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A kind of fluorescence measuring method of nitromethane
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A technology for the determination of nitromethane and fluorescence, which is applied in the field of fluorescence sensing, and achieves the effects of strong practicability, simple operation and high sensitivity
Active Publication Date: 2022-05-13
HUBEI FUBO CHEM & IND CO LTD +1
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[0004] Aiming at the deficiencies in the existing determination of nitromethane distillates by gas chromatography on aqueous samples of nitromethane distillates and nitromethane in nitromethane production wastewater, the present invention provides a low-cost, simple-to-operate, high-sensitivity, and strong-practicability , good selectivity, no need for additional separation and pretreatment of complex matrix components, and a fluorescence measurement method that can directly detect nitromethane by using a graphite carbon nitride fluorescence sensor
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Embodiment 1
[0089] Preparation of graphite carbon nitride fluorescent probe:
[0090] Add 0.15 g of sodium citrate dihydrate and 0.44 g of melamine to 45 ml of double distilled water, and after ultrasonic treatment for 5 min, transfer the mixture to a 100 ml autoclave, heat at 200 ° C for 3 h, and use a high-speed centrifuge to 1.0 × 10 4 Centrifuge at a speed of rpm for 25 minutes, and the solution obtained by filtering impurities is graphitic carbon nitride.
Embodiment 2
[0092] Preparation of graphite carbon nitride fluorescent probe:
[0093] Add 0.3 g of sodium citrate dihydrate and 0.88 g of melamine to 80 ml of double distilled water, and after ultrasonic treatment for 10 min, transfer the mixture to a 200 ml autoclave, heat at 250 ° C for 5 h, and after cooling, use a high-speed centrifuge to 1.3 × 10 4 Centrifuge at a speed of rpm for 40 minutes, and the solution obtained by filtering impurities is graphitic carbon nitride.
Embodiment 3
[0095] Preparation of graphite carbon nitride fluorescent probe:
[0096] Add 0.2 g of sodium citrate dihydrate and 0.587 g of melamine to 70 ml of double distilled water, and after ultrasonic treatment for 8 min, transfer the mixture to a 200 ml autoclave, heat at 220°C for 4 h, and after cooling, use a high-speed centrifuge to 1.2 × 10 4 Centrifuge at a speed of rpm for 30 minutes, and the solution obtained by filtering impurities is graphitic carbon nitride.
[0097] SEM image from graphitic carbon nitride (eg Figure 6 ), it can be seen that graphitic carbon nitride is in the form of flakes, which are relatively uniformly dispersed in aqueous solution.
[0098] From the infrared spectrum of graphitic carbon nitride (such as Figure 7 ) can be seen, graphitic carbon nitride at 1417cm -1 ,1631cm -1 ,3147cm -1 ,3431cm -1 There are obvious peaks at , respectively representing the stretching vibrations of C-N, C=O, N-H, O-H, indicating that the surface of graphitic carbon...
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Abstract
The invention belongs to the technical field of fluorescence sensing, and in particular relates to a method for measuring fluorescence of nitromethane. The graphite carbon nitride fluorescent probe was prepared by reacting sodium citrate dihydrate with melamine, and its fluorescence intensity showed a linear quenching relationship at the emission wavelength of 434nm with the change of nitromethane concentration. Aqueous samples of nitromethane distillates and nitromethane in nitromethane production wastewater. The invention has the advantages of convenient operation, good specific selectivity, high sensitivity, fast response time and good accuracy.
Description
technical field [0001] The invention belongs to the technical field of fluorescence sensing, and in particular relates to a fluorescence measuring method for nitromethane, more specifically, relates to a method for measuring nitromethane with a graphite carbon nitride fluorescent probe. Background technique [0002] Nitromethane is a colorless oily liquid with a wide range of uses. It is used in organic synthesis and can be used to synthesize pesticides such as chloropicrin and nitroalcohol. It can also be used as a sensitizer and co-solvent in explosives and weapon propellants. and important raw materials for pharmaceutical intermediates. Studies have shown that nitromethane is converted into methyl isocyanate in the body, and long-term exposure to low concentrations of nitromethane can cause toxic changes in the basal ganglia and brain. Therefore, it is very important to detect the content of nitromethane. [0003] The existing methods for detecting nitromethane are main...
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