Visual colorimetric fluorine ion sensing test-paper and use thereof
A technology of fluoride ion and test paper, which is applied in the direction of analyzing materials through chemical reactions and observing the influence of chemical indicators on materials. It can solve problems such as difficult detection and achieve simple discrimination and good selective recognition. , Ease of use
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Embodiment 1
[0029] Embodiment 1 (synthesis of coordination compound, improved synthetic method of the present invention)
[0030] 0.238 g (1.2 mmol) of 2,4-dinitrophenylhydrazine, bis(bipyridyl)(4,5-diazafluorenone) ruthenium complex 0.88 g (1 mmol) was added to a 5 ml A mixed solution of phosphoric acid in 25 ml of acetonitrile and 25 ml of ethanol was refluxed for 8 hours in a nitrogen atmosphere, concentrated to 5 ml, and 100 ml of ethanol solution was added to precipitate a brown precipitate, which was filtered and washed three times with ethanol. The precipitate was dissolved in 5 ml of water, and KPF was added 6 A dark black precipitate precipitated out, was filtered off, washed with ethanol and dried in vacuo, with a yield of 60%. Elemental analysis (C 10 h 8 N 2 ) 2 Ru(C 17 h 10 N 6 o 5 )(PF 6 ) 2 Values are C, 41.6; H, 2.6; N, 13.2%, theoretical values are C, 41.7; H, 2.4; N, 13.1%. NMR analysis 1 H NMR (500MHz, CD 3 CN, T-toluene sulfonic acid), δ (ppm): 8.96 (...
Embodiment 2
[0031] Embodiment 2 (selective experiment)
[0032] The acetonitrile solution (5 × 10 -5 M), respectively adding 1 equivalent of F - , 10 equivalents of H 2 PO 4 - , 20 equivalents of Cl - , Br - , I - , HSO 4 - , NO 3 - Tetrabutylamine salt solution, a color change is obtained (attached figure 1 ) and measure the absorption spectrum (attached figure 2 ) and fluorescence spectra (with image 3 ): obvious color change to fluoride ion, 10 times the amount of H 2 PO 4 - There is a certain change, for 20 times the amount of Cl - , Br - , I - , HSO 4 - , NO 3 - No meaningful color change was seen.
Embodiment 3
[0033] Embodiment 3 (color reaction)
[0034] Prepare the acetonitrile solution of the coordination compound of Example 1 and p-toluenesulfonic acid (1: 1), prepare the tetrabutylamine fluorine solution, mix the two solutions, and make the concentration of the coordination compound solution be 1×10 -5 M, the change of fluorine concentration, the measured visible ultraviolet spectrum ( Figure 4 ) and fluorescence spectra ( Figure 5 ). Measure the change of absorbance value at 580nm ( Figure 6 ). The binding constant between the coordination compound of Example 1 and the fluoride ion was calculated by nonlinear least square method as log K=6.71±0.04.
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