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Method for detecting concentration of persulfate ions by using conjugated polyelectrolyte-silver

A technology of conjugated polyelectrolyte and persulfate, which is applied in measuring devices, material analysis through optical means, instruments, etc., can solve the problems of low analysis sensitivity, tedious and time-consuming synthesis process, complex probe synthesis, etc.

Inactive Publication Date: 2018-07-13
HUNAN NORMAL UNIVERSITY
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Problems solved by technology

However, the above technical process is cumbersome and requires high equipment. The analysis process is time-consuming and laborious, and the analysis sensitivity is not high, which is not conducive to the actual production and monitoring applications that usually contain lower concentrations of persulfate.
[0004] Fluorescence detection has the characteristics of simplicity, rapidity, sensitivity, and no labeling, and has been widely used in bisulfite ions or sulfite ions (CN106496197A), sulfide ions (CN103323440A, CN102004100A, CN106442448A), thiosulfate ions (CN106770103A) etc., but the synthesis of its probes is complicated, and the probes often have certain toxicity to cells or organisms, the detection process is complicated and time-consuming, and the synthesis method is not easy to master
Conjugated polymers are a new type of high-sensitivity fluorescent sensing detection platform. Patents have been reported for fluoride ions (CN105295009A), copper ions (CN101824139A), ATP (CN105348493A) and BSA (CN103588960A) and other biomolecules and cells ( CN105348493A), etc., however, most of the conjugated polymer probes can only be dissolved in organic solvents, have poor water solubility, and the synthesis process is cumbersome and time-consuming

Method used

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  • Method for detecting concentration of persulfate ions by using conjugated polyelectrolyte-silver

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preparation example Construction

[0087] The preparation method reference example 10 of silver nanosheet solution

[0088] Under the condition of avoiding light at room temperature, add 1.5 mL, 30 mmol / L trisodium citrate solution, 1.5 mL, 0.7 mmol / L (K-30, M w ~29000 g / mol) polyvinylpyrrolidone solution and 60 μL 30% hydrogen peroxide solution (the mass ratio of silver nitrate, trisodium citrate, polyvinylpyrrolidone and hydrogen peroxide is 1: 31: 72: 160) , after mixing and stirring evenly, quickly add 250 μL, 100 mmol / L sodium borohydride sodium borohydride solution at one time, stir and react rapidly for 30 min, the solution turns from yellow to deep yellow and finally to deep purple, and it is ready.

[0089] After testing, the concentration of silver nanosheets was 1×10 -4 mol / L, the particle size of the silver nanosheets is less than or equal to 50 nm, and the wavelength is 551 nm after being measured by an ultraviolet spectrophotometer.

[0090] Reference example 11 for the preparation method of buff...

Embodiment 1～5

[0093] (1) Mix 30μL, 40μL, 50μL, 60μL, 70μL, 1×10 -4 mol / L aqueous solution of conjugated polyelectrolyte reference example 1 with 50 μL, 1×10 -4 mol / L of the silver nanosheet solution obtained in Reference Example 10 and 500 μL of the buffer solution obtained in Reference Example 11 were dissolved in water, added water to make up to 1 mL, and stirred for 10 minutes to obtain homogeneous systems 1 to 5, respectively, and measure the fluorescence intensity F 0 ;

[0094] (2) Add the solution containing the persulfate ion to be tested (theoretical concentration is 9×10 -5 mol / L), after stirring for 30 min, the fluorescence intensity F was measured respectively;

[0095] (3) Calculate Y=(F 0 -F) / F 0 =0.877, 0.898, 0.912, 0.913, 0.912, and then express the relationship between persulfate ion and fluorescence intensity Y=0.526×log C (S 2 o 8 2- )+3.044, R=0.955, respectively get persulfate ion concentration=7.58×10 -5 , 8.3×10 -5 , 8.91×10 -5 , 8.92×10 -5 , 8.91×10 ...

Embodiment 6～9

[0102] (1) Dispense 50 μL, 1×10 -4 mol / L aqueous solution of conjugated polyelectrolyte reference example 2, respectively mixed with 25 μL, 50 μL, 75 μL, 100 μL, 1×10 -4 mol / L of the silver nanosheet solution obtained in Reference Example 10 and 500 μL of the buffer solution obtained in Reference Example 11 were dissolved in water, added water to make up to 1 mL, and stirred for 10 minutes to obtain homogeneous systems 6 to 9, respectively, and measure their fluorescence intensity F 0 ;

[0103] (2) In the homogeneous system 6-9 obtained in step (1), respectively, add the solution containing the persulfate ion to be tested (theoretical concentration is 8×10 -5 mol / L), after stirring for 30 min, the fluorescence intensity F was measured respectively;

[0104] (3) Calculate Y=(F 0 -F) / F 0 =0.842, 0.876, 0.856, 0.839, and then express the relationship between persulfate ion and fluorescence intensity Y=0.526×log C (S 2 o 8 2- )+3.044, R=0.955, respectively get persulfa...

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Abstract

The invention discloses a method for detecting the concentration of persulfate ions by using conjugated polyelectrolyte-silver. The method comprises the following steps of: (1) dissolving conjugated-polyelectrolyte aqueous solution, nanosilver solution and buffering solution in water, after stirring for reaction, obtaining a homogeneous system and measuring fluorescence intensity F0 of the homogeneous system; (2) adding solution containing persulfate ions to be detected into the homogeneous system obtained in the step (1), and after stirring for reaction, measuring fluorescence intensity F ofthe homogeneous system; (3) calculating Y according to a formula Y=(F0-F) / F0, and then obtaining the concentration of the persulfate ions according to a formula expressing the relation between the persulfate ions and the fluorescence intensity, namely Y=0.526*logC(S2O8<2->)+3.044, R=0.955. The method disclosed by the invention is simple and easy in implementation, accurate and rapid, good in selectivity and high in sensitivity, the lowest detection limit is 9*10<-7>mol / L, and the detection linearity in the range of 1*10<-6> to 9*10<-5>mol / L is good.

Description

technical field [0001] The invention relates to a method for detecting the concentration of persulfate ions, in particular to a method for detecting the concentration of persulfate ions by using conjugated polyelectrolyte-silver. Background technique [0002] Persulfate has strong oxidizing properties and has been widely used in many aspects such as water and soil decontamination, circuit board manufacturing, cosmetics and polymerization. For example, ammonium persulfate is an excellent initiator for water-based adhesive synthesis. Water-based adhesives are an important raw material commonly used to bond cigarettes and filters. As an important part of cigarettes, the composition of water-based adhesives is also one of the key factors affecting the quality and grade of cigarettes. Therefore, methods for detecting harmful chemicals in water-based adhesives have been paid more and more attention. Common chemicals in water-based adhesives such as ammonium persulfate can harm ...

Claims

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Application Information

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IPC IPC(8): G01N21/64C08G61/12
CPCC08G61/122C08G2261/124C08G2261/146C08G2261/18C08G2261/3142C08G2261/3221C08G2261/3328C08G2261/413C08G2261/522C08G2261/64G01N21/643
Inventor 黄红梅肖毅史慧珍杜慧凤何晓晓张友玉
Owner HUNAN NORMAL UNIVERSITY
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