CN108181301B - Sensor device for detecting carbon monoxide gas and analysis method thereof - Google Patents
Sensor device for detecting carbon monoxide gas and analysis method thereof Download PDFInfo
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Abstract
The invention discloses a sensor device (shown in figure 1) capable of detecting carbon monoxide (CO) gas and an analysis method thereof. Introducing a CO sample into a polytetrafluoroethylene tube through a sample introduction needle 1, stably introducing CO into a quartz container 3 by taking air as carrier gas, activating under the irradiation of a 2 ultraviolet lamp, then introducing the CO into the surface of an insulating medium 5 coated with a sensing material along with the carrier gas to perform catalytic oxidation reaction (the insulating medium is sleeved in the quartz tube 4), filtering an optical signal generated by the reaction through a light filter 7, collecting the optical signal by a photomultiplier 6, and realizing the quantitative detection of the CO through conversion treatment and calculation. The invention utilizes the ultraviolet lamp to assist the catalytic oxidation reaction, constructs the catalytic luminescence reaction device based on the non-metal catalyst, and improves the detection sensitivity (the detection limit of CO can reach 6 ppm). The device is simple and environment-friendly, has low energy consumption, and can be used for detecting CO in the environment.
Description
Technical Field
The invention relates to an Ultraviolet lamp (UV) assisted functionalized graphite phase carbon nitride sensing material (marked as g-C)3N4-tri-s-acid) device for detecting carbon monoxide (CO) gas and method for analyzing the same.
Background
In recent years, gas sensing analysis has received much attention due to its unique advantages in real-time monitoring of atmospheric pollutants (especially CO gas), and various optical (Journal of American Chemistry, 2009,131, 15669-15677) and electrical (train-Trends in Analytical Chemistry) based analyses,2006, 25, 937-. Among them, a catalytic luminescence (CTL) sensing analysis method, which is established based on a phenomenon that a gas molecule generates chemiluminescence by oxidation on a surface of a material having a catalytic activity, is receiving attention from researchers in the fields of analytical science and environmental analytical science. The sensor established on the basis of the CTL has the characteristics of simple and convenient operation, wide linear range, strong humidity interference resistance, high sensitivity, good selectivity and the like, so the gas sensor is considered to have good application prospect. However, since CO gas is high in the air atmosphereThe stability is not easy to occur in the catalytic oxidation process, so that the catalytic luminescence sensing system is not easy to detect, and therefore, the catalytic oxidation process of CO gas needs to be promoted by pretreating the CO gas or improving the function of the sensing material, the catalytic luminescence phenomenon of the sensing material on the surface of the material is enhanced, and the sensitivity of the catalytic luminescence sensing system for detecting CO is improved. The current method for pre-treating CO gas is mainly Dielectric Barrier Discharge (DBD Discharge), such as Nana project group, which utilizes DBD auxiliary Discharge to enhance the catalytic luminescence signals of hydrocarbon and CO gas (Analytical Chemistry, 2012, 84, 4830-4836; Nanoscale, 2014, 6, 3069-3072), and this technique shows good Analytical characteristics. However, the energy change caused by the air medium and the voltage fluctuation in the DBD medium discharging process causes the stability of the sample pretreatment process to be low, and the discharging process generates a large amount of ozone to pollute the atmosphere, thereby limiting the wide popularization of the detection technology and requiring the development of new technology.
Disclosure of Invention
The invention provides a sensor device for detecting carbon monoxide gas and an analysis method thereof. The method aims to solve the problem that the CO gas is difficult to detect in the traditional catalytic luminescence analysis and detection. The sensor device comprises a sample injection needle, an ultraviolet lamp, a quartz container, a quartz tube, an insulating medium, a photomultiplier and an optical filter. The sensor device in the ultraviolet lamp arrange in the top of quartz container, both ends communicate through polytetrafluoroethylene gas pipeline about the quartz container, CO gas is injected into the gas pipeline through the syringe needle, the controllable insulating medium of temperature coats functionalized graphite looks nitrogen sensing material, and arranges the quartz tube in, the light window top of photomultiplier is arranged in to the light filter, the quartz tube is arranged in the light filter top, the quartz tube has air inlet and gas outlet, the gas pipeline that the quartz container right-hand member came out directly links to each other with the air inlet of quartz tube, the gas outlet connects a section polytetrafluoroethylene pipe and discharges waste gas.
When the sensor device is used, air is used as carrier gas to convey CO gas activated by the ultraviolet lamp to the surface of the insulating medium coated with the functional graphite-phase carbon nitride sensing material, chemiluminescence is generated after catalytic oxidation, a photomultiplier is used for recording luminescence signals of different concentrations, and the carbon monoxide sample gas can be quantitatively detected by adopting linear regression analysis.
The invention combines the high activation and high stability of the ultraviolet lamp, introduces the non-metal catalyst, avoids the poisoning of the traditional metal catalyst, improves the reaction activity of the catalytic material and reactants, has simple device, environmental protection and low energy consumption, can be used for detecting CO gas in the environment, greatly reduces the detection limit of the catalytic reaction (reaching 6 ppm) by the aid of the ultraviolet lamp and the synergistic action of the functionalized graphite-phase carbon nitride sensing material, and improves the detection sensitivity.
The present invention further provides a method for detecting carbon monoxide gas using the sensor device and the analysis method thereof, comprising the steps of: and inserting CO gas into a gas pipeline through a sample injection needle for sample injection, stably introducing the CO gas into a quartz container by using air as carrier gas, activating under the irradiation of an ultraviolet lamp, and introducing the activated CO gas to the surface of the insulating medium coated with the functional graphite-phase carbon nitride sensing material. The functional graphite phase carbon nitride sensing material is prepared by sintering common precursors such as melamine, urea, guanidine hydrochloride and the like and then performing nitric acid reflux treatment; the temperature of the insulating medium is controllable and is arranged in the quartz tube; the insulating medium can be a ceramic sheet or a ceramic rod; the gas pipeline is made of polytetrafluoroethylene materials; the power of the ultraviolet lamp is 400W. The analysis method comprises the steps of carrying out catalytic oxidation on CO gas on the surface of a functionalized graphite phase nitrogen sensing material to generate a chemiluminescence signal, recording the catalytic luminescence signals under different CO gas concentrations through a photomultiplier, and carrying out quantitative detection on the CO gas by adopting linear regression analysis; wherein the sample volume of the CO gas is 5-500 mu L; the wavelength range of the optical filter is 400 nm-640 nm; the carrier gas is air, and the flow rate of the carrier gas is 50-450 mL/min; the temperature of catalytic oxidation is 140-235 ℃; the detection limit of CO gas can reach 6 ppm.
The invention has the following beneficial effects: the sensor device and the analysis method combine high activation and high stability of an ultraviolet lamp, improve the reaction activity of catalytic materials and reactants, greatly improve the sensitivity, have the characteristics of low energy consumption, good repeatability and long service life, and can be used for detecting trace CO gas in the environment. The invention also has the following advantages: (1) the sensor device has a simple structure, and the gas path only adopts one path of air which is used as a carrier gas and an oxidant source, so that instability caused by a plurality of gas paths is avoided; (2) the ultraviolet lamp device in the sensor device is simple, environment-friendly and low in cost. (3) The invention adopts the functional graphite-phase carbon nitride sensing material which is low in cost and easy to synthesize, introduces the non-metallic catalyst and avoids the poisoning of the traditional metallic catalyst. (4) The analysis method reduces the detection limit of CO gas (up to 6 ppm), and is favorable for detecting trace CO gas in the environment.
Drawings
FIG. 1 is a schematic diagram of a sensor device capable of detecting carbon monoxide (CO) gas, 1 being a sample injection needle, 2 being an ultraviolet lamp, 3 being a quartz container, 4 being a quartz tube, 5 being an insulating medium, 6 being a photomultiplier and 7 being a light filter.
Fig. 2 is a graph of CTL response signals of the functionalized graphite-phase carbon nitride sensing material to CO gas.
FIG. 3 is a linear relationship of CO gas concentration to its CTL response signal at the sensing device.
Detailed Description
The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. The functionalized graphite-phase carbon nitride sensing materials used in the examples described below were made by acid treatment after calcination. The water used in the experimental process in the following examples is ultrapure water, which is treated by a Yopu ultrapure water purification system. All samples in the following examples were not purified prior to use. The apparatus and the analysis method of the present invention will be further described with reference to the drawings attached to the specification, but the apparatus and the analysis method of the present invention are not limited to the following examples.
The sensor device comprises a sample injection needle, an ultraviolet lamp, a quartz container, a quartz tube, an insulating medium, a photomultiplier and an optical filter. The sensor device in the ultraviolet lamp arrange in the top of quartz container, both ends communicate through polytetrafluoroethylene gas pipeline about the quartz container, CO gas is injected into the gas pipeline through the syringe needle, the controllable insulating medium of temperature coats functionalized graphite looks nitrogen sensing material, and arranges the quartz tube in, the light window top of photomultiplier is arranged in to the light filter, the quartz tube is arranged in the light filter top, the quartz tube has air inlet and gas outlet, the gas pipeline that the quartz container right-hand member came out directly links to each other with the air inlet of quartz tube, the gas outlet connects a section polytetrafluoroethylene pipe and discharges waste gas.
When the sensor device (shown in figure 1) is used, CO gas is inserted into a polytetrafluoroethylene tube through a sample injection needle 1 for sample injection (the sample injection amount is 5-500 mu L), the CO gas is stably introduced into a quartz container 3 by using air as carrier gas (the flow is 50-450 mL/min), activation is carried out under the irradiation of a 400W ultraviolet lamp 2, and the activated CO gas is introduced to the surface of an insulating medium 5 coated with a functional graphite phase carbon nitride sensing material; the insulating medium is sleeved in the quartz tube 4; a photomultiplier tube 6 is arranged below the quartz tube and is used for collecting optical signals after being filtered by an optical filter 7 (the wavelength range is 400 nm-640 nm). And (2) performing a chemiluminescence catalytic oxidation reaction on the CO gas on the functionalized carbon nitride at a certain catalytic oxidation temperature (140-235 ℃), generating chemiluminescence, collecting and recording luminescence signals through a photomultiplier, processing all signal data through software, performing linear regression analysis, and finally completing the quantitative detection of the CO gas.
Example 1
A sample of 30 mu L of CO gas is fed into the sensor device, the air carrier gas flow rate is 100 mL/min, the wavelength of the optical filter is 460 nm, the catalytic oxidation temperature is 187 ℃, and the functional graphite phase carbon nitride sensing material responds to a CO gas CTL signal as shown in figure 2 a.
Example 2
And (3) introducing 30 mu L of CO gas into the sensor device, wherein the flow rate of the air carrier gas is 200 mL/min, the wavelength of the optical filter is 460 nm, the catalytic oxidation temperature is 187 ℃, and the CTL response signal of the functionalized graphite-phase carbon nitride sensing material to the CO gas is shown in figure 2 b.
Example 3
And (3) introducing 30 mu L of CO gas into the sensor device, wherein the air carrier gas flow rate is 100 mL/min, the wavelength of the optical filter is 490 nm, the catalytic oxidation temperature is 187 ℃, and the CTL response signal of the functionalized graphite-phase carbon nitride sensing material to the CO gas is shown in figure 2 c.
Example 4
A sample of 30 mu L of CO gas is fed into the sensor device, the air carrier gas flow rate is 100 mL/min, the wavelength of the optical filter is 460 nm, the catalytic oxidation temperature is 228 ℃, and the functional graphite phase carbon nitride sensing material responds to a CO gas CTL signal as shown in figure 2 d.
Example 5
When 30 mu L of CO gas is injected into the sensor device, the wavelength of the optical filter is 460 nm, the flow rate of air carrier gas is 100 mL/min, and the catalytic oxidation temperature is 187 ℃, the detection signal of the functionalized graphite phase carbon nitride sensing material responding to the CO gas is the highest, so that the detection under the condition is the optimal condition, and the response and the linearity of the catalytic luminescence analysis method to the CO gas are researched under the optimal condition. Obtaining different CO gas response signals when the sampling quantity of the CO gas is 5-500 mu L; from the relationship of the concentration in direct proportion to the response signal, a linear relationship (as shown in fig. 3) between the CO gas concentration and the response signal was obtained, and the detection limit of CO gas was calculated to be 6 ppm.
Claims (3)
1. A sensor device capable of detecting carbon monoxide (CO) gas, characterized in that:
the sensor device comprises a sample injection needle, an ultraviolet lamp, a quartz container, a quartz tube, an insulating medium, a photomultiplier and an optical filter; the sensor device is characterized in that an ultraviolet lamp is arranged above a quartz container, the left end and the right end of the quartz container are communicated through a polytetrafluoroethylene gas pipeline, CO gas is injected into the gas pipeline through a sample injection needle, a temperature-controllable insulating medium is coated with a functional graphite-phase carbon nitride sensing material and is arranged in the quartz tube, an optical filter is arranged above an optical window of a photomultiplier, the quartz tube is arranged above the optical filter and is provided with an air inlet and an air outlet, the gas pipeline coming out of the right end of the quartz container is directly connected with the air inlet of the quartz tube, and the air outlet is connected with a polytetrafluoroethylene tube to discharge waste gas.
2. The sensor device of claim 1, wherein: the power of an ultraviolet lamp in the sensor device is 400W.
3. An analytical method for detecting carbon monoxide gas by a sensor device according to claim 1, characterized in that:
(1) the analysis method is a catalytic luminescence sensing analysis, wherein CO gas is stably introduced into a quartz container by utilizing air as carrier gas, the CO gas activated by the ultraviolet lamp is conveyed to the surface of the functional graphite-phase carbon nitride sensing material, chemiluminescence is generated after catalytic oxidation, a photomultiplier records chemiluminescence signals with different concentrations, and the CO gas can be quantitatively detected by adopting linear regression analysis;
(2) the wavelength range in the analysis method is 400 nm-640 nm;
(3) in the analysis method, the sample volume of the CO gas is 5-500 mu L;
(4) in the analysis method, the carrier gas is air, and the flow rate of the carrier gas is 50-450 mL/min;
(5) in the analysis method, the catalytic oxidation temperature is 140-235 ℃;
(6) the detection limit of CO gas in the analysis method is 6 ppm.
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| US11573220B2 (en) * | 2018-12-31 | 2023-02-07 | Baker Hughes Oilfield Operations Llc | Cataluminescence for downhole fluid analysis |
| CN111878720A (en) * | 2020-06-16 | 2020-11-03 | 江门市雷居照明电器有限公司 | Industrial and mining lamp |
| CN112782174A (en) * | 2020-12-25 | 2021-05-11 | 西南化工研究设计院有限公司 | High-frequency electrodeless argon discharge ionization detector and method for analyzing sulfur and phosphorus compounds in gas |
| CN113758892A (en) * | 2021-10-15 | 2021-12-07 | 北方民族大学 | Coal mine production data screening method based on big data analysis |
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