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胶粘剂中挥发性醛类化合物的环境气候箱释放模拟及高效液相色谱检测方法研究
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程欲晓,顾中怡,赵波,郭争云,金樱华 上海海关工业品与原材料检测技术中心 
基金项目:国家重点研发专项(2016YFF0203704);质检总局科技专项(2015IK229)
中文摘要:建立了检测胶粘剂施工后13种挥发性醛类化合物释放量的环境气候箱-高效液相色谱(HPLC)法。胶粘剂涂覆于基材上,置于恒温、恒湿的气候箱中,采用2,4-二硝基苯肼(DNPH)吸附管从气候箱采样口进行取样,醛类化合物与DNPH发生化学反应生成稳定的苯腙类衍生物,用乙腈进行淋洗、解吸,定容后进行HPLC分析。采用Kromasil KR100-5 C18色谱柱(250 mm×4.6 mm,5 μm)分离,以乙腈-水为流动相在流速1.0 mL/min下进行梯度洗脱,色谱柱温度为40 ℃,检测波长为360 nm。结果表明:13种醛类化合物在一定质量浓度范围内具有良好的线性关系(r≥0.997 7),检出限(LOD)为1.6~20.8 μg/m3,回收率为86.3%~115%,相对标准偏差为3.5%~8.6%。该方法具有良好的准确度和精密度,为粘合剂施工后醛类化合物释放量的检测提供了一种新方法。
中文关键词:胶粘剂  环境气候箱  高效液相色谱  醛类化合物  释放量
 
Determination of Emission Quantity of Volatile Aldehydes in Adhesive by High Performance Liquid Chromatography with Environmental Chamber
Abstract:A high performance liquid chromatographic(HPLC) method with environmental chamber was developed for the determination of emission quantity of volatile aldehydes in adhesive.Adhesive was spread on the surface of support which was then placed at the center of an environmental chamber.A sufficient volume of environmental chamber air was drawn at an appropriate flow through silicagel tubes impregnated with 2,4-dinitrophenylhydrazine(DNPH) reagent.Aldehydes reacted with DNPH to form non volatile dinitrophenylhydrazones which were desorbed with acetonitrile,and then analyzed by HPLC.The separation was performed on a Kromasil KR100-5 C18 column(250 mm×4.6 mm,5 μm) by gradient elution with acetonitrile and water as mobile phases at a flow rate of 1.0 mL/min.The column temperature was 40 ℃,and the detection wavelength was 360 nm.Results showed that 13 aldehydes had good linear relationships(r≥0.997 7),and the limits of detection(LOD) were in the range of 1.6-20.8 μg/m3.Recoveries for the analytes ranged from 86.3% to 115% with relative standard deviations(RSD) of 3.5%-8.6%.With good precision and accuracy,the method provided a new approach for determination of emission quantity of volatile aldehydes in adhesive after application.
Key Words:adhesive  environmental chamber  high performance liquid chromatography  aldehydes  emission quantity
引用本文:程欲晓,顾中怡,赵波,郭争云,金樱华.胶粘剂中挥发性醛类化合物的环境气候箱释放模拟及高效液相色谱检测方法研究[J].分析测试学报,2020,39(3):396-400.
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