CN212722751U - NO2 conversion system - Google Patents

NO2 conversion system Download PDF

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CN212722751U
CN212722751U CN202020730085.XU CN202020730085U CN212722751U CN 212722751 U CN212722751 U CN 212722751U CN 202020730085 U CN202020730085 U CN 202020730085U CN 212722751 U CN212722751 U CN 212722751U
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electromagnetic valve
way electromagnetic
gas
flowmeter
conversion system
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荀其宁
张文申
宋磊
辛宗伟
胡国星
许峰
侯倩倩
李胜凯
朱天一
冀克俭
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Shandong Non Metallic Material Research Institute
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Shandong Non Metallic Material Research Institute
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Abstract

The utility model discloses a NO2A transformation system belongs to the technical field of analysis and detection. NO in the utility model2The conversion system comprises a flowmeter I, a sampling bottle, a mixing chamber, a gas washing bottle, an absorption unit, a flowmeter II and a flowmeter III; comprises a gas sampling system, a pipeline purging system and a conversion system, realizes automatic operation through a comprehensive control platform, and has the functions of sampling and fast conversionThe method has the advantages that the method has an integrated function, is suitable for the rapid conversion of nitrogen dioxide in gas, utilizes an ion chromatography-mass spectrometry combination method with high sensitivity and high accuracy on inorganic anions as a testing means, completely converts the nitrogen dioxide in the gas into nitrate ions for testing, and converts the measured concentration of the nitrate ions into the content of the nitrogen dioxide in the gas.

Description

NO (nitric oxide)2Conversion system
Technical Field
The utility model belongs to the technical field of the analysis detects, concretely relates to NO2A transformation system.
Background
Nitrogen dioxide is a red brown gas, is very soluble in water, has strong stimulation effect on eyes, nasal cavities, respiratory tracts and lungs, and is combined with water to generate nitric acid which corrodes and destroys lung tissues and can cause lung edema. Industrial and domestic waste gases (e.g. NO)2、SO2、H2S, CO, etc.) and the environmental pollution problems (such as haze, acid rain, greenhouse effect, etc.) faced by people are also increasing. Therefore, effective monitoring and management of the emission of the polluted gas become an indispensable treatment means at present. NO gas is a typical pollution gas in industrial waste gas and domestic waste gas, has high chemical activity and strong corrosivity, can react with moisture or hydrocarbon in the air, is a main source for forming secondary pollutants such as acid rain, photochemical smog, haze and the like, and seriously threatens the health of people and living environment where people live.
At present, the content of nitrogen dioxide in gas is determined by adopting a naphthyl ethylenediamine hydrochloride spectrophotometry (Saltzman method). The principle of the method is that anhydrous acetic acid, sulfanilic acid and naphthyl ethylenediamine hydrochloride are prepared into absorption liquid for sampling, nitrogen dioxide gas is absorbed and converted into nitrous acid and nitric acid, the nitrous acid and the sulfanilic acid are subjected to diazotization reaction in the presence of the anhydrous acetic acid, then the diazotization reaction is coupled with the naphthyl ethylenediamine hydrochloride to generate rose-red azo dye, the color depth of the azo dye is in direct proportion to the concentration of the nitrogen dioxide in a gas sample, and a spectrophotometer is adopted to measure the absorbance at the wavelength of 540-545 nm, so that the content of the nitrogen dioxide in the gas is obtained. The method has the advantages of long and time-consuming operation steps, slow reaction process, easy deterioration of the aminobenzenesulfonic acid by the absorption liquid, and easy interference of factors such as environmental temperature, reaction time, ozone in air and the like on the measurement result, so that the repeatability and the accuracy of the test result are low.
The ion chromatography-mass spectrometry is a high-sensitivity test method for detecting anions and cations in water by installing a mass spectrometry detector behind an ion exchange resin column. The method has good selectivity to inorganic anions, high accuracy and sensitivity, and can avoid the interference of environmental factors such as reaction temperature, reaction time and the like on the detection result. At present, the method can be used for measuring nitrate ions in water, and the method for measuring the content of nitrogen dioxide in gas is not reported.
SUMMERY OF THE UTILITY MODEL
Aiming at NO in the prior art2The problems of long operation steps for gas detection, slow reaction process, easy interference on test results and the like are solved, the utility model discloses a NO2Conversion system, the utility model discloses gas conversion system simple structure realizes automatic operation through integrated control platform, has sample and quick conversion integration function, is applicable to the quick conversion of nitrogen dioxide in the gas. The method uses an ion chromatography-mass spectrometry combination method with high sensitivity and high accuracy on inorganic anions as a test means, completely converts nitrogen dioxide in the gas into nitrate ions for testing, and converts the measured concentration of the nitrate ions into the content of the nitrogen dioxide in the gas.
The utility model discloses a following technical scheme realizes:
NO (nitric oxide)2The conversion system is characterized by comprising a flowmeter I, a sampling bottle, a mixing chamber, a gas washing bottle, an absorption bottle, a flowmeter II and a flowmeter III;
the inlet of the flowmeter I is connected with the outlet of the pressure reducing valve I, the inlet of the pressure reducing valve I is communicated with a gas sample, and the outlet of the flowmeter I is connected with the inlet of the sampling bottle through the one-way electromagnetic valve I and the three-way electromagnetic valve I; the outlet of the sampling bottle is connected with the inlet of the mixing chamber through a three-way electromagnetic valve II, the outlet of the mixing chamber is connected with the gas washing bottle through a three-way electromagnetic valve III and a one-way electromagnetic valve II, and is connected with the absorption unit through a one-way electromagnetic valve III;
the outlet of the pressure reducing valve II is respectively connected with a flowmeter III and a flowmeter II through a three-way electromagnetic valve IV, and the inlet of the pressure reducing valve II is communicated with carrier gas; the outlet of the flowmeter III is connected with a sampling bottle through a one-way electromagnetic valve V and a three-way electromagnetic valve I; the outlet of the flowmeter II is connected with the sampling bottle through a one-way electromagnetic valve IV and a three-way electromagnetic valve II.
Further, said NO2The conversion system comprises a gas sampling system, a pipeline purging system and a conversion system.
Furthermore, the gas sampling system, the pipeline purging system and the conversion system are automatically controlled by the comprehensive control platform.
Furthermore, the flowmeter I, the flowmeter II and the flowmeter III are differential pressure type mass flow controllers.
Furthermore, the sampling bottle is made of an inner polished stainless steel material, and the volume of the sampling bottle is 100-500 mL; the volume of the gas washing bottle is 100-500 mL.
Furthermore, the mixing chamber adopts the design of a return type static gas mixing scheme and is made of an inner polishing stainless steel material.
Furthermore, the absorption bottles are n U-shaped porous glass plate absorption tubes which are connected in series and have the volume of 10-50 mL, and n is more than or equal to 1 and less than or equal to 5.
Advantageous effects
The utility model relates to a nitrogen dioxide turns into conversion system of nitrate ion fast in gas, simple structure realizes automatic operation through the integrated control platform, has sample and quick conversion integration function, is applicable to the absorption and the conversion of gas sample, the quick conversion of nitrogen dioxide in the specially adapted gas.
Drawings
FIG. 1 is NO2A schematic representation of a conversion system;
FIG. 2 is a flow diagram of a gas sampling system;
FIG. 3 is a flow diagram of a line purge system;
FIG. 4 is a flow chart of the conversion of nitrogen dioxide to nitrate ions in a gas sample;
wherein: 1. the device comprises a pressure reducing valve I, a flow meter I, a single-way electromagnetic valve I, a three-way electromagnetic valve I, a sampling bottle 5, a comprehensive control platform 6, a three-way electromagnetic valve II, a mixing chamber 8, a three-way electromagnetic valve III, a single-way electromagnetic valve II, a gas washing bottle 11, an absorption unit 12, a single-way electromagnetic valve III, a single-way electromagnetic valve 14, a single-way electromagnetic valve IV, a flow meter II, a flow meter 16, a single-way electromagnetic valve V, a flow meter III 18, a three-way electromagnetic valve IV, a flow meter.
Detailed Description
In order to make the technical solution of the present invention better understood, the following clear and complete description of the technical solution of the present invention shall be included in the scope of the present application, based on the embodiments in the present application, and other similar embodiments obtained by those of ordinary skill in the art without creative efforts.
NO in the utility model2The transformation system is shown in FIG. 1: the device comprises a flowmeter I2, a sampling bottle 5, a mixing chamber 8, a gas washing bottle 11, an absorption unit 12, a flowmeter II 15 and a flowmeter III 17;
the inlet of the flowmeter I2 is connected with the outlet of the pressure reducing valve I1, and the outlet of the flowmeter I2 is connected with the inlet of the sampling bottle 5 through a one-way electromagnetic valve I3 and a three-way electromagnetic valve I4; the outlet of the sampling bottle 5 is connected with the inlet of the mixing chamber 8 through a three-way electromagnetic valve II 7, the outlet of the mixing chamber 8 is connected with a gas washing bottle 11 through a three-way electromagnetic valve III 9 and a one-way electromagnetic valve II 10, and is connected with an absorption unit 12 through a one-way electromagnetic valve III 13;
the outlet of the pressure reducing valve II 19 is respectively connected with a flowmeter III 17 and a flowmeter II 15 through a three-way electromagnetic valve IV 18, and the inlet of the pressure reducing valve II 19 is communicated with carrier gas; the outlet of the flowmeter III 17 is connected with the sampling bottle 5 through a one-way electromagnetic valve V16 and a three-way electromagnetic valve I4; the outlet of the flowmeter II 15 is connected with the sampling bottle 5 through a one-way electromagnetic valve IV 14 and a three-way electromagnetic valve II 7; the whole system and the components adopt internal polishing treatment.
The conversion system comprises a gas sampling system, a pipeline purging system and a conversion system and is automatically controlled by the comprehensive control platform 6.
Example 1
NO in example 12The transformation system is shown in figure 1, the sampling bottle 5 is a 150mL sampling bottle with a fixed volume, the absorption unit 12 is 3 series-connected 25mL porous glass plate absorption tubes, and the gas washing bottle 11 is a 500mL gas washing bottle; when in use, 20ml of potassium hydroxide absorption liquid with the concentration of 0.2mol/L is injected into each porous glass plate absorption tube of the absorption unit 12, and 400ml of potassium hydroxide solution with the concentration of 1mol/L is injected into the gas washing bottle 11.
A method for collecting gas (nitrogen dioxide nominal content: 200 mu mol/mol) sample in aluminum alloy gas cylinder and NO of the sample2The transformation and detection method is as follows:
(1) firstly, opening a gas sample to be tested (gas in an aluminum alloy gas cylinder), a pressure reducing valve I1, a one-way electromagnetic valve 3, a three-way electromagnetic valve I4, a three-way electromagnetic valve II 7, a three-way electromagnetic valve III 9 and a one-way electromagnetic valve II 10 (the gas sample sampling process is shown by an arrow in a figure 2), controlling the outlet pressure of the pressure reducing valve I to be 0.1Mpa, controlling a passing gas flowmeter I2 to be 100mL/min, carrying out gas replacement for 5min, and closing the gas sample to be tested, the pressure reducing valve I1, the one-way electromagnetic valve I3, the three-way electromagnetic valve I4, the three-way electromagnetic valve II 7, the three-way electromagnetic valve;
(2) after sampling is finished, opening carrier gas (high-purity oxygen), sequentially opening a pressure reducing valve II 19, a one-way electromagnetic valve IV 14, a three-way electromagnetic valve II 7, a three-way electromagnetic valve II 9 and a one-way electromagnetic valve II 10, controlling the outlet pressure of the pressure reducing valve II 19 to be 0.1Mpa, purging the pipeline for 5min by the gas flow of a flow meter II 15, and finishing purging the pipeline after sampling (the pipeline purging flow is shown by an arrow in figure 3);
(3) after the pipeline purging is finished, closing the single-way electromagnetic valve II 10, opening the single-way electromagnetic valve III 13, and then sequentially opening the single-way electromagnetic valve V16, the three-way electromagnetic valve I4 and the three-way electromagnetic valve II 9 to perform absorption and conversion of nitrogen dioxide in the gas sample (the absorption and conversion process is shown by an arrow in figure 4); the outlet pressure of the pressure reducing valve II is controlled to be 0.1Mpa in the absorption process, the flow of the gas flowmeter III 17 is controlled to be 100mL/min, and the absorption is carried out for 10 min;
(4) ion chromatography-mass spectrometry detection:
a) constant volume of absorption liquid
Combining the absorption liquid in the 3 porous glass plate absorption tubes after the gas is treated by the treatment system, and fixing the volume to a 100mL volumetric flask by using distilled water;
b) preparation of series standard solutions of nitrate ions in water
Taking 6 100mL volumetric flasks, adding 0.1mL, 0.5mL, 1mL, 3mL, 5mL and 7mL 100mg/L nitrate ion standard solution in water respectively, adding pure water for constant volume and shaking up to obtain nitrate series standard solutions in water with the concentrations of 0.1, 0.5, 1.0, 3.0, 5.0 and 7.0mg/L respectively.
c) Detecting: injecting 25 mu L of nitrate series standard solution into an ion chromatography-mass spectrometer in an automatic sample injection mode, drawing a standard curve according to peak area and content (mg/L) of each corresponding nitrate series standard solution, measuring the sample solution under the same condition, and obtaining the content (mg/L) of nitrate ions in the sample solution according to the standard curve; calculating the content of nitrogen dioxide in the gas according to the formula (1);
Figure DEST_PATH_GDA0002898284760000041
in the formula:
Figure DEST_PATH_GDA0002898284760000051
-the content of nitrogen dioxide in the gas, mol/mol;
Figure DEST_PATH_GDA0002898284760000052
measurement of samplesThe content of nitrate ions in the product solution is mg/L;
V1-sample solution volumetric volume, mL;
V0-sampling tube volume, L;
Vm-molar volume at the temperature, pressure at which the gas sample is taken, L/mol.
The ion chromatography-mass spectrometry conditions of the present example were: ion chromatography-mass spectrometer model: ICS5000+ MSQ; a chromatographic column: AS 11-HC; a detector: mass spectrometry detector (ESI source); column temperature: 35 ℃; mobile phase: pure water; flow rate: 0.25 mL/min; sample introduction amount: 25 mu L of the solution;
the nitrogen dioxide content of the gas sample was measured 6 times, the average of the measurements being 202. mu. mol/mol with a relative error of 1%.
Example 2
NO in example 22The conversion system is shown in FIG. 1, the sampling bottle 5 is a 300mL volumetric sampling bottle, the absorption unit 12 is 5 serially connected 15mL porous glass plate absorption tubes, and the gas washing bottle 11 is a 500mL gas washing bottle. When in use, 10ml of potassium hydroxide absorption solution with the concentration of 0.1mol/L is injected into each porous glass plate absorption tube, and 500ml of potassium hydroxide solution with the concentration of 1mol/L is injected into the gas washing bottle 11. The flow meter I2, the flow meter II 15 and the flow meter III 17 are 200mL/min, and other setting conditions are the same as those in the embodiment 1;
collecting gas (nitrogen dioxide nominal content: 100 mu mol/mol) in an aluminum alloy gas cylinder;
NO thereof2The transformation and detection methods were the same as in example 1;
the nitrogen dioxide content of the gas sample was measured 6 times, the average of the measurements was 98.8. mu. mol/mol, and the relative error was-1.2%.
Example 3
NO in example 32The transformation system is shown in FIG. 1, the sampling bottle 5 is a 100mL volumetric sampling bottle, the absorption unit 12 is 2 serially connected 50mL porous glass plate absorption tubes, and the gas washing bottle 11 is a 500mL gas washing bottle. When in use, 40ml of potassium hydroxide absorption solution with the concentration of 0.05mol/L is injected into each porous glass plate absorption tube, and 500ml of potassium hydroxide absorption solution with the concentration of 500ml is injected into the gas washing bottle 111mol/L potassium hydroxide solution; the flow meter I2, the flow meter II 15 and the flow meter III 17 are 150 mL/min;
a method for collecting a gas (nominal content of nitrogen dioxide: 50 mu mol/mol) sample in an aluminum alloy gas cylinder;
the NO2 conversion and detection method are the same as in example 1;
the nitrogen dioxide content of the gas sample was measured 6 times, the average of the measurements being 50.7. mu. mol/mol with a relative error of 1.4%.

Claims (7)

1. NO (nitric oxide)2The conversion system is characterized by comprising a flowmeter I, a sampling bottle, a mixing chamber, a gas washing bottle, an absorption unit, a flowmeter II and a flowmeter III;
the inlet of the flowmeter I is connected with the outlet of the pressure reducing valve I, the inlet of the pressure reducing valve I is communicated with a gas sample, and the outlet of the flowmeter I is connected with the inlet of the sampling bottle through the one-way electromagnetic valve I and the three-way electromagnetic valve I; the outlet of the sampling bottle is connected with the inlet of the mixing chamber through a three-way electromagnetic valve II, the outlet of the mixing chamber is connected with the gas washing bottle through a three-way electromagnetic valve III and a one-way electromagnetic valve II, and is connected with the absorption unit through a one-way electromagnetic valve III;
the flow meter II and the flow meter III are connected with the outlet of the pressure reducing valve II through a three-way electromagnetic valve IV, and the inlet of the pressure reducing valve II is communicated with carrier gas; the outlet of the flowmeter III is connected with a sampling bottle through a one-way electromagnetic valve V and a three-way electromagnetic valve I; the outlet of the flowmeter II is connected with the sampling bottle through a one-way electromagnetic valve IV and a three-way electromagnetic valve II.
2. NO according to claim 12Conversion system, characterized in that said NO2The conversion system comprises a gas sampling system, a pipeline purging system and a conversion system.
3. NO according to claim 22The conversion system is characterized in that the gas sampling system, the pipeline purging system and the conversion system are automatically controlled by a comprehensive control platform.
4. The reforming system according to claim 1, wherein said flow meters I, II, III are differential pressure mass flow controllers.
5. The conversion system of claim 1, wherein the sampling bottle is made of an inner polished stainless steel material and has a volume of 100-500 mL; the volume of the gas washing bottle is 100-500 mL.
6. The reforming system according to claim 1, wherein the mixing chamber is designed using a reentrant static mixing scheme and is made of an inner polished stainless steel material.
7. The conversion system according to claim 1, wherein the absorption units are n series-connected U-shaped porous glass plate absorption tubes with the volume of 10-50 mL, and n is more than or equal to 1 and less than or equal to 5.
CN202020730085.XU 2020-05-07 2020-05-07 NO2 conversion system Active CN212722751U (en)

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