Patent US3954408A successfully refreshed from Google Patents.
← Back to Patent Explorer
US3954408A Expired / Lapsed US ⏱️ 0.0 years remaining

Apparatus and process for chromatographic product detection

Assignee: Sandoz Inc
•
Filing: 1974-11-29
•
Granted: 1976-05-04
•
Expires: 1994-11-29
📄 Original PDF 🌐 Google Patents 🔄 Sync Now

Abstract

Abstract Apparatus and process for detecting the products of either liquid or gas chromatographic analysis, which products may be either radioactively tagged or not tagged. In one aspect, it provides a moving wire apparatus for conveying a liquid chromatographic sample through a combustion furnace, where the combustion products are conveyed to a catalytic system. Non-radioactive samples are routed through a nickel catalytic converter; and thence, to a flame ionisation detector. Radioactive samples are conveyed from the combustion furnace through either a copper-oxide or an iron catalytic furnace, depending upon whether the sample is tagged with Carbon-14 or tritium. The products of the catalytic furnaces are detected by means of a radioactive detector. Means are also provided for introducing gas chromatographic products into the system for detection.

Inventors

  • 👤 Harry A. Dugger

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-29 23:27
CPC Classifications
G; G01; G01N; G01N30/00; G01N30/02; G01N30/84; G01N30/62; G01N30/64; G01N30/68; G01N31/00; G01N31/12; G01N2030/8411; G01N2030/8417; G01N2030/8429; G01N2030/8435

Claims Analysis

Total Claims: 24
Claim 1
Independent Claim 246 words
A process for detecting products of liquid chromatographic analysis, which products may be either radioactively tagged with Carbon-14 or tritium or not tagged which comprises the steps of: a. Applying either a radioactively Carbon-14 tagged, a tritium tagged or a non-tagged chromatographic sample to a moving wire; b. Moving the sample on the wire first through an evporator oven to dry the sample, and then through a combustion furnace to combust the sample with a combustion gas to form either non-radioactive or Carbon-14 tagged or tritium tagged carbon dioxide gas and water; c. When non-radioactive carbon dioxide gas is formed in step b), contacting the non-radioactive carbon dioxide gas with a nickel catalyst in a first catalytic furnace to convert the carbon dioxide gas to non-radioactive methane and hydrogen; d. Conveying non-radioactive methane to a first detector means for sample detection; e. When Carbon-14 tagged radioactive carbon dioxide gas is formed in step b), conveying the Carbon-14 tagged radioactive carbon dioxide and water to a drying chamber to remove the water, and conveying the carbon dioxide gas to a second detector means for sample detection; f. When tritium tagged radioactive carbon dioxide gas is formed in step b), conveying the tritium tagged radioactive water and carbon dioxide gas to a second catalytic furnace and contacting the water with an iron catalyst in the presence of hydrogen to convert the water to tritium gas and conveying the tritium gas to the second detector means for sample detection.
Claim 2
Dependent Claim 246 words
A process for detecting products of liquid chromatographic analysis, which products may be either radioactively tagged with Carbon-14 or tritium or not tagged which comprises the steps of: a. Applying either a radioactively Carbon-14 tagged, a tritium tagged or a non-tagged chromatographic sample to a moving wire; b. Moving the sample on the wire first through an evporator oven to dry the sample, and then through a combustion furnace to combust the sample with a combustion gas to form either non-radioactive or Carbon-14 tagged or tritium tagged carbon dioxide gas and water; c. When non-radioactive carbon dioxide gas is formed in step b), contacting the non-radioactive carbon dioxide gas with a nickel catalyst in a first catalytic furnace to convert the carbon dioxide gas to non-radioactive methane and hydrogen; d. Conveying non-radioactive methane to a first detector means for sample detection; e. When Carbon-14 tagged radioactive carbon dioxide gas is formed in step b), conveying the Carbon-14 tagged radioactive carbon dioxide and water to a drying chamber to remove the water, and conveying the carbon dioxide gas to a second detector means for sample detection; f. When tritium tagged radioactive carbon dioxide gas is formed in step b), conveying the tritium tagged radioactive water and carbon dioxide gas to a second catalytic furnace and contacting the water with an iron catalyst in the presence of hydrogen to convert the water to tritium gas and conveying the tritium gas to the second detector means for sample detection.
Claim 3
Dependent Claim 20 words
The process according to claim 1, wherein the conversion temperature in the first catalytic furnace is from 600°C to 1000°C.
Claim 4
Dependent Claim 20 words
The process according to claim 2, wherein the conversion temperature in the second catalytic furnace is from 600°C to 1000°C.
Claim 5
Dependent Claim 12 words
The process according to claim 3, wherein the combustion gas is oxygen.
Claim 6
Dependent Claim 244 words
A process for detecting products of liquid chromatographic analysis, which products may be either radioactively tagged with Carbon-14 or tritium or not tagged, which comprises the steps of: a. Applying either a radioactively Carbon-14 tagged, a tritium tagged or a non-tagged chromatographic sample to a moving wire; b. Moving the sample on the wire first through an evaporator oven to dry the sample, and then through a combustion furnace to combust the sample with a combustion gas to form either non-radioactive or Carbon-14 tagged or tritium tagged carbon dioxide gas and water; c. When non-radioactive carbon dioxide gas is formed in step b), contacting the carbon dioxide gas with a nickel catalyst in a first catalytic furnace to convert the carbon dioxide gas to methane and hydrogen; d. Conveying non-radioactive methane to a first detector means for sample detection; e. When Carbon-14 tagged radioactive carbon dioxide gas is formed in step b), conveying Carbon-14 tagged methane to a second catalytic furnace and contacting the methane with a copper-oxide catalyst to convert the methane to carbon dioxide gas and conveying the carbon dioxide gas to a second detector means for sample detection; f. When tritium tagged radioactive methane is formed in step b), conveying tritium tagged methane to a third catalytic furnace and contacting the methane with an iron catalyst in the presence of hydrogen to convert the methane to tritium gas and conveying the tritium gas to the second detector means for sample detection.
Claim 7
Dependent Claim 244 words
A process for detecting products of liquid chromatographic analysis, which products may be either radioactively tagged with Carbon-14 or tritium or not tagged, which comprises the steps of: a. Applying either a radioactively Carbon-14 tagged, a tritium tagged or a non-tagged chromatographic sample to a moving wire; b. Moving the sample on the wire first through an evaporator oven to dry the sample, and then through a combustion furnace to combust the sample with a combustion gas to form either non-radioactive or Carbon-14 tagged or tritium tagged carbon dioxide gas and water; c. When non-radioactive carbon dioxide gas is formed in step b), contacting the carbon dioxide gas with a nickel catalyst in a first catalytic furnace to convert the carbon dioxide gas to methane and hydrogen; d. Conveying non-radioactive methane to a first detector means for sample detection; e. When Carbon-14 tagged radioactive carbon dioxide gas is formed in step b), conveying Carbon-14 tagged methane to a second catalytic furnace and contacting the methane with a copper-oxide catalyst to convert the methane to carbon dioxide gas and conveying the carbon dioxide gas to a second detector means for sample detection; f. When tritium tagged radioactive methane is formed in step b), conveying tritium tagged methane to a third catalytic furnace and contacting the methane with an iron catalyst in the presence of hydrogen to convert the methane to tritium gas and conveying the tritium gas to the second detector means for sample detection.
Claim 8
Dependent Claim 20 words
The process according to claim 5, wherein the conversion temperature in the first catalytic furnace is from 600°C to 1000°C.
Claim 9
Dependent Claim 20 words
The process according to claim 6, wherein the conversion temperature in the second catalytic furnace is from 600°C to 1000°C.
Claim 10
Dependent Claim 20 words
The process according to claim 7, wherein the conversion temperature in the third catalytic furnace is from 600°C to 1000°C.
Claim 11
Dependent Claim 12 words
The process according to claim 8, wherein the combustion gas is oxygen.
Claim 12
Dependent Claim 147 words
A process for detecting products of a gas chromatographic analysis, which products may be either radioactively tagged with Carbon-14 or tritium, or not tagged which comprises the steps of: a. Conveying a non-tagged gas chromatographic sample from the gas chromatograph to a first detector means for sample detection; b. Conveying a Carbon-14 tagged gas chromatographic sample from the gas chromatograph to a first catalytic furnace and contacting the gas sample with copper-oxide to convert the gas sample to carbon dioxide gas and conveying the carbon dioxide gas to a second detector means for sample detection; c. Conveying a tritium tagged gas chromatographic sample from the gas chromatograph to a second catalytic furnace and contacting the gas sample with an iron catalyst in the presence of hydrogen to convert the gas sample to tritium gas, and conveying the tritium gas to the second detector means for sample detection.
Claim 13
Dependent Claim 147 words
A process for detecting products of a gas chromatographic analysis, which products may be either radioactively tagged with Carbon-14 or tritium, or not tagged which comprises the steps of: a. Conveying a non-tagged gas chromatographic sample from the gas chromatograph to a first detector means for sample detection; b. Conveying a Carbon-14 tagged gas chromatographic sample from the gas chromatograph to a first catalytic furnace and contacting the gas sample with copper-oxide to convert the gas sample to carbon dioxide gas and conveying the carbon dioxide gas to a second detector means for sample detection; c. Conveying a tritium tagged gas chromatographic sample from the gas chromatograph to a second catalytic furnace and contacting the gas sample with an iron catalyst in the presence of hydrogen to convert the gas sample to tritium gas, and conveying the tritium gas to the second detector means for sample detection.
Claim 14
Dependent Claim 26 words
The process according to claim 10, wherein the conversion temperature in both the first catalytic furnace and the second catalytic furnace is from 600° to 1000°C.
Claim 15
Independent Claim 405 words
An apparatus for detecting products of chromatographic analysis, which products may be either radioactively tagged or not tagged which comprise in combination: a. A movable wire having liquid chromatographic sample receiving means; b. An evaporator oven mounted in tandem with a combustion furnace, the wire adapted to move a sample first through the evaporator oven and then through the combustion furnace; c. The evaporator oven having gas egress means, and the combustion furance having at least one gas ingress means and gas egress means; the evaporator oven adapted to remove solvent from a liquid sample leaving a solute remaining on the wire, and the combustion furnace adapted to convert the solute to a gaseous combustion product with a combustion gas; d. The combustion furnace gas egress means in flow communication with a first valve means; e. The first valve means in flow communication with ingress means for a first catalytic furnace; and a second valve means; the catalytic furnace, adapted to convert the gaseous combustion product from the combustion furnace to a gaseous reaction product and having gas egress means in flow communication with a first detector means; f. The second valve means in flow communication with a third valve means and adapted to emit or not the gaseous combustion product to the third valve means; g. The third valve means in flow communication with a fourth valve means and an external, inert gas source, and adapted to either emit the gaseous combustion product to the fourth valve means or to emit the inert gas to the fourth valve means; h. The fourth valve means in flow communication with a drying chamber and a fifth valve means, and adapted to shunt the gaseous combustion product to either the drying chamber or to the fifth valve means; i. The fifth valve means in flow communication with a second catalytic furnace and a source of reaction gas, and adapted to shunt the gaseous combustion product to the second catalytic furnace for conversion to a gaseous reaction product, and simultaneously, emit a reaction gas to the second catalytic furnace; j. The drying chamber and the second catalytic furnace each in flow communication with a sixth valve means, which valve means is in flow communication with a second detector means, the valve means adapted to shunt the gaseous combustion product from the drying chamber or the gaseous reaction product from the second catalytic furnace to the second detector means.
Claim 16
Independent Claim 405 words
An apparatus for detecting products of chromatographic analysis, which products may be either radioactively tagged or not tagged which comprise in combination: a. A movable wire having liquid chromatographic sample receiving means; b. An evaporator oven mounted in tandem with a combustion furnace, the wire adapted to move a sample first through the evaporator oven and then through the combustion furnace; c. The evaporator oven having gas egress means, and the combustion furance having at least one gas ingress means and gas egress means; the evaporator oven adapted to remove solvent from a liquid sample leaving a solute remaining on the wire, and the combustion furnace adapted to convert the solute to a gaseous combustion product with a combustion gas; d. The combustion furnace gas egress means in flow communication with a first valve means; e. The first valve means in flow communication with ingress means for a first catalytic furnace; and a second valve means; the catalytic furnace, adapted to convert the gaseous combustion product from the combustion furnace to a gaseous reaction product and having gas egress means in flow communication with a first detector means; f. The second valve means in flow communication with a third valve means and adapted to emit or not the gaseous combustion product to the third valve means; g. The third valve means in flow communication with a fourth valve means and an external, inert gas source, and adapted to either emit the gaseous combustion product to the fourth valve means or to emit the inert gas to the fourth valve means; h. The fourth valve means in flow communication with a drying chamber and a fifth valve means, and adapted to shunt the gaseous combustion product to either the drying chamber or to the fifth valve means; i. The fifth valve means in flow communication with a second catalytic furnace and a source of reaction gas, and adapted to shunt the gaseous combustion product to the second catalytic furnace for conversion to a gaseous reaction product, and simultaneously, emit a reaction gas to the second catalytic furnace; j. The drying chamber and the second catalytic furnace each in flow communication with a sixth valve means, which valve means is in flow communication with a second detector means, the valve means adapted to shunt the gaseous combustion product from the drying chamber or the gaseous reaction product from the second catalytic furnace to the second detector means.
Claim 17
Dependent Claim 25 words
The apparatus according to claim 12, wherein the first detector means is a flame ionisation detector, and the second detector means is a radioactive detector.
Claim 18
Independent Claim 431 words
An apparatus for detecting products of chromatographic analysis, which products may be either radioactively tagged or not tagged, which comprise in combination: a. A movable wire having liquid chromatographic sample receiving means; b. An evaporator oven mounted in tandem with a combustion furnace, the wire adapted to move a sample first through the evaporator oven, and then through the combustion furnace; c. The evaporator oven having gas egress means, and the combustion furnace having at least one gas ingress means and gas egress means, the evaporator oven adapted to remove solvent from a liquid sample leaving a solute remaining on the wire, and the combustion furnace adapted to convert the solute to a gaseous combustion product with a combustion gas; d. The combustion furnace gas egress means in flow communication with ingress means for a first catalytic furnace; the catalytic furance, adapted to convert the gaseous combustion product from the combustion furnace to a gaseous reaction product and having gas egress means in flow communication with a first valve means; e. The first valve means in flow communication with a first detector means and a second valve means and adapted to shunt the gaseous reaction product to the first detector means or the second valve means; f. The second valve means in flow communication with a third valve means and adapted to emit or not the gaseous reaction product to the third valve means; g. The third valve means in flow communication with a fourth valve means and an external, inert gas source and adapted to either emit the gaseous reaction product to the fourth valve means or to emit the inert gas to the fourth valve means; h. The fourth valve means in flow communication with a second catalytic furnace and a fifth valve means, and adapted to shunt the gaseous reaction product to either the second catalytic furnace for conversion to a second gaseous reaction product or to the fifth valve means; i. The fifth valve means in flow communication with a third catalytic furnace and a source of reaction gas, and adapted to shunt the gaseous reaction product to the third catalytic furnace for conversion to a third gaseous reaction product, and simultaneously, emit a reaction gas to the third catalytic furnace; j. The second catalytic furnace and the third catalytic furnace each in flow communication with a sixth valve means, which valve means is in flow communication with a second detector means, the valve means adapted to shunt the gaseous reaction product from the second catalytic furnace or the third catalytic furnace to the second detector means.
Claim 19
Independent Claim 431 words
An apparatus for detecting products of chromatographic analysis, which products may be either radioactively tagged or not tagged, which comprise in combination: a. A movable wire having liquid chromatographic sample receiving means; b. An evaporator oven mounted in tandem with a combustion furnace, the wire adapted to move a sample first through the evaporator oven, and then through the combustion furnace; c. The evaporator oven having gas egress means, and the combustion furnace having at least one gas ingress means and gas egress means, the evaporator oven adapted to remove solvent from a liquid sample leaving a solute remaining on the wire, and the combustion furnace adapted to convert the solute to a gaseous combustion product with a combustion gas; d. The combustion furnace gas egress means in flow communication with ingress means for a first catalytic furnace; the catalytic furance, adapted to convert the gaseous combustion product from the combustion furnace to a gaseous reaction product and having gas egress means in flow communication with a first valve means; e. The first valve means in flow communication with a first detector means and a second valve means and adapted to shunt the gaseous reaction product to the first detector means or the second valve means; f. The second valve means in flow communication with a third valve means and adapted to emit or not the gaseous reaction product to the third valve means; g. The third valve means in flow communication with a fourth valve means and an external, inert gas source and adapted to either emit the gaseous reaction product to the fourth valve means or to emit the inert gas to the fourth valve means; h. The fourth valve means in flow communication with a second catalytic furnace and a fifth valve means, and adapted to shunt the gaseous reaction product to either the second catalytic furnace for conversion to a second gaseous reaction product or to the fifth valve means; i. The fifth valve means in flow communication with a third catalytic furnace and a source of reaction gas, and adapted to shunt the gaseous reaction product to the third catalytic furnace for conversion to a third gaseous reaction product, and simultaneously, emit a reaction gas to the third catalytic furnace; j. The second catalytic furnace and the third catalytic furnace each in flow communication with a sixth valve means, which valve means is in flow communication with a second detector means, the valve means adapted to shunt the gaseous reaction product from the second catalytic furnace or the third catalytic furnace to the second detector means.
Claim 20
Dependent Claim 22 words
The apparatus according to claim 14, wherein the first valve means is also in flow communication with gas chromatographic sample receiving means.
Claim 21
Dependent Claim 25 words
The appratus according to claim 15, wherein the first detector means in a flame ionisation detector, and the second detector means is a radioactive detector.
Claim 22
Independent Claim 276 words
An apparatus for detecting products of chromatographic analysis, which products may be either radioactively tagged or not tagged, which comprise in combination: a. A first valve means in flow communication with a gas chromatographic sample receiving means, a first detector means, and a second valve means and adapted to shunt the gas chromatographic sample to the first detector means or the second valve means; b. The second valve means in flow communication with a third valve means and adapted to emit or not the gas chromatographic sample to the third valve means; c. The third valve means in flow communication with a fourth valve means and an external, inert gas source and adapted to either emit the gas chromatographic sample to the fourth valve means or to emit the inert gas to the fourth valve means; d. The fourth valve means in flow communication with a first catalytic furnace and a fifth valve means, and adapted to shunt the gas chromatographic sample to either the first catalytic furnace for conversion to a gaseous reaction product or to the fifth valve means; e. The fifth valve means in flow communication with a second catalytic furnace and a source of reaction gas, and adapted to shunt the chromatographic sample to the second catalytic furnace for conversion to a gaseous reaction product and simultaneously, emit a reaction gas to the third catalytic furnace; f. The first catalytic furnace and the second catalytic furnace each in flow communication with a sixth valve means, which valve means is in flow communication with a second detector means, the valve means adapted to shunt the gaseous reaction product from the second catalytic means.
Claim 23
Independent Claim 276 words
An apparatus for detecting products of chromatographic analysis, which products may be either radioactively tagged or not tagged, which comprise in combination: a. A first valve means in flow communication with a gas chromatographic sample receiving means, a first detector means, and a second valve means and adapted to shunt the gas chromatographic sample to the first detector means or the second valve means; b. The second valve means in flow communication with a third valve means and adapted to emit or not the gas chromatographic sample to the third valve means; c. The third valve means in flow communication with a fourth valve means and an external, inert gas source and adapted to either emit the gas chromatographic sample to the fourth valve means or to emit the inert gas to the fourth valve means; d. The fourth valve means in flow communication with a first catalytic furnace and a fifth valve means, and adapted to shunt the gas chromatographic sample to either the first catalytic furnace for conversion to a gaseous reaction product or to the fifth valve means; e. The fifth valve means in flow communication with a second catalytic furnace and a source of reaction gas, and adapted to shunt the chromatographic sample to the second catalytic furnace for conversion to a gaseous reaction product and simultaneously, emit a reaction gas to the third catalytic furnace; f. The first catalytic furnace and the second catalytic furnace each in flow communication with a sixth valve means, which valve means is in flow communication with a second detector means, the valve means adapted to shunt the gaseous reaction product from the second catalytic means.
Claim 24
Dependent Claim 25 words
The apparatus according to claim 17, wherein the first detector means is a flame ionisation detector, and the second detector means is a radioactive detector.

References Cited (Backward Citations)

US2634360A Cited
US3128619A Cited
US3292420A Cited
US3692492A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-05-04 1979-11-03 1980-05-04 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-05-04 1983-11-03 1984-05-04 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-05-04 1987-11-03 1988-05-04 $7700.00 Window Closed / Lapsed

Assigned Categories & Tags

No categories assigned to this patent yet.

Assign Category Tag