顶空气相色谱法测定pvc 中的残留氯乙烯单体含量的探讨.docVIP

精品论文 参考文献 顶空气相色谱法测定pvc 中的残留氯乙烯单体含量的探讨 王菲WANG Fei曰杨军喜YANG Jun-xi（乌海市产品质量计量检测所，乌海016000）（Wuhai City Product Quality Measurement Test，Wuhai 061000，China）摘要院测定pvc 中的残留氯乙烯单体含量,国标GB/T 4615-2008 中采用手动平衡和手动自顶空取样，此方法人为因素干扰多，试验结果重复性差，样品平衡温度不稳定，本文采用自动顶空进样器进样，压力平衡进样技术，使用全封闭传输系统，顶空样品在毛细管线中无扩散；顶空样品在进样过程中无载气稀释，很大程度减少了样品平衡条件的变化，免除了用水浴锅恒温的繁琐步骤。本文的顶空进样器采用压力平衡进样技术以保证得到窄的色谱峰形。可以提供更高的检测灵敏度和确保分析结果的重现性和准确性。 　　Abstract: Manual balancing and manual automatic headspace sampling are usually adopted in GB/T 4615-2008 when detecting thecontent of residual vinyl chloride monomer in pvc. These methods are always interfered by factitious factors, with poor repeatability of thetest results and unstable equilibrium temperature of samples. This article adopts pressure balanced sampling technique, uses automaticheadspace sampler to sample, and uses fully enclosed transmission system so that the headspace samples are without diffusion in thecapillary line. There is no carrier gas dilution for headspace samples in the sampling process, so it greatly decreases the variation of thesample equilibrium conditions and eliminates the tedious steps of water bath temperature. This article adopts pressure balanced samplingtechnique with automatic headspace sampler, to ensure getting the narrow chromatographic peak. It can provide higher sensitivity ofdetection and ensure the repeatability and accuracy of analysis.关键词院pvc；气相；残留氯乙烯单体；顶空进样Key words: pvc；gas phase；residual vinyl chloride monomer；headspace sampling 　　中图分类号院TQ320.77 文献标识码院A 文章编号院1006-4311（2014）06-0313-021. 　　1 仪器、材料和试剂PE Clarus 580 气相色谱仪，HS 40A 自动顶空进样器；容积为23.5mL 的顶空进样瓶；氯乙烯标准气体5ppm、10.4ppm、30ppm；1.2 气相色谱操作条件色谱柱：GDX-301（高分子小球）装于2m伊1/8〞(OD)填充柱（中科院兰州化学物理研究所色谱中心提供）；进样口温度150益；FID 检测器温度260益；柱温90益；流速N230mL/min，H245mL/min，空气450mL/min；1.3 全自动顶空进样器操作条件压力21psi，针温95益，传输线温度115益，炉温90益，加压2min，拔针时间0.5min，进样时间0.05min；1.4 标准曲线的制作用排水法分别从装有5ppm、10.4ppm、30ppm 氯乙烯标准气体钢瓶中准确取出标准气体于顶空进样瓶中，放置于全自动顶空进样器的转盘上，在全自动顶空进样器中恒温10min，加压，进样，峰面积定量，绘标准曲线；1.5 样品分析称取pvc 约4g 于顶空进样瓶中，恒温60min，以下步