CN101881734B - Detection method of metal ions - Google Patents
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- CN101881734B CN101881734B CN2010101940410A CN201010194041A CN101881734B CN 101881734 B CN101881734 B CN 101881734B CN 2010101940410 A CN2010101940410 A CN 2010101940410A CN 201010194041 A CN201010194041 A CN 201010194041A CN 101881734 B CN101881734 B CN 101881734B
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Abstract
The invention discloses a detection method of metal ions. In the method, based on a gold nanoparticles-sulfide system, by virtue of the interaction among the gold nanoparticles, a hydrolysate of a sulfide and the detected metal ions or the interaction among the gold nanoparticles, a sulfhydryl compound and the detected metal ions, resonance absorption of plasmas on the surface of the gold nanoparticles changes so that the color and the ultraviolet visible absorption strength of the gold nanoparticles changes. By adopting the method, the detected metal ions in the solution system can be rapidly detected by directly distinguishing change of solution color through eyes or a simple apparatus. The detection method has the advantages of simple and convenient operation, low detection cost, high detection sensitivity, small sampling quantity and wide application scope.
Description
Technical field
The present invention relates to the detection range of metallic ion, particularly the detection method of a metal ion species.
Background technology
Along with development of science and technology, human also increasing to the demand of resource, in order to accelerate development of science and technology, the mankind excessively ask for resource to nature, thereby cause current society to face a big problem-environmental pollution.At present, environmental pollution has become a very important problem.Industry " three wastes " (waste water,waste gas and industrial residue) has caused the discharging of very havoc, particularly industrial waste water especially outstanding to the pollution of water resource to environment.For example; Contain a large amount of heavy metal ion in the industrial waste water of industries such as industrial and mineral, chemical industry, battery, plating; Some enterprise does not add these waste water to handle or handle a little and just is discharged in the water body, causes heavy metal pollution more and more serious, directly affects human health and natural ecological environment.
For instance, Hg
2+Be the most stable existence form of inorganic mercury, brain, nervous system, kidney and the internal system etc. to the human or animal produce serious destruction easily; In addition, rivers and lakes and marine microbe can convert the inorganic mercury ion to methyl mercury (CH
3Hg
+) accumulate in vivo, get in people or other animal body direct threats human beings'health through food chain.Cd
2+Be that water body weight is wanted pollution source, its toxicity is very big; It can suppress growth and development of plants by the plant absorption and by enrichment, and can get in the food chain entering humans and animals body.When by the Cd of enrichment
2+After getting into human body, can cause that it is cardiovascular, the damage of lung, kidney and histoorgans such as bone and testis, the health of serious threat humans and animals body.Work as Cd
2+Enrichment can cause that the people poisons or even death, the life security that serious threat is human to finite concentration in human body.Co
2+Poison and can cause then that human body apocleisis, nausea,vomiting,diarrhea, precordialgia, face and four limbs are rubescent, fash, temporarily nerve deafness, renal damage, stomachache; Idol can cause reactions such as pigmentation, thyromegaly, heart rate quickening, also can suppress erythrocytic formation.
To the main at present policy of relying mainly on prevention, preventing and treating combination that adopts of heavy metal pollution; Though equipment such as atomic absorption (AAS), atomic fluorescence absorption (AFS) and the inductive couple plasma-mass spectrum logotype appearance etc. of special detection metallic ion are arranged now; But these instruments cost an arm and a leg, and often have defectives such as sample preparation steps complicacy, sample poorly water-soluble, other ion interference be serious when being used for metal ion detection.In view of present national economy situation, a lot of conditions do not possess or technological jejune unit or individuality can't adopt above-mentioned sophisticated equipment that heavy metal is carried out conventional sense, cause pollution source to enlarge; And, utilize the method for instrument detecting can not realize to water quality in real time, detect on the spot.In order to reduce environmental pollution; Guarantee human had rehemorrhage and the sustainable development that keeps economic society; Accomplish early to detect, early administer; Reduce the cost of pollution control, heavy-metal pollution is controlled at minimum level to the mankind's harm, must accomplish fast, detect in real time the toxicity kations such as mercury ion in the water body.Therefore, research and develop a kind of highly sensitive, selectivity good, simple to operate, sampling amount is few and with low cost directly detects Hg fast
2+, Cd
2+, Co
2+Method in the toxic metal ion seems very urgently and needs.
Summary of the invention
Technical matters to be solved by this invention is how simply, fast and delicately: detect Hg
2+, Cd
2+And Co
2+In the toxic metal ion.
For addressing the above problem, the invention provides the detection method of a metal ion species, adopt the golden nanometer particle of surface with different electric charges, based on the variation of golden nanometer particle surface plasma body resonant vibration absorption peak, simple, the common toxicity kation of fast detecting.
The detection method of one metal ion species comprises step:
(1) in the tetrachloro alloy aqueous acid, adds surface protectant and reductive agent, make the detection liquid that contains the surface protectant gold nano-particles modified;
(2) the above-mentioned detection liquid of two parts of identical and equivalent is provided; Isopyknic said metal ion solution and solution to be detected of not containing is added said two parts respectively and detects in the liquid, form corresponding first mixed solution and second mixed solution;
Described not contain said metal ion solution identical with the solvent of solution to be detected, is selected from water or ethanol;
(3) according to the color of second mixed solution with respect to the change color of first mixed solution or change with respect to the first mixed solution UV, visible light absorption intensity according to second mixed solution, judge whether there is said metallic ion in the solution to be detected.
Also can judge that with respect to the change color required time of first mixed solution GOLD FROM PLATING SOLUTION to be detected belongs to the concentration range of ion simultaneously according to the color of second mixed solution; Change with respect to the first mixed solution UV, visible light absorption intensity according to second mixed solution, calculate the content of metallic ion described in the solution to be detected.
Described surface protectant is selected from cetyl trimethyl ammonium bromide (CTAB), contain in the compound of sulfydryl one or more; Use the different surface protective agent can obtain the golden nanometer particle of surface, can optionally detect tested metallic ion and reduce the interference of other non-tested metallic ion with needed different electric charges.
The described preferred TGA of compound of sulfydryl, in the glutathione one or both of containing.
Described reductive agent is selected from sodium borohydride (NaBH
4).
Described solution to be detected can be that the water sample in the environment also can be the solution that the water-soluble or organic solvent of other environmental samples forms, and is dissolved in the solution that forms in water or the ethanol like solid-state environmental sample, urine, blood etc. in the biomedicine.
In the step (1), after the described detection liquid that contains the surface protectant gold nano-particles modified is preferably regulated the pH value with acid or alkali, carry out all the other operations.Regulate the pH that detects liquid, to satisfy the best requirement of different systems to the pH value, suitable pH not only can save detection time and the interference of getting rid of non-detection material, but also can improve detectability and detection sensitivity.
If described metallic ion is Hg
2+, then also comprise step: in said first mixed solution and second mixed solution, add the sulfocompound of equivalent respectively, judge by said step (3) then; Described surface protectant is selected from cetyl trimethyl ammonium bromide; Described sulfocompound is selected from thioacetamide; The described detection liquid that contains the surface protectant gold nano-particles modified is with salt acid for adjusting pH value to 3.57.
Judge in the said solution to be detected and whether contain Hg
2+Method be specially: if the color of said second mixed solution becomes indigo plant or color burn with respect to the color of said first mixed solution, then judge in the solution to be detected and contain Hg
2+If the color of said second mixed solution does not have variation or said second mixed solution not to change with respect to the said first mixed solution UV, visible light absorption intensity with respect to the color of said first mixed solution, then judge not contain Hg in the solution to be detected
2+
The concentration of described sulfocompound in second mixed solution is high more, and required time of the change color of second mixed solution is short more.
If described metallic ion is Cd
2+, then described surface protectant is selected from cetyl trimethyl ammonium bromide and TGA, and the described detection liquid that contains the surface protectant gold nano-particles modified is regulated pH value to 11.7 with NaOH.
Judge in the said solution to be detected and whether contain Cd
2+Method be specially: if the color of said second mixed solution shoals with respect to the color redness of said first mixed solution or redness is taken off, then judge in the solution to be detected to contain Cd
2+If the color of said second mixed solution does not have variation or said second mixed solution not to change with respect to the said first mixed solution UV, visible light absorption intensity with respect to the color of said first mixed solution, then judge not contain Cd in the solution to be detected
2+
If described metallic ion is Co
2+, then described surface protectant is selected from cetyl trimethyl ammonium bromide and TGA, and the described detection liquid that contains the surface protectant gold nano-particles modified is regulated pH value to 10.0 with NaOH.
Judge in the said solution to be detected and whether contain Co
2+Method be specially: if said second mixed solution becomes rufous, then judge in the solution to be detected and contain Co
2+If the said second mixed solution color does not have variation or said second mixed solution not to change with respect to the said first mixed solution UV, visible light absorption intensity with respect to the color of said first mixed solution, then judge not contain Co in the solution to be detected
2+
The described concentration of compound in second mixed solution that contains sulfydryl is high more, and required time of the change color of second mixed solution is short more.
Change with respect to the first mixed solution UV, visible light absorption intensity according to second mixed solution, calculate the content of metallic ion described in the solution to be detected, calculate, specifically comprise according to this area prior standard working curve method:
Prepare the solution of a series of different metal ion concentrations in advance according to the compound method of said second mixed solution; Detect the UV, visible light absorption intensity at 300nm-1000nm respectively; UV, visible light absorption intensity with each solution is an ordinate; The concentration of each solution is horizontal ordinate, the drawing standard working curve;
Detect the UV, visible light absorption intensity of second mixed solution under the same conditions, draw the concentration (being content) of metallic ion in second mixed solution through standard working curve.
Find that through experiment described metallic ion is Hg
2+, the preferred 560nm of detection wavelength of UV, visible light absorption intensity; Described metallic ion is Cd
2+, the preferred 530nm of detection wavelength of UV, visible light absorption intensity; Described metallic ion is Co
2+, the preferred 500nm of detection wavelength of UV, visible light absorption intensity.
The present invention is based on golden nanometer particle-sulfide system, the hydrolysate that utilizes golden nanometer particle and sulfide is (like S
2-) and the interaction of metallic ion to be detected; The perhaps interaction of golden nanometer particle and sulfhydryl compound and metallic ion to be detected; The resonance absorption that causes the golden nanometer particle surface plasma changes, thereby causes golden nanometer particle color and UV, visible light absorption intensity to change.Directly differentiate the variation of solution colour, can detect the metallic ion to be detected in the solution system apace through naked eyes or simple device equipment.To such an extent as to because the time speed and the shade of change color of the amount difference solution of gold nanoparticles of contained metallic ion to be detected in the sample can carry out qualitative and quantitative detection to metallic ion to be detected.
The inventive method; Simple to operation, detection is with low cost, detection sensitivity is high and sampling amount is few; Be applicable to the detection of various water samples such as lake water quality of river investigation, sewage effluent water quality detection, the urgent water safety detection of outdoor activities and domestic water, applied range.
Utilize the inventive method can realize Hg
2+, Cd
2+And Co
2+, fast detection simple and convenient in the toxic metal ion.
Embodiment
Embodiment 1 detects the preparation of liquid
The tetrachloro alloy aqueous acid 5mL that gets 5mmol/L joins in the deionized water of 71mL; The CTAB WS 24mL that under stirring condition, adds 0.5mmol/L; Then lentamente to the sodium borohydride aqueous solution that wherein adds 1.6mL 1mmol/L; Continue at ambient temperature to stir 30 minutes, can obtain containing the detection liquid of CTAB gold nano-particles modified.
Embodiment 2 detects the preparation of liquid
In the detection liquid that contains the CTAB gold nano-particles modified that 100ml embodiment 1 makes, add 100 μ l TGAs, mix, promptly obtain containing the detection liquid of CTAB and TGA gold nano-particles modified.
Hg in embodiment 3 water samples
2+Detection
At first, get the detection liquid that contains the CTAB gold nano-particles modified that makes among the 10ml embodiment 1, regulate the pH value to 3.57 that detects liquid, obtain the pH value and be 3.57 detection liquid with the aqueous hydrochloric acid solution of 0.1mol/L.
Then, prepare the test tube A and the test tube B of two same specifications; In test tube A and test tube B, add identical and isopyknic above-mentioned pH value respectively and be 3.57 detection liquid.
Then, in test tube A and test tube B, add isopyknic 1ml ultrapure water and 1ml water sample to be detected respectively;
Once more, the thioacetyl amine aqueous solution that in test tube A and test tube B, adds 30 microlitre 20mmol/L respectively.
At last, test tube A and test tube B are placed at ambient temperature, observe the situation of change of solution among test tube A and the test tube B.
In 5 minutes,, then judge and contain Hg in the water sample if the color of solution changes with respect to solution colour among the test tube A and promptly becomes indigo plant or color burn among the test tube B
2+And Hg in the water sample
2+Concentration is more than or equal to 5.0 * 10
-5Mol/L.
If after 5 minutes among the test tube B color of solution do not change with respect to the color of solution among the test tube A and promptly do not become indigo plant or color is not deepened; Continue to place at ambient temperature 30 minutes; Observe change color again; If the color of solution changes with respect to the color of solution among the test tube A and promptly becomes indigo plant or color burn among the test tube B, then judge and contain Hg in the water sample
2+And Hg in the water sample
2+Concentration is more than or equal to 1.0 * 10
-5Mol/L and smaller or equal to 5.0 * 10
-5Mol/L.
If after 30 minutes among the test tube B color of solution do not change with respect to the color of solution among the test tube A and promptly do not become indigo plant or color is not deepened; Continue to place at ambient temperature 1.5 hours; Observe change color again, if the color of solution changes with respect to the color of solution among the test tube A and promptly becomes indigo plant or color burn and then judge and contain Hg in the water sample among the test tube B
2+And Hg in the water sample
2+Concentration is more than or equal to 5.0 * 10
-6Mol/L and smaller or equal to 1.0 * 10
-5Mol/L.If the color of solution does not change among the test tube B, then judge Hg in the water sample
2+Concentration is lower than 5.0 * 10
-6Mol/L or do not contain Hg
2+
Cd in embodiment 4 water samples
2+Detection
At first, get the detection liquid that contains CTAB and TGA gold nano-particles modified that makes among the embodiment 2 of 10ml, regulate the pH value to 11.7 that detects liquid, obtain the pH value and be 11.7 detection liquid with the sodium hydrate aqueous solution of 0.1mol/L.Other steps are except that need not in test tube A and test tube B, to add respectively the thioacetyl amine aqueous solution of equivalent, and are all identical with embodiment 3.
In 5 minutes, if among the test tube B color of solution to change with respect to solution colour among the test tube A be that redness shoals or redness is taken off, then judge and contain Cd in the water sample
2+And Cd in the water sample
2+Concentration is more than or equal to 5.0 * 10
-5Mol/L.
If after 5 minutes among the test tube B color of solution not change with respect to the color of solution among the test tube A be that redness does not shoal or redness is not taken off; Continue to place at ambient temperature 30 minutes; Observe change color again; If to change with respect to the color of solution among the test tube A be that redness shoals or redness is taken off to the color of solution among the test tube B, then judge and contain Cd in the water sample
2+And Cd in the water sample
2+Concentration and more than or equal to 1.0 * 10
-5Mol/L and smaller or equal to 5.0 * 10
-5Mol/L.
If after 30 minutes among the test tube B color of solution not change with respect to the color of solution among the test tube A be that redness does not shoal or redness is not taken off; Continue to place at ambient temperature 1.5 hours; Observe change color again, if among the test tube B color of solution to change with respect to the color of solution among the test tube A be that redness shoals or redness is taken off and then judged and contain Cd in the water sample
2+And Cd in the water sample
2+Concentration and more than or equal to 5.0 * 10
-6Mol/L and smaller or equal to 1.0 * 10
-5Mol/L.
If after 2 hours among the test tube B color of solution to change with respect to the color of solution among the test tube A be that redness shoals or redness is taken off, then judge to detect in the water sample and contain Cd
2+And Cd in the water sample
2+Concentration and more than or equal to 5.0 * 10
-6Mol/L and smaller or equal to 5.0 * 10
-7Mol/L.If the color of solution does not change among the test tube B, then judge not contain Cd in the water sample
2+
Co in embodiment 5 water samples
2+Detection
At first, get the detection liquid that contains CTAB and TGA gold nano-particles modified that makes among the embodiment 2 of a certain amount of 10ml, regulate the pH value to 10.0 that detects liquid, obtain the pH value and be 10.0 detection liquid with the sodium hydrate aqueous solution of 0.1mol/L.Other steps are except that need not in test tube A and test tube B, to add respectively the thioacetyl amine aqueous solution of equivalent, and are all identical with embodiment 3.
If after adding water sample to be detected, the color of solution becomes rufous immediately among the test tube B, then judges to contain Co in the water sample
2+And Co in the water sample
2+Concentration is 5.0 * 10
-5More than the mol/L.
If after adding water sample to be detected, the color of solution becomes rufous in 3 minutes among the test tube B, then judges and contains Co in the water sample
2+And Co in the water sample
2+Concentration is more than or equal to 5.0 * 10
-6Mol/L and smaller or equal to 5.0 * 10
-5Mol/L.
If after adding water sample to be detected, the color of solution shoals in 3 minutes among the test tube B, then judges and contains Co in the water sample
2+And Co in the water sample
2+Concentration is more than or equal to 5.0 * 10
-7Mol/L and smaller or equal to 5.0 * 10
-6Mol/L.
If the color of solution does not change among the test tube B, then judge Co in the water sample
2+Concentration is lower than 5.0 * 10
-7Mol/L or do not contain Co
2+
Claims (4)
1. the detection method of a metal ion species comprises step:
(1) in the tetrachloro alloy aqueous acid, adds surface protectant and reductive agent, make the detection liquid that contains the surface protectant gold nano-particles modified;
(2) the above-mentioned detection liquid of two parts of identical and equivalent is provided; Isopyknic said metal ion solution and solution to be detected of not containing is added said two parts respectively and detects in the liquid, form corresponding first mixed solution and second mixed solution;
Described not contain said metal ion solution identical with the solvent of solution to be detected, is selected from water or ethanol;
(3) according to the color of second mixed solution with respect to the change color of first mixed solution or according to of the variation of second mixed solution with respect to the first mixed solution UV, visible light absorption intensity, judge whether there is said metallic ion in the solution to be detected;
Described reductive agent is selected from sodium borohydride;
Described metallic ion is Hg
2+, comprise step: in said first mixed solution and second mixed solution, add the sulfocompound of equivalent respectively, judge by said step (3) then;
Described surface protectant is selected from cetyl trimethyl ammonium bromide;
Described sulfocompound is selected from thioacetamide;
The described detection liquid that contains the surface protectant gold nano-particles modified is with salt acid for adjusting pH value to 3.57;
Perhaps, described metallic ion is Cd
2+, described surface protectant is cetyl trimethyl ammonium bromide and TGA, the described detection liquid that contains the surface protectant gold nano-particles modified is regulated pH value to 11.7 with NaOH;
Perhaps, described metallic ion is Co
2+, described surface protectant is cetyl trimethyl ammonium bromide and TGA, the described detection liquid that contains the surface protectant gold nano-particles modified is regulated pH value to 10.0 with NaOH.
2. the detection method of metallic ion according to claim 1 is characterized in that, the color of said second mixed solution becomes indigo plant or color burn with respect to the color of said first mixed solution, judges in the solution to be detected and contains Hg
2+The color of said second mixed solution does not have variation or said second mixed solution not to change with respect to the said first mixed solution UV, visible light absorption intensity with respect to the color of said first mixed solution, judges not contain Hg in the solution to be detected
2+
3. the detection method of metallic ion according to claim 1 is characterized in that, the color of said second mixed solution shoals with respect to the color redness of said first mixed solution or redness is taken off, and judges in the solution to be detected to contain Cd
2+The color of said second mixed solution does not have variation or said second mixed solution not to change with respect to the said first mixed solution UV, visible light absorption intensity with respect to the color of said first mixed solution, judges not contain Cd in the solution to be detected
2+
4. the detection method of metallic ion according to claim 1 is characterized in that, said second mixed solution becomes rufous, judges in the solution to be detected and contains Co
2+The said second mixed solution color does not have variation or said second mixed solution not to change with respect to the said first mixed solution UV, visible light absorption intensity with respect to the color of said first mixed solution, judges not contain Co in the solution to be detected
2+
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|---|---|---|---|
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|---|---|---|---|
| CN2010101940410A CN101881734B (en) | 2010-06-07 | 2010-06-07 | Detection method of metal ions |
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| CN101881734B true CN101881734B (en) | 2012-02-01 |
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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 |
| CN101710076B (en) * | 2009-12-29 | 2012-07-04 | 东北师范大学 | Lead ion colorimetric detection probes and application method thereof |
| CN101949855B (en) * | 2010-08-10 | 2011-11-23 | 中国科学院宁波材料技术与工程研究所 | Method for detecting metal cation by utilizing VA group or VIA group element compound |
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