US3925023A - Flame ionization detector - Google Patents

Flame ionization detector Download PDF

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Publication number
US3925023A
US3925023A US418121A US41812173A US3925023A US 3925023 A US3925023 A US 3925023A US 418121 A US418121 A US 418121A US 41812173 A US41812173 A US 41812173A US 3925023 A US3925023 A US 3925023A
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United States
Prior art keywords
nozzle
invention according
burner
source
supplying
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Expired - Lifetime
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US418121A
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English (en)
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Rudolf Kaiser
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Individual
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Individual
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/626—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using heat to ionise a gas

Definitions

  • the substance to be detected is h i fed to the first burner nozzle, with hydrogen as the [58] Field of Search H 23/254 EF, 254 E, 232 C fuel gas being fed to the first nozzle when detecting hydrocarbon compounds and to the second nozzle when detecting nitrogen compounds.
  • both nozzles and the salt UNITED STATES PATENTS source are kept at a negative potential and when de 3 9 3/l953 Giuffrida 23/254 EF tecting nitrogen compounds, the second nozzle is at a i; g'flg -ja 2 5552 negative potential and the first nozzle and salt source l ert, r A A 3,692,492 9/1972 Poli, Jr. et al. r. 23/254 E at a poslnve potential or ground.
  • the substance to be detected is fed, whether detecting hydrocarbons or nitrogen or other hetero compounds, to the first burner nozzle and the fuel gas fed to the first burner nozzle when detecting hydrocarbons and to the second burner nozzle when detecting nitrogen or other hetero compounds.
  • the first and second burner nozzles are connected to a negative voltage and when detecting nitrogen or other hetero compounds, the second burner nozzle is connected to a negative voltage and the first burner nozzle connected to a ground or positive voltage.
  • the detector of the present invention can be rapidly switched without requiring mechanical changes in the system to obtain maximum selectivity for hydrocarbons or maximum selectivity for nitrogen compounds. In each mode of operation, the system retains high sensitivity to the compound which is being detected.
  • FIG. 1 is a schematic illustration of the system of the present invention configured for the detection of nitrogen or other hetero compounds.
  • FIG. 2 is a similar schematic diagram illustrating the configuration of the present system for the detection of hydrocarbon compounds.
  • FIG. 1 is a schematic illustration of the system of the present invention, configured for the detection of nitrogen or other hetero compounds.
  • the detection chamber itself is designated by the reference numeral 1.
  • a first burner nozzle 4 This burner nozzle has a feed line inserted into the central axes of its housing below, preferably through an insulating feed through made of a material such as Teflon (tetra-fluor ethylene).
  • a funnelshaped collector electrode is mounted in the top of the chamber above the burner nozzle 4 and similarly may have its connections brought through insulating feedthroughs in typical fashion.
  • a holder 5 Arranged above the burner 4, i.e., between the burner 4 and the collector 3, is a holder 5 into which there is placed a salt source 7.
  • the salt source comprises a dish 6 of platinum, into which is fused rubidium bromide or other suitable salt.
  • Structurally attached to the holder 5 is a second burner nozzle 8 and its associated feed line. Coupling between the holder 5 and the burner 8 is through an adjustable coupling 13 which permits relative motion therebetween to adjust the nozzle of the second burner 8 from the salt source 7.
  • the burner 4 When detecting a nitrogen or other hetero compound, the burner 4 is fed with the sample along its central axes as indicated.
  • Burner 4 additionally has a second inlet through which air for combustion is fed as indicated.
  • the burner 8 in this arrangement is fed with the fuel gas, H,, as indicated.
  • the burner nozzle 8 is electrically connected to a negative voltage source 11.
  • the holder 5 for the salt source is connected to an additional positive voltage source 10.
  • the burner nozzle 4 is also connected to a positive voltage source 9.
  • the other side of each of the voltage sources is connected to ground and to the one input of an amplifier 12.
  • the other input to amplifier 12 is taken from the collector electrode 3 in conventional fashion. In a well known manner, the amplifier output is then provided to a recorder 33 or the like.
  • the nozzles 4 and 8 along with their feed lines will preferably be made of steel in conventional fashion.
  • the hydrogen fed to the burner nozzle 8 as the fuel device will be ignited in well known fashion by an ignition device (not shown) which is provided within the chamber 1.
  • the tip of the flame produced therefrom will touch the salt source 7.
  • Air from combustion is provided in well known fashion by the air inlet at the burner 4.
  • the sample to be examined for traces of nitrogen is fed-in through the nozzle 4.
  • the preferred voltages at each of the points will be as follows: a negative potential of approximately 200 to 300 V, being provided by the voltage source 11 to the burner nozzle 8; a voltage which is at ground or slightly positive being provided to the holder 5; and similarly, a ground or positive voltage being provided by the voltage source 9 to the burner nozzle 4.
  • Each of the voltage supplies 9, 10 and 11 will preferably be adjustable for voltages between 0 and 300 volts.
  • the combination of the holder 5 and nozzle 8 will be axially moveable so that the spacing of these parts from the nozzle 4 can be adjusted.
  • the background ionization current which interferes in trace analysis is greatly reduced.
  • the salt source 7 grounded or at a small positive voltage of about 10 V, results in a maximum selectivity with a very small background current and a small flame.
  • This setting gives a medium nitrogen sensitivity. If the flow of hydrogen and therewith, the size of the flame is increased, the nitrogen sensitivity can also be increased. In that case, a voltage of about 90 V should be connected to the salt source.
  • Sensitivity and selectivity for detecting nitrogen is also influenced by the position of the salt source relative to flame from the burner nozzle 8 and the position of these parts relative to the nozzle 4 and the collector electrode 3.
  • the hydrogen supply and the ratio of com bustion air which is fed into the hydrogen stream must also be adjusted to obtain maximum sensitivity. Furthermore, the adjustment of the positive voltage at the nozzle 4 will have an effect. In the arrangement of FIG. 1, maximum sensitivities of 3 to Coul/g are attainable and maximum selectivities of l:90,000 obtainable.
  • the negative supply 11 is directly connected to burner nozzle 8.
  • Supply is connected to holder 5 through a switch 15 and supply 9 connected to burner nozzle 4 through a switch 17.
  • the other terminals of each of the switches 15 and 17 are connected to supply 1 1.
  • FIG. 2 illustrates the arrangement of the system for the detection of hydrocarbons. Essentially, the same elements are present as were described above, with identical parts given the same reference numerals.
  • both nozzles 4 and 8 and the holder 5 are now all connected to the negative supply 11. That is, switches 15 and 17 are switched from their respective positive supply connections to the negative supply 11. As noted above, this supply is adjustable between 0 and 300 V and for use in detecting hydrocarbons, should be adjusted to a voltage of between approximately 200 and 300 V.
  • the fuel is now fed in through the noule 4 along with the sample as indicated. Combustion air is supplied in the same manner as noted above.
  • the nozzle 8 no longer acts as a fuel supply with its hydrogen supply being shut off, but only as an additional electrode in the system.
  • a flame ionization detector comprising:
  • an enclosed detection chamber having a central axis associated therewith;
  • a collector electrode arranged in the upper portion of said chamber, essentially along said axis;
  • a first burner nozzle in the lower portion of said chamber, arranged with its outlet directed upward along said axis;
  • g. means for selectively supplying a fuel gas to one of said first and second nozzles
  • k. means for selectively coupling said first burner nozzle to one of said negative supply and said means for supplying one of a positive and ground potential, whereby, by selectively feeding said fuel gas to said second nozzle and coupling said first nozzle to said means for supplying one of a positive and ground potential, a nitrogen or other hetero compound sample may be fed to said first nozzle for detection, and by selectively feeding said fuel gas to said first nozzle and coupling said first nozzle to said negative supply a hydrocarbon may be fed to said first nozzle and detected.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth 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)
US418121A 1972-11-21 1973-11-21 Flame ionization detector Expired - Lifetime US3925023A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE2257099A DE2257099C3 (de) 1972-11-21 1972-11-21 Flammenionisationsdetektor

Publications (2)

Publication Number Publication Date
USB418121I5 USB418121I5 (xx) 1975-01-28
US3925023A true US3925023A (en) 1975-12-09

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ID=5862366

Family Applications (1)

Application Number Title Priority Date Filing Date
US418121A Expired - Lifetime US3925023A (en) 1972-11-21 1973-11-21 Flame ionization detector

Country Status (6)

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US (1) US3925023A (xx)
CH (1) CH566553A5 (xx)
DE (1) DE2257099C3 (xx)
FR (1) FR2207605A5 (xx)
GB (1) GB1446085A (xx)
IT (1) IT999463B (xx)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4203726A (en) * 1978-02-28 1980-05-20 Varian Associates, Inc. Thermionic detector
US4273559A (en) * 1977-08-08 1981-06-16 Varian Associates, Inc. Elemental superselective gas chromatographic detection apparatus and method
US4311664A (en) * 1976-12-08 1982-01-19 Wojskowy Instytut Chemii I Radiometrii Flame-photometric detector burner of gas chromatograph
US4318708A (en) * 1977-08-23 1982-03-09 Ab Volvo Method of investigation or control of catalysts or catalyst reactions
US4508685A (en) * 1981-06-09 1985-04-02 Carlo Erba Strumentazione S.P.A. Modified-flame thermionic detector for gas chromatographs and method for the identification of components in sample under analysis

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2728099C2 (de) * 1977-06-22 1984-09-06 Siemens AG, 1000 Berlin und 8000 München Thermoionisationsdetektor zum Nachweis von Heteroatome enthaltenden organischen Verbindungen
JPS59200954A (ja) * 1983-04-20 1984-11-14 バリアン・アソシエイツ・インコ−ポレイテツド Ｇｃ及びｌｃ溶出物の検出のための２重炎イオン化検出器
WO1986006836A1 (en) * 1985-05-17 1986-11-20 Shimadzu Corporation Detector for gas chromatograph
DE102020114455A1 (de) 2020-05-29 2021-12-02 Krohne Messtechnik Gmbh Vorrichtung für den mobilen Nachweis von organischen Verbindungen und Verfahren zur Herstellung der Vorrichtung

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3372994A (en) * 1965-01-08 1968-03-12 Health Education Welfare Usa Flame ionization detector
US3425806A (en) * 1965-03-22 1969-02-04 Us Health Education & Welfare Method and means for detecting a halogen or phosphorus in a gaseous material
US3504976A (en) * 1966-05-04 1970-04-07 Beckman Instruments Inc Process and apparatus for the detection of halogens
US3692492A (en) * 1971-02-08 1972-09-19 Mine Safety Appliances Co Apparatus for measuring carbon monoxide and total hydrocarbons in gas sample

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3372994A (en) * 1965-01-08 1968-03-12 Health Education Welfare Usa Flame ionization detector
US3425806A (en) * 1965-03-22 1969-02-04 Us Health Education & Welfare Method and means for detecting a halogen or phosphorus in a gaseous material
US3504976A (en) * 1966-05-04 1970-04-07 Beckman Instruments Inc Process and apparatus for the detection of halogens
US3692492A (en) * 1971-02-08 1972-09-19 Mine Safety Appliances Co Apparatus for measuring carbon monoxide and total hydrocarbons in gas sample

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4311664A (en) * 1976-12-08 1982-01-19 Wojskowy Instytut Chemii I Radiometrii Flame-photometric detector burner of gas chromatograph
US4273559A (en) * 1977-08-08 1981-06-16 Varian Associates, Inc. Elemental superselective gas chromatographic detection apparatus and method
US4318708A (en) * 1977-08-23 1982-03-09 Ab Volvo Method of investigation or control of catalysts or catalyst reactions
US4203726A (en) * 1978-02-28 1980-05-20 Varian Associates, Inc. Thermionic detector
US4508685A (en) * 1981-06-09 1985-04-02 Carlo Erba Strumentazione S.P.A. Modified-flame thermionic detector for gas chromatographs and method for the identification of components in sample under analysis

Also Published As

Publication number Publication date
FR2207605A5 (xx) 1974-06-14
DE2257099A1 (de) 1974-06-12
CH566553A5 (xx) 1975-09-15
DE2257099B2 (de) 1974-10-17
GB1446085A (en) 1976-08-11
USB418121I5 (xx) 1975-01-28
IT999463B (it) 1976-02-20
DE2257099C3 (de) 1975-07-03

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