Preparation method of electrochemiluminescence biosensor for detecting organochlorine pesticides
A luminescent biology and electrochemistry technology, used in chemiluminescence/bioluminescence, scientific instruments, and analysis by chemical reaction of materials, etc., can solve the problems of cumbersome process and low yield, and achieve simple preparation and low cost. , the effect of increasing the intensity of electrochemiluminescence
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Embodiment 1
[0042] Example 1 FeMn-TiO 2 / MoS 2 preparation of
[0043] (1) Add 0.6 g of molybdenum disulfide powder, 0.2 mmol of iron salt and 0.2 mmol of manganese salt into 3 mL of n-butyllithium solution, and stir for 12 hours under nitrogen protection at 60 °C to obtain the reacted solution;
[0044] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 60 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain iron , Molybdenum disulfide nanomaterials co-intercalated with manganese;
[0045] (3) Add 500 mg of molybdenum disulfide nanomaterials co-intercalated with iron and manganese prepared in step (2) into 5 mL of tetrabutyl titanate, and after stirring for 1 hour, slowly add 0.5 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 160°C for 18 hours;
[0046] (4) The reaction product obtained in step (3) was centrifuged and washed three
Embodiment 2
[0052] Example 2 FeMn-TiO 2 / MoS 2 preparation of
[0053] (1) Add 0.6 g of molybdenum disulfide powder, 1.0 mmol of iron salt and 1.0 mmol of manganese salt into 5 mL of n-butyllithium solution, and stir for 24 hours under nitrogen protection at 30 °C to obtain the reacted solution;
[0054] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 30 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain iron , Molybdenum disulfide nanomaterials co-intercalated with manganese;
[0055] (3) Add 200 mg of molybdenum disulfide nanomaterials co-intercalated with iron and manganese prepared in step (2) into 5 mL of tetrabutyl titanate, stir for 1 hour, then slowly add 0.6 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 180°C for 20 hours;
[0056] (4) The reaction product obtained in step (3) was centrifuged and washed three times wi
Embodiment 3
[0062] Example 3 FeMn-TiO 2 / MoS 2 preparation of
[0063] (1) Add 0.6 g of molybdenum disulfide powder, 2.0 mmol of iron salt and 2.0 mmol of manganese salt into 10 mL of n-butyllithium solution, and stir for 48 hours under nitrogen protection at 50 °C to obtain the reacted solution;
[0064] (2) Wash the reacted solution in step (1) with a non-polar solvent, and then perform ultrasonic treatment in a water bath at 50 °C. After the treatment, wash the treated solution with a non-polar solvent, and dry it in vacuum to obtain iron , Molybdenum disulfide nanomaterials co-intercalated with manganese;
[0065] (3) Add 10 mg of molybdenum disulfide nanomaterials co-intercalated with iron and manganese prepared in step (2) into 5 mL of tetrabutyl titanate, stir for 1 hour, then slowly add 0.8 mL of hydrofluoric acid while stirring acid, then reacted in a reactor at 200°C for 24 hours;
[0066] (4) The reaction product obtained in step (3) was centrifuged and washed three times wi
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