Method for detecting mercury ions based on Silica/chitosan/Ru nanoparticle electrochemiluminescence method
A nanoparticle and composite nanoparticle technology is applied in the field of mercury ion detection based on Silica/chitosan/Ru nanoparticle electrochemiluminescence method, which can solve the problems of high time-consuming and cost, affecting identification characteristics, etc., and achieve low cost and high sensitivity. The effect of detection
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Embodiment 1
[0029] In this embodiment, the heavy metal ion Hg contained in the aqueous solution sample can be detected by the method of electrochemiluminescence detection. 2+ , specifically implemented by the following steps:
[0030] (1) Synthesis of silica composite nanoparticles doped with chitosan and bipyridyl ruthenium (abbreviation: Silica / chitosan / Ru)
[0031] At room temperature, mix 1.8 mL of TritonX-100, 1.8 mL of n-hexanol and 7.5 mL of cyclohexane evenly, add 260 μL of ultrapure water under stirring, and after stirring for 30 minutes, add 100 μL of 0.1% (w / v) chitosan Sugar (Chitosan) and 50 μL concentration of 0.01mol / L bipyridyl ruthenium (Ru(bpy) 3 2+ , formula C 30 h 24 Cl 2 N 6 Ru . 6H 2 O, the molecular weight is 748.62), and add 0.1mol / L NaOH to adjust the system to neutrality, continue to stir for 60min, then add 90μL of tetraethyl orthosilicate and 60μL of ammonia water into the reaction system, keep stirring for 22h, after the reaction is completed , add ac...
Embodiment 2
[0046] In this example, in step (1) at room temperature, mix 1.8 mL of TritonX-100, 1.8 mL of n-hexanol and 7.2 mL of cyclohexane evenly, add 200 μL of ultrapure water under stirring, and after stirring for 25 minutes, add 120 μL of 0.1 % (w / v) chitosan and 72 μL concentration of 0.01mol / L bipyridyl ruthenium, and 0.1mol / L NaOH was added to adjust the system to neutrality, and after stirring for 40 min, 120 μL tetraethyl orthosilicate and 72 μL Aqueous ammonia was added to the reaction system, so that the volume ratio of ethyl orthosilicate to chitosan, bipyridyl ruthenium and n-hexanol was 1:1:0.5:15, and the stirring was continued for 20 hours. After the reaction was completed, acetone was added to break the emulsion. Collected by centrifugation, washed 4 times with absolute ethanol and ultrapure water respectively, to obtain a solution of silica composite nanoparticles (abbreviation: Silica / chitosan / Ru) doped with chitosan and bipyridyl ruthenium, and the finally obtained Si...
Embodiment 3
[0049] In this example, in step (1) at room temperature, mix 1.8 mL of TritonX-100, 1.8 mL of n-hexanol and 7.74 mL of cyclohexane evenly, add 300 μL of ultrapure water while stirring, and after stirring for 20 minutes, add 93.6 μL of 0. 1% (w / v) chitosan and 57.6 μL concentration of 0.01mol / L bipyridyl ruthenium, and 0.1mol / L NaOH was added to adjust the system to neutrality, and after stirring for 60 minutes, 72 μL of orthosilicate ethyl Add 57.6 μL of ammonia water into the reaction system, make the volume ratio of tetraethyl orthosilicate to chitosan, bipyridyl ruthenium, and n-hexanol 1:1.3:0.8:25, and keep stirring for 24 hours. After the reaction is completed, add acetone Demulsification, centrifugation, and washing twice with absolute ethanol and ultrapure water respectively, to obtain a silica composite nanoparticle (abbreviation: Silica / chitosan / Ru) solution doped with chitosan and bipyridyl ruthenium. The obtained Silica / chitosan / Ru solution was centrifuged step by ...
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