Gas chromatograph for continuous operation with infrared spectrometer

• US 4,038,055 A
• Filed: 10/10/1975
• Issued: 07/26/1977
• Est. Priority Date: 10/10/1975
• Status: Expired due to Term

• Current Assignee: Block Engineering, LLC
• Original Assignee: Block Engineering, LLC
• Inventors: Tobias, Reginald, Varano, Antonio
• Primary Examiner(s): Adee, John
• Application Number:
  US05/621,404
• Time in Patent Office: 655 Days
• Field of Search: 55/67, 55/197, 55/386, 55/267, 23/232 C, 73/23.1
• US Class Current: 96/102
• CPC Class Codes: G01N 30/74 Optical detectors measurement of intensity, velocity, spectral content, polarisation, or phase of infrared, visible or ultraviolet light G01J

Abstract

An improved gas chromatograph for "on line" use with absorption spectrum analyzers, particularly, infrared spectrometers. The new chromatograph has been adapted for compatibility with a variety of absorption spectrum analysis instruments from the standpoint of cycling time, dimensions, thermal characteristics and convenience in handling extremely small and highly reactive chemical sample materials.

Claims

1. An improved gas chromatograph in combination with an absorption spectrum analyzer, the chromatograph comprising upper and lower cojoined chambers, the lower chamber having measured dimensions, the absorption spectrum analyzer having a measured dimension test sample well, the chromatograph lower chamber being dimensioned to fit within the test sample well;

the upper chamber being thermally insulated, provided with heating and thermostat means, the chromatograph further comprising a chromatograph column and an injection port, the column being mounted within the upper chamber and connected at its input to the injection port;

a detector, a sample cell and a plurality of valves, the detector cell and at least two multiport valves being mounted juxtaposed to a heated thermostated metal plate means positioned within the lower chamber;

the cell, when mounted to the aforesaid plate being positioned transversally of the lower chamber, short tubular connections between, respectively, the column and valves between the detector and valves, and between the cell and valves, whereby, eluted sample materials emitted by the column may be entrained and momentarily retained within the sample cell, the chromatograph lower chamber with the transverse sample cell being positioned within, yet thermally insulated from the analyzer test sample well, while absorption spectrum analysis procedures are completed.

2. The apparatus combination of claim 1 above wherein the absorption spectrum analyzer is an infrared spectrometer.

3. The apparatus combination of claim 1 above, a flow restrictor, wherein at least one valve port connects to the flow restrictor and the restrictor connects to exhaust into the atmosphere, whereby the chromatograph column pressure measured at the output of the column and the sample cell pressure may be maintained during operation at gauge pressures greater than one atmosphere.

4. The combination apparatus of claim 1, wherein the upper chamber heating means is comprised of means for heating and circulation of heated air through the chamber.

5. The combination device of claim 4, wherein the chromatograph column is wound into a flat spiral and mounted within the thermally insulated upper chamber with the axis of the flat spiral at right angles to the vertical.

6. The combination apparatus of claim 5 above, wherein there is a second chromatograph column, the second column being wound into a flat spiral and mounted juxtaposed and coaxially with the first column within the upper chamber whereby the first column is an analytic column and the second column is a reference column and both columns are maintained in identical thermal condition with the heated air circulating about them.

7. The combination apparatus of claim 1 above, wherein the heated thermostated plate means positioned within the lower chamber is comprised of a first and a second matching plates, the plates being recessed respectively to accommodate enclosed mounting of two thermal conductivity detectors within the juxtaposed plates, external surfaces upon the plates for mounting the two multiport valves, and an external concavity for mounting the sample cell, the valves and cell when mounted to the plates being in thermal contact therewith, and heater coils and thermostat means juxtaposed to the plates to maintain the plates assembled with the detectors, valves and sample cell within a specified temperature range, whereby the chromatograph components mounted within the lower chamber and adjacent to the absorption spectrum analyzer are maintained within a specified operating temperature, but the adjacent analyzer is not excessively heated by the chromatograph.

8. An improved gas chromatograph comprising an upper chamber and a lower chamber, the chambers being cojoined metal enclosures thermally insulated respectively one from the other, the chromatograph further comprising a chromatograph column and an injection port, the column being mounted within the upper chamber and connected at its input to the injection port heat generating means mounted within the upper chamber, adapted to maintain the column at an elevated temperature;

a detector, a sample cell and a plurality of multiport valves, the detector cell and at least two multiport valves being mounted juxtaposed to a heated, insulated and thermostated metal plate means, the metal plate means being positioned within the lower chamber;

the cell, when mounted to the aforesaid plate being positioned transversally of the lower chamber, short tubular connections between respectively, the column and valves, between the detector and valves, and between the cell and valves, whereby eluted sample materials emitted by the column may be entrained and momentarily retained within the sample cell, the chromatograph lower chamber enclosure with the transverse sample cell mounted therein thermally insulated from the upper chamber heat source, whereby absorption spectrum analysis procedures may be performed upon sample materials entrained within the cell without communicating excessive heat from the chromatograph through the lower chamber enclosure into juxtaposed absorption spectrum analysis equipment.