树脂工艺品总挥发性有机物的测定研究  

Study on Determination of Total Volatile Organic Compounds in Resin Crafts

作　　者：黄宗平[1] 黄长春[1] 普旭力[1] 林海霞[1] 涂星朋[1] 黄龙[1] 董清木[1] 

机构地区：[1]厦门出入境检验检疫局,福建厦门361012

出　　处：《工程塑料应用》2013年第8期78-82,共5页Engineering Plastics Application

基　　金：国家质检总局科技计划项目(2012IK124);国家质检总局科技计划项目(2009IK075)

摘　　要：通过测定总挥发物、水分及沸点大于250℃的有机化合物,建立了树脂工艺品中总挥发性有机物的测定方法。研究了烘干温度条件、卡氏炉分析条件,讨论和优化了超声萃取条件和气相色谱工作参数。结果表明,在125℃下恒温120 min,可测得总挥发物,卡氏炉在温度200℃、载气流量为50 mL/min、加热20 min条件下,与卡尔费休滴定仪连用可准确测定水分含量。样品用三氯甲烷在60℃超声萃取40 min,选择HP–5色谱柱,用气相色谱法测定高沸点有机物,可获得良好的灵敏度和准确的定量结果。方法的相对标准偏差(n=6)低于5%。6家实验室对5个不同含量水平下的样品的3次平行测定结果表明,实验室内和实验室间的相对标准偏差分别为1.0%～1.8%和4.8%～7.2%。建立的方法能满足实际工作要求。A method was developed for determination of the total volatile organic compounds in resin craft by determining the total volatile materials, water contents and organic compounds whose boiling points are more than 250 ℃ . The drying temperature conditions and analysis conditions for the oven sample-changer were investigated. The ultrasonic extraction conditions and gas chromatography（GC） parameters were discussed and optimized. The test results show that the total volatile materials can be determined under 125℃ drying for 2 h. The water contents were obtained precisely with Karl Fischer moisture ti-trator with oven sample-changer under 200℃ drying temperature, 50 mL/min carrier gas flux for 20 rain. The test results for high boiling-point compounds also show that good sensitivity and accurate quantitative performances are achieved by GC-FID when the samples are ultrasonic-extracted with chloroform for 40 min at 60℃ and HP-5 capillary is chosen. The relative standard deviations （RSDs, n=6） are all less than 5%. The test results of 3 replicates by 6 laboratories for 5 different content level＇ s samples show that the laboratory RSDs are 1.0% - 1.8% and interlaboratory RSDs are 4.8% - 7.2%. The established method can fully meet the requirements of practical work.

关 键 词：总挥发性有机物 总挥发物 水分 卡尔费休滴定 气相色谱 树脂工艺品 

分 类 号：O656.3[理学—分析化学]