Visual colorimetric fluorine ion sensing test-paper and use thereof
A test method, the technology of fluorine ion, is applied in the direction of analyzing the material through the chemical reaction, and analyzing the material through the observation of the influence of the chemical indicator, which can solve the problems such as difficult detection, and achieve simple discrimination, low price, Facilitate the effect of quality control detection
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Embodiment 1
[0029] Embodiment 1 (synthesis of coordination compound, improved synthetic method of the present invention)
[0030] 0.88 g (1 mmol) of 0.238 g (1.2 mmol) of 2,4-dinitrophenylhydrazine, two (dipyridyl) (4,5-diazafluorenone) ruthenium complexes were added to 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 1 0N 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): ...
Embodiment 2
[0031] Embodiment 2 (selective experiment)
[0032] The acetonitrile solution (5 x 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 fluoride solution, mix the two solutions, and make the concentration of the coordination compound solution be 1 x 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 ( Image 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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