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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[0032] Example 1: A method for preparing CdSe / ZnS core-shell quantum dots, the steps are as follows:
[0033] (1) 5mL of deionized water, add 0.19mmol NaOH while stirring, and pass N 2 After 10 minutes, add 0.035mmol of Se powder, add 0.051mmol of A1 powder after 10 minutes of reaction, heat up to 85℃, ultrasonic for 15min, get 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 a 10% by mass NaOH solution -9.0, stirring at room temperature for 10min, adding Na 2 The Se precursor solution is heated to 85°C and ultrasonicated for 25 minutes to prepare a 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 it at 85°C for 10 minutes; at the same time, add 4.5mL of 0.01mol / L thioacetamide solution and...
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[0038] Example 2: Drawing a 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; Dissolve the CdSe / ZnS quantum dots prepared in Example 1 in a phosphate buffer to prepare a 0.02 mg / mL CdSe / ZnS quantum dot solution;
[0040] (2) Take 1mL CdSe / ZnS quantum dot solution and 20uL 4-nitrotoluene standard solution in a 10mL colorimetric tube, dilute to 10mL with deionized water, shake it up, and after standing for 10min, add an appropriate amount of the Transfer the solution to a quartz cuvette, use 415nm as the excitation wavelength, and the excitation and emission slits are both 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; the concentration o...
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[0045] Example 3 Detection of trace amounts of 4-nitrotoluene
[0046] (1) Accurately weigh out 5.000g sample, add 20ml water / acetonitrile extraction solution with a volume ratio of 1:1, then add 0.10g disodium ethylenediaminetetraacetic acid, ultrasound for 30 minutes, centrifuge at room temperature, extract the supernatant and residue Use the extract to extract once, combine the two extracts, filter, and spin-evaporate the filtrate to dryness and dilute to 1.00 ml 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 to 10mL with deionized water, shake it, and after standing for 5min, add an appropriate amount Transfer the solution to a quartz cuvette, use 415nm as the excitation wavelength, and record the fluorescence emission intensity at 580nm;
[0048] According to the standard curve, the concentration C of 4-nitrotoluene was calculated and the recove...
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