Application of nano fluorescent probe SiO2 (at) Tb in detection of Fe < 3 + > in water body
A nano-fluorescent probe and water body technology, which is applied in the direction of fluorescence/phosphorescence, color/spectral characteristic measurement, and measurement devices, can solve the problems of being easily affected by the environmental background, achieve good selectivity and sensitivity, and be easy to operate. The effect of simple equipment
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Embodiment 1
[0039] Provide a ratiometric fluorescent probe SiO 2 The preparation of @Tb includes the following steps:
[0040] 1) Put 0.5 g of nano-SiO with a particle size of 9 nm 2 It was dispersed in 50 mL of ethanol by ultrasonic, and then 0.1 mL of 3-aminopropyl triethoxysilane (APTES) was added to react for 24 h. After the reaction is completed, the obtained product is centrifuged at high speed to obtain amino-modified silica nanoparticles (SiO 2 @NH 2 ).
[0041] 2) ultrasonically disperse the obtained amino-modified silica nanoparticles in 50 mL of tetrahydrofuran, add 0.1 g of trimellitic anhydride (TMA), stir and react for 8 h at room temperature, centrifuge the product at high speed, and wash with tetrahydrofuran and ethanol solution , to remove unreacted TMA to obtain carboxyl-modified silica nanoparticles (SiO 2 @COOH).
[0042] 3) ultrasonically disperse the carboxyl-modified silica nanoparticles obtained above in 30 mL of ethanol, drop an appropriate amount of triethy...
Embodiment 2
[0043] Example 2: Selectivity experiment
[0044] 1) Preparation of sample suspension: the nano-fluorescent probe SiO prepared in Example 1 was 2 @Tb (1 mg) was ultrasonically dispersed in 10 mL of deionized water to obtain uniformly dispersed SiO 2 @Tb suspension.
[0045] 2) Prepare aqueous solutions of different metal cations with a concentration of 0.01M respectively, and the cations are Fe 3+ , Na + , K + , Ba 2+ , Mg 2+ , Ca 2+ , Fe 2+ , Mn 2+ , Co 2+ .
[0046] 3) Detection method: take the SiO prepared in 1) for each 2 Put 2 mL of @Tb suspension in a cuvette, add the aqueous solutions (0.01 M, 20 μL) of different metal cations prepared in step 2), turn on the fluorescence spectrometer, and record the fluorescence emission spectrum under the excitation of ultraviolet light with a wavelength of 237 nm. The spectral data were analyzed, and the fluorescence intensity I at 545 nm and 461 nm was obtained from the emission spectrum 545 , I 461 , find I 545 / I ...
Embodiment 3
[0048] Example 3: Titration experiment to obtain working curve
[0049] 1) SiO 2 Preparation of @Tb Suspension: Same as Example 2.
[0050] 2) Prepare Fe with a concentration of 0.1 mM 3+ solution.
[0051] 3) Titration experiment: take the SiO prepared in 1) 2 Put 2.0 mL of @Tb suspension in a cuvette, turn on the fluorescence spectrometer, and record the emission spectrum under the excitation of ultraviolet light. Then add 20 μL, 20 μL, 20 μL, 20 μL, 20 μL, 20 μL, 40 μL, 40 μL, 40 μL, 40 μL, 40 μL Fe 3+ Aqueous solution (0.1mM), mix well, use 237nm excitation wavelength for excitation and record luminescence emission spectrum, record SiO 2 @Tb suspension fluorescence intensity and calculate I 545 / I 461 ratio to I 545 / I 461 The ratio of Fe to Fe 3+ The concentration of , and the data are fitted to obtain the linear equation (2):
[0052] y=8.74886-0.35993[C] (2)
[0053] where, y: fluorescence emission intensity I 545 / I 461 Ratio; [C]:Fe 3+ content.
[0054...
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