顶空气相色谱法测定镍电解液中磺化煤油

镍电解液中残留的有机物会导致镍板表面形成气孔,影响产品外观质量。为检测电解液中重要的有机物组分磺化煤油的含量,实验使用静态顶空气相色谱法,基于氢焰离子化(FID)检测器,无需萃取直接进样测定。通过试验优化了顶空分析的主要条件,确定了最佳的平衡温度(80 ℃) 和平衡时间(60 min)。在最佳条件下,方法的检出限为0.008 mg/L(3S/N),线性范围为0.1～100 mg/L,校准曲线线性相关系数大于0.96。对比镍电解液实际样品与磺化煤油标准溶液的色谱图,各组分出峰位置一致;2个样品测定结果的相对标准偏差(RSD,n=6)为5.3%和4.5%,回收率为92%～104%。

Determination of sulfonated kerosene in nickel electrolyte by headspace gas chromatography

The residual organic matters in nickel electrolyte would cause air holes on nickel plate surface, thus influencing the appearance quality of products. In order to determine the content of sulfonated kerosene (which was an important component of organic matters) in nickel electrolyte, the static-state headspace gas chromatography was adopted in the experiment. The hydrogen flame ionization detector (FID) was used for direct sampling and determination without extraction. The experimental conditions of headspace analysis were optimized. The optimal equilibrium temperature (80 ℃) and equilibrium time (60 min) were obtained. Under the optimized conditions, the detection limit of method was 0.008 mg/L (3S/N), the linear range was 0.1-100 mg/L, and the linear correlation coefficient of calibration curve was higher than 0.96. The chromatograms of actual nickel electrolyte sample and standard solution of sulfonated kerosene were compared. It was found that the peak position of each component was consistent. The relative standard deviation (RSD, n=6) of determination results of two samples was 5.3% and 4.5%. The recoveries were between 92% and 104%.