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US3198001A - Connection between chromatographic column and valve system - Google Patents

Connection between chromatographic column and valve system Download PDF

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Publication number
US3198001A
US3198001A US268389A US26838963A US3198001A US 3198001 A US3198001 A US 3198001A US 268389 A US268389 A US 268389A US 26838963 A US26838963 A US 26838963A US 3198001 A US3198001 A US 3198001A
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United States
Prior art keywords
column
oven
valve system
union
connection
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Expired - Lifetime
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US268389A
Inventor
Charles R Ferrin
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Instrument Inc
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Instr Inc
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Priority to US268389A priority Critical patent/US3198001A/en
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Publication of US3198001A publication Critical patent/US3198001A/en
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    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • 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
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3046—Control of physical parameters of the fluid carrier of temperature temperature control of column inlet
    • 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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/30—Control of physical parameters of the fluid carrier of temperature
    • G01N2030/3084—Control of physical parameters of the fluid carrier of temperature ovens
    • 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
    • G01N30/60—Construction of the column
    • G01N30/6034—Construction of the column joining multiple columns
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T137/00—Fluid handling
    • Y10T137/6851—With casing, support, protector or static constructional installations
    • Y10T137/7036—Jacketed

Definitions

  • the present invention relates to connecting a chromatographic column with sample valves which are located in the controlled temperature of an oven.
  • Valve systems are used from which samples feed to a chromatographic column which have their temperature controlled in order to properly prepare the sample for introduction into the column. Also, electrical power has been used to heat the columns for their operation. In providing this connection between Valves and column, there are at least the problems of providing .a connection which is iluid tight, providing an electrical power connection for resistance-heating of the column and maintaining thermal stability for the sample .as the sample is transferred from the valve system 'to the column.
  • An object of the present invention is to provide thermal stability for a sample as the sample is transferred from a valve system to a chromatographic column, providing the sample without loss and providing connection to a source of electrical power.
  • the present invention contemplates a controlled oven having mounted therein a valve system for preparing a sample for insertion in a chromatographic column.
  • the body of thermal insulation is mounted adjacent the o e and a metallic union mounted on the body with a central passage therethrough.
  • a conduit is mechanically communicated with the union passage through the body of insulation and the conduit then led to the inside of the oven.
  • a tube for transport of the sample from the valve system to the column extends through the conduit to communicate with the union.
  • the invention further contemplates leads for electrical power extending through the body of thermal insulation to the union and electrically isolated from the valve system.
  • the drawing illustrates a sectioned elevation of a connection structure embodying the present invention to extend from an oven-heated valve system to a chromatographic column.
  • the drawing illustrates an oven structure 10, but the drawing does not shown the valve system mounted within the oven so the temperature of the system and the sample handled by the system will have its temperature controlled.
  • the source of heat for the oven, controls for the source, etc., are not shown.
  • the structure that is shown is -a portion of oven 10, provided with a lid 11 which is hinged at 12 to gain access to the inside of the oven.
  • a wall 13 of the oven is also partially shown, and on the outside of the oven wall a body 14 for thermal insulation is indicated.
  • the connection embodying the present invention is mounted within the thermal insulation body 14.
  • An opening 15 is provided through wall 13 for communication between the interior of oven and the insulation body 14.
  • a metallic cover plate 16 is provided for insulation body 14 and an access opening 17 provided through this plate. The connection of the present invention extends between openings and 17.
  • the body of a union 18 of selected size is mounted over access opening 17 in plate 16.
  • the body of the union is provided with a central passage which ex- 3,198,901 Patented Aug. 3, 1965 tends completely through the body.
  • the central passage is threaded at 19 to receive tube coupling 20.
  • a chromatographic column 21 is .sealed into coupling 20.
  • the junction between column 21 and coupling 20 is both fluid tight and electrically completed.
  • Tube 22 is extended up into coupling 20 for communication with column 21. Tube 22 also extends down through the insulation body 14, through opening 15 in wall 13 and into fluid communication with the valve system which is not shown.
  • Tubing 22 brings the sample to be analyzed from the valve system in oven 10 to column 21.
  • Tubing 22 is relatively long, extending from the interior of oven 10 to junction with column 21 in coupling 20.
  • One of the objects of the present invention is is to maintain the thermal stability of the sample within tubing 22.
  • a comparatively large conduit 23 is provided to sheathe the tubing 22, extending from union 18 through opening 15 in wall 13.
  • Conduit 23 is mechanically sealed to wall opening 15 by means of coupling structure 24, carried in the opening 15 of wall 13. Conduit 23 is, therefore, extended from coupling 24 .to union 18. This conduit 23 does not touch sample tubing 22, but provides ample volume about tub ing 22 for circulation of oven heat. The oven heat, conducted over substantially the complete length of tubing 22, maintains the tubing 22 thermally stable.
  • junction station 25 is provided bet-ween the oven-end of sample tubing 22 and the valve system.
  • Junction station 25 includes a special filled Teflon body 26 which is mounted on wall :13. Tube 22 is coupled to internal passage 27 of body 26. Station 25 provides fluid communication between tube 28, coming directly from the heated valve system, and sample tube 22. At the same time, body 25 maintains the two tubes electrically insulated from each other. Electrical power applied to directly heat column 21 will then not be shorted through the tube 28.
  • a source of electrical power is provided to heat column 21. This source of electrical power is not shown, however, lead 29 from the source is shown, extending through insulating body 14 to complete electrical connection with union 25) at 30. Through lead 29, the source of electrical power supplies the resistance-heating of column 21 while the thermally stable samples are fed to the column through tube 22.
  • a connection between the inlet valve system and column of a gas chromatograph including,
  • a metallic union mounted on the thermal insulation body and having an access opening therethrough in from external the insulation body to internal the insulation body
  • a conduit mechanically communicated with the internal end of the union and extending through the insulation body and into communication with the adjacent oven
  • a first tube communicated with the column through the union and extended through the conduit and into the oven, a second tube fluid communicated between the first tube and valve system and electrically insulated from the first tube,
  • connection system between the inlet valve system and column of a gas chromatograph including,
  • a metallic union mounted on thethermal insulation body and having an access opening therethrough from external the insulation body to internal the insulation body
  • conduit mounted on the internal end of the union and extending through the insulation body and into communication with the adjacent oven

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  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Sampling And Sample Adjustment (AREA)

Description

INVENTOR. CHARLES FERHIN BY dfl, L441 ATTORNEY C. R. FERRIN Aug. 3, 1965 CONNECTION BETWEEN CHROMATOGRAPHIC COLUMN AND VALVE SYSTEM Filed March 27, 1963 FROM VALVE SYSTEM gin-i 3,198,001 CONNECTION BETWEEN CHROMATGGRAPHIC COLUMN AND VALVE SYSTEM Charles R. Ferrin, Tulsa, Okla, assigns: to Instruments,
Inc., Tulsa, Okla, a corporation of Oklahoma Filed Mar. 27, 1963, Ser. No. 268,389 2 Claims. (Cl.73-23.1)
The present invention relates to connecting a chromatographic column with sample valves which are located in the controlled temperature of an oven.
Valve systems are used from which samples feed to a chromatographic column which have their temperature controlled in order to properly prepare the sample for introduction into the column. Also, electrical power has been used to heat the columns for their operation. In providing this connection between Valves and column, there are at least the problems of providing .a connection which is iluid tight, providing an electrical power connection for resistance-heating of the column and maintaining thermal stability for the sample .as the sample is transferred from the valve system 'to the column.
An object of the present invention is to provide thermal stability for a sample as the sample is transferred from a valve system to a chromatographic column, providing the sample without loss and providing connection to a source of electrical power.
The present invention contemplates a controlled oven having mounted therein a valve system for preparing a sample for insertion in a chromatographic column. The body of thermal insulation is mounted adjacent the o e and a metallic union mounted on the body with a central passage therethrough. A conduit is mechanically communicated with the union passage through the body of insulation and the conduit then led to the inside of the oven. A tube for transport of the sample from the valve system to the column extends through the conduit to communicate with the union.
The invention further contemplates leads for electrical power extending through the body of thermal insulation to the union and electrically isolated from the valve system.
Other objects, advantages and features of this invention will become apparent to one skilled in the art upon consideration of the written specification, appended claims, and attached drawings, wherein;
The drawing illustrates a sectioned elevation of a connection structure embodying the present invention to extend from an oven-heated valve system to a chromatographic column.
The drawing illustrates an oven structure 10, but the drawing does not shown the valve system mounted within the oven so the temperature of the system and the sample handled by the system will have its temperature controlled. The source of heat for the oven, controls for the source, etc., are not shown. The structure that is shown is -a portion of oven 10, provided with a lid 11 which is hinged at 12 to gain access to the inside of the oven.
A wall 13 of the oven is also partially shown, and on the outside of the oven wall a body 14 for thermal insulation is indicated. The connection embodying the present invention is mounted within the thermal insulation body 14.
An opening 15 is provided through wall 13 for communication between the interior of oven and the insulation body 14. A metallic cover plate 16 is provided for insulation body 14 and an access opening 17 provided through this plate. The connection of the present invention extends between openings and 17.
The body of a union 18 of selected size is mounted over access opening 17 in plate 16. In turn, the body of the union is provided with a central passage which ex- 3,198,901 Patented Aug. 3, 1965 tends completely through the body. On the external side of union body 18 the central passage is threaded at 19 to receive tube coupling 20.
A chromatographic column 21 is .sealed into coupling 20. The junction between column 21 and coupling 20 is both fluid tight and electrically completed.
The other, inner, end of the central passage of union 18 receives one end of a relatively small sample tubing 22. Tube 22 is extended up into coupling 20 for communication with column 21. Tube 22 also extends down through the insulation body 14, through opening 15 in wall 13 and into fluid communication with the valve system which is not shown.
Tubing 22 brings the sample to be analyzed from the valve system in oven 10 to column 21. Tubing 22 is relatively long, extending from the interior of oven 10 to junction with column 21 in coupling 20. One of the objects of the present invention is is to maintain the thermal stability of the sample within tubing 22. To maintain thermal stability, a comparatively large conduit 23 is provided to sheathe the tubing 22, extending from union 18 through opening 15 in wall 13.
Conduit 23 is mechanically sealed to wall opening 15 by means of coupling structure 24, carried in the opening 15 of wall 13. Conduit 23 is, therefore, extended from coupling 24 .to union 18. This conduit 23 does not touch sample tubing 22, but provides ample volume about tub ing 22 for circulation of oven heat. The oven heat, conducted over substantially the complete length of tubing 22, maintains the tubing 22 thermally stable.
A junction station is provided bet-ween the oven-end of sample tubing 22 and the valve system. Junction station 25 includes a special filled Teflon body 26 which is mounted on wall :13. Tube 22 is coupled to internal passage 27 of body 26. Station 25 provides fluid communication between tube 28, coming directly from the heated valve system, and sample tube 22. At the same time, body 25 maintains the two tubes electrically insulated from each other. Electrical power applied to directly heat column 21 will then not be shorted through the tube 28.
A source of electrical power is provided to heat column 21. This source of electrical power is not shown, however, lead 29 from the source is shown, extending through insulating body 14 to complete electrical connection with union 25) at 30. Through lead 29, the source of electrical power supplies the resistance-heating of column 21 while the thermally stable samples are fed to the column through tube 22.
From the foregoing it will be seen that this invention is one well adapted to attain all of the ends and objects hereinabove set forth, together with other advantages which are obvious and which are inherent to the apparatus.
It will be understood that certain features and subcombinations are of utility and may be employed without reference to other features and subcombinations. This is contemplated by and is within the scope of the claims.
As many possible embodiments may be made of the invention without departing from the scope thereof, it is to be understood that all matter herein set forth or shown in the accompanying drawings is to be interpreted as illustrative and not in a limiting sense.
The present invention having been described, what is claimed is:
1. A connection between the inlet valve system and column of a gas chromatograph, including,
an oven having a controlled intern-a1 temperature,
a thermal insulation body adjacent the oven,
a metallic union mounted on the thermal insulation body and having an access opening therethrough in from external the insulation body to internal the insulation body,
a chromatograph column mechanically communicated with the external end of the access opening of the union,-
, a conduit mechanically communicated with the internal end of the union and extending through the insulation body and into communication with the adjacent oven,
a first tube communicated with the column through the union and extended through the conduit and into the oven, a second tube fluid communicated between the first tube and valve system and electrically insulated from the first tube,
and an electrical power lead extended through the body of insulation and into electrical connection with the union for resistance heating of the column.
2. A connection system between the inlet valve system and column of a gas chromatograph, including,
an oven having a controlled internal temperature,
a thermal insulation body adjacent the oven,
a metallic union mounted on thethermal insulation body and having an access opening therethrough from external the insulation body to internal the insulation body,
a chromatograph column of selected size mounted on the external end of the access opening of the union,
a conduit mounted on the internal end of the union and extending through the insulation body and into communication with the adjacent oven,
a fluid connection bet-Ween the valve system and conduit which also electrically insulates between the valve system and conduit,
and an electrical power lead extended through the body of insulation to connect with the column to resistance-heat the column.
, References Cited by the Examiner UNITED STATES PATENTS 259,698 6/82 Magin l37575 2,963,898 12/60 Reynolds et al 7323 3,115,766 12/63 Winters 7323 OTHER REFERENCES Panchromatogr'aph, a publication of W. G. Pye & Co. Ltd., York Street, Cambridge, England, bulletin No. 150/ 5M/6.62/=F & I, published June 1962.
RICHARD C. QUEISSER, Primary Examiner.
ROBERT L. EVANS, Examiner.

Claims (1)

  1. 2. A CONNECTION SYSTEM BETWEEN THE INLET VALVE SYSTEM AND COLUMN OF A GAS CHROMATOGRAPH, INCLUDING, AN OVEN HAVING A CONTROLLED INTERNAL TEMPERATURE, A THERMAL INSULATION BODY ADJACENT THE OVEN, A METALLIC UNION MOUNTED ON THE THERMAL INSULATION BODY AND HAVING AN ACCESS OPENING THERETHROUGH FOR EXTERNAL THE INSULATION BODY TO INTERNAL THE INSULATION BODY, A CHROMATOGRAPH COLUMN OF SELECTED SIZE MOUNTED ON THE EXTERNAL END OF THE ACCESS OPENING OF THE UNION, A CONDUIT MOUNTED ON THE INTERNAL END OF THE UNION AND EXTENDING THROUGH THE INSULATION BODY AND INTO COMMUNICATION WITH THE ADJACENT OVEN, A FLUID CONNECTION BETWEEN THE VALVE SYSTEM AND CONDUIT WHICH ALSO ELECTRICALLY INSULATES BETWEEN THE VALVE SYSTEM AND CONDUIT, AND AN ELECTRICAL POWER LEAD EXTENDED THROUGH THE BODY OF INSULATION TO CONNECT WITH THE COLUMN TO RESISTANCE-HEAT THE COLUMN.
US268389A 1963-03-27 1963-03-27 Connection between chromatographic column and valve system Expired - Lifetime US3198001A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3309504A (en) * 1964-08-24 1967-03-14 Combustion Eng System for heating chromatographic columns
US3366149A (en) * 1965-07-15 1968-01-30 Varian Aerograph Injection system for gas chromatography
US4271703A (en) * 1979-10-03 1981-06-09 Phillips Petroleum Company High temperature sampling system for liquid chromatography
US4630637A (en) * 1984-09-15 1986-12-23 Kernforschungsanlage Julich Gmbh Gas flow regulator for gases with condensable components
US4735259A (en) * 1984-02-21 1988-04-05 Hewlett-Packard Company Heated transfer line for capillary tubing
WO1991018288A1 (en) * 1990-05-18 1991-11-28 Martin Marietta Energy Systems, Inc. Gas chromatograph-mass spectrometer (gc/ms) system for quantitative analysis of reactive chemical compounds
WO1997014957A1 (en) * 1995-10-16 1997-04-24 Thermedics Detection Inc. High speed gas chromatography
EP1837650A1 (en) * 2006-03-24 2007-09-26 Agilent Technologies, Inc. Thermally conductive sheath for fluid conduit

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US259698A (en) * 1882-06-20 Beer-faucet
US2963898A (en) * 1957-08-27 1960-12-13 Central Scientific Co Gas chromatography unit
US3115766A (en) * 1957-11-22 1963-12-31 Standard Oil Co Gas chromatography apparatus

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US259698A (en) * 1882-06-20 Beer-faucet
US2963898A (en) * 1957-08-27 1960-12-13 Central Scientific Co Gas chromatography unit
US3115766A (en) * 1957-11-22 1963-12-31 Standard Oil Co Gas chromatography apparatus

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3309504A (en) * 1964-08-24 1967-03-14 Combustion Eng System for heating chromatographic columns
US3366149A (en) * 1965-07-15 1968-01-30 Varian Aerograph Injection system for gas chromatography
US4271703A (en) * 1979-10-03 1981-06-09 Phillips Petroleum Company High temperature sampling system for liquid chromatography
US4735259A (en) * 1984-02-21 1988-04-05 Hewlett-Packard Company Heated transfer line for capillary tubing
US4630637A (en) * 1984-09-15 1986-12-23 Kernforschungsanlage Julich Gmbh Gas flow regulator for gases with condensable components
WO1991018288A1 (en) * 1990-05-18 1991-11-28 Martin Marietta Energy Systems, Inc. Gas chromatograph-mass spectrometer (gc/ms) system for quantitative analysis of reactive chemical compounds
US5083450A (en) * 1990-05-18 1992-01-28 Martin Marietta Energy Systems, Inc. Gas chromatograph-mass spectrometer (gc/ms) system for quantitative analysis of reactive chemical compounds
AU654485B2 (en) * 1990-05-18 1994-11-10 Martin Marietta Energy Systems, Inc. Gas chromatograph-mass spectrometer (GC/MS) system for quantitative analysis of reactive chemical compounds
WO1997014957A1 (en) * 1995-10-16 1997-04-24 Thermedics Detection Inc. High speed gas chromatography
US5808178A (en) * 1995-10-16 1998-09-15 Thermedics Detection Inc. High speed gas chromatography
EP1837650A1 (en) * 2006-03-24 2007-09-26 Agilent Technologies, Inc. Thermally conductive sheath for fluid conduit

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