CN102374986A - Method for detecting mercury ions by using surface modified gold nano particles - Google Patents
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- CN102374986A CN102374986A CN201010253948XA CN201010253948A CN102374986A CN 102374986 A CN102374986 A CN 102374986A CN 201010253948X A CN201010253948X A CN 201010253948XA CN 201010253948 A CN201010253948 A CN 201010253948A CN 102374986 A CN102374986 A CN 102374986A
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Abstract
The invention provides a method for detecting mercury ions by using surface modified gold nano particles, comprising the following steps: mixing a detection reagent with an aqueous solution to be detected, adjusting the pH value of the mixed solution to let the detection system to be acidic, and determining where mercury ions exist in the aqueous solution according to the color change of the aqueous solution, wherein, a solution of gold nano particles with surface modified by 11-sulfydrl-1-trimethyl ammonium is used as the detection reagent. Sunlight can be added for auxiliary irradiation to increase the sensitivity of the detection. The method has high sensitivity, excellent selectivity, visual reading form, and no need of any large-scale devices. The invention can be used for detecting drinking water.
Description
Technical field
The invention belongs to the mercury ion detecting field, relate in particular to a kind of method of utilizing the next visual detection mercury ion of gold nano grain of surface modification.
Background technology
Mercury ion all has very big harm as a kind of common heavy metal ion to human body and environment.The technology that is used for mercury ion detecting at present mainly contains: utilize organic molecule 1.; 2. galvanochemistry; 3. inductivity coupled plasma mass spectrometry (ICP-MS); 4. atomic absorption spectrum (AA); 5. based on the visual detection of gold nano grain.Wherein, utilize the organic molecule detection mainly to comprise and utilize organic dyestuff and fluorescence molecule to detect, organic dyestuff causes utilizing the sensitivity of organic dyestuff detection mercury ion not high because of its lower molar absorption coefficient.Utilize fluorescence molecule to detect mercury ion and need use expensive luminaire.Electrochemical Detection, ICP-MS and AA also all need expensive instrument, and complex operation.The nanometer technology of fast development; For the detection of metallic ion brings opportunity; Because gold nano grain has very high molar absorption coefficient, higher more than 1000 times than organic molecule usually, so the visual detection metallic ion of utilization gold nano grain possesses higher sensitivity usually.
At present; The technology that the utilization gold nano grain detects mercury ion is a lot, is included in the DNA that the gold nano grain finishing contains thymine, and thymine can combine with the mercury ion specificity; Thereby cause nanoparticle aggregate, [1-4] is said like hereinafter listed non-patent literature.The shortcoming of this method is that DNA costs an arm and a leg, and instability is prone to degraded, and preservation condition is harsh, need be through control external condition like the control temperature or add specific enzyme, thus accurately control the binding ability of DNA and mercury ion.And detection sensitivity is not high enough, generally more than 100nM (every liter of nanomole).Detection speed is slower in addition, needs a few minutes to dozens of minutes usually.
Another kind method is the mercaptan that contains the carboxyl ending in the gold nano grain finishing, and is of hereinafter listed non-patent literature 5, forms compound through mercury ion and carboxyl chelating, thereby causes nanoparticle aggregate.The shortcoming of this method be carboxyl can also with other metallic ions such as cadmium ion, lead ion chelating, so selectivity is bad, need adds screening agent and could improve selectivity.
Non-patent literature described in the preceding text:
1.J.S.Lee，M.S.Han，C.A.Mirkin，Angew.Chem.Int.Ed.，2007，46，4093.Colorimetric?Detection?of?Mercuric?Ion(Hg
2+)in?Aqueous?Media?using?DNA-Functionalized?Gold?Nanoparticles.
2.D.Li，A.Wieckowska，I.Willner，Angew.Chem.Int.Ed.，2008，47，927.Optical?Analysis?of?Hg
2+?Ions?by?Oligonucleotide-Gold-Nanoparticle?Hybrids?and?DNA-Based?Machines.
3.J.Liu，Y.Lu，J.Am.Chem.Soc.，2003，125，6642.A?Colorimetric?Lead?Biosensor?Using?DNA?zyme-Directed?Assembly?of?Gold?Nanoparticles.
4.X.Xue，F.Wang，X.Liu，J.Am.Chem.Soc.，2008，130，3244.One-step，room?temperature，colorimetric?detection?of?mercury?(Hg
2+)using?DNA/nanoparticle?conjugates.
5.C.C.Huang，H.T.Chang，Chem.Commun.，2007，1215.Parameters?for?selective?colorimetric?sensing?of?mercury(II)?in?aqueous?solutions?using?mercaptopropionic?acid-modified?gold?nanoparticles.
Summary of the invention
The objective of the invention is to overcome the defective of above-mentioned prior art, provide a kind of highly sensitive, selectivity good, cost is low and detect the method for mercury ion in the water efficiently.
For achieving the above object; The present invention provides a kind of gold nano grain that utilizes surface modification to detect the method for mercury ion, utilize the surface by the solution of the gold nano grain of 11-sulfydryl-1-trimethyl ammonium modification as detectable, with this detectable and aqueous solution to be measured; And to make mixed solution be acid; Judge through WS change in color whether mercury ion exists in the WS,, have mercury ion to exist in the WS then to be measured if the color of mixed solution becomes purple or blue by redness; If the color no change of mixed solution, no mercury ion exists in the WS then to be measured.
According to method provided by the present invention, wherein, judge through WS change in color whether mercury ion exists in the WS again with above-mentioned detectable and aqueous solution to be measured and irradiation under sunshine.
According to method provided by the present invention, wherein the diameter of gold nano grain is about 13nm (nanometer).
According to method provided by the present invention, wherein the preferred pH value of above-mentioned mixed solution is 1～2.5, and more preferably the pH value is 1.
The form of reading of the present invention is visual, need not rely on any large-scale instrument, and is simple, and fast, cost is low, has outstanding selectivity, and is highly sensitive, and institute can detected ion concentration of mercury scope be 3 * 10
-8M～1 * 10
-2M (every liter of mole), whether the mercury ion content that can be used for detecting in the potable water exceeds standard.
Description of drawings
Followingly the embodiment of the invention is described further with reference to accompanying drawing, wherein:
Fig. 1. the gold nano grain that mercury ion causes is assembled synoptic diagram.
Fig. 2. the TEM photo after gold nano grain is assembled among the present invention.
Fig. 3. the absorbance of gold nano grain in acid (a) and alkalescence (b) environment.
Fig. 4. the relation of minimal detectable concentration and pH value.
Fig. 5. the solution absorbency that ion concentration of mercury is different.
Fig. 6. the TEM of the gold nano grain that is synthesized (transmission electron microscope) photo, size is about 13 nanometers.
Fig. 7. under the sunshine subsidiary conditions, the absorbance of variable concentrations mercury ion.
Fig. 8. the different metal ion solution is at the absorbance changing value at 520nm place.
Embodiment
In order to prove the validity of this method in mercury ion detecting, in following examples, utilize the known WS to be measured of ion concentration of mercury to detect.In addition, utilize ultraviolet-visible spectrophotometer to measure the accumulation process of gold nano grain, naked eyes are detected the science and accurate evidence more of providing.
Embodiment 1.
A practical implementation step according to mercury ion detecting method provided by the invention comprises:
1) prepare the WS to be measured, the ion concentration of mercury of this WS to be measured is that 1 μ M (every liter of micromole), pH value are 1.
2) solution that utilizes the gold nano grain that the surface modified by 11-sulfydryl-1-trimethyl ammonium is as detectable; With volume is that 5 μ L, gold nano grain concentration are that this kind detectable of 150nM joins in the WS acid to be measured that volume is 495 μ L; Form mixed solution; Make that the ultimate density of gold nano grain is 1.5nM, the concentration of mercury ion does not change basically.
3) solution colour becomes blueness by redness rapidly, shows that gathering has taken place gold nano grain, and after 8 hours, the gold nano grain after the gathering forms black precipitate at the bottom of bottle, and supernatant is the colourless WS.
According to method provided by the invention, the detectable that present embodiment is used is to utilize 11-sulfydryl-1-trimethyl ammonium to modify gold nano grain surface as ligand molecular and form.With 11-sulfydryl-1-trimethyl ammonium on the surface chemical modification of gold nano grain, sulfydryl is covalently bound through gold-sulfide linkage and gold surface, and trimethyl ammonium then is exposed to the outermost layer (showing like Fig. 1) of gold nano grain.The gold nano grain of this functionalization can be dispersed in the WS, makes the WS show red.Because mercury ion and sulfydryl have very strong binding ability; In sour environment; Electrostatic repulsion forces between trimethyl ammonium, the hydrogen ion in the sour environment and the mercury ion three of ligand molecular end; Make and can impel the motion aggravation of mercury ion in solution mercury ion to combine, thereby ligand molecular is replaced (see figure 1) from the gold nano grain surface with the sulfydryl of gold surface.The minimizing of gold nano grain surface ligand molecule can cause gold nano grain to assemble (Fig. 2), and the WS color after the gathering is rendered as purple or blueness.Whether change to judge whether mercury ion exists in the WS through WS color, thereby reach the purpose that detects mercury ion.Since the binding ability of other metallic ions and sulfydryl a little less than, so can part not replaced from gold nano grain, so body series has outstanding selectivity.
Wherein, in the described method of present embodiment, also can use acid (for example hydrochloric acid, sulfuric acid etc.) adjustment pH value again, as long as this testing process is in sour environment earlier with after above-mentioned detectable and the aqueous solution to be measured.This is because the quaternary ammonium salt on gold nano grain surface is positively charged, can with the hydrogen ion generation Coulomb repulsion in the sour environment, thereby gold nano grain is dispersed in the water, in ultraviolet-visible spectrum, absorption curve can not change.And in alkaline environment; The positive charge on gold nano grain surface and the hydroxyl radical negative ion in the alkaline environment pass through dipole-dipole interaction; Thereby gold nano grain is assembled; The variation of its absorption curve shows as the absorption peak red shift, to about the 600nm, and forms a broad peak (see figure 3) by the 520nm red shift.So the detection among the present invention must be accomplished in sour environment, alkaline environment can have interference to mercury ion detecting.
Therefore, hydrionic concentration has very big influence to the detection of mercury ion in the sour environment.In order to prove this influence, the inventor has studied the minimal detectable concentration under different pH condition.Concrete test procedure comprises:
1) prepares the mercury ion WS (A that a series of concentration are successively decreased
1, A
2A
n), the ion concentration of mercury scope is between 0.5 μ M～8mM;
2) the above-mentioned detectable of 50 μ L being joined volume respectively is the mercury ion WS (A that a series of concentration of 4950 μ L are successively decreased
1, A
2A
n) in, form mixed solution (M
1, M
2M
n), gold nano grain concentration is 150nM in the detectable, makes that the ultimate density of gold nano grain is 1.5nM in the above-mentioned mixed solution;
3) with mixed solution M
1Be divided into some parts of (M
11, M
12M
1m), utilize the above-mentioned mixed solution (M of hydrochloric acid each part of adjustment
11, M
12M
1m) the pH value, the pH value of the above-mentioned mixed solution of each part is not waited, and scope is between 1～7;
4) to the above-mentioned mixed solution (M of other ion concentration of mercury
2... M
n) repeating step 3).
5) find out the detected minimum ion concentration of mercury of the pairing ability of each pH value, process chart as shown in Figure 4.
Can find out that from Fig. 4 the pH value is low more, institute's detected ion concentration of mercury of ability is just low more.In the pH value is 1.0 o'clock, and the minimal detectable concentration that can reach is 1 μ M (every liter of micromole), and along with the pH value increases, minimal detectable concentration also increases, and in the time of between pH 2.5～7.0, the minimal detectable concentration that can reach is about 5mM (every liter of mM).Therefore, in order to reach sensitivity preferably, the pH value of the mixed solution of the detectable and the WS to be measured is preferably 1～2.5, and more preferably the pH value is 1.0.
Along with ion concentration of mercury reduces; Solution colour changes more and more not obvious; Be under 1.0 the condition in the preferred pH value of above-mentioned mixed solution, the minimal detectable concentration that changes that can naked eyes distinguishes between colors is 1 μ M, i.e. the minimal detectable concentration of the present invention under no any instrument is assisted is 1 μ M.In order to verify the result of this sensitivity, the applicant has tested the different solution of ion concentration of mercury with ultraviolet-visible spectrophotometer, and (ion concentration of mercury is respectively 0 μ M, 1 μ M; 2 μ M; 3 μ M, 4 μ M) variation of absorbance, the absorbance at 520nm place reduces and increases along with ion concentration of mercury; Absorbance about 640nm reduces along with ion concentration of mercury and reduces (Fig. 5) simultaneously, explains that its change color is more and more not obvious.The minimal detectable concentration of the present invention under no any instrument is auxiliary is 1 μ M, under the auxiliary detection of ultraviolet-visible spectrophotometer, can further reduce detectable concentration, improves detection sensitivity.
In the described method of present embodiment, in the mixed solution of the above-mentioned detectable and the WS to be measured, the ultimate density of gold nano grain is not limited to 1.5nM, for example can be in 1～10nM scope.Gold nano grain concentration also is not limited to 150nM in the detectable; As long as after solution to be measured mixes; The ultimate density of gold nano grain is got final product in 1～10nM scope, but the gold nano grain concentration in the detectable should not be low excessively, otherwise can reduce the concentration of mercury ion in the above-mentioned mixed solution greatly; Thereby it is not obvious to cause solution colour to change, and influences the detection of mercury ion.
In the described method of present embodiment, the diameter of gold nano grain can be 13nm left and right sides (see figure 6).The preparation of gold nano grain can be adopted existing sodium citrate reduction gold chloride preparation method, electrochemical reducing, radiation reducing process etc.The surface modifying method of gold nano grain comprises ligand exchange method, NaBH
4Reducing process etc.
Embodiment 2.
Can also utilize the auxiliary irradiation of sunshine to improve sensitivity according to mercury ion detecting method provided by the invention, its practical implementation step comprises:
1) prepare the WS to be measured, the ion concentration of mercury of this WS to be measured is that 30nM (every liter of nanomole), pH value are 1.
2) solution that utilizes the gold nano grain that the surface modified by 11-sulfydryl-1-trimethyl ammonium is as detectable; With this detectable of solar light irradiation after 30 seconds; Be that 5 μ L (microlitre), gold nano grain concentration are that the above-mentioned detectable of 150nM joins in the WS to be measured that volume is 495 μ L with volume immediately; Form mixed solution, make that the ultimate density of gold nano grain is 1.5nM, the concentration of mercury ion does not change basically.
3) solution colour becomes blueness by redness rapidly, shows that gathering has taken place gold nano grain.
According to method provided by the present invention, behind the irradiation sunshine, because behind the gold nano grain absorption photon; The photo-thermal conversion can take place, and the energy on gold nano grain surface is increased, thus the gold-sulfide linkage on activation gold nano grain surface; Make mercury ion interrupt gold-sulfide linkage more easily, from the gold surface desorption, cause gold nano grain to be assembled ligand molecular; Thereby the mercury ion detecting under the realization lower concentration improves sensitivity.
Wherein, also can shine sunshine more earlier with after above-mentioned detectable and the aqueous solution to be measured according to embodiments of the invention.Can also in above-mentioned detectable and aqueous solution to be measured, shine sunshine.The solar light irradiation time was not limited to 30 seconds, for example in 20 seconds to 40 seconds scopes.Sunshine can be the nature sunshine, also can be the light that the sunshine energizer is launched, and the power of sunshine energizer for example can be 300W.
The inventor has also studied under the sunshine subsidiary conditions, the minimal detectable concentration that the present invention can reach.Concrete grammar comprises:
1) prepares the mercury ion WS (A that a series of concentration are successively decreased
1, A
2A
n), the ion concentration of mercury scope is between 0nM～600nM.
2) the above-mentioned detectable of 5 μ L being joined volume respectively is the mercury ion WS (A that a series of concentration of 495 μ L are successively decreased
1, A
2A
n) in, form mixed solution (M
1, M
2M
n), gold nano grain concentration is 150nM in the detectable, makes that the ultimate density of gold nano grain is 1.5nM in the above-mentioned mixed solution;
3) utilize hydrochloric acid, with above-mentioned mixed solution (M
1, M
2M
n) the pH value be adjusted into 1.
4) the above-mentioned mixed solution (M of solar light irradiation that launches with the sunshine energizer of 300W
1, M
2M
n) 30 seconds.
Test findings is as shown in Figure 7, and along with the rising of ion concentration of mercury, the absorption peak at 670nm place increases gradually, and the absorption peak at 520nm place reduces gradually.Can find out that from above-mentioned test findings the minimum ion concentration of mercury that solution colour is changed is 30nM, see among Fig. 7 shown in the dotted line.This detectable concentration is the least concentration that known visual detection can reach
In order to confirm selectivity of the present invention, the inventor has also studied other metallic ions to interference of the present invention.These ions comprise Al
3+, Ba
2+, Ca
2+, Cd
2+, Co
2+, Cr
2+, Cu
2+, Fe
2+, Fe
3+, Hg
2+, K
+, Mg
2+, Mn
2+, Na
+, Ni
2+, Pb
2+, Zn
2+Be dissolved in these metallic ions in the distilled water respectively; Form the WS that ion concentration is 100 μ M; Utilizing according to the abovementioned embodiments of the present invention, the method described in 1 detects; Discovery has only mercury ion that solution colour is changed, and other ions do not change, thereby has verified that the present invention has good selectivity.Simultaneously, test the variation of its absorption value through ultraviolet-visible spectrophotometer, variation has taken place in the absorption value of the above-mentioned solution after having only mercury ion to add, and its absorption peak to the 600nm, and is accompanied by broadening of absorption peak by the 520nm red shift.Through relatively adding the variation of the absorbance at 520nm place before and after the metallic ion, can see obviously that the present invention has goodish selectivity (Fig. 8) to mercury ion.
It should be noted last that above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is specified with reference to embodiment; Those of ordinary skill in the art is to be understood that; Technical scheme of the present invention is made amendment or is equal to replacement, do not break away from the spirit and the scope of technical scheme of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (10)
1. a gold nano grain that utilizes surface modification detects the method for mercury ion, comprising:
1) utilize the surface by the solution of the gold nano grain of 11-sulfydryl-1-trimethyl ammonium modification as detectable;
2) with this detectable and aqueous solution to be measured, wherein the mixed solution of gained is acid;
3) judge through the mixed solution change in color whether mercury ion exists in the WS to be measured.
2. the method for detection mercury ion according to claim 1 is characterized in that, in above-mentioned steps 2) in, earlier with after above-mentioned detectable and the aqueous solution to be measured, adjust the pH value of mixed solution again, it is acid making detection architecture.
3. the method for detection mercury ion according to claim 1 is characterized in that, in above-mentioned steps 2) in, adjustment pH value of aqueous solution to be measured is acid, again with above-mentioned detectable and aqueous solution to be measured earlier.
4. according to the method for claim 2 or 3 described detection mercury ions, it is characterized in that the pH value of the mixed solution of the above-mentioned detectable and the WS to be measured is 1～2.5.
5. the method for detection mercury ion according to claim 4 is characterized in that, the pH value of the mixed solution of the above-mentioned detectable and the WS to be measured is 1.
6. the method for detection mercury ion according to claim 1 is characterized in that, in above-mentioned steps 2) in, also comprise solar light irradiation.
7. the method for detection mercury ion according to claim 6 is characterized in that, in above-mentioned steps 2) in, earlier detectable is carried out solar light irradiation, again with above-mentioned detectable and aqueous solution to be measured.
8. the method for detection mercury ion according to claim 6 is characterized in that, after above-mentioned detectable and aqueous solution to be measured, and irradiation under sunshine again.
9. according to the method for claim 1-3 or the described detection mercury ion of 6-8, it is characterized in that the diameter of above-mentioned gold nano grain is about 13 nanometers.
10. according to the method for each described detection mercury ion in claim 1 to 3 or 6 to 8, it is characterized in that in the mixed solution of the detectable and the WS to be measured, the concentration of gold nano grain is in 1～10nM scope.
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| CN103226103A (en) * | 2013-04-04 | 2013-07-31 | 哈尔滨师范大学 | Colorimetric detection probe of mercury ion and application method thereof |
| CN105115963A (en) * | 2015-07-17 | 2015-12-02 | 湖南大学 | Heavy metal mercury detection method |
| CN106583747A (en) * | 2016-12-06 | 2017-04-26 | 南华大学 | Preparation of protamine gold nanoclusters and application in analogue enzyme color comparison and fluorescence detection |
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| CN109575915A (en) * | 2018-12-17 | 2019-04-05 | 鲁东大学 | A kind of method of amphiphilic polymer modified AuNPs colorimetric detection organic mercury |
| CN115178746A (en) * | 2022-07-13 | 2022-10-14 | 宁波大学 | Preparation method and application of gold nanoparticles for detecting mercury ions in cosmetic water |
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| CN102962446A (en) * | 2012-11-13 | 2013-03-13 | 中国科学院长春应用化学研究所 | Method for activating noble metal nano particles by liquid phase dissolving |
| CN103226103A (en) * | 2013-04-04 | 2013-07-31 | 哈尔滨师范大学 | Colorimetric detection probe of mercury ion and application method thereof |
| CN103226103B (en) * | 2013-04-04 | 2015-02-04 | 哈尔滨师范大学 | Colorimetric detection probe of mercury ion and application method thereof |
| CN105115963A (en) * | 2015-07-17 | 2015-12-02 | 湖南大学 | Heavy metal mercury detection method |
| CN106583747A (en) * | 2016-12-06 | 2017-04-26 | 南华大学 | Preparation of protamine gold nanoclusters and application in analogue enzyme color comparison and fluorescence detection |
| CN107727596A (en) * | 2017-09-30 | 2018-02-23 | 中国石油大学(华东) | A kind of method of the micro mercury ion of quick detection |
| CN107727596B (en) * | 2017-09-30 | 2019-11-08 | 中国石油大学(华东) | A method of quickly detecting micro mercury ion |
| CN109575915A (en) * | 2018-12-17 | 2019-04-05 | 鲁东大学 | A kind of method of amphiphilic polymer modified AuNPs colorimetric detection organic mercury |
| CN109575915B (en) * | 2018-12-17 | 2021-08-24 | 鲁东大学 | Method for colorimetric detection of organic mercury by using amphiphilic polymer modified AuNPs |
| CN115178746A (en) * | 2022-07-13 | 2022-10-14 | 宁波大学 | Preparation method and application of gold nanoparticles for detecting mercury ions in cosmetic water |
| CN115178746B (en) * | 2022-07-13 | 2024-03-01 | 宁波大学 | Preparation method and application of gold nanoparticles for detecting mercury ions in cosmetic water |
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