Preparation method and application of physiological pH sensing binuclear ruthenium complex
A technology of ruthenium complexes and bridging ligands, which is applied in ruthenium organic compounds, chemical instruments and methods, platinum group organic compounds, etc., can solve the problems of rare application of ruthenium-based metal complexes, and achieve stable structure and easy operation Effect
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Embodiment 1
[0025] Embodiment one, the preparation of ruthenium complex
[0026] 1.1 Preparation of Ligand HL:
[0027] Ligand HL was prepared according to the route shown in the following formula:
[0028]
[0029] 150mg pyrazino[2,3-f][1,10]phenanthroline-2-carboxylic acid, 112mg 1,10-phenanthroline-5,6-diamine, and 22g
[0030] Add polyphosphoric acid into a 25mL three-necked bottle, protect it with nitrogen, and stir it mechanically to mix it evenly. First heated to 120°C, then
[0031] Afterwards, the temperature was raised to 190° C. for 7 hours, and the mixture changed from red transparent to dark green. Cool to room temperature under nitrogen protection,
[0032] The resulting viscous liquid was poured into ice water to obtain a light yellow-green precipitate, which was neutralized with ammonia water, and the color of the precipitate deepened. Suction
[0033] The precipitate was collected, washed with water, extracted with methanol, and dried in vacuo to obtain 139 mg (5...
Embodiment 2
[0038] Embodiment two, the influence of pH change on the ultraviolet-visible absorption spectrum and photoluminescence spectrum of the Britton-Roberson (BR) buffer solution of ruthenium complex
[0039] The ultraviolet-visible absorption spectrum was measured on a UV-2600 ultraviolet-visible spectrophotometer, and the BR buffer solution was used as a reference solution during the measurement. Fluorescence emission spectra were measured on a Cary Eclipse fluorescence spectrophotometer. The quantum efficiency of luminescence is obtained by ruthenium terpyridine [Ru(bpy) 3 ] 2+ as a standard (Φ std =0.028), the measured concentration is 1.0×10 -6 mol / L [Ru(bpy) 3 ] 2+ The UV-visible absorption spectrum and emission spectrum of the aqueous solution, read the absorbance A at 468nm of the UV-visible absorption spectrum std and the integrated intensity I of the emission spectrum std , according to formula (1):
[0040] Φ=Φ std (A std / A)(I / I std ) (1)
[0041] Φ and Φ st...
Embodiment 3
[0043] Embodiment three, the mensuration of unknown water sample pH
[0044] Take a certain amount of unknown water sample, add sodium chloride to it to a concentration of 0.1M, and add a quantitative complex to make the concentration 2μM, measure the ultraviolet absorption and emission spectra of the water sample, and calculate the According to the standard curve (Fig. 2(c)) for the luminescence quantum yield, read the pH corresponding to the quantum yield, so as to know the pH of the unknown water sample.
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