CN103357885A - Preparation method and application for Raman-enhanced silver colloid - Google Patents
Preparation method and application for Raman-enhanced silver colloid Download PDFInfo
- Publication number
- CN103357885A CN103357885A CN2012100959635A CN201210095963A CN103357885A CN 103357885 A CN103357885 A CN 103357885A CN 2012100959635 A CN2012100959635 A CN 2012100959635A CN 201210095963 A CN201210095963 A CN 201210095963A CN 103357885 A CN103357885 A CN 103357885A
- Authority
- CN
- China
- Prior art keywords
- raman
- elargol
- preparation
- strengthens
- melamine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention provides a preparation method for Raman-enhanced silver colloid. The preparation method includes steps of respectively preparing silver nitrate solution with the molar concentration of 8X10(-4)-1.5X10(-3)mol/L and sodium citrate aqueous solution with the molar concentration of 3.2X10(-2)-3.4X10(-2)mol/L; stirring or vibrating the silver nitrate solution, heating the silver nitrate solution by microwaves, dripping sodium citrate into the silver nitrate solution to obtain a mixture after the silver nitrate solution is boiling, and heating the mixture by microwaves until the mixture is boiling to obtain the Raman-enhanced silver colloid. The total amount of substrates of the dripped sodium citrate is 1.5-1.7 times that of silver nitrate. The invention further provides application of the Raman-enhanced silver colloid prepared by the preparation method to melamine detection.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to preparation method and application thereof that a kind of Raman strengthens elargol.
Background technology
Raman spectrum (Raman spectra) is a kind of scattering spectrum.The Raman spectrum analysis method is based on the Raman scattering effect that India scientist C.V. Raman (Raman) was found in nineteen twenty-eight, obtain molecular vibration, rotation aspect information for the different scattering spectrum analysis of incident light frequency, and be applied to a kind of analytical method of molecular structure research.The advantages such as Raman detection is quick, accurate because of it, can't harm more and more are widely used in each detection field.But Raman detection still has its shortcoming so far, that be exactly one of Raman scattering light intensity percentage of only accounting for incident laser intensity even 1,000,000/, if only strengthen Raman signal then produce little effect by improving incident intensity! And cross strong incident laser and can destroy some detected materials and make it that some physical and chemical changes occur, thereby do not reach accurately and the purpose of Non-Destructive Testing.
1974, the people such as Fleishmann found, smooth silver electrode surface is carried out after roughening processes, and obtained to be adsorbed on first the high-quality Raman spectrum of monolayer Pyridine Molecules on the silver electrode surface.Subsequently VanDuyne and partner thereof the experiment by system is compared with the Raman scattering signal of pyridine in calculating the Raman scattering signal of finding to be adsorbed on each Pyridine Molecules on the coarse silver surface and solution phase, strengthen about 6 orders of magnitude (namely 1,000,000 times), point out that this is a kind of surface enhanced effect relevant with rough surface, is called as the SERS effect.
SERS (SERS), be adsorbed on the compound of roughening metal surface because the surperficial local plasmon excimer caused Electromagnetic enhancement that is excited, and the cluster on the rough surface and adsorb the active site that the molecular composition Raman on it strengthens, the two effect makes the Raman scattering of determinand produce great enhancement effect.Its enhancer can reach 10
3～10
7, found that the metal that can produce SERS has a few metals such as Ag, take the enhancement effect of Ag as best, the most commonly used.This technology has selectively good and highly sensitive advantage, and actual detectability can reach 10～12 gram levels.Can distinguish the different molecule of the same race of isomer, Adsorption on Surface orientation etc., be the important tool of research surface and interface process, is the powerful measure of the close compound of Qualitative Identification chemical constitution.Can be used as the detector of liquid-phase chromatographic analysis.
Application number is that the Chinese patent of 200910045447.X discloses a kind of method for preparing silver nano-particles with surface-enhanced Raman effects.Its preparation method may further comprise the steps: (1) is dissolved in the silver nitrate of 0.0255g in the 150mL ultra-pure water; (2) plant acid solution of adding 5mL dilute concentration; (3) mentioned solution is quickly heated up to boiling; (4) slowly add the trisodium citrate of 3mL 1%; (5) keep the solution boiling temperature, reacted 6 hours, make colloidal sol; (6) colloidal sol that makes is at room temperature cooled off, 4 ℃ of lower preservations.
Application number is the preparation facilities that 200610020241.8 Chinese patent discloses a kind of nano silver colloid.Described device comprises the drive circuit, phase inverter of step-down, rectification, voltage stabilizing and stabling current installation composition, as 99.99% fine silver sheet of positive and negative electrode and the agitating device that brine electrolysis is flowed, the dispersant of nano silver colloid forms by distilled water or through the pure water of water quality adjustment, water softening, electric current is soluble in water by generation silver ion and particulate silver behind the fine silver sheet, become the colloid dispersate, obtain the nano silver colloid with definite concentration.
Application number is that 200610066967.5 Chinese patent discloses a kind of nano-class silver colloidal solution and preparation method thereof, by stabilizing agent, mix reducing agent I, mix reducing agent II, silver salt, pure water form.
Application number is the preparation method that 201010166358.3 Chinese patent discloses nano-class silver colloidal solution, be 0.1%～10% alkylation cyclodextrin aqueous solution with molality with mass percent to be that the silver ammino solution of 0.01～1.0mol/L mixes with 1: 100～1: 10 volume ratio, under 10～100 ℃ temperature conditions, stir 1～120min, namely obtain the nano-class silver colloidal solution that average grain diameter is 1～100nm.
The weak point that above patented technology method exists is:
1. nanometer elargol preparation time is oversize, keeps the solution boiling temperature, reacts 6 hours, makes colloidal sol;
2. the preparation facilities of the complexity that the needs that have are special comprises drive circuit, phase inverter of step-down, rectification, voltage stabilizing and stabling current installation composition etc.;
3. the complex chemical composition that has comprises stabilizing agent, mixing reducing agent I, mixes reducing agent II, silver salt, pure water composition.Solvent uses wide in variety, causes easily environmental pollution;
4. the Nano Silver size distribution that obtains is wide, is unfavorable for further application.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective of prior art, provides a kind of Raman to strengthen preparation method and the application thereof of elargol.
The present invention is achieved in that a kind of Raman strengthens the preparation method of elargol, and it comprises the steps:
Preparing respectively molar concentration is 8 * 10
-4～1.5 * 10
-3The liquor argenti nitratis ophthalmicus of mol/L and molar concentration are 3.2 * 10
-2～3.4 * 10
-2The sodium citrate aqueous solution of mol/L;
Stir or shake described liquor argenti nitratis ophthalmicus, and it is carried out heating using microwave, after the solution boiling, splash into natrium citricum, heating using microwave obtains described Raman and strengthens elargol to boiling, and wherein, total amount of substance of the natrium citricum of dropping is 1.5～1.7 times of silver nitrate.
And the Raman that the preparation method of above-mentioned Raman enhancing elargol obtains strengthens the application of elargol in Raman spectroscopy detection melamine.
Raman of the present invention strengthens the preparation method of elargol, and simple, preparation process is quick, and it is remarkable that the Raman for preparing strengthens elargol surface enhancing effect.The enhancing elargol that the preparation method who uses Raman of the present invention to strengthen elargol obtains can be realized smoothly all multicomponent mensuration such as food, medicine, feed, chemical products, comprise the mensuration of various raw materials, semi-finished product, finished product and the illegal additive of various additives etc., particularly can realize detecting to the low content composition.For guaranteeing the quality of food, medicine, health and the life security of safeguarding the consumer provide safeguard, simultaneously can greatly reduce the product testing cost, the hope that makes the production scene fast, accurately screen substandard product becomes a reality, in time stop low-quality goods and flow to market, its economic benefit and social benefit all are very considerable.
Description of drawings
Fig. 1 is the flow chart that the Raman of the embodiment of the invention strengthens the elargol preparation method;
Fig. 2 is that the nanometer elargol of heating by electric cooker preparation is used for the spectrogram that the metrifonate LR laser raman is measured;
Fig. 3 is that the Raman of the embodiment of the invention strengthens the spectrogram that elargol is used for metrifonate LR laser raman mensuration;
Fig. 4 is the LR laser raman spectrogram that the embodiment of the invention 2 is measured melamine;
Fig. 5 is the LR laser raman spectrogram that the embodiment of the invention 3 is measured melamine;
Fig. 6 is the LR laser raman spectrogram that the embodiment of the invention 4 is measured melamine;
Fig. 7 is the LR laser raman spectrogram that the embodiment of the invention 5 is measured melamine;
Fig. 8 is the LR laser raman spectrogram that the embodiment of the invention 6 is measured melamine;
Fig. 9 is the LR laser raman spectrogram that Comparative Examples 1 of the present invention is measured melamine;
Figure 10 is the LR laser raman spectrogram that Comparative Examples 2 of the present invention is measured melamine;
Figure 11 is the LR laser raman spectrogram that Comparative Examples 3 of the present invention is measured water.
The specific embodiment
In order to make purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
See also Fig. 1, the embodiment of the invention is shown provides a kind of Raman to strengthen the preparation method of elargol, and it comprises the steps:
S01: preparing respectively molar concentration is 8 * 10
-4～1.5 * 10
-3The liquor argenti nitratis ophthalmicus of mol/L and molar concentration are 3.2 * 10
-2～3.4 * 10
-2The sodium citrate aqueous solution of mol/L;
S02: stir or shake described liquor argenti nitratis ophthalmicus, and it is carried out heating using microwave, after the solution boiling, splash into natrium citricum, heating using microwave obtains described Raman and strengthens elargol to boiling, wherein, total amount of substance of the natrium citricum of dropping is 1.5～1.7 times of silver nitrate.
Among the step S01, the concentration of silver nitrate and the concentration of natrium citricum are all influential to size and the pattern of the Raman enhancing elargol of last acquisition, and silver nitrate concentration overrich, the nanometer elargol that obtains tend to reunite, and size is inhomogeneous.Silver nitrate concentration is excessively low, and the nanometre glue of acquisition is known from experience affects the effect that Raman strengthens.Preferably, the concentration of silver nitrate is 9 * 10
-4～1.1 * 10
-3Mol/L.Natrium citricum can play the effect of stabilizing agent, does not need additionally to add surfactant again, namely can obtain uniform Raman enhancing elargol by adjusting subsequent parameter.
Among the step S02, stir or shake described liquor argenti nitratis ophthalmicus and be preferably 20～40min, and it is carried out heating using microwave, behind solution boiling 1～3min, splash into sodium citrate solution, stir rapidly, it is kept evenly, after being heated to boiling again, splash into sodium citrate solution, repeat 3～5 times.Total amount of substance of the natrium citricum that drips is 1.5～1.7 times of silver nitrate.More preferably, the Raman that obtains being strengthened elargol purifies with centrifugal method.Particularly, this method of purification is: under 10000～15000 rev/mins speed, and centrifugal 5～10min, remove supernatant, i.e. less the and deformed silver-colored particulate of particle, precipitation adds again ultrasonic dispersion behind the water, so repeat 2～4 times, can obtain the higher Raman of purity and strengthen elargol.Adopt heating using microwave can obtain Raman and strengthen preferably elargol of effect.If adopt the common mode heating, such as electrical heating, the modes such as oil bath heating heat liquor argenti nitratis ophthalmicus, also can obtain the nanometer elargol, but adopt nanometer elargol poor effect in " metrifonate " standard liquid (concentration is 100 μ g/mL) is measured of common mode heating acquisition, the characteristic peak of " metrifonate " do not occur.Fig. 2 is the nanometer elargol that the mode of employing heating by electric cooker adds hot preparation, and it is to the non-constant of enhancing effect of the Raman spectrogram of metrifonate, and the significantly characteristic peak of " metrifonate " appears in the nanometer elargol that adopts heating using microwave to obtain under the similarity condition, see Fig. 3.
The preparation method that Raman provided by the invention strengthens elargol is simple, and the time is short, need not specific device, equipment is common, cheap, and need not the compounds such as stabilizing agent, surfactant, and is environment friendly and pollution-free, technical key point is grasped easily, and is with low cost, easily commercial application.
The Raman that the preparation method that the embodiment of the invention also provides this Raman to strengthen elargol obtains strengthens the application of elargol in Raman spectroscopy detection melamine.
Raman strengthens elargol can mix with solution to be detected after point on aluminium foil, dry or drying after carry out Raman spectroscopy, also can put first on aluminium foil, dry or drying after, upper melamine solution again, dry or dry after detection.The diameter of the sample spot that obtains on the aluminium foil is 2～4mm.Preferably, Raman is strengthened silver paste points on aluminium foil, the diameter of silver paste points is 2～4mm, dry or dry after room temperature drip again melamine solution after placing 24h, its Raman strengthens better effects if, from spectrogram, the enhancing at peak is more obvious.
1mg/mL (7.9 * 10
-3Mol/L) the melamine aqueous solution does not adopt enhancement measures, and laser Raman spectrometer is measured, and can't see any characteristic peak of melamine, and is the same with the collection of illustrative plates of pure water.If content is 3mg/kg (2.4 * 10
-5Mol/kg) extract just more can't have been measured with laser Raman spectrometer, and uses Raman to strengthen the characteristic peak that elargol just can obtain melamine.
At present, have report to detect melamine in the milk with the Ou Putusi Contrast agent, but their sample is interpolation a certain amount of melamine in the milk artificially.Strengthen the prepared Raman of elargol preparation method with above-mentioned Raman and strengthen elargol and not only can detect melamine in the milk, and can carry out to the problem milk powder that retains actual sample and detect.Because milk is different from the processing technology of milk powder, so that the detection of the melamine in the milk powder is more difficult.Directly adding melamine in the milk does not have heating process, and problem milk powder can heat in process, makes this water-soluble weak material of melamine in heating process, solution better, and dispersion more even causes the difficulty of extraction.The prepared Raman of preparation method that adopts Raman provided by the present invention to strengthen elargol strengthens elargol can detect melamine in the milk powder accurately in the LR laser raman method, compares additive method, more has simple and efficiently, and its detectability is also very low.
Below embodiment by concrete preparation method and application illustrate that above-mentioned LR laser raman strengthens the preparation method of elargol and the LR laser raman of preparation strengthens the application of elargol in melamine detects.
Embodiment 1:
Take by weighing 25mg silver nitrate reagent (analyzing pure) and be dissolved in the 150mL high purity water, get silver nitrate aqueous solution; The sodium citrate solution of preparation 1%: take by weighing the analytically pure natrium citricum of 1g, be settled to 100mL with high purity water, its molar concentration is 0.034mol/L.Above-mentioned silver nitrate aqueous solution is placed in the beaker of 400mL, at room temperature vigorous stirring 30min.The liquor argenti nitratis ophthalmicus that mixes is inserted microwave-oven-heating, behind solution boiling 1min, slowly splash into the sodium citrate solution of 1mL 1% in the solution with the droplet pipe, stir rapidly with glass bar, make it keep evenly being heated to again boiling, drip again the sodium citrate solution of 1mL 1%, stir rapidly with glass bar, it is kept evenly.Repeat above-mentioned steps, drip continuously 4 times, the total amount of sodium citrate solution reaches 4mL, obtains described LR laser raman and strengthens elargol.With supercentrifuge LR laser raman being strengthened elargol purifies, centrifuge tube with the 10mL volume, under 12000 rev/mins of conditions, then centrifugal 5min discards transparent supernatant in the centrifuge tube, and each centrifuge tube adds high purity water 5mL, centrifuge tube is covered tightly, insert in the ultrasonic cleaner, at room temperature ultrasonic concussion 5min carries out centrifugal treating according to above-mentioned condition after making the interior nano-Ag particles of pipe and high purity water fully mixing again; Collect all LR laser ramans enhancing elargol elargol after centrifugal three times and be settled to 7～10mL.
Embodiment 2:
The purified LR laser raman of embodiment 1 preparation is strengthened silver paste points on aluminium foil, and the diameter of round dot is about 3mm, after 45 ℃ of Electric heat oven dryings, put the melamine pressed powder at the aluminium foil that drips elargol, add lightshade cover, focus, carry out Raman spectroscopy, at characteristic peak 674.2cm
-1The intensity maximum can reach 56000 (seeing also Fig. 4).
Embodiment 3:
The melamine aqueous solution that the LR laser raman of embodiment 1 preparation is strengthened elargol and 1mg/mL is to mix at 1: 1 according to volume ratio, then puts 20 μ L on aluminium foil, and the diameter of round dot is about 3mm, after 45 ℃ of Electric heat oven dryings, carries out Raman spectroscopy, at 701.3cm
-1The peak intensity at place reaches 24000 (seeing also Fig. 5).
Embodiment 4:
With the LR laser raman of embodiment 1 preparation strengthen elargol with silver paste points on aluminium foil, the diameter of each round dot is about 3mm, after 45 ℃ of Electric heat oven dryings, goes up the melamine aqueous solution 10 μ L of 1mg/mL again, naturally dries rear Raman spectroscopy, at 701.3cm
-1The peak intensity at place reaches 17000 (seeing also Fig. 6).
Embodiment 5:
With the LR laser raman of embodiment 1 preparation strengthen elargol with silver paste points on aluminium foil, the diameter of each round dot is about 3mm, at room temperature places 25h after 45 ℃ of Electric heat oven dryings, the melamine aqueous solution 10 μ L of upper 1mg/mL, naturally dry rear Raman spectroscopy, at 679.6cm
-1The peak intensity at place reaches 28000 (seeing also Fig. 7).
Embodiment 6:
With the LR laser raman of embodiment 1 preparation strengthen elargol with silver paste points on aluminium foil, the diameter of each round dot is about 3mm, after 45 ℃ of Electric heat oven dryings, selects the melamine milk powder extract 10 μ L of 3mg/kg again, naturally dries rear Raman spectroscopy, at 679.6cm
-1The peak intensity at place is greater than 21000.(seeing also Fig. 8).Wherein, the preparation method of melamine milk powder extract is: take by weighing 2g (being accurate to 0.01g) milk powder and mould in the triangular flask in 50mL tool plug, add 15mL trichloroacetic acid solution (1%) and 5mL acetonitrile, ultrasonic extraction 10min, again behind the mechanical shaking extraction 10min, with the centrifugal 10min of 4000r/min.Supernatant is behind the Filter paper filtering of trichloroacetic acid solution-wet, be settled to 25mL with trichloroacetic acid solution, pipette 5mL filtrate and be transferred to solid-phase extraction column (mixed type cation exchange solid-phase extraction column, matrix are the polystyrene-divinylbenzene high polymer of benzene sulfonic acid, 60mg, 3mL) in.Use successively 3mL water and 3mL methanol wash, be evacuated near doing after, with 6mL ammonification methanol solution (accurately measuring 5mL ammoniacal liquor and 95mL methyl alcohol, mixing) wash-out.Whole SPE process flow velocity is no more than 1mL/min.Eluent blows near dried with nitrogen under 50 ℃, gets residue and measures.
Comparative Examples 1:
Utilize the light shield of laser Raman spectrometer, measured pure melamine standard reference material (purity is＞99.0%) pressed powder.Obtain principal character peak 674.2cm
-1, maximum intensity＞20000 (asking for an interview Fig. 9).
Comparative Examples 2:
Directly on aluminium foil, the diameter of round dot is about 3mm, after 45 ℃ of Electric heat oven dryings, carries out Raman spectroscopy (seeing also Figure 10) with the melamine aqueous solution of 20 μ L 1mg/mL.
Comparative Examples 3:
On aluminium foil, the diameter of round dot is about 3mm with 20 μ L pure water points, after 45 ℃ of Electric heat oven dryings, carries out Raman spectroscopy (seeing also Figure 11).
The characteristic peak of melamine has 385cm
-1, 586.8cm
-1, 674.2cm
-1, 776.3cm
-1, 985.1cm
-1, 1559.8cm
-1Deng.Can find out on the Raman collection of illustrative plates that obtains from Comparative Examples 1 (Fig. 9) and embodiment 2 (Fig. 4), adopt Raman to strengthen elargol after, melamine pressed powder characteristic peak strength increase is more than one times.Comparing embodiment 3 and embodiment 4, can find out, the Raman signal intensity that the method that embodiment 3 adopts first hybrid Raman to strengthen elargol and the melamine aqueous solution obtains is large, and among the embodiment 4, after nanometer elargol drying, the signal strength signal intensity of putting again the melamine aqueous solution is little, but Raman is strengthened after room temperature is placed 25h after the elargol drying characteristic peak 679.6cm
-1Intensity can reach 28000 (seeing also embodiment 5 and Fig. 7).Comparative Examples 2 does not adopt Raman to strengthen elargol, and its Raman spectrogram (Figure 10) be can't see the characteristic peak of melamine, and is the same with the Raman spectrogram (Figure 11) of pure water in the Comparative Examples 3.Need to prove, melamine solid and liquid, and the variation (red shift or blue shift) of Raman-shifted wavenumbers can occur in this characteristic peak when condition determination changes of liquid, such as 674.2cm
-1, 701.3cm
-1, 679.6cm
-1
The above only is preferred embodiment of the present invention, not in order to limiting the present invention, all any modifications of doing within the spirit and principles in the present invention, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the preparation method of a Raman enhancing elargol is characterized in that, comprises the steps:
Preparing respectively molar concentration is 8 * 10
-4～1.5 * 10
-3The liquor argenti nitratis ophthalmicus of mol/L and molar concentration are 3.2 * 10
-2～3.4 * 10
-2The sodium citrate aqueous solution of mol/L;
Stir or shake described liquor argenti nitratis ophthalmicus, and it is carried out heating using microwave, after the solution boiling, splash into natrium citricum, heating using microwave obtains described Raman and strengthens elargol to boiling, and wherein, total amount of substance of the natrium citricum of dropping is 1.5～1.7 times of silver nitrate.
2. Raman as claimed in claim 1 strengthens the preparation method of elargol, it is characterized in that, also comprises described Raman is strengthened the step that elargol carries out centrifugal purification.
3. Raman as claimed in claim 1 strengthens the preparation method of elargol, it is characterized in that the solubility of described liquor argenti nitratis ophthalmicus is 9 * 10
-4～1.1 * 10
-3Mol/L.
4. Raman as claimed in claim 2 strengthens the preparation method of elargol, it is characterized in that described centrifugal purification is under 10000～15000 rev/mins speed, and centrifugal 5～10min removes supernatant, and precipitation adds again ultrasonic dispersion behind the water.
5. Raman as claimed in claim 1 strengthens the preparation method of elargol, it is characterized in that the time of described stirring or concussion is 20～40min.
6. Raman as claimed in claim 1 strengthens the preparation method of elargol, it is characterized in that, described boiling keeps 1～3min.
7. Raman as claimed in claim 1 strengthens the preparation method of elargol, it is characterized in that the dropping of described natrium citricum divides to be carried out for 3～5 times.
8. strengthen the application of Raman enhancing elargol in Raman spectroscopy detection melamine of preparation method's acquisition of elargol such as the described Raman of claim 1～7.
9. Raman enhancing elargol as claimed in claim 8 is characterized in that in the application of Raman spectroscopy detection melamine described Raman strengthens silver paste points on aluminium foil, and oven dry after room temperature is placed 24h, is put the melamine sample again and carried out Raman mensuration.
10. Raman as claimed in claim 9 strengthens elargol in the application of Raman spectroscopy detection melamine, it is characterized in that, described Raman enhancing silver paste points is 2～4mm at the diameter of the silver paste points that aluminium foil forms.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210095963.5A CN103357885B (en) | 2012-04-01 | 2012-04-01 | A kind of Raman strengthens preparation method and the application thereof of elargol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210095963.5A CN103357885B (en) | 2012-04-01 | 2012-04-01 | A kind of Raman strengthens preparation method and the application thereof of elargol |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103357885A true CN103357885A (en) | 2013-10-23 |
| CN103357885B CN103357885B (en) | 2016-06-22 |
Family
ID=49360619
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210095963.5A Expired - Fee Related CN103357885B (en) | 2012-04-01 | 2012-04-01 | A kind of Raman strengthens preparation method and the application thereof of elargol |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103357885B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174916A (en) * | 2015-08-27 | 2015-12-23 | 哈尔滨工业大学 | Preparation method for nano-structure oxide ceramic material and application and detection method for trace substance amount by using the nano-structure oxide ceramic material |
| CN113637420A (en) * | 2021-07-16 | 2021-11-12 | 郑州大学 | Flexible Raman-enhanced adhesive tape and preparation method thereof |
| CN114437389A (en) * | 2022-03-02 | 2022-05-06 | 五邑大学 | Ordered nano-folded cellulose composite membrane with high surface Raman enhancement effect and preparation method thereof |
| CN115464132A (en) * | 2022-08-18 | 2022-12-13 | 太原理工大学 | Controllable preparation method of phytate-coated silver nanoparticles |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006045655A (en) * | 2004-08-09 | 2006-02-16 | Mitsubishi Materials Corp | Silver nanoparticle and production method therefor |
| CN101482509A (en) * | 2009-03-03 | 2009-07-15 | 福建师范大学 | Method for detecting animal active unicellular sample by surface reinforced Raman spectrum |
| CN101569932A (en) * | 2009-01-16 | 2009-11-04 | 上海师范大学 | Method for preparing silver nano-particles with surface-enhanced Raman effects |
| CN102175664A (en) * | 2011-02-17 | 2011-09-07 | 福建师范大学 | Method for detecting surface enhanced Raman spectra of blood RNA |
| CN102183502A (en) * | 2011-01-14 | 2011-09-14 | 楚雄师范学院 | Method for preparing nano silver film with enhanced Raman scattering substrate based on microwave technique |
| CN102288592A (en) * | 2011-05-18 | 2011-12-21 | 福建师范大学 | Method for quantitative detection of uric acid based on surface enhanced Raman spectroscopy (SERS) technology |
-
2012
- 2012-04-01 CN CN201210095963.5A patent/CN103357885B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006045655A (en) * | 2004-08-09 | 2006-02-16 | Mitsubishi Materials Corp | Silver nanoparticle and production method therefor |
| CN101569932A (en) * | 2009-01-16 | 2009-11-04 | 上海师范大学 | Method for preparing silver nano-particles with surface-enhanced Raman effects |
| CN101482509A (en) * | 2009-03-03 | 2009-07-15 | 福建师范大学 | Method for detecting animal active unicellular sample by surface reinforced Raman spectrum |
| CN102183502A (en) * | 2011-01-14 | 2011-09-14 | 楚雄师范学院 | Method for preparing nano silver film with enhanced Raman scattering substrate based on microwave technique |
| CN102175664A (en) * | 2011-02-17 | 2011-09-07 | 福建师范大学 | Method for detecting surface enhanced Raman spectra of blood RNA |
| CN102288592A (en) * | 2011-05-18 | 2011-12-21 | 福建师范大学 | Method for quantitative detection of uric acid based on surface enhanced Raman spectroscopy (SERS) technology |
Non-Patent Citations (3)
| Title |
|---|
| 刘琨等: "微波法制备银胶体及其在表面增强拉曼散射中的应用", 《光散射学报》 * |
| 王锭笙等: "亚单分子层三聚氰胺的便携式拉曼检测", 《光散射学报》 * |
| 马枫茹等: "以新型银胶为衬底的超低浓度R6G的拉曼光谱检测", 《光散射学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105174916A (en) * | 2015-08-27 | 2015-12-23 | 哈尔滨工业大学 | Preparation method for nano-structure oxide ceramic material and application and detection method for trace substance amount by using the nano-structure oxide ceramic material |
| CN105174916B (en) * | 2015-08-27 | 2017-06-16 | 哈尔滨工业大学 | Using micro-nano structure oxide ceramic material to the detection method of trace materials content |
| CN113637420A (en) * | 2021-07-16 | 2021-11-12 | 郑州大学 | Flexible Raman-enhanced adhesive tape and preparation method thereof |
| CN114437389A (en) * | 2022-03-02 | 2022-05-06 | 五邑大学 | Ordered nano-folded cellulose composite membrane with high surface Raman enhancement effect and preparation method thereof |
| CN114437389B (en) * | 2022-03-02 | 2023-11-07 | 五邑大学 | Ordered nano-pleated cellulose composite membrane with high surface Raman enhancement effect and preparation method thereof |
| CN115464132A (en) * | 2022-08-18 | 2022-12-13 | 太原理工大学 | Controllable preparation method of phytate-coated silver nanoparticles |
| CN115464132B (en) * | 2022-08-18 | 2024-04-12 | 太原理工大学 | Controllable preparation method of phytic acid coated silver nano particles |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103357885B (en) | 2016-06-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Hu et al. | Characterization and analytical separation of fluorescent carbon nanodots | |
| Xue et al. | Surface-imprinted core–shell Au nanoparticles for selective detection of bisphenol A based on surface-enhanced Raman scattering | |
| Awual et al. | Investigation of palladium (II) detection and recovery using ligand modified conjugate adsorbent | |
| Sánchez‐Cortés et al. | Anomalous Raman bands appearing in surface‐enhanced Raman spectra | |
| Tang et al. | Fabrication of Au nanorod‐coated Fe3O4 microspheres as SERS substrate for pesticide analysis by near‐infrared excitation | |
| Li et al. | Functional femtoliter droplets for ultrafast nanoextraction and supersensitive online microanalysis | |
| Ezoddin et al. | Ultrasound-assisted supramolecular dispersive liquid–liquid microextraction based on solidification of floating organic drops for preconcentration of palladium in water and road dust samples | |
| Lin et al. | Au nanoplates as robust, recyclable SERS substrates for ultrasensitive chemical sensing | |
| CN105108171B (en) | A kind of preparation method of the nano particle of strong Raman signal | |
| CN103357885A (en) | Preparation method and application for Raman-enhanced silver colloid | |
| CN103364388B (en) | A kind of laser raman detection method of Sudan red 1 | |
| Chen et al. | Ag‐nanoparticle‐modified single Ag nanowire for detection of melamine by surface‐enhanced Raman spectroscopy | |
| Fathirad et al. | Ultrasound-assisted emulsification solidified floating organic drops microextraction of ultra trace amount of Te (IV) prior to graphite furnace atomic absorption spectrometry determination | |
| CN102677212A (en) | Surface-enhanced Raman scattering active substrate and preparation method thereof | |
| Li et al. | Fabrication of pollutant-resistance SERS imprinted sensors based on SiO2@ TiO2@ Ag composites for selective detection of pyrethroids in water | |
| CN105567227A (en) | Method for extracting graphene quantum dots from coffee-ground solid waste | |
| Ghosh et al. | One-pot synthesis of 2-thenoyltrifluoroacetone surface functionalised SrF 2: Eu 3+ nanoparticles: trace level detection of water | |
| CN107589106B (en) | Method for preparing surface enhanced Raman scattering substrate | |
| Alvarez-Toral et al. | Synthesis of amino-functionalized silica nanoparticles for preparation of new laboratory standards | |
| Ye et al. | A simple label-free rhodamine 6G SERS probe for quantitative analysis of trace As 3+ in an aptamer–nanosol | |
| CN102980879B (en) | Preparation method of surface enhancement raman scattering substrate | |
| Guo et al. | Preparation of SiO2@ Ag@ molecular imprinted polymers hybrid for sensitive and selective detection of amoxicillin using surface-enhanced Raman scattering | |
| CN111289491B (en) | Method for detecting triadimefon and triadimenol in tobacco based on surface enhanced Raman spectroscopy | |
| Zhou et al. | Microwave-assisted preparation of boron acid modified expanded graphite for the determination of chloramphenicol in egg samples | |
| Ferrer et al. | Turning “on” and “off” nucleation and growth: Microwave assisted synthesis of CdS clusters and nanoparticles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 518055 Guangdong, Nanshan District, Taoyuan street, Ping Shan Industrial Park, the east side of the 9 floor, building 5, East Patentee after: SHENZHEN YU CHI TESTING TECHNOLOGY Co.,Ltd. Address before: 518055 Guangdong, Nanshan District, Taoyuan street, Ping Shan Industrial Park, the east side of the 9 floor, building 5, East Patentee before: SHENZHEN YU CHI DETECTION TECHNOLOGY Co.,Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160622 |