Apparatus and method for pumping supercritical fluid and measuring flow thereof

• US 5,755,559 A
• Filed: 06/26/1996
• Issued: 05/26/1998
• Est. Priority Date: 07/13/1990
• Status: Expired due to Fees

• Current Assignee: Teledyne Isco, Inc. (Thermo Fisher Scientific Incorporated)
• Original Assignee: Isco, Inc. (Teledyne Technologies Incorporated)
• Inventors: Davison, Dale A., Winter, Robin R., Jameson, Daniel Gene, Allington, Robert William, Tehrani, Yoossef, Clay, Dale
• Primary Examiner(s): Drodge, Joseph W.
• Application Number:
  US08/673,177
• Time in Patent Office: 699 Days
• Field of Search: 210/87, 210/90, 210/91, 210/136, 210/134, 210/137, 210/138, 210/143, 210/198.2, 210/634, 210/635, 210/656, 210/739, 210/741, 210/101, 417/18, 417/20, 417/22, 417/26, 417/43, 417/44.2, 417/44.6, 417/2, 417/3, 417/5, 417/15, 417/44, 417/8, 417/53, 417/437, 73/861.42, 73/861.43, 73/861.44
• US Class Current: 417/53
• CPC Class Codes: B01D 11/0203 with a supercritical fluid
• CPC Class Codes: B01D 11/0407 the supercritical fluid acting as solvent for the solute
• CPC Class Codes: B01D 15/40 using supercritical fluid as mobile phase or eluent
• CPC Class Codes: F04B 15/08 the liquids having low boiling points
• CPC Class Codes: F04B 2201/0209 Duration of piston stroke
• CPC Class Codes: F04B 2205/03 Pressure in the compression chamber
• CPC Class Codes: F04B 2205/05 Pressure after the pump outlet
• CPC Class Codes: F04B 2205/09 Flow through the pump
• CPC Class Codes: F04B 49/065 and making use of computers
• CPC Class Codes: F04B 53/08 Cooling; Heating; Preventing freezing
• CPC Class Codes: F04B 53/143 Sealing provided on the piston
• CPC Class Codes: F04B 9/042 the means being cams
• CPC Class Codes: F05B 2230/41 Hardening; Annealing
• CPC Class Codes: F05C 2201/0493 Tin
• CPC Class Codes: F05C 2253/12 Coating
• CPC Class Codes: F16K 15/1823 for ball check valves
• CPC Class Codes: G01F 1/34 by measuring pressure or differential pressure
• CPC Class Codes: G01N 1/34 Purifying; Cleaning processes or apparatus for extracting or separating nucleic acids from biological samples C12N15/1003
• CPC Class Codes: G01N 1/40 Concentrating samples
• CPC Class Codes: G01N 2001/4033 sample concentrated on a cold spot, e.g. condensation or distillation
• CPC Class Codes: G01N 2001/4061 : Solvent extraction
• CPC Class Codes: G01N 2030/6013 : interfaces to detectors
• CPC Class Codes: G01N 2035/0441 : for samples
• CPC Class Codes: G01N 30/02 : Column chromatography
• CPC Class Codes: G01N 30/28 : Control of physical parameters of the fluid carrier
• CPC Class Codes: G21F 5/015 : for storing radioactive sources, e.g. source carriers for irradiation units; Radioisotope containers

Abstract

In a piston pump for pumping liquid carbon dioxide at a temperature below 30 degrees Fahrenheit and pressures at least as high as 7500 psi, the volume leaving the pump is determined by measuring only pressure or other parameter related to flow and movement of the plunger. The position of the piston is measured and the resulting displacement is integrated to determine volume of fluid pumped.

Claims

1. A system for pumping and for measuring the outlet flow of a very compressible fluid at a predetermined flow rate and a high pressure, comprising:

a reciprocating pump having a cyclic period of fluid delivery with a start and a finish;

said reciprocating pump including a pumping chamber means adapted to contain fluid at a predetermined pressure, a movable volume-displacement means which moves cyclicly between two extreme positions for displacing a maximum and a minimum volume from the pumping chamber;

an inlet check valve, an outlet valve and an outlet line carrying the outlet fluid flow;

a flow-onset sensing means for transducing a signal related to a start of high pressure fluid flow to a first electric signal;

a sensing means for detecting the times at which the said displacement means is substantially located at one of its said extreme positions during each of the said cycles of movement;

a differentiating means for operating upon the first electric signal to produce a second electric signal dependent on rates of change in the first electric signal;

a detection means for sensing the second electric signal and for detecting a change in the rate of change of the pressure during each of said cyclic motions of the said displacement means;

a switching means turned on for a time duration by the detection means after the start of the cyclic period of fluid delivery and turned off by said second electric signal;

said displacement means having a position transducer whose output is a third electric signal proportional to displacement within the said pumping chamber; and

a time integral means which cyclicly integrates the said third electric signal during the time duration wherein the integral of the third signal is proportional to the outlet flow of the pump.

2. A system according to claim 1 in which a utilization means controls the predetermined flow rate of the fluid.

3. A system according to claim 1 wherein:

the flow-onset sensing means includes a pressure transducer means for sensing the said fluid pressure within the pumping chamber;

the differentiating means is a single differentiator, producing a first derivative signal;

the detection means includes means for detecting a change in the first derivative signal from a high positive level to a lower positive level, and;

the sensing means includes means for detecting the time at which the displacement means displaces substantially the said maximum volume from the pumping chamber.

4. A system according to claim 3 wherein:

the pressure transducer senses the fluid pressure within the outlet line;

the differentiating means is a single differentiator that produces a second electric signal proportional to the first derivative of a said pressure within the outlet line, and;

the sensing means includes means for detecting the time at which the displacement means displaces substantially at the said maximum volume from the pumping chamber.

5. A system according to claim 4 wherein the said detection means detects a change in the first derivative from a negative level to a positive level.

6. A system according to claim 1 in which the sensing means is a pressure sensor and the signal is a pressure signal.

7. A system according to claim 1 in which the sensing means is a flow meter.

8. A system according to claim 1 wherein:

the flow-onset sensing means includes a pressure transducer wherein the pressure transducer senses the fluid pressure within the pumping chamber, the differentiating means is a double differentiator providing a first and second derivative; and

, the detection means detects a change in the second derivative from a zero level to a negative level, and;

the sensing means detects the time at which the displacement means displaces substantially the said maximum volume from the pumping chamber.

9. A system according to claim 8 wherein:

the pressure transducer senses the said fluid pressure within the pumping chamber;

the differentiating means is a single differentiator which produces a second electric signal proportional to a first derivative of said pressure within the pumping chamber and;

the said detection means detects a change from the said first derivative from a small positive to a large negative value to determine the finish of fluid delivery and detects a change in the first derivative from a large positive value to a smaller positive value to determine the finish of fluid delivery.

10. A system for pumping and for measuring the outlet flow of a very compressible fluid from a high pressure pump, comprising:

a reciprocating pump having a cyclic period of fluid delivery wherein the period of flow delivery has a start and a finish, a pumping chamber containing fluid at a pressure, a movable displacement means which moves cyclicly between two extreme positions in the pumping chamber, one of said extreme positions corresponding to the finish of the cyclic period of fluid delivery, an inlet check valve, an outlet check valve and an outlet line carrying the outlet flow of fluid;

a pressure transducer means for transducing a characteristic indicating the start of fluid delivery pressure of the said high pressure fluid to a first electric signal;

a differentiating means for operating upon the first electric signal to produce a second electric signal dependent on rates of change in the first electric signal;

detection means for sensing the said second electric signal and for detecting changes in a rate of change of pumping by the high pressure pump during the said cyclic motions of the displacement means, whereby changes of the second electric signal indicate the start and finish of fluid delivery during a cycle of the pump, wherein a start of fluid delivery is determined by a change in the rate of change of the second signal after a the said finish of fluid delivery and a finish of fluid delivery is determined by an event that takes place after a start of said fluid delivery;

switch means controlled by said detection means to be turned on at said start of the period of fluid delivery and turned off at said finish of the period of fluid delivery;

said displacement means having a position transducer whose output is a third electric signal proportional to displacement within the pumping chamber;

a time integral means which cyclicly integrates the third electric signal between time limits set by the time period during which the switch means is on, and;

a utilization means which utilizes the time integral as an amount proportional to the outlet flow of fluid from the pump.

11. A system according to claim 10 in which the event is a change in the rate of change of the second electrical signal.

12. A system according to claim 10 further including a sensing means that senses one of the two extreme positions, and the event is the sensing of the one of the two extreme position of the displacement means that corresponds to the finish of flow delivery.

13. A system according to claim 10 wherein:

the pressure transducer means senses the said fluid pressure in the outlet line;

the differentiating means being a single differentiator which produces a first electric signal porportional to the first derivative of the pressure within the outlet line and;

the sensing means detects a change in said first derivative from a negative value to a positive value to determine a start of fluid delivery and detects a change in said first derivative from a postive value to a negative value to determine a finish of fluid delivery.

14. A method of pumping and measuring the outlet flow of a very compressible fluid used for supercritical extractions, comprising the steps of:

pumping fluid with a reciprocating pump having a plurality of cyclic periods of fluid delivery each of which has a start and a finish, a pumping chamber containing liquid at a pressure, a movable volume-displacement means which has a cyclic motion between two extreme positions wherein a maximum and a minimum volume are displaced from the pumping chamber;

generating a signal with a pressure transducer means which transduces the pressure of high pressure fluid flow to a first electric signal;

detecting the times at which the said displacement means is substantially located at one its said extreme positions during each of the cyclic motions;

differentiating said first electric signal with a differentiating means to produce a second electric signal dependent on rates of change in the said first electric signal;

sensing the second electric signal with a sensing means;

detecting a change in the rate of change of the said high pressure with a detection means during each of said cyclic motions of the said displacement means;

turning on a switching means for a time duration upon the detection the second electric signal after the start of the period of fluid delivery and turning off the switching means at the end of the time duration;

generating a third electric signal with a position transducer, the output of which is proportional to displacement within the said pumping chamber;

cyclicly integrating the third electric signal between time limits set by the said time duration during which the said switching means is on wherein an integral of the third electric signal is obtained; and

utilizing the integral of the third electric signal as an amount proportional to the outlet flow of the pump.

15. A method according to claim 14 wherein:

the pressure transducer means senses the said fluid pressure within the pumping chamber;

the differentiating means produces a first derivative signal;

the detection means detects a change in the said first derivative signal from a high positive level to a lower positive level; and

the sensing means detects the time at which the displacement means displaces substantially the said maximum volume from the pumping chamber.

16. A method according to claim 14 wherein:

the pressure transducer means senses the said fluid pressure within the pumping chamber;

double differentiating the signal;

detecting a change in the second derivative from a zero level to a negative level, and;

detecting the time at which the displacement means displaces substantially the said maximum volume from the pumping chamber.

17. A method according to claim 14 wherein the pressure transducer senses the said fluid pressure within the outlet line;

the said differentiating means producing a second electric signal proportional to the first derivative of the said pressure within the outlet line, and;

detecting the time at which the displacement means displaces substantially at the said maximum volume from the pumping chamber.

18. A method according to claim 14 wherein the said detection means detects a change in the said first derivative from a negative level to a positive level.

19. A method for pumping and measuring the outlet flow of a very compressible fluid used for supercritical extraction, comprising the steps of:

pumping fluid with a reciprocating pump having a plurality of cyclic periods of fluid delivery each of which has a start and a finish;

said step of pumping including the substeps of moving a movable displacement means which has cyclic motions between two extreme positions in a pumping chamber, to pump into an outlet line carrying the outlet flow;

transducing the pressure of the said high pressure fluid to a first electric signal;

producing a second electric signal dependent on rates of change in the said first electric signal;

sensing the said second electric signal and detecting changes in the rate of change of the said high pressure during the said cyclic motions of the said displacement means, wherein the changes in the second electric signal indicate the start and finish of fluid delivery during a cycle of the pump,

determining said start of fluid delivery by a change in the rate of change of the said second signal after a said finish of fluid delivery and determining said finish of fluid delivery by a change in the rate of change of the said second signal after a start of said fluid delivery;

turning on switch means in response to said detection means at the said start of the period of fluid delivery and turning off the switch means at the finish of the period of fluid delivery;

generating a second electric signal on said displacement means with a position transduceer proportional to displacement within the said pumping chamber;

cyclicly integrating the second electric signal between time limits set by the time period during which the said switch means is on, and;

utilizing the said integral as an amount proportional to the outlet flow of the pump.

20. A method according to claim 19 further comprising the steps of:

sensing the fluid pressure within the pumping chamber and producing a second electric signal proportional to the first derivative of said pressure within the pumping chamber and;

detecting a change from the said first derivative from a small positive to a large negative value to determine the finish of fluid delivery; and

detecting a change in the said first derivative from a large positive value to a smaller positive value to determine the finish of fluid delivery.

21. A method according to claim 20 further comprising the steps of:

sensing said fluid pressure in the outlet line;

producing a first electric signal proportional to the first derivative of the fluid pressure within the outlet line by differentiating said pressure and;

detecting a change in the said first derivative from a negative value to a positive value for determining a start of fluid delivery and detecting a change in the said first derivative from a positive value to a negative value for determining a finish of fluid delivery.