[특허]Pressure stepped microwave assisted digestion

Pressure stepped microwave assisted digestion 원문보기

IPC분류정보
국가/구분	United States(US) Patent 등록
국제특허분류(IPC7판)	B01J-019/12 G01N-001/44 H05B-006/80 H05B-006/64
출원번호	US-0395002 (2016-12-30)
등록번호	US-10067043 (2018-09-04)
발명자 / 주소	Barclay, David A. Lambert, Joseph J. Jennings, William E. Herman, David L.
출원인 / 주소	CEM Corporation
대리인 / 주소	Parsons Summa
인용정보	피인용 횟수 : 0 인용 특허 : 46

초록 ▼

An instrument and method for high pressure microwave assisted chemistry are disclosed. The method includes the steps of applying microwave radiation to a sample in a sealed vessel while measuring the temperature of the sample and measuring the pressure generated inside the vessel and until the measured pressure reaches a designated set point, opening the vessel to release gases until the pressure inside the vessel reaches a lower designated set point, closing the vessel, and repeating the steps of opening the vessel at designated pressure set points and closing the vessel at designated pressure set points to the sample until the sample reaction reaches a designated high temperature. The designated set points can controllably differ from one another as the reaction proceeds. Microwave energy can be applied continuously or intermittently during the opening and closing steps. The apparatus includes a microwave cavity, a microwave transparent pressure resistant reaction vessel in the cavity, a cap on the reaction vessel, a pressure sensor for measuring pressure in the vessel, a temperature sensor, and means for opening and closing the cap at predetermined pressure set points measured by the pressure sensor to release pressure from the vessel.

대표청구항 ▼

1. A method of high pressure microwave assisted chemistry comprising: exerting a defined downward pressure against a flexible lid that seals a microwave-transparent vessel with a sample and at least one acid inside the vessel, with the acid being selected from the group consisting of sulfuric, nitric, phosphoric, hydrochloric, hydrofluoric, perchloric and mixtures thereof;applying microwave radiation to the sample and the acid in the sealed vessel to heat the sample and the acid while measuring the temperature of the sample and the acid;measuring the pressure generated inside the vessel and until the measured pressure reaches a designated set point above atmospheric pressure;releasing gases from the vessel through the flexible lid when the measured pressure inside the vessel exceeds the defined downward pressure and reaches a lower designated set point that remains above atmospheric pressure;closing the vessel while the pressure inside the vessel remains above atmospheric pressure; and;repeating the steps of opening the vessel at designated pressure set points and closing the vessel at designated pressure set points, and applying microwave radiation to the sample and the acid inside the vessel until the sample reaction inside the vessel reaches a designated temperature. 2. A method according to claim 1 comprising applying microwave radiation during any of the opening or closing steps. 3. A method according to claim 1 comprising applying the microwave radiation until the pressure reaches a designated set point above atmospheric pressure. 4. A method according to claim 1 wherein the step of repeating the opening of the vessel comprises opening the vessel at two designated measured pressure set points that are different pressures from one another. 5. A method according to claim 1 comprising applying a single mode of microwave radiation to the sample. 6. A method according to claim 1 comprising opening the vessel at a temperature above the atmospheric boiling point of the acid. 7. A method according to claim 6 comprising moderating the application of microwave energy in response to the measured temperature. 8. A method according to claim 1 further comprising thermally managing the sample temperature. 9. A method according to claim 1 comprising proactively cooling the reaction vessel during any one or more of the steps of applying microwave radiation, releasing gases from the vessel, and closing the vessel. 10. A method according to claim 9 comprising cooling the vessel by directing a fluid into contact with the vessel.

이 특허에 인용된 특허 (46)

Lautenschlger Werner (Leutkirch DEX), Apparatus for performing chemical and physical pressure reactions.
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Revesz Robert N. (Monroe NC), Apparatus for preventing explosions during microwave heated solvent extractions.
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Baraille,Eric Laurent; Cartigny,Michel Pierre; Gailhard,Thierry Rene, Appliance for cooking foods under pressure comprising a temperature sensor.
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Stefansky Frederick M. (Longmont CO), Architecture for 2½inch diameter single disk drive.
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Jennings, William Edward; King, Edward Earl, Attenuator system for microwave-assisted chemical synthesis.
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Rasmussen John (8433 South Ave. Youngstown OH 44514), Condensate trap and drain for systems under pressure.
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Lillelund Stig (Gentofte DKX) Olsen Eskil H. (Gentofte DKX), Container with pressure-release lid.
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Renoe Brian W. (Matthews NC) King Edward E. (Charlotte NC) Yurkovich Dale A. (Charlotte NC), Control of continuous microwave digestion process.
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Denny Patrick J. (Darlington GBX), Desulphurization.
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Floyd Terry S. (Clover SC) Hargett ; Jr. Wyatt P. (Matthews NC), Digestion and sterilization methods and apparatus.
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Lautenschlager Werner,DEX, Heating chamber with pressure responsive door mounting.
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Floyd Terry (4527 Island Fork Rd. Lake Wylie SC 29710), High pressure and high temperature digestion vessel.
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Floyd Terry S. (4527 Island Fork Rd. Lake Wylie SC 29710), High pressure and high temperature digestion vessel.
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Stalling David L., High pressure relief for microwave digestion vessel assembly.
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Duffy John W. (Tama IA) Funke Robert A. (Anna TX) Shollenbarger David W. (Marshalltown IA), High-low pressure pilot.
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Rojek Arnaldo (Sao Paulo BRX), Lid with a pressure release hole and a removable seal, for vacuum sealing of glasses and other glass containers used to.
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Schachter Myron M. (Washington DC) Boyer Kenneth W. (Springfield VA), Method and apparatus for destroying organic matter to facilitate trace inorganic element analysis.
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Kingston Howard M., Method and apparatus for microwave assisted chemical reactions.
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Hargett, Jr., Wyatt P.; Thomas, James E., Method and apparatus for microwave assisted high throughput high pressure chemical synthesis.
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Lilienthal ; II Peter F. (Princeton NJ) Pawlenko Ivan (Holland PA) Wong Ching-Ping (Lawrenceville NJ), Method for encapsulating electronic conductors.
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Haswell Stephen J. (Cottingham GB2) Barclay David A. (Stourbridge GB2), Microwave heated digesting system for digesting materials to be analyzed.
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Collins Michael J. (Charlotte NC) Manchester Dennis P. (Matthews NC), Microwave heating apparatus for laboratory analyses.
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Schalk Andreas (Graz ATX) Kettisch Peter (Graz ATX) Sinabell Helmut (Graz ATX) Zach Johannes (Marein ATX), Microwave oven with temperature and pressure measuring device.
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Mengel Clare L. (5530 Longfellow Rd. Santa Barbara CA 93111), Microwave permeable pressure compensating container.
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Neas Edwin D. (Indian Trail NC) Floyd Terry S. (Clover SC), Microwave-based Kjeldahl method.
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Hukvari Istvan S. (Bettendorf IA) Albert Henry J. (Bettendorf IA) Moon Vernon G. (Moline IL) Steffenson Michael R. (Davenport IA), Pressure and temperature reaction vessel, method, and apparatus.
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Dalquist H. David (Minnetonka MN) Jorgensen Jorgen A. (Bloomington MN) Keleny Lloyd G. (Champlin MN) Nygren Donald W. (St. Louis Park MN) Taylor John N. (St. Louis Park MN), Pressure cooker for microwave ovens.
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Jennings,William E., Pressure measurement and relief for microwave-assisted chemical reactions.
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Buermann Henry, Pressure release safety cap.
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Thomas James Edward ; Hargett ; Jr. Wyatt Price ; King Edward Earl, Pressure sensing reaction vessel for microwave assisted chemistry.
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Thomas James Edward ; Hargett ; Jr. Wyatt Price ; King Edward Earl, Pressure sensing reaction vessel for microwave assisted chemistry.
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Hayes, Brittany L.; Collins, Michael J., Reaction and temperature control for high power microwave-assisted chemistry techniques.
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Hope, Rodney C.; Thrash, Jr., Thomas B.; Norton, Dennis S., Regulator with erosion resistant seal assemblies.
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Morris ; Neal R., Reusable closures for hermetically sealing containers.
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Hargett ; Jr. Wyatt Price, Sealing closure for high pressure vessels in microwave assisted chemistry.
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Dudek Daniel H. (Cockeysville MD), Sterilization method and apparatus for spices and herbs.
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Florkey,Edward J.; Gatchell,Ronald A.; Jones,Richard L.; Coyle,Michael J.; Stewart,Philip M., Sterilizer including air purging system and pressure actuated door seal.
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Chang, Lingo; Suter, Roger; Burkhard, Alan, System for controlling the operating pressures within a subterranean borehole.
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Grillo Angelo C. ; Burgener Paul E.,CAX, System for open and closed vessel microwave chemistry.
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Hargett Wyatt P. (Matthews NC) Littau Sara E. (Charlotte NC), Ventable rupture diaphragm-protected container for heating contained materials by microwave radiation.
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Miller,Albert R.; Moore,David N., Venting liner.
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