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机构地区:[1]广州广电计量检测股份有限公司,广州510656
出 处:《理化检验(化学分册)》2018年第1期35-38,共4页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基 金:科技部科技型中小企业技术创新基金(11C26244405491);广州市科技型中小企业技术创新基金(2014J4200047)
摘 要:提出了气相色谱-质谱法测定塑料和电子电气产品中N-乙烯基吡咯烷酮的含量的方法。样品1.000 0 g用四氢呋喃10 mL超声提取30 min,提取液经0.45μm聚四氟乙烯滤头过滤后,采用气相色谱-质谱法进行测定,以DB-624毛细管色谱柱进行程序升温,在全扫描模式下选择m/z 56,111,28,41为定性离子,在选择离子监测模式下以m/z 111为定量离子。N-乙烯基吡咯烷酮的质量浓度在0.05~10 mg·L^(-1)内与其峰面积呈线性关系,检出限(3S/N)为0.1 mg·kg^(-1)。按标准加入法进行回收试验,回收率在94.9%~114%之间,相对标准偏差(n=7)在0.040%~1.6%之间。A method was proposed for the determination of N-vinyl-2-pyrrolidone (NVP) in plastic, electronic and electrical products by gas chromatography-mass spectrometry (GC-MS). The sample of 1. 000 0 g was extracted ultrasonically with tetrahydrofuran of 10 mL for 30 rain, and the extract was filtered through PTFE membrane and then determined by GC-MS using DB-624 capillary column for temperature programming. The quanlitative ions (m/z 56, 111, 28, 41) and the quantitative ion (m/z 111) were selected in SCAN and SIM, respectively, linear relationship between values of peak area and mass concentration of NVP was obtained in range of 0. 05-10 mg · L^-1 with detection limit(3S/N) of 0. 1 mg· kg^-1. Test for recovery was made by standard addition method, giving results in the range of 94. 9%-114%, with RSDs (n=7) ranged from 0. 040% to 1.6%.
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