CN102087222B - Method for specifically detecting divalent mercury ions - Google Patents
Method for specifically detecting divalent mercury ions Download PDFInfo
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- CN102087222B CN102087222B CN201110047567A CN201110047567A CN102087222B CN 102087222 B CN102087222 B CN 102087222B CN 201110047567 A CN201110047567 A CN 201110047567A CN 201110047567 A CN201110047567 A CN 201110047567A CN 102087222 B CN102087222 B CN 102087222B
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Abstract
The invention discloses a method for specifically detecting divalent mercury ions. The method comprises the following steps: 1) preparing gold nano solution; 2) mixing the sample to be detected with melamine solution; and 3) detecting the sample to be detected. Specific and rapid detection of the mercury ions in the sample is realized by adopting the method. Compared with the traditional methods, the method disclosed by the invention has the following advantages: not only does the method have higher sensitivity and specificity, but also the detection time is short, the sample is simple to process, and visual convenient analysis of the mercury ions in the sample can be realized without using any instrument.
Description
Technical field
The present invention relates to a kind of new method of easy, quick, specific detection dimercurion.
Background technology
Mercury is a kind of common toxic heavy metal, mainly with dimercurion (Hg
2+) the form existence, can both produce great harm to human beings'health and environment.Mercury ion shows very strong affinity to also having the ligand of sulphur atom in the human body on the one hand, can cause that the sulfydryl of protein, enzyme and film combines; Mercury ion can be deposited on human body brain, liver, etc. in the organ, produce slow poisoning, infringement kidney, brain, stomach and enteron aisle, even cause death, the serious physiology toxicity that therefore has.On the other hand, mercury ion has lasting contaminative, is prone to the biological concentration property of animal migration and height, and it can be accumulated in environment, in human body, causes the human body various diseases through food chain transport.In addition, mercury and mercury salt thereof being widely used in industry caused spreading unchecked of mercury pollution more.Therefore the detection for mercury pollution becomes environmental monitoring protection major issue day by day, and development of new mercury ion detecting new method is significant for environmental protection, prevention from suffering from the diseases, great environmental pollution monitoring.
The most widely used at present detection mercury technology is atomic absorption spectrum and atomic emission spectrum.In addition, some other method such as neutron activation analysis method, anodic stripping voltammetry, x ray fluorescence spectrometry, plasma induction spectrum, dithizone colorimetric method and measure methods such as suspension method and bio-sensing with nephelometer and also be applied in the mercury ion detecting.These method general costs are higher, need complicated instrument and skilled operating personnel, can not or inconvenience use out of doors; Generally carry out in the laboratory, exist consuming timely, analytical procedure is complicated; Analytical instrument is expensive, and the low and sample of SF is difficult for shortcomings such as preservation.In some cases, need the environmental pollution situation in time to understand so that formulate corresponding treatment Countermeasures rapidly, therefore develop a kind of simple, fast, the specific detection metal mercury ions method important that seems.The method that the present invention uses has realized simply, quick, specific detection mercury ion.
Summary of the invention
The method that the purpose of this invention is to provide a kind of easy, quick, specific detection dimercurion.
A kind of specific detection dimercurion method may further comprise the steps:
Prepare gold nano solution respectively, melamine solution, the dimercurion solution of various normal concentrations (0,0.5,1,2,5,8,10,50mg/L); Earlier melamine solution is mixed with the dimercurion solution of various normal concentrations respectively, gold nano solution is added respectively in the various mixed solutions again, change color is observed in reaction, and uv-spectrophotometric instrument detecting signal, the production standard curve; Testing sample adds the gold nano solution reaction again with after melamine solution is mixed, and detects to obtain the result.
The compound method of described gold nano solution: add 1.5mL 100mM gold chloride in the 148.5mL water, be heated with stirring to adverse current, add the sodium citrate of 15mL 38.8mM fast, continue heating 20min, stop heated and stirred to room temperature and get final product.
Prepare the dimercurion standard solution of various concentration respectively, the dimercurion solution of each concentration is mixed with volume ratio with 5 μ M melamine solution respectively at 1: 1.Dimercurion solution is with after melamine solution is mixed; Shook two minutes with whirlpool mixed instrument point, left standstill 1 hour.
Get 90 μ L gold nano solution and add the dimercurion of the various concentration of 10 μ L and the mixed solution of melamine respectively; Fully mixing left standstill under the room temperature 20 minutes, observed change in color; Solution dilution to 700 μ L, and is changed with uv-spectrophotometric instrument detecting signal.
Melamine has outstanding electron-donating group, and it attracts with the electrostatic interaction of passing through between the gold nano through amino mutually, makes gold nano generation coagulation, and color changes blueness into by redness.Simultaneously, amino also can with mercury ion generation complex reaction.After melamine and mercury ion generation complex reaction, its amino is occupied by mercury ion, and melamine is not combined with gold nano, and coagulation does not take place gold nano, and color does not change.Through the contrast of color, to reach purpose quick, the specific detection mercury ion.
Through this method, realized mercury ion specificity, the fast detecting in the sample.This method is compared with classic method, not only has higher sensitivity and specificity; Simultaneously; Detection time is short, sample preparation is simple; Mercury ion carries out visual convenient analysis under not using any instrument condition, just can realizing sample, can detect the mercury ion of 1mg/L through ultraviolet-visible pectrophotometer, and visual detection can detect the mercury ion of 5mg/L.
Description of drawings
Fig. 1 is the principle key diagram of the inventive method;
Fig. 2 detects step for the inventive method;
The different ion concentration of mercury photos that Fig. 3 detects for the present invention;
Fig. 4 quantitatively schemes for the different ion concentration of mercury that the present invention detects;
Fig. 5 is for detecting other metallic ion photos of 10mg/L with step of the present invention;
Fig. 6 quantitatively schemes for the different heavy metal ion of 10mg/L that the present invention detects;
Fig. 7 confirms figure for melamine optium concentration of the present invention.
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
1) prepare gold nano:
148.5mL add 1.5mL 100mM gold chloride in the water, be heated with stirring to adverse current, add the sodium citrate of 15mL 38.8mM fast, continue heating 20min, stop heated and stirred to room temperature and get final product;
2) confirming of melamine optium concentration:
0 μ M, 1 μ M, 2 μ M, 4 μ M, 5 μ M, 8 μ M melamines add 90 μ L AuNPs solution respectively, react two minutes, observe change color, and uv-spectrophotometric instrument detecting signal changes.
3) testing sample detects:
The mercury ion of variable concentrations 0,0.5,1,2,5,8,10,50mg/L, the reaction of 5 μ M melamine solution was shaken two minutes with the miniature whirlpool mixed instrument point of WH-2, left standstill 1 hour.
Get 90 μ L AuNPs solution and add the above-mentioned mixed solution of 10 μ L respectively; With the abundant mixing of liquid-transfering gun, left standstill under the room temperature 20 minutes, observe change in color; Solution dilution is changed to 700 μ L and with uv-spectrophotometric instrument detecting signal, and calculate the lowest detection line.
Prepare Cd, Cr, Fe, Ni, Pb, the Hg ion of 20mg/L respectively, each ion and the melamine solution of 20mg/L are mixed at 1: 1, shook two minutes, left standstill 1 hour with the miniature whirlpool mixed instrument point of WH-2.Get 84 μ L AuNPs solution and add the above-mentioned solution of 16 μ L respectively, with the abundant mixing of liquid-transfering gun, left standstill under the room temperature 20 minutes, observe change in color, deionized water is diluted to 700 μ L, and change in detection signal.Detecting wavelength ratio is A520/A650.
Test result analysis
A, ion concentration of mercury influence
Along with the increase of ion concentration of mercury, more mercury ions and melamine reaction, the free melamine molecule that exists is fewer and feweri, and the gold nano aggregation extent that is caused by melamine reduces, and the gold nano color becomes redness (like Fig. 3,4) by blueness.
B, selectivity are probed into
Through this method, detected other metallic ions, discovering only has mercury ion can produce obvious detection signal, explains that this method has than high specific (seeing Fig. 5,6).
Claims (5)
1. the method for a specific detection dimercurion is characterized in that, prepares gold nano solution respectively, melamine solution, the dimercurion solution of various normal concentrations; Earlier melamine solution is mixed with the dimercurion solution of various normal concentrations respectively, gold nano solution is added respectively in the various mixed solutions again, change color is observed in reaction, and uv-spectrophotometric instrument detecting signal, the production standard curve; Testing sample adds the gold nano solution reaction again with after melamine solution is mixed, and detects to obtain the result.
2. the method for specific detection dimercurion according to claim 1 is characterized in that,
The compound method of described gold nano solution: add 1.5mL 100mM gold chloride in the 148.5mL water, be heated with stirring to adverse current, add the sodium citrate of 15mL 38.8mM fast, continue heating 20min, stop heated and stirred to room temperature and get final product.
3. the method for specific detection dimercurion according to claim 1 is characterized in that,
Prepare 0,0.5,1,2,5,8,10 respectively, the dimercurion standard solution of 50mg/L, the dimercurion solution of each concentration is mixed with volume ratio with 5 μ M melamine solution respectively at 1: 1.
4. the method for specific detection dimercurion according to claim 3 is characterized in that,
Dimercurion solution is with after melamine solution is mixed; Shook two minutes with whirlpool mixed instrument point, left standstill 1 hour.
5. according to the method for claim 1 or 2 or 4 described specific detection dimercurions; It is characterized in that, get 90 μ L gold nano solution and add the dimercurion of the various concentration of 10 μ L and the mixed solution of 5 μ M melamines respectively, fully mixing; Left standstill under the room temperature 20 minutes; Observe change in color, solution dilution to 700 μ L, and is changed with uv-spectrophotometric instrument detecting signal.
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| CN103163095A (en) * | 2013-03-25 | 2013-06-19 | 江南大学 | Visual multifunctional detection method based on nano-silver |
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| CN106932390A (en) * | 2017-03-28 | 2017-07-07 | 桂林理工大学 | Hg based on analyte catalytic polymerization2+Colorimetric detection method |
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| US20080081376A1 (en) * | 2006-08-24 | 2008-04-03 | University Of Central Florida Research Foundation, Inc. | Mercury sensor using anisotropic gold nanoparticles and related water remediation |
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| WO2010016803A1 (en) * | 2008-08-05 | 2010-02-11 | Agency For Science, Technology And Research | Methods, compositions, and articles comprising stabilized gold nanoclusters |
| CN101726473A (en) * | 2009-10-29 | 2010-06-09 | 广西师范大学 | Method of catalytic resonance scattering spectral determination of mercury by using aptamer modified nanogold |
| CN101776608A (en) * | 2009-10-29 | 2010-07-14 | 广西师范大学 | Method for measuring trace Hg2+ by using aptamer modified nano gold rhenium catalysis-tellurium particle resonance scattering spectrum |
| CN101750442A (en) * | 2009-12-11 | 2010-06-23 | 华中师范大学 | Monodispersive bimetal Au/Pt nano-particle modified electrode for detecting mercury in water and preparation method thereof |
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| CN103163095A (en) * | 2013-03-25 | 2013-06-19 | 江南大学 | Visual multifunctional detection method based on nano-silver |
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Inventor after: Luo Shenglian Inventor after: Chen Zhang Inventor after: He Yejuan Inventor after: Lin Chan Inventor after: Xi Qiang Inventor after: Tang Yanhong Inventor after: Liu Chengbin Inventor after: Cai Qingyun Inventor before: Luo Shenglian Inventor before: He Yejuan Inventor before: Chen Zhang Inventor before: Xi Qiang Inventor before: Liu Chengbin Inventor before: Cai Qingyun |
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Free format text: CORRECT: INVENTOR; FROM: LUO SHENGLIAN HE YEJUAN CHEN ZHANG XI QIANG LIU CHENGBIN CAI QINGYUN TO: LUO SHENGLIAN CHEN ZHANG HE YEJUAN LIN CHAN XI QIANG TANG YANHONG LIU CHENGBIN CAI QINGYUN |
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