A kind of fluorescein derivative ultraviolet sensor and the method for detecting nickel ion
An ultraviolet sensor and fluorescein technology, applied in chemical instruments and methods, fluorescence/phosphorescence, color/spectral characteristic measurement, etc., can solve the problems of difficult application of metal ion real-time on-line monitoring, expensive equipment, etc., and achieve low cost and synthetic method Simple, high-yield results
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Embodiment 1
[0039] The preparation method of ultraviolet sensor:
[0040] From the reaction of fluorescein hydrazide and 4-bromo-2-hydroxybenzaldehyde.
[0041] Synthesis of fluorescein hydrazide: take a 100mL three-necked flask, weigh 1.500g (4.5mmol) fluorescein and dissolve it in 30mL of absolute ethanol, stir vigorously at room temperature and slowly add (5mL, hydrazine hydrate content > 98% ). The reaction mixture was then heated to reflux with stirring for 8 h during which time the solution was freed from suspended particles and a clear solution was obtained. After cooling to room temperature, the subsequent solution was poured into 200 mL of water, at which point a yellow precipitate formed immediately and allowed to stand for 2 h. Filter and wash several times with water and ethanol. The crude product was purified by recrystallization from ethanol to afford 1.08 g of off-white solid (70%).
[0042] Synthesis of the target product: take a 100mL three-necked flask, weigh 0.173g ...
Embodiment 2
[0049] The specific method for detecting nickel ions by the fluorescein-like ultraviolet sensor:
[0050] Configuration 5×10 -5 The nickel ion test solution of M, the method for the nickel ion wherein is detected by the fluorescein class ultraviolet sensor synthesized in the application embodiment 1, concrete steps are:
[0051] Step 1: Dissolve the fluorescein-like ultraviolet sensor synthesized in Example 1 in solvent ethanol, and use solvent ethanol to constant volume in a 100ml volumetric flask to obtain a concentration of 1.0×10 -3 Sensor stock solution for M;
[0052] Step 2: Dissolve nickel chloride in solvent ethanol, and use solvent ethanol to set the volume in a 100ml volumetric flask to obtain a concentration of 1.0×10 -2 Nickel ion stock solution of M; the pipetting concentration is 1.0×10 -2 The nickel ion stock solution of M is placed in a 100ml volumetric flask, and the solvent ethanol is used to constant volume to obtain a concentration of 1.0×10 -4 The nic...
Embodiment 3
[0056] Selectivity of FBH UV-Vis absorption spectrum for metal ions:
[0057] ethanol / H at a volume ratio of 9:1 2 In the O system, it is determined that the ultraviolet sensor (FBH) is added to the metal ion Ni 2+ UV-Vis absorption spectra before and after.
[0058] Step 1: Dissolve the reactive dye fluorescent sensor synthesized in Example 1 in solvent ethanol, and use solvent ethanol to set the volume in a 100ml volumetric flask to obtain a concentration of 1.0×10 -3 Sensor stock solution for M;
[0059] Step 2: Dissolve nickel salt in solvent deionized water, use solvent deionized water to set the volume in a 100ml volumetric flask, and obtain a concentration of 1.0×10 -2 Each metal ion stock solution of M;
[0060] Step 3: Pipette 0.05ml respectively to a concentration of 1.0×10 -2 For the nickel ion stock solution of M, add 0.5ml of the sensor stock solution obtained in step 1, and then pipette 1ml of H 2 After the addition of O, use solvent ethanol to make constan...
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