CN111610278A - Method and device for switching and measuring sulfur trioxide in isopropanol solution by ion chromatography valve - Google Patents

Method and device for switching and measuring sulfur trioxide in isopropanol solution by ion chromatography valve Download PDF

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Publication number
CN111610278A
CN111610278A CN202010549649.4A CN202010549649A CN111610278A CN 111610278 A CN111610278 A CN 111610278A CN 202010549649 A CN202010549649 A CN 202010549649A CN 111610278 A CN111610278 A CN 111610278A
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way valve
point
column
communicated
pump
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张勤
叶明立
刘春红
童小忠
祁志福
张国鑫
邹正伟
张雨婷
施益品
竺赛威
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Zhejiang Energy Group Research Institute Co Ltd
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Zhejiang Energy Group Research Institute Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N30/08—Preparation using an enricher
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/16—Injection
    • G01N30/20—Injection using a sampling valve
    • G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports

Abstract

The invention relates to a device for switching and measuring sulfur trioxide in an isopropanol solution by an ion chromatographic valve, which comprises a first pump, a second pump, a six-way valve I, a six-way valve II, a protective column, an analytical column, an inhibitor, a conductivity detector, an enrichment column, a trapping column, a quantitative ring, a sample injector and a waste liquid bottle; the second pump is connected to a point C of the first six-way valve through the trapping column, the quantitative ring is connected with a point D and a point A of the first six-way valve, the sample injector is connected to a point E of the first six-way valve, and a point F of the first six-way valve is connected to the waste liquid bottle; the first pump is connected to a point C of the six-way valve II, the enrichment column is connected with a point D and a point A of the six-way valve II, and a point E of the six-way valve II is connected to the waste liquid bottle. The invention has the beneficial effects that: the invention adoptsAbsorbing SO in the sample with 80% isopropanol3Conversion to SO4 2‑To inhibit SO2Dissolution and oxidation in solution, thereby reducing SO2On-line pretreatment method of valve switching can remove SO caused by high-concentration isopropanol on the influence of measurement result4 2‑The influence of (2) is measured.

Description

Method and device for switching and measuring sulfur trioxide in isopropanol solution by ion chromatography valve
Technical Field
The invention relates to a device for detecting sulfur trioxide in flue gas, in particular to a method and a device for switching and measuring sulfur trioxide in an isopropanol solution by using an ion chromatography valve.
Background
The tail exhaust gas of the thermal power plant contains smoke dust and SOx、NOxMercury and compounds thereof. The sulfur oxides in the flue gas are mostly sulfur dioxide (SO)2) In which there is a part of SO2Will oxidize into SO3。SO3Is a substance which is very easy to absorb moisture, sulfuric acid mist formed after moisture absorption can be adhered to boiler equipment and downstream equipment of SCR system to form H2SO4Also can be mixed with NH3Reaction to produce ammonium bisulfate [ (NH)4)HSO4]And ammonium sulfate [ (NH)4)2SO4]Can cause corrosion of pipelines, equipment and chimneys, generates opaque phenomenon of smoke discharge, and SO3When the air is discharged into the atmosphere, the air can not only cause the generation of haze weather and acid rain, but also cause great harm to human bodies, and corresponding countermeasures and measures are taken for researchMeasure, grasp SO3Accurate detection is particularly necessary. The relevant documents are as follows:
Srivastava R K,Miller C A,Erickson C,et al.Emissions of SulfurTrioxide from Coal-Fired Power Plants[J].Journal of the Air&Waste ManagementAssociation,2004,54(6):750-762.
SO in building clean coal burning process3Experimental study of Generation [ J]Energy engineering, 2009, (6):46-49.
Plum blossom King, plum blossom military, a turned flue, etc. the generation of SO3 in the flue gas of coal burning and the treatment thereof [ J ] chemical equipment technology, 2018,039(001):1-6.
Liu Tao, Zhang Dun, ion chromatography measures sulfur trioxide [ J ] in flue gas of coal-fired power plants environmental impact evaluation 2016,38(5):76-78.
At present, SO in flue gas is measured3The method mainly comprises a precipitation titration method, a spectrum method, a thorium reagent titration method, an ion chromatography method and the like. Xiaoyu pavilion and the like adopt a precipitation titration method to determine SO in flue gas of coal-fired power plants3Has certain limitation that high-concentration SO exists in the flue gas2Under the action of high temperature and in the presence of water vapor, the catalyst is very easy to oxidize and absorb water to generate H2SO3SO that the measurement result is higher and SO in the flue gas3The concentration is low, and a small measurement error in the process of titration by the precipitation method brings a large relative error. King gold sleeve et al adopt ultraviolet absorption spectrum to monitor SO of coal-fired power plant on line3Transmitting ultraviolet light beam with specific spectrum to penetrate through the smoke pool to be detected, and detecting according to different light intensity absorption degrees of the smoke, SO3With SO2The absorption spectra of (A) have a certain overlap, the actual operation is due to SO2The concentration is far higher than SO3Concentration of and SO3The sulfuric acid is combined with water molecules and cannot be detected, and the method has great influence on the detection result. Huangmeifen et al respectively absorb and simultaneously determine SO in flue gas by one-time absorption by adopting a hydrogen peroxide-barium chloride-thorium reagent method and an 80% isopropanol-barium chloride-thorium reagent method2And SO3The concentration, not only the time consumption for titration but also errors exist, the dosage of the indicator and the acidity of the solution can influence the detection result, and the accuracy of the detection resultGreatly reducing the cost. The relevant documents are as follows:
xiaoyu pavilion, Jiaman, Xuli, and the like, an analysis method of sulfur trioxide and sulfuric acid fog drops in flue gas [ J ] environmental science, 2012,25(5):43-48.
Wangjin sleeve, coal-fired power plant sulfur trioxide emission on-line monitoring technology research [ D ]. North China university of electric Power, 2019.
Study on measuring method of sulfur dioxide and sulfur trioxide in Huangmeifen, Shenshilin, flue gas [ J ] physicochemical examination, chemistry Manual, 1994,030(003) 10-12.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method and a device for measuring sulfur trioxide in an isopropanol solution by switching an ion chromatographic valve.
The device for switching and measuring sulfur trioxide in an isopropanol solution by using the ion chromatographic valve comprises a first pump, a second pump, a six-way valve I, a six-way valve II, a protective column, an analytical column, an inhibitor, a conductivity detector, an enrichment column, a trapping column, a quantitative ring, a sample injector and a waste liquid bottle; the second pump is connected to a point C of the first six-way valve through the trapping column, the quantitative ring is connected with a point D and a point A of the first six-way valve, the sample injector is connected to a point E of the first six-way valve, and a point F of the first six-way valve is connected to the waste liquid bottle; the first pump is connected to a point C of the six-way valve II, the enrichment column is connected with a point D and a point A of the six-way valve II, a point E of the six-way valve II is connected to the waste liquid bottle, a point B of the six-way valve II is connected to the protection column, and the protection column, the analysis column, the suppressor and the conductivity detector are sequentially connected to the waste liquid bottle; point B of the first six-way valve is connected to point F of the second six-way valve.
Preferably, the method comprises the following steps: when the first six-way valve is in a Load state, the point C of the first six-way valve is communicated with the point B, the point E of the first six-way valve is communicated with the point D, and the point A of the first six-way valve is communicated with the point F; when the first six-way valve is in the Inject state, the point C of the first six-way valve is communicated with the point D, the point A of the first six-way valve is communicated with the point B, and the point E of the first six-way valve is communicated with the point F; when the six-way valve II is in a Load state, the point C of the six-way valve II is communicated with the point B, the point F of the six-way valve II is communicated with the point A, and the point D of the six-way valve II is communicated with the point E; and when the six-way valve II is in the Inject state, the point C of the six-way valve II is communicated with the point D, the point A of the six-way valve II is communicated with the point B, and the point F of the six-way valve II is communicated with the point E.
The analysis and detection method of the device for switching and measuring the sulfur trioxide in the isopropanol solution by using the ion chromatographic valve comprises the following steps:
s1, sample loading
The first six-way valve and the second six-way valve are both kept in a Load state, a sample to be detected after isopropanol pretreatment is injected into a quantitative ring connected to the first six-way valve through a sample injector, the injected redundant sample enters a waste liquid bottle, a second pump is started, deionized water is injected into the first six-way valve through a trapping column by the second pump, flows through the enrichment column and then enters the waste liquid bottle; KOH leacheate is injected into the six-way valve II by the first pump, flows through the protective column, the analytical column, the suppressor and the conductivity detector in sequence to flush the chromatographic analysis system, and then enters a waste liquid bottle;
s2 enrichment
After the sample introduction is finished, the first six-way valve is switched to the Inject state, the second six-way valve is still in the Load state, deionized water in a second pump transfers the sample from the quantitative ring to the enrichment column, and SO is generated in the transfer process4 2-Is reserved by the enriching column, and the isopropanol flows into a waste liquid bottle along with the deionized water;
s3, analysis
After enriching for a period of time, switching the six-way valve to enable the first six-way valve to be in a Load state and the second six-way valve to be in an Inject state, and taking KOH in the first pump as a mobile phase to enrich SO in the column4 2-Separating by analytical column, and detecting by conductivity detector.
The invention has the beneficial effects that: the invention adopts 80 percent isopropanol absorption liquid to absorb SO in a sample3Conversion to SO4 2-To inhibit SO2Dissolution and oxidation in solution, thereby reducing SO2On-line pretreatment method of valve switching can remove SO caused by high-concentration isopropanol on the influence of measurement result4 2-The method has the advantages of simple operation, high sensitivity, low detection limit and the like, and is suitable for detecting the content of sulfur trioxide in the pollutants discharged in the thermal power industry.
Drawings
FIG. 1 is a schematic view of an ion chromatography apparatus in a loaded state;
FIG. 2 is a schematic view of an ion chromatography apparatus during sample enrichment;
FIG. 3 is a schematic view of an ion chromatography apparatus for sample analysis.
Description of reference numerals: the device comprises a first pump 1, a second pump 2, a six-way valve I3, a six-way valve II 4, a protection column 5, an analytical column 6, a suppressor 7, a conductivity detector 8, an enrichment column 9, a trapping column 10, a quantitative ring 11, a sample injector 12 and a waste liquid bottle 13.
Detailed Description
The present invention will be further described with reference to the following examples. The following examples are set forth merely to aid in the understanding of the invention. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Example one
The embodiment of the application provides a device for measuring sulfur trioxide in isopropanol solution by switching ion chromatographic valve, and SO in sample pretreated by detecting 80% isopropanol by using ion chromatographic valve switching system4 2-In an amount to realize the control of SO3And (5) detecting the content. The device comprises: the device comprises a first pump 1, a second pump 2, a six-way valve I3, a six-way valve II 4, a protection column 5, an analytical column 6, a suppressor 7, a conductivity detector 8, an enrichment column 9, a trapping column 10, a quantitative ring 11, a sample injector 12 and a waste liquid bottle 13. The second pump 2 is connected to a point C of the first six-way valve 3 through the trapping column 10, the quantitative ring 11 is connected with a point D and a point A of the first six-way valve 3, the sample injector 12 is connected to a point E of the first six-way valve 3, and a point F of the first six-way valve 3 is connected to the waste liquid bottle 13; the first pump 1 is connected to a point C of a six-way valve II 4, the enrichment column 9 is connected with a point D and a point A of the six-way valve II 4, a point E of the six-way valve II 4 is connected to a waste liquid bottle 13, a point B of the six-way valve II 4 is connected to a protection column 5, and the protection column 5, the analysis column 6, the suppressor 7 and the conductivity detector 8 of the chromatographic analysis system are sequentially connected to the waste liquid bottle 13; point B of the first six-way valve 3 is connected to point F of the second six-way valve 4.
Example two
On the basis of the first embodiment, the second embodiment of the present application provides a method for determining sulfur trioxide in an isopropanol solution by switching an ion chromatography valve: SO in the sample is absorbed by 80 percent isopropanol absorption liquid3Conversion to SO4 2-Removal of SO from high concentration isopropyl alcohol using valve-switched on-line pretreatment4 2-The influence of (2) is measured. Starting a second pump 2, injecting a pretreated sample to be detected into a quantitative ring 11, connecting a trapping column 10 between the second pump 2 and a six-way valve I3 to prevent anions in water from influencing a final result, switching the six-way valve I3, transferring the sample from the quantitative ring 11 to an enrichment column 9 by using deionized water, and transferring SO (sulfur oxide) in the process of transferring4 2-Is retained by the enrichment column 9 while the isopropanol flows with the deionized water into the waste bottle 13. Then the six-way valve II 4 is switched, KOH is used as a mobile phase to enrich SO in the column 94 2-The separation is carried out by an analytical column 6 and then the detection is carried out in a detection pool. Detected SO4 2-The content is SO3The method comprises the following specific steps:
using an instrument: an ion chromatograph; ion Pac AG15 anion protection column (4mm × 50mm), Ion Pac AS15 anion analysis column (4mm × 250mm), AERS-500(4mm) anion suppressor, Ion Pac UTAC-ULP1 anion trapping column (5mm × 23mm), Ion Pac TAC-ULP1 anion enrichment column (5mm × 23mm), KOH leaching solution generator and CR-CTC continuous automatic regeneration trapping column, a peristaltic pump, quantitative ring (6 μ L), sample injector 12, waste liquid bottle 13.
Analytical procedure
a. Sample loading
The first six-way valve 3 and the second six-way valve 4 are both kept in a Load state; when the six-way valve I3 is in a Load state, the point C of the six-way valve I3 is communicated with the point B, the point E of the six-way valve I3 is communicated with the point D, and the point A of the six-way valve I3 is communicated with the point F; when the six-way valve II 4 is in the Load state, the point C of the six-way valve II 4 is communicated with the point B, the point F of the six-way valve II 4 is communicated with the point A, and the point D of the six-way valve II 4 is communicated with the point E; injecting a sample to be detected, which is pretreated by 80% isopropanol, into a quantitative ring 11 connected to a first six-way valve 3 through a sample injector 12, enabling the injected redundant sample to enter a waste liquid bottle 13, starting a second pump 2, injecting deionized water into the first six-way valve 3 through a trapping column 10 by the second pump 2, flowing through an enrichment column 9, and then entering the waste liquid bottle 13; the KOH leacheate is injected into the six-way valve two 4 by the first pump 1, flows through the protective column 5, the analytical column 6, the suppressor 7 and the conductivity detector 8 in sequence to flush the chromatographic analysis system, and then enters the waste liquid bottle 13.
b. Enrichment of
After the sample introduction is finished, switching the first six-way valve 3 to an Inject state, and keeping the second six-way valve 4 in a Load state; when the first six-way valve 3 is in the Inject state, the point C of the first six-way valve 3 is communicated with the point D, the point A of the first six-way valve 3 is communicated with the point B, and the point E of the first six-way valve 3 is communicated with the point F; when the six-way valve II 4 is in the Load state, the point C of the six-way valve II 4 is communicated with the point B, the point F of the six-way valve II 4 is communicated with the point A, and the point D of the six-way valve II 4 is communicated with the point E; deionized water in the second pump 2 transfers the sample from the dosing ring 11 to the enrichment column 9, SO being transferred during the transfer process4 2-Is retained by the enrichment column 9 while the isopropanol flows with the deionized water into the waste bottle 13.
c. Analysis of
After enrichment is carried out for 0.6min, the six-way valve is switched to enable the first six-way valve 3 to be in a Load state and the second six-way valve 4 to be in an project state; when the six-way valve I3 is in a Load state, the point C of the six-way valve I3 is communicated with the point B, the point E of the six-way valve I3 is communicated with the point D, and the point A of the six-way valve I3 is communicated with the point F; when the six-way valve II 4 is in the Inject state, the point C of the six-way valve II 4 is communicated with the point D, the point A of the six-way valve II 4 is communicated with the point B, and the point F of the six-way valve II 4 is communicated with the point E; KOH in the first pump 1 is used as a mobile phase to enrich SO in the column 94 2-The separation is carried out by the analytical column 6 and then the detection is carried out by the conductivity detector 8.

Claims (3)

1. The utility model provides a sulfur trioxide's device in switching survey isopropyl alcohol solution of ion chromatography valve which characterized in that: comprises a first pump (1), a second pump (2), a six-way valve I (3), a six-way valve II (4), a protective column (5), an analytical column (6), a suppressor (7), a conductivity detector (8), an enrichment column (9), a trapping column (10), a quantitative ring (11), a sample injector (12) and a waste liquid bottle (13); the second pump (2) is connected to a point C of the first six-way valve (3) through the trapping column (10), the quantitative ring (11) is connected with a point D and a point A of the first six-way valve (3), the sample injector (12) is connected to a point E of the first six-way valve (3), and a point F of the first six-way valve (3) is connected to the waste liquid bottle (13); the device comprises a six-way valve II, a first pump (1), an enrichment column (9), a waste liquid bottle (13), a protection column (5), an analysis column (6), a suppressor (7) and a conductivity detector (8), wherein the first pump (1) is connected to a point C of the six-way valve II (4), the enrichment column (9) is connected with a point D and a point A of the six-way valve II (4), a point E of the six-way valve II (4) is connected to the waste liquid bottle (13), a point B of the six-way valve II (4) is connected to the protection column (5); point B of the first six-way valve (3) is connected to point F of the second six-way valve (4).
2. The device for switching and measuring sulfur trioxide in isopropanol solution according to claim 1, characterized in that: when the first six-way valve (3) is in the Load state, the point C of the first six-way valve (3) is communicated with the point B, the point E of the first six-way valve (3) is communicated with the point D, and the point A of the first six-way valve (3) is communicated with the point F; when the first six-way valve (3) is in the Inject state, the point C of the first six-way valve (3) is communicated with the point D, the point A of the first six-way valve (3) is communicated with the point B, and the point E of the first six-way valve (3) is communicated with the point F; when the six-way valve II (4) is in the Load state, the point C of the six-way valve II (4) is communicated with the point B, the point F of the six-way valve II (4) is communicated with the point A, and the point D of the six-way valve II (4) is communicated with the point E; when the six-way valve II (4) is in the Inject state, the point C of the six-way valve II (4) is communicated with the point D, the point A of the six-way valve II (4) is communicated with the point B, and the point F of the six-way valve II (4) is communicated with the point E.
3. The analytical detection method for the device for measuring sulfur trioxide in isopropanol solution by switching the ion chromatographic valve as claimed in claim 1, is characterized by comprising the following steps:
s1, sample loading
The six-way valve I (3) and the six-way valve II (4) are both kept in a Load state, a sample to be detected after isopropanol pretreatment is injected into a quantitative ring (11) connected to the six-way valve I (3) through a sample injector (12), the injected redundant sample enters a waste liquid bottle (13), a second pump (2) is started, deionized water is injected into the six-way valve I (3) through a trapping column (10) by the second pump (2), flows through an enrichment column (9), and then enters the waste liquid bottle (13); KOH leacheate is injected into a six-way valve II (4) by a first pump (1), flows through a protection column (5), an analysis column (6), a suppressor (7) and a conductivity detector (8) in sequence to wash a chromatographic analysis system, and then enters a waste liquid bottle (13);
s2 enrichment
After the sample introduction is finished, the first six-way valve (3) is switched to the Inject state, the second six-way valve (4) is still in the Load state, deionized water in the second pump (2) transfers the sample from the quantitative ring (11) to the enrichment column (9), and SO is generated in the transfer process4 2-Is retained by the enrichment column (9), and the isopropanol flows into a waste liquid bottle (13) along with the deionized water;
s3, analysis
After enriching for a period of time, switching the six-way valve to enable the first six-way valve (3) to be in a Load state, enabling the second six-way valve (4) to be in an Inject state, and enabling KOH in the first pump (1) to be used as a mobile phase to enrich SO in the column (9)4 2-The separation is carried out by an analytical column (6) and then the detection is carried out by a conductivity detector (8).
CN202010549649.4A 2020-06-16 2020-06-16 Method and device for switching and measuring sulfur trioxide in isopropanol solution by ion chromatography valve Pending CN111610278A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114324635A (en) * 2021-12-20 2022-04-12 杭州医学院 Method for measuring bromate in drinking water by using ion chromatography online matrix elimination system

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114324635A (en) * 2021-12-20 2022-04-12 杭州医学院 Method for measuring bromate in drinking water by using ion chromatography online matrix elimination system
CN114324635B (en) * 2021-12-20 2024-04-16 杭州医学院 Method for measuring bromate in drinking water by utilizing ion chromatography on-line matrix elimination system

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