Improvement of speed of separation in packed column gas chromatography
Improvement of speed of separation in packed column gas chromatography
复制标题
DOI：
10.1021/ac00251a011
复制
发表时间：
1982-12
影响因子：
7.4
通讯作者：
R. J. Jonker;H. Poppe;J. Huber
中科院分区：
文献类型：
--
作者：
R. J. Jonker;H. Poppe;J. Huber
本文提出了提高填充柱气相色谱分离速度的一般策略。从气相中分散的最优化方程出发，讨论了进样量、固定相中的传质、检测和进样等各种限制因素。当高分离速度与合理的信噪比和动态范围相结合时，填料柱上级开管柱。优化导致显着的小型化的色谱系统。在实验部分中，长度在32和250 mm之间的柱，填充有10 µ\硅质颗粒的浆料，显示出产生最小h值为2的hv曲线。S-3.5，渗透系数约为1.2 × 10 - 3。最快的色谱图显示峰标准偏差为2 ms，理论塔板数超过14000/s。速度的提高促进了信号增强方法，如系综平均，这在一个例子中得到了证明。在过去的十年里，气相色谱中填充柱的效率一直是很少创新努力的主题。这是完全可以理解的，因为我们在高效开管柱色谱的开发和分析应用上付出了巨大的努力。此外，对于已经能够每10-30分钟得出一个结果的分析方法，加快其速度的动机并不强烈，因为通常认为取样、样品预处理和结果解释等需要相当数量的时间。
The general strategy for the Improvement of speed of sepa-ration in packed column gas chromatography Is addressed. Starting from optimization equations for the dispersion In the gase phase, we discuss the various other limiting factors such as sample capacity, mass transfer In the stationary phase, detection, and Injection. The packed column Is found to be superior to the open tubular column when a high separation speed Is to be combined with a reasonable signal to noise ratio and dynamic range. The optimization leads to a significant miniaturization of the chromatographic system. In the experimental part, columns between 32 and 250 mm In length, slurry packed with 10 µ\siliceous particles, are shown to produce hv curves with a minimum h value of 2. S-3.5 and a permeability factor of about 1.2 X 10~ 3. The fastest chromatograms show peak standard deviations of 2 ms, and more than 14 000 theoretical plates/s. The Increased speed facilitates signal enhancement methods like ensemble averaging which Is demonstrated in an example.The efficiency of the packed column in gas chromatography has been the subject oflittle innovative effort duringthe last decade. This is quite understandable because of the tre-mendous efforts which were rightly spent on the development and analytical application of high efficiency open tubular column chromatography. Also the incentive for speeding up an analytical method already capable of yielding a result every 10-30 min has not been very strong, as is often argued that sampling, sample pretreatment, and interpretation of the results etc. require times of comparable magnitude.