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    气相色谱法快速测定橡皮擦中的甲醛

    Rapid Determination of Formaldehyde in Eraser by GC

    • 摘要: 采用柱前衍生-气相色谱法测定橡皮擦中的甲醛。样品经粉碎,过0.180 mm筛后,称取2.000 0 g,用20 mL水于70 ℃浸提20 min,冷却后再超声提取30 min,离心。10.0 mL提取液中加入2,4-二硝基苯肼0.5 mL,于70 ℃衍生反应15 min,冷却后用5 mL甲苯萃取2次,萃取液经DB-5色谱柱分离,采用电子捕获检测器对甲醛衍生物进行检测。甲醛的线性范围为0.105~10.5 mg·L-1,检出限(3S/N)为0.01 mg·L-1,加标回收率在88.6%~92.4%之间。测定值的相对标准偏差(n=6)为2.1%。应用该方法测得32种橡皮擦样品中的甲醛的质量比在0.135~48.5 mg·kg-1之间。

       

      Abstract: GC combined with pre-column derivatizaiton was used to determine formaldehyde in eraser. After being crushed to the size of 0.180 mm, 2.0000 g of sample was extracted with 20 mL water at 70 ℃ for 20 min and cooled, and then extracted ultrasonically for 30 min. After centrifugation, 10.0 mL of the extract derivatized with 0.5 mL of 2,4-dinitrophenylhydrazine at 70 ℃ for 15 min. The solution was cooled and then extracted with 5 mL of toluene for two times. The extract was separated on a DB-5 chromatographic column and formaldehyde derivative was detected by electron capture detector. The linearity range of formaldehyde was 0.105-10.5 mg·L-1 and the detection limit (3S/N) was 0.01 mg·L-1. Recovery rates obtained by standard addition method were in the range of 88.6%-92.4%, and RSDs (n=6) was 2.1%. This method was applied to the determination of formaldehyde in 32 kinds of erasers, giving results in the range of 0.135-48.5 mg·kg-1.

       

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