# US 6,296,769 B1 · Multi-chambered supercritical fluid extraction cartridge and processes using it

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- Number: US 6,296,769 B1
- Document ID: US6296769B1
- Status: Granted
- Kind: B1
- Application number: 09/366,128
- Filed: 1999-08-02
- Granted: 2001-10-02
- Earliest claimed: 1990-07-13
- Assignees: Isco, Inc.
- Inventors: Henry Walters; Dale Messer; Dale Clay; Robert W. Allington
- Web page: https://patentgrep.com/patent/US6296769B1

## CPC

- F04B 9/042: {the means being cams}
- B01D 11/0203: {with a supercritical fluid}
- B01D 11/0407: {the supercritical fluid acting as solvent for the solute}
- F04B 15/08: the liquids having low boiling points
- F04B 49/065: {and making use of computers}
- F16K 15/1823: {for ball check valves}
- G01F 1/34: by measuring pressure or differential pressure
- G01N 1/34: Purifying; Cleaning {(processes or apparatus for extracting or separating nucleic acids from biological samples C12N15/1003)}
- G01N 1/40: Concentrating samples
- G01N 30/28: Control of physical parameters of the fluid carrier
- G21F 5/015: for storing radioactive sources, e.g. source carriers for irradiation units; Radioisotope containers
- F04B 2205/03: Pressure in the compression chamber
- F04B 2205/05: Pressure after the pump outlet
- F04B 2205/09: Flow through the pump
- F05B 2230/41: Hardening; Annealing
- F05C 2201/0493: Tin
- F05C 2253/12: Coating
- G01N 30/02: Column chromatography
- G01N 30/6034: {joining multiple columns}
- G01N 30/6069: {with compartments or bed substructure}
- G01N 30/6091: {Cartridges}
- G01N 2001/4033: {sample concentrated on a cold spot, e.g. condensation or distillation}
- G01N 2001/4061: {Solvent extraction}
- G01N 2030/009: {Extraction}
- G01N 2030/6013: {interfaces to detectors}
- G01N 2035/0441: {for samples}
- F04B: POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS (machines for liquids, or pumps, of rotary-piston or oscillating-piston type F04C; non-positive-displacement pumps F04D; pumping of fluid by direct contact of another fluid or by using inertia of fluid to be pumped F04F)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- F16K: VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING {(devices for emptying and evacuating the excess liquid in valves or conduits F16L55/07)}
- G01F: MEASURING VOLUME, VOLUME FLOW, MASS FLOW OR LIQUID LEVEL; METERING BY VOLUME
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)
- G21F: PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR (radiation protection by pharmaceutical means A61K8/00, A61Q17/04; in cosmonautic vehicles B64G1/54; combined with a reactor G21C11/00; combined with X-ray tubes H01J35/16; combined with X-ray apparatus H05G1/02)
- F05B: INDEXING SCHEME RELATING TO WIND, SPRING, WEIGHT, INERTIA OR LIKE MOTORS, TO MACHINES OR ENGINES FOR LIQUIDS COVERED BY SUBCLASSES F03B, F03D AND F03G
- F05C: INDEXING SCHEME RELATING TO MATERIALS, MATERIAL PROPERTIES OR MATERIAL CHARACTERISTICS FOR MACHINES, ENGINES OR PUMPS OTHER THAN NON-POSITIVE-DISPLACEMENT MACHINES OR ENGINES

## Abstract

A multiple chamber sample holding cartridge is used with a supercritical fluid extractor that causes membranes dividing the cartridge into chambers to rupture upon the pressurization of the sample cartridge, thereby allowing the intermixing of materials contained in the chambers. The neutral oil and loss determination of soybean and other oilseed oils by supercritical fluid extraction is efficient with this two-chambered sample cartridge.

## Claims

### Claim 1

A method of supercritical fluid extraction comprising the steps of:
applying supercritical fluid to a first chamber of a sample cartridge while preventing flow to a second chamber;
after supercritical fluid has been applied to said first chamber of said cartridge, permitting said supercritical fluid from said first chamber to flow into a second chamber;
permitting at least a portion of the fluid from said second chamber to be collected.

### Claim 2 (depends on 1)

A method in accordance with claim 1 in which the fluid is permitted to flow from said first chamber into said second chamber at a predetermined pressure differential between said first chamber and second chamber.

### Claim 3 (depends on 1)

A method in accordance with claim 1 in which the step of applying supercritical fluid to said first chamber includes the step of applying supercritical fluid to a sample in said first chamber.

### Claim 4 (depends on 3)

A method in accordance with claim 3 in which the step of permitting fluid to flow from said first chamber into said second chamber includes the step of permitting fluid to flow from said first chamber into said second chamber containing a separating material.

### Claim 5 (depends on 4)

A method in accordance with claim 4 in which said fluid is applied to said first chamber at a predetermined pressure less than an operating pressure of said cartridge and released into said second chamber after pressure has equalized between said first chamber and a source of the predetermined pressure whereby the sample may be separated in said second chamber in a sufficiently short period of time to avoid plugging of the separating material in said second chamber.

### Claim 6 (depends on 5)

A method in accordance with claim 5 in which said separating material and fluid are used for neutral oil and loss determination.

### Claim 7 (depends on 1)

A method according to claim 1 wherein the flow of fluid to the second chamber is blocked by a membrane separating the first and second chambers.

### Claim 8 (depends on 1)

A method according to claim 1 in which the flow of fluid to the second chamber is permitted by an increase in pressure in the first chamber beyond a predetermined design pressure.

### Claim 9 (depends on 8)

A method according to claim 8 wherein the flow of fluid to the second chamber is blocked by a membrane separating the first and second chambers and the flow of fluid into the second chamber is permitted by causing the membrane to be ruptured by pressure.

### Claim 10 (depends on 1)

A method according to claim 1 in wherein the fluid is permitted to flow when a pressure difference between the first and second chambers is at least 20 percent of the operating pressure of the cartridge.

### Claim 11 (depends on 1)

A method according to claim 1 wherein extract is assayed after being collected from said second chamber.

### Claim 12 (depends on 11)

A method according to claim 11 in which the first chamber includes a sample and the second chamber includes a separating medium.
