Vacuum gas chromatography using short glass capillary columns combined with mass spectrometry
Vacuum gas chromatography using short glass capillary columns combined with mass spectrometry
复制标题
使用短玻璃毛细管柱的真空气相色谱法与质谱联用
DOI：
10.1021/ac50030a039
复制
发表时间：
1978
影响因子：
7.4
通讯作者：
M. E. Parrish
中科院分区：
文献类型：
--
作者：
F. Hatch;M. E. Parrish
本文介绍了一种短玻璃毛细管柱与质谱仪直接连接，在低于大气压条件下操作的真空气相色谱技术。本文用货车-Deemter曲线比较了23米和12米玻璃毛细管柱常压和亚常压操作的结果。使用氦气、氮气和异丁烷载气。分离可以在低至50托的柱压下实现。在最佳流速下，减压操作产生的柱效率比正常气相色谱操作的柱效率低^ 30%。然而，在高流速下，减压操作可提供比大气压GC操作高100%的柱效率。使用短开口管状柱的气相色谱的优点已在文献（1-3）中描述过。10至30 m的毛细管柱通常可提供10000至60000个有效理论塔板，并提供与最佳填充柱相当或上级的分离。玻璃毛细管柱具有极惰性和能够非常快速分析的优点（3）。短毛细管柱也可以在高流速下操作，这允许在显著低于化合物沸点的温度下洗脱化合物（4），
The technique of vacuum gas chromatography in which a short glass capillary column Is directly connectedto a mass spectrometer and operated under subatmospherlc pressure conditions Is described. Van Deemter curves are presented for comparison between atmospheric and subatmospherlc operation with a 23-m and a 12-m glass capillary column. Helium, nitrogen, and Isobutane carrier gases are employed. Separations can be achieved at column pressures as low as 50 Torr. At the optimum flow velocities, reduced pressure operation produces column efficiencies^ 30% lower than those of normal gas chromatographic operation. However, at high flow velocities, reduced pressure operation can provide column efficiencies^ 100% higher than atmospheric pressure GC operation.The advantages of gas chromatography using short open tubular columns have been described previously in the lit-erature (1-3). Capillary columns of 10 to 30 m generally can provide 10000 to 60000 effective theoretical plates and provide separations comparable or superior to those provided by the bést packed columns. Glass capillary columns have the advantage of being extremely inert and capable of very fast analyses (3). The short capillary columns also can be operated at high flow velocities which allow the elution of compounds at temperatures significantly below their boiling points (4),