US3513636A - Gas divider system - Google Patents

Gas divider system Download PDF

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Publication number
US3513636A
US3513636A US652460A US3513636DA US3513636A US 3513636 A US3513636 A US 3513636A US 652460 A US652460 A US 652460A US 3513636D A US3513636D A US 3513636DA US 3513636 A US3513636 A US 3513636A
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United States
Prior art keywords
gas
sample
splitter
stream
flow
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Expired - Lifetime
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US652460A
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English (en)
Inventor
Istvan Halasz
Hartmut Bruderreck
Werner Schneider
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Scholven Chemie AG
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Scholven Chemie AG
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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
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • 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
    • G01N30/10—Preparation using a splitter

Definitions

  • a bypass splitter is placed upstream of the gas analyzer which taps from the main gas flow in the sampling line as much partial gas flow as is needed to provide the analyzer with the quantity which it requires.
  • sample injectors require a certain minimum sample volume and ratio to carrier gas in order to provide for satisfaction and eflicient "sample injection and mixing. Therefore, only a small fraction of the sample quantity actually injected by the sample injecting means (e.g., injection syringe) may be permitted to get into the separating column and thus be analyzed.
  • sample injecting means e.g., injection syringe
  • the usual procedure is to inject a measured amount of the sample into a carrier gas current and mix it in the gaseous state, with the carrier gas.
  • the sample may be liquid and transformed, if neces' sary, to the gaseous state.
  • the dividing of the sample carrier mixture is then performed by dividing the composite gas current in a sample divider, which contains a flow dividing means.
  • One part of the divided composite current is fed to the separating column, and the other (called the by-pass branch) is led away through an adjustable throttle and may be vented. This throttle makes it possible for the ratio of the two partial currents to be precisely adjused.
  • the ratio of the partial currents is adjusted before the injection of the sample, in such a manner, for example, that the partial current flowing through the separating column is in a ratio on the order of 1:99 to that which is tapped off ahead of the separating column and vented, then, when a sample of, for example, milligrams, is in- 3,513,636 Patented May 26, 1970 jected by means of the sample injecting device into the carrier gas, theoretically 0.05 milligram enters the separating column, and 4.95 milligrams are by-passed around the separating column through a by-pass line.
  • one aspect of this invention resides in a gas stream splitting apparatus comprising a feed line; a first gas stream splitter, at least two lines extending from said first splitter, at least one of which extends in a different direction than said feed line; and a second gas stream splitter in said line of different direction, which second splitter has at least two lines extending therefrom, one of which extends in a different direction than the feed line to said second splitter and communicates with the feed line to said first splitter.
  • This invention eliminates the disparity of composition caused by a gas splitter, or at least compensates in such a manner that the initial feed to the splitter apparatus has the same composition as the partial gas stream being subjected to analysis.
  • a second flow divider is provided between the main stream and one of the partial streams which, by the variation of the composition of the partial currents which occurs in it, compensates for the corresponding variations occurring at the main splitter.
  • a compensation splitter is introduced, which compensates the separation of the components of the samples which occurs at the main splitter due to differences in their molecular mass.
  • compensation splitter in such a manner that it feeds back into the main stream preferentially those components which are present in its own partial stream in an excess above the original composition of the sample.
  • the dimensions of the compensation splitter can be determined empirically.
  • One advantageous system is to locate the compensation splitter at the point of discharge from a nozzle into the main stream. A suction effect then is caused by the nozzle, which positively draws a portion of the partial stream through the compensation splitter and feeds such back into the main stream.
  • the composition of the sample gas be uniform over the entire flow cross section at the point where stream splitting occurs. If this requirement is not already satisfiedand this may be the case in gas chromatography, for example, if the injection of the sample into the carrier gas is performed just upstream of the main splitterone or more mixing means, such as cross-sectional restrictions (mixing nozzles), can be provided in the line leading to the main or first splitter.
  • mixing means such as cross-sectional restrictions (mixing nozzles)
  • a mixing chamber 1 is provided having a carrier gas inlet line 2 and a sample injector 4. Where the mixing chamber 1 is not sufficient to intimately mix the carrier gas and the sample to provide a uniform gas phase mixture of the two, additional mixing and vaporizing systems 5 and 8 are provided.
  • the vaporizing systems 5 may consist of metal chips packed in a tube.
  • the mixing means 8 may be cross-sectional restrictions of this tube.
  • the greater part of the gas mixture is deflected from its original direction of flow and flows through the annular space 18 formed by the mantle tube 14 and an outer wall 30, exiting into a holding vessel 20. From the holding vessel 20, the gas flows through a needle valve 22 to an outlet 24 from which it may be vented. The smaller portion of the gas stream passes without deflection through the tap 16 into a capillary column 26 and passes on into a flame ionization detector 28 or other analyzing means.
  • a compensation splitter is formed by apertures 12.
  • the sample stream is enriched with lighter molecules from the by-pass stream in such a manner as to compensate for the heavier molecules preferentially passing through the tap 16, by reason of their momentum as set forth above, and into the separating column.
  • the optimum dimensions of the above-mentioned structural components can be determined by experiment with respect to any given system under consideration.
  • a sample splitter of the kind described above has the special peculiarity that the splitting of a gas stream can be performed homogeneously, i.e., without difference in the concentration of the components in the partial, split streams.
  • the advantages achievable by the invention consist in that very small amounts of a sample having a wide boiling range corresponding to great mass differences in the sample molecules, e.g., n-heptane and n-hexadecane, can be divided, without any difference in the relative quantity ratio of the individual components of the sample after division as compared with the relative quantity ratios in the original sample before division.
  • n-heptane and n-hexadecane can be divided, without any difference in the relative quantity ratio of the individual components of the sample after division as compared with the relative quantity ratios in the original sample before division.
  • the hold tank 20 assures, in the case of the gas chromatograph shown in the embodiment of the drawing, that the gas composition at throttle 22 does not vary while the mixture of carrier gas and sample is passing through the tap at 16. Otherwise, it might happen that a mixture of carrier gas and sample might still be present at the tap 'while the mixture of carrier gas and sample is already flowing through throttle 22. That is, a change in the density and viscosity of the gas at point 22 induces a change in the velocity of flow at point 16. But a change in the velocity of flow at point 16 must not occur at the time when the mixture of carrier gas and sample is passing point 16, because otherwise serious trouble would have to be expected. Consequently, the hold 'tank volume is made sufficiently great so that the mixture of sample and carrier gas is not simultaneously passing through the tap 16 and the throttling means 22.
  • This invention is applicable to gas analyzers other than gas chromatographs since it is directed to providing a sample to be analyzed, rather than directed toward the analysis itself.
  • the length of the nozzle is 4.0 mm., with an inner diameter of mm. at the upper end and with an inner diameter of 0.7 mm. at the lower end.
  • the mantle tube 14 has an inner diameter of 2.5 mm. and an outer diameter of 4.0 mm.
  • the diameter of apertures 12 is 0.9 mm.
  • Six alpertures are situated in equal distance around the mantle tube 14 in equal height with the lower end of nozzle 10. The distance of the apertures from the lower end of the mantle tube 14 is 22 mm. The distance of the lower end of mantle tube 14 from the upper end of tap 16 is 1.5 mm.
  • the outer wall 30 has an inner diameter of 6 mm.
  • the volume of the holding vessel 20 has to be larger than the volume of the injected and evaporated sample and the carrier gas in which it is evapon'zed under the temperature and pressure conditions in the said holding vessel 20.
  • the holding vessel 20 was a cylindrical tube, 200 mm. in length and with an inner diameter of 65 mm.
  • Each of the vaporizing systems 6 are 5 mm. in length, with an inner diameter of 2 mm.
  • the inner diameters of the mixing means 8 are 0.5 mm.
  • the bypass ratio was varied from 1:200 up to 1:5100; the inlet pressure of the nitrogen carrier gas varied from 1 to 5 atmospheres; the temperature of the gas divider system was varied between 200 and 300 C.
  • Each single analysis was repeated at least eight times. The deviation of the averages of single runs was in any case smaller than :L1% relative, compared to the known figures of the weighed-in sample.
  • Apparatus for providing a small portion of a gas phase material having the same composition proportions as the entire gas phase from which it is derived comprising (A) a chamber means,
  • Apparatus as claimed in claim 1 including a holding tank connected to said gas exhaust line.
  • Apparatus as claimed in claim 2 including a throttle valve downstream of said holding tank.
  • Apparatus as claimed in claim 4 including gas mixing means upstream of said nozzle.

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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)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
  • Sampling And Sample Adjustment (AREA)
US652460A 1966-07-16 1967-07-11 Gas divider system Expired - Lifetime US3513636A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1966SC039271 DE1673068B2 (de) 1966-07-16 1966-07-16 Vorrichtung zur beaufschlagung eines gasanalysators, insbesondere eines gaschromatographen, mit einer teilmenge eines hauptgasstromes

Publications (1)

Publication Number Publication Date
US3513636A true US3513636A (en) 1970-05-26

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Application Number Title Priority Date Filing Date
US652460A Expired - Lifetime US3513636A (en) 1966-07-16 1967-07-11 Gas divider system

Country Status (5)

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US (1) US3513636A (de)
CH (1) CH452934A (de)
DE (1) DE1673068B2 (de)
GB (1) GB1167554A (de)
NL (1) NL157718B (de)

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3656277A (en) * 1969-03-28 1972-04-18 Tno Method and device for gas chromatography
US4124358A (en) * 1976-05-11 1978-11-07 Siemens Aktiengesellschaft Sample-injection device for process gas chromatography with capillary columns
JPS5643557A (en) * 1979-09-19 1981-04-22 Hitachi Ltd Sample divider
FR2623290A1 (fr) * 1987-11-03 1989-05-19 K I Khromato Procede d'analyse chromatographique de melanges de substances liquides et chromatographe en phase gazeuse pour la mise en oeuvre de ce procede
US4873058A (en) * 1987-03-16 1989-10-10 Siemens Aktiengesellschaft Flow divider for gas chromatographs
US5047073A (en) * 1990-02-27 1991-09-10 Transducer Research, Inc. Sorption separation apparatus and methods
US20040050251A1 (en) * 2001-12-28 2004-03-18 Paolo Magni Method and device for vaporization injection of high volumes in gas chromatographic analysis
US20050039602A1 (en) * 2002-07-24 2005-02-24 Andrew Tipler Analyte pre-concentrator for gas chromatography
US9297740B2 (en) 2013-05-17 2016-03-29 Azbil Corporation Particle detecting device and particle detecting method
CN106168612A (zh) * 2016-08-31 2016-11-30 许继集团有限公司 一种气体分析进样装置

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3132638A1 (de) * 1981-08-18 1983-03-10 Vsesojuznyj naučno-issledovatel'skij i konstruktorskij institut chromatografii, Moskva Verfahren zur einfuehrung von proben in einem gaschromatografen und vorrichtung zur durchfuehrung dieses verfahrens
US5315885A (en) * 1992-01-30 1994-05-31 Baker Hughes Incorporated Sample dispersing apparatus and method

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2267354A (en) * 1940-02-02 1941-12-23 Northon Louis Irving Prevention of reverse flow in water supply systems
US3103942A (en) * 1961-09-22 1963-09-17 Du Pont Apparatus and process for distributing viscous liquids
US3357233A (en) * 1964-10-05 1967-12-12 Phillips Petroleum Co Fluid control system for analyzers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2267354A (en) * 1940-02-02 1941-12-23 Northon Louis Irving Prevention of reverse flow in water supply systems
US3103942A (en) * 1961-09-22 1963-09-17 Du Pont Apparatus and process for distributing viscous liquids
US3357233A (en) * 1964-10-05 1967-12-12 Phillips Petroleum Co Fluid control system for analyzers

Cited By (18)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3656277A (en) * 1969-03-28 1972-04-18 Tno Method and device for gas chromatography
US4124358A (en) * 1976-05-11 1978-11-07 Siemens Aktiengesellschaft Sample-injection device for process gas chromatography with capillary columns
JPS5643557A (en) * 1979-09-19 1981-04-22 Hitachi Ltd Sample divider
US4873058A (en) * 1987-03-16 1989-10-10 Siemens Aktiengesellschaft Flow divider for gas chromatographs
FR2623290A1 (fr) * 1987-11-03 1989-05-19 K I Khromato Procede d'analyse chromatographique de melanges de substances liquides et chromatographe en phase gazeuse pour la mise en oeuvre de ce procede
US5047073A (en) * 1990-02-27 1991-09-10 Transducer Research, Inc. Sorption separation apparatus and methods
US6955709B2 (en) * 2001-12-28 2005-10-18 Thermo Electron S.P.A. Method and device for vaporization injection of high volumes in gas chromatographic analysis
US20040050251A1 (en) * 2001-12-28 2004-03-18 Paolo Magni Method and device for vaporization injection of high volumes in gas chromatographic analysis
US20040187682A2 (en) * 2001-12-28 2004-09-30 Thermo Finnigan Italia S.P.A. Method and device for vaporization injection of high volumes in gas chromatographic analysis
US20050039602A1 (en) * 2002-07-24 2005-02-24 Andrew Tipler Analyte pre-concentrator for gas chromatography
US6974495B2 (en) * 2002-07-24 2005-12-13 Andrew Tipler Analyte pre-concentrator for gas chromatography
US20060021504A1 (en) * 2002-07-24 2006-02-02 Andrew Tipler Analyte pre-concentator for gas chromatography
US7311757B2 (en) 2002-07-24 2007-12-25 Perkinelmer Las, Inc. Analyte pre-concentrator for gas chromatography
US20080098887A1 (en) * 2002-07-24 2008-05-01 Andrew Tipler Analyte Pre-Concentrator For Gas Chromatography
US7572319B2 (en) 2002-07-24 2009-08-11 Perkinelmer Las, Inc. Analyte pre-concentrator for gas chromatography
US9297740B2 (en) 2013-05-17 2016-03-29 Azbil Corporation Particle detecting device and particle detecting method
CN106168612A (zh) * 2016-08-31 2016-11-30 许继集团有限公司 一种气体分析进样装置
CN106168612B (zh) * 2016-08-31 2017-09-12 许继集团有限公司 一种气体分析进样装置

Also Published As

Publication number Publication date
NL6708613A (de) 1968-01-17
DE1673068A1 (de) 1971-07-08
DE1673068B2 (de) 1976-07-01
NL157718B (nl) 1978-08-15
CH452934A (de) 1968-03-15
GB1167554A (en) 1969-10-15

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