CN102253006A - Rapid mercury detection method based on self-assembly of gold nanorods - Google Patents
Rapid mercury detection method based on self-assembly of gold nanorods Download PDFInfo
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- CN102253006A CN102253006A CN2011100999835A CN201110099983A CN102253006A CN 102253006 A CN102253006 A CN 102253006A CN 2011100999835 A CN2011100999835 A CN 2011100999835A CN 201110099983 A CN201110099983 A CN 201110099983A CN 102253006 A CN102253006 A CN 102253006A
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- gold nanorods
- mercury
- self assembly
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Abstract
The invention discloses a rapid mercury detection method based on self-assembly of gold nanorods. The method of the invention mainly comprises the following steps: a nanorod self-assembly chain with substantially enlarged surface plasma resonance signals is formed through inducing the gold nanorods by phosphates; and a mercuric compound (the mercuric compound comprises inorganic mercuric ions and organic mercury) is reduced to elemental mercury by a strong reductant sodium borohydride to change properties of surface plasmas of the gold nanorods, and the surface plasma signals are enlarged by the nanorod self-assembly chain. So the sensitive and rapid mercury detection method is established. The method of the present invention has the advantages of simple operation, good reappearance, and easy popularization.
Description
Technical field
The invention belongs to a kind of method that detects mercury, be specifically related to a kind of gold nanorods self assembly that phosphate induces of passing through and the surface plasma body resonant vibration signal amplified the method for setting up a kind of sensitivity, fast detecting mercury based on gold nanorods.
Background technology
Mercury is to be present in natural a kind of important meals element, because it has multiple peculiar property, mercury and compound thereof are used very extensive in industrial and agricultural production.But mercury is a kind of chemical substance with serious physiology toxicity, even its concentration is very low, it also is a kind of poisonous and hazardous environmental contaminants.Because it has persistence, easily animal migration and biological concentration highly, makes mercury become one of environmental contaminants at present of greatest concern.Development detects and the method and the material of the removal of mercury are to find and control the important means of polluting.Therefore press for quick, easy, the highly sensitive method of searching and detect mercury.Detection to mercury in the environmental sample mainly is to realize by methods such as atomic absorption spectrum, atomic emission spectrum, atomic fluorescence spectrophotometry, inductivity coupled plasma mass spectrometries at present.Though these methods have very high sensitivity and accuracy, but need large-scale expensive instrument, long analytical cycle, complicated sample pre-treatment process, also than higher, these all make it be difficult to use in the field quick detection of environmental sample to operating personnel's requirement.The novel mercury ion detecting method of other also is being developed in recent years, and with respect to classic method, these methods have simple economy, reach the advantage of high sensitivity fast, but the shortcoming of selective limitation.Therefore and in ecologic environment, the existence of other ions that the mercury of trace invariably accompanies a large amount of develops high sensitivity and has a mercury ion detecting method of high selectivity significant to environment measuring and food safety monitoring.
The gold nanorods diameter is approximately 10-20nm, length is the solid gold right cylinder of 40-200nm.Gold nanorods shows horizontal plasma wave (TPW) and longitudinal plasma wave (LPW), and gold nanorods excites the variation of caused horizontal plasma wave personal attendant transverse width not obvious along the transverse width direction, generally at 520nm.And nanometer rods longitudinal length direction excites the longitudinal plasma wave that causes long, but changes along with the variation of nanometer rods aspect ratio very sensitively, and promptly the longitudinal plasma wave that the nanometer rods of different aspect ratios is corresponding different is long.When gold nanorods carries out the one dimension self assembly (comprise shoulder to shoulder with head meet and discuss dual mode), its surface plasma volume property can change, the self assembly mode that head is met and discussed enlarges markedly the surface plasma signal, thereby can develop the method for highly sensitive detection mercury.
Summary of the invention
The method that provides a kind of character of significantly amplifying by the surface plasma body resonant vibration signal of gold nanorods self assembly chain to come fast detecting mercury is provided at existing above-mentioned defective in the prior art.
Method of the present invention comprises the step of following order:
(1) in the dispersed system of gold nanorods, induce and make it form one dimension gold nanorods self assembly chain by adding phosphate, simultaneously, monitor the surface plasma body resonant vibration wavelength change of gold nanorods self assembly chain in real time at a visible infrared region;
(2) after the curve of spectrum of the surface plasma of gold nanorods self assembly chain is stable, adds strong reductant again, and make the concentration of reductive agent maintain 10
-5Mol/L;
(3) then, add mercurous component to be measured;
(4) the simple substance mercury that restores of strong reductant and gold nanorods form the amalgam compound, thereby change the plasma resonance character of gold nanorods, with the amplification that is changed significantly of its surface plasma body resonant vibration signal, in view of the above, can detect ultratrace mercury in the solution by gold nanorods self assembly chain.
More particularly, described phosphate is sodium phosphate, potassium phosphate, ammonium phosphate, and phosphatic concentration is 10 in the solution
-1～10
-4Mol/L.
The described strong reductant that is used to reduce mercury is a sodium borohydride.
Described dispersed system is a water phase surfactant mixture, comprises cetyltrimethyl ammonium cationoid surfactant, is specially: cetyl trimethyl ammonium bromide, hexadecyldimethyl benzyl ammonium phenyl ammonium bromide, cetyltriethylammonium bromide aqueous solution; Described water phase surfactant mixture concentration is 10
-3～10
-4Between the mol/L scope.
The mercury that detects comprises inorganic mercury ion and organic mercury, and the least concentration that detects mercury ion is 10
-14Mol/L.
The present invention uses the principle that gold nanorods self assembly chain causes that the surface plasma body resonant vibration wavelength significantly amplifies, and the concentration of mercury is detected.When adding the mercury compound of variable concentrations in the solution, under the reductive agent effect, be reduced into simple substance mercury, because simple substance mercury can form amalgam with gold nanorods, the grain size and the aspect ratio of single gold nanorods have been changed, cause the surface plasma signal of nanometer rods to change, and gold nanorods self assembly chain has amplified the sort signal variation, and the concentration by the situation of change of surface plasma signal to mercury detects, and is limited to 10 under detecting
-14Mol/L.
The inventive method is to prepare on the basis of gold nanorods by existing document, and the gold nanorods dispersed system obtains by related reagent and technical finesse, by adding phosphate the surface plasma wave progress row of this nanometer rods self assembly is regulated.Add phosphate in the gold nanorods system, implement monitoring with visible-near-infrared spectrum, by adding gold nanorods and its plasma resonance red shift of wavelength of phosphatic concentration adjustment, thereby obtain stable existence in the gold nanorods self assembly chain of aqueous phase to required wavelength.
The present invention's employing adds the phosphate method makes gold nanorods form the self assembly chain, by reductive agent the mercury compound in the determinand (comprising inorganic mercury and organic mercury) is reduced into simple substance mercury, form the amalgam compound with gold nanorods, significantly change the surface plasma volume property of gold nanorods self assembly chain, thus the unusual mercury compound of sensitive detection ultratrace.Simple to operate, the favorable reproducibility of the inventive method is easy to penetration and promotion.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the gold nanorods self assembly chain that generates in the embodiment of the invention.
Fig. 2 be the gold nanorods in the embodiment of the invention and generate gold nanorods self assembly chain after corresponding local surface plasma resonance spectrogram.
Fig. 3 be in the embodiment of the invention with the mercury effect after the transmission electron microscope picture of gold nanorods self assembly chain.
Fig. 4 is gold nanorods self assembly chain in the embodiment of the invention and the mercury ion (HgCl that detects three kinds of variable concentrations
2) time gold nanorods self assembly chain surface plasma resonance optical spectrum figure.
Fig. 5 is the surface plasma resonance optical spectrum figure that detects the gold nanorods self assembly chain of mercury (methyl mercury) front and back in the embodiment of the invention, wherein, a is for detecting the surface plasma resonance optical spectrum figure of the preceding gold nanorods self assembly chain of mercury, and b is the gold nanorods self assembly chain surface plasma body resonant vibration spectrogram after the mercury effect.
Embodiment
The present invention is described in further detail below in conjunction with drawings and Examples.
Embodiment 1:
At first, the gold nanorods solution of getting 3mL is the dispersed system of gold nanorods, and wherein, the concentration of surfactant cetyl trimethyl ammonium bromide is 10
-3Mol/L.The surface plasma resonance optical spectrum figure of its gold nanorods as shown in Figure 2.Then, in this gold nanorods dispersed system, add 0.lmL sodium radio-phosphate,P-32 solution (concentration is 0.1 mol/L), and implement monitoring with the Visible-to-Near InfaRed absorption spectrum simultaneously, corresponding local surface plasma resonance spectrogram was as shown in Figure 2 after it generated gold nanorods self assembly chain.The transmission electron microscope picture of gold nanorods self assembly chain as shown in Figure 1.Add the sodium borohydride solution (concentration is 0.001 mol/L) of 0.03mL after the surface plasma curve of spectrum is stablized 30 minutes, after 2 minutes, adding ion concentration of mercury more respectively is 10
-5Mol/L, 10
-8Mol/L, 10
-9Inorganic mercury (the HgCl of mol/L
2) sample, implement monitoring with the Visible-to-Near InfaRed absorption spectrum, remarkable blue shift (reducing) takes place as shown in Figure 4 in its surface plasma body resonant vibration wavelength.Fig. 3 be with the mercury effect after the transmission electron microscope picture of gold nanorods self assembly chain.
Embodiment 2:
At first, getting 3mL gold nanorods solution is the dispersed system of gold nanorods, and wherein, the concentration of surfactant cetyl trimethyl ammonium bromide is 10
-3Mol/L.The surface plasma resonance optical spectrum figure of its gold nanorods as shown in Figure 2.Then, in this gold nanorods dispersed system, add 0.lmL sodium radio-phosphate,P-32 solution (concentration is 0.1 mol/L), and implement monitoring with the Visible-to-Near InfaRed absorption spectrum simultaneously, corresponding local surface plasma resonance spectrogram was as shown in Figure 2 after it generated gold nanorods self assembly chain.The transmission electron microscope picture of gold nanorods self assembly chain as shown in Figure 1.The sodium borohydride solution (concentration is 0.001 mol/L) that after the surface plasma curve of spectrum is stablized 30 minutes, adds 0.03mL, after 2 minutes, add organic mercury (methyl mercury) sample again, implement monitoring with the Visible-to-Near InfaRed absorption spectrum, remarkable blue shift (reducing) takes place in its surface plasma body resonant vibration wavelength, as shown in Figure 5.
Claims (5)
1. method based on gold nanorods self assembly fast detecting mercury is characterized in that comprising the step of following order:
(1) in the dispersed system of gold nanorods, induce and make it form one dimension gold nanorods self assembly chain by adding phosphate, simultaneously, monitor the surface plasma body resonant vibration wavelength change of gold nanorods self assembly chain in real time at a visible infrared region;
(2) after the curve of spectrum of the surface plasma of gold nanorods self assembly chain is stable, adds strong reductant again, and make the concentration of reductive agent maintain 10
-5Mol/L;
(3) then, add mercurous component to be measured;
(4) the simple substance mercury that restores of strong reductant and gold nanorods form the amalgam compound, thereby change the plasma resonance character of gold nanorods, with the amplification that is changed significantly of its surface plasma body resonant vibration signal, in view of the above, can detect ultratrace mercury in the solution by gold nanorods self assembly chain.
2. the method based on gold nanorods self assembly fast detecting mercury according to claim 1, it is characterized in that: described phosphate is sodium phosphate, potassium phosphate, ammonium phosphate, phosphatic concentration is 10 in the solution
-1～10
-4Mol/L.
3. the method based on gold nanorods self assembly fast detecting mercury according to claim 1 and 2 is characterized in that: the described strong reductant that is used to reduce mercury is a sodium borohydride.
4. the method based on gold nanorods self assembly fast detecting mercury according to claim 3, it is characterized in that: described dispersed system is a water phase surfactant mixture, comprise cetyltrimethyl ammonium cationoid surfactant, be specially: cetyl trimethyl ammonium bromide, hexadecyldimethyl benzyl ammonium phenyl ammonium bromide, cetyltriethylammonium bromide aqueous solution; Described water phase surfactant mixture concentration is 10
-3～10
-4Between the mol/L scope.
5. the method based on gold nanorods self assembly fast detecting mercury according to claim 4, it is characterized in that: the mercury of detection comprises inorganic mercury ion and organic mercury, the least concentration that detects mercury ion is 10
-14Mol/L.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103008678A (en) * | 2012-10-10 | 2013-04-03 | 南京航空航天大学 | Tetrahydrofuran-induced gold nanorod controllable assembly and preparation method thereof |
| CN103048295A (en) * | 2012-12-19 | 2013-04-17 | 湖南科技大学 | Method for detecting multiple metal ions based on property of localized surface plasmon and application thereof |
| CN106290182A (en) * | 2016-07-18 | 2017-01-04 | 西安交通大学 | The simple and easy method of a kind of gold nanorods self assembly and the application in mercury ion detecting thereof |
| CN107290313A (en) * | 2017-06-12 | 2017-10-24 | 湖南科技大学 | A kind of preparation method and application of the golden copper composite Nano cluster of Two Colour Fluorescence |
| CN107389387A (en) * | 2017-06-26 | 2017-11-24 | 杭州超距科技有限公司 | Portable trace mercury analyzer |
| CN108828047A (en) * | 2018-07-02 | 2018-11-16 | 北京师范大学 | A method of detection Mercury in Water Body ion |
| CN108841378A (en) * | 2018-07-03 | 2018-11-20 | 山东交通学院 | A kind of preparation method and application of functional modification carbon quantum dot |
| CN113984860A (en) * | 2021-10-27 | 2022-01-28 | 合肥工业大学 | Au/MOFs nano composite material and detection method of trace methyl mercury ions |
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| WO2007017689A2 (en) * | 2005-08-09 | 2007-02-15 | Cambridge Enterprise Limited | Nanorod thin-film transistors |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103008678A (en) * | 2012-10-10 | 2013-04-03 | 南京航空航天大学 | Tetrahydrofuran-induced gold nanorod controllable assembly and preparation method thereof |
| CN103008678B (en) * | 2012-10-10 | 2014-12-17 | 南京航空航天大学 | Tetrahydrofuran-induced gold nanorod controllable assembly and preparation method thereof |
| CN103048295A (en) * | 2012-12-19 | 2013-04-17 | 湖南科技大学 | Method for detecting multiple metal ions based on property of localized surface plasmon and application thereof |
| CN103048295B (en) * | 2012-12-19 | 2015-08-19 | 湖南科技大学 | Based on local surface plasma nature examination many kinds of metal ions method and application |
| CN106290182A (en) * | 2016-07-18 | 2017-01-04 | 西安交通大学 | The simple and easy method of a kind of gold nanorods self assembly and the application in mercury ion detecting thereof |
| CN107290313A (en) * | 2017-06-12 | 2017-10-24 | 湖南科技大学 | A kind of preparation method and application of the golden copper composite Nano cluster of Two Colour Fluorescence |
| CN107389387A (en) * | 2017-06-26 | 2017-11-24 | 杭州超距科技有限公司 | Portable trace mercury analyzer |
| CN108828047A (en) * | 2018-07-02 | 2018-11-16 | 北京师范大学 | A method of detection Mercury in Water Body ion |
| CN108841378A (en) * | 2018-07-03 | 2018-11-20 | 山东交通学院 | A kind of preparation method and application of functional modification carbon quantum dot |
| CN108841378B (en) * | 2018-07-03 | 2021-03-09 | 山东交通学院 | Preparation method and application of functionalized modified carbon quantum dots |
| CN113984860A (en) * | 2021-10-27 | 2022-01-28 | 合肥工业大学 | Au/MOFs nano composite material and detection method of trace methyl mercury ions |
| CN113984860B (en) * | 2021-10-27 | 2023-07-18 | 合肥工业大学 | Au/MOFs nanocomposite and detection method of trace methyl mercury ions |
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|---|---|
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