CN102337119A - Preparation method of fluorescein sodium solution containing nano-sized metal particles - Google Patents
Preparation method of fluorescein sodium solution containing nano-sized metal particles Download PDFInfo
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- CN102337119A CN102337119A CN2010102381531A CN201010238153A CN102337119A CN 102337119 A CN102337119 A CN 102337119A CN 2010102381531 A CN2010102381531 A CN 2010102381531A CN 201010238153 A CN201010238153 A CN 201010238153A CN 102337119 A CN102337119 A CN 102337119A
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Abstract
The invention belongs to the technical field of fluorescent materials, and provides a preparation method of fluorescein sodium solution containing nano-sized metal particles. The method comprises steps for preparing metal crystal seed sol, steps for preparing nano-sized metal particle sol, and steps for preparing the fluorescein sodium solution containing the nano-sized metal particles. According to the method provided by the invention, the nano-sized metal particle sol is prepared by using ascorbic acid; the nano-sized metal particle sol is added to a fluorescein sodium solution according to a preset amount, such that the luminous intensity of fluorescein sodium under a low concentration is greatly improved, and detection accuracy is ensured when low-concentration fluorescein sodium is adopted.
Description
Technical field
The invention belongs to the fluorescent material technical field, relate in particular to a kind of Fluress preparation method of containing metal nano particle.
Background technology
The chemical name of uranine is 9-(o-hydroxy-phenyl)-6-hydroxyl-3H-xanthene-3-ketone disodium salt, has the sub-productive rate of higher specific absorbance and appropriate vol, is one of fluorescent material of using morely in the fluorescent probe.Yet; The self quenching phenomenon can be because of taking place in the resonance energy transfer process in uranine; So often along with the rising of label concentration in the application process, its fluorescence intensity reduces on the contrary gradually, therefore need it be controlled in the low concentration scope and use; Again because of fluorescence intensity causes the muting sensitivity that detects a little less than, thereby bring difficulty to detection.
Summary of the invention
The purpose of the embodiment of the invention is to provide a kind of Fluress preparation method of containing metal nano particle, solves uranine and when lower concentration, a little less than the luminous intensity, brings the difficult technologies problem to detection.
The embodiment of the invention is achieved in that a kind of Fluress preparation method of containing metal nano particle, comprises the steps:
The mixing solutions of preparing metal compound and organic additive and alkali metal borohydride solution; The concentration of said metallic compound is below 0.5mmol/L; The mixing solutions of said alkali metal borohydride solution, metallic compound and organic additive is mixed, and ageing makes metal crystal seed colloidal sol; Wherein, said organic additive is Trisodium Citrate, Tripotassium Citrate or Vinylpyrrolidone polymer;
The preparing metal compound water solution adds cetyl trimethylammonium bromide and said metal crystal seed colloidal sol at the said metallic compound aqueous solution, obtains the metallic compound mixed solution of containing metal crystal seed colloidal sol; In the metallic compound mixed solution of said containing metal crystal seed colloidal sol, add xitix, the solution pH value is adjusted into alkalescence, the metals ion in the compound liquid of reducing metal obtains metal nanoparticle colloidal sol;
The preparation Fluress adds described metal nanoparticle colloidal sol, obtains the Fluress of containing metal nano particle; Wherein, the content of above-mentioned metal in Fluress is 1 * 10
-4-1 * 10
-7Mol/L.
The method of the embodiment of the invention; Reductive action through xitix prepares metal nanoparticle; And utilize this metal nanoparticle to strengthen the luminous intensity of uranine, reached, guaranteed that uranine is under the lower concentration situation the remarkable enhanced effect of uranine luminous intensity; Have stronger luminous intensity, guaranteed the susceptibility of lower concentration uranine in detection.
Description of drawings
Fig. 1 is the pl-contrast spectrogram of Fluress that contains the silver nano-grain of the embodiment of the invention 1 and do not contain the silver nano-grain of the embodiment of the invention 1;
Fig. 2 is the pl-contrast spectrogram of Fluress that contains the gold nano grain of the embodiment of the invention 2 and do not contain the gold nano grain of the embodiment of the invention 2;
Fig. 3 is the pl-contrast spectrogram of Fluress that contains the silver nano-grain of the embodiment of the invention 3 and do not contain the silver nano-grain of the embodiment of the invention 3;
Fig. 4 is the uranine photoluminescence spectra figure of comparative example's 6 of the present invention silver-containing nanoparticles.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The preparation method of the embodiment of the invention; Reductive action through xitix prepares metal nanoparticle; And utilize this metal nanoparticle to strengthen the luminous intensity of uranine, reached, guaranteed that uranine is under the lower concentration situation the remarkable enhanced effect of uranine luminous intensity; Have stronger luminous intensity, guaranteed the susceptibility of lower concentration uranine in detection.
The embodiment of the invention provides a kind of Fluress preparation method of containing metal nano particle, comprises the steps:
The mixing solutions of preparing metal compound and organic additive and alkali metal borohydride solution; The concentration of said metallic compound is below 0.5mmol/L; The mixing solutions of said alkali metal borohydride solution, metallic compound and organic additive is mixed, and ageing makes metal crystal seed colloidal sol; Wherein, said organic additive is Trisodium Citrate, Tripotassium Citrate or Vinylpyrrolidone polymer;
The preparing metal compound water solution adds cetyl trimethylammonium bromide and said metal crystal seed colloidal sol at the said metallic compound aqueous solution, obtains the metallic compound mixed solution of containing metal crystal seed colloidal sol; In the metallic compound mixed solution of said containing metal crystal seed colloidal sol, add xitix, the solution pH value is adjusted into alkalescence, the metals ion in the compound liquid of reducing metal obtains metal nanoparticle colloidal sol;
The preparation Fluress adds described metal nanoparticle colloidal sol, obtains the Fluress of containing metal nano particle; Wherein, the content of above-mentioned metal in Fluress is 1 * 10
-4-1 * 10
-7Mol/L.
The Fluress preparation method of the containing metal nano particle of the embodiment of the invention, concrete steps are following:
Preparation metal crystal seed colloidal sol: the mixing solutions of preparing metal compound and organic additive, in this mixed solution, the concentration of metallic compound is 0.01-0.5mmol/L; The concentration of organic additive is 0.05-0.5mmol/L;
Wherein, the metallic compound of the embodiment of the invention comprises one or more in Silver Nitrate, hydrochloro-auric acid, Platinic chloride, the Palladous chloride; The organic additive of the embodiment of the invention is Trisodium Citrate, Tripotassium Citrate or Vinylpyrrolidone polymer K30 (PVP) etc., can make the metal crystal seed stable, does not reunite;
The concentration of the metallic compound of the embodiment of the invention surpasses this concentration below 0.5mmol/L, the metal crystal seed particle diameter of this step preparation can be excessive, do not reach the purpose as crystal seed;
Compound concentration is 1 * 10
-3-1 * 10
-1The alkali metal borohydride solution of mol/L; Said alkali metal borohydride comprises Peng Qinghuana, POTASSIUM BOROHYDRIDE 97MIN etc.;
Above-mentioned alkali metal borohydride solution is joined in the mixing solutions of above-mentioned metallic compound and organic additive, obtain metal crystal seed colloidal sol;
In the embodiment of the invention, should use the above-mentioned reductive agent of capacity, preferably above-mentioned alkali metal borohydride and above-mentioned metallic compound pressed amount of substance than 3.6: 1-15: 1 mixes;
Amount of substance ratio through with above-mentioned alkali metal borohydride and metallic compound is controlled at 3.6: 1-15: 1 scope has guaranteed that above-mentioned metallic compound can Restore All;
Preparation metal nanoparticle colloidal sol: the preparing metal compound water solution, add cetyl trimethylammonium bromide (CTAB), making the content of this CTAB in this metal compound solution is 1 * 10
-4-5 * 10
-2G/ml, this CTAB can play stabilization, and security deposit's metal nano-particle is not reunited, and plays the effect that influences the metal nanoparticle growth pattern simultaneously;
Employed metallic compound is with metallic compound a kind of or not of the same race in the metallic compound that uses in the above-mentioned metal crystal seed colloidal sol preparation process in the embodiment of the invention and the preparation process of above-mentioned metal nanoparticle colloidal sol.For example, in preparation metal crystal seed colloidal sol, can use hydrochloro-auric acid, and in preparation metal nanoparticle colloidal sol, can use hydrochloro-auric acid, also can use Silver Nitrate, form the metal nanoparticle colloidal sol of at least two kinds of metallic combinations thus;
The water that the embodiment of the invention is used is deionized water preferably;
By above-mentioned metal crystal seed colloidal sol and metallic compound aqueous solution volume ratio 1: 37-1: 3.75 are added to above-mentioned metal crystal seed colloidal sol in this metal compound solution that contains CTAB, obtain the metallic compound mixed solution of containing metal crystal seed colloidal sol;
Xitix is added to the metallic compound mixed solution of above-mentioned containing metal crystal seed colloidal sol, is 8-12 with the solution pH value, stirs 1-6 hour, obtains metal nanoparticle colloidal sol;
In the embodiment of the invention, should use the xitix of capacity, preferably with xitix and metallic compound in molar ratio 1: 1-10: 1 mixes;
The embodiment of the invention uses xitix as reductive agent, therefore under the original effect of metal crystal seed at xitix, regrows, and forms the metal nanoparticle with suitable pattern and size.Be controlled at 1 through mol ratio in addition: 1-10 with xitix and metallic compound: 1 scope, thus guarantee that the metallic compound in the metal compound water solution can be reduced fully; Xitix can directly add, and also can be made into aqueous ascorbic acid;
Preparation contains the Fluress of metal nanoparticle: preparation 1 * 10
-3-1 * 10
-7The Fluress of mol/L adds above-mentioned metal nanoparticle colloidal sol, makes that the content of above-mentioned metal in Fluress is 1 * 10
-4-1 * 10
-7Mol/L obtains the Fluress of containing metal nano particle;
Wherein, the employed solvent of preparation uranine can be all kinds of SOLVENTS, and preferably water is or/and ethanol.
The method of the embodiment of the invention; Reductive action through xitix prepares metal nanoparticle; And utilize this metal nanoparticle to strengthen the luminous intensity of uranine, reached, guaranteed that uranine is under the lower concentration situation the remarkable enhanced effect of uranine luminous intensity; Have stronger luminous intensity, guaranteed the susceptibility of lower concentration uranine in detection.
Embodiment 1
The embodiment of the invention provides a kind of Fluress preparation method of containing metal nano particle, and is specific as follows:
Prepare silver-colored crystal seed colloidal sol: preparation contains the aqueous solution 20mL of 0.5mmol/L Silver Nitrate and 0.5mmol/L Trisodium Citrate;
Compound concentration is the sodium borohydride aqueous solution of 0.1mol/L;
In the ratio of Peng Qinghuana and the amount of substance of Silver Nitrate is that 3.6: 1 ratio adds the 0.36mL sodium borohydride aqueous solution fast in the Silver Nitrate mixing solutions, and continuation magnetic agitation 10min, and at room temperature ageing 10h obtains silver-colored crystal seed colloidal sol then;
Preparation silver nano-grain colloidal sol: the 3.4mg Silver Nitrate is dissolved in the 18.5mL deionized water, and is 1 * 10 by CTAB content
-3G/mL adds 0.0185gCTAB in silver nitrate aqueous solution;
1: 37 ratio of volume ratio in silver-colored crystal seed colloidal sol and silver nitrate aqueous solution is added 0.5mL silver crystal seed colloidal sol in silver nitrate aqueous solution, obtain the Silver Nitrate mixed solution of argentiferous crystal seed colloidal sol;
Compound concentration is the aqueous ascorbic acid of 0.02mol/L;
In the ratio of the amount of substance of xitix metallizing thing is that 1: 1 ratio adds the 1mL aqueous ascorbic acid in the Silver Nitrate mixing solutions of above-mentioned argentiferous crystal seed colloidal sol;
Sodium hydroxide solution with 1mol/L is adjusted to 8 with the above-mentioned PH that contains the mixing solutions of xitix, continues magnetic agitation 6h at last again, can obtain 20mL concentration and be roughly 1 * 10
-3The silver nano-grain colloidal sol of mol/L;
The Fluress of preparation silver-containing nanoparticles: preparation 2mL concentration is 1 * 10
-3The uranine ethanolic soln of mol/L is got 1mL uranine ethanolic soln and is joined in the mixed solution that 8.95mL absolute ethyl alcohol and 0.05mL deionized water form, and obtaining 10mL uranine concentration is 1 * 10
-4Mol/L is used as blank correlated Fluress.
Toward other 1mL concentration is 1 * 10
-3Add the 8.95mL absolute ethyl alcohol in the uranine ethanolic soln of mol/L, drip the silver nano-grain colloidal sol 0.05mL of above-mentioned preparation after shaking up again, shaking up and promptly obtaining uranine content is 1 * 10
-4Mol/L, silver content are 5 * 10
-6The Fluress of mol/L with silver nano-grain;
The luminous intensity of present embodiment empty contrast is shown in the curve a among Fig. 1, and the luminous intensity of uranine that contains embodiment of the invention silver nano-grain is shown in the curve b among Fig. 1.As can beappreciated from fig. 1, the luminous intensity of curve b is about 2.5 times of luminous intensity of curve a.The method of the embodiment of the invention has significant enhancement to the uranine luminous intensity.
The embodiment of the invention provides a kind of Fluress preparation method of containing metal nano particle, and is specific as follows:
Preparation Jin Jing plants colloidal sol: preparation contains the aqueous solution 20mL of 0.1mmol/L hydrochloro-auric acid and 0.05mmol/L PVP;
Compound concentration is the sodium borohydride aqueous solution of 0.1mol/L;
In the ratio of Peng Qinghuana and the amount of substance of hydrochloro-auric acid is that 15: 1 ratio adds the 0.3mL sodium borohydride aqueous solution fast in the hydrochloro-auric acid mixing solutions, and continuation magnetic agitation 15min, and at room temperature ageing 12h obtains Jin Jing and plants colloidal sol then;
Preparation gold nano particle colloidal sols: the 4.12mg hydrochloro-auric acid is dissolved in the 17mL deionized water, and is 5 * 10 by CTAB content
-3G/mL adds 0.085gCTAB in aqueous solution of chloraurate;
1: 8.5 ratio of the volume ratio of down payment crystal seed colloidal sol and aqueous solution of chloraurate is added 2mL Jin Jing in the aqueous solution of chloraurate and is planted colloidal sol, obtains containing the hydrochloro-auric acid mixed solution that Jin Jing plants colloidal sol;
Compound concentration is the aqueous ascorbic acid of 0.04mol/L;
In the ratio of the amount of substance of xitix metallizing thing is that 4: 1 ratio is planted toward the above-mentioned Jin Jing of containing in the hydrochloro-auric acid mixed solution of colloidal sol and added the 1mL aqueous ascorbic acid;
The above-mentioned mixing solutions pH value that contains xitix is adjusted to 9 with the sodium hydroxide solution of 1mol/L, continues magnetic agitation 4h at last again, can obtain 20mL concentration and be about 5 * 10
-4The gold nano particle colloidal sols of mol/L;
Preparation contains the Fluress of gold nano grain: preparation 2mL concentration is 5 * 10
-5The uranine ethanolic soln of mol/L is got 1mL uranine ethanolic soln and is joined in the mixed solution that 8.98mL absolute ethyl alcohol and 0.02mL deionized water form, and obtaining 10mL uranine concentration is 5 * 10
-6Mol/L is used as blank correlated Fluress.
Toward other 1mL concentration is 5 * 10
-5Add the 8.98mL absolute ethyl alcohol in the uranine ethanolic soln of mol/L, drip the gold nano colloidal sol 0.02mL of above-mentioned preparation after shaking up again, shaking up and promptly obtaining uranine content is 5 * 10
-6Mol/L, gold content are 1 * 10
-6The Fluress of mol/L with fluorescence enhancement;
The luminous intensity of the blank of the embodiment of the invention is shown in curve a among Fig. 2; The luminous intensity of uranine that contains embodiment of the invention gold nano grain is shown in curve b among Fig. 2.As can beappreciated from fig. 2, the luminous intensity of curve b is about 3 times of luminous intensity of curve a.The method of the embodiment of the invention has significant enhancement to the luminous intensity of uranine.
Embodiment 3
The embodiment of the invention provides a kind of Fluress preparation method of containing metal nano particle, and is specific as follows:
Prepare silver-colored crystal seed colloidal sol: preparation contains the aqueous solution 20mL of 0.025mmol/L Silver Nitrate and 0.25mmol/L Trisodium Citrate;
Compound concentration is 1 * 10
-3The sodium borohydride aqueous solution of mol/L;
In the ratio of Peng Qinghuana and the amount of substance of Silver Nitrate is that 5: 1 ratio adds the 0.5mL sodium borohydride aqueous solution fast in the Silver Nitrate mixing solutions, and continuation magnetic agitation 20min, and at room temperature ageing 6h obtains silver-colored crystal seed colloidal sol then;
Preparation silver nano-grain colloidal sol: the 6.8mg Silver Nitrate is dissolved in the 30mL deionized water, and is 1 * 10 by CTAB content
-2G/mL adds 0.3gCTAB in silver nitrate aqueous solution;
1: 3.75 ratio of volume ratio in silver-colored crystal seed colloidal sol and silver nitrate aqueous solution is added 8mL silver crystal seed colloidal sol in silver nitrate aqueous solution, obtain the Silver Nitrate mixing solutions of argentiferous crystal seed colloidal sol;
Compound concentration is the aqueous ascorbic acid of 0.1mol/L;
In the ratio of the amount of substance of xitix metallizing thing is that 5: 1 ratio adds the 2mL aqueous ascorbic acid in the Silver Nitrate mixing solutions of above-mentioned argentiferous crystal seed;
The pH value of gained mixing solutions is adjusted to 10 with the sodium hydroxide solution of 1mol/L, continues magnetic agitation 3h at last again, can obtain 40mL concentration and be about 1 * 10
-3The silver nano-grain colloidal sol of mol/L;
The Fluress of preparation silver-containing nanoparticles: preparation 2mL concentration is 5 * 10
-4The uranine ethanolic soln of mol/L is got 1mL uranine ethanolic soln and is joined in the 9mL deionized water, and obtaining 10mL uranine concentration is 5 * 10
-5Mol/L is used as blank correlated Fluress;
Toward other 1mL concentration is 5 * 10
-4Add the 8.9mL deionized water in the uranine ethanolic soln of mol/L, drip the silver-colored Nano sol 0.1mL of above-mentioned preparation after shaking up again, shaking up and promptly obtaining uranine content is 5 * 10
-5Mol/L, silver content are 1 * 10
-5The Fluress of mol/L with fluorescence enhancement.
The luminous intensity of the blank of the embodiment of the invention is shown in curve a among Fig. 3, and the luminous intensity of uranine of silver nano-grain that contains the embodiment of the invention is shown in curve b among Fig. 3.As can beappreciated from fig. 3, the luminous intensity of curve b is about 3.3 times of luminous intensity of curve a.The method of the embodiment of the invention has significant enhancing to the uranine luminous intensity.
Embodiment 4
The embodiment of the invention provides a kind of Fluress preparation method of containing metal nano particle, and is specific as follows:
Preparation platinum crystal seed colloidal sol: preparation contains the aqueous solution 20mL of 0.05mmol/L Platinic chloride and 0.2mmol/LPVP;
Compound concentration is 1 * 10
-2The POTASSIUM BOROHYDRIDE 97MIN aqueous solution of mol/L;
In the ratio of POTASSIUM BOROHYDRIDE 97MIN and the amount of substance of Platinic chloride is that 12: 1 ratio adds the 1.2mL POTASSIUM BOROHYDRIDE 97MIN aqueous solution fast in the Platinic chloride mixing solutions, and continuation magnetic agitation 30min, and at room temperature ageing 10h obtains platinum crystal seed colloidal sol then;
Preparation Pt nanoparticle colloidal sol: the 5.18mg Platinic chloride is dissolved in the 93mL deionized water, and is 1 * 10 by CTAB content
-4G/mL adds 0.0093gCTAB in chloroplatinic acid aqueous solution;
1: 18.6 ratio of volume ratio in platinum crystal seed colloidal sol and chloroplatinic acid aqueous solution is added 5mL platinum crystal seed colloidal sol in chloroplatinic acid aqueous solution, obtain the Platinic chloride mixing solutions of platiniferous crystal seed colloidal sol;
Compound concentration is the aqueous ascorbic acid of 0.05mol/L, and is that 10: 1 ratio adds the 2mL aqueous ascorbic acid in the Platinic chloride mixing solutions of above-mentioned platiniferous crystal seed in the ratio of the amount of substance of xitix metallizing thing;
The pH value that will contain the mixing solutions of xitix is adjusted to 11 with the sodium hydroxide solution of 1mol/L, continues magnetic agitation 3h at last again, can obtain 100mL concentration and be about 1 * 10
-4The Pt nanoparticle colloidal sol of mol/L;
Preparation contains the Fluress of Pt nanoparticle: preparation 1mL concentration is 1 * 10
-6The uranine aqueous solution of mol/L adds the 8.99mL deionized water in this uranine aqueous solution, drip the platinum Nano sol 0.01mL of above-mentioned preparation after shaking up again, and shaking up and promptly obtaining uranine content is 1 * 10
-7Mol/L, platinum content are 1 * 10
-7The Fluress of mol/L.
The method of the embodiment of the invention also has enhancement to the luminous intensity of uranine and noted earlier basic identical, does not just repeat at this.
Embodiment 5
The embodiment of the invention provides a kind of Fluress preparation method of containing metal nano particle, and is specific as follows:
Preparation palladium crystal seed colloidal sol: preparation contains the aqueous solution 20mL of 0.2mmol/L Palladous chloride and 0.3mmol/LPVP;
Compound concentration is 5 * 10
-2The POTASSIUM BOROHYDRIDE 97MIN aqueous solution of mol/L;
In the ratio of POTASSIUM BOROHYDRIDE 97MIN and the amount of substance of Palladous chloride is that 9: 1 ratio adds the 0.72mL POTASSIUM BOROHYDRIDE 97MIN aqueous solution fast in the Palladous chloride mixing solutions, and continuation magnetic agitation 60min, and at room temperature ageing 8h obtains palladium crystal seed colloidal sol then;
Preparation palladium nano-particles colloidal sol: the 5.3mg Palladous chloride is dissolved in the 28mL deionized water, and is 5 * 10 by CTAB content
-2G/mL adds 1.4gCTAB in palladium chloride aqueous solution;
1: 28 ratio of volume ratio in palladium crystal seed colloidal sol and palladium chloride aqueous solution is added 1mL palladium crystal seed colloidal sol in palladium chloride aqueous solution, obtain containing the Palladous chloride mixing solutions of palladium crystal seed colloidal sol;
Compound concentration is the aqueous ascorbic acid of 0.18mol/L, and is that 6: 1 ratio adds the 1mL aqueous ascorbic acid in the ratio of the amount of substance of xitix metallizing thing in the above-mentioned Palladous chloride mixing solutions that contains the palladium crystal seed;
The pH value of the above-mentioned mixing solutions that contains xitix is adjusted to 12 with the sodium hydroxide solution of 1mol/L, continues magnetic agitation 1h at last again, can obtain 30mL concentration and be about 1 * 10
-3The palladium nano-particles colloidal sol of mol/L;
Preparation contains the Fluress of palladium nano-particles: preparation 1mL concentration is 1 * 10
-2The uranine aqueous solution of mol/L adds the 8mL deionized water in this uranine aqueous solution, drip the palladium Nano sol 1mL of above-mentioned preparation after shaking up again, and shaking up and promptly obtaining uranine content is 1 * 10
-3Mol/L, palladium content are 1 * 10
-4The Fluress of mol/L.
The method of the embodiment of the invention also has enhancement to the luminous intensity of uranine and noted earlier basic identical, does not just repeat at this.
Comparative Examples 6
Take by weighing the 0.0034g Silver Nitrate and be dissolved in the 19mL deionized water, in silver nitrate aqueous solution, add 0.035g Trisodium Citrate and 0.035gPVP then;
Under quick condition of stirring, adding 1mL concentration fast is the Hydrazine Hydrate 80 of 100mM, stirring reaction 40min afterwards, and promptly getting silver content is 1 * 10
-3Mol/L silver nano-grain colloidal sol.(concentration of Silver Nitrate in wherein testing, the addition of Trisodium Citrate and PVP is adjustable, and the reaction times can suitably change, the add-on of Hydrazine Hydrate 80 is along with the amount of Silver Nitrate changes (purpose is to guarantee to be reduced into silver-colored particle to silver ions fully) accordingly)
Preparation 2mL concentration is 5 * 10
-4The uranine ethanolic soln of mol/L is got 1mL uranine ethanolic soln and is joined in the 9mL deionized water, and obtaining 10mL uranine concentration is 5 * 10
-5Mol/L is used as blank correlated Fluress;
Toward other 1mL concentration is 5 * 10
-4Add the 8.9mL deionized water in the uranine ethanolic soln of mol/L, drip the silver-colored Nano sol 0.1mL of above-mentioned preparation after shaking up again, shaking up and promptly obtaining uranine content is 5 * 10
-5Mol/L, silver content are 1 * 10
-5The Fluress of mol/L with fluorescence enhancement.(this implements the silver concentration in row gained silver sol, and the silver concentration in uranine concentration and the uranine is consistent with embodiment 3 all)
The luminous intensity of the blank of Comparative Examples 6 is shown in curve a among Fig. 4, and the uranine luminous intensity of silver nano-grain that contains Comparative Examples 6 is shown in curve b among Fig. 4.Can find out that from figure the luminous intensity of the luminous strength ratio curve a of curve b is strong by 27.5%.The preparation method of Comparative Examples 6 is not very obvious to the enhancement of uranine luminous intensity.And the embodiment of the invention 1,2,3, the resorcinolphthalein luminous intensity is remained on more than the twice; Therefore the luminous intensity of the Fluress of the method for embodiment of the invention acquisition is significantly strengthened; Surpass the Fluress that contains nano particle colloidal sol of containing metal nano particle colloidal sol not or the preparation of other reductive agent, have remarkable advantages.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the Fluress preparation method of a containing metal nano particle comprises the steps:
The mixing solutions of preparing metal compound and organic additive and alkali metal borohydride solution; The concentration of said metallic compound is below 0.5mmol/L; The mixing solutions of said alkali metal borohydride solution, metallic compound and organic additive is mixed, and ageing makes metal crystal seed colloidal sol; Wherein, said organic additive is Trisodium Citrate, Tripotassium Citrate or Vinylpyrrolidone polymer;
The preparing metal compound water solution adds cetyl trimethylammonium bromide and said metal crystal seed colloidal sol at the said metallic compound aqueous solution, obtains the metallic compound mixed solution of containing metal crystal seed colloidal sol; In the metallic compound mixed solution of said containing metal crystal seed colloidal sol, add xitix, the solution pH value is adjusted into alkalescence, the metals ion in the compound liquid of reducing metal obtains metal nanoparticle colloidal sol;
The preparation Fluress adds described metal nanoparticle colloidal sol, obtains the Fluress of containing metal nano particle; Wherein, the content of above-mentioned metal in Fluress is 1 * 10
-4-1 * 10
-7Mol/L.
2. preparation method as claimed in claim 1 is characterized in that said metallic compound comprises one or more in Silver Nitrate, hydrochloro-auric acid, Platinic chloride, the Palladous chloride.
3. preparation method as claimed in claim 1 is characterized in that, the concentration of said organic additive in the mixing solutions of said metallic compound and organic additive is 0.05-0.5mmol/L.
4. preparation method as claimed in claim 1 is characterized in that, the concentration of said metallic compound in the mixing solutions of said metallic compound and organic additive is 0.01-0.5mmol/L.
5. preparation method as claimed in claim 1 is characterized in that, said alkali metal borohydride is a kind of in Peng Qinghuana or the solution of potassium borohydride, and the concentration of said alkali metal borohydride solution is 1 * 10
-3-1 * 10
-1Mol/L.
6. preparation method as claimed in claim 1; It is characterized in that; In the said mixing solutions blended step with said alkali metal borohydride solution, metallic compound and organic additive, press said alkali metal borohydride and metallic compound mol ratio 3.6: 1-15: 1 mixes.
7. preparation method as claimed in claim 1; It is characterized in that; Said in said metallic compound aqueous solution adding cetyl trimethylammonium bromide and said metal crystal seed colloidal sol step, the concentration of said cetyl trimethylammonium bromide in the said metallic compound aqueous solution is 1 * 10
-4-5 * 10
-2G/ml.
8. preparation method as claimed in claim 1; It is characterized in that; Said in the step of said metallic compound aqueous solution adding cetyl trimethylammonium bromide and said metal crystal seed colloidal sol, be 1 by said metal crystal seed colloidal sol and metallic compound aqueous solution volume ratio: 37-1: 3.75 mix.
9. preparation method as claimed in claim 1 is characterized in that, in the said step that in the metallic compound mixed solution of said containing metal crystal seed colloidal sol, adds xitix, the add-on of said xitix and the mol ratio of metallic compound are 1: 1-10: 1.
10. preparation method as claimed in claim 1 is characterized in that, said pH value is 8-12.
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| WO2014118041A1 (en) * | 2013-02-04 | 2014-08-07 | Siemens Aktiengesellschaft | Stabilization of aqueous xanthene dye solutions by means of antichaotropic compounds |
| CN108395887A (en) * | 2018-05-03 | 2018-08-14 | 西安交通大学 | A kind of preparation method of fluorescent powder/noble metal nano particles composite material |
| CN108827923A (en) * | 2018-06-29 | 2018-11-16 | 天津科技大学 | A kind of low cost exempts to mark the new method of quickly detection organophosphorus pesticide without enzyme |
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| CN101191794A (en) * | 2007-08-27 | 2008-06-04 | 中国科学院理化技术研究所 | One-dimensional nanostructured fluorescent chemical biosensor and method for making same and uses |
| US20100008854A1 (en) * | 2008-07-11 | 2010-01-14 | Seung Joo Haam | Metal nanocomposite, preparation method and use thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101191794A (en) * | 2007-08-27 | 2008-06-04 | 中国科学院理化技术研究所 | One-dimensional nanostructured fluorescent chemical biosensor and method for making same and uses |
| US20100008854A1 (en) * | 2008-07-11 | 2010-01-14 | Seung Joo Haam | Metal nanocomposite, preparation method and use thereof |
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| Title |
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| 余林海等: "纳米金对荧光素的荧光增效作用", 《分析化学研究简报》 * |
| 孙双姣等: "金纳米微粒的制备和表征及其在生化分析中的应用", 《贵金属》 * |
| 庄严等: "金纳米粒子对染料分子光学性质的影响", 《稀有金属材料与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014118041A1 (en) * | 2013-02-04 | 2014-08-07 | Siemens Aktiengesellschaft | Stabilization of aqueous xanthene dye solutions by means of antichaotropic compounds |
| CN108395887A (en) * | 2018-05-03 | 2018-08-14 | 西安交通大学 | A kind of preparation method of fluorescent powder/noble metal nano particles composite material |
| CN108827923A (en) * | 2018-06-29 | 2018-11-16 | 天津科技大学 | A kind of low cost exempts to mark the new method of quickly detection organophosphorus pesticide without enzyme |
| CN108827923B (en) * | 2018-06-29 | 2021-05-07 | 天津科技大学 | Novel method for quickly detecting organophosphorus pesticide with low cost and without enzyme or label |
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| CN102337119B (en) | 2014-05-07 |
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