
Abstract:To establish a method for the determination of sulfate ion in ferric oxide powder by ion chromatography with suppression conductivity detector. The hydrochloric acid was used to decomposed samples, with 1.0 mmol/L sodium bicarbonate and 3.2 mmol/L sodium carbonate as mobile phase, and the flow rate was 0.7 mL/min, the colume temperature was 35 ℃, inject volumn was 20 μL. The results show that the sulfate had a good calibration linear ship in the range of 0.5～100 mg/L, the linear equation of sulfate was y=0.228 9x-0.038 3, R2=0.999 96. The recovery from 97.38% to 104.42%, RSD=1.01%, and the limit of detection was 0.002%. This method has the benefits of easy operation, highly sensitive, and good reproducibility. It can be used as a quality detection method of sulfate ion in ferric oxide powder.
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Key words:
- mineral product analysis /
- ferric oxide powder /
- ion chromatography /
- sulfate ion
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表 1 线性范围、回归方程、相关系数和检出限
Table 1. Linear range、regression equation、correlation of coefficient and detection limit
被检测
离子线性范围/
（mg/L）回归
方程相关
系数检出
限/%SO42- 0.5～100 y=0.228 9x-0.038 3 0.999 96 0.002 
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表 2 精密度实验结果
Table 2. Results of precision
硫酸根离子 保留时间/min 峰面积/(（μs/cm.min) RSD/% 1 27.62 1.433 1.01 2 27.61 1.451 3 27.62 1.436 4 27.62 1.425 5 27.62 1.469 6 27.61 1.443 7 27.61 1.432 8 27.63 1.427
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表 3 回收率
Table 3. Rate of recovery
样品 本底值/
（mg/L）加标量/
（mg/L）加标后测定值/
（mg/L）回收率/% 1 2.257 0.50 2.879 104.42 1 2.257 5.00 7.346 101.22 1 2.257 50.00 51.452 98.46 2 40.468 0.50 39.895 97.38 2 40.468 5.00 46.668 102.64 2 40.468 50.00 89.265 98.67
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表 4 样品结果
Table 4. Results of samples
流程
样品本法/% SN/T 3323.2—2012/% GB/T 6730.16—2016/% 1 2.65 2.61 2 0.81 0.83 3 0.13 0.12 4 0.080 0.083 5 0.045 0.047 6 0.026 0.029
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