公开(公告)号：US5215556A

公开(公告)日：1993-06-01

申请号：US868917

申请日：1992-04-15

申请人： Joseph F. Hiller ,  Glen H. Hughes ,  Daniel P. Martin

发明人： Joseph F. Hiller ,  Glen H. Hughes ,  Daniel P. Martin

IPC分类号： G01N30/02 ,  G01N30/30

CPC分类号： G01N30/30 ,  G01N2030/025 ,  G01N2030/3015 ,  G01N2030/3023

摘要： Apparatus and method for temperature gradient capillary gas chromatography wherein the chromatography column is surrounded by an inner tube and the inner tube is surrounded by an outer tube. A first heat transfer fluid is heated to a first temperature and is flowed between the inner tube and the column in the same direction as the flow of carrier gas through the capillary column. A second heat transfer fluid is heated to a second temperature and is flowed in the opposite direction between the outer tube and the inner tube, the second temperature being lower than the first temperature. The invention is also an improved capillary gas chromatography method of the type that generally includes the steps of flowing a carrier gas through a capillary gas chromatography column to a detector, introducing a sample to be analyzed into the column and then detecting chromatographically resolved components of interest of the sample, the method having an optimum carrier gas velocity through the column, wherein the improvement of the instant invention is to establish a negative temperature gradient along at least a portion of the longitudinal length of the capillary gas chromatography column and to flow the carrier gas through the capillary gas chromatography column at less than the optimum carrier gas velocity.

摘要翻译： 用于温度梯度毛细管气相色谱的装置和方法，其中色谱柱被内管包围，内管被外管包围。 第一传热流体被加热到第一温度，并且沿着与通过毛细管柱的载气流相同的方向在内管和塔之间流动。 第二传热流体被加热到第二温度，并且在外管和内管之间沿相反方向流动，第二温度低于第一温度。 本发明还是改进的毛细管气相色谱法，其通常包括将载气通过毛细管气相色谱柱流动到检测器的步骤，将要分析的样品引入柱中，然后检测色谱分辨的感兴趣组分 该方法具有穿过柱的最佳载气速度，其中本发明的改进是沿着毛细管气相色谱柱的纵向长度的至少一部分建立负温度梯度并使载体流动 气体通过毛细管气相色谱柱小于最佳载气速度。

公开(公告)号：US5048322A

公开(公告)日：1991-09-17

申请号：US402327

申请日：1989-09-05

申请人： Joseph F. Hiller ,  Terrence McCabe ,  Paul L. Morabito

发明人： Joseph F. Hiller ,  Terrence McCabe ,  Paul L. Morabito

IPC分类号： G01N30/02 ,  G01N30/08 ,  G01N30/10 ,  G01N30/12 ,  G01N30/16 ,  G01N30/30

CPC分类号： G01N30/16 ,  G01N30/08 ,  G01N30/30 ,  G01N2030/025 ,  G01N2030/085 ,  G01N2030/165 ,  G01N2030/167 ,  G01N2030/3046 ,  G01N2030/3069 ,  G01N2030/3084 ,  G01N30/10

摘要： The invention describes a large volume on-column gas chromatographic method for analyzing trace levels of high molecular weight and polar compounds in a sample and an apparatus for performing the method. A column inlet coupled to an analytical column is heated rapidly to concentrate difficult to chromatograph compounds onto the analytical column resulting in an increase in the detectability of the compounds.

摘要翻译： 本发明描述了用于分析样品中痕量水平的高分子量和极性化合物的大容量柱内气相色谱法和用于实施该方法的装置。 与分析柱相连的色谱柱入口被快速加热，难以将色谱化合物浓缩到分析柱上，导致化合物的可检测性增加。

公开(公告)号：US4962042A

公开(公告)日：1990-10-09

申请号：US448410

申请日：1989-12-08

申请人： Paul L. Morabito ,  Richard G. Melcher ,  Joseph F. Hiller ,  Terrence McCabe

发明人： Paul L. Morabito ,  Richard G. Melcher ,  Joseph F. Hiller ,  Terrence McCabe

IPC分类号： G01N30/06 ,  G01N30/14 ,  G01N30/16 ,  G01N30/20 ,  G01N30/30 ,  G01N30/32

CPC分类号： G01N30/14 ,  G01N2030/062 ,  G01N2030/165 ,  G01N2030/3046 ,  G01N2030/324 ,  G01N30/20

摘要： In one embodiment the invention is a method for on-column valved injection gas chromatography by on-column injecting more than 5 microliters and less than one milliliter of sample consisting of a solvent and a component of interest into a retention gap/capiliary column system with an injection valve at a first carrier gas flow rate, followed by a substantially higher carrier gas flow rate to blow the solvent of the sample out of the system at a rapidly increased rate and then a return to a lower flow rate to chromatograph the component of interest. In another embodiment, less than 5 microliters of sample consisting of a solvent and a component of interest is on-column injected into a capillary column using an injection valve and a relatively high column inlet pressure of gas to move the sample from the injection valve into the colunm rapidly and with reduced carryover. Then, the pressure of carrier gas is reduced to a normal pressure for chromatography of the component of interest.

摘要翻译： 在一个实施方案中，本发明是一种柱上带阀注入气相色谱法的方法，其通过柱上注入超过5微升和小于1毫升由溶剂和感兴趣组分组成的样品的保留间隙/毛细管柱系统中， 以第一载气流速的喷射阀，然后以显着更高的载气流速将样品的溶剂以快速增加的速率吹出系统，然后返回到较低的流速以色谱分离 利益。 在另一个实施方案中，使用注射阀和相对较高的柱入口压力将小于5微升由溶剂和感兴趣组分组成的样品柱内注入毛细管柱，以将样品从注射阀移动到 快速，随身携带。 然后，将载气的压力降低至感兴趣组分的色谱法的常压。

公开(公告)号：US5001071A

公开(公告)日：1991-03-19

申请号：US254538

申请日：1988-10-06

申请人： Paul L. Morabito ,  Joseph F. Hiller ,  Terrence McCabe ,  Thomas L. Peters

发明人： Paul L. Morabito ,  Joseph F. Hiller ,  Terrence McCabe ,  Thomas L. Peters

IPC分类号： G01N30/16

CPC分类号： G01N30/16 ,  G01N2030/165

摘要： A method for on-column injection of large sample volumes using the retention gap technique in capillary gas chromatography for sample components of interest that would be obscured by the large solvent peak otherwise inherent in the technique. This interference from the large solvent peak is removed by venting carrier flow from the retention gap to waste for a limited time, long enough to discard much of the solvent without serious loss of the sample component of interest.

摘要翻译： 使用保留间隙技术在毛细管气相色谱法中对目标样品组分进行柱内注射大量样品体积的方法，其将被技术中固有的大溶剂峰所掩蔽。 来自大溶剂峰的这种干扰通过将载体流从保持​​间隙排出到废物一段有限的时间来消除，足够长的时间来丢弃大部分溶剂，而不会使感兴趣的样品组分严重损失。

公开(公告)号：US5338514A

公开(公告)日：1994-08-16

申请号：US111808

申请日：1993-08-25

申请人： Paul L. Morabito ,  Terrence McCabe ,  Joseph F. Hiller

发明人： Paul L. Morabito ,  Terrence McCabe ,  Joseph F. Hiller

IPC分类号： G01N30/02 ,  G01N30/10 ,  G01N30/12 ,  G01N30/16 ,  G01N30/38 ,  G01N30/72 ,  G01N30/00

CPC分类号： G01N30/7213 ,  G01N30/12 ,  G01N2030/025 ,  G01N2030/126 ,  G01N2030/165 ,  G01N2030/385 ,  G01N30/10

摘要： Method and apparatus for gas chromatography/mass spectroscopy including a retention gap, a capillary gas chromatography column and a mass spectrometer, the improvement being a valve that facilitates temporarily venting the carrier gas from between the retention gap and the capillary gas chromatography column immediately after the injection of a sample. The valve also facilitates an alternate flow of carrier gas into the mass spectrometer during the venting operation.

摘要翻译： 包括保留间隙，毛细管气相色谱柱和质谱仪的气相色谱/质谱法的方法和装置，其改进是有利于在紧随着保留间隙和毛细管气相色谱柱之后临时排出载气的阀 注射样品。 在排气操作期间，该阀还有助于将载气交替流入质谱仪。