US3656277A - Method and device for gas chromatography - Google Patents

Method and device for gas chromatography Download PDF

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Publication number
US3656277A
US3656277A US22184A US3656277DA US3656277A US 3656277 A US3656277 A US 3656277A US 22184 A US22184 A US 22184A US 3656277D A US3656277D A US 3656277DA US 3656277 A US3656277 A US 3656277A
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United States
Prior art keywords
septum
channel
column
gas
separating
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Expired - Lifetime
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US22184A
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English (en)
Inventor
Peter Slingerland
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Nederlandse Organisatie voor Toegepast Natuurwetenschappelijk Onderzoek TNO
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Nederlandse Organisatie voor Toegepast Natuurwetenschappelijk Onderzoek TNO
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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
    • G01N30/18—Injection using a septum or microsyringe

Definitions

  • ABSTRACT An improved method and device for gas chromatography in which the ill effect of septum-bleeding is eliminated by allowing a small stream of carrier gas to leak out of the top section of the column into the atmosphere at a location between the septum and the main stream of carrier gas.
  • the invention relates to a method for the separation of the substances present in a mixture, in which method a small quantity of the mixture is introduced into the separating column of a gas chromatograph by means of a needle syringe, whose needle is pierced through the septum which consists of an elastic material and which seals the top section of the column, and in which method the mixture injected is carried through the separating column with the aid of a carrier gas stream introduced at the top section of the column.
  • This method is the normal use of conventional devices for gas chromatography and is generally known in the art. It is also known in the art that in operating with a programmed proceeding of the column temperature and sensitive detectors a part of the measuring result may be composed of signals not originating from the substances in the sample injected. Such signals may very much interfere with the interpretation of the chromatogram.
  • the signals not related to the sample are often effected by substances emanating from the septum. Those cumulate at the top section of the column when the latter is rapidly being cooled at the end of a temperature programme and at a following temperature programme they behave like a sample injected.
  • the invention is characterized in that the gas stream is carried in and through the column in such a way that a section of the column comprising the septum is situated outside the gas stream and in that via this section of the column a small part of the gas stream is discharged from the column.
  • the amount of the part of the gas stream introduced that is immediately discharged at the top section of the column together with substances, if any, emanating from the septum, is not essential. On discharging quantities of l to ml/min, fully satisfactory results were obtained. Besides, the discharge of gas has no effect whatsoever on the operation of the gas chromatograph.
  • the invention also relates to a gas chromatograph for the implementation of the method described, whose injector, which forms the top section of the separating column of the gas chromatograph, is provided in the usual way with a feedthrough channel for gas and an opening sealed by the septum consisting of an elastic material.
  • the gas chromatograph according to the invention is characterized in that the said opening is situated in a section of the injector that branches off from the feed-through gas channel and in that this part of the injector is connected with the environment by a small gas discharge opening.
  • the discharge opening is preferably provided with a fine adjustment screw or with a capillary whose length is chosen in accordance with the dischar e veloci desired.
  • the invention will be further e ucidate below with reference to the drawing, which shows an embodiment of the injector section of a gas chromatograph.
  • Injector 1 forms the top section of column 2 of the gas chromatograph.
  • Column 2 which consists of a glass or metal tube, is filled up to injector l with the fine-grained adsorbent 3.
  • Column 2 is situated in a thermostat (not shown in the drawing), whose temperature can be adjusted to a constant value, or be programmed.
  • Injector l is provided with heater 4 so as to be heated up to about 25 to 50 C above the column tem perature.
  • Injector 1 comprises several channels. Of these, channel 5 is sealed by septum 6, consisting of a disc of an elastic material, which is pressed down by nut 7. The latter is provided with opening 8, which is situated in line with channel 5.
  • Channel 9 is situated in cross piece 10, to which a hose or tube for the supply of the carrier gas can be connected.
  • Channel 11 in cross piece 12 communicates with channel 5 between channel 9 and septum 6. Via an adjusting device, if desired, it forms an open communication of channel 5 with the environment.
  • a method of operating a gas chromatographic column having a channel extending between a septum of elastic material and a means for separating substances present in a mixture comprising maintaining in the portion of the channel adjacent the means for separating a flow of carrier gas into the means for separating while maintaining in a section of said channel between said portion and said septum a reverse flow of carrier gas toward the septum and through a channel outlet.
  • a gas chromatographic column comprising separating means for separating substances present in a mixture, a septum of elastic material, channel means sealed to said septum and disposed for forming a channel extending between said separating means and said septum, means arranged relative to said channel means for introducing a carrier gas into said channel means, whereby carrier gas may flow through said separating means, and conduit means arranged relative to said channel means for creating a reverse flow of a part of said carrier gas away from said separating means, toward said septum, in said channel means.

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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)
US22184A 1969-03-28 1970-03-24 Method and device for gas chromatography Expired - Lifetime US3656277A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
NL6904800A NL6904800A (enrdf_load_stackoverflow) 1969-03-28 1969-03-28

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US3656277A true US3656277A (en) 1972-04-18

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US22184A Expired - Lifetime US3656277A (en) 1969-03-28 1970-03-24 Method and device for gas chromatography

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NL (1) NL6904800A (enrdf_load_stackoverflow)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3778975A (en) * 1970-11-09 1973-12-18 Ici Ltd Gas chromatography
US3920420A (en) * 1973-05-04 1975-11-18 Rech Activities Petrolieres El Method and device for injecting liquid samples into a system for chromatographic separation in gas phase
US4242107A (en) * 1976-05-25 1980-12-30 Anthony Jenkins Apparatus for the separation of a constituent from an atmosphere
US5252109A (en) * 1991-04-24 1993-10-12 Carlo Erba Strumentazione S.P.A. Gas chromatographic injector

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3063286A (en) * 1959-07-14 1962-11-13 Standard Oil Co Sample introduction system for gas chromatography apparatus
US3150516A (en) * 1961-09-27 1964-09-29 Victor J Linnenbom Analysis of gases in a liquid solution
US3513636A (en) * 1966-07-16 1970-05-26 Scholven Chemie Ag Gas divider system

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3063286A (en) * 1959-07-14 1962-11-13 Standard Oil Co Sample introduction system for gas chromatography apparatus
US3150516A (en) * 1961-09-27 1964-09-29 Victor J Linnenbom Analysis of gases in a liquid solution
US3513636A (en) * 1966-07-16 1970-05-26 Scholven Chemie Ag Gas divider system

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Brudeweck, et al., Journal of Gas Chromatography, May 1967, pp. 217 225. *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3778975A (en) * 1970-11-09 1973-12-18 Ici Ltd Gas chromatography
US3920420A (en) * 1973-05-04 1975-11-18 Rech Activities Petrolieres El Method and device for injecting liquid samples into a system for chromatographic separation in gas phase
US4242107A (en) * 1976-05-25 1980-12-30 Anthony Jenkins Apparatus for the separation of a constituent from an atmosphere
US5252109A (en) * 1991-04-24 1993-10-12 Carlo Erba Strumentazione S.P.A. Gas chromatographic injector

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Publication number Publication date
NL6904800A (enrdf_load_stackoverflow) 1970-09-30

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