Preparation method and application of CdSe/ZnS core-shell quantum dots
A technology of core-shell quantum dots and nuclear quantum dots, which is applied in the detection of trace explosives 4-nitrotoluene, and in the field of preparation of CdSe/ZnS core-shell quantum dots, which can solve the problem of no public 4-nitrotoluene compound technology Enlightenment, did not disclose the technical characteristics of core-shell quantum dot nitroaromatic compound nanomaterials, etc., to achieve the effects of good fluorescence stability, stable structure, and increased reaction rate
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Embodiment 1
[0032] Embodiment 1: A preparation method of CdSe / ZnS core-shell quantum dots, the steps are as follows:
[0033] (1) 5mL of deionized water, under stirring, add 0.19mmol NaOH, pass N 2 After 10min, add 0.035mmol of Se powder, add 0.051mmol of A1 powder after 10min of reaction, raise the temperature to 85°C, and sonicate for 15min to obtain a clear Na 2 Se precursor solution;
[0034] (2) Dissolve 0.12mmol of cadmium perchlorate in 50mL of deionized water, add 0.120mmol of methionine and 0.125mmol of mercaptopropionic acid under stirring, and adjust the pH to 8.5 with 10% NaOH solution -9.0, stir at room temperature for 10min, add Na 2 For the Se precursor solution, the temperature was raised to 85°C, and the ultrasonic wave was used for 25 minutes to prepare the CdSe nuclear quantum dot solution;
[0035] (3) Add 0.110mmol of methionine and 0.110mmol of mercaptopropionic acid to the CdSe nuclear quantum dot solution, and keep warm at 85°C for 10min; at the same time, add 0...
Embodiment 2
[0038] Embodiment 2: draw standard curve, the steps are as follows:
[0039] (1) Dissolve 4-nitrotoluene in water / acetonitrile with a volume ratio of 1:2 to obtain 2.4×10 -9 mol / L~3.1×10 -7 mol / L 4-nitrotoluene standard solution; the CdSe / ZnS quantum dots prepared in Example 1 were dissolved in phosphate buffer to obtain a 0.02 mg / mL CdSe / ZnS quantum dot solution;
[0040] (2) Take 1mL of CdSe / ZnS quantum dot solution and 20uL of 4-nitrotoluene standard solution in a 10mL colorimetric tube, dilute it to 10mL with deionized water, shake it up, let it stand for 10min, and then add an appropriate amount of the The solution is transferred to a quartz cuvette, using 415nm as the excitation wavelength, the excitation and emission slits are 5nm, record the functional relationship between the fluorescence emission intensity at 580nm and the concentration of 4-nitrotoluene, and draw a standard curve;
[0041] 4-nitrotoluene has a fluorescence quenching effect on CdSe / ZnS quantum dots...
Embodiment 3
[0045] The detection of embodiment 3 trace 4-nitrotoluene
[0046] (1) Accurately weigh 5.000g of sample, add 20ml of water / acetonitrile extraction solution with a volume ratio of 1:1, then add 0.10g of disodium ethylenediaminetetraacetate, ultrasonicate for 30 minutes, centrifuge at room temperature, extract the supernatant, and the residue Extract once again with the extract, combine the two extracts, filter, spin the filtrate to dryness, and set the volume to 1.00ml to prepare a sample solution of 4-nitrotoluene;
[0047] (2) Take 1mL of CdSe / ZnS quantum dot solution and 20uL of 4-nitrotoluene sample solution in a 10mL colorimetric tube, dilute it to 10mL with deionized water, shake it up, let it stand for 5min, and then add an appropriate amount of The solution is transferred to a quartz cuvette, and 415nm is used as the excitation wavelength to record the fluorescence emission intensity at 580nm;
[0048] According to the standard curve, calculate the concentration C of ...
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