US3850579A - Ionization current detector for chromatographic analysis - Google Patents

Ionization current detector for chromatographic analysis Download PDF

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Publication number
US3850579A
US3850579A US00359854A US35985473A US3850579A US 3850579 A US3850579 A US 3850579A US 00359854 A US00359854 A US 00359854A US 35985473 A US35985473 A US 35985473A US 3850579 A US3850579 A US 3850579A
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US
United States
Prior art keywords
nozzle
test sample
gas
chamber
heated
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Expired - Lifetime
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US00359854A
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English (en)
Inventor
H Dubsky
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Czech Academy of Sciences CAS
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Czech Academy of Sciences CAS
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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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/64—Electrical detectors
    • G01N30/70—Electron capture detectors
    • 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
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/64—Electrical detectors
    • G01N30/68—Flame ionisation detectors

Definitions

  • Such gaseous test product is generally introduced into the detector on a moving linear conveyer (typically a wire) on which a test sample is coated. Inside the detector the sample is either directly volatilized by the hydrogen flame itself or, in more complex designs, is volatilized first in a separate pyrometer portionof the detector, and the resulting gaseous product is forced by a gas stream into the hydrogen flame. In either case, the increase in ionization current in the presence of the gaseous product is employed for chromatographic analysis of the product in the normal manner.
  • the present invention contemplates an improved ionization detector that is more sensitive, efficient and noise-free than existing designs and that is compatible with a rotary conveyer.
  • the detector is provided with a nozzle having an elongated central chamber centered on a longitudinal axis of the detector.
  • the nozzle has a gas port in radial communication with an intermediate portion of the chamber.
  • the input end of the nozzle is positioned in axially spaced relation to, and concentric with, a heat source including a heated cylinder through which a first gas (such as nitrogen) is directed upward toward the nozzle.
  • a first gas such as nitrogen
  • the test sample-collecting periphery of a rotary conveyer is disposed at the longitudinal axis of the detector intermediate the heated tube and the input of the nozzle. In this position, the hot nitrogen directed at the conveyer periphery volatilizes the collected test sample.
  • the resulting gaseous test product is sucked up into a partial vacuum formed in the nozzle when a second heated gas (e.g., hydrogen) is forced through the gas port into the intermediate portion of the nozzle, which is advantageously constricted relative to the input and output ends of the nozzle.
  • a second heated gas e.g., hydrogen
  • the hydrogen constituent of the resulting admixture of gases in the nozzle is ignited when mixed with air introduced into a diffusor section coupled to the upper end of the nozzle.
  • the resulting hydrogen flame ionizes the gaseous test product, and the increase in ionization current level in the diffusor is sensed by a pair of electrodes therein.
  • FIGURE depicts an improved ionization detector in accordance with the invention for use with a rotary (centrifugal) conveyer.
  • an illustrative ionization detector constructed in accordance with the invention has a longitudinal axis which is intersectedjby a peripheral region of a rotary conveyer designated as 3.
  • Such conveyer may be arranged in a conventional manner to re? tate a column of a raw material sample (not shown) and to collect the sample, after centrifugal action, on the conveyer periphery.
  • test sample (not shown) on the conveyer periphery is exposed to an axial stream of a first gas from a source 31 (illustratively nitrogen).
  • a source 31 illustrated as nitrogen
  • Such gas is heated to a temperature illustratively in the range of 200 800C by passing it through the interior of a cylinderfil which is heated via a surrounding coil 2.
  • the heated gas serves to volatilize the overlying test sample on the conveyer periphery.
  • an elongated nozzle 4 Disposed above the periphery of the conveyer 3 and axially aligned with the heated tube 1 is the input end of an elongated nozzle 4 which serves: asa fraction collector.
  • the nozzle 4 has an interior passage or chamber including an intermediate portion 32, which is preferably constricted as shown so that the fraction collector defines a Laval nozzle.
  • a second gas illustratively hydrogen
  • a tube 6 defines a gas in the nozzle which communicates with the interior of the constrictedintermediate portion 32.
  • the hydrogen gas thus introduced into the portion 32 is preheated in a suitable manner to a temperature of about 500C.
  • Such introduced hydrogen gas is transported upwardly through the nozzle chamber and into a diffusor 7 that communicates with the upper end of the nozzle chamber for ionizing the test sample as described below and for measuring changes in the ambient ionization current caused thereby.
  • the hydrogen flame which may be rectified and made more uniform by the provision of an auxiliary screen 10 disposed in the diffusor 7 above the air inlet tube 12, results in the generation of ions of hydrogen.
  • the resulting ambient ionic current in the diffusor 7 (in the absence of the test sample) is picked up by a pair of electrodes 8,9 and passed through an amplifier 33 to a suitable ionization current recorder 34, which may be calibrated to a desired reference current level.
  • An enhancement of detector performance can be obtained if the nozzle 4 is preheated to a temperature in the range of 200 800C. Such heating can bevaccomplished, e.g., by means of an auxiliary heating coil 5 disposed around the nozzle 4.
  • thermo-ionization phenomenon will of 1.
  • an ionization apparatus for'the chromatographic analysis of a test sample :
  • an elongated nozzle including a central chamber'having input and output ends and an intermediate portion, and a gas port disposed at the nozzle periphery in radial communication with the intermediate portion of the chamber; means disposed in axially spaced relation to the input end of the nozzle for directing a first heated gas axially toward the input end of the nozzle chamber;
  • conveyer means for transporting a test sample to a position axially aligned with and intermediate the directing means and the input end of the nozzle chamber whereby the heated first gas from the di recting means volatilizes the test sample;
  • Another advantageous characteristic of the described scheme is that a high degree of noise suppression has been observed when the auxiliary screen is used.
  • the electrodes 8 and 9 are shown as separate elements within the diffusor 7.
  • One of such electrodes may alternatively be constituted by a portion of the detector wall (e.g., the wall of diffusor 7 or nozzle 4, if conductive) or by an internal component of the detector (e.g., the screen 10 or the supply tube 6, if conductive).
  • the gas directing means includes an axiallyaligned heated cylinder through which the first gas is passed.
  • the ionizing means comprises means for introducing forced air adjacent the output end of the nozzle chamber to ignite the heated second gas to form a flame, said flame serving to ignite and ionize the volatilized test sample.
  • the ionizing means further comprises an auxiliary rectifying screen disposed above the forced air introducing means.
  • volatilized test sample contains a material selected from the group consisting of phosporous and the halogens, and in which the apparatus further comprises an alkaline metal salt disposed on the auxiliary screen.

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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)
US00359854A 1972-05-15 1973-05-14 Ionization current detector for chromatographic analysis Expired - Lifetime US3850579A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CS325972A CS154807B1 (de) 1972-05-15 1972-05-15

Publications (1)

Publication Number Publication Date
US3850579A true US3850579A (en) 1974-11-26

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Family Applications (1)

Application Number Title Priority Date Filing Date
US00359854A Expired - Lifetime US3850579A (en) 1972-05-15 1973-05-14 Ionization current detector for chromatographic analysis

Country Status (6)

Country Link
US (1) US3850579A (de)
CS (1) CS154807B1 (de)
DE (1) DE2323927A1 (de)
EG (1) EG10968A (de)
IN (1) IN138831B (de)
IT (1) IT987299B (de)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3967931A (en) * 1974-09-25 1976-07-06 Research Corporation Flame aerosol detector for liquid chromatography
US4202666A (en) * 1978-02-24 1980-05-13 Tracor, Inc. Method and apparatus for preventing the destruction of an alkali source of a nitrogen-phosphorous detector
US5760291A (en) * 1996-09-03 1998-06-02 Hewlett-Packard Co. Method and apparatus for mixing column effluent and make-up gas in an electron capture detector
US20150330956A1 (en) * 2014-05-16 2015-11-19 Waters Technologies Corporation Flame Ionization Detection Burner Assemblies for Use in Compressible Fluid-Based Chromatography Systems
US20160209026A1 (en) * 2015-01-19 2016-07-21 Siemens Aktiengesellschaft Device For Regulating A Burner System

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102013222675A1 (de) * 2013-11-07 2015-05-07 Robert Bosch Gmbh Ionisationssensor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3372000A (en) * 1964-02-27 1968-03-05 Beckman Instruments Inc Flame ionization detector
US3574549A (en) * 1967-02-20 1971-04-13 Shell Oil Co Microanalyzer for thermal studies
US3744973A (en) * 1970-08-11 1973-07-10 Ceskoslovenska Akademie Ved Chromatographic detection apparatus
US3753654A (en) * 1971-07-14 1973-08-21 Shell Oil Co Method for determining organic materials in water

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3372000A (en) * 1964-02-27 1968-03-05 Beckman Instruments Inc Flame ionization detector
US3574549A (en) * 1967-02-20 1971-04-13 Shell Oil Co Microanalyzer for thermal studies
US3744973A (en) * 1970-08-11 1973-07-10 Ceskoslovenska Akademie Ved Chromatographic detection apparatus
US3753654A (en) * 1971-07-14 1973-08-21 Shell Oil Co Method for determining organic materials in water

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3967931A (en) * 1974-09-25 1976-07-06 Research Corporation Flame aerosol detector for liquid chromatography
US4202666A (en) * 1978-02-24 1980-05-13 Tracor, Inc. Method and apparatus for preventing the destruction of an alkali source of a nitrogen-phosphorous detector
US5760291A (en) * 1996-09-03 1998-06-02 Hewlett-Packard Co. Method and apparatus for mixing column effluent and make-up gas in an electron capture detector
US20150330956A1 (en) * 2014-05-16 2015-11-19 Waters Technologies Corporation Flame Ionization Detection Burner Assemblies for Use in Compressible Fluid-Based Chromatography Systems
US10191020B2 (en) * 2014-05-16 2019-01-29 Waters Technologies Corporation Flame ionization detection burner assemblies for use in compressible fluid-based chromatography systems
US10877006B2 (en) 2014-05-16 2020-12-29 Waters Technologies Corporation Flame ionization detection burner assemblies for use in compressible fluid-based chromatography systems
US20160209026A1 (en) * 2015-01-19 2016-07-21 Siemens Aktiengesellschaft Device For Regulating A Burner System
US10054309B2 (en) * 2015-01-19 2018-08-21 Siemens Aktiengesellschaft Device for regulating a burner system

Also Published As

Publication number Publication date
DE2323927A1 (de) 1974-02-14
IT987299B (it) 1975-02-20
EG10968A (en) 1976-11-30
CS154807B1 (de) 1974-04-30
IN138831B (de) 1976-04-03

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