Multiple solvent delivery system

• US 5,360,320 A
• Filed: 02/27/1992
• Issued: 11/01/1994
• Est. Priority Date: 02/27/1992
• Status: Expired due to Term

• Current Assignee: Teledyne Isco, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Isco, Inc. (Teledyne Technologies Incorporated)
• Inventors: Allington, Robert W., Jameson, Daniel G.
• Primary Examiner(s): Bertsch, Richard A.
• Assistant Examiner(s): MCANDREWS JR, ROLAND G
• Application Number:
  US07/843,624
• Time in Patent Office: 978 Days
• Field of Search: 417/2, 417/3, 417/4, 417/5, 417/6, 417/7, 417/18, 417/44 A, 417/53, 417/63, 417/45
• US Class Current: 417/4
• CPC Class Codes: G01N 30/34 of fluid composition, e.g. gradient G01N30/36 takes precedence
• CPC Class Codes: G05D 11/131 by measuring the values related to the quantity of the individual components G05D11/139 takes precedence

Abstract

To control a solvent composition in a supercritical fluid system, a first pump pumps a first solvent through a first conduit into a mixer and a second pump pumps a second solvent through a second conduit into the mixer. First and second transducers measure the pressure in the first and second conduits and generate first and second signals proportional to the pressures. Each pressure signal is multiplied by a corresponding programmed concentration signal and compared to the programmed pressure in a feedback system to generate an error signal. The error signal is multiplied by concentration signals from a programmer to control the pumping rate of each pump. The pumps pressurize each fluid one at a time at the start of a run. The pressurization process is also used for producing disturbance-free flow as delivery is changed from one pump to another during prolonged runs.

Claims

1. A supercritical fluid extraction system, comprising:

a supercritical fluid extraction means;

multi-solvent delivery means for supplying a gradient of comparable solvents at a controlled pressure and converting to a pressure vessel communicating with said supercritical fluid extraction means;

said multi-solvent delivery means for supplying including;

a source of a first solvent;

first means for pumping the first solvent through a first pump outlet into a first conduit;

a second solvent;

second means for pumping the second solvent through a second outlet into a second conduit;

first transducer means for measuring the pressure in said first conduit and generating a first signal proportional to the pressure and for measuring the pressure in said second conduit and generating a second signal proportional to the pressure;

mixer means communicating with said first and second conduits for mixing said first and second solvents and applying the mixed solvent solution to said supercritical fluid extraction system;

programmed means for generating third and fourth electrical signals representing programmed concentration of said first and second solvents respectively in said mixed solvent solution applied to said supercritical fluid extraction system;

means for generating a fifth signal representing a programmed pressure;

means for multiplying said first signal by said third signal, wherein a sixth signal proportional to said pressure in said first conduit multiplied by the programmed concentration of the first solvent in the mixed solvent solution is generated;

means for multiplying said second signal by said fourth signal, wherein a seventh signal proportional to the programmed concentration of said second solvent in the mixed solvent solution multiplied by said pressure in said second conduit is generated;

means for adding said sixth and seventh signals;

feedback comparison means for comparing the sum of said sixth and seventh signals with said signal representing the programmed pressure to generate an error signal;

means for multiplying said error signal by said third signal and supplying it to said first means for pumping to control said pumping rate wherein the pumping rate of the said first means is maintained in programmed concentration proportion to the flow rate at a pressure equal to said programmed pressure; and

means for multiplying the error signal by said fourth signal to generate a signal for controlling said second means for pumping, wherein the second means for pumping pumps at a rate of programmed concentration proportion to the flow rate at the programmed pressure, whereby said mixture of solvents is controlled at a programmed concentration of solvents at a programmed pressure.

2. A multi-solvent delivery system comprising:

first means for pumping a first solvent through a first pump outlet into a first conduit;

second means for pumping a second solvent through a second outlet into a second conduit;

first transducer means for measuring pressure in said first conduit and generating a first signal proportional to the pressure;

second transducer means for measuring pressure in said second conduit and converting it to a second pressure signal;

mixer means communicating with said first and second conduits for mixing said first and second solvents and applying the mixed solvents to an outlet port;

programmed means for generating third and fourth electrical signals representing proportions of said first and second solvents in said mixture applied to said mixer outlet port;

means for generating a fifth signal representing programmed pressure;

means for multiplying said first signal by said third signal wherein a sixth signal proportional to said pressure in said first conduit multiplied by the proportion of solvent to be programmed in said first solvent is generated;

means for multiplying said second signal by said fourth signal to generate a seventh signal representing the fraction of said second solvent multiplied by said pressure in said second conduit;

means for adding said sixth and seventh signals;

feedback comparison means for comparing the sum of said sixth and seventh signals with said signal representing the programmed pressure to generate an error signal;

means for multiplying said error signal by said third signal and supplying it to said first means for pumping to control said pumping rate wherein the pumping rate is maintained in concentration proportion to the flow rate at a pressure equal to said programmed pressure; and

means for multiplying the error signal by said fourth signal to generate a signal for controlling said second means for pumping wherein the second means for pumping pumps at a rate in concentration proportion to the flow rate at a pressure equal to the said programmed pressure, whereby said mixture of solvents is controlled in a programmed concentration of solvents at a programmed pressure.

3. A method of supplying a supercritical system with a programmed plurality of solvents comprising the steps of:

pumping a first fluid with a first pump up to a valve upstream of the supercritical system;

pumping a second fluid from a second pump to the same valve;

measuring pressure in a first conduit connecting an outlet port of said first pump to said valve to obtain a first signal;

measuring pressure in a second conduit between an outlet port of the second pump and the valve to obtain a second signal;

multiplying the first signal by a third signal representing the concentration of the first fluid in the total fluid mixture to obtain a fourth signal;

multiplying the second signal by a program signal;

representing the concentration of the second fluid in the total mixture to generate a fifth signal;

comparing said fourth signal with a pressure reference point and using an error signal to control said first pump, whereby the first fluid is controlled; and

comparing the fourth signal with said pressure reference point and using the error signal to control said second pump whereby the second fluid is controlled.

4. A fluid control system comprising:

a plurality of pumps delivering fluid into a common mixing conduit;

a back-flow-preventing check valve between the pump fluid outlet and the mixer on all but one of the pumps which is the primary fluid delivery pump;

means to control the pressurization of said pumps so as to ramp the pressures of the secondary pumps to match the pressure of the primary fluid delivery pump;

pressure transducer means for measuring the pressure in the common mixing conduit downstream of the back flow preventing check valves and generating a signal proportional to the pressure;

means for detecting fluctuations of said pressure signal indicating the pressure equalization of a secondary pump; and

means to control the fluid delivery of the pumps at a controlled pressure or flow rate after the pressure are detected to be equal.

5. A fluid control system comprising:

at least first and second pump means;

a first fluid source adapted to be pumped by said first pump means;

a second fluid source adapted to be pumped by said second pump means;

a first fluid output line connected to said first pump means;

a second fluid output line connected to said second pump means;

a first check valve adapted to permit flow from said first output line into a mixer;

a second check valve adapted to permit flow from said second output line to said mixer;

a first pressure transducer in said first output line;

a second pressure transducer in said second output line;

means for detecting a sudden change in a characteristic of the pressure from one of said first and second transducers, whereby a signal is provided indicating an opening of a check valve; and

means for starting a refill cycle of one of said first and second pumps in timed relation with detection of said signal.

6. A fluid control system comprising:

at least first and second pump means;

a first fluid source adapted to be pumped by said first pump means;

a second fluid source adapted to be pumped by said second pump means;

a first fluid output line connected to said first pump means;

a second fluid output line connected to said second pump means;

a first check valve adapted to permit flow from said first output line into a mixer;

a second check valve adapted to permit flow from said second output line to said mixer;

a first pressure transducer in said first output line;

a second pressure transducer in said second output line; and

means for detecting a sudden change in a characteristic of the pressure from one of said first and second transducers, whereby an opening of a check valve is detected.

7. A fluid control system according to claim 6 in which the detected opening of a check valve causes the speed of a corresponding pump to be changed to a programmed pumping rate.

8. A fluid control system comprising:

a plurality of pumps;

a corresponding plurality of check valves; and

means for causing delivery pressures of at least two of said plurality of pumps to match by detecting that their corresponding opening to a common fluid port have opened;

said means for causing delivery pressures of at least two of said plurality of pumps to match includes means for forcing the pressures to match by connecting pressure transducers to the common fluid port by means of a manual or automatic valve.

9. A fluid control system according to claim 8 in which said means for causing delivery pressures of at least two of said plurality of pumps to match by detecting that their corresponding check valves to a common fluid port have opened comprises means for forcing said check valves to open by pumping fluid through the check valves.

10. A fluid control system comprising:

a plurality of pumps;

a corresponding plurality of check valves; and

means for causing delivery pressures of at least two of said plurality of pumps to match by detecting that their corresponding opening to a common fluid port have opened; and

means for adjusting the pressures signals of a plurality of transducers to match wile the pumps are known to be at the same delivery pressure.

11. A fluid control system according to claim 10 further including means for using the pressure matching information to shorten the time and improve the accuracy of pressure matching for the purpose of equilibrating pressures from pump stroke to pump stroke in a multiple pump fluid delivery system.

12. A method of applying solvent to a supercritical fluid system comprising the steps of:

applying a first fluid from a first pump to a valve located upstream of the supercritical fluid system until pressure in the flow path reaches a predetermined setpoint pressure value;

controlling the pressure of the first fluid by a feedback circuit from a transducer in the flow path between a second pump and the valve at said setpoint pressure;

automatically opening said valve to permit the flow to the downstream side of said supercritical fluid system; and

pumping fluid until pressure has stabilized and continuing the pumping until the supercritical process is completed.

13. A method according to claim 12 further comprising the steps of:

blocking said fluid downstream of said supercritical fluid system with a second valve;

pumping a second fluid to a pressure a predetermined increment of pressure below a preset pressure;

opening said second valve; and

increasing the pressure of said second fluid to said preset pressure value, wherein the pressure of said second fluid is controlled by a feedback system having a transducer in the flow path between the second pump and said first valve.

14. A method in accordance with claim 13 further including the step of pumping the first and second fluids in a constant flow mode after said first and second fluids are flowing and said second valve has been opened.

15. A method in accordance with claim 13 further including the step of pumping the first and second fluids in a constant pressure mode after said first and second fluids are flowing and said second valve has been opened.

16. A method in accordance with claim 13 wherein the step of controlling the second pump includes the substeps of multiplying pressure in a conduit between said second pump and said first valve by a programmed proportion of final fluid mixture to be sent to the supercritical system which is a ratio of said second fluid to the programmed total fluid to form a product, comparing the product to the setpoint value and controlling the pumping rate of pumping of said first pump with an error signal from the comparison multiplied by the proportion of said first fluid to the total fluid.

17. A fluid control system comprising:

at least first and second pump means;

a first fluid source adapted to be pumped by said first pump means;

a second fluid source adapted to be pumped by said second pump means;

a first outlet conduit connected to said first pump means;

a second outlet conduit connected to said second pump means;

means for combining fluid flow from said first and second conduits to obtain combined fluids;

means for obtaining a first signal representing a pressure of the combined fluids;

means for comparing the first signal with a reference pressure signal to obtain an error signal;

program means for generating a second signal representing a programmed concentration of the first fluid in the combined fluids to be pumped by said first pump means into said first conduit and for generating a third signal representing a programmed concentration of the second fluid in the combined fluids to be pumped by said second pump means into said second conduit;

means for multiplying said error signal by said second signal to obtain a fourth signal and using said fourth signal to control a pumping rate of the first pump means; and

means for multiplying said error signal by said third signal to obtain a fifth signal and using the fifth signal to control a flow rate of said second pump means, whereby the concentration and pressure of said combined fluids is controlled.

18. A fluid control system in accordance with claim 17 in which:

said means for generating a signal representing the pressure of said combined fluids includes a first transducer means for measuring the pressure in the first outlet conduit of said first pump means;

means for multiplying said pressure signal by said third signal;

second transducer means for measuring the outlet pressure of said second pump means;

means for multiplying a signal from said second transducer means by the fourth signal; and

means for combining said third and fourth signals, whereby a signal representing the pressure of the combined flow rates is obtained from pressure signals at the outlet of each of a plurality of pumps.

19. A fluid control system in accordance with claim 17 in which the fluid control system is adapted to supply fluid to an apparatus for utilizing the fluid and the fluid control system includes:

a first valve in a flow circuit between said means for combining fluid flow and said apparatus utilizing the fluid; and

means for closing said valve during start-up of the fluid control system.

20. A fluid control system in accordance with claim 19 further including a second valve means communicating with an outlet of said apparatus for utilizing said fluids adapted to be closed during a second stage of the start-up procedure of said fluid control system.

21. A fluid control system in accordance with claim 20 further comprising:

a first check valve connected to said first outlet conduit downstream of said means for obtaining a first signal and upstream of said means for combining fluid flow from said first and second conduits; and

second check valve means communicating with said second outlet conduit downstream from said means for obtaining a second signal and upstream from said means for combining fluids, whereby said first and second check valves permit flow from said first and second outlet conduit means into said means for combining fluids and restrict flow from said means for combining fluids to said first and second pump means respectively.

22. A fluid control system according to claim 21 further including means for detecting when said first outlet conduit reaches the programmed pressure and beginning an increase in pressure in said second outlet conduit.