IP Library Granted Patent US 9,539,524
Granted Patent B2
US 9,539,524 · App. 14/333,661 · Granted Jan 10, 2017

Pump and injector for liquid chromatography

Inventors: Stanley D. Stearns (Houston, TX); Ales Plistil (Houston, TX)
Assignee: Valco Instruments Company, L.P.
B01D15/14F04B19/006Y10T137/85978
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Quick Facts
Patent No.
US 9,539,524
App. No.
14/333,661
Granted
Jan 10, 2017
Kind
B2
Abstract

A combined dual pump-injector valve utilizing a single piece of material to house the barrel for each of the two piston-based pumps and to provide the stator of the associated valve, thus eliminating any need for connections between the pumps and the valve, and therefore eliminating the potential for high-pressure leaks or pressure reductions. The combined dual pump-injector valve permits injection of nanoliter-sized samples into a chromatographic column such that complete analyses can be completed with microliters of mobile phase with nanoliters of a sample.

Claims (113)

1. An integral nano-scale pump and injection valve system ( 100 ) for high performance liquid chromatography comprising:

an integrated barrel-stator ( 110 ), said integrated barrel-stator ( 110 ) having a first elongate barrel ( 116 ), a second elongate barrel ( 116 B), and a stator ( 210 ) integrally formed of a single piece of monolithic material, said integrated barrel-stator ( 110 ) having an integrated barrel-stator first section ( 220 ) and an integrated stator barrel second section ( 222 ),

said stator ( 210 ) having a stator first side ( 240 ),

said first elongate barrel ( 116 ) having a first elongate barrel first open end ( 430 ) in said integrated barrel-stator first section ( 220 ) and a second open end ( 2704 ) at said integrated stator barrel-stator second section ( 222 ), and a sidewall ( 2708 ) defining a first interior chamber ( 208 ) adapted to receive a supply of fluid at second open end ( 2704 ),

said first elongate barrel second open end ( 2704 ) at said stator first side ( 240 ) and providing a second stator orifice ( 2814 ),

said second elongate barrel ( 116 B) having a second elongate barrel first open end ( 430 B) in said integrated stator barrel first section ( 220 ) and a second elongate barrel second open end ( 2704 ) at said integrated barrel-stator second section ( 222 ), and a second elongate barrel sidewall ( 2708 B) defining an second interior chamber ( 208 B) adapted to receive a supply of fluid at first open end ( 2704 B),

said second elongate barrel second open end ( 2704 B) at said stator first side ( 240 ) and providing a first stator orifice ( 2812 ),

said stator ( 210 ) having a first stator fluid supply port ( 2806 ) for communication with a liquid supply and having a second stator fluid supply port ( 2810 ) for communication with a liquid supply,

said stator ( 210 ) having a third stator port ( 2804 ) and having a fourth stator port ( 2808 ),

said stator ( 210 ) in contact at a surface of a stator lace ( 2802 ) with a surface of a rotor face ( 602 ) of a rotor ( 214 ), said stator ( 210 ) adapted to communicate with said rotor ( 214 ) at said first stator fluid supply port ( 2806 ) and adapted to communicate with said rotor ( 214 ) at said second stator fluid supply port ( 2810 ), said first stator orifice ( 2812 ) and said second stator orifice ( 2814 ) being non-overlapping;

a first longitudinal plunger ( 206 ) slidably disposed within said first interior chamber ( 208 ), said first longitudinal plunger ( 206 ) being of substantially uniform cross section, a second longitudinal plunger ( 206 B) slidably disposed within said second interior chamber ( 208 B), said second longitudinal plunger ( 206 B) being of substantially uniform cross section,

said rotor ( 214 ) having a first channel ( 604 ) in said rotor face ( 602 ) and a second channel ( 612 ) in said rotor face ( 602 ),

said rotor ( 214 ) rotable with respect to said stator ( 210 ) about a centerpoint of said stator ( 210 ) between a load position ( 202 ) and an injection position ( 302 ),

said load position ( 202 ) defined by said second stator orifice ( 2814 ) in communication with said first stator fluid supply port ( 2806 ) via said first channel ( 2904 ) and said first stator orifice ( 2812 ) in communication with said second stator fluid supply port ( 2810 ) via said second channel ( 2906 ), and

said injection ( 302 ) position defined by said second stator orifice ( 2814 ) in communication with said third stator port ( 2804 ) via said first channel ( 2904 ) and said first stator orifice ( 2812 ) in communication with said fourth stator port ( 2808 ) via said second channel ( 2906 ).

2. The integral nano-scale pump and injection valve system of claim 1 further comprising:

a first hard plastic seal ( 406 ) about said first longitudinal plunger ( 206 ) sized to it within said first elongate barrel ( 116 ) and to fit about said first longitudinal plunger ( 206 ) without contacting said first longitudinal plunger ( 206 );

a flexible seal ( 408 ) about said first longitudinal plunger ( 206 ) sized to fit within said first elongate barrel ( 116 ) and to fit about said first longitudinal plunger ( 206 ) adjacent said first hard plastic seal ( 406 );

a second hard plastic seal ( 410 ) about said first longitudinal plunger ( 206 ) sized to fit within said first elongate barrel ( 116 ) and to fit about said first longitudinal plunger ( 206 ) without contacting said first longitudinal plunger ( 206 ) and adjacent said flexible seal ( 408 );

a driving disk ( 412 ) having a bore therethrough sized to fit about said first longitudinal plunger ( 206 ) without interference, said driving disk ( 412 ) having a driving disk first end ( 428 ) and a driving disk second end ( 426 ), said driving disk ( 412 ) sized to freely fit within said integrated barrel-stator ( 110 ) adjacent first elongate barrel ( 116 ), said driving disk having a shoulder ( 422 ) near said driving disk first end ( 428 ), and a neck ( 424 ) at said driving disk second end ( 426 ), said neck ( 424 ) sized to fit within first elongate barrel ( 116 ) and to contact said first hard plastic seal ( 406 );

a sleeve with external threads ( 416 ) having a bore therethrough sized to permit movement of said first longitudinal plunger ( 206 ) without interference, said sleeve with external threads ( 416 ) sized to a sleeve with internal threads ( 432 ) within said integrated barrel-stator ( 110 ) adjacent said first elongate barrel ( 116 ); and

a spring ( 418 ) contacting said shoulder ( 422 ) of said driving disk ( 412 ) and an end of said sleeve with external threads ( 416 ).

3. The integral nano-scale pump and injection valve system of claim 2 , further comprising a first pump actuator ( 108 ) associated with a plunger-driving piston ( 212 ) attached to said first longitudinal plunger ( 206 ).

4. The integral nano-scale pump and injection valve system of claim 3 , further comprising a valve actuator associated with a driveshaft ( 216 ) attached to said rotor ( 214 ).

5. The integral nano-scale pump and injection valve of claim 2 further comprising:

said stator ( 210 ) having a fifth stator port ( 508 ), a sixth stator port ( 510 ), a seventh stator port ( 512 ), an eighth stator port ( 514 ), a ninth stator port ( 516 ) and a tenth stator port ( 518 );

said rotor ( 214 ) having a third rotor slot ( 606 ) in said rotor face ( 602 ), a fourth rotor slot ( 608 ) in said rotor face ( 602 ) and a fifth rotor slot ( 610 ) in said rotor face ( 602 ); and

wherein said load position further comprises

said third stator port ( 504 ) adapted for communication via a first external connector ( 706 a ) with a three-way connector ( 708 ), said fourth stator port ( 520 ) adapted for communication via a second external connector ( 706 b ) with said three-way connector ( 708 ); and said fifth stator port ( 508 ) adapted for communication via a third external connector ( 706 c ) with said three-way connector ( 708 );

said sixth stator port ( 510 ) in communication with said seventh stator port ( 512 ) via said third rotor slot ( 606 ), said seventh stator port ( 512 ) adapted for communication with a sample loop return;

said eighth stator port ( 514 ) adapted for communication with a fluid sample source and in communication with said ninth stator port ( 516 ) via said fourth rotor slot ( 608 );

said ninth stator port ( 516 ) adapted for communication with said sixth stator port ( 510 ) via an external sample loop ( 702 );

said tenth stator port ( 518 ) adapted for communication with an input to a chromatographic device ( 704 ) and in communication with said fifth rotor slot ( 610 );

and wherein said injection position further comprises:

said third stator port ( 504 ) in communication via said first external connector ( 706 a ) with said three-way connector ( 708 ), said fourth stator port ( 520 ) in communication via said second external connector ( 706 b ) with said three-way connector ( 708 ); and said fifth stator port ( 508 ) in communication via said third external connector ( 706 c ) with said three-way connector ( 708 )

said fifth stator port ( 508 ) in communication with said sixth stator port ( 510 ) via said third rotor slot ( 606 );

said sixth stator port ( 510 ) in communication with said ninth stator port ( 516 ) via said external sample loop ( 702 );

said ninth stator port ( 516 ) in communication with said tenth stator port ( 518 ) via said fifth rotor slot ( 610 );

said eighth stator port ( 514 ) adapted for communication with said fluid sample source and in communication with said seventh stator port ( 512 ) via said fourth rotor slot ( 608 );

said seventh stator port ( 512 ) adapted for communication with a sample loop return; and

said tenth stator port ( 518 ) adapted for communication with said input to said chromatographic device ( 704 ).

6. The integral nano-scale pump and injection valve of claim 5 , wherein said third external connector is a static mixer.

7. The integral nano-scale pump and injection valve system of claim 5 , further comprising a first pump actuator ( 108 ) associated with a plunger-driving piston ( 212 ) attached to said first longitudinal plunger ( 206 ).

8. The integral nano-scale pump and injection valve system of claim 7 , further comprising a valve actuator associated with a driveshaft ( 216 ) attached to said rotor ( 214 ).

9. The integral nano-scale pump and injection valve system of claim 5 , further comprising

said chromatographic device ( 1104 ) being a chromatographic column ( 1104 );

said stator ( 210 ) having an eleventh stator port ( 928 ), a twelfth stator port ( 930 ), and a thirteen stator port ( 932 ); and

said rotor ( 214 ) having a sixth rotor slot ( 1014 );

wherein said load position ( 202 ) further comprises

said eleventh stator port ( 928 ) being adapted to communicate to an input of a chromatographic detector ( 1106 );

said twelfth stator port ( 930 ) being adapted to receive an output of said chromatographic column ( 1104 );

said twelfth stator port ( 930 ) in communication with thirteenth stator port ( 932 ) via said sixth rotor slot ( 1014 );

and wherein said injection position ( 302 ) further comprises

said twelfth stator port ( 930 ) being adapted to receive an output of said chromatographic column ( 1104 );

said twelfth stator port ( 930 ) in communication with said eleventh stator port ( 928 ) via said sixth rotor slot ( 1014 ); and

said eleventh stator port ( 928 ) being adapted to communicate to an input of a chromatographic detector ( 1106 ).

10. The integral nano-scale pump and injection valve system of claim 9 , further comprising a first pump actuator ( 108 ) associated with a plunger-driving piston ( 2 ) attached to said first longitudinal plunger ( 206 ).

11. The integral nano-scale pump and injection valve system of claim 10 , further comprising a valve actuator associated with a driveshaft ( 216 ) attached to said rotor ( 214 ).

12. The integral nano-scale pump and injection valve system of claim 2 further comprising:

said stator ( 210 ) having a fifth stator port ( 1308 ), a sixth stator port ( 1310 ), a seventh stator port ( 1312 ), and an eighth stator port ( 1314 );

said rotor ( 214 ) having a third rotor slot ( 606 ) in said rotor face ( 602 ), and

wherein said load position further comprises:

said third stator port ( 1304 ) adapted for communication via a first external connector ( 1506 a ) with a three-way connector ( 1508 ), said fourth stator port ( 1316 ) adapted for communication via a second external connector ( 1506 b ) with said three-way connector ( 1508 ), said sixth stator port ( 1310 ) adapted for communication via a third external connector ( 706 c ) with said three-way connector ( 1508 );

said fifth stator port ( 1308 ) adapted for communication with an input to a chromatographic device ( 704 );

said eighth stator port ( 1314 ) adapted for communication with a fluid sample source and in communication with said seventh stator port ( 1312 ) via said third rotor slot ( 1406 );

and wherein said injection position further comprises:

said third stator port ( 1304 ) in communication via said first external connector ( 1506 ) with said three-way connector ( 1508 ), said fourth stator port ( 1316 ) in communication via said second external connector ( 1506 b ) with said three-way connector ( 1508 ), said sixth stator port ( 1310 ) in communication via said third external connector ( 706 c ) with said three-way connector ( 1508 );

said sixth stator port ( 1310 ) in communication with said fifth stator port ( 1308 ) via said third rotor slot ( 1406 );

said fifth stator port ( 1308 ) adapted for communication with said input to said chromatographic device ( 704 ); and

wherein said third rotor slot ( 1406 ) is adapted to contain said sample for processing.

13. The integral nano-scale pump and injection valve system of claim 12 , further comprising a first pump actuator ( 108 ) associated with a plunger-driving piston ( 212 ) attached to said first longitudinal plunger ( 206 ).

14. The integral nano-scale pump and injection valve system of claim 13 , further comprising a valve actuator associated with a driveshaft ( 216 ) attached to said rotor ( 214 ).

15. The integral nano-scale pump and injection valve system of claim 12 further comprising:

said chromatographic device ( 1904 ) being a chromatographic column ( 1904 );

said stator ( 210 ) having a ninth stator port ( 1724 ) and a tenth stator port ( 1726 );

said rotor ( 214 ) having a fourth rotor slot ( 1810 ) in said rotor face ( 602 ); and

wherein said load position ( 202 ) further comprises:

said tenth stator port ( 1726 ) being adapted to receive an output of said chromatographic column ( 1904 );

said ninth stator port ( 1724 ) being adapted to communicate to an input of a chromatographic detector ( 1906 );

wherein said injection position ( 302 ) further comprises:

said tenth stator port ( 1726 ) being adapted to receive an output of said chromatographic column ( 1904 );

said tenth stator port ( 1726 ) in communication with said ninth stator port ( 1724 ) via said fourth rotor slot ( 1810 ); and

said ninth stator port ( 1724 ) being adapted to communicate to an input of a chromatographic detector ( 1106 ).

16. The integral nano-scale pump and injection valve system of claim 15 , further comprising a first pump actuator ( 108 ) associated with a plunger-driving piston ( 212 ) attached to said first longitudinal plunger ( 206 ).

17. The integral nano-scale pump and injection valve system of claim 16 , further comprising a valve actuator associated with a driveshaft ( 216 ) attached to said rotor ( 214 ).

18. The integral nano-scale pump and injection valve of claim 12 , wherein said third external connector is a static mixer.

19. An integral nano-scale pump and injection valve system ( 100 ) for high performance liquid chromatography comprising:

an integrated barrel-stator ( 110 ), said integrated barrel-stator ( 110 ) having a first elongate barrel ( 116 ), a second elongate barrel ( 116 B), and a stator ( 216 ) integrally formed of a single piece of monolithic material, said integrated barrel stator ( 110 ) having an integrated barrel-stator first section ( 220 ) and an integrated stator barrel second section ( 222 ),

said stator ( 210 ) having a stator first side ( 240 ),

said first elongate barrel ( 116 ) having a first elongate barrel first open end ( 430 ) in said integrated stator barrel first section ( 220 ) and a second open end ( 2704 ) at said integrated barrel-stator second section ( 222 ), and a sidewall ( 2708 ) defining a first interior chamber ( 208 ) adapted to receive a supply of fluid at second open end ( 2704 ),

said first elongate barrel second open end ( 2704 ) at said stator first side ( 240 ) and providing a second stator orifice ( 2112 ),

said second elongate barrel ( 116 B) having a second elongate barrel first open end ( 430 B) in said integrated stator barrel first section ( 220 ) and a second elongate barrel second open end ( 2704 ) at said integrated barrel-stator second section ( 222 ), and a second elongate barrel sidewall ( 2708 B) defining an second interior chamber ( 208 B) adapted to receive a supply of fluid at first open end ( 2704 B),

said second elongate barrel second open end ( 2704 B) at said stator first side ( 240 ) and providing a first stator orifice ( 2110 );

said stator ( 210 ) having a first stator fluid supply port ( 2102 ) for communication with a liquid supply and having a second stator fluid supply port ( 2108 ) for communication with a liquid supply,

said stator ( 210 ) having a third stator port ( 2104 ) and having a fourth stator port ( 2106 ),

said stator ( 210 ) in contact at a surface of a stator face ( 502 ) with a surface of a rotor face ( 602 ) of a rotor ( 214 ), said stator ( 210 ) adapted to communicate with said rotor ( 214 ) at said first stator fluid supply port ( 2102 ) and adapted to communicate with said rotor ( 214 ) at said second stator fluid supply port ( 2108 ), said first stator orifice ( 2110 ) and said second stator orifice ( 2112 ) being non overlapping;

a first longitudinal plunger ( 206 ) slidably disposed within said first interior chamber ( 208 ), said first longitudinal plunger ( 206 ) being of substantially uniform cross section;

a second longitudinal plunger ( 206 B) slidably disposed within said second interior chamber ( 208 B), said second longitudinal plunger ( 206 B) being of substantially uniform cross section;

said rotor ( 214 ) having a first channel ( 604 ) in said rotor face ( 602 ) and a second channel ( 612 ) in said rotor face ( 602 );

said rotor ( 214 ) rotable with respect to said stator ( 210 ) about a centerpoint of said stator ( 210 ) among a first position ( 2306 ) in which said first pump ( 118 ) is dispensing while said second pump ( 120 ) is loading, a second position ( 2406 ) in which said first pump ( 118 ) is dispensing and said second pump ( 120 ) is dispensing and a third position ( 2506 ) in which said first pump ( 118 ) is loading while said second pump ( 120 ) is dispensing;

said first position ( 2306 ) defined by said second stator orifice ( 2112 ) in communication with said third stator port-and-slot ( 2104 ) via said first rotor slot ( 2204 ), said third stator port-and-slot ( 2104 ) adapted for communication with a three-way connector output ( 2304 ), said first stator orifice ( 2110 ) in communication with said second stator port ( 2108 ) via said second rotor slot ( 2206 ), and said third stator port ( 2108 ) adapted for communication with a supply ( 2302 );

said second position ( 2406 ) defined by said second stator orifice ( 2112 ) in communication with said third stator port-and-slot ( 2104 ) via said first rotor slot ( 2204 ), said third stator port-and-slot ( 2104 ) adapted for communication with said three-way connector output ( 2304 ), said first stator orifice ( 2110 ) in communication with said fourth stator port-and-slot ( 2106 ) via said second rotor slot ( 2206 ), said fourth stator port-and-slot ( 2106 ) adapted for communication with said three-way connector output ( 2304 ), and

said third position ( 2506 ) defined by said second stator orifice ( 2112 ) in communication with said third stator port-and-slot ( 2102 ) via said first rotor slot ( 2204 ), said first stator port-and-slot ( 2102 ) adapted for communication with a supply ( 2302 ), said first stator orifice ( 2110 ) in communication with said fourth stator port-and-slot ( 2106 ) via said second rotor slot ( 2206 ), said fourth stator port-and-slot ( 2106 ) adapted for communication with said three-way connector output ( 2304 ).

20. The integral nano-scale pump and injection valve system of claim 19 further comprising:

a first hard plastic seal ( 406 ) about said first longitudinal plunger ( 206 ) sized to fit within said first elongate barrel ( 116 ) and to fit about said first longitudinal plunger ( 206 ) without contacting said first longitudinal plunger ( 206 );

a flexible seal ( 408 ) about said first longitudinal plunger ( 206 ) sized to fit within a first elongate barrel ( 116 ) and to fit about said first longitudinal plunger ( 206 ) adjacent said first hard plastic seal ( 406 );

a second hard plastic seal ( 410 ) about said first longitudinal plunger ( 206 ) sized to fit within first elongate barrel ( 116 ) and to fit about said first longitudinal plunger ( 206 ) without contacting said first longitudinal plunger ( 206 ), and adjacent said flexible seal ( 408 );

a driving disk ( 412 ) having a bore therethrough sized to fit about said first longitudinal plunger ( 206 ) without interference, a driving disk first end ( 428 ) and a driving disk second end ( 426 ), said driving disk ( 412 ) sized to freely fit within said integrated barrel-stator ( 110 ) adjacent first elongate barrel ( 116 ), said driving disk having a shoulder ( 422 ) near said driving disk first end ( 428 ), and a neck ( 424 ) at said driving disk second end ( 426 ), said neck ( 424 ) sized to fit within first elongate barrel ( 116 ) and to contact said first hard plastic seal ( 406 );

a sleeve with external threads ( 416 ) having a bore therethrough sized to permit movement of said first longitudinal plunger ( 206 ) without interference, said sleeve with external threads ( 416 ) sized to a sleeve with internal threads ( 432 ) within said integrated barrel-stator ( 110 ) adjacent said first elongate barrel ( 116 ); and

a spring ( 418 ) contacting said shoulder ( 422 ) of said driving disk ( 412 ) and an end of said sleeve with external threads ( 416 ).

21. The integral nano-scale pump and injection valve system of claim 20 , further comprising a first pump actuator ( 108 ) associated with a plunger-driving piston ( 212 ) attached to said first longitudinal plunger ( 206 ).

22. The integral nano-scale pump and injection valve system of claim 21 , further comprising a valve actuator associated with a driveshaft ( 216 ) attached to said rotor ( 214 ).

23. The integral nano-scale pump and injection valve of claim 19 , wherein said third external connector is a static mixer.

Assignments (2)
CONVERSION OF CORPORATE ENTITY Recorded Feb 18, 2022
From: VALCO INSTRUMENTS COMPANY, L.P.
To: VALCO INSTRUMENTS COMPANY, INC.
Reel/Frame 059232/0008 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 17, 2014
From: STEARNS, STANLEY D; PLISTIL, ALES
To: VALCO INSTRUMENTS COMPANY, L.P.
Reel/Frame 033331/0949 →
Continuity (3)
Continuation In Part 14156197 · Jan 15, 2014
Provisional Application 61753299 · Jan 16, 2013
Related Publication 20140326650A1 · Nov 6, 2014