程序升温毛细管气相色谱法保留温度的作用是什么

2025-03-03 06:47:31
推荐回答(3个)
回答1:

保留温度的作用是在程序升温达到一个平台保留一段平衡时间,可以起到缓冲和稳定作用,主要是平衡时间.

回答2:

温度越高分子运动越快,在气化后的分子,小分子比大分子运动的更快,所以温度的调整对分离作用非常的明显

回答3:

  程序升温气化进样(PTV)

  将气休或液体样品注入气化室处于低温的内衬管后,立即按设定的程序升温步骤,迅速提高气化室的温度。再实现样品的快速气化。此种气化室的结构如图1 所示。它的绪构特点是:

  ①气化室既有实现快速升温的程序升温电热装置,又有可使之快速降温的半导体致冷装置或可通人致冷剂〔液态N2,或CO2)的进、出口通道;

  ②配有分流阀,可实现分流进样和不分流进样;

  ③进样口可采用无隔垫进样头,配有专用的停止阀。也可配备有隔垫的进样头。

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  由上述结构可看出,它在实现程序升温气化进样的同时,也兼有分流/不分流进样和冷柱头进样的功能,是用于毛细管柱气相色谱分析的通用进样器。由于其构造复杂,其价格约为分流/不分流进样器的3倍,为冷柱头进样器的1.5倍,因其功能齐全,高挡气相色谱仪已配备了此种通用进样器。

  此进样器具有既可将样品低温捕集又可将样品快速气化的功能,完全清除了宽沸程祥品的进样失真和分流歧视;可在气化室实现对样品的浓缩。使不挥发物滞留在内衬管中,保护了毛细管柱。它其有的进样操作方式如下:

  ①程序升温气化分流进样,适合于绝大部分样品分析,当进行方法研究或筛选样品时应首先使用此种进样方式。

  ②程序升温气化不分流进样,适合于痕量组分分析,其操作要求和一般不分流进样相似,仅瞬间不分流时间间隔要长一些,约0.5~1.5min,且进样晕可大于一般不分流进样。

  ③冷柱头进样,不启动程序升温,适合于受热易分解样品的分析。

  ④溶剂消除不分流进样.可选择性地除去样品中的大量溶剂,达到浓缩痕量组分的目的。进样时。先关闭分流阀.控制气化室温度稍低于溶剂的沸点、缓慢注入样品,进祥后立即打开分流阀可采用大的放空流量(可高达每分钟几百毫升),同时以低的程序升温速率升高气化室的温度.加速溶剂的气化,待大部分溶剂蒸气放空后,立即关闭分流阀,待气化室达到设定高于柱温的温度,可启动色谱柱程序升温程序进行样品分析。此方法的缺点是有部分低沸点组分会随溶剂一起放空,而使分析获得的样品组成失真。

  由以上介绍的用于毛细管柱的分流进样、不分流进样、冷柱头进样和程序升温气化进祥四种不同操作方式.可看到影响毛细管柱分离效果的因素远比填充柱复杂。但也提供了改善分离效果的更多调节因素。现在毛细管柱的使用范围己远远超过填充柱,因此掌握毛细管柱的不同进样技术,也已成为色谱分析工作者必须掌握的基本功。

  建议您可以到行业内专业的网站进行交流学习!
  分析测试百科网乐意为你解答实验中碰到的各种问题,基本上问题都能得到解答,有问题可去那提问,百度上搜下就有。

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