Naked eye visual colorimetric method-based probe for detecting nickel ions and preparation method and applications thereof
A technology of nickel ion and detection kit, which is applied in the direction of color/spectral characteristic measurement, color-changing fluorescent materials, chemical instruments and methods, etc., can solve the problems of cumbersome and expensive analysis methods, and achieve good selectivity, simple synthesis route and sensitivity high effect
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Embodiment 1
[0028] Embodiment 1: Synthetic nickel ion probe
[0029] 1) Dissolve 2,4-dihydroxybenzaldehyde (5.52g), N-acetylglycine (4.68g), anhydrous sodium acetate (9.844g) in acetic anhydride (200ml), heat and reflux and stir for four hours. The reaction mixture was poured into ice water (600ml), and a yellow precipitate appeared. The precipitate was then filtered, washed with ice water, and dried under reduced pressure to obtain a yellow solid. The product was further reacted after purification.
[0030] 2) In a certain concentration of hydrochloric acid and ethanol solution (v / v=2:1), 3-acetamido-7-acetoxycoumarin (2.61g) was refluxed and stirred for 2 hours. Then the solution was poured into ice water (80ml), and 30% aqueous sodium hydroxide solution was added to adjust the pH value to 5-6, then the solution was concentrated to 30ml, and the crude product was precipitated and collected. This is followed by recrystallization from ethanol to precipitate 3-amino-7-hydroxycoumarin. ...
Embodiment 2
[0032] Embodiment 2: Preparation and use of nickel ion detection kit
[0033] 1) Dissolve the probes in Example 1 in a mixture of water and ethanol, and configure the concentration to be 10 -3 M solution, as stock solution 2. Phosphate buffer solution with pH 8 was prepared as stock solution 1.
[0034] 2) Dilute stock solution 2 with stock solution 1 to obtain 2×10 -6 For the solution of M, take 5 parts of the solution whose volume is 3ml, respectively add equal volume concentrations of (1) 0×10 -6 M; (2) 0.5×10 -6 M; (3) 2×10 -6 M; (4) 5×10 -6 M; (5) 10×10 -6 M nickel ion solution. Measure the change of its ultraviolet absorbance at 535nm ( figure 2 ), the UV spectrum is used as the nickel ion detection working curve.
[0035] 3) Taking the detection working curve prepared in (2) as a reference, take 2×10 in (2) -6 M solution 3ml, the sample to be tested (the same as the nickel ion solution added in (4) in volume) is added in this stock solution, measure the absor...
Embodiment 3
[0038]Embodiment 3: Preparation and use of nickel ion detection test paper
[0039] Dissolve the probe in 1 in ethanol to prepare a 2mM solution and apply it directly on the surface of the filter paper, dry it and cut it into long strips. Soak in (a) 1×10 -6 M; (b) 1×10 -5 M; (c) 1×10 -4 M; (d) 1×10 -3 M; (e) 0M nickel ion solution for 30 seconds. Take it out and use it as a standard color comparison card.
[0040] The manganese ion detection test paper of the present invention is directly immersed in the sample solution to be tested for 30 seconds. After taking it out, the nickel ion concentration in the actual water sample can be semi-quantitatively measured by visual colorimetry and compared with a standard color card.
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