离子色谱-电导法检测格瓦斯中痕量溴酸盐

该研究建立了用离子色谱-电导检测法测定格瓦斯中痕量溴酸盐的分析方法。试样经石油醚洗去油脂，用超纯水振摇提取，依次过0.22 μm微孔滤膜、Dionex OnGuard II RP小柱及Dionex OnGuard II Ag/H小柱处理后进样检测，选用IonPac AS19阴离子交换分离柱，8～45 mmol/L KOH淋洗液梯度洗脱，流速1.0 mL/min，采用抑制型电导检测器检测。结果表明，溴酸盐在1.0～100.0 μg/L质量浓度范围内线性良好，相关系数R2为0.999 8；精密度试验结果相对标准偏差（RSD）：保留时间RSD为0.21%、峰面积RSD为0.44%；方法检出限（LOD）为0.048 μg/g，定量限（LOQ）为0.16 μg/g；在2.5 μg/L、5.0 μg/L、25.0 μg/L三个质量浓度添加水平下，平均加标回收率为93.08%～98.05%。该方法精密度、准确性和稳定性良好，操作简便，适用于格瓦斯中痕量溴酸盐检测。

Determination of trace bromate in Kvass by ion chromatography with conductivity detection

A new method for the determination of trace bromate in Kvass by ion chromatography with conductivity detection was established. The samples were washed with petroleum ether to remove oil, extracted by shaking with ultra-pure water, injected and determined after treatment with 0.22 μm microporous filter membrane, Dionex OnGuard II RP column and Dionex OnGuard II Ag/H column. IonPac AS19 anion exchange separation column was selected. Gradient elution with 8-45 mmol/L KOH eluent was performed at a flow rate of 1.0 ml/min and detected by inhibitory conductance detector. The results showed that the bromate had good linearity in the mass concentration range of 1.0-100.0 μg/L, the correlation coefficient R2 was 0.999 8. The relative standard deviation (RSD) of precision test results was as follows: RSD of retention time 0.21% and RSD of peak area 0.44%. The limit of detection (LOD) of the method was 0.048 μg/g, and the limit of quantification (LOQ) was 0.16 μg/g. At the 3 addition levels of mass concentration 2.5 μg/L, 5.0 μg/L and 25.0 μg/L, the average standard recovery rate was 93.08%-98.05%. The method had good precision, accuracy and stability, and was easy to operate, which was suitable for the determination of trace bromate in Kvass.