Retention time stability in a gas chromatographic apparatus

• US 5,476,000 A
• Filed: 03/31/1994
• Issued: 12/19/1995
• Est. Priority Date: 03/31/1994
• Status: Expired due to Term

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Hewlett-Packard Company (HP Inc.)
• Inventors: Henderson, Robert, Wikfors, Edwin
• Primary Examiner(s): Noland, Thomas P.
• Assistant Examiner(s): Brock, Michael J.
• Application Number:
  US08/220,432
• Time in Patent Office: 628 Days
• Field of Search: 73/23.24, 73/23.27, 73/23.42, 73/23.22, 73/23.36, 55/270, 95/15, 95/19, 95/22, 95/23, 95/82, 96/102
• US Class Current: 73/23.27
• CPC Class Codes: G01F 1/34 by measuring pressure or differential pressure
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/324 speed, flow rate
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence
• CPC Class Codes: G01N 30/8668 using retention times
• CPC Class Codes: G01N 30/8672 not depending on an individual instrument, e.g. retention time indexes or calibration transfer

Abstract

The effect of barometric pressure variation on the retention time stability of a chromatographic analytical system is compensated by active control of the amount of fluid flow by way of a fluid flow controller, preferably in the form of an electronic pressure control system. Control signals are derived by: receiving data representative of a desired operating condition parameter, such as column inlet pressure; sensing actual operating condition parameters such as inlet pressure p_i and barometric pressure p_atm ; determining a desired average linear velocity of the fluid flow according to the desired operating system parameter; determining an actual average linear velocity of the fluid flow according to the sensed plurality of actual operating condition parameters; and controlling, as a function of a predetermined relationship of the desired average linear velocity to the actual average linear velocity, the amount of fluid flow to cause the actual average linear velocity to substantially equal the desired average linear velocity.

Claims

1. A method for performing a chromatographic analysis of a fluid in a separation column having an outlet subject to a barometric pressure p_atm, comprising the steps of:

providing fluid flow of the fluid in the separation column;

sensing a plurality of actual operating condition parameters to which the fluid flow is subjected, the plurality including the barometric pressure p_atm ;

providing information representative of a desired operating condition parameter;

determining a desired average linear velocity of the fluid flow according to the desired operating system parameter;

determining an actual average linear velocity of the fluid flow according to the sensed plurality of actual operating condition parameters; and

controlling, as a function of a predetermined relationship of the desired average linear velocity to the actual average linear velocity, the amount of fluid flow to cause the actual average linear velocity to substantially equal the desired average linear velocity.

2. The method of claim 1, wherein the information representative of a desired operation condition parameter includes data representative of desired inlet pressure (p_i).

3. The method of claim 1, wherein the information representative of a desired operating condition parameter includes data representative of a fluid flow rate.

4. The method of claim 1, wherein the information representative of a desired operation condition parameter includes data representative of a desired average linear velocity of the fluid at the column outlet (μ

_o).

5. The method of claim 1, wherein the fluid flow control is provided by a signal-controlled inlet pressure valve, and the step of controlling the fluid flow further comprises computing an adjusted inlet pressure that will adjust the actual average linear velocity to the desired average linear velocity, and further comprising the step of applying a control signal representative of the adjusted inlet pressure to the inlet pressure valve.

6. The method of claim 1, wherein the fluid flow control is provided by a signal-controlled volumetric flow controller, and the step of determining an adjustment to the fluid flow further comprises computing an adjusted volumetric flow rate that will adjust the actual average linear velocity to the desired average linear velocity, and further comprising the step of applying a control signal representative of the adjusted volumetric flow rate to the flow controller.

7. The method of claim 1, wherein the step of determining the actual average linear velocity is performed in accordance with an actual operating condition parameter selected from the following group:

Tc=Column Temperature (Absolute Temperature),

Ts=Standard Ambient Temperature (Absolute Temperature),

Ps=Standard Ambient Pressure (referenced to 1 atm=760 torr),

d=Column diameter,

L=Column length,

p_i =Inlet Pressure,

p_o =Outlet Pressure,

μ

_o =Linear velocity of fluid at column outlet,

μ

=Average linear velocity of fluid,

F_co =column volumetric flow

η

=Fluid Viscosity.

8. The method of claim 1, wherein the relationship is provided according to the formula:

space="preserve" listing-type="equation">μ

.sub.ref ≡

μ

.sub.actual (

     8)

wherein μ

_ref =desired average linear velocity, and μ

_actual =the actual average linear velocity, respectively, of the fluid flow.

9. The method of claim 8, wherein the fluid comprises a carrier gas.

10. The method of claim 8, wherein the step of sensing a plurality of operating condition parameters includes receiving a first sense signal representative of the separation column inlet pressure p_i and a second sense signal representative of the separation column outlet pressure p_o.

11. The method of claim 10, wherein the step of sensing a plurality of operating condition parameters includes referencing one of the first sense signal and the second sense signal to a signal representative of the ambient barometric pressure p_atm.

12. The method of claim 9, wherein the relationship is provided according to the formula:

##EQU8## where;

p_i is the absolute inlet pressure, p_id is the inlet pressure provided as a desired operating condition parameter, p_o is the outlet pressure, p_or is the sensed barometric pressure, p_gd is the desired gauge pressure as a desired operating condition parameter, and p_o1atm is the outlet pressure at 1 atmosphere.

13. The method of claim 9, further comprising the steps of:

providing the fluid flow from the separation column outlet to a detector; and

combining a support gas with the fluid flow to the detector, wherein the step of sensing a plurality of operating condition parameters includes receiving a third sense signal representative of a detector support gas pressure.

14. The method of claim 9, wherein a sample is injected into said fluid through an injection port, and wherein the flow of said carrier gas is controlled upstream from said injection port.

15. The method of claim 9, wherein a sample is injected into said fluid through an injection port, and wherein the flow of said fluid is controlled downstream from said injection port.

16. Apparatus for performing a chromatographic analysis of a fluid in a separation column having an outlet subject to a barometric pressure p_atm, comprising:

fluid flow controller for providing a selectable flow of the fluid in the separation column;

a plurality of transducers for sensing a respective plurality of actual operating condition parameters to which the fluid flow is subjected, the plurality including the barometric pressure p_atm ;

means for providing information representative of a desired operating condition parameter;

a processor for;

a. determining a desired average linear velocity of the fluid flow according to the desired operating system parameter,

b. determining an actual average linear velocity of the fluid flow according to the sensed plurality of actual operating condition parameters;

c. determining, as a function of a predetermined relationship of the desired average linear velocity to the actual average linear velocity, the amount of fluid flow to cause the actual average linear velocity to substantially equal the desired average linear velocity; and

an interface for providing a control signal representative of the determined fluid flow amount to the fluid flow controller.

17. The apparatus of claim 16, wherein the information providing means further comprises an information input device.

18. The apparatus of claim 16, further comprising an information output device.

19. The apparatus of claim 16, further comprising a memory device for providing a program representing the predetermined relationship of the desired average linear velocity to the actual average linear velocity,.

20. The apparatus of claim 16, wherein the fluid flow controller further comprises an inlet pressure valve, and the determined fluid flow amount further comprises an adjusted inlet pressure.

21. The apparatus of claim 16, wherein the fluid flow controller further comprises a volumetric flow controller, and the determined fluid flow amount further comprises an adjusted volumetric flow rate.

22. The apparatus of claim 16, wherein the fluid comprises a carrier gas.

23. The apparatus of claim 16, wherein the plurality of transducers includes a pressure sensor for providing a first sense signal representative of the separation column inlet pressure p_i.

24. The apparatus of claim 23, wherein the plurality of transducers includes a pressure sensor for providing a sense signal representative of the separation column outlet pressure p_o.

25. The apparatus of claim 16, wherein the predetermined relationship is provided according to:

space="preserve" listing-type="equation">μ

.sub.ref ≡

μ

.sub.actual (

     8)

wherein μ

_ref =desired average linear velocity, and μ

_actual =the actual average linear velocity, respectively, of the fluid flow.

26. The apparatus of claim 25, wherein the predetermined relationship is further provided according to:

##EQU9##

27. The apparatus of claim 16, further comprising an injection port wherein a sample may be injected into said fluid, and wherein the fluid flow controller is located to control the fluid flow upstream from said injection port.

28. The apparatus of claim 16, further comprising an injection port wherein a sample may be injected into said fluid, and wherein the fluid flow controller is located to control the fluid flow downstream from said injection port.

29. The apparatus of claim 16, further comprising:

detector for receiving the fluid flow from the separation column outlet;

means for combining support gas with the fluid flow to the detector; and

pressure sensor for providing a sense signal representative of an actual operating parameter in the form of the detector support gas flow.