IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0951760
(2001-09-11)
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발명자
/ 주소 |
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출원인 / 주소 |
- SpectrolAnalytical Instruments
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대리인 / 주소 |
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인용정보 |
피인용 횟수 :
10 인용 특허 :
56 |
초록
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An improved on-stream analyzer for monitoring sulfur or nitrogen content of liquid petroleum or beverage products is described. It consists of the following main components: a sample injector for injecting predetermined fixed volumes of the liquid into a thermal oxidizer (pyrolyzer) at a preset, con
An improved on-stream analyzer for monitoring sulfur or nitrogen content of liquid petroleum or beverage products is described. It consists of the following main components: a sample injector for injecting predetermined fixed volumes of the liquid into a thermal oxidizer (pyrolyzer) at a preset, controlled rate, a thermal oxidizer in which an inert carrier gas and oxygen are introduced at measured and preset, controlled rates to thermally oxidize the sample at a temperature of about 1050° C., sample conditioner to control the relative humidity and temperature of the resulting gas mixture, an electrochemical cell sensitive to sulfur dioxide (SO 2 ) or NO to measure the concentration of SO 2 or NO in the gas mixture, and a programmable logic controller (PLC) to calculate the sulfur content of the original sample and manage the analyzer. Although the analyzer is designed primarily for monitoring sulfur content of petroleum and beverage products, it is recognized that essentially the same equipment can be used to analyze any liquid having a suitable viscosity and capable of being completely thermally oxidized under the conditions specified.
대표청구항
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1. An on-stream analyzer for measuring the concentration of a substance in a fluid sample, said analyzer comprising:a. a sample injector for injecting a sample at a preset and controlled rate, the sample injector further comprising a pressure regulator coupled to a flow restrictor to control the rat
1. An on-stream analyzer for measuring the concentration of a substance in a fluid sample, said analyzer comprising:a. a sample injector for injecting a sample at a preset and controlled rate, the sample injector further comprising a pressure regulator coupled to a flow restrictor to control the rate of sample flow;b. a port for a carrier gas and a port for a pyrolysis gas;c. a thermal oxidizer comprising a tube furnace and a pyrolysis tube, connected to the sample injector;d. a sample conditioner, connected to and located downstream from the thermal oxidizer, said sample conditioner comprising a dryer wherein said dryer further comprises two concentric tubes, an inner tube composed of a membrane for transferring water vapor and an outer tube composed of inert material, wherein the dryer is configured such that during use a dry purge gas is in fluid communication with the inner tube and a sample gas is in fluid communication with the annular space between the inner and outer tube, and further wherein the inner tube is connected to an orifice to maintain positive pressure;e. a detector, connected to the sample conditioner, to measure the concentration of oxidized substance contained within the sample gas; andf. a programmable logic controller, connected to the detector, to calculate the concentration of oxidized substance contained within the gas mixture and consequently the concentration of substance in the original fluid sample. 2. The analyzer of claim 1 further wherein the flow restrictor is a metering valve. 3. The analyzer of claim 1 wherein the flow restrictor is a length of capillary tubing having a diameter of from about 0.001 to about 0.020 inches. 4. The analyzer of claim 3 wherein the capillary tubing has a diameter of about 0.004 inches. 5. The analyzer of claim 1 further comprising a container to enclose the thermal oxidizer. 6. The analyzer of claim 5 wherein, during operation of the analyzer, an outer surface temperature of the container does not exceed the lower explosive temperature of the sample being analyzed and the container prevents ingress of vapors of the sample being analyzed. 7. The analyzer of claim 1 wherein the carrier gas comprises argon, helium, mixtures thereof or mixtures of argon or helium with oxygen. 8. The analyzer of claim 1 wherein the pyrolysis gas comprises oxygen. 9. The analyzer of claim 1 further comprising one or more electronic flowmeters to measure the flow rates of carrier and pyrolysis gases introduced, and the total flow rate of the gas mixture. 10. The analyzer of claim 9, further comprising metering valves for controlling the flow rates of the carrier and pyrolysis gases. 11. The analyzer of claim 9 wherein the electronic flowmeters are connected to the programmable logic controller. 12. The analyzer of claim 9 wherein the electronic flowmeter further comprises a gas flow alarm to indicate a flow rate of carrier gas, pyrolysis gas, or gas mixture that falls outside a preselected range. 13. The analyzer of claim 1 wherein the tube furnace produces a temperature range of from about 1000° C. to about 1200° C. 14. The analyzer of claim 1 wherein the tube furnace produces a temperature of about 1050° C. 15. The analyzer of claim 1 wherein the detector comprises an assembly having one or more electrochemical cells. 16. The analyzer of claim 15 wherein one or more electrochemical cells measures the concentration of SO 2 in the mixture. 17. The analyzer of claim 15 wherein one or more electrochemical cells measures the concentration of NO in the mixture. 18. The analyzer of claim 15 wherein the one or more electrochemical cells further comprises an electrochemical cell capable of detecting SO 2 and an electrochemical cell capable of detecting NO. 19. The analyzer of claim 1 further comprising a combustible gas sensor to indicate the presence of combustible gas vapors. 20. The analyzer of claim 1 further comprising a humidifier located upstream from the assembly havi ng one or more electrochemical cells. 21. The analyzer of claim 20 wherein the humidifier operates to maintain a relative humidity level of about 15 to 90%. 22. The analyzer of claim 20 wherein the humidifier comprises an alarm to indicate a relative humidity level which falls outside a preselected range. 23. The analyzer of claim 1 wherein the fluid sample is routed to the thermal oxidizer via the injector by non-electrical valves. 24. The analyzer of claim 23 wherein the non-electrical valves are pneumatically operated. 25. The analyzer of claim 1 wherein the sample conditioner further comprises a filter, and a heat trace element, the heat trace element further comprising self-limiting electrical heating wires effective to maintain the gas stream temperature above its dewpoint from the pyrolysis tube to the dryer. 26. The sample conditioner of claim 25 wherein the filter is a chemically inert membrane designed to prevent solid particles or liquid drops from passing downstream without significantly restricting the gas flow. 27. The analyzer of claim 1, further comprising a fluid sample outlet stream and a non-electric flow indicator to indicate the flow rate of the fluid sample outlet stream. 28. The analyzer of claim 1, further comprising a means for introducing one or more calibration fluids, contained in one or more calibration sample reservoirs, to the injector employing gas pressure and pneumatically operated valves. 29. The analyzer of claim 28, further comprising one or more metering valves to control the flow rate of the calibration fluids. 30. The analyzer of claim 1, further comprising solenoid valves controlled by the programmable logic controller to effectuate flow of a calibration gas directly to the detector, bypassing the thermal oxidizer and sample conditioner. 31. The analyzer of claim 1, further comprising solenoid valves and pneumatically-actuated pressure switches to send signals via solenoid valves to the programmable logic controller to indicate low gas pressure. 32. The analyzer of claim 1 wherein the inert material is a fluoropolymer or stainless steel. 33. The analyzer of claim 1 wherein the membrane is a membrane having sulfonic acid groups. 34. The analyzer of claim 1 wherein the orifice has a diameter of about 0.001 to about 0.05 inches. 35. The analyzer of claim 34 wherein the orifice has a diameter of about 0.0122 inches. 36. The analyzer of claim 34 wherein the electronic flow meter further comprises an alarm to indicate a purge gas flow that falls outside a preselected range. 37. The analyzer of claim 1 further comprising a metering valve to control the purge gas flow. 38. The analyzer of claim 37 further comprising an electronic flow meter, connected to the programmable logic controller, to monitor the purge gas flow. 39. An on-stream analyzer for detecting a substance in a fluid sample, said analyzer comprising:a. a fluid sample injector for injecting a sample at a preset and controlled rate;b. a thermal oxidizer, connected to the sample injector, to inject the sample into the thermal oxidizer and means to introduce a carrier gas and a pyrolysis gas to the sample under oxidation conditions;c. a sample conditioner, connected to the thermal oxidizer, to control the conditions of a resulting mixture, wherein the conditioner further comprises a dryer for removing water vapor, wherein the dryer further comprises two concentric tubes, an inner tube composed of a membrane for transferring water vapor and an outer tube composed of an inert material, wherein the dryer is configured such that a dry purge gas is in fluid communication with the inner tube and the sample gas is in fluid communication with the annular space between the inner and outer tube, and further wherein the inner tube is connected to an orifice to maintain positive pressure;d. one or more electrochemical cells, connected to the sample conditioner, to measure the concentration of a substance contained within the sample; ande. a progr ammable logic controller, connected to the electrochemical cells, to calculate the concentration of a substance contained within the mixture. 40. The analyzer of claim 39 wherein the sample injector further comprises a pressure regulator coupled to a metering valve to control the rate of sample flow. 41. The analyzer of claim 39 wherein the sample injector further comprises a pressure regulator coupled to a length of capillary tubing having a diameter of from about 0.0001 to about 0.020 inches to control the rate of sample flow. 42. The analyzer of claim 39 wherein the inert material is a fluoropolymer or stainless steel. 43. The analyzer of claim 39 wherein the membrane is a membrane having sulfonic acid groups. 44. An on-stream analyzer for detecting a substance in a liquid sample, said analyzer comprising:a. a liquid sample injector for injecting a sample at a preset and controlled rate, wherein the sample injector further comprises a pressure regulator coupled to a metering valve to control the rate of sample flow;b. a combustible gas sensor to detect the presence of combustible gas vapors;c. a thermal oxidizer comprising a tube furnace and a pyrolysis tube, connected to the sample injector and enclosed within a container;d. a port for a carrier gas and a port for a pyrolysis gas;e. a sample conditioner, connected to the thermal oxidizer, to control the conditions of a resulting mixture, wherein the conditioner further comprises:a dryer for removing water vapor, wherein the dryer comprises two concentric tubes, an inner tube composed of a perfluorinated membrane having sulfonic acid groups and an outer tube composed of a fluoropolymer, wherein the dryer is configured such that a dry purge gas is in fluid communication with the inner tube and the sample gas is in fluid communication with the annular space between the inner and outer tube, and further wherein the inner tube is connected to an orifice to maintain positive pressure;a heat trace element comprising self-limiting electrical heating wires effective to maintain the gas stream temperature above its dewpoint from the pyrolysis tube to the dryer;a humidifier that operates to maintain a relative humidity level of the gas stream from about 15 to about 90%, the humidifier further comprising an alarm to indicate a humidity level which falls outside the preselected humidity level;f. one or more electrochemical cells, connected to the sample conditioner, to measure the concentration of a substance contained within the sample;g. one or more pneumatic valves for introducing calibration samples and one or more calibration sample reservoirs;h. one or more solenoid valves, connected to the programmable logic controller, to effectuate flow of one or more calibration gases directly to the detector, bypassing the thermal oxidizer and sample conditioner;i. one or more pneumatically operated valves to effectuate the routing of the liquid and calibration samples; andj. a programmable logic controller, connected to the electrochemical cell, to calculate the concentration of pollutants contained within the mixture.
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