摘要
建立了在线中和、富集待测离子后用离子色谱对高纯氢氧化钠中痕量阴离子进行检测的分析方法。样品经超纯水溶解、稀释后直接进样。试样经外接纯水输送至In Guard H消除OH-基体干扰，然后经过富集柱浓缩待测阴离子，再经阀切换技术进入离子色谱系统，以淋洗液发生器产生的KOH为淋洗液，流速为1.0 mL/min，采用IonPac AS11-HC分析柱分离后，电导检测器检测。结果表明，在0.1~10.0 mg/L的线性范围内，氯离子、硫酸根、氯酸根的线性相关系数分别为0.999 8，0.999 6和0.999 2。方法对于氯离子、硫酸根、氯酸根的检出限分别为0.03，0.07，0.06 mg/kg，加标回收率分别为92%~104%，91%~111% 和 92%~106%，相对标准偏差（n=7）均小于2.0%。
An ion chromatographic（IC） method was developed for the determination of trace anions in high purity sodium hydroxide after sample neutralization and column concentration.Samples were dissolved and diluted with de-ionized water,and then injected into the IC system directly without any further pretreatment．The sample solution was delivered with de-ionized water,firstly on-line filtrated with In Guard H column for pre removing OH-,and then concentrated with IonPac TAC ULP column.The anions under test in the enrichment column were delivered in the IC system when the valve was switched．With the eluent KOH produced by eluent generator at a flow rate of 1.0 mL/min,the anions were separated on an IonPac AS11-HC column and detected with conductivity detector,then quantitively analyzed by the external standard method．The results indicated that the correlation coefficients of chloride,sulfate,chlorate were 0.999 8,0.999 6 and 0.999 2,respectively,in the linear range of 0.1-10.0 mg/L.The detection limits for chloride,sulfate,chlorate were 0.03,0.07,0.06 mg/kg,respectively,and their spiked recoveries were 92%-104%,91%-111% and 92%-106%,respectively,with their relative standard deviations （n=7） not less than 2.0%.The method was applied in the determination of anions in high purity sodium hydroxide samples with satisfactory results.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第9期1152-1156,共5页
Journal of Instrumental Analysis
关键词
高纯氢氧化钠
氯离子
硫酸盐
氯酸盐
在线中和富集
离子色谱
high purity sodium hydroxide
chloride
sulfate
chlorate
on-line sample neutralization and column concentration
ion chromatography（IC）
