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    氧瓶燃烧-离子色谱法测定卤化丁基橡胶和胶塞中氯和溴的含量

    Determination of Chlorine and Bromine in Halogenated Butyl Rubber and Stoppers by Oxygen Flask Combustion-Ion Chromatography

    • 摘要: 将样品剪成约1 mm3的小块,称取样品10.0 mg用无灰滤纸包裹好。在氧瓶中加入10 mL水,以2 L·min-1的流量向氧瓶通氧气1 min,点燃包裹样品的滤纸,迅速放入氧瓶中,用瓶塞密封,静置15 min,振摇后取水溶液供离子色谱分析。采用Dionex AS19阴离子分析柱(4 mm×250 mm,5.0 μm)进行分离,柱温为30℃,以20 mmol·L-1氢氧化钾溶液为淋洗液进行洗脱,流量为1.0 mL·min-1。Cl-和Br-的质量浓度分别在0.5~10,1.0~20 mg·L-1内与其对应的色谱峰面积呈线性关系,检出限(3S/N)分别为0.003,0.025 mg·L-1。加标回收率分别为96.9%~106%,90.4%~108%,测定值的相对标准偏差(n=6)小于3.0%。该方法适用于卤化丁基橡胶和胶塞中卤素的鉴别和含量测定。

       

      Abstract: The sample was cut into small cubs of about 1 mm3, and 10.0 mg of the sample was taben and wrapped up in a piece of ashless filter paper. 10 mL of water was added to the oxygen flask, and then oxygen was introduced through the oxygen flask at a flow rate of 2 L·min-1 for 1min. The filter paper of the wrapped sample was ignited and transferred quickly into the oxygen flask, which was sealed tightly and kept standing for 15 min. After shaking, the solution was taken out for IC analysis. Dionex AS19 anion analytical column (4 mm×250 mm, 5.0 μm) with column temperature of 30℃ was used for seperation, and 20 mmol·L-1 KOH solution was used as mobile phase for elution at a flow rate of 1.0 mL·min-1. Linear relatioships were found beween values of peak area and concentration of Cl-, Br- in the ranges of 0.5-10 mg·L-1 and 1.0-20 mg·L-1 respectively. The detection limits (3S/N) were 0.003 mg·L-1 for Cl- and 0.025 mg·L-1 for Br-. Values of recovery obtained by standard addition method were in the ranges of 96.9%-106% for Cl- and 90.4%-108% for Br-, and RSDs (n=6) were less than 3.0%. The method was suitable for use to distinguish and determine the halogens in the halogenated butyl rubber and stoppers.

       

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