CN214011146U - Analysis system for total sulfur and subentry sulfur in coal gas - Google Patents
Analysis system for total sulfur and subentry sulfur in coal gas Download PDFInfo
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- CN214011146U CN214011146U CN202023107415.9U CN202023107415U CN214011146U CN 214011146 U CN214011146 U CN 214011146U CN 202023107415 U CN202023107415 U CN 202023107415U CN 214011146 U CN214011146 U CN 214011146U
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Abstract
The utility model discloses an analysis system for total sulfur and itemized sulfur in coal gas, which comprises a sampling unit, a separation unit, a gas circuit connection unit and a detection unit, wherein the sampling unit comprises a first fixed-volume sampling tube, a second fixed-volume sampling tube and a ten-way valve; the separation unit comprises a subentry sulfur separation unit and a total sulfur separation unit, and the subentry sulfur separation unit comprises a subentry sulfur chromatographic column; the total sulfur separation unit comprises a total sulfur analysis chromatographic column, a six-way valve and a tee joint; the gas path connecting unit comprises a pipeline and a cross joint; the detection unit includes a first flame photometric detector and a second flame photometric detector. The utility model discloses an analytic system detectivity is high, and stability is good, and analysis cycle is short, and measurement accuracy is high, can satisfy the simultaneous determination of total sulphur and subentry sulphur in the coal gas. The utility model discloses an analytical method has major breakthrough in analysis cycle, data validity, chromatograph stability and manufacturing cost.
Description
Technical Field
The utility model relates to a matter analytic system especially relates to an analytic system that is arranged in total sulphur of coal gas and branch sulphur.
Background
The coal gas has many kinds and complex components, such as blast furnace gas, coke oven gas and the like, wherein the main sulfides are hydrogen sulfide, carbonyl sulfide, sulfur dioxide, carbon disulfide, thiophene, methyl sulfide, methyl mercaptan and other unknown components. At present, most of sulfur in coal gas is detected by hydrogen sulfide, and the hydrogen sulfide in the coal gas is detected by an iodometry method, a formaldehyde absorption-pararosaniline absorption method, a constant potential electrolysis method, a non-infrared dispersion absorption method and a gas chromatography method, but the method is not a real total sulfur and subentry sulfur analysis, and the total sulfur is detected by adopting an ICP emission spectrum and a microcoulomb titration method, so that the sampling is complex and the period is long. Therefore, it is an urgent problem for those skilled in the art to develop an analysis system for total sulfur and fractional sulfur in coal gas.
SUMMERY OF THE UTILITY MODEL
The utility model relates to a solve the above-mentioned not enough, the utility model provides an analytic system that is arranged in coal gas total sulphur and branch item sulphur is applicable to various coal gas on-line monitoring chromatograph and laboratory complete machine system, carries out accurate analysis to the sample, shortens analysis cycle.
The above object of the present invention is achieved by the following technical solutions: an analysis system for total sulfur and subentry sulfur in coal gas comprises a sampling unit, a separation unit, a gas circuit connection unit and a detection unit, wherein the sampling unit comprises a first fixed-volume sampling tube, a second fixed-volume sampling tube and a ten-way valve, and the analysis system is guaranteed to be free of air leakage when a sample enters the separation unit for switching; the separation unit comprises a fractional sulfur separation unit and a total sulfur separation unit, and the fractional sulfur separation unit comprises a fractional sulfur chromatographic column; the total sulfur separation unit comprises a total sulfur analysis chromatographic column, a six-way valve and a tee joint, and the component separation is completed through valve cutting and back flushing; the gas path connecting unit comprises a pipeline and a cross joint; the detection unit includes a first flame photometric detector and a second flame photometric detector.
Furthermore, in the sampling unit, a sample gas inlet pipeline is connected with the interface of the ten-way valve, two ends of a first fixed-volume sampling pipe are connected with the 1 st interface and the 4 th interface of the ten-way valve, a second fixed-volume sampling pipe is connected with the 5 th interface and the 8 th interface of the ten-way valve, and a sample vent is connected with the 9 th interface of the ten-way valve;
in the gas path connection unit, carrier gas forms three paths of carrier gas after passing through the four-way valve, wherein the three paths of carrier gas are respectively a first path of carrier gas connected with the 3 rd interface of the ten-way valve, a second path of carrier gas connected with the 7 th interface of the ten-way valve and a third path of carrier gas connected with the 3 rd interface of the six-way valve;
in the item sulfur separation unit, an inlet of an item sulfur chromatographic column is connected with a 2 nd interface of the ten-way valve, and an outlet is directly connected with a first flame photometric detector;
in the total sulfur separation unit, the 6 th interface of the ten-way valve is connected with the 6 th interface of the six-way valve, the two ends of the total sulfur analysis chromatographic column are respectively connected with the 1 st interface and the 4 th interface of the six-way valve, and the 2 nd interface and the 5 th interface of the six-way valve are connected with the second flame photometric detector through a three-way interface.
Further, the total sulfur analytical column was a 30m 0.53mm 3um SE-30 capillary column.
Further, the fractional sulfur chromatography column was a 50m 0.53mm 3um SE-30 capillary chromatography column.
Further, the pipeline used by the pipeline is passivated, so that a passivation treatment layer is formed on the inner wall of the pipeline, sulfide peak type tailing is prevented, and the influence on measurement accuracy caused by adsorption of a sample is prevented.
An analysis method for total sulfur and subentry sulfur in coal gas comprises the following steps:
(1) fractional sulfur analysis: when the ten-way valve is in a reset state, air inlet is started, after sample gas to be detected passes through the first sampling tube with a certain volume, the ten-way valve is switched to enter a sample introduction state, the sample gas in the first sampling tube with a certain volume enters the fractional sulfur chromatographic column under the drive of the first carrier gas, and air, carbon dioxide, hydrogen sulfide, carbonyl sulfide, carbon disulfide and the like sequentially flow into the first flame photometric detector for detection;
(2) total sulfur analysis: the second fixed-volume sampling tube is driven by a second path of carrier gas and reaches the six-way valve through a pipeline, in the reset state of the six-way valve, sample gas is separated through the total sulfur analysis chromatographic column and passes through the tee joint with a third path of carrier gas, and the components of air and carbon dioxide firstly enter a second flame photometric detector;
(3) back flushing: when the carbon dioxide flows out of the total sulfur analysis chromatographic column, switching the ten-way valve to enter a back flushing flow, and quickly flushing the sulfur components after the carbon dioxide out of the total sulfur analysis chromatographic column by the third path of carrier gas from the rear end of the total sulfur analysis chromatographic column through the tee joint to enter a second flame photometric detector for detection;
(4) resetting: and (4) after the step (3) is finished for 1 minute, resetting the six-way valve and the ten-way valve and waiting for the next analysis.
The utility model discloses an analytic system design characteristics and advantage characteristics:
1. the method adopts an integrated full-integration (all in one) technical design idea, and realizes the high-efficiency and convenient online detection of trace sulfur components (total sulfur, hydrogen sulfide and organic sulfur) for the first time by adopting a double-valve double-flame photometric detector (FPD detector) process.
2. The whole gas path adopts a sulfur passivation pipe to prevent trace sulfides from being adsorbed; the chromatographic system adopts a high-sensitivity flame photometric detector (FPD detector), and the detection precision is higher.
3. A full-automatic sample introduction system is designed, and the time interval can be set automatically. The device comprises a built-in gas path pressure stabilizing device, built-in pretreatment equipment and a built-in gas path selection system; and a zero gas generator and a hydrogen gas generator are integrated in the analysis system.
4. The designed online analysis system is provided with the purging flow path, so that purging time during sample switching is reduced, analysis efficiency is improved, and analysis precision and accuracy are improved. The whole system adopts an anti-corrosion and anti-adsorption system, so that the service life of the instrument is longer, the detection limit and accuracy of low-concentration impurities are improved, and the analysis precision is higher.
Compared with the prior art, the utility model the advantage be:
the utility model discloses an analytic system detectivity is high, and stability is good, and analysis cycle is short, and measurement accuracy is high, can satisfy the simultaneous determination of total sulphur and subentry sulphur in the coal gas.
The utility model discloses an analytical method has major breakthrough in analysis cycle, data validity, chromatograph stability and manufacturing cost.
1. The total sulfur analysis period is shortened. And after the target peak carbon dioxide flows out, the six-way valve is switched to enter a back-blowing mode, so that sulfides can be back-blown into the detector, the interference of high-boiling-point organic matters on the analysis of the next period is eliminated, the stability and the recognition degree of component retention time are ensured, the analysis period is shortened, and the service life of the chromatographic column is prolonged.
2. The analysis result meets the requirements. The needle valve is added at the front end of the total hydrocarbon empty column, the amount of the sample entering the two chromatographic columns is adjusted, and the ratio of the total hydrocarbon peak area to the methane peak area is controlled, so that the response ratio of the amount of the sample entering the two chromatographic columns on the detector is in the optimal state, and the effectiveness of each analysis data is ensured.
3. Greatly improving the stability of the chromatograph. The adoption of chromatographic column does not carry out split sample injection, all samples enter the chromatographic column, the split discrimination phenomenon is eliminated, the adoption of the large-caliber capillary column has small base line fluctuation generated after valve switching, the sensitivity of the instrument is improved, and the detection limit is lower.
4. The production cost is reduced. Compared with the traditional chemical analysis method, the analysis method shortens the analysis time. The gas circuit connection is simple, the material and labor loss during assembly and debugging are reduced, and the production cost is reduced.
Drawings
Fig. 1 is a schematic structural diagram of the analysis system of the present invention.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
As shown in fig. 1, an analysis system for total sulfur and fractional sulfur in gas comprises a sampling unit, a separation unit, a gas path connection unit and a detection unit, wherein the sampling unit comprises a first fixed-volume sampling tube 101, a second fixed-volume sampling tube 102 and a ten-way valve 103, so that no air leakage affects the analysis system when a sample enters the separation unit for switching; the separation unit comprises a fractional sulfur separation unit and a total sulfur separation unit, and the fractional sulfur separation unit comprises a fractional sulfur chromatographic column 104; the total sulfur separation unit comprises a total sulfur analysis chromatographic column 107, a six-way valve 108 and a tee joint 109, and component separation is completed through valve cutting and back flushing; the gas path connecting unit comprises a pipeline 111 and a cross joint 105; the detection unit comprises a first flame photometric detector 106 and a second flame photometric detector 110.
Further, in the sampling unit, a sample gas inlet pipeline is connected with a 10 th interface of the ten-way valve 103, two ends of a first fixed-volume sampling pipe 101 are connected with a 1 st interface and a 4 th interface of the ten-way valve 103, a second fixed-volume sampling pipe 102 is connected with a 5 th interface and an 8 th interface of the ten-way valve 103, and a sample vent is connected with a 9 th interface of the ten-way valve 103;
in the gas path connection unit, the carrier gas 112 forms three paths of carrier gas after passing through the cross joint 105, wherein the three paths of carrier gas are respectively a first path of carrier gas connected with the 3 rd interface of the ten-way valve 103, a second path of carrier gas connected with the 7 th interface of the ten-way valve 102 and a third path of carrier gas connected with the 3 rd interface of the six-way valve 108;
in the item sulfur separation unit, an inlet of an item sulfur chromatographic column 104 is connected with a 2 nd interface of the ten-way valve 103, and an outlet is directly connected with a first flame photometric detector 106;
in the total sulfur separation unit, the 6 th interface of the ten-way valve 103 is connected with the 6 th interface of the six-way valve 108, two ends of the total sulfur analysis chromatographic column 107 are respectively connected with the 1 st interface and the 4 th interface of the six-way valve 108, and the 2 nd interface and the 5 th interface of the six-way valve are connected with the second flame photometric detector 110 through the 10 th and 9 th interfaces of the three-way valve.
Further, the total sulfur analysis column 107 was a 30m 0.53mm 3um SE-30 capillary column.
Further, the fractional sulfur chromatography column 104 was a 50m 0.53mm 3um SE-30 capillary chromatography column.
Further, the pipe 111 is passivated, so that a passivation layer is formed on the inner wall of the pipe 111, sulfide peak type tailing is prevented, and the sample is prevented from being adsorbed to influence the measurement accuracy.
An analysis method for total sulfur and subentry sulfur in coal gas comprises the following steps:
(1) fractional sulfur analysis: when the ten-way valve 103 is in a reset state, air inlet is started, after sample gas to be detected passes through the first sampling tube 101 with a certain volume, the ten-way valve 103 is switched to enter a sample injection state, the sample gas in the first sampling tube 101 with a certain volume enters the fractional sulfur chromatographic column 104 under the drive of the first carrier gas, and air, carbon dioxide, hydrogen sulfide, carbonyl sulfide, carbon disulfide and the like sequentially flow into the first flame photometric detector 106 for detection;
(2) total sulfur analysis: the second fixed-volume sampling tube 102 is driven by the second path of carrier gas to reach the six-way valve 108 through a pipeline, under the reset state of the six-way valve 108, the sample gas is separated by the total sulfur analysis chromatographic column 107 and passes through the tee 109 with the third path of carrier gas, and the components of air and carbon dioxide firstly enter the second flame photometric detector 110;
(3) back flushing: when the carbon dioxide flows out of the total sulfur analysis chromatographic column 107, the ten-way valve 103 is switched to enter a back blowing process, and the third path of carrier gas quickly blows the sulfur components after the carbon dioxide out of the total sulfur analysis chromatographic column 107 from the rear end of the total sulfur analysis chromatographic column 107 in a back blowing manner and enters a second flame photometric detector 110 for detection through a tee 109;
(4) resetting: and (4) after the step (3) is finished for 1 minute, resetting the six-way valve and the ten-way valve and waiting for the next analysis.
The above only is the embodiment of the present invention, not limiting the patent scope of the present invention, all the equivalent structures or equivalent processes that are used in the specification and the attached drawings or directly or indirectly applied to other related technical fields are included in the patent protection scope of the present invention.
Claims (4)
1. An analysis system for total sulfur and fractional sulfur in coal gas, characterized in that: the device comprises a sampling unit, a separation unit, a gas circuit connection unit and a detection unit, wherein the sampling unit comprises a first fixed-volume sampling tube, a second fixed-volume sampling tube and a ten-way valve; the separation unit comprises a fractional sulfur separation unit and a total sulfur separation unit, and the fractional sulfur separation unit comprises a fractional sulfur chromatographic column; the total sulfur separation unit comprises a total sulfur analysis chromatographic column, a six-way valve and a tee joint; the gas path connecting unit comprises a pipeline and a cross joint; the detection unit comprises a first flame photometric detector and a second flame photometric detector;
in the sampling unit, a sample gas inlet pipeline is connected with a 10 th interface of the ten-way valve, two ends of a first constant volume sampling pipe are connected with a 1 st interface and a 4 th interface of the ten-way valve, a second constant volume sampling pipe is connected with a 5 th interface and an 8 th interface of the ten-way valve, and a sample vent is connected with a 9 th interface of the ten-way valve;
in the gas path connection unit, carrier gas forms three paths of carrier gas after passing through the four-way valve, wherein the three paths of carrier gas are respectively a first path of carrier gas connected with the 3 rd interface of the ten-way valve, a second path of carrier gas connected with the 7 th interface of the ten-way valve and a third path of carrier gas connected with the 3 rd interface of the six-way valve;
in the item sulfur separation unit, an inlet of an item sulfur chromatographic column is connected with a 2 nd interface of the ten-way valve, and an outlet is directly connected with a first flame photometric detector;
in the total sulfur separation unit, the 6 th interface of the ten-way valve is connected with the 6 th interface of the six-way valve, the two ends of the total sulfur analysis chromatographic column are respectively connected with the 1 st interface and the 4 th interface of the six-way valve, and the 2 nd interface and the 5 th interface of the six-way valve are connected with the second flame photometric detector through a three-way interface.
2. The analysis system for total sulfur and fractional sulfur in coal gas according to claim 1, wherein: the total sulfur analytical column was a 30m 0.53mm 3um SE-30 capillary column.
3. The analysis system for total sulfur and fractional sulfur in coal gas according to claim 1, wherein: the fractional sulfur chromatography column was a 50m 0.53mm 3um SE-30 capillary chromatography column.
4. The analysis system for total sulfur and fractional sulfur in coal gas according to claim 1, wherein: and a passivation treatment layer is arranged on the inner wall of the pipeline.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202023107415.9U CN214011146U (en) | 2020-12-22 | 2020-12-22 | Analysis system for total sulfur and subentry sulfur in coal gas |
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| CN202023107415.9U CN214011146U (en) | 2020-12-22 | 2020-12-22 | Analysis system for total sulfur and subentry sulfur in coal gas |
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