Method and apparatus for preconcentrating a gaseous sample

• US 10,067,100 B2
• Filed: 04/27/2016
• Issued: 09/04/2018
• Est. Priority Date: 04/30/2015
• Status: Active Grant

• Current Assignee: Thermo Fisher Scientific GmbH (Thermo Fisher Scientific Incorporated)
• Original Assignee: Thermo Fisher Scientific GmbH (Thermo Fisher Scientific Incorporated)
• Inventors: Krummen, Michael, Schwieters, Johannes, Schlueter, Hans-Juergen, Kracht, Oliver
• Primary Examiner(s): Nagpaul, Jyoti
• Application Number:
  US15/139,703
• Publication Number:
  US 20160320355A1
• Time in Patent Office: 860 Days
• CPC Class Codes: G01N 2030/324 speed, flow rate
• CPC Class Codes: G01N 2030/383 by using auxiliary fluid
• CPC Class Codes: G01N 2030/8868 elemental analysis, e.g. isotope dilution analysis
• CPC Class Codes: G01N 2030/8886 Analysis of industrial production processes
• CPC Class Codes: G01N 30/10 using a splitter
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence

Abstract

A system for concentrating an analyte gas in a gas stream of an analytical system is provided. The system comprises at least one separation device, at least one gas inlet line, at least one detector, at least one gas outlet line, a first split line in connected to the gas inlet line, and a first split valve for controlling gas flow in the first split line. Also provided is a method for concentrating an analyte gas.

Claims

1. A system for concentrating an analyte gas in a gas stream of an analytical system, the system comprising

at least one separation device, for separating components of an analyte gas;

at least one gas inlet line, for delivering the analyte gas from a supply of analyte gas to the separation device;

at least one detector, for detecting components of the analyte gas;

at least one gas outlet line, for delivering the components from the separation device to the detector;

a first split line in fluid communication with the gas inlet line at a first junction, and a first split valve for controlling gas flow in the first split line;

wherein opening of the first split line releases a part of a gas flow through the first split line and thereby reduces a flow rate through the separation device.

2. The system of claim 1, further comprising a second split line in fluid communication with the gas outlet line at a second junction, upstream from the detector, and a second split valve for controlling gas flow in the second split line.

3. The system of claim 2, wherein the second split valve for controlling gas flow is arranged at the second junction, the valve having a first position in which gas is able to flow through the second split line and the gas outlet line towards the detector, and a second position in which gas is able to flow along the gas outlet line towards the detector but is prevented from flowing along the second split line.

4. The system of claim 2, wherein the first split line and the second split line meet at a split line junction, and wherein a flow control gas line is connected to the split line junction.

5. The system of claim 4, wherein the split line junction comprises a split line valve for selectively controlling gas flow in the first split line, the second split line and/or the flow control gas line.

6. The system of claim 4, wherein the flow control gas line further comprises a flow controlling device that is provided as a first restriction line and a second restriction line that meet at a restriction junction that is fluidly connected to the flow control gas line, and wherein the first restriction line and the second restriction line each comprise a fixed flow restriction for controlling gas flow.

7. The system of claim 6, wherein a valve for controlling gas flow is positioned at the restriction junction, the valve having a first position, in which gas is able to flow through the first restriction line but is prevented from flowing through the second restriction line, and a second position, in which gas is able to flow through the second restriction line but is prevented from flowing through the first restriction line.

8. The system of claim 1, wherein the first and/or second split valve has a first position in which gas is able to flow through the split line, and a second position in which gas is prevented from flowing through the split line.

9. The system of claim 1, wherein the first split line and/or the second split line is open to atmosphere.

10. The system of claim 1, wherein the first split line and/or the second split line is connected to a gas supply line for providing gas into the supply of analyte gas and/or a sample introduction system for providing a sample into the supply of analyte gas.

11. The system of claim 1, wherein the first split valve for controlling gas flow is arranged at the first junction, the valve having a first position in which gas is able to flow through the first split line and the gas inlet line towards the separating device, and a second position in which gas is able to flow along the gas inlet line towards the separation device but is prevented from flowing through the first split line.

12. The system of claim 1, wherein the analyte gas is provided in a carrier gas that is preferably selected from helium and argon.

13. The system of claim 1, where the supply of analyte gas is provided by a chemical reactor.

14. The system of claim 1, further comprising a chemical trap that is arranged upstream of the separation device on the gas inlet line.

15. The system of claim 1, further comprising a secondary carrier gas inlet line that is fluidly connected to the gas inlet line at a carrier gas junction, between the analyte gas supply and the first split line.

16. The system of claim 15, wherein the secondary carrier gas inlet line is provided with gas flow control means for controlling gas flow into the gas inlet line.

17. The system of claim 15, further comprising an analyte gas split line that is arranged on the gas inlet line, between the analyte gas supply and the carrier gas junction, the analyte gas split line further comprising a valve for directing flow of gas through the analyte gas split line, the valve having a first position in which analyte gas is able to flow through the analyte gas split line and in which gas is prevented from flowing through the gas inlet line downstream from the analyte gas split line, and a second position in which analyte gas is prevented from flowing through the analyte gas split line but is able to flow through the gas inlet line.

18. The system of claim 15, further comprising a valve arranged at, or in fluid communication with, the carrier gas junction, wherein the valve has a first position in which gas is able to flow from the analyte gas supply through the gas inlet line towards the first junction and in which the secondary carrier gas is prevented from flowing into the gas inlet line, and a second position in which analyte gas is prevented from flowing from the analyte gas supply through the gas inlet line towards the first junction and in which the secondary carrier gas is able to flow into the gas inlet line, towards the first junction.

19. The system of claim 1, further comprising a second separation device, wherein the second separation device is arranged downstream from the second split line, between the second split line and the detector.

20. The system of claim 1, further comprising a controller for controlling valve position of at least one of the valves, and wherein the controller optionally receives an input from the detector, and wherein the position of at least one valve is based on the determination of presence or absence of at least one component of the analyte gas.

21. The system of claim 20, wherein the controller receives an input from the detector about at least one analyte gas, and wherein the position of at least one valve is adjusted based on a determination of the concentration of the analyte gas.

22. The system of claim 20, wherein the controller is configured to simultaneously adjust the position of two or more valves, so that the controller is configured to adjust the position of the first split valve and the second split valve, so that when the first split valve is open the second split valve is closed, and so that when the first split valve is closed the second split valve is open.

23. The system of claim 1, wherein the separation device is a gas chromatograph.

24. A method of concentrating a sample gas for detection in a continuous flow retention-based analytical device having a gas inlet and a gas outlet, the method comprising steps of:

providing a flow of gas into the analytical device at a first flow rate, wherein the gas contains an analyte gas comprising at least one component that is retained in the device and a carrier gas that is not retained;

reducing the flow rate of the carrier gas into the analytical device to a second flow rate prior to at least one selected component of the analyte gas emerging at the gas outlet of the analytical device, by splitting away a part of the gas stream through a first split line on, or in fluid communication with, an inlet gas line that is connected to the gas inlet, wherein the second flow rate is lower than the first flow rate;

whereby the at least one selected component of the analyte gas is concentrated in the carrier gas as it travels through the retention-based analytical device at the second flow rate.

25. The method of claim 24, wherein the analytical device is a separation device.

26. The method of claim 24, wherein the first flow rate is in the range of 40 to 400 mL/min, and wherein the second flow rate is in the range of 10 to 100 mL/min.

27. The method of claim 24, wherein the reducing of flow rate of the carrier gas to the second flow rate is performed simultaneously with, or immediately following, the replacing of the mixture of analyte gas and carrier gas with carrier gas.

28. The method of claim 24, wherein the emerging of analyte gas at the outlet of the separation device is monitored by an analyte gas detector that is located within, or downstream from, the separation device.

29. The method of claim 28, wherein gas flow rate into the analyte gas detector is maintained so as to be substantially equal to the second flow rate when the gas enters the analytical device at the first flow rate, by splitting away excess gas flow through a second split line on, or in fluid communication with, an outlet gas line between the outlet of the analytical device and the detector, said second split line being closed when the gas enters into the analytical device at the second flowrate.

30. The method of claim 24, further comprising providing a first split line for the flow of gas upstream of the gas inlet and providing a second split line downstream of the outlet for the analyte and carrier gas;

and further comprising having the first split line closed and the second split line open while the gas flows into the device at the first flow rate and having first split line open and the second split line closed while the carrier gas flows into the device at the second flow rate.

31. The method of claim 24, wherein the analyte gas comprises a plurality of components that are temporarily retained in the device;

the method further comprising reducing the flow rate of the carrier gas into the analytical device to the second flow rate prior to at least one selected component of the analyte gas emerging at the gas outlet of the analytical device;

whereby the at least one selected component of the analyte gas is concentrated in the carrier gas as it travels through the retention-based analytical device at the second flow rate.

32. The method of claim 31, further comprising reducing the flow rate of the carrier gas into the analytical device to the second flow rate after at least one non-selected component of the analyte gas has emerged at the gas outlet of the analytical device.