公开(公告)号：US4713963A

公开(公告)日：1987-12-22

申请号：US879022

申请日：1986-06-26

申请人： Daryl Sharp

发明人： Daryl Sharp

IPC分类号： G01N30/16 ,  G01N30/72 ,  G01N31/08

CPC分类号： G01N30/7206 ,  G01N2030/165 ,  G01N2030/7226 ,  G01N30/728

摘要： A method and device for analyzing samples containing mixtures of organic compounds using vacuum chromatography is disclosed. The method and device are particularly useful for obtaining mass spectra for identification purposes. The method involves passing a sample dissolved in a solvent through a column with a carrier gas and depositing a thin layer of the sample in the interior of a short column. The short column is then attached to an MS interface. The device comprises a combination of a variable molecular separator and a column alignment component. The alignment component may also be used as a direct probe injector. This device and method allow the separation and MS analysis of mixtures of intermediate molecular weight compounds.

摘要翻译： 公开了一种使用真空色谱分析含有有机化合物混合物的样品的方法和装置。 该方法和装置对于获得用于识别目的的质谱特别有用。 该方法包括将溶解在溶剂中的样品通过载体载气柱并将样品的薄层沉积在短柱的内部。 然后将该短列连接到MS接口。 该装置包括可变分子分离器和柱对准组分的组合。 对准部件也可以用作直接探针喷射器。 该装置和方法允许中等分子量化合物的混合物的分离和MS分析。

公开(公告)号：US20040050251A1

公开(公告)日：2004-03-18

申请号：US10450165

申请日：2003-07-30

发明人： Paolo Magni

IPC分类号： B01D053/02

CPC分类号： G01N30/16 ,  G01N30/12 ,  G01N2030/025 ,  G01N2030/127 ,  G01N2030/165 ,  G01N2030/167

摘要： This invention concerns a method and apparatus for vaporization injection of large volumes of liquid sample (substance to be analysednullsolvent) introduced by means of the needle of a syringe onto a heated vaporization chamber which is part of an injector applied to a device for gas chromatographic analysis, the sample being sent in form of a liquid band travelling through said vaporization chamber at high speed until reaching stopping and vaporization means positioned adjacent to the inlet of a capillary to collect the vapours. In order to inject large volumes without modifying the vaporization chamber and without samples parts losses, in splitless mode, a drawing up of the sample vapours from the vaporization chamber into said capillary is made by means of a local action of volume contraction, caused by recondensation of at least the solvent vapours in this capillary, said capillary being in the form of a pre-column with no stationary phase, maintained at low temperature at least during the injection.

摘要翻译： 本发明涉及一种用于将大量待注射器针引入的液体样品（待分析物质+溶剂）蒸发注入加热的蒸发室的方法和装置，该蒸发室是喷射器的一部分，该喷射器应用于气体装置 色谱分析，样品以高速行进通过所述蒸发室的液体带的形式发送，直到达到停止并且蒸发装置位于与毛细管的入口相邻以收集蒸气。 为了注入大量而不改变蒸发室并且没有样品部件损失，在不分流模式下，样品蒸气从汽化室进入毛细管的方法是通过由再缩合引起的体积收缩的局部作用 至少在该毛细管中的溶剂蒸气，所述毛细管呈不具有固定相的预柱形式，至少在注射期间保持在低温。

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。

公开(公告)号：US4935145A

公开(公告)日：1990-06-19

申请号：US348240

申请日：1989-05-05

申请人： Hernan J. Cortes ,  Curtis D. Pfeiffer ,  Bruce E. Richter

发明人： Hernan J. Cortes ,  Curtis D. Pfeiffer ,  Bruce E. Richter

IPC分类号： G01N30/02 ,  G01N30/16 ,  G01N30/46 ,  G01N30/88

CPC分类号： G01N30/465 ,  G01N30/88 ,  G01N2030/025 ,  G01N2030/165 ,  G01N30/462

摘要： Apparatus and method for on-line coupled liquid chromatography and gas chromatography analysis includes a retention gap which allows injection of a substantial volume of sample-carrying eluent and concentrates bands, obviating adverse effects on the resolution or peak shape of the components of interest. The retention gap is used to simultaneously receive and vaporize liquid solvent in a manner highly suitable for purposes of gas chromatographically separating solutes of interest dispersed in the liquid chromatography solvent.

摘要翻译： 用于在线耦合液相色谱和气相色谱分析的装置和方法包括保留间隙，其允许注入大量样品携带洗脱液和浓缩物带，消除对感兴趣组分的分辨率或峰形的不利影响。 保留间隙用于以非常适合气相色谱分离分散在液相色谱溶剂中的目的溶质的方式同时接收和蒸发液体溶剂。

公开(公告)号：US06955709B2

公开(公告)日：2005-10-18

申请号：US10450165

申请日：2002-12-19

申请人： Paolo Magni

发明人： Paolo Magni

IPC分类号： G01N30/02 ,  G01N30/12 ,  G01N30/16 ,  B01D15/08

CPC分类号： G01N30/16 ,  G01N30/12 ,  G01N2030/025 ,  G01N2030/127 ,  G01N2030/165 ,  G01N2030/167

摘要： This invention concerns a method and apparatus for vaporization injection of large volumes of liquid sample (substance to be analysed+solvent) introduced by a syringe needle into a heated vaporization chamber which is part of an injector coupled operatively to a device for gas chromatographic analysis. The sample is sent in the form of a liquid band traveling through the vaporization chamber at high speed until it reaches a stopping and vaporization device positioned adjacent to the inlet of a capillary to collect the vapors. In order to inject large volumes without modifying the vaporization chamber and without partial losses of the samples, the sample vapors, in splitless mode, are drawn up from the vaporization chamber into the capillary by virtue of the local action of volume contraction caused by recondensation of at least the solvent vapors in the capillary.

摘要翻译： 本发明涉及一种用于将大量体积的待注射针引入的液体样品（待分析物质+溶剂）蒸发注入加热的蒸发室的方法和装置，所述加热蒸发室是可操作地连接到用于气相色谱分析的装置的喷射器的一部分。 样品以以高速行进通过蒸发室的液体带的形式发送，直到其到达位于毛细管入口附近的停止和蒸发装置以收集蒸气。 为了注入大量而不改变蒸发室并且没有样品的部分损失，样品蒸汽以不分流模式从蒸发室通过由缩合引起的体积收缩引起的局部作用从气化室中吸入毛细管中 至少毛细管中的溶剂蒸气。

公开(公告)号：US5400666A

公开(公告)日：1995-03-28

申请号：US252955

申请日：1994-06-01

申请人： Wei J. Song

发明人： Wei J. Song

IPC分类号： G01N1/00 ,  G01N30/02 ,  G01N30/16 ,  G01N30/18 ,  G01N35/06

CPC分类号： G01N35/1079 ,  G01N30/18 ,  G01N2030/025 ,  G01N2030/165

摘要： Methods and apparatus for preventing the failure of slender syringe needles used for on column injection in gas chromatographs are disclosed. A needle holder designed to support the needle precludes bucking deflection beyond the maximum allowable value. In a preferred embodiment, the needle used is a tapered needle that has a proximal diameter and a distal diameter that is smaller that the proximal diameter. In these embodiments, the diameter of the bore through the needle holder is slightly larger than the proximal diameter to permit the full insertion of the entire needle structure. The needle holder bore diameter is sufficiently small, however, to preclude catastrophic failure due to buckling.

摘要翻译： 公开了用于防止在气相色谱仪中用于柱注射的细长注射器针筒失效的方法和装置。 设计用于支撑针的针架可防止超过最大允许值的翘曲偏移。 在优选实施例中，使用的针是具有近端直径和远端直径小于近端直径的锥形针。 在这些实施例中，通过针保持器的孔的直径略大于近端直径，以允许整个针结构的完全插入。 针保持器孔直径足够小，但是防止由于弯曲引起的灾难性故障。

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：US4967590A

公开(公告)日：1990-11-06

申请号：US408609

申请日：1989-09-18

申请人： David J. Miller ,  Steven B. Hawthorne

发明人： David J. Miller ,  Steven B. Hawthorne

IPC分类号： G01N30/02 ,  G01N30/16 ,  G01N30/18 ,  G01N30/20

CPC分类号： G01N30/20 ,  G01N2030/165 ,  G01N30/02 ,  G01N30/18

摘要： An injector for use with a capillary supercritical fluid chromatography (SFC) apparatus includes an operable four-port switching valve having a body portion and a rotor rotatably mounted within the body portion. The rotor has a hole therethrough which will selectively register with pairs of aligned ports. Thus, the rotor is rotatable between a loading position, wherein a first and third port are in communication, and a chromatographic position, wherein a second and fourth port are in communication. A first tubular member extends from the third port and is connected to a retention gap, which is in turn connected to an end of a capillary SFC column. A bypass tube connects the fourth port to the first tubular member. The loading position of the rotor and the first tubular member form a straight pathway to permit a needle to be inserted therethrough into the retention gap to inject a sample. A method is also disclosed whereby said injector permits the venting of a sample solvent from the injector by cycling the rotor, between the chromatographic and loading positions for predetermined time intervals.

摘要翻译： 用于毛细管超临界流体色谱（SFC）装置的注射器包括可操作的四端口切换阀，其具有主体部分和可旋转地安装在主体部分内的转子。 转子具有穿过其中的孔，其将选择性地对准成对的对准端口。 因此，转子可在其中第一和第三端口连通的装载位置和色谱位置之间旋转，其中第二和第四端口连通。 第一管状构件从第三端口延伸并连接到保持间隙，保持间隙又连接到毛细管SFC柱的端部。 旁通管将第四端口连接到第一管状构件。 转子和第一管状部件的装载位置形成直线路径，以允许针穿过其插入保持间隙中以注射样品。 还公开了一种方法，其中所述喷射器允许通过在色谱和装载位置之间循环转动预定时间间隔来从喷射器排出样品溶剂。

公开(公告)号：US07818994B2

公开(公告)日：2010-10-26

申请号：US11596194

申请日：2005-05-11

申请人： Fausto Munari ,  Paolo Magni ,  Koni Grob

发明人： Fausto Munari ,  Paolo Magni ,  Koni Grob

IPC分类号： G01N1/00 ,  G01N30/12

CPC分类号： G01N30/12 ,  G01N2030/127 ,  G01N2030/165 ,  G01N30/34 ,  G01N30/16 ,  G01N2030/126

摘要： The present invention relates to a method for injecting a sample (i.e. a material to be analyzed that may be dissolved in a solvent) in a vaporization chamber or in a pre-column or a gas chromatograper, this method implying separately injecting a co-solvent, with the co-solvent being injected in advance of the sample and/or in a point in the vaporization chamber other than the sample injection point.

摘要翻译： 本发明涉及一种用于在蒸发室或预柱或气相色谱仪中注入样品（即待分析物质可溶于溶剂的方法），该方法意味着分别注入共溶剂 ，其中共溶剂在样品之前和/或在除了样品注入点之外的蒸发室中的点中注入。

公开(公告)号：US20080257013A1

公开(公告)日：2008-10-23

申请号：US11596194

申请日：2005-05-11

申请人： Fausto Munari ,  Paolo Magni ,  Koni Grob

发明人： Fausto Munari ,  Paolo Magni ,  Koni Grob

IPC分类号： G01N1/00

CPC分类号： G01N30/12 ,  G01N2030/127 ,  G01N2030/165 ,  G01N30/34 ,  G01N30/16 ,  G01N2030/126

摘要： The present invention relates to a method for injecting a sample (i.e. a material to be analyzed that may be dissolved in a solvent) in a vaporization chamber or in a pre-column or a gas chromatograper, this method implying separately injecting a co-solvent, with the co-solvent being injected in advance of the sample and/or in a point in the vaporization chamber other than the sample injection point.

摘要翻译： 本发明涉及一种用于在蒸发室或预柱或气相色谱仪中注入样品（即待分析物质可溶于溶剂的方法），该方法意味着分别注入共溶剂 ，其中共溶剂在样品之前和/或在除了样品注入点之外的蒸发室中的点中注入。