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Mercury ion fluorescent color-developing agent and detecting method

A compound, mercury ion technology, applied in the field of mercury ion fluorescent coloration compounds and mercury ion detection and test paper, can solve the problems of low fluorescence yield, lack of detection metals, lack of water solubility of color reagents, etc. The effect of high selectivity and good selective recognition

Inactive Publication Date: 2010-05-19
南京金霸环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the systems that have been developed encounter difficulties in practical application due to the lack of water solubility of chromogenic reagents, lack of high selectivity for detecting metals, and low fluorescence yield.

Method used

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  • Mercury ion fluorescent color-developing agent and detecting method
  • Mercury ion fluorescent color-developing agent and detecting method
  • Mercury ion fluorescent color-developing agent and detecting method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1 (the synthesis of compound RFc)

[0029] Add 0.428 g of rhodamine-6G hydrazine compound (1 mmol), 0.214 g of ferrocene monoaldehyde (1 mmol), and 3 drops of glacial acetic acid into 30 ml of ethanol, reflux for 120 minutes, cool to room temperature, and collect the light yellow precipitate by filtration , washed with water, methanol, and anhydrous ether for several times. Vacuum dry. Yield: 0.547g, 87.5%. Elemental analysis calculated value RFc (C 37 h 36 N 4 o 2 Fe): H 5.81%, C 71.13%, N 8.97%. Analytical values: H 5.83%, C 71.22%, N 8.98%; ESI-MS: m / z 625.4, assigned to [RFc+H] + Ion peak (calculated as [RFc+H] + =625.2. 1 H NMR (DMSO-d6) H8.041 (1H, s), 7.877 (1H, d, J = 7.0Hz), 7.568 (1H, t, J = 15.0Hz), 7.521 (1H, t, J = 15.0Hz ), 6.978(1H, d, J=6.5Hz), 6.372(1H, s), 6.215(1H, s), 4.358(2H, s), 4.315(2H, s), 3.825(5H, s), 3.161 (4H, m, J = 182Hz), 1.851 (6H, s), 1.174 (6H, t, J = 25.5Hz); IR (solid KBr): 2360.4(s), 1705.2(s), 1620.03(m), 1619...

Embodiment 2

[0030] Embodiment 2 (selective experiment)

[0031] Formulate compound RFc into 1×10 -5 M aqueous solution stock solution, with metal ion salts (Li(I), Na(I), K(I), Ag(I), Mg(II), Ca(II), Cu(II), Ba(II), Perchlorates of Pb(II), Mn(II), Co(II), Ni(II), Cd(II), Zn(II), Hg(II), Fe(II) sulfates), new Prepare metal ion stock solution (concentration 10 -2 M) for experiments. In the test experiment, take compound RFc stock solution 2mL, and take other metal ion solutions so that Na in the final solution + , K + , Ca 2+ and Mg 2+ The ion is 125 times that of compound RFc, Hg 2+ Ions are 25 times that of compound RFc, and other metal ions are 50 times that of compound RFc, adjust the concentration for testing, excite at 500nm, and measure the fluorescence spectrum. see attached results image 3 .

Embodiment 3

[0032] Embodiment 3 (high concentration fluorescence titration working curve)

[0033] Take by weighing the compound RFc 0.0624 gram of embodiment 1, be dissolved in the N, N-dimethylformamide (DMF) of 100mL, obtain 10 -3 M's solution. Use a pipette to pipette 1 mL of the above solution, dilute to 100 mL with double distilled water in a volumetric flask, and prepare 1×10 -5 M stock solution (L1). Weigh 0.0203 g of perchloric acid perchlorate hexahydrate, dissolve in water, and prepare 4.0×10 with a 10ML volumetric flask -3 M standard stock solution (F1). Measure 12.0 ml of RFc stock solution L, add the calculated amount of mercury ion stock solution F1, prepare a standard test solution, excite at 500nm, and test its fluorescence intensity at 550nm. The test results are attached Figure 4 . Calculate the compound RFc of embodiment 1 and the binding constant of mercury ion with nonlinear least square method to be K=2.15×10 4 m -1 .

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Abstract

The compound thereof is ferrocenyl replacing rhodmine-6G. Said compound can be used to detect the mercury ion in highly selectivity; when the mercury concentration is lower than 2ppb, it also can be detected by the invention; other ions such as Pb2+,Ag+,Fe2+,Zn2+,Cd2+,Mn2+,Co2+,Ni2+ and Cu2+ have no interference.

Description

technical field [0001] The invention belongs to the technical field of recognition, combination and detection of mercury cations for optical detection, and specifically relates to a rhodamine compound with a ferrocenyl group, and uses the compound as a mercury ion fluorescence detection method for recognition and color development, as well as for the recognition and color development of mercury Ion test strips. Background technique [0002] Due to the high toxicity of mercury ions and their salts, they are widely used in industry and widely distributed in the environment (Boening, D.W.Chemosphere, 2000, 40, 1335-1351), in recent years, scientists and technicians have devoted themselves to the development of highly selective, efficient and feasible Mercury ion chemical detection methods, especially those based on fluorescence, visible ultraviolet absorption, discoloration and other physical property changes, have achieved positive results. However, most of the systems that h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/76C09K11/06
Inventor 吴大雨黄薇白志平段春迎
Owner 南京金霸环保科技有限公司