US3633027A - Mass spectrometer connected to a gap chromatograph through a valved molecule separator - Google Patents
Mass spectrometer connected to a gap chromatograph through a valved molecule separator Download PDFInfo
- Publication number
- US3633027A US3633027A US23715A US3633027DA US3633027A US 3633027 A US3633027 A US 3633027A US 23715 A US23715 A US 23715A US 3633027D A US3633027D A US 3633027DA US 3633027 A US3633027 A US 3633027A
- Authority
- US
- United States
- Prior art keywords
- separator
- stage
- mass spectrometer
- ion source
- nozzle
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 22
- 238000009792 diffusion process Methods 0.000 description 5
- 238000003780 insertion Methods 0.000 description 3
- 230000037431 insertion Effects 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000003446 memory effect Effects 0.000 description 1
- RETIMRUQNCDCQB-UHFFFAOYSA-N mepivacaine hydrochloride Chemical compound Cl.CN1CCCCC1C(=O)NC1=C(C)C=CC=C1C RETIMRUQNCDCQB-UHFFFAOYSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
- G01N30/7293—Velocity or momentum separators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0422—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for gaseous samples
Definitions
- GASCHROMATO GRAPH References Cited UNITED STATES PATENTS 3,471,692 10/ l 969 Llewellyn Q. 250/419 G 3,080,754 3/1963 Johnson 250/419 G FOREIGN PATENTS 221,621 7/1968 Sweden 250/419 G Primary ExaminerJames W. Lawrence Assistant Examiner-C. E. Church Attorney-Christen & Sabol AISTRAC'I: An instrument for analyzing organic chemical compounds is provided. The instrument comprises a gas chromatograph which via a molecule separator is connected to the ion source of a mass spectrometer. The separator consists of a number of series connected evacuating stages, each stage being connected to a vacuum pump. Each stage is provided with an input jet nozzle and a coaxial output nozzle, a slide being insertable between these nozzles in the first stage so as to make it possible to switch off the flow through the separator.
- the present invention relates to an instrument for analyzing organic chemical compounds, the instrument comprising a gas chromatograph, a molecule separator and a mass spectrometer, the molecule separator being connected between the output of the gas chromatograph and the input of the ion source of the mass spectrometer, the separator including at least one separating stage consisting of an evacuation chamber connected to a vacuum pump, a jet input nozzle via which molecules in gas phase are supplied from the gas chromatograph and an output nozzle coaxial with the jet nozzle.
- so called molecule separators are used for separating a carrier gas, usually helium, from the specimen to be analyzed and for reducing the pressure in the ion source of the mass spectrometer.
- Becker-Ryhage-Separator differs from different kinds of separators from the so called Becker-Ryhage-Separator however having several advantages in comparison to the others.
- the enrichment is high, the loss of specimen is small, the dead volume is small and the memory effect is negligible.
- the Becker-Ryhage-Separator is generally made in two stages. In the first stage the pressure is reduced to 0.001 mm. Hg by an oil diffusion pump. In this way approximately 99 percent of the carrier gas is evacuated while at least 75 percent of the specimen remains. The pressure will then be further reduced at the ion source of the mass spectrometer.
- FIG. 1 shows a two-stage separator according to the invention provided with a switching-off arrangement in the form of a slide;
- FIG. 2 shows another embodiment of a two-stage separator according to the invention in which the second separator stage has been combined with the ion source.
- reference 1 denotes a mounting flange for connection of a gas chromatograph G
- reference 2 denotes the first separator stage
- reference 3 denotes the second separator stage
- reference 4 denotes the mounting flange oflthe ion source of the mass spectrometer M.
- the input jet nozzle of the separator stages are denoted 5a and 5b respectively and the output nozzles are denoted 6a and 6!: respectively.
- Reference 7 denotes the slide by means of which the gas flow can be switched off or at least be prevented from passing into the second separator stage.
- Reference 8 denotes a bellows which controls the position of the slide 7
- reference 9 denotes a knob for moving the bellows.
- the slide can be set into two positions and 11b, which positions are adjusted by means of a screw 10.
- References 12 and 13 denote connections leading to a mechanical vacuum pump and an oil diffusion pump respectively.
- the slide 7 is inserted between the nozzles 5a and 6a.
- the distance between these nozzles these about 0.1 mm. and thus the slide should have this dimension.
- the nozzle 5a does also have a diameter of about 0.1 mm.
- the slide does not necessarily have to seal this nozzle completely but a small leakage :into the separator housing can be permitted. It has turned out in practice that in spite of this leakage the mechanical vacuum pump provides a pressure which is sufficiently low for making the oil diffusion pump work and for not making it necessary to have the ion source switched off. Even if the pressure in the first separator stage 2 is as much as 1 mm. Hg, instead of the normal value 0.01 mm. Hg, the system works satisfactory. Thus the pumps do not have to be switched off.
- the slide 7 can be shaped so as to seal only the output nozzle 6a.
- the slide 7 could be provided with a slot in the surface turned to the input nozzle 5a. This shaping of the slide is suitable when a gas flow through only the gas chromatograph column is wanted, for instance after mounting the column.
- the dead volume after the separator is reduced considerably.
- the volume of the tap between the separator and the ion source is approximately 0.5 ml. and the connecting pipes have a volume of approximately the same size. If these values are compared with the area of the channel through the separator (0.8 mm?) and the area of the nozzle (0.008 mm?) the significanceof the reduced dead volume is understood.
- a reduced volume after the separator means less than a reduced volume before the separator, the pressure conditions being completely different, but a reduced volume is still desirable.
- the insertion of some sort of tap before the separator is not suitable as this will increase the dead volume.
- Each person skilled within this field is aware of the drawbacks of such an arrangement, especially when capillary columns are used in the gas chromatograph.
- a tap mounted before the separator further makes it more difficult to remove the flange for cleaning the nozzle 5a.
- the other nozzles do not have to be cleaned so often as the pressure and thus the fouling is less at these nozzles.
- the switching ofi' means consist of a slide.
- the slide can of course be shaped in different ways and the insertion of the slide between the nozzles of the separator can be arranged in dif ferent ways. If only a sealing of the output nozzle is wanted it might thus be suitable to make the top of the output nozzle radially movable.
- FIG. 2 a new way of connecting the separator to a mass spectrometer is shown.
- This connection is made possible by using the present invention.
- the references denote the same members as in FIG. 1, the difference being that reference 15 denotes the connection leading to the ion source and references 14a and Nb denote the nozzle of the second separator stage.
- Reference 16 denotes the connection of the high vacuum system which in this case is the same for the second separator stage and the ion source housing. in this embodiment the dead volume is considerably decreased in comparison with the embodiment of FIG. 1. On the other hand the flexibility will be somewhat reduced.
- An instrument for analyzing organic-chemical compounds comprising a gas chromatograph, a molecule separator and a mass spectrometer having a housing, the molecule separator being connected between the output of the gas chromatograph and the input of the ion source of the mass spectrometer, the molecule separator including at least one separating stage consisting of an evacuation chamber connected to a vacuum pump, a jet input nozzle from which molecules in gas phase are supplied from the gas chromatograph and an output nozzle coaxial with the jet nozzle, characterized in that the molecule separator comprises a slide element, and means mounting said slide element for movement in a direction transverse to the axis of said input of output nozzles so as to be inserted between the jet nozzle and the output nozzle to close the space therebetween and cut off the gas flow through the molecule separator and to be movable to another position to permit said gas flow.
- An instrument according to claim 1 characterized in that the surface of said slide element is shaped to seal the output nozzle and to provide space for leakage at the jet input nozzle when the slide element is in an inserted position.
- An instrument according to claim 1 characterized in, that the number of stages is at least two, the last stage being combined with the housing of the ion source.
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SE05621/69A SE325726B (enrdf_load_stackoverflow) | 1969-04-21 | 1969-04-21 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3633027A true US3633027A (en) | 1972-01-04 |
Family
ID=20266851
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US23715A Expired - Lifetime US3633027A (en) | 1969-04-21 | 1970-03-30 | Mass spectrometer connected to a gap chromatograph through a valved molecule separator |
Country Status (4)
Country | Link |
---|---|
US (1) | US3633027A (enrdf_load_stackoverflow) |
FR (1) | FR2045486A5 (enrdf_load_stackoverflow) |
GB (1) | GB1267121A (enrdf_load_stackoverflow) |
SE (1) | SE325726B (enrdf_load_stackoverflow) |
Cited By (29)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3842266A (en) * | 1973-04-11 | 1974-10-15 | Us Air Force | Atmospheric sampling probe for a mass spectrometer |
JPS5011582U (enrdf_load_stackoverflow) * | 1973-05-28 | 1975-02-06 | ||
JPS5047697A (enrdf_load_stackoverflow) * | 1973-08-27 | 1975-04-28 | ||
JPS5063489U (enrdf_load_stackoverflow) * | 1973-10-12 | 1975-06-09 | ||
US4016421A (en) * | 1975-02-13 | 1977-04-05 | E. I. Du Pont De Nemours And Company | Analytical apparatus with variable energy ion beam source |
US4298795A (en) * | 1978-09-08 | 1981-11-03 | Japan Spectroscopic Co. Ltd | Method and apparatus for introducing samples to a mass spectrometer |
US4629478A (en) * | 1984-06-22 | 1986-12-16 | Georgia Tech Research Corporation | Monodisperse aerosol generator |
US4687929A (en) * | 1984-06-22 | 1987-08-18 | Georgia Tech Research Corporation | Monodisperse aerosol generator |
US4762995A (en) * | 1984-06-22 | 1988-08-09 | Georgia Tech Research Corporation | Monodisperse aerosol generator |
US4791292A (en) * | 1986-04-24 | 1988-12-13 | The Dow Chemical Company | Capillary membrane interface for a mass spectrometer |
US4924097A (en) * | 1984-06-22 | 1990-05-08 | Georgia Tech Rss. Corp | Monodisperse aerosol generator for use with infrared spectrometry |
US5024952A (en) * | 1989-06-26 | 1991-06-18 | Union Carbide Chemicals And Plastics Technology Corporation | Method for obtaining analytes from liquid menstrua for analysis |
US5137553A (en) * | 1990-03-02 | 1992-08-11 | Sge International Pty. Ltd. | Molecular jet separator |
WO1997036177A1 (de) * | 1996-03-27 | 1997-10-02 | Balzers Aktiengesellschaft | Anordnung zum verbinden eines tiefdruckeinganges eines gasanalysegerätes |
US20070205362A1 (en) * | 2006-03-03 | 2007-09-06 | Ionsense, Inc. | Sampling system for use with surface ionization spectroscopy |
US20080067348A1 (en) * | 2006-05-26 | 2008-03-20 | Ionsense, Inc. | High resolution sampling system for use with surface ionization technology |
US20080087812A1 (en) * | 2006-10-13 | 2008-04-17 | Ionsense, Inc. | Sampling system for containment and transfer of ions into a spectroscopy system |
US20080191412A1 (en) * | 2007-02-09 | 2008-08-14 | Primax Electronics Ltd. | Automatic document feeder having mechanism for releasing paper jam |
US20090090858A1 (en) * | 2006-03-03 | 2009-04-09 | Ionsense, Inc. | Sampling system for use with surface ionization spectroscopy |
US8207497B2 (en) | 2009-05-08 | 2012-06-26 | Ionsense, Inc. | Sampling of confined spaces |
US8440965B2 (en) | 2006-10-13 | 2013-05-14 | Ionsense, Inc. | Sampling system for use with surface ionization spectroscopy |
US8754365B2 (en) | 2011-02-05 | 2014-06-17 | Ionsense, Inc. | Apparatus and method for thermal assisted desorption ionization systems |
US8901488B1 (en) | 2011-04-18 | 2014-12-02 | Ionsense, Inc. | Robust, rapid, secure sample manipulation before during and after ionization for a spectroscopy system |
US9337007B2 (en) | 2014-06-15 | 2016-05-10 | Ionsense, Inc. | Apparatus and method for generating chemical signatures using differential desorption |
US9899196B1 (en) | 2016-01-12 | 2018-02-20 | Jeol Usa, Inc. | Dopant-assisted direct analysis in real time mass spectrometry |
US10636640B2 (en) | 2017-07-06 | 2020-04-28 | Ionsense, Inc. | Apparatus and method for chemical phase sampling analysis |
US10825673B2 (en) | 2018-06-01 | 2020-11-03 | Ionsense Inc. | Apparatus and method for reducing matrix effects |
US11424116B2 (en) | 2019-10-28 | 2022-08-23 | Ionsense, Inc. | Pulsatile flow atmospheric real time ionization |
US11913861B2 (en) | 2020-05-26 | 2024-02-27 | Bruker Scientific Llc | Electrostatic loading of powder samples for ionization |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3080754A (en) * | 1961-07-10 | 1963-03-12 | Charles Y Jolmson | Direct method of measuring neutral gas temperatures |
US3471692A (en) * | 1967-03-27 | 1969-10-07 | Varian Associates | Gas analyzer system employing a gas chromatograph and a mass spectrometer with a gas switch therebetween |
-
1969
- 1969-04-21 SE SE05621/69A patent/SE325726B/xx unknown
-
1970
- 1970-03-30 US US23715A patent/US3633027A/en not_active Expired - Lifetime
- 1970-04-13 GB GB1267121D patent/GB1267121A/en not_active Expired
- 1970-04-20 FR FR7014215A patent/FR2045486A5/fr not_active Expired
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3080754A (en) * | 1961-07-10 | 1963-03-12 | Charles Y Jolmson | Direct method of measuring neutral gas temperatures |
US3471692A (en) * | 1967-03-27 | 1969-10-07 | Varian Associates | Gas analyzer system employing a gas chromatograph and a mass spectrometer with a gas switch therebetween |
Cited By (70)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3842266A (en) * | 1973-04-11 | 1974-10-15 | Us Air Force | Atmospheric sampling probe for a mass spectrometer |
JPS5011582U (enrdf_load_stackoverflow) * | 1973-05-28 | 1975-02-06 | ||
JPS5047697A (enrdf_load_stackoverflow) * | 1973-08-27 | 1975-04-28 | ||
JPS5063489U (enrdf_load_stackoverflow) * | 1973-10-12 | 1975-06-09 | ||
US4016421A (en) * | 1975-02-13 | 1977-04-05 | E. I. Du Pont De Nemours And Company | Analytical apparatus with variable energy ion beam source |
US4298795A (en) * | 1978-09-08 | 1981-11-03 | Japan Spectroscopic Co. Ltd | Method and apparatus for introducing samples to a mass spectrometer |
US4629478A (en) * | 1984-06-22 | 1986-12-16 | Georgia Tech Research Corporation | Monodisperse aerosol generator |
US4687929A (en) * | 1984-06-22 | 1987-08-18 | Georgia Tech Research Corporation | Monodisperse aerosol generator |
US4762995A (en) * | 1984-06-22 | 1988-08-09 | Georgia Tech Research Corporation | Monodisperse aerosol generator |
US4924097A (en) * | 1984-06-22 | 1990-05-08 | Georgia Tech Rss. Corp | Monodisperse aerosol generator for use with infrared spectrometry |
US4791292A (en) * | 1986-04-24 | 1988-12-13 | The Dow Chemical Company | Capillary membrane interface for a mass spectrometer |
US5024952A (en) * | 1989-06-26 | 1991-06-18 | Union Carbide Chemicals And Plastics Technology Corporation | Method for obtaining analytes from liquid menstrua for analysis |
US5137553A (en) * | 1990-03-02 | 1992-08-11 | Sge International Pty. Ltd. | Molecular jet separator |
WO1997036177A1 (de) * | 1996-03-27 | 1997-10-02 | Balzers Aktiengesellschaft | Anordnung zum verbinden eines tiefdruckeinganges eines gasanalysegerätes |
US6310340B1 (en) | 1996-03-27 | 2001-10-30 | Unaxis Balzers Aktiengesellschaft | Arrangement for connecting a low-pressure inlet of a gas analyzer |
US20070205362A1 (en) * | 2006-03-03 | 2007-09-06 | Ionsense, Inc. | Sampling system for use with surface ionization spectroscopy |
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EP1992005A4 (en) * | 2006-03-03 | 2010-02-03 | Ionsense Inc | SAMPLING SYSTEM FOR USE WITH SURFACE IONIZATION SPECTROSCOPY |
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US7777181B2 (en) | 2006-05-26 | 2010-08-17 | Ionsense, Inc. | High resolution sampling system for use with surface ionization technology |
US20080067358A1 (en) * | 2006-05-26 | 2008-03-20 | Ionsense, Inc. | Apparatus for holding solids for use with surface ionization technology |
US8481922B2 (en) | 2006-05-26 | 2013-07-09 | Ionsense, Inc. | Membrane for holding samples for use with surface ionization technology |
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US8440965B2 (en) | 2006-10-13 | 2013-05-14 | Ionsense, Inc. | Sampling system for use with surface ionization spectroscopy |
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US9899196B1 (en) | 2016-01-12 | 2018-02-20 | Jeol Usa, Inc. | Dopant-assisted direct analysis in real time mass spectrometry |
US10636640B2 (en) | 2017-07-06 | 2020-04-28 | Ionsense, Inc. | Apparatus and method for chemical phase sampling analysis |
US10825673B2 (en) | 2018-06-01 | 2020-11-03 | Ionsense Inc. | Apparatus and method for reducing matrix effects |
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Also Published As
Publication number | Publication date |
---|---|
DE2014459B2 (de) | 1976-05-06 |
SE325726B (enrdf_load_stackoverflow) | 1970-07-06 |
GB1267121A (enrdf_load_stackoverflow) | 1972-03-15 |
DE2014459A1 (de) | 1970-11-05 |
FR2045486A5 (enrdf_load_stackoverflow) | 1971-02-26 |
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