US3918911A
Expired / Lapsed
US
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Method and apparatus for preparation of liquid samples
Assignee: Safran Aerosystems SAS
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Filing: 1971-09-28
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Granted: 1975-11-11
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Expires: 1991-09-28
Abstract
Abstract Liquid samples for liquid scintillation counting are prepared by catalytic combustion of successive radioactive samples, continuous withdrawal of the combustion products which flow along a water extraction column and a CO2 extraction column arranged in cascade. In each column there is a countercurrent flow of a selective solvent scintillation solution and of the gaseous combustion products which are intimately mixed by a rotating serrated paddle.
Inventors
- 👤 Andrew Reich
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-09 06:48
CPC Classifications
G; G01; G01N; G01N31/00; G01N31/12; G01T; G01T1/00; G01T1/16; G01T1/20; G01T1/204
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
273 words
An apparatus for the preparation of liquid samples, comprising a vertical combustion furnace, a bed of combustion catalyst in said furnace, means for dropping successive samples on said catalyst bed through a closable passage at the top of said furnace, means for introducing a predetermined flow rate of oxygen into said furnace above said bed, first gas outlet means in said furnace under said bed from which combustion gas can be continuously withdrawn during the combustion of a sample, a water collection column located in series relation along the path of the gas from the furnace, first gas inlet means in the water collection column connected to the first gas outlet means, solvent feeding means for contiNuously introducing a solvent into the water collection column above the first gas inlet means so that the gas and solvent will mix through counter-current flow, second gas outlet means in the water collection column above the portion thereof where the gas and solvent are mixed and means through which a sample can be withdrawn located below said portion, a CO2 collection column located in series relation along the path of the gas from the water collection column, second gas inlet means in the CO2 collection column connected to the second gas outlet means, solvent feeding means for continuously introducing a solvent into the CO2 collection column above the second gas inlet means so that the gas and solvent will mix through countercurrent flow, third gas outlet means in the CO2 collection column above the portion thereof where the gas and solvent are mixed and means through which a sample can be withdrawn located below said portion.
Claim 2
Independent Claim
273 words
An apparatus for the preparation of liquid samples, comprising a vertical combustion furnace, a bed of combustion catalyst in said furnace, means for dropping successive samples on said catalyst bed through a closable passage at the top of said furnace, means for introducing a predetermined flow rate of oxygen into said furnace above said bed, first gas outlet means in said furnace under said bed from which combustion gas can be continuously withdrawn during the combustion of a sample, a water collection column located in series relation along the path of the gas from the furnace, first gas inlet means in the water collection column connected to the first gas outlet means, solvent feeding means for contiNuously introducing a solvent into the water collection column above the first gas inlet means so that the gas and solvent will mix through counter-current flow, second gas outlet means in the water collection column above the portion thereof where the gas and solvent are mixed and means through which a sample can be withdrawn located below said portion, a CO2 collection column located in series relation along the path of the gas from the water collection column, second gas inlet means in the CO2 collection column connected to the second gas outlet means, solvent feeding means for continuously introducing a solvent into the CO2 collection column above the second gas inlet means so that the gas and solvent will mix through countercurrent flow, third gas outlet means in the CO2 collection column above the portion thereof where the gas and solvent are mixed and means through which a sample can be withdrawn located below said portion.
Claim 3
Dependent Claim
18 words
Device according to claim l, wherein each said column is provided with means for circulating a cooling fluid.
Claim 4
Dependent Claim
97 words
An apparatus according to claim 1, wherein each column comprises: a vertical cylinder, a paddle mounted in said cylinder for rotation about the axis of said cylinder, the lateral edges of said paddle being close to the wall of said cylinder and notched; motor means located out of said cylinder for driving said paddle; inlet and outlet means for said gas, inlet means for the admission of a liquid solvent and outlet means for the liquid sample, said inlet and outlet means being arranged for countercurrent circulations of the solvent and of the gas within the cylinder.
Claim 5
Dependent Claim
11 words
Device according to claim 3, wherein the solvent contains a scintillator.
Claim 6
Dependent Claim
51 words
Device according to claim 3, comprising a metering pump for progressively injecting a predetermined volume of solvent into each cylinder for a time period which begins immediately upon admission of the combustion gas from a sample into the cylinder and continues beyond completion of passage of said gas through the cylinder.
Claim 7
Dependent Claim
26 words
Device according to claim 3, having a sequence control unit for automatically controlling the sequence of necessary operations in response to introduction of a starting sample.
Claim 8
Independent Claim
155 words
AN APPARATUS FOR THE PREPARATION OF LIQUID SAMPLES, HAVING: A VERTICAL COMBUSTION CATALYST IN SAID FURNACE, MEANS FOR INTRODUCING OXYGEN AT A PREDETERMINED FLOW RATE INTO SAID FURNACE ABOVE SAID BED, MEANS FOR CONTINUOUSLY WITHDRAWING COMBUSTION GAS FROM SAID FURNACE UNDER SAID BED AND DIRECTING IT TO CASCADED MEANS FOR SELECTIVE SOLVENT COLLECTION OF WATER AND CO2,, SAMPLE LOADING MEANS COMPRISING AN UPPER END FITTING FOR SAID FURNACE, A VERTICAL PASSAGE FORMED IN SAID FITTING AND COMMUNITCATING WITH SAID FURNACE, A RADIAL PASSAGE AND OPENING INTO SAID VERTICAL PASSAGE, A SEAT FORMED IN SAID VERTICAL PASSAGE BETWEEN SAID RADIAL PASSAGE AND SAID FURNACE, A VALVE MEMBER MOVABLE BETWEEN A NORMAL POSITION WHERE IT CLOSES SAID SEAT AND AN OPEN POSITION WHERE IT CLEARS SAID SEAT OPENING OF SAID RACIAL PASSAGE, MEANS FOR INTRODUCING STARTING SAMPLES ONE AT A TIME ALONG SAID PASSAGE AND MEANS FOR FORCIBLY OPENING SAID VALVE MENBER IN RESPONSE TO SAID INTRODUCTION.
Claim 9
Independent Claim
155 words
AN APPARATUS FOR THE PREPARATION OF LIQUID SAMPLES, HAVING: A VERTICAL COMBUSTION CATALYST IN SAID FURNACE, MEANS FOR INTRODUCING OXYGEN AT A PREDETERMINED FLOW RATE INTO SAID FURNACE ABOVE SAID BED, MEANS FOR CONTINUOUSLY WITHDRAWING COMBUSTION GAS FROM SAID FURNACE UNDER SAID BED AND DIRECTING IT TO CASCADED MEANS FOR SELECTIVE SOLVENT COLLECTION OF WATER AND CO2,, SAMPLE LOADING MEANS COMPRISING AN UPPER END FITTING FOR SAID FURNACE, A VERTICAL PASSAGE FORMED IN SAID FITTING AND COMMUNITCATING WITH SAID FURNACE, A RADIAL PASSAGE AND OPENING INTO SAID VERTICAL PASSAGE, A SEAT FORMED IN SAID VERTICAL PASSAGE BETWEEN SAID RADIAL PASSAGE AND SAID FURNACE, A VALVE MEMBER MOVABLE BETWEEN A NORMAL POSITION WHERE IT CLOSES SAID SEAT AND AN OPEN POSITION WHERE IT CLEARS SAID SEAT OPENING OF SAID RACIAL PASSAGE, MEANS FOR INTRODUCING STARTING SAMPLES ONE AT A TIME ALONG SAID PASSAGE AND MEANS FOR FORCIBLY OPENING SAID VALVE MENBER IN RESPONSE TO SAID INTRODUCTION.
Claim 10
Dependent Claim
53 words
Apparatus according to claim 7 having means for detecting changes in the coefficient of heat transfer of gases at the outlet of the furnace, means for measuring the flow rate of said gases, and means for measuring the time duration between successive changes, whereby the weight of each radioactive sample may be determined.
Claim 11
Dependent Claim
27 words
Apparatus according to claim 7 comprising resilient means exerting a force on said valve member which biases it toward its seat against the pressure in said furnace.
Claim 12
Dependent Claim
32 words
Apparatus according to claim 7, having a solenoid for actuation of said valve member against a return spring which exerts a force on said valve member which biases it toward said seat.
Claim 13
Dependent Claim
28 words
AppAratus according to claim 7, having means for heating the withdrawed means which convey the gaseous combustion products to the water collection means to a temperature above 100*C.
Claim 14
Dependent Claim
46 words
Apparatus according to claim 7, wherein the furnace comprises a heating sleeve, a cylindrical tube located in said sleeve and clamped vertically between an upper end fitting in which the starting sample inlet is formed and a lower end fitting in which the outlet is formed.
Claim 15
Dependent Claim
31 words
Device according to claim 12, wherein said means for supplying oxygen into the furnace comprise a plurality of ducts formed obliquely in the upper end fitting and directed towards the valve.
Claim 16
Independent Claim
350 words
An apparatus for the preparation of liquid samples, comprising a vertical combustion furnace, a bed of combustion catalyst in said furnace, means for dropping successive samples on said catalyst bed through a closable passage at the top of said furnace, means for introducing a predetermined flow rate of oxygen into said furnace above said bed, first gas outlet means in said furnace under said bed from which combustion gas can be continuously withdrawn during the combustion of a sample, a water collection column located in series relation along the path of the gas from the furnace, first gas inlet means in the water collection column connected to the first gas outlet means, solvent feeding means for continuously introducing a solvent into the water collection column above the first gas inlet means so that the gas and solvent will mix through counter-current flow, second gas outlet means in the water collection column above the portion thereof where the gas and solvent are mixed and first means through which a liquid sample can be withdrawn located below said portion, a CO2 collection column located in series relation along the path of the gas from the water collection column, second gas inlet means in the CO2 collection column connected to the second gas outlet means, solvent feeding means for continuously introducing a solvent into the CO2 collection column above the second gas inlet means so that the gas and solvent will mix through countercurrent flow, third gas outlet means in the CO2 collection column above the portion thereof where the gas and solvent are mixed and second means through which a liquid sample can be withdrawn located below said portion, each of said first and second means through which a liquid sample can be withdrawn including an intermediary overflow chamber, means for bubbling a flow of neutral gas in the volume of liquid sample retained in said chamber, and means for returning vapour and gas to the column from which the liquid sample is withdrawn, said vapour and gas being returned from a zone of said outlet means located downstream of said chamber.
Claim 17
Independent Claim
350 words
An apparatus for the preparation of liquid samples, comprising a vertical combustion furnace, a bed of combustion catalyst in said furnace, means for dropping successive samples on said catalyst bed through a closable passage at the top of said furnace, means for introducing a predetermined flow rate of oxygen into said furnace above said bed, first gas outlet means in said furnace under said bed from which combustion gas can be continuously withdrawn during the combustion of a sample, a water collection column located in series relation along the path of the gas from the furnace, first gas inlet means in the water collection column connected to the first gas outlet means, solvent feeding means for continuously introducing a solvent into the water collection column above the first gas inlet means so that the gas and solvent will mix through counter-current flow, second gas outlet means in the water collection column above the portion thereof where the gas and solvent are mixed and first means through which a liquid sample can be withdrawn located below said portion, a CO2 collection column located in series relation along the path of the gas from the water collection column, second gas inlet means in the CO2 collection column connected to the second gas outlet means, solvent feeding means for continuously introducing a solvent into the CO2 collection column above the second gas inlet means so that the gas and solvent will mix through countercurrent flow, third gas outlet means in the CO2 collection column above the portion thereof where the gas and solvent are mixed and second means through which a liquid sample can be withdrawn located below said portion, each of said first and second means through which a liquid sample can be withdrawn including an intermediary overflow chamber, means for bubbling a flow of neutral gas in the volume of liquid sample retained in said chamber, and means for returning vapour and gas to the column from which the liquid sample is withdrawn, said vapour and gas being returned from a zone of said outlet means located downstream of said chamber.
Claim 18
Dependent Claim
11 words
The apparatus in claim 14, wherein said neutral gas is nitrogen.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-11-10 | 1979-05-12 | 1979-11-11 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-11-10 | 1983-05-12 | 1983-11-11 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-11-10 | 1987-05-12 | 1987-11-11 | $7700.00 | Window Closed / Lapsed |