A method for detecting hydrogen sulfide based on cataluminescence of nano yttrium oxide-indium oxide composite material

Abstract

The present application relates to the technical field of detection, and especially to a method for detecting hydrogen sulfide based on nano yttrium oxide-indium oxide composite material catalytic luminescence, which provides a method for detecting hydrogen sulfide based on nano Y2O3-In2O3 composite material catalytic luminescence, and adopts nano Y2O3-In2O3 composite material to detect hydrogen sulfide; in the nano Y2O3-In2O3 composite material, the molar ratio of Y and In is 0.8-1.2:1.The present application uses nano Y2O3-In2O3 composite material as sensitive material for detecting hydrogen sulfide by catalytic luminescence, and the surface of the nano Y2O3-In2O3 composite material has a large number of active oxygen, which promotes the reaction of hydrogen sulfide, and can realize rapid and accurate detection of hydrogen sulfide.The method has the advantages of high sensitivity, good specificity, good reproducibility and stability, fast response speed, high precision and the like.

Description

Technical Field

[0001] This invention relates to the field of detection technology, and in particular to a method for detecting hydrogen sulfide based on catalytic luminescence of nano-yttrium oxide-indium oxide composite material. Background Technology

[0002] Hydrogen sulfide is a colorless and harmful gas with the chemical formula H₂S. It is flammable and can form explosive mixtures with air. It ignites and explodes upon contact with open flames or high heat, and reacts violently with concentrated nitric acid, fuming sulfuric acid, or other strong oxidizers, resulting in an explosion. Furthermore, sulfides are potent neurotoxins and have a strong irritant effect on mucous membranes. Inhalation of high concentrations of H₂S can cause sudden death, and severe poisoning can leave neurological and psychiatric sequelae. In recent years, hydrogen sulfide poisoning accidents have occurred frequently. Developing sensitive, accurate, simple, and economical online monitoring methods for hydrogen sulfide is of great significance for preventing such accidents.

[0003] In view of this, the present invention is hereby proposed. Summary of the Invention

[0004] The purpose of this invention is to provide a method for detecting hydrogen sulfide based on the catalytic luminescence of nano-Y2O3-In2O3 composite material. The method uses nano-Y2O3-In2O3 composite material as the sensitive material and has the advantages of good reproducibility, good stability, fast response speed, high accuracy, high sensitivity and good specificity.

[0005] In order to achieve the above-mentioned objectives of the present invention, the following technical solution is adopted:

[0006] This invention provides a method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material, which uses nano-Y2O3-In2O3 composite material to detect hydrogen sulfide;

[0007] In the nano-Y2O3-In2O3 composite material, the molar ratio of Y to In is 0.8 to 1.2:1.

[0008] Furthermore, the preparation method of the nano-Y2O3-In2O3 composite material includes the following steps: Y salt, In salt, urea and sodium salicylate are subjected to a solvothermal reaction, followed by washing, drying and calcination in sequence to obtain the nano-Y2O3-In2O3 composite material.

[0009] Furthermore, the Y salt includes YCl3; the In salt includes InCl3.

[0010] Further, the molar ratio of the Y salt, the urea, and the sodium salicylate is 1:(2-5):(0.2-0.5).

[0011] Furthermore, the temperature of the solvothermal reaction is 150–200°C, and the time of the solvothermal reaction is 4–8 hours.

[0012] Furthermore, the calcination temperature is 350–450°C, and the calcination time is 2–5 hours.

[0013] Furthermore, the method for detecting hydrogen sulfide based on the catalytic luminescence of nano-Y2O3-In2O3 composite material includes the following steps: after hydrogen sulfide gas enters the catalytic luminescence reactor, it reacts under the catalysis of the nano-Y2O3-In2O3 composite material, and the luminescence signal of the gas after the reaction is detected.

[0014] Furthermore, the detection wavelength of the emitted light signal is 290–555 nm.

[0015] Furthermore, the reaction temperature in the catalytic luminescence reactor is 180–300°C.

[0016] Furthermore, the carrier gas includes air, and the flow rate of the carrier gas is 100–750 mL / min.

[0017] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0018] This invention provides a method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material. The nano-Y2O3-In2O3 composite material is used as the sensitive material for detecting hydrogen sulfide, and catalytic luminescence is utilized to detect hydrogen sulfide. The surface of the nano-Y2O3-In2O3 composite material has a large number of active oxygens, which promote the reaction of hydrogen sulfide, improve the signal intensity, and realize rapid and accurate detection of hydrogen sulfide.

[0019] The present invention provides a method for detecting hydrogen sulfide based on the catalytic luminescence of nano-Y2O3-In2O3 composite materials. This method can determine hydrogen sulfide with high sensitivity and specificity without interference from other substances; it has good reproducibility and stability and can be used for long-term monitoring of hydrogen sulfide; it also has the advantages of fast response speed and high accuracy. Attached Figure Description

[0020] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0021] Figure 1The XRD patterns are of nano-Y2O3 in Comparative Example 1, nano-In2O3 in Comparative Example 2, and nano-Y2O3-In2O3 composite material in Example 1 of this invention.

[0022] Figure 2 These are TEM images of nano-Y2O3 (Comparative Example 1), nano-In2O3 (Comparative Example 2), and nano-Y2O3-In2O3 composite material (Example 1) of the present invention.

[0023] Figure 3 The response signals of different gases on the surfaces of nano-Y2O3 in Comparative Example 1, nano-In2O3 in Comparative Example 2, and nano-Y2O3-In2O3 composite material in Example 1 are shown.

[0024] Figure 4 The results are obtained by seven parallel determinations of hydrogen sulfide using the method of Example 1 of this invention.

[0025] Figure 5 The results are from the stability test of the method in Embodiment 1 of the present invention.

[0026] Figure 6 The catalytic luminescence response curves of hydrogen sulfide at different concentrations on the surface of nano-Y2O3-In2O3 composite material are shown in the figure.

[0027] Figure 7 This is the hydrogen sulfide standard curve of the method in Example 1 of the present invention. Detailed Implementation

[0028] The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments. However, those skilled in the art will understand that the embodiments described below are some embodiments of the present invention, but not all embodiments, and are only used to illustrate the present invention, and should not be regarded as limiting the scope of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Where specific conditions are not specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall be followed. Where the manufacturers of reagents or instruments are not specified, they are all conventional products that can be purchased commercially.

[0029] The following is a detailed description of a method for detecting hydrogen sulfide based on the catalytic luminescence of nano-Y2O3-In2O3 composite material according to an embodiment of the present invention.

[0030] In some embodiments of the present invention, a method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material is provided. The method uses nano-Y2O3-In2O3 composite material to detect hydrogen sulfide. In the nano-Y2O3-In2O3 composite material, the molar ratio of Y to In is 0.8 to 1.2:1.

[0031] In some embodiments of the present invention, a method for online monitoring of hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material is provided, comprising: using nano-Y2O3-In2O3 composite material to monitor hydrogen sulfide online; wherein the molar ratio of Y to In in the nano-Y2O3-In2O3 composite material is 0.8 to 1.2:1.

[0032] This invention provides a method for detecting hydrogen sulfide based on the catalytic luminescence of nano-Y2O3-In2O3 composite material. The method utilizes the nano-Y2O3-In2O3 composite material to specifically catalyze the hydrogen sulfide oxidation, causing it to generate a luminescent signal at a specific wavelength, thereby achieving rapid and accurate detection of hydrogen sulfide.

[0033] The design of the sensitive material is crucial for catalytic luminescence detection methods. This invention employs a nano-Y₂O₃-In₂O₃ composite material as the sensitive material to detect hydrogen sulfide using catalytic luminescence. This method offers advantages such as high sensitivity, good specificity, good reproducibility, good stability, fast response speed, and high accuracy.

[0034] The band gap of In₂O₃ is 3.6 eV, and its work function is 5.0 eV. The band gap of Y₂O₃ is 5.6 eV, and its work function is 2.0 eV. Due to the significant difference in band gaps and work functions between the two materials, when nano-Y₂O₃-In₂O₃ composite materials are prepared, an easy junction forms at the interface between the two materials. This facilitates the formation of more active oxygen on the surface of the nano-Y₂O₃-In₂O₃ composite material, thereby promoting the reaction of hydrogen sulfide and improving signal intensity.

[0035] In some embodiments of the present invention, the molar ratio of Y to In in the nano-Y2O3-In2O3 composite material is 0.8 to 1.2:1; preferably, the molar ratio of Y to In in the nano-Y2O3-In2O3 composite material is 1:1.

[0036] In some embodiments of the present invention, the preparation method of nano Y2O3-In2O3 composite material includes the following steps: Y salt, In salt, urea and sodium salicylate are subjected to a solvothermal reaction, followed by washing, drying and calcination in sequence to obtain nano Y2O3-In2O3 composite material.

[0037] In some specific embodiments of the present invention, the solvothermal reaction includes: dissolving Y salt, In salt, urea and sodium salicylate in an organic solvent, and then placing them in a reaction vessel for a solvothermal reaction.

[0038] In some embodiments of the present invention, the Y salt includes YCl3; the In salt includes InCl3. The raw materials affect the properties of the prepared material. Using the above-mentioned types of Y salts and In salts can yield high-performance nano-Y2O3-In2O3 composite materials.

[0039] In some specific embodiments of the present invention, the organic solvent includes N,N-dimethylformamide (DMF).

[0040] In some embodiments of the present invention, the molar ratio of Y salt, urea and sodium salicylate is 1:(2-5):(0.2-0.5); preferably, the molar ratio of Y salt, urea and sodium salicylate is 1:(2-4):(0.3-0.4).

[0041] In some embodiments of the present invention, the temperature of the solvothermal reaction is 150–200°C and the time of the solvothermal reaction is 4–8 h; preferably, the temperature of the solvothermal reaction is 170–190°C and the time of the solvothermal reaction is 5–7 h.

[0042] In some specific embodiments of the present invention, washing includes alternating centrifugal washing with ethanol and deionized water.

[0043] In some specific embodiments of the present invention, the drying temperature is 50–100°C.

[0044] In some embodiments of the present invention, the calcination temperature is 350–450°C and the calcination time is 2–5 h; preferably, the calcination temperature is 400°C and the calcination time is 3 h.

[0045] The microstructure of a catalyst has a significant impact on its catalytic luminescence detection performance. The nano-Y₂O₃-In₂O₃ prepared by the above method in this invention is an amorphous composite material, wherein both Y₂O₃ and In₂O₃ are cubic phases, ensuring the effectiveness of catalytic luminescence detection.

[0046] In some embodiments of the present invention, a method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material includes the following steps: after hydrogen sulfide gas enters the catalytic luminescence reactor, it reacts under the catalysis of nano-Y2O3-In2O3 composite material, and the luminescence signal of the gas after the reaction is detected.

[0047] After hydrogen sulfide gas enters the catalytic luminescence reactor, the reactor is heated to the corresponding reaction temperature. The hydrogen sulfide gas comes into contact with the nano-Y2O3-In2O3 composite material. On the surface of the nano-Y2O3-In2O3 composite material, the hydrogen sulfide gas is oxidized by oxygen in the air, generating a catalytic luminescence signal.

[0048] Hydrogen sulfide gas can produce a strong catalytic luminescence signal under the catalysis of nano-Y2O3-In2O3 composite material, while other substances such as ammonium sulfide, dimethyl sulfide, trimethylamine, trichloroethylene, n-hexane, methanol, ethanol, n-propanol, n-butanol, isobutanol, sec-butanol, formaldehyde, acetaldehyde, formic acid, ethyl acetate, benzene, toluene, o-xylene, m-xylene, p-xylene, styrene, ethylene glycol methyl ether, ethylene glycol ethyl ether, and ammonia do not produce a signal under the same conditions.

[0049] In some embodiments of the present invention, the detection wavelength of the light emission signal is 290–555 nm; typically, but not limitingly, for example, the detection wavelength of the light emission signal can be a range of 290 nm, 320 nm, 350 nm, 370 nm, 400 nm, 420 nm, 450 nm, 470 nm, 500 nm, 520 nm, 550 nm, or any combination thereof.

[0050] In some specific embodiments of the present invention, the detection wavelength of the light emission signal is 320-380 nm; preferably 350 nm.

[0051] In some embodiments of the invention, the reaction temperature in the catalytic light-emitting reactor is 180–300°C; typically, but not limitingly, for example, the reaction temperature in the catalytic light-emitting reactor is a range of 180°C, 200°C, 220°C, 240°C, 260°C, 280°C, 300°C, or any combination thereof.

[0052] In some specific embodiments of the present invention, the reaction temperature in the catalytic luminescence reactor is 200-250°C; preferably 223°C.

[0053] In some embodiments of the invention, the carrier gas comprises air, and the flow rate of the carrier gas is 100 to 750 mL / min; typically, but not limitingly, for example, the flow rate of the carrier gas is a range of 100 mL / min, 200 mL / min, 300 mL / min, 400 mL / min, 500 mL / min, 600 mL / min, 700 mL / min, or any combination thereof.

[0054] In some specific embodiments of the present invention, the flow rate of the carrier gas is 500-700 mL / min; preferably 650 mL / min.

[0055] In some specific embodiments of the present invention, the method for detecting hydrogen sulfide based on the catalytic luminescence of nano-Y2O3-In2O3 composite material has the following specific conditions: the detection wavelength of the luminescence signal is 350 nm; the reaction temperature is 223 °C; the carrier gas is air, and the flow rate of the carrier gas is 650 mL / min.

[0056] Under the above detection conditions, the detection limit for hydrogen sulfide is 6 ppm, and the test has a rapid response capability.

[0057] In some embodiments of the present invention, in the method for detecting hydrogen sulfide based on nano-Y2O3-In2O3 composite material catalytic luminescence, the catalyst layer of the catalytic luminescence reactor is made of nano-Y2O3-In2O3 composite material. Apart from the catalyst layer of the catalytic luminescence reactor, the present invention does not strictly limit other structures and materials of the catalytic luminescence reactor.

[0058] In some specific embodiments of the present invention, the catalytic light-emitting reactor includes a sampling unit, a catalytic light-reflecting reaction unit, and a detection unit; wherein, the catalytic light-reflecting reaction unit includes a cavity structure and a heat-conducting substrate disposed in the cavity structure, the surface of the heat-conducting substrate is attached with a catalytic layer, and the material of the catalytic layer is a nano-Y2O3-In2O3 composite material.

[0059] In some specific embodiments of the present invention, the thickness of the catalyst layer is 1.5 to 3 mm.

[0060] In some specific embodiments of the present invention, the thermally conductive substrate includes a ceramic heating rod; the cavity includes a quartz cavity.

[0061] In some specific embodiments of the present invention, the method for preparing the catalyst layer includes: sintering the Y2O3-In2O3 composite material onto the surface of a thermally conductive substrate; preferably, the sintering temperature is 350-400°C and the sintering time is 20-30 min.

[0062] Hydrogen sulfide gas is fed into the catalytic luminescence reaction unit through the sampling unit. The heat-conducting substrate is heated to the corresponding reaction temperature. The hydrogen sulfide gas comes into contact with the catalyst layer. On the surface of the catalyst layer, the hydrogen sulfide is oxidized by oxygen in the air, generating a catalytic luminescence signal, which is detected, analyzed and displayed by the detection unit.

[0063] In some specific embodiments of the present invention, a method for detecting hydrogen sulfide based on nano-Y2O3-In2O3 composite material catalytic luminescence includes: sending a series of standard working gas samples containing hydrogen sulfide into the catalytic luminescence reaction unit via a sampling unit, detecting the luminescence signal of the gas after the reaction via a detection unit, plotting a standard curve of hydrogen sulfide with the concentration of the standard working gas samples as the abscissa and the intensity of the luminescence signal as the ordinate; substituting the intensity of the luminescence signal of the gas to be tested into the standard curve of hydrogen sulfide to calculate the concentration of hydrogen sulfide in the gas to be tested.

[0064] Example 1

[0065] The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite materials provided in this embodiment includes the following steps:

[0066] Hydrogen sulfide gas was prepared using headspace gas mixing and used as the test gas. After the test gas was sent to the catalytic luminescence reaction unit through the sampling unit, the thermally conductive substrate was heated to the corresponding reaction temperature. The hydrogen sulfide gas came into contact with the catalyst layer, and the hydrogen sulfide on the surface of the catalyst layer was oxidized by oxygen in the air, generating a catalytic luminescence signal, which was detected, analyzed and displayed by the detection unit.

[0067] The detection conditions were as follows: the catalyst layer was made of nano-Y2O3-In2O3 composite material; the detection wavelength of the luminescence signal was 350 nm; the reaction temperature was 223 ℃; the carrier gas was air; and the flow rate of the carrier gas was 650 mL / min.

[0068] The preparation method of nano-Y2O3-In2O3 composite material includes the following steps:

[0069] Under stirring conditions, 0.1953 g YCl3, 0.2212 g InCl3, 0.180 g urea and 0.063 g sodium salicylate were dissolved in 50 mL N,N-dimethylformamide (DMF). The solution was then transferred to a polytetrafluoroethylene high-pressure reactor and reacted at 180 °C for 6 h. After the reaction, the resulting precipitate was washed alternately by centrifugation with ethanol and deionized water, and then dried in an oven at 80 °C to obtain the precursor. The obtained precursor was then calcined in a muffle furnace at 400 °C for 3 h to obtain nano-Y2O3-In2O3 composite material.

[0070] Comparative Example 1

[0071] The method for detecting hydrogen sulfide based on catalytic luminescence of nanomaterials provided in this comparative example refers to Example 1, except that the catalyst layer is made of nano-Y2O3.

[0072] The preparation method of nano-Y2O3 includes the following steps:

[0073] Under stirring conditions, 0.1953 g YCl3, 0.180 g urea, and 0.063 g sodium salicylate were dissolved in 50 mL N,N-dimethylformamide (DMF). The solution was then transferred to a polytetrafluoroethylene high-pressure reactor and reacted at 180 °C for 6 h. After the reaction, the resulting precipitate was washed alternately by centrifugation with ethanol and deionized water, and then dried in an oven at 80 °C to obtain the precursor. The obtained precursor was then calcined in a muffle furnace at 400 °C for 3 h to obtain nano-Y2O3.

[0074] Comparative Example 2

[0075] The method for detecting hydrogen sulfide based on catalytic luminescence of nanomaterials provided in this comparative example refers to Example 1, except that the catalyst layer is made of nano-In2O3.

[0076] The preparation method of nano-In2O3 includes the following steps:

[0077] Under stirring conditions, 0.2212 g InCl3, 0.180 g urea, and 0.063 g sodium salicylate were dissolved in 50 mL N,N-dimethylformamide (DMF). The solution was then transferred to a polytetrafluoroethylene high-pressure reactor and reacted at 180 °C for 6 h. After the reaction, the resulting precipitate was washed alternately by centrifugation with ethanol and deionized water, and then dried in an oven at 80 °C to obtain the precursor. The obtained precursor was then calcined in a muffle furnace at 400 °C for 3 h to obtain nano-In2O3.

[0078] Experimental Example 1

[0079] X-ray diffraction (XRD) tests were performed on the nano-Y2O3-In2O3 composite material prepared in Example 1, the nano-Y2O3 prepared in Comparative Example 1, and the nano-In2O3 prepared in Comparative Example 2. The results are as follows: Figure 1 As shown.

[0080] from Figure 1 As can be seen from the diffraction peak positions, both the prepared nano-Y₂O₃ and nano-In₂O₃ are cubic phases, with standard PDF card numbers 79-1257 and 44-1087, respectively. The XRD pattern of the nano-Y₂O₃-In₂O₃ composite material shows characteristic color peaks for both nano-Y₂O₃ and nano-In₂O₃, indicating the successful preparation of the nano-Y₂O₃-In₂O₃ composite.

[0081] Transmission electron microscopy (TEM) was performed on the nano-Y2O3-In2O3 composite material prepared in Example 1, the nano-Y2O3 prepared in Comparative Example 1, and the nano-In2O3 prepared in Comparative Example 2. The results are as follows: Figure 2 As shown. Figure 2 In the diagram, (A) represents nano-Y2O3, (B) represents nano-In2O3, and (C) represents a nano-Y2O3-In2O3 composite material.

[0082] from Figure 2 It can be seen that nano-Y2O3 and nano-In2O3 are irregular particles, and the morphology of the nano-Y2O3-In2O3 composite material has not changed and remains irregular particles.

[0083] Experimental Example 2

[0084] Hydrogen sulfide at 150 ppm was tested using the methods of Example 1, Comparative Example 1, and Comparative Example 2, respectively. The hydrogen sulfide gas in Example 1, Comparative Example 1, and Comparative Example 2 was replaced with propionaldehyde, butyraldehyde, ammonium sulfide, dimethyl sulfide, trimethylamine, trichloroethylene, hexane, methanol, ethanol, propanol, butanol, isobutanol, sec-butanol, formaldehyde, acetaldehyde, formic acid, ethyl acetate, benzene, toluene, o-xylene, m-xylene, p-xylene, styrene, ethylene glycol methyl ether, ethylene glycol ethyl ether, and ammonia, respectively. The results are as follows: Figure 3 As shown.

[0085] from Figure 3 It can be seen that, compared with individual nano-Y2O3 materials or nano-In2O3 materials, the signal of hydrogen sulfide detection using nano-Y2O3-In2O3 composite material is enhanced by 13.4 times and 3.3 times respectively, while the signals of n-propanaldehyde and n-butyraldehyde are not significantly increased, and other gases do not produce signals; indicating that the detection of hydrogen sulfide using nano-Y2O3-In2O3 composite material has the advantages of high sensitivity and good specificity.

[0086] Experimental Example 3

[0087] The method of Example 1 was used to perform seven parallel determinations of 150 ppm hydrogen sulfide gas, and the results are as follows: Figure 4 As shown.

[0088] from Figure 4 The relative standard deviation of the seven parallel determinations was 3.6%, indicating that the nano-Y2O3-In2O3 composite material has good reproducibility as a catalytic luminescence sensitive material for detecting hydrogen sulfide.

[0089] The method of Example 1 was used to determine 150 ppm of hydrogen sulfide gas in parallel over 7 days, and the results are as follows. Figure 5 As shown.

[0090] from Figure 5 It can be seen that the relative standard deviation of parallel measurements over 7 days is 2.6%, indicating that the nano-Y2O3-In2O3 composite material has good stability as a catalytic luminescence sensitive material for detecting hydrogen sulfide, which is of great significance for long-term monitoring.

[0091] Test Example 4

[0092] Achieving a rapid response to the target analyte is a prerequisite for rapid detection. Using the method of Example 1, hydrogen sulfide gas at concentrations of 40 ppm, 150 ppm, and 250 ppm was measured, and the resulting kinetic response curves are shown below. Figure 6 As shown; Figure 6 Curve 1 shows a value of 40 ppm, curve 2 shows a value of 150 ppm, and curve 3 shows a value of 250 ppm.

[0093] from Figure 6 It can be seen that the luminescence signal increases with increasing hydrogen sulfide concentration, but the curve shapes are similar. The signal reaches its maximum value about 3 seconds after sample injection, and it takes about 18 seconds for the signal to return to the baseline from the maximum value, indicating that the method has a rapid response capability to hydrogen sulfide and has good application in rapid online monitoring of hydrogen sulfide.

[0094] Experimental Example 5

[0095] Using the method described in Example 1, hydrogen sulfide standard gas samples with concentrations of 15 ppm, 40 ppm, 100 ppm, 150 ppm, 200 ppm, 250 ppm, 300 ppm, and 400 ppm were measured. The measured luminescence intensity was then linearly regressed against the concentration, and the results are as follows: Figure 7 As shown.

[0096] from Figure 7 The obtained linear regression equation is I = 9.297c - 61.95, where I is the luminescence intensity, c is the hydrogen sulfide concentration, and the correlation coefficient R is... 2 =0.9977, and the detection limit is 6 ppm when the signal-to-noise ratio is 3.

[0097] Experimental Example 6

[0098] To further verify the application value of the method of this invention, 100 ppm of hydrogen sulfide was mixed with 2000 ppm of potential interfering substances to prepare four artificial samples, and the recovery rate of hydrogen sulfide was determined. The measured signal values ​​were substituted into the standard linear regression equation to calculate the measured concentration values, and the recovery rate was calculated by comparing the measured values ​​with the standard values. The results are shown in Table 1.

[0099] Table 1

[0100]

[0101] As can be seen from Table 1, the recovery rate is between 96.4% and 101.5%, which is good, indicating that this method has good application prospects.

[0102] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite materials, characterized in that, Hydrogen sulfide was detected using a nano-Y2O3-In2O3 composite material; In the nano-Y2O3-In2O3 composite material, the molar ratio of Y to In is 0.8~1.2:1; The preparation method of the nano-Y2O3-In2O3 composite material includes the following steps: Y salt, In salt, urea and sodium salicylate are subjected to a solvothermal reaction, followed by washing, drying and calcination to obtain the nano-Y2O3-In2O3 composite material.

2. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 1, characterized in that, The Y salt includes YCl3; the In salt includes InCl3.

3. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 1, characterized in that, The molar ratio of the Y salt, the urea, and the sodium salicylate is 1:(2~5):(0.2~0.5).

4. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 1, characterized in that, The temperature of the solvothermal reaction is 150~200℃, and the time of the solvothermal reaction is 4~8h.

5. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 1, characterized in that, The calcination temperature is 350~450℃, and the calcination time is 2~5h.

6. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 1, characterized in that, The process includes the following steps: after hydrogen sulfide gas enters the catalytic luminescence reactor, it reacts under the catalysis of the nano-Y2O3-In2O3 composite material, and the luminescence signal of the gas after the reaction is detected.

7. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 6, characterized in that, The detection wavelength of the emitted light signal is 290~555nm.

8. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 6, characterized in that, The reaction temperature in the catalytic luminescence reactor is 180~300℃.

9. The method for detecting hydrogen sulfide based on catalytic luminescence of nano-Y2O3-In2O3 composite material according to claim 6, characterized in that, The carrier gas includes air, and the flow rate of the carrier gas is 100~750 mL / min.

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