高级检索

    离子色谱法测定碳酸锂中氯离子和硫酸根离子的含量

    Determination of Chloride and Sulfate in Lithium Carbonate by Ion Chromatography

    • 摘要: 取碳酸锂样品0.500 g,加适量水溶解,用水定容至100 mL。分取试液10.00 mL在不去除碳酸根基体的前提下直接进行离子色谱分析。采用阴离子交换柱Dionex IonPac AS11作为分离柱,用氢氧化钾淋洗液发生器产生的15 mmol·L-1 KOH溶液为流动相,流量为1.0 mL·min-1,柱温为30 ℃进行色谱分离和测定。氯离子和硫酸根离子的线性范围分别在16.0 mg·L-1和3.2 mg·L-1以内,检出限(3s/k)分别为0.004,0.01 mg·L-1。对同一个样品进行精密度试验,测定值的相对标准偏差(n=6)小于2.7%。 按标准加入法进行回收试验,回收率在93.8%~106%之间。分析结果表明,样品测定结果与电化学法和在线去除基体离子色谱法的测定结果相符。

       

      Abstract: Sample of lithium carbonate (0.500 g) was dissolved in some water, and made up its volume to 100 mL with water. An aliquot of 10.00 mL of the sample solution was taken for IC separation of Cl- and SO42- ions without removing the matrix carbonate. The anion exchange column Dionex IonPac AS11 was used for separation at column temperature of 30 ℃ and 15 mmol·L-1 KOH solution produced by a KOH eluant generator was used as the mobile phase, with flow-rate of 1.0 mL·min-1. Linearity ranges for Cl- and SO42- were within 16.0, 3.2 mg·L-1, with values of detection limits (3s/k) of 0.004, 0.01 mg·L-1, respectively. Test for precision was made with a same sample, giving values of RSDs (n=6) less than 2.7%. Test for recovery was made by standard addition method, giving results in the range of 93.8%-106%. As shown by the results of analysis of substantial samples, consistent values were obtained as compared with those found by electrochemical method and ion chromatography with on-line matrix removing.

       

    /

    返回文章
    返回