离子色谱-电导抑制法测定电子级双氧水中6种阴离子

Determination of 6 anions in electronic grade hydrogen peroxide by ion chromatography-conductivity inhibition method

建立离子色谱-抑制电导法同时测定电子级双氧水中F^(-)、Cl^(-)、NO_(2)^(-)、NO_(3)^(-)、SO_(4)^(2-)、PO_(4)^(3-)6种阴离子的分析方法。样品采用大体积直接进样,用阀切换技术消除基体干扰,样品经过UTAC-XLP1阴离子捕获柱预浓缩,选用AS-19型阴离子交换柱进行色谱分离,以KOH为淋洗液进行梯度洗脱,柱温为35℃,流量为0.3 mL/min,进样体积为250μL,用电导检测器检测,以外标法定量。6种阴离子在各自的质量浓度范围内与色谱峰面积呈良好的线性关系,相关系数均大于0.999,方法检出限为0.1~1.0μg/L。以市售电子级双氧水为基体进行加标回收试验,加标回收率为92.0%~102.0%,测定结果的相对标准偏差为2.07%~6.65%(n=6)。该方法适用于电子级双氧水中6种痕量阴离子的同时测定。

A method for simultaneous determination of 6 anions including F^(-),Cl^(-),NO_(2)^(-),NO_(3)^(-),SO_(4)^(2-),PO_(4)^(3-)in electronic grade hydrogen peroxide by ion chromatography-conductivity inhibition method was established.The samples were direct injected with large volume,valve switching technology was adopted to eliminate collective interference.The samples were preconcentrated by UTAC-XLP1 anion trapping column and separated by AS-19 anion exchange column,gradient elution was carried out with KOH as eluent,the column temperature was 35℃,at a flow rate of 0.3 mL/min,and the injection volume was 250μL.All of target compounds were detected by conductivity detector and quantified by external standard method.The mass concentrations of six anions had good linear relationships with the chromatographic peak areas in their respective ranges,the correlation coefficients were all more than 0.999,and the detection limits of this method were 0.1-1.0μg/L.The standard addition recovery test was carried out with commercially available electronic grade hydrogen peroxide as the matrix,the recoveries were 92.0%-102.0%,and the relative standard deviations of the results were 2.07%-6.65%(n=6).The method is suitable for simultaneous determination of six trace anions in electronic grade hydrogen peroxide.