CN111239327A - SO (SO)3Concentration testing method and device thereof - Google Patents
SO (SO)3Concentration testing method and device thereof Download PDFInfo
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- 238000012360 testing method Methods 0.000 title claims abstract description 18
- 238000005070 sampling Methods 0.000 claims abstract description 67
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- ZSLUVFAKFWKJRC-IGMARMGPSA-N 232Th Chemical compound [232Th] ZSLUVFAKFWKJRC-IGMARMGPSA-N 0.000 claims abstract description 14
- 229910052776 Thorium Inorganic materials 0.000 claims abstract description 14
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- 238000004448 titration Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 239000011550 stock solution Substances 0.000 claims description 6
- 239000012496 blank sample Substances 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000002474 experimental method Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 abstract description 19
- 238000000605 extraction Methods 0.000 abstract description 9
- 238000005259 measurement Methods 0.000 abstract description 6
- 238000006477 desulfuration reaction Methods 0.000 abstract description 5
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- 239000003546 flue gas Substances 0.000 description 34
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- AKEJUJNQAAGONA-UHFFFAOYSA-N sulfur trioxide Inorganic materials O=S(=O)=O AKEJUJNQAAGONA-UHFFFAOYSA-N 0.000 description 13
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- KMUONIBRACKNSN-UHFFFAOYSA-N potassium dichromate Chemical compound [K+].[K+].[O-][Cr](=O)(=O)O[Cr]([O-])(=O)=O KMUONIBRACKNSN-UHFFFAOYSA-N 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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Abstract
The application discloses a SO3The concentration testing equipment comprises a sampling gun, wherein one end of the sampling gun is connected with a heating filter, one end of the heating filter is connected with a sampling pipe, a heating connecting pipe and a first thermometer are sequentially arranged on the sampling pipe, and one end of the sampling pipe is connected with a control condensing pipe; the application also discloses an SO3The concentration test method comprises the following steps: s1, vacuumizing for 4-6 minutes before sampling, sampling by an air pump, dissolving in isopropanol solution to obtain sample solution, wherein the sampling volume is more than 0.5m3Cleaning interference is avoided; s2, weighing 0.20g of thorium reagent, and dissolving in 100mL of deionized water to obtain a thorium reagent solution with the mass concentration of 2000 mg/L. The invention has less interference factors when extracting the smoke, stable extraction and strong processing capacity, and the measurement is convenient and quick after extracting the smokeThe method has the advantages of short period and high determination precision, reduces labor cost and time cost of detection, and provides accurate data for subsequent recording and desulfurization detection work.
Description
Technical Field
The invention relates toSO3The technical field of concentration detection, in particular to a SO3A concentration test method and apparatus thereof.
Background
The energy structure of China is mainly coal, and most of sulfur in the coal is SO in the coal combustion process2In the form of small SO in flue gas2Conversion to SO3Typically, there is about 1-2% SO in the furnace2Is oxidized into SO3The toxicity of the compound is the same as that of sulfuric acid, and the compound has strong stimulation and corrosion effects on tissues such as skin, mucosa and the like, and can cause conjunctivitis, edema and corneal opacity to cause blindness; causing respiratory irritation symptoms, dyspnea and pulmonary edema in severe cases; high concentration causes larynx spasm or glottic edema to die, after oral administration, the digestive tract is burned to form ulcer, severe patients may have gastric perforation, peritonitis, larynx spasm and glottic edema, kidney damage, shock, etc., and chronic effects include dental erosion, chronic bronchitis, emphysema and liver cirrhosis, etc.
The energy supply pattern of China mainly based on coal does not change radically in the future for a long time, and due to limited environmental capacity, the atmospheric pollution situation is increasingly severe, disastrous weather such as haze, acid rain and the like frequently occurs, PM2.5 and SO3SO control is imminent in need of pollutant reduction3The emission reduction should also be paid high attention, SO the SO in the flue gas needs to be treated3The concentration is accurately detected, recording and subsequent processing are facilitated, whether the emission reaches the standard is detected, and therefore an SO is provided3The concentration test method and the device thereof solve the problems.
Disclosure of Invention
The present application provides a SO3The concentration testing method and the device thereof solve the problems of low measuring precision, time and labor waste of the traditional detection mode.
The present application provides a SO3Concentration test equipment, including the sampling rifle, the one end of sampling rifle is connected with the heating filter, the one end of heating filter is connected with the sampling pipe, install heating connecting pipe and first temperature on the sampling pipe in proper orderThe meter, sampling pipe one end is connected with the control condenser pipe, the one end of control condenser pipe is connected with accuse temperature circulation water bath device, install circulating water pump in the accuse temperature circulation water bath device, the other end of control condenser pipe is connected on circulating water pump, the other end of control condenser pipe is connected with secondary filter, secondary filter's one end is connected with the droplet separator, the one end of droplet separator is connected with the desicator, the one end of desicator is connected with the aspiration pump through the connecting pipe, install flowmeter, second thermometer and manometer on the connecting pipe in proper order.
Preferably, the flow rate of the pumped air in the control condensation pipe is controlled to be 8L/min.
Preferably, the temperature of the temperature-controlled circulating water bath device is 60-72 ℃.
Preferably, the sampling tube adopts a heating tube or a silicone tube.
Preferably, the temperature of the heating filter is 200-.
SO (SO)3The concentration test method comprises the following steps:
s1, vacuumizing for 4-6 minutes before sampling, sampling by an air pump, dissolving in isopropanol solution to obtain sample solution, wherein the sampling volume is more than 0.5m3Cleaning interference is avoided;
s2, weighing 0.20g of thorium reagent, and dissolving the thorium reagent in 100mL of deionized water to obtain a thorium reagent solution with the mass concentration of 2000 mg/L;
s3, weighing 3.90gBa (ClO)4)2·3H2Dissolving O in 20mL deionized water, transferring into 100mL volumetric flask, and adding the isopropanol solution to constant volume to obtain Ba (ClO)4)2Storing in standard stock solution at 4 deg.C, and sucking Ba (ClO)4)21.00mL of standard stock solution is put in a 100mL volumetric flask, the isopropanol solution is used for fixing the volume to the scale, and standard use solution of 0.001mol/L is prepared;
s4, transferring the sample solution into a conical flask, and adjusting the pH value of the sample solution to 3.5 through a sodium hydroxide solution or a hydrochloric acid solution;
s5, adding 4 drops of the thorium reagent solution into the sample solution, titrating with the standard use solution, indicating that the titration reaches an end point when the liquid in the conical flask is changed from orange to light red, repeating the titration experiment, taking the average value of the volumes of the consumed titration solution for 2 times, determining the standard use liquid volume and the standard state sampling volume by the standard use liquid volume and the laboratory blank sample solution, and completing the determination within 24 hours.
Preferably, the concentration of the HCl solution and the NaOH solution is 0.1 mol/L.
Preferably, the volume concentration of the isopropanol solution is 80%.
According to the technical scheme, the application provides the SO3The concentration test method and the equipment thereof are prepared before sampling, the condenser pipe and the secondary filter are ensured to be clean, the condenser pipe and the secondary filter are cleaned by acetone, the condenser pipe and the secondary filter are dried in the air, if solid foreign matters which are difficult to clean exist on the condenser pipe and the secondary filter, the condenser pipe and the secondary filter can be cleaned by potassium dichromate treatment, a single-point non-constant speed test close to the center of a flue is adopted during detection, when a sampling gun is installed, a flue gas vortex area is avoided, a vertical flue is preferably selected, a place which is not suitable for causing great interference to a gas dynamic field at the position of an elbow, a valve and a section change is selected as a detection position, if the detection position is provided with an interference point, the detection position is a certain distance away from the interference point, if the detection position is positioned at the downstream of the interference point, a straight pipeline with the diameter of 4-7D (equivalent diameter of the flue) is preferably positioned at the interference point, and if, should avoid the place dangerous to the installation of the detecting instrument, detection personnel's operation, the testing instrument is installed on safe, convenient test platform as far as possible, measure the flue gas humidity, flue gas temperature, flue gas velocity of flow, main flue gas parameter of the flue gas pressure, while sampling the flue gas after dry dedusting and desulfurization, the temperature of the heating sampling gun is set at 260 ℃; when the flue gas is sampled after denitration, the temperature of a heating sampling gun is set at 200 ℃, when the humidity of the flue gas is more than 15 percent or the total moisture content of coal as fired in a boiler is more than 10 percent, the temperature of a circulating water bath boiler is preferably controlled at 65-72 ℃, and when the humidity of the flue gas is within 15 percent or the total moisture content of the coal as fired in the boiler is within 15 percentWhen the amount is below 10%, the temperature of the circulating water bath is preferably controlled at 60-65 deg.C, before sampling, the sample is pumped for 4-6 min to avoid cleaning interference, and the sampling volume is more than 0.5m3And after sampling is finished, the condenser pipe and the secondary filter are repeatedly washed and controlled by using 80% isopropanol washing liquor, when the condenser pipe and the sampling gun are connected and controlled by using the silicone tube, the silicone tube needs to be washed, the washing liquor is collected into the volumetric flask, sampling records are made, next group of sampling is carried out, the average value of the volume of the titration liquid is consumed for 2 times, and the determination is finished within 24 hours.
Compared with the prior art, the invention has the beneficial effects that:
1. when the device extracts the flue gas, interference components in the flue gas can be removed, the flue gas cannot cause loss, and the accuracy of measurement and experimental data is improved;
2. the method has the advantages of short experimental period and high measurement precision, and can obtain experimental data in time and provide data for detection and flue gas treatment;
in conclusion, the invention has the advantages of less interference factors during the extraction of the flue gas, stable extraction, strong processing capacity, convenient and quick determination after the extraction of the flue gas, short period and high determination precision, reduces the labor cost and time cost of detection, and provides accurate data for subsequent recording and desulfurization detection work.
Drawings
In order to more clearly illustrate the technical solution of the present application, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious to those skilled in the art that other drawings can be obtained according to the drawings without any creative effort.
FIG. 1 shows a SO according to the present invention3The structure of the concentration test device is shown schematically.
In the figure: the device comprises a sampling gun 1, a heating filter 2, a heating connecting pipe 3, a first thermometer 4, a control condenser 5, a temperature-controlled circulating water bath device 6, a circulating water pump 7, a secondary filter 8, a droplet separator 9, a dryer 10, a flowmeter 11, a second thermometer 12, a pressure gauge 13 and an air pump 14.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings.
See FIG. 1, a SO3The concentration testing equipment comprises a sampling gun 1, wherein one end of the sampling gun 1 is connected with a heating filter 2, the sampling in a high-dust environment reduces the influence on the sampling, the temperature of the heating filter 2 is 200-260 ℃, and the temperature of the heating sampling gun 1 is set at 260 ℃ when the flue gas is sampled after dry dedusting and desulfurization; when flue gas is sampled after denitration, the temperature of a heating sampling gun 1 is set to be 200 ℃, one end of a heating filter 2 is connected with a sampling pipe, the sampling pipe adopts a heating pipe or a silica gel pipe and has certain high-temperature bearing capacity, a heating connecting pipe 3 and a first thermometer 4 are sequentially arranged on the sampling pipe, the internal temperature is kept, whether the temperature measured by the first thermometer 4 reaches a specified value or not is reduced, the error of converting the standard volume is reduced, one end of the sampling pipe is connected with a control condenser pipe 5, preparation is carried out before sampling, the control condenser pipe 5 and a secondary filter 8 are ensured to be clean, when the control condenser pipe 5 and the sampling gun 1 are connected by the silica gel pipe, the silica gel pipe needs to be leached, one end of the control condenser pipe 5 is connected with a temperature control circulating water bath device 6, the temperature of the temperature control circulating water bath device 6 is 60-72 ℃, when the flue gas humidity is more than 15, the temperature of the circulating water bath is preferably controlled to be 65-72 ℃, when the humidity of the flue gas is within 15 percent or the total moisture content of the coal as fired in the boiler is below 10 percent, circulating water bath, the temperature should be controlled at 60-65 ℃, measurement calculation error is reduced, the air exhaust flow speed in the control condenser pipe 5 is controlled at 8L/min, a circulating water pump 7 is installed in the temperature control circulating water bath device 6, the other end of the control condenser pipe 5 is connected to the circulating water pump 7, the other end of the control condenser pipe 5 is connected to a secondary filter 8, the influence of impurities in smoke on measurement is reduced, one end of the secondary filter 8 is connected with a droplet separator 9, one end of the droplet separator 9 is connected with a dryer 10, the content of moisture in the smoke is reduced, the accuracy of sampling volume is improved, one end of the dryer 10 is connected with an air pump 14 through a connecting pipe, and flow is sequentially installed on the connecting pipe.The flowmeter 11 is used for measuring the temperature, the second thermometer 12 is used for measuring the air extraction quantity of the air extraction pump 14 through the flowmeter 11, the air extraction pump 14 is used for controlling the air extraction flow speed in the condensation pipe 5 to be 8L/min, and the sampling flow of the air extraction pump is calculated according to the following formula;
Vpump＝8.0*[273/(273+tcondenser)]*[(Ba+Pcondenser)/Ba]；
in the formula: vpump-the air pump samples the flow (standard condition), L/min;
tcondenser-controlling the water bath temperature of the water bath apparatus at ° c;
Ba-local atmospheric pressure, Pa;
Pcondensercontrolling static pressure Pa of flue gas at an inlet of the condensing pipe;
8.0-control condenser tube flow (working condition), L/min.
SO (SO)3The concentration test method comprises the following steps:
s1, vacuumizing for 4-6 minutes before sampling, sampling by the air pump 14, dissolving in 80% isopropanol solution to obtain sample solution, preparing equal amount of blank sample solution, and comparing with a control group with a sampling volume of more than 0.5m3Cleaning interference is avoided;
s2, weighing 0.20g of thorium reagent, dissolving the thorium reagent in 100mL of deionized water by adopting superior purity to obtain a thorium reagent solution with the mass concentration of 2000mg/L for color development;
s3, weighing 3.90gBa (ClO)4)2·3H2Dissolving O in 20mL deionized water, transferring into 100mL volumetric flask, and adding 80% isopropanol to desired volume to obtain Ba (ClO)4)2Standard stock solution with concentration of 0.10mol/L, cold storage at 4 deg.C for one month at most, absorbing Ba (ClO) when in use4)21.00mL of standard stock solution is put in a 100mL volumetric flask, and the volume is fixed to the scale by 80% isopropanol solution to prepare 0.001mol/L standard use solution;
s4, transferring the sample solution into a conical flask, wherein the conical flask is 250mL, adjusting the pH value of the sample solution to 3.5 by using a sodium hydroxide solution or a hydrochloric acid solution, and the concentrations of an HCl solution and an NaOH solution are both 0.1 mol/L;
s5, adding 4 drops of thorium reagent solution into the sample solution, titrating with standard use solution, when the liquid in the conical flask is changed from orange to light red, indicating that the titration reaches the end point, repeating the titration experiment, taking the average value of the volume of the consumed titration solution for 2 times, determining the standard use liquid volume by the standard use solution volume and the laboratory blank sample solution, and completing the determination within 24 hours;
SO3the mass concentration is calculated according to the following formula:
C＝[0.001*(V-V0)/Vnd]*80.06*1000；
C-Mass concentration of Sulfur trioxide in flue gas, mg/m3；
V-volume of sample measurement Standard use solution, L;
V0-determining a standard use solution volume, L, for a laboratory blank sample solution;
Vnd-conversion to a standard state downsampled volume, m 3;
80.06-molar mass of SO3, g/mol.
According to the technical scheme, preparation is carried out before sampling, the condenser control pipe 5 and the secondary filter 8 are ensured to be clean, the cleaning is carried out by acetone, the drying is carried out in the air, if solid foreign matters which are difficult to clean are arranged on the condenser control pipe and the secondary filter 8, the solid foreign matters can be cleaned after being treated by potassium dichromate, a single-point non-constant speed test close to the center of a flue is adopted during detection, when the sampling gun 1 is installed, a flue gas vortex area is avoided, a vertical flue is preferably selected, a place which has great interference on a gas dynamic field at an elbow, a valve and a section change position is not preferably selected as a detection position, if the detection position is provided with an interference point, the detection position is at a certain distance from the interference point, if the detection position is positioned at the downstream of the interference point, a straight pipeline with the diameter of 4-7D (equivalent diameter of the flue) is preferably positioned at the interference point, if the detection position is positioned at the upstream of the interference point, should avoid the installation of the detecting instrumentThe method comprises the following steps that (1) a testing instrument is arranged on a safe and convenient testing platform as much as possible, main flue gas parameters such as flue gas humidity, flue gas temperature, flue gas flow velocity and flue gas pressure are measured, and when flue gas is sampled after dry dedusting and desulfurization, the temperature of a heating sampling gun 1 is set at 260 ℃; when flue gas is sampled after denitration, the temperature of a heating sampling gun 1 is set at 200 ℃, when the humidity of the flue gas is more than 15 percent or the total moisture content of coal as fired in a boiler is more than 10 percent, the temperature of a circulating water bath kettle is preferably controlled at 65-72 ℃, when the humidity of the flue gas is less than 15 percent or the total moisture content of the coal as fired in the boiler is less than 10 percent, the temperature of the circulating water bath kettle is preferably controlled at 60-65 ℃, before sampling, in order to avoid cleaning interference, the circulating water bath kettle is evacuated for about 4-6 minutes, and the sampling volume is more than 0.5m3And after sampling is finished, the condenser pipe 5 and the secondary filter 8 are repeatedly washed and controlled by using 80% isopropanol washing liquor, when the condenser pipe 5 and the sampling gun 1 are controlled by adopting the connection of the silicone tube, the silicone tube needs to be washed, the washing liquor is collected into a volumetric flask, sampling records are made, next group of sampling is carried out, the average value of the volume of the titration liquid is consumed for 2 times, and the determination is finished within 24 hours.
Other embodiments of the present application will be apparent to those skilled in the art from consideration of the specification and practice of the application disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the application and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope of the disclosure being indicated by the following claims.
It will be understood that the present application is not limited to the precise arrangements described above and shown in the drawings and that various modifications and changes may be made without departing from the scope thereof. The above-described embodiments of the present application do not limit the scope of the present application.
Claims (8)
1. SO (SO)3Concentration test equipment, including sampling rifle (1), its characterized in that: one end of the sampling gun (1) is connectedThere are heating filter (2), the one end of heating filter (2) is connected with the sampling pipe, install heating connecting pipe (3) and first thermometer (4) on the sampling pipe in proper order, sampling pipe one end is connected with control condenser pipe (5), the one end of control condenser pipe (5) is connected with accuse temperature circulation water bath device (6), install circulating water pump (7) in accuse temperature circulation water bath device (6), the other end of control condenser pipe (5) is connected on circulating water pump (7), the other end of control condenser pipe (5) is connected with secondary filter (8), the one end of secondary filter (8) is connected with droplet separator (9), the one end of droplet separator (9) is connected with desicator (10), the one end of desicator (10) is connected with aspiration pump (14) through the connecting pipe, and the connecting pipe is sequentially provided with a flowmeter (11), a second thermometer (12) and a pressure gauge (13).
2. A SO according to claim 13The concentration testing equipment is characterized in that the flow rate of the exhaust air in the condensation pipe (5) is controlled to be 8L/min.
3. A SO according to claim 13The concentration testing equipment is characterized in that the temperature of the temperature-controlled circulating water bath device (6) is 60-72 ℃.
4. A SO according to claim 13The concentration test equipment is characterized in that the sampling pipe adopts a heating pipe or a silicone tube.
5. A SO according to claim 13Concentration test device, characterized in that the temperature of the heated filter (2) is 200-260 ℃.
6. SO (SO)3The concentration test method is characterized by comprising the following steps:
s1, vacuumizing for 4-6 minutes before sampling, sampling by an air pump, dissolving in isopropanol solution to obtain sample solution, wherein the sampling volume is more than 0.5m3Cleaning interference is avoided;
s2, weighing 0.20g of thorium reagent, and dissolving the thorium reagent in 100mL of deionized water to obtain a thorium reagent solution with the mass concentration of 2000 mg/L;
s3, weighing 3.90gBa (ClO)4)2·3H2Dissolving O in 20mL deionized water, transferring into 100mL volumetric flask, and adding the isopropanol solution to constant volume to obtain Ba (ClO)4)2Storing in standard stock solution at 4 deg.C, and sucking Ba (ClO)4)21.00mL of standard stock solution is put in a 100mL volumetric flask, the isopropanol solution is used for fixing the volume to the scale, and standard use solution of 0.001mol/L is prepared;
s4, transferring the sample solution into a conical flask, and adjusting the pH value of the sample solution to 3.5 through a sodium hydroxide solution or a hydrochloric acid solution;
s5, adding 4 drops of the thorium reagent solution into the sample solution, titrating with the standard use solution, indicating that the titration reaches an end point when the liquid in the conical flask is changed from orange to light red, repeating the titration experiment, taking the average value of the volumes of the consumed titration solution for 2 times, determining the standard use liquid volume and the standard state sampling volume by the standard use liquid volume and the laboratory blank sample solution, and completing the determination within 24 hours.
7. A SO according to claim 63The concentration test method is characterized in that the concentrations of the HCl solution and the NaOH solution are both 0.1 mol/L.
8. A SO according to claim 63Concentration test method, characterized in that the volume concentration of the isopropanol solution is 80%.
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