公开(公告)号：US4814612A

公开(公告)日：1989-03-21

申请号：US31150

申请日：1987-03-25

Applicant: Marvin L. Vestal ,  Calvin R. Blakely ,  Gordon J. Fergusson

Inventor： Marvin L. Vestal ,  Calvin R. Blakely ,  Gordon J. Fergusson

IPC: G01N30/30 ,  G01N30/32 ,  G01N30/72 ,  H01J49/04 ,  H01J49/10 ,  H01J49/28

CPC classification number: H01J49/049 ,  G01N30/7253 ,  H01J49/0445 ,  H01J49/0486 ,  G01N2030/3038 ,  G01N2030/3053 ,  G01N30/32

Abstract: This disclosure is concerned with method and apparatus for vaporizing liquid solutions in order to detect, quantitate, and/or determine physical or chemical properties of samples present in liquid solution. Mixtures may be separated by an on-line liquid chromatographic column and the methods used for detection, quantitation, identification, and/or determination of chemical and physical properties include mass spectrometry, photoionization, flame ionization, electron capture, optical photometry, including UV, visible, and IR regions of the spectrum, light scattering, light emission, atomic absorption, and any other technique suitable for detecting or analyzing molecules or particles in a gaseous or vacuum environment. The method and apparatus involves controlled partial vaporization of the solution. Methods are disclosed for controlling the degree of partial vaporization and the temperature at which this vaporization occurs, and for maintaining this degree of vaporization essentially constant even though the solvent flow rate and/or composition may vary in either a controlled or an uncontrolled fashion. This "thermospray" method and apparatus allows the solvent to be substantially vaporized to produce a supersonic free jet containing a fractionGOVERNMENT SUPPORTThe invention described herein was made in the course of work under a grant or award from the Department of Health and Human Services (formerly Health Education and Welfare).

Abstract translation: 本公开涉及用于蒸发液体溶液以便检测，定量和/或确定液体溶液中存在的样品的物理或化学性质的方法和装置。 混合物可以通过在线液相色谱柱分离，用于检测，定量，鉴定和/或测定化学和物理性质的方法包括质谱法，光离子化，火焰离子化，电子捕获，光学光度法，包括UV， 可见光和红外光谱区域，光散射，发光，原子吸收以及适用于在气态或真空环境中检测或分析分子或颗粒的任何其他技术。 该方法和装置包括溶液的受控部分蒸发。 公开了用于控制部分蒸发程度和发生该蒸发的温度的方法，并且为了使该蒸发程度基本上恒定，即使溶剂流速和/或组成可以以受控或不受控制的方式变化。 这种“热喷涂”方法和装置允许溶剂基本上蒸发，以产生含有一部分未蒸发溶剂的超音速自由射流，作为夹带在射流中的液滴。 比溶剂挥发性低的溶质优先包含在液滴中。 公开了用于控制过程发生温度的方法，以防止溶质的不希望的化学改性（例如热解），并防止溶质过早蒸发。

公开(公告)号：US3888107A

公开(公告)日：1975-06-10

申请号：US27723672

申请日：1972-08-02

Applicant: DOW CHEMICAL CO

Inventor： LANGER HORST G ,  AYERS EARL D

IPC: G01N25/48 ,  H01J49/04 ,  G01N25/00

CPC classification number: H01J49/0422 ,  G01N25/4866 ,  H01J49/0486

Abstract: This invention relates to a thermal analysis cell which is capable of supplying meaningful data in a high vacuum which is particularly useful for operations within a mass spectrometer or similar instrument which allows the heating of samples within the confinement of the mass spectrometer vacuum or within the ion source and has means for withdrawal from or addition to the cell of gases or vaporized materials. The cell comprises a silver block to facilitate achieving uniform heat throughout the cell. The silver block has a capped end having an aperture therein. The block is insulated against the push-through shaft by a section of boron nitride which is an excellent thermal insulator. The silver cell is equipped with well(s) containing control and reference temperature sensors. A third and larger well is designed to contain the sample. Inlet and outlet passages are provided through the block to facilitate gas or vapor movement in the capped area. The sample itself is loaded into a glass or metal capillary and pushed into the well and onto a needle which is coupled to a thermocouple temperature sensor assembly.

Abstract translation: 本发明涉及一种能够在高真空中提供有意义的数据的热分析单元，其特别适用于质谱仪或类似仪器内的操作，该仪器允许在质谱仪真空限制或离子内进行样品加热 来源，并且具有从气体或蒸发材料的细胞中排出或添加的装置。 该电池包括银块以便于在整个电池中实现均匀的热量。 银块具有在其中具有孔的封端。 该块通过一部分优异的绝热体的氮化硼部分与穿通轴绝缘。 银电池配有包含控制和参考温度传感器的井。 第三个和更大的井被设计为容纳样品。 通过该块提供入口和出口通道，以便于在封盖区域内进行气体或蒸气运动。 将样品本身装载到玻璃或金属毛细管中并推入孔中并连接到耦合到热电偶温度传感器组件的针上。

公开(公告)号：US20160086784A1

公开(公告)日：2016-03-24

申请号：US14826388

申请日：2015-08-14

Applicant: Bruker Daltonik GmbH

Inventor： Andreas BREKENFELD ,  Martin ENGEL

IPC: H01J49/04 ,  H01J49/10

CPC classification number: H01J49/0486 ,  C03B19/12 ,  C04B35/14 ,  H01J49/0422 ,  H01J49/044 ,  H01J49/045 ,  H01J49/0477 ,  H01J49/10 ,  Y02P40/57

Abstract: The invention relates to an ionization chamber for connection to a mass spectrometer. The ionization chamber has a temperature-control block with a gas inlet and a gas channel which starts at the gas inlet and leads into a gas outlet. A temperature-control device is positioned along the gas channel and ensures that a gas flowing in the gas channel is brought to a specific temperature, i.e. it is heated or cooled, before it enters the ionization chamber. The temperature-control block has a formed part into which a structure of the gas channel is incorporated and which is fabricated by means of a sol-gel process, for example out of a glass or ceramic material.

Abstract translation: 本发明涉及一种用于连接到质谱仪的电离室。 电离室具有温度控制块，其具有气体入口和气体通道，其从气体入口开始并导入气体出口。 温度控制装置沿着气体通道定位，并且确保在气体通道中流动的气体在进入电离室之前被带到特定温度，即被加热或冷却。 温度控制块具有形成部分，其中结合有气体通道的结构，并且其通过溶胶 - 凝胶法制造，例如由玻璃或陶瓷材料制成。

公开(公告)号：US4999493A

公开(公告)日：1991-03-12

申请号：US514658

申请日：1990-04-24

Applicant: Mark Allen ,  Ivor A. S. Lewis

Inventor： Mark Allen ,  Ivor A. S. Lewis

IPC: G01N30/72 ,  H01J49/04

CPC classification number: H01J49/165 ,  G01N30/7266 ,  G01N30/7273 ,  H01J49/044 ,  H01J49/0486

Abstract: Improved techniques are provided for forming ionized molecules from electrosprayed droplets for analysis by a mass spectrometer. A high voltage is applied to a capillary tube for spraying droplets at substantially atmospheric pressure or above, and the electrosprayed droplets contain sample solute of interest and solvent. The electrosprayed droplets are passed into an ion generating chamber which is maintained at a pressure in the range of from 0.2 Torr to 10 Torr. The walls of the ion generating chamber are controllably heated to a temperature which will desolvate the droplets and produce ionized molecules of interest for analysis by the mass spectrometer. The electrospray technique does not rely upon a countercurrent heated gas flow, and provides a particularly simple and inexpensive means to couple electrospray ionization to either quadrupole or magnetic mass analyzers.

Abstract translation: 提供了用于从电喷雾液滴形成离子化分子以进行质谱分析的改进技术。 将高电压施加到用于在基本上大气压以上喷雾液滴的毛细管，并且电喷雾的液滴含有目标溶剂和溶剂。 电喷雾的液滴进入离子产生室，其保持在0.2托至10托的压力范围内。 离子发生室的壁被可控地加热到将使液滴脱溶质并产生离子化分子的温度，由质谱仪分析。 电喷雾技术不依赖于逆流加热的气流，并且提供了将电喷雾离子化耦合到四极杆或磁性质量分析器的特别简单和便宜的手段。

公开(公告)号：US4861989A

公开(公告)日：1989-08-29

申请号：US163060

申请日：1988-03-02

Applicant: Marvin L. Vestal ,  Calvin R. Blakley ,  Gordon J. Fergusson

Inventor： Marvin L. Vestal ,  Calvin R. Blakley ,  Gordon J. Fergusson

IPC: G01N30/30 ,  G01N30/32 ,  G01N30/72 ,  H01J49/04 ,  H01J49/10

CPC classification number: H01J49/049 ,  G01N30/7253 ,  H01J49/0445 ,  H01J49/0486 ,  G01N2030/3038 ,  G01N2030/3053 ,  G01N30/32

Abstract: This disclosure is concerned with method and apparatus for vaporizing liquid solutions in order to detect, quantitate, and/or determine physical or chemical properties of samples present in liquid solution. Mixtures may be separated by an on-line liquid chromatographic column and the methods used for detection, quantitation, indentification, and/or determination of chemical and physical properties include mass spectrometry, photoionization, flame ionization, electron capture, optical photometry, including UV, visible, and IR regions of the spectrum, light scattering, light emission, atomic absorption, and any other technique suitable for detecting or analyzing molecules or particles in a gaseous or vacuum environment. The method and apparatus involves controlled partial vaporization of the solution. Methods are disclosed for controlling the degree of partial vaporization and the temperature at which this vaporization occurs, and for maintaining this degree of vaporization essentially constant even though the solvent flow rate and/or composition may vary in either a controlled or an uncontrolled fashion. This "thermospray" method and apparatus allows the solvent to be substantially vaporized to produce supersonic free jet containing a fraction of unvaporized solvent as liquid droplets entrained in the jet. Solutes which are less volatile than the solvent are preferentially contained in the droplets. Methods are diGOVERNMENT SUPPORTThe invention described herein was made in the course of work under a grant or award from the Department of Health, Education, and Welfare.

Abstract translation: 本公开涉及用于蒸发液体溶液以便检测，定量和/或确定液体溶液中存在的样品的物理或化学性质的方法和装置。 混合物可以通过在线液相色谱柱分离，用于检测，定量，鉴定和/或测定化学和物理性质的方法包括质谱法，光离子化，火焰离子化，电子捕获，光学光度法，包括UV， 可见光和红外光谱区域，光散射，发光，原子吸收以及适用于在气态或真空环境中检测或分析分子或颗粒的任何其他技术。 该方法和装置包括溶液的受控部分蒸发。 公开了用于控制部分蒸发程度和发生该蒸发的温度的方法，并且为了使该蒸发程度基本上恒定，即使溶剂流速和/或组成可以以受控或不受控制的方式变化。 这种“热喷涂”方法和装置允许溶剂基本上蒸发以产生含有一部分未蒸发溶剂的超音速自由射流，作为夹带在射流中的液滴。 比溶剂挥发性低的溶质优先包含在液滴中。 公开了用于控制该过程发生温度的方法，以防止溶质的不希望的化学改性（例如，热解）和防止溶质过早汽化。

公开(公告)号：US3667279A

公开(公告)日：1972-06-06

申请号：US3667279D

申请日：1969-10-08

Applicant: DOW CHEMICAL CO

Inventor： LANGER HORST G

IPC: G01N25/00 ,  H01J49/04

CPC classification number: H01J49/0486 ,  G01N25/00

Abstract: This invention relates to a thermal analysis cell which is capable of supplying meaningful data in a high vacuum and which is particularly useful for operations within a mass spectrometer or similar instrument which allows the heating of samples within the confinement of the mass spectrometer vacuum or adjacent to the ion source. The cell comprises a silver block to guarantee uniform heat throughout the cell. It is insulated against the push-through shaft by a section of boron nitride, which is an excellent thermal insulator, and by sapphire or alumina, for example. The silver cell is equipped with two equal temperature sensing wells containing sample and reference temperature sensing means. A third and usually smaller well, designed to contain the block temperature sensing means, is usually provided. The sample itself is loaded into a metal cup which is secured to its well, and which contacts the temperature sensing means. A similar cup, usually containing non-reactive material, is inserted in the reference well and contacts its temperature sensing means, usually a thermocouple. The cell assembly has a detachable temperature sensing head part.

Abstract translation: 本发明涉及一种能够在高真空中提供有意义的数据的热分析单元，其特别适用于质谱仪或类似仪器内的操作，该仪器允许在质谱仪的限制范围内加热样品或真空 离子源。 该电池包括银块以保证整个电池均匀的热量。 例如，通过一部分氮化硼（其是优异的绝热体）和蓝宝石或氧化铝与穿通轴绝缘。 银电池配备有两个等温感测井，其中包含样品和参考温度检测装置。 通常提供设计成容纳块温度检测装置的第三和通常较小的孔。 样品本身装载到金属杯中，该金属杯固定到其井上，并与温度感测装置接触。 通常含有非反应性材料的类似的杯子插入参考孔中并接触其温度感测装置，通常是热电偶。 电池组件具有可拆卸的温度感测头部。

公开(公告)号：US3667278A

公开(公告)日：1972-06-06

申请号：US3667278D

申请日：1969-10-08

Applicant: DOW CHEMICAL CO

Inventor： LANGER HORST G ,  KARLE FRANKLIN J ,  AYERS EARL D

IPC: G01N25/48 ,  H01J49/04 ,  G01N25/00

CPC classification number: H01J49/0486 ,  G01N25/4866

Abstract: This invention relates to a thermal analysis cell which is capable of supplying meaningful data in a high vacuum and which is particularly useful for operations within a mass spectrometer or similar instrument which allows the heating of samples within the confinement of the mass spectrometer vacuum or adjacent to the ion source. The cell comprises a silver block to guarantee uniform heat throughout the cell. It is insulated against the push-through shaft by a section of boron nitride, which is an excellent thermal insulator, and by sapphire or alumina, for example. The silver cell is equipped with two equal temperature sensing wells containing sample and reference temperature sensing means. The sample itself is loaded into a metal cup which is usually secured to its well, and which contacts the temperature sensing means. A similar cup, usually containing non-reactive material, is inserted in the reference well and contacts its temperature sensing means, usually thermocouple. The cell assembly has a detachable temperature sensing head part. External means are provided for utilizing the output of the reference temperature sensing element for use in controlling the heating of the cell.

Abstract translation: 本发明涉及一种能够在高真空中提供有意义的数据的热分析单元，其特别适用于质谱仪或类似仪器内的操作，该仪器允许在质谱仪的限制范围内加热样品或真空 离子源。 该电池包括银块以保证整个电池均匀的热量。 例如，通过一部分氮化硼（其是优异的绝热体）和蓝宝石或氧化铝与穿通轴绝缘。 银电池配备有两个等温感测井，其中包含样品和参考温度检测装置。 样品本身被装载到金属杯中，金属杯通常固定在其井上，并与温度感测装置接触。 通常含有非反应性材料的类似的杯子插入参考孔中并接触其温度感测装置，通常是热电偶。 电池组件具有可拆卸的温度感测头部。 提供外部装置以利用参考温度感测元件的输出来用于控制电池的加热。