CN100334452C - Capacity setting, loop circulating gas analysis and appts. for constant sulfur instrument - Google Patents
Capacity setting, loop circulating gas analysis and appts. for constant sulfur instrument Download PDFInfo
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- CN100334452C CN100334452C CNB2004100231089A CN200410023108A CN100334452C CN 100334452 C CN100334452 C CN 100334452C CN B2004100231089 A CNB2004100231089 A CN B2004100231089A CN 200410023108 A CN200410023108 A CN 200410023108A CN 100334452 C CN100334452 C CN 100334452C
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Abstract
The present invention relates to a capacity fixed and loop closed cyclic gas analyzing method for a sulfur determiner. The present invention is characterized in that a pipeline communicated with a reaction furnace is provided with an electrolytic bath, a filter and gas chambers, which of the four and the reaction furnace form a closed circuit; a measuring and controlling unit is used for controlling the opening of gas valves and a gas pump arranged on the pipeline, and thereby, gas to be measured is circulated in the pipeline and the gas chambers; then, the gas of fixed capacity is pumped from the closed circuit, and the sulfur content of a test sample is measured by scale transformation. A device is that the inner part and the outer part of the reaction furnace are connected with a communicating pipe, and the communicating pipe is orderly connected with the two gas chambers, the gas valves, the filter, the electrolytic bath and the gas pump in series and enters the reaction furnace to form a closed circuit; the inlet end and the outlet end of the rear gas chamber are connected with a by-pass pipe which is provided with the two gas valves, and the gas pump is connected at the place between the two gas valves, is communicated with the reaction furnace, and is simultaneously connected with a waste gas treating device by another gas valve. The present invention makes the gas generated by the combustion of a test sample fully circulate, the concentration of the gas in the whole gas chambers and the pipeline is uniform, the testing accuracy is improved, and the sensitivity requirement of a sensor testing head is low.
Description
Technical field:
The present invention relates to the method for a kind of measurement solid or liquid combustible sulfur content, be specifically related to a kind of closed cycle method extraction sample that adopts and reach by the designed device of this method, be mainly used in industry or departments such as coal, oil, chemical industry, electric power, scientific research, teaching with the method for analyzing.
Background technology:
At present, constant sulphur appliance in the prior art field adopts the sulfur content in the coulometry mensuration sample, the sulfur dioxide gas that produces after sample burns in reacting furnace is introduced into the filtrator inner filtration by the pipeline that links to each other with the reacting furnace inner chamber, titration in electrolytic cell then, give birth to iodine and electricity according to electricity and give birth to the content that electric weight that bromine consumed is measured sulphur in the sample, adopt the mode of extracting gases in the test process while burning, airshed will be aspired for stability, owing to need continuous drawing gas in the mensuration process, and the distribution of the time of gas concentration is very uneven, therefore, and when gas concentration is low, susceptibility to transducer probe assembly requires height, is difficult to measure accurately.This method is had relatively high expectations to transducer probe assembly and airflow stability, otherwise can influence the accuracy of measurement.
Summary of the invention:
Technical matters to be solved by this invention is the defective that overcomes above-mentioned prior art, provides a kind of low to transducer probe assembly and airflow stability requirement, can accurately measure the closed cycle analysis method for gases and the device of sulfur content in the sample.
Technical matters of the present invention is to realize by following technical scheme.It is characterized in that it be by with pipeline that the specimen reaction stove communicates on the electrolytic cell of measuring usefulness is set, filtrator and a plurality of air chamber and a plurality of air pump, and make electrolytic cell, filtrator, each air chamber and air pump and reacting furnace are connected to form closed circuit by pipeline, utilize the unlatching of air valve and air pump set on the measurement and control unit pilot piping, thereby gas to be measured is circulated in pipeline and air chamber, in closed circuit, extract the gas of constant volume then, carry out ratiometric conversion by measurement and control unit, give birth to iodine according to electricity again and give birth to the electric weight that bromine is consumed, finish mensuration sulfur content in the sample with electricity.
The present invention comprises reacting furnace, electrolytic cell, filtrator and measurement and control unit according to the designed device of said method, it is characterized in that the external a connecting pipe of described reacting furnace burner hearth cavity, form the closed-loop path with entering in the reacting furnace burner hearth after first air chamber, first air valve, second air chamber, second air valve, filtrator, electrolytic cell, first air pump, the 7th air valve, the 9th air valve are connected in series in regular turn; Into and out of end, be connected to a by-pass pipe at second air chamber, this pipe is provided with first air valve, the 4th air valve, is connected to second air pump between two air valves, and this second air pump is communicated with reacting furnace, is connected with emission-control equipment by the 8th air valve simultaneously.At the second air chamber two ends, also be provided with one with its arranged side by side the 3rd air chamber of arrangement.
The present invention adopts closed circuit can make the gas after sample burns fully obtain circulation, can guarantee gas concentration uniformity in its whole air chamber and the pipeline, has improved the accuracy of test, has reduced the susceptibility requirement of sensor side head simultaneously.
Description of drawings:
Fig. 1 is apparatus of the present invention embodiment one synoptic diagram;
Fig. 2 is apparatus of the present invention embodiment two synoptic diagram.
Among the figure:
The 1-reacting furnace; 2-first air chamber; 3-first air valve;
The 4-second air valve 5-the 3rd air valve 6-second air chamber;
7-the 3rd air chamber 8-the 4th air valve 9-the 5th air valve;
10-filtrator 11-the 6th air valve 12-electrolytic cell;
13-first air pump; 14-the 7th air valve 15-emission-control equipment;
16-the 8th air valve 17-second air pump; 18-the 9th air valve;
The 19-measurement and control unit.
Embodiment:
The applicant is through discovering, existing coulometry adopts the assay method of sample extracting gases while burning, because gas flow is to adopt the open type circuit, therefore, the concentration of gas can be very inhomogeneous, thereby can cause the instability of test.The present invention circulates in the loop of a sealing by making the gas after the burning, then by the trend of gas in the operation valve control loop is set, the uneven problem of gas concentration in the time of can solving test, the gas that only extracts less capacity during mensuration gets final product, thereby has realized the technique effect that the present invention will reach.Concrete grammar of the present invention is: establish a connecting pipe and communicate with the specimen reaction stove, one or more air chambers are set on this pipeline simultaneously, air valve, filtrator, the electrolytic cell of air pump and mensuration usefulness, and make each air chamber, air valve, filtrator, air pump and electrolytic cell form closed circuit by pipeline and reacting furnace, the gas that is produced behind the reacting furnace internal reaction can flow in this loop, utilize measurement and control unit to control the unlatching of air valve and air pump set on its pipeline then, thereby gas to be measured is circulated on the pipeline of setting and in the air chamber, in the air chamber of setting, extract the gas of constant volume then, the gas gross that is produced after by measurement and control unit reacting furnace being reacted again and the constant volume gas volume of extraction carry out ratiometric conversion, just can finish the mensuration to sulfur content in the sample.
The present invention has designed the complete control device of a cover according to said method, Fig. 1 has showed an Application Example of the present invention, it comprises reacting furnace 1, electrolytic cell 12, filtrator 10 and measurement and control unit 19, it is characterized in that at the external a connecting pipe of reacting furnace 1 burner hearth cavity, in regular turn with first air chamber 2, second air valve 4, second air chamber 6, the 5th air valve 9, filtrator 10, electrolytic cell 12, first air pump 13, the 7th air valve 14, enter in reacting furnace 1 burner hearth after the 9th air valve 18 serial connections, form the closed-loop path, gas after the burning can circulate in this closed-loop path, so that it is evenly distributed when being in arbitrary position.Wherein second air valve, 4 may command gases enter in second air chamber 6, and the 5th air valve 9 enters the switch of filtrator 10 for pilot-gas, and the 7th air valve 14, the 9th air valve 18 are the switch of pilot piping closed circuit.At second air chamber 6 into and out of end, also be connected to a by-pass pipe, this pipe is provided with first air valve 3, the 4th air valve 8, be connected to second air pump 17 between two air valves, this second air pump 17 is communicated with reacting furnace 1, is connected with emission-control equipment 15 by the 8th air valve 16 simultaneously, after sample mensuration finishes, can the gentle indoor gas of pipeline be extracted by second air pump 17, discharge, enter next test process by emission-control equipment 15.
For the negative pressure of avoiding the excessive generation of air pressure in the closed-loop path causes the power of gas first air pump, 13 needs when extracting too big, offer a branch line respectively at second air chamber 6 and electrolytic cell 12 inlet ends, can connect with outside air, the 3rd air valve 5 and the 6th air valve 11 are housed respectively on this pipeline, control its keying by it.
As shown in Figure 2, the present invention is for fully holding gas, at second air chamber, 6 two ends, also can be provided with one with its 3rd air chamber 7 of arrangement side by side.
The course of work of the present invention:
(1) earlier reacting furnace 1 is warming up to 1150 ℃ of constant temperature, keeps the interior device environment of pipeline to be in steady state (SS) simultaneously, at this moment reacting furnace 1 oven door opening, sample is sent in the burner hearth, second air pump 17 is opened, and second air valve 4, the 4th air valve 8, the 9th air valve 18 are opened, and all the other air pumps, air valve are closed;
(2) reacting furnace 1 fire door is closed, sample takes fire, and at this moment, second air pump 17 is opened, and second air valve 4, the 4th air valve 8, the 9th air valve 18 are opened, and all the other air pumps, air valve are closed.The gas of sample burning enters at the effect lower edge of second air pump 17 first air chamber 2, second air chamber 6 and forms circulation in reacting furnace 1 burner hearth, makes in first air chamber 2, second air chamber 6 and the whole pipeline distribution of gas even;
(3) behind the sample all burnt, oven door opening, at this moment second air pump 17, first air pump 13 are opened, the 3rd air valve 5, first air valve 3, the 8th air valve 16, the 7th air valve 14, the 5th air valve 9 are opened, second air valve 4, the 4th air valve 8, the 9th air valve 18 are closed, place second air chamber, 6 interior gases after process filter 10 filters under the effect of first air pump 13, to enter electrolytic cell 12 titration, undertaken measuring its sulfur content after the ratiometric conversion by measurement and control unit 19.Simultaneously, waste gas in first air chamber 2 and the waste gas of measuring after finishing enter discharge in the emission-control equipment 15 by second air pump 17, first air pump 13, finish whole mensuration process.
The present invention also can be applicable in the analysers such as spectrum, infrared, galvanochemistry and carries out gas sample and gas composition analysis.
Claims (3)
1, a kind of closed cycle analysis method for gases of measuring the combustible sulfur content, it is characterized in that it be by with pipeline that the specimen reaction stove communicates on the electrolytic cell of measuring usefulness is set, filtrator and a plurality of air chamber and a plurality of air pump, and make electrolytic cell, filtrator, each air chamber and air pump and reacting furnace are connected to form closed circuit by pipeline, utilize the unlatching of air valve and air pump set on the measurement and control unit pilot piping, thereby gas to be measured is circulated in pipeline and air chamber, in closed circuit, extract the gas of constant volume then, carry out ratiometric conversion by measurement and control unit, give birth to iodine according to electricity again and give birth to the electric weight that bromine is consumed, finish mensuration sulfur content in the sample with electricity.
2, a kind of closed cycle gas analyzing apparatus of measuring the combustible sulfur content, comprise reacting furnace (1), electrolytic cell (12), filtrator (10) and measurement and control unit (19), it is characterized in that the external a connecting pipe of described reacting furnace (1) burner hearth cavity, enter formation closed-loop path in reacting furnace (1) burner hearth in regular turn with after first air chamber (2), first air valve (4), second air chamber (6), second air valve (9), filtrator (10), electrolytic cell (12), first air pump (13), the 7th air valve (14), the 9th air valve (18) are connected in series; At second air chamber (6) into and out of end, be connected to a by-pass pipe, this pipe is provided with first air valve (3), the 4th air valve (8), is connected to second air pump (17) between two air valves, this second air pump (17) is communicated with reacting furnace (1), is connected with emission-control equipment (15) by the 8th air valve (16) simultaneously.
3, a kind of closed cycle gas analyzing apparatus of measuring the combustible sulfur content according to claim 2 is characterized in that at second air chamber (6) two ends, also be provided with one with its arranged side by side the 3rd air chamber (7) of arrangement.
Priority Applications (1)
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CNB2004100231089A CN100334452C (en) | 2004-04-15 | 2004-04-15 | Capacity setting, loop circulating gas analysis and appts. for constant sulfur instrument |
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CNB2004100231089A CN100334452C (en) | 2004-04-15 | 2004-04-15 | Capacity setting, loop circulating gas analysis and appts. for constant sulfur instrument |
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CN1563933A CN1563933A (en) | 2005-01-12 |
CN100334452C true CN100334452C (en) | 2007-08-29 |
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Cited By (1)
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CN110426252A (en) * | 2019-07-05 | 2019-11-08 | 北京空间飞行器总体设计部 | A kind of visualization microgravity gas trapping experimental rig |
Families Citing this family (3)
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CN102520013B (en) * | 2011-12-22 | 2013-12-11 | 中国科学技术大学 | Hot-film gas extinguishing chemical concentration sensing module |
CN105510425B (en) * | 2016-01-29 | 2018-08-07 | 湖南省计量检测研究院 | A kind of coulomb of Sulfur inspector |
CN108490111B (en) * | 2018-05-21 | 2023-09-01 | 沈阳工程学院 | Constant volume pipe type flame propagation measuring device |
Citations (8)
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SU800860A1 (en) * | 1979-04-11 | 1981-01-30 | Предприятие П/Я Р-6900 | Electrohemical gasanalyzer |
US4532023A (en) * | 1983-03-12 | 1985-07-30 | Kernforschungsanlage Julich Gmbh | Electrochemical gas analyzer for determination of sulphur dioxide content of gases |
EP1000334A1 (en) * | 1998-05-12 | 2000-05-17 | Elf Exploration Production | Analyzer for continuously measuring h 2?s contained in a gas and device including same for regulating the air flow rate injected into an h 2?s sulphur oxidation reactor |
CN2483718Y (en) * | 2001-03-19 | 2002-03-27 | 长沙三德实业有限公司 | High temp. combustion tube of infrared sulphur analysis instrument |
US20030178323A1 (en) * | 2000-05-22 | 2003-09-25 | Andreas Fiedler | Method and apparatus for anlyzing a component in a liquid sample |
DE10321357A1 (en) * | 2002-05-13 | 2003-12-04 | Ech Elektrochemie Halle Gmbh | Quantitative electrochemical determination e.g. for environmental pollutant monitoring, of absorbed pyrolysis gases from small samples |
CN2591623Y (en) * | 2002-02-08 | 2003-12-10 | 长沙三德实业有限公司 | Automatic industrial analysis meter/sulfur determinator with gate control apparatus |
CN2704841Y (en) * | 2004-06-18 | 2005-06-15 | 长沙三德实业有限公司 | Volume fixing and closed loop cyclic gas analyzer of sulfur determiner |
-
2004
- 2004-04-15 CN CNB2004100231089A patent/CN100334452C/en not_active Expired - Fee Related
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
SU800860A1 (en) * | 1979-04-11 | 1981-01-30 | Предприятие П/Я Р-6900 | Electrohemical gasanalyzer |
US4532023A (en) * | 1983-03-12 | 1985-07-30 | Kernforschungsanlage Julich Gmbh | Electrochemical gas analyzer for determination of sulphur dioxide content of gases |
EP1000334A1 (en) * | 1998-05-12 | 2000-05-17 | Elf Exploration Production | Analyzer for continuously measuring h 2?s contained in a gas and device including same for regulating the air flow rate injected into an h 2?s sulphur oxidation reactor |
US20030178323A1 (en) * | 2000-05-22 | 2003-09-25 | Andreas Fiedler | Method and apparatus for anlyzing a component in a liquid sample |
CN2483718Y (en) * | 2001-03-19 | 2002-03-27 | 长沙三德实业有限公司 | High temp. combustion tube of infrared sulphur analysis instrument |
CN2591623Y (en) * | 2002-02-08 | 2003-12-10 | 长沙三德实业有限公司 | Automatic industrial analysis meter/sulfur determinator with gate control apparatus |
DE10321357A1 (en) * | 2002-05-13 | 2003-12-04 | Ech Elektrochemie Halle Gmbh | Quantitative electrochemical determination e.g. for environmental pollutant monitoring, of absorbed pyrolysis gases from small samples |
CN2704841Y (en) * | 2004-06-18 | 2005-06-15 | 长沙三德实业有限公司 | Volume fixing and closed loop cyclic gas analyzer of sulfur determiner |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110426252A (en) * | 2019-07-05 | 2019-11-08 | 北京空间飞行器总体设计部 | A kind of visualization microgravity gas trapping experimental rig |
CN110426252B (en) * | 2019-07-05 | 2021-09-24 | 北京空间飞行器总体设计部 | Visual microgravity gas trapping test device |
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