Gas chromatograph device

• US 4,123,236 A
• Filed: 02/28/1975
• Issued: 10/31/1978
• Est. Priority Date: 02/28/1975
• Status: Expired due to Term

• Current Assignee: Block Engineering, LLC
• Original Assignee: Block Engineering, LLC
• Inventors: Brown, David C.A.G., Hirschfeld, T.
• Primary Examiner(s): Adee, John
• Application Number:
  US05/553,989
• Time in Patent Office: 1,341 Days
• Field of Search: 55/67, 55/197, 55/386, 23/232 C, 73/23.1
• US Class Current: 96/104
• CPC Class Codes: G01N 2030/326 pumps
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence

Abstract

An improved high resolution chromatograph device operable at column pressures ranging between one and fifty atmospheres absolute measured at the column exit, means for closely regulating the column carrier gas velocity including intermittent stop flow operation, and sample collection chamber means to facilitate contamination free handling and concentration of collected pure sample during spectral or other analysis of eluted samples. Velocity and stop flow control without loss of chromatographic resolution permits matching operation time of chromatograph to that of spectral or other analysis devices.

Claims

1. An improved gas chromatograph apparatus comprised of a pressure resistant gas chromatograph column, the column having an inlet opening at a first end and an outlet opening at a second end, an injection port means mounted to the column inlet opening, a reservoir of pressurized carrier gas, adjustable inlet pressure regulation means connecting the carrier gas reservoir to the injection port, the injection port means being provided with means for combining sample gaseous mixtures with the pressurized carrier gas and introducing these gases under pressure into the inlet opening of the column, adjustable flow restrictive means, the flow restrictive means being mounted to the column outlet opening, the flow restrictive means being adapted to adjust the pressure within the column in the vicinity of the column outlet opening from 1 atmosphere absolute upward to at least 50 atmospheres absolute pressure, whereby with appropriate adjustment of the flow restrictive means chromatograph separations of sample gas mixtures may be conducted within the column at absolute pressures measured at the column outlet opening in the range upward from one atmosphere to above 50 atmospheres absolute pressure, whereby the velocity of the gases flowing through the column may be adjusted to conform to a preselected value by simultaneously adjusting the flow restricting means at the outlet opening to fix the desired column pressure and adjusting the inlet pressure regulation means to fix the desired carrier gas column pressure, the aforesaid chromatograph apparatus further being a sample collection chamber, the sample collection chamber having an input port and an output port, the sample collection chamber input port being connected to the column outlet opening and the sample collection chamber output port being connected to the adjustable flow restriction means, a stop valve, the stop valve having a first and a second side, the first side being mounted to the flow restriction means and the second side venting to the atmosphere, whereby eluted pressurized samples of gas may be collected at low gas velocities in the sample collection chamber.

2. The gas chromatograph device with a sample collection chamber device of claim 1 wherein the sample collection chamber has a second input port and a second output port, the two input ports and the two output ports, respectively, being selectively closed and opened by means of our stop valves mounted, respectively, on each of the two input and two output ports, the second input port being connected to a supply of pressurized carrier gas, the second output port opens to the atmosphere, whereby during normal operation, the second input port and second output port valves are closed during the flushing cycle to prepare for receiving a sample into the chamber, the first input and first output valves are closed, the second ports opened and pressurized carrier gas passed through the sample chamber.

3. An improved gas chromatograph apparatus for stop flow operation comprised of a pressure resistant gas chromatograph column, the column having an inlet opening at a first end and an outlet opening at a second end, an injection port, the injection port being mounted to the column inlet opening and being provided with means for introducing under pressure a flow of carrier gas and sample gaseous mixtures into the column, a flow restrictive means, the flow restrictive means being mounted below the column outlet and being adapted to fix and maintain gas pressure within the column, so that when measured at the column outlet a pressure selected from within the range between 2 atmospheres and 50 atmospheres absolute pressure may be maintained within the column, the flow restrictive means being further adapted to regulate at the selected pressure the velocity of the gases moving through the column, a quick response first stop valve, the stop valve being mounted juxtaposed to the column outlet opening, and a sample chamber, the sample chamber being provided with an input port and an output port, a second stop valve being mounted to the chamber output port, the flow restrictive means being mounted to the second stop valve on the sample chamber output port, the sample chamber input port being mounted to the quick response stop valve, whereby separated eluted gaseous samples may be collected, concentrated under pressure and held within the sample chamber for additional analysis by intermittently opening the quick action first stop valve to connect the input port of the sample chamber to the chromatograph column, then after entraining the gaseous sample within the sample chamber closing the quick action first stop valve and the second stop valve on the sample chamber outlet port to retain the isolated gaseous sample within the chamber.

4. A gas chromatograph device with a sample collection chamber comprised of a pressure resistant gas chromatograph column, the column having an inlet opening at a first end and an outlet opening at a second end, an injection port, the injection port being mounted to the column inlet opening and being provided with means for introducing under pressure a flow of carrier gas and sample gaseous mixtures into the column, a flow restrictive means, the flow restrictive means being mounted to means in pressure connected relationship to the column outlet opening, and being adapted to sustain pressures within the column so that when measured at the column outlet a pressure selected from within the range between two atmospheres and fifty atmospheres absolute may be maintained within the column, the flow restrictive means being further adapted to regulate at the selected pressure the velocity of the gases moving through the column, a quick response first stop valve, the stop valve being mounted juxtaposed to the column outlet opening, and a sample chamber, the sample chamber being provided with a first inlet port and a first outlet port, the sample chamber first inlet port being mounted to the quick response first stop valve, the flow restrictive means being mounted to the sample chamber first outlet port, the sample chamber having a second inlet port and a second outlet port, the second inlet port and the two outlet ports, respectively, being selectively closed and opened by means of separate stop valves mounted, respectively, on the second inlet and the two outlet ports, the second inlet port being connected to a supply of pressurized carrier gas, the second outlet port through the aforesaid stop valve opening to the atmosphere, whereby separated eluted gaseous samples concentrated under pressure may be separately collected and held within the sample chamber for additional analysis by intermittently opening the quick action first stop valve to connect the inlet port of the sample chamber to the chromatograph column, then after entraining the gaseous sample chamber closing the quick action first stop valve and the remaining sample chamber valves to retain the isolated gaseous sample therein and whereby the sample chamber may be prepared to receive succeeding samples by flushing with carrier gas wherein the first input port and first output port stop valves are pg,26 closed and the second input port and second output port stop valves are opened, pressurized carrier gas passed through the sample chamber, then the second inlet port and second outlet port stop valves are closed and the device is ready for normal operation.