A method for f‑colorimetric detection
A technology of colorimetry and molar ratio, applied in color/spectral characteristic measurement, fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of slow recognition and complex structure, and achieve the effect of simple method, mild reaction conditions and easy operation
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Embodiment 1
[0032] Synthesis of square amide compound 1
[0033] Add 220.0 mg of phthalaldehyde and 361.3 mg of hydroxylamine hydrochloride in a reaction vessel with water as a solvent, then add 5% mol of Ru and 436.9 mg of sodium bicarbonate as a catalyst, heat the oil bath to 100 ° C and stir at a constant temperature After 24 hours, 196.8 mg of phthalamide was obtained with a yield of 60%.
[0034] Add 91.1mg of phthalamide and 40.0mg of zinc trifluoromethanesulfonate to a mixed solvent containing toluene and N,N-dimethylformamide (volume ratio 19 / 1), stir well to dissolve, then add 81.3μL Diethyl squarylate was heated to 100°C in an oil bath and stirred at constant temperature for 12 hours to obtain a reddish-brown precipitate. After the reaction was completed, the system was cooled to room temperature, filtered with suction and washed with toluene, and the obtained reddish-brown precipitate was the target product. After drying and weighing, 127.5 mg of the product was obtained, and...
Embodiment 2
[0041] Using artificially prepared samples containing fluoride ions, its F - content of 10 -5 ,2×10 -5 , 4×10 -5 , 10 -4 , 2×10 -4. Gather ultraviolet absorption spectrum after fully stirring evenly, adopt detection method of the present invention to the F of above-mentioned sample - The content was tested, and the test results are shown in the table below.
[0042] Table 1: Samples using squaramide derivatives 1 vs. F - Quantitative identification detection of
[0043] sample
[0044] Theoretical content
[0045] As can be seen from the results shown in table 1, adopt the inventive method to F - The actual detection value obtained by testing the content is basically the same as the content value added when making the sample, with a small error range.
Embodiment 3
[0047] Configure several vials with a concentration of 5×10 -5 mol / L square amide solution, adding concentration of 5 × 10 -4 mol / L of the following ion solution: F - , Cl - 、Br - , I - 、PF 6 - , SO 4 2- , NO 3 - and NO 2 - , after shaking each vial of solution slightly, we can observe the addition of F - The square amide of the solution immediately changed from light yellow to orange, and the others had no obvious phenomenon (such as Figure 4 ). Show thus, adopt the present invention's selectivity to F - to test.
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