气相色谱法测定胶粘剂中的游离甲醛
Determination of Free-formaldehyde in Adhesivesby Gas Chromatography
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摘要: 采用超声波萃取胶粘剂中游离甲醛,经2,4-二硝基苯肼衍生后用气相色谱-电子捕获检测器法测定.对提取方法、衍生化条件及色谱条件进行了研究,确定了甲醛检测的最佳条件.研究数据显示,该方法对甲醛的检出限为0.175 μg/g,在0.1~60 .0 μg/mL浓度范围内,线性相关系数R2=0.9999;在1、2和8 μg/mL 3个添加水平下的添加回收率在98.97%~102.24%之间,5个实验室对同一样品中甲醛含量测定值的相对标准偏差为4.0%.结果表明本方法简便、快速、检测限低、回收率高、重现性好.Abstract: A method for the determination of free-formaldehyde in adhesives by ultrasonic extraction, 2,4-dinitrophenylhydrazine derivatization, and gas chromatography coupled with electron capture detection (GC-ECD) has been developed. Optimum conditions of extraction, derivatization and chromatography were studied. The detection limit of this method for formaldehyde was 0.175 μg/g. The linear range was 0.1~60.0 μg/mL, R2=0.9999. The recoveries ranged from 98.97%to 102.24% at 1, 2 and 8 μg/mL. The relative standard deviation of formaldehyde content determined by 5 laboratories was 4.0%. Results showed that the method is convenient, rapid, and with low detection limit, high recovery and high repeatability.
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Key words:
- ultrasonic extraction /
- gas /
- chromatography /
- formaldehyde /
- adhesives
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