US3056277A - Vapor fractometers - Google Patents

Vapor fractometers Download PDF

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Publication number
US3056277A
US3056277A US797370A US79737059A US3056277A US 3056277 A US3056277 A US 3056277A US 797370 A US797370 A US 797370A US 79737059 A US79737059 A US 79737059A US 3056277 A US3056277 A US 3056277A
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sample
columns
vapor
column
carrier gas
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Expired - Lifetime
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US797370A
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English (en)
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Brenner Nathaniel
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Applied Biosystems Inc
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Perkin Elmer Corp
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Priority to US797370A priority Critical patent/US3056277A/en
Priority to DEP16281U priority patent/DE1879759U/de
Priority to CH244160A priority patent/CH384900A/de
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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
    • G01N30/46—Flow patterns using more than one column
    • G01N30/466—Flow patterns using more than one column with separation columns in parallel

Definitions

  • This invention relates to vapor fractionation and more particularly to a unique vapor fractometer apparatus which produces improved analyses.
  • Vapor fractometry also known as vapor fraction chromatography
  • vapor fraction chromatography is a well-known analytical method for the analysis of multi-component samples.
  • Two methods are most widely used for vapor fractometry. One of these is known as the clution-adsorption method, and the other is known as the elution-partition method of separation.
  • a vapor sample is injected into a carrier gas, and the combination is then passed through a column containing a separating material. The material contained in the column slows the rate of progress of the different components of the sample by varying amounts, so that the carrier gas as it exits from the column contains bands of the various components of the sample.
  • the columns which are used in chromatographic apparatus may be of several typesfor example, the well-known packed column and a newer coated column which comprises a tube having its internal surface coated with the separating material.
  • the separating material may be either liquid or solid-alone, as in the coated tube, or in combination with various supporting materials.
  • vapor fractometry is a widely used and useful analytical procedure, there are certain problems which, up until the present time, have not been solved.
  • One of these problems relates to the complete separation of all the components which may exist in a given sample.
  • many gas samples contain oxygen, nitrogen, and carbon dioxide and it is often desired to measure the concentration of each of these components in a sample.
  • oxygen, nitrogen and carbon dioxide cannot be resolved in any system of single columns or columns in series unless highly cumbersome temperature programming systems o extremely long elution times are employed. The reason for this is that nitrogen and oxygen can be resolved only on powerful adsorbents which have excessive retention characteristics with respect to carbon dioxide.
  • the primary object of this invention is to provide an apparatus capable of accurately separating and analyzing heretofore difiicultly separable components of a sample mixture. Another object is to provide a measurement system in the vapor fractometer itself which reflects the amount of sample injected by ordinary sampling methods.
  • the above objects are achieved by providing a vapor fractometer for separating a sample into its constituents in accordance with their physical characteristics.
  • the fractometer comprises a source of carrier gas and means for introducing the sample into the carrier gas. At least two columns are provided having a common inlet in series flow relationship with the carrier gas path. The columns define parallel paths for the How of carrier gas and sample and at least one of the columns contains material for which the components of the sample have different afiinities.
  • the detection means are then provided in series with the common outlet of the parallel columns for measuring the concentrations of the components present in the carrier gas. It is understood that the term parallel as used throughout this specification means functionally parallel and not necessarily physically parallel.
  • FIG. 1 is a drawing in schematic form of one embodiment of the present invention and FIG. 2 is a Fractogram of an example of an analysis employing the present invention.
  • a source 10 of carrier gas is illustrated in combination with a gas regulator 12 for providing gas to a conduit 14.
  • Conduit 14 divides into two branch conduits 16 and 18.
  • Conduit 18 conducts carrier gas to the reference side of detector 21.
  • Conduit 16 conducts the carrier gas to parallel columns 20 and 22.
  • a sample is injected into the carrier gas at sample injection point 24.
  • Variable flow restriction elements 26 and 28 are provided in each of columns 20 and 22 for the proper apportionment of the gas flow therebetween.
  • restriction element 26 independently of the rate of gas flow through column 22 controlled by element 28.
  • the time relation of the eluted bands from columns 20 and 22 may be separately regulated and adjusted so that the bands of each can be time displaced in a predetermined order.
  • the outlets of columns 20 and 2 are joined at point 30 and are connected by conduit 32 to the sensing cell of detector 21 and from there to an appropriate vent.
  • a measuring circuit 34 such as a Wheatstone bridge, develops an output voltage which varies according to the difference in certain physical characteristics between the gases in the reference and sensing cells of detector 21. This difference is transmitted to recorder 36 where it is recorded as the percentage of a given component in the sampling mixture.
  • a one meter column was packed with silica-gel
  • a two meter column was packed with a synthetic zeolite and the two columns placed in parallel in a standard vapor fractometer.
  • a gaseous sample comprising oxygen, nitrogen, and carbon dioxide was injected into the inert carrier gas. That part of the sample which passed through the column containing silica-gel was separated into two parts-oxygen and nitrogen appearing as one band and carbon dioxide as the second. That portion of the sample which passed through the column containing the synthetic zeolite was separated to yield an oxygen band and a nitrogen band.
  • the carbon dioxide was irreversibly held by the latter column.
  • a separation of oxygen, nitrogen, carbon monoxide, methane, and higher hydrocarbons up to C may be etfected in one sample run by placing a synthetic zeolite for the separation of oxygen, nitrogen, methane and carbon monoxide in parallel with a standard partition column containing dimethylsulfonane for the separation of the C; to C, fractions. Quantitative measurements of the foregoing analyses are obtained by calibration using known standards under identical conditions.
  • This invention is also suited for the analysis of gaseous samples when employing the small-diameter internallycoated columns known to the art as capillary columns. Columns of this type are described by Marcel J. E. Golay in an article entitled, Theory and Practice of Gas-Liquid Partition Chromatography With Coated Capillaries,” appearing in the book Gas Chromatography published in 1958 by Academic Press Incorporated. Such a column may be used in this invention either in parallel with a similar column, or with a standard packed column.
  • a separation column may be provided in parallel with a non-separating column.
  • the non-separating column would thereby provide a single peak readout having an area proportional to a fixed percentage of the total sample. This area could then be used as the basis for internal normalization calculation.
  • a standard sampling method may be utilized, although only a very small portion of the sample taken would be actually passed through the adsorption column.
  • a vapor fraetometer for separating a sample into its constituents in accordance with their physical characteristics comprising a source of carrier gas; means defining a path for said carrier gas; means for introducing a sin gle sample into said carrier gas; at least two columns having a common inlet in series flow relationship with said path defining means, said columns defining parallel paths for the simultaneous flow of said carrier gas and sample, eachof said columns containing a diflferent material for which the components of the sample have different afiinities; flow control means adapted to control the relative flow rates between said columns; and detection means in series flow relationship with the outlets of said parallel columns for measuring the concentrations of said components in said carrier gas.
  • a vapor fractometer for separating a sample into its constituents in accordance with their physical characeristics comprising a source of carrier gas; means defining a path for said carrier gas; means for introducing a single sample into said carrier gas; at least two chromatographic separating columns having a common inlet in series flow relationship with said path defining means, said columns defining parallel paths for the simultaneous flow of said carrier gas and sample, each one of said columns comprising a tube internally coated with a different substance for which the components of the sample have different afiinities; flow control means adapted to control the relative flow rates between said columns; and detection means in series flow relationship with the common outlet of said parallel columns for measuring the concentrations of said components in said carrier gas.

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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)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
US797370A 1959-03-05 1959-03-05 Vapor fractometers Expired - Lifetime US3056277A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
US797370A US3056277A (en) 1959-03-05 1959-03-05 Vapor fractometers
DEP16281U DE1879759U (de) 1959-03-05 1960-03-03 Gaschromatographiegeraet.
CH244160A CH384900A (de) 1959-03-05 1960-03-03 Gaschromatographiegerät

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US797370A US3056277A (en) 1959-03-05 1959-03-05 Vapor fractometers

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3159020A (en) * 1957-04-22 1964-12-01 Donner Walter Gas chromatograph
US3250057A (en) * 1963-03-13 1966-05-10 Texaco Trinidad Chromatographic separation of gaseous mixtures
US3257775A (en) * 1962-10-20 1966-06-28 Bodenseewerk Perkin Elmer Co Chromatography method and means
US3263488A (en) * 1963-03-04 1966-08-02 Hewlett Packard Co Method for gas chromatography
US3386279A (en) * 1965-03-01 1968-06-04 Beckman Instruments Inc Time resolution analysis apparatus
US3405550A (en) * 1964-12-31 1968-10-15 Mobil Oil Corp Chromatographic method and apparatus for determining trace concentrations of water
US3451255A (en) * 1966-04-07 1969-06-24 James R Neville Gas analysis apparatus
US3879181A (en) * 1972-03-09 1975-04-22 Showa Denko Kk Gas chromatograph, specimen capsule for use therein and process for gas chromatography
US4226112A (en) * 1978-01-30 1980-10-07 Gomidas Jibelian Method and apparatus for analyzing gases
US4470298A (en) * 1978-01-30 1984-09-11 Gomidas Jibelian Method and apparatus for analyzing gases
US4650499A (en) * 1985-11-27 1987-03-17 Phillips Petroleum Company Gas chromatographic apparatus and method
US20040050064A1 (en) * 2002-06-21 2004-03-18 Darko Segota Method and system for regulating internal fluid flow within an enclosed or semi-enclosed environment
US20040104309A1 (en) * 2002-06-21 2004-06-03 Darko Segota Method and system for regulating external fluid flow over an object's surface, and particularly a wing and diffuser
US20050098685A1 (en) * 2002-06-21 2005-05-12 Darko Segota Method and system for regulating pressure and optimizing fluid flow about a fuselage similar body
US20050106017A1 (en) * 2002-06-21 2005-05-19 Darko Segota Method and system for regulating fluid over an airfoil or a hydrofoil

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2728219A (en) * 1953-09-08 1955-12-27 Nat Res Dev Means for measuring the density of a fluid
FR1170329A (fr) * 1956-03-27 1959-01-13 Vickers Electrical Co Ltd Chromatographie en phase vapeur
US2868011A (en) * 1955-12-16 1959-01-13 Gulf Research Development Co Multiple-column chromatographic apparatus

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2728219A (en) * 1953-09-08 1955-12-27 Nat Res Dev Means for measuring the density of a fluid
US2868011A (en) * 1955-12-16 1959-01-13 Gulf Research Development Co Multiple-column chromatographic apparatus
FR1170329A (fr) * 1956-03-27 1959-01-13 Vickers Electrical Co Ltd Chromatographie en phase vapeur

Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3159020A (en) * 1957-04-22 1964-12-01 Donner Walter Gas chromatograph
US3257775A (en) * 1962-10-20 1966-06-28 Bodenseewerk Perkin Elmer Co Chromatography method and means
US3263488A (en) * 1963-03-04 1966-08-02 Hewlett Packard Co Method for gas chromatography
US3250057A (en) * 1963-03-13 1966-05-10 Texaco Trinidad Chromatographic separation of gaseous mixtures
US3405550A (en) * 1964-12-31 1968-10-15 Mobil Oil Corp Chromatographic method and apparatus for determining trace concentrations of water
US3386279A (en) * 1965-03-01 1968-06-04 Beckman Instruments Inc Time resolution analysis apparatus
US3451255A (en) * 1966-04-07 1969-06-24 James R Neville Gas analysis apparatus
US3879181A (en) * 1972-03-09 1975-04-22 Showa Denko Kk Gas chromatograph, specimen capsule for use therein and process for gas chromatography
US4226112A (en) * 1978-01-30 1980-10-07 Gomidas Jibelian Method and apparatus for analyzing gases
US4470298A (en) * 1978-01-30 1984-09-11 Gomidas Jibelian Method and apparatus for analyzing gases
US4650499A (en) * 1985-11-27 1987-03-17 Phillips Petroleum Company Gas chromatographic apparatus and method
US20040050064A1 (en) * 2002-06-21 2004-03-18 Darko Segota Method and system for regulating internal fluid flow within an enclosed or semi-enclosed environment
US20040104309A1 (en) * 2002-06-21 2004-06-03 Darko Segota Method and system for regulating external fluid flow over an object's surface, and particularly a wing and diffuser
US20050098685A1 (en) * 2002-06-21 2005-05-12 Darko Segota Method and system for regulating pressure and optimizing fluid flow about a fuselage similar body
US20050106017A1 (en) * 2002-06-21 2005-05-19 Darko Segota Method and system for regulating fluid over an airfoil or a hydrofoil
US20050106016A1 (en) * 2002-06-21 2005-05-19 Darko Segota Method and system for regulating fluid flow over an airfoil or a hydrofoil
US7048505B2 (en) 2002-06-21 2006-05-23 Darko Segota Method and system for regulating fluid flow over an airfoil or a hydrofoil
US7278825B2 (en) 2002-06-21 2007-10-09 Darko Segota Method and system for regulating fluid over an airfoil or a hydrofoil
US7296411B2 (en) 2002-06-21 2007-11-20 Darko Segota Method and system for regulating internal fluid flow within an enclosed or semi-enclosed environment
US7475853B2 (en) 2002-06-21 2009-01-13 Darko Segota Method and system for regulating external fluid flow over an object's surface, and particularly a wing and diffuser

Also Published As

Publication number Publication date
CH384900A (de) 1965-02-26
DE1879759U (de) 1963-09-26

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