高压离子色谱法测定次氯酸钠中溴酸盐含量

Determination of Bromate in Sodium Hypochlorite by High Pressure Ion Chromatography

摘要: 通过高压离子色谱仪，采用AS-19-4 μm耐高压阴离子色谱柱，以8 mmol的淋洗液浓度进行等度淋洗，在流速1.0 ml/min、电流量87 mA、柱温30℃、定量环选取500 uL的色谱条件下，使用ADRS-600 (4 mm)阴离子电解再生抑制器进行检测。检测样品依据GB 19106-2013次氯酸钠中的试液A制备方法进行制备，通过研究分析后，稀释500倍后测定。实验结果表明：次氯酸钠中溴酸盐达到了很好的分离效果，且检测数据稳定，重现性良好，线性相关系数r ≥ 0.999，多次测定相对标准偏差(RSD)在0.64%~2.05%之间，平均回收率为106%，检出限为0.0020 mg/L。由此得出，本实验方法简便高效、灵敏度高、线性良好，可以用于测定次氯酸钠中溴酸盐含量。

Abstract: The high-pressure ion chromatograph was carried out on an AS-19-4 μm high pressure-resistant anion column with a concentration of 8 mmol eluent, the flow rate was 1.0 ml/min, the current was 87 mA, the column temperature was 30˚C, and the quantitative ring was selected under the conditions of 500 μL. The ADRS-600 (4 mm) anionic electrolytic regeneration inhibitor was used for detection. The test samples were prepared according to the preparation method of test solution A in sodium hypochlorite according to GB 19106-2013. After the analysis, the bromate in sodium hypochlorite was diluted 500 times and measured. The results showed that the bromate in sodium hypochlorite can achieve a good separation effect, the test data were stable with good reproducibility, and the linear correlation coefficient r ≥ 0.999. The relative standard deviation (RSD) was between 0.64% and 2.05%, the average recovery was 106%, and the detection limit was 0.0020 mg/L. It is concluded that this method is simple, efficient, sensitive, and linear, and can be used for the determination of bromate content in sodium hypochlorite.