CN103207160B - Rapid determination method for thiocyanate with nanogold as coloring probe - Google Patents
Rapid determination method for thiocyanate with nanogold as coloring probe Download PDFInfo
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- CN103207160B CN103207160B CN201310124281.7A CN201310124281A CN103207160B CN 103207160 B CN103207160 B CN 103207160B CN 201310124281 A CN201310124281 A CN 201310124281A CN 103207160 B CN103207160 B CN 103207160B
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- thiocyanate
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Abstract
The invention discloses a rapid determination method for thiocyanate with nanogold as a coloring probe. The thiocyanate can selectively prevent the nanogold from aggregating in acid solution, so that changes of the color of solution and the characteristics of ultraviolet absorption spectrum can be shown. The method disclosed by the invention has high detection sensitivity. The detection limit of color changes observed by naked eyes is 1mumol/L, the linearity range of the ratio determination of absorbance is 0.25-2mumol/L and the detection limit of the ratio determination of absorbance is 0.14mumol/L. A water sample can be simply pretreated and then the content of thiocyanate radical in the water sample can be determined by the method.
Description
Technical field
The present invention relates to take the quick content assaying method of thiocyanate ion that nm of gold is colour developing probe, belong to analytical chemistry and field of nanometer technology.
Background technology
Nm of gold is because it is easy to preparation and biological functional, good biological stability and unique spectral characteristic paid close attention to widely.The surface plasma absorption band of nm of gold is positioned at the visible region of electromagnetic wave spectrum, and is subject to the impact of the pattern of Micelle-like Nano-structure of Two.Typical colloidal nano gold is claret, and their aggregation presents purple or blueness, and this is due to surface plasma absorption band due to nm of gold moves to long wavelength.Method based on this principle of change color in nm of gold accumulation process has been widely used in and has detected cell, protein, DNA, metallic ion and little molecule etc.Yet the accumulation process that it should be pointed out that nm of gold is subject to the impact of many external factor, therefore can produces false positive signal and obtain incorrect result.In order to obtain higher selectivity and accuracy, based on anti-gathering or the coloration method of the nm of gold of disperseing again become one and well select.
Thiocyanate (SCN
-) being widely used in medicine, dyeing, in the industries such as photograph.For example, due to the hypertoxicity chemical composition of its generation (CN
-, CNCl) can cause serious environment (especially aquatic environment) harm, therefore measuring thiocyanate has very important realistic meaning.At present, the detection method of thiocyanate mainly comprises atomic absorption spectrophotometry, electrochemical methods, vapor-phase chromatography, capillary electrophoresis, Micellar Electrokinetic Capillary Chromatography, the chromatography of ions etc.Yet, these method testing process relative complex, time-consuming, expensive and can relate to some harmful reagent.
The present invention is directly usingd nm of gold prepared by sodium citrate reducing process as colour developing probe, the characteristic (i.e. anti-aggregation) of utilizing thiocyanate energy selectivity to stop golden nanometer particle to be assembled, provides a kind of quick, safe, easy, sensitive thiocyanate new detecting method.
Summary of the invention
The object of the invention is to take nm of gold prepared by sodium citrate reducing process as colour developing probe, a kind of quick, safe, easy, sensitive thiocyanate new detecting method is provided.
To achieve these goals, the present invention is by the following technical solutions:
Of the present invention a kind of
take nm of gold as colour developing probe thiocyanate rapid assay methods, it is characterized in that utilizing thiocyanate energy selectivity to stop nm of gold in acid solution, to produce the characteristic of assembling, and the variation that shows solution colour and ultra-violet absorption spectrum feature comes
measure thiocyanate concn.
Described
take nm of gold as colour developing probe thiocyanate rapid assay methods, be characterized in utilizing the variation characteristic of visualization solution colour with the concentration of judgement thiocyanate.
Described
take nm of gold as colour developing probe thiocyanate rapid assay methods, be characterized in utilizing the absorbance ratio A of solution ultra-violet absorption spectrum
700/ A
520concentration with judgement thiocyanate.
Described
take nm of gold as colour developing probe thiocyanate rapid assay methodsbe characterized in that used nm of gold adopts the method preparation of sodium citrate reduction gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution that adds rapidly 3 milliliters of 0.1g/L, reaction solution is from the light yellow claret that becomes, after continuing to reflux 15 minutes, reaction solution is naturally cooled to room temperature and forms nm of gold.
Described
take nm of gold as colour developing probe thiocyanate rapid assay methodsbe characterized in that 5:1 mixes by nano-Au solution with containing variable concentrations thiocyanate salt solution by volume, adding 0.2 milliliter of sulfuric acid solution to make to mix sulfuric acid final concentration in rear solution is 8 mmol/L, places 5-8 minute for 30 ℃, visualization color characteristic or mensuration absorbance ratio A
700/ A
520, when visualization color characteristic, along with the increase of thiocyanate concn, the color of nm of gold becomes purple-aubergine-redness from blueness gradually, and the detection of visualization is limited to 1 μ mol/L; When measuring absorbance ratio A
700/ A
520time, the absorbance ratio A along with the increase of thiocyanate concn
700/ A
520reduce gradually Δ A within the scope of 2.5 ~ 2 μ mol/L
700/ A
520linear with thiocyanate concn, detect and be limited to 0.14 μ mol/L.
Described
take nm of gold as colour developing probe thiocyanate rapid assay methods, being characterized in that used nm of gold particle diameter is 13 nm, concentration is 3.2 nmol/L.
Described
take golden nanometer particle as colour developing probe thiocyanate rapid assay methodsbe characterized in that 5:1 by volume mixes by nano-Au solution with containing the testing sample thiocyanate salt solution of variable concentrations, adding 0.2 milliliter of sulfuric acid solution to make to mix sulfuric acid final concentration in rear solution is 8 mmol/L, places 5 minutes visualization color characteristic or mensuration absorbance ratio A for 30 ℃
700/ A
520concentration with judgement thiocyanate.
Described
take golden nanometer particle as colour developing probe thiocyanate rapid assay methods, be characterized in that the volume of thiocyanate salt solution and nano-Au solution is preferably 0.05 milliliter and 0.25 milliliter.
Of the present invention a kind of
take the method for nm of gold thiocyanate in colour developing probe Fast Measurement water sample, comprise the steps: that in the water sample of 10 milliliters, adding ethylenediamine tetraacetic acid to make to mix ethylenediamine tetraacetic acid final concentration in rear solution is 1 mmol/L, after 0.22 μ m membrane filtration, obtains sample solution; After adding 0.05 milliliter of above-mentioned sample solution and 0.2 milliliter of sulfuric acid to make to mix in 0.25 milliliter of nm of gold, in solution, sulfuric acid final concentration is 8 mmol/L, places 5 minutes then visualization change color or mensuration absorbance ratio A for 30 ℃
700/ A
520, according to solution colour and color standards series of comparisons or undertaken quantitatively by absorbance ratio typical curve, obtain
thiocyanate ion content in water sample.
Described
take the method for nm of gold thiocyanate in colour developing probe Fast Measurement water samplebe characterized in that used nm of gold adopts the method preparation of following sodium citrate reduction gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution that adds rapidly 3 milliliter of 0.1 g/L, reaction solution is from the light yellow claret that becomes, after continuing to reflux 15 minutes, reaction solution is naturally cooled to room temperature and forms nm of gold.
Specifically, technical scheme of the present invention is:
(1) preparation of nm of gold:
The all glasswares that use in following process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.The preparation method of nm of gold is: the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution that adds rapidly 3 milliliter of 0.1 g/L, reaction solution is by from the light yellow claret that becomes, after continuing to reflux 15 minutes, reaction solution is naturally cooled to room temperature.The nm of gold particle diameter of gained is 13 nm, and concentration is about 3.2 nmol/L, 4 ℃ of preservations.
(2) mensuration of thiocyanate
The nano-Au solution that adds 0.25 milliliter of step () to prepare in 0.05 milliliter of thiocyanate sample solution, then add 0.20 milliliter of 20 mmol/L sulfuric acid (in mixed solution, the final concentration of sulfuric acid is 8 mmol/L), after mixing, at 30 ℃, place 5 minutes the absorbance ratio (A at the variation of visualization color or mensuration 700 nm and 520 nm wavelength places
700/ A
520).According to solution colour and color standards series of comparisons or undertaken quantitatively by absorbance ratio typical curve.The detection of visualization is limited to 1 μ mol/L, and the detection of dulling luminosity ratio pH-value determination pH is limited to 0.14 μ mol/L.
Advantage of the present invention:
(1) the present invention is based on thiocyanate and can stop nm of gold in acid solution, to produce gathering, thereby show the variation of solution colour and ultra-violet absorption spectrum feature, can be directly used in the content detection of thiocyanate.
(2) nm of gold used in the present invention is directly obtained by sodium citrate reduction gold chloride, and without further modifying, preparation process is simple and quick.
(3) the present invention is low to the processing requirements of sample, and anti-interference is good, only needs to add ethylenediamine tetraacetic acid to measure in water sample.
(4) detection speed of the present invention is fast, can in 5 minutes, complete pre-service and the detection of actual water sample.
(5) detection sensitivity of the present invention is high, and the detection by visual inspection change color is limited to 1 μ mol/L, and the detection of dulling luminosity ratio pH-value determination pH is limited to 0.14 μ mol/L.
Accompanying drawing explanation
Fig. 1 is the uv absorption spectra of nm of gold under 8 mmol/L sulfuric acid existence conditions.
Fig. 2 is the uv absorption spectra after nm of gold and thiocyanate effect under 8 mmol/L sulfuric acid existence conditions.
Fig. 3 is the absorbance ratio figure after nm of gold and thiocyanate effect under different aggregation inducing agent effects.
Fig. 4 is the absorbance ratio figure after nm of gold and thiocyanate effect under variable concentrations sulfuric acid existence condition.
Fig. 5 is that under 8 mmol/L sulfuric acid existence conditions, the absorbance ratio after nm of gold and the effect of variable concentrations thiocyanate is schemed over time.
Fig. 6 is the change color figure after nm of gold and the effect of variable concentrations thiocyanate under 8 mmol/L sulfuric acid existence conditions.Concrete change color is from left to right shown as, and when thiocyanate not, solution is aobvious blue; When thiocyanate concn is 1 μ mol/L, solution shows purple; When thiocyanate concn is 1.5 μ mol/L, solution displaing amaranth; When thiocyanate concn is 2 μ mol/L, solution is aobvious red.
Fig. 7 is the absorbance ratio variation diagram after nm of gold and the effect of variable concentrations thiocyanate under 8 mmol/L sulfuric acid existence conditions.
Fig. 8 is Δ A under 8 mmol/L sulfuric acid existence conditions
700/ A
520(blank group A
700/ A
520deduct experimental group A
700/ A
520) with the linear relationship chart of thiocyanate concn.
Embodiment
Embodiment 1:
The chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution that adds rapidly 3 milliliter of 0.1 g/L, reaction solution, from the light yellow claret that becomes, after continuing to reflux 15 minutes, is slowly cooled to room temperature by reaction solution.The nm of gold particle diameter of gained is 13 nm, and concentration is about 3.2 nmol/L, 4 ℃ of preservations.The all glasswares that use in above process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.
Embodiment 2:
In the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 ml distilled water and 0.2 milliliter of sulfuric acid (after mixing, in solution, sulfuric acid final concentration is 8 mmol/L), place 5 minutes for 30 ℃.Nm of gold color becomes blueness from claret, absorbance ratio (A
700/ A
520) increase (see figure 1).
Embodiment 3:
In the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 milliliter of thiocyanate salt solution (after mixing, in solution, thiocyanate final concentration is 2 μ mol/L) and 0.2 milliliter of sulfuric acid (after mixing, in solution, sulfuric acid final concentration is 8 mmol/L), place 5 minutes for 30 ℃.Nm of gold color remains unchanged substantially, absorbance ratio (A
700/ A
520) compared with the little (see figure 2) of the absorbance ratio of embodiment 2.
Embodiment 4:
In the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 milliliter of thiocyanate salt solution (after mixing, in solution, thiocyanate final concentration is 2 μ mol/L) and 0.2 milliliter of different aggregation inducing agent (sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, acetic acid, sodium chloride) (after mixing, in solution, aggregation inducing agent final concentration is 8 mmol/L), place 5 minutes for 30 ℃, measure absorbance ratio A
700/ A
520.Blank group replaces thiocyanate salt solution with distilled water.As shown in Figure 3, by the caused Δ A of thiocyanate
700/ A
520(blank group A
700/ A
520deduct experimental group A
700/ A
520) in sulfuric acid solution, reach maximum.
Embodiment 5:
In the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 milliliter of thiocyanate salt solution (after mixing, in solution, thiocyanate final concentration is 2 μ mol/L) and 0.2 milliliter of variable concentrations (after mixing, in solution, sulfuric acid final concentration is 0-10 mmol/L) sulfuric acid, place 5 minutes for 30 ℃, measure absorbance ratio A
700/ A
520.Blank group replaces thiocyanate salt solution with distilled water.As shown in Figure 4, Δ A
700/ A
520when being 8 mmol/L, sulfuric acid final concentration reaches maximum.
Embodiment 6:
In the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 milliliter of thiocyanate salt solution (after mixing, in solution, thiocyanate final concentration is respectively 0,1,2 μ mol/L) and 0.2 milliliter of sulfuric acid (after mixing, in solution, sulfuric acid final concentration is 8 mmol/L), place 0.5-8 minute for 30 ℃, measure absorbance ratio A
700/ A
520.Blank group replaces thiocyanate salt solution with distilled water.As shown in Figure 5, absorbance ratio A
700/ A
520all after 5 minutes, reach maximum.
Embodiment 7:
The thiocyanate salt solution and the 0.2 milliliter of sulfuric acid (after mixing, in solution, sulfuric acid final concentration is 8 mmol/L) that in the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 milliliter of variable concentrations, place 5 minutes for 30 ℃, the variation of visualization color, result as shown in Figure 6.When thiocyanate not, solution is aobvious blue; When thiocyanate concn is 1 μ mol/L, solution shows purple; When thiocyanate concn is 1.5 μ mol/L, solution displaing amaranth; When thiocyanate concn is 2 μ mol/L, solution is aobvious red.
Embodiment 8:
In the nm of gold making at 0.25 milliliter of embodiment 1, add thiocyanate salt solution and 0.2 milliliter of sulfuric acid (after mixing, in solution, sulfuric acid final concentration is 8 mmol/L) of 0.05 milliliter of variable concentrations, place 5 minutes for 30 ℃, measure absorbance ratio A
700/ A
520.As shown in Figure 7, absorbance ratio A
700/ A
520increase with thiocyanate concn reduces, Δ A within the scope of 0.25 ~ 2 μ mol/L
700/ A
520with the linear (see figure 8) of thiocyanate concn, detect and be limited to 0.14 μ mol/L.
Embodiment 9:
In the water sample of 10 milliliters, add ethylenediamine tetraacetic acid (after mixing, in solution, ethylenediamine tetraacetic acid final concentration is 1 mmol/L), after 0.22 μ m membrane filtration, obtain sample solution.In the nm of gold making at 0.25 milliliter of embodiment 1, add 0.05 milliliter of above-mentioned sample solution and 0.2 milliliter of sulfuric acid (after mixing, in solution, sulfuric acid final concentration is 8 mmol/L), place 5 minutes for 30 ℃, the variation of visualization color or mensuration absorbance ratio A
700/ A
520.8 content that calculate thiocyanate in water samples in conjunction with the embodiments, the mensuration recovery of sample is 94.8% ~ 101.3%, relative standard deviation is 1.6-3.2%.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention, are equal to replacement and improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. one kind
take nm of gold as colour developing probe thiocyanate rapid assay methods, it is characterized in that utilizing thiocyanate energy selectivity to stop nm of gold in sulfuric acid solution, to produce the characteristic of assembling, and the variation that shows solution colour and ultra-violet absorption spectrum feature comes
measure thiocyanate concn.
2. according to claim 1
take nm of gold as colour developing probe thiocyanate rapid assay methods, it is characterized in that utilizing the variation characteristic of visualization solution colour with the concentration of judgement thiocyanate.
3. according to claim 1
take nm of gold as colour developing probe thiocyanate rapid assay methods, it is characterized in that utilizing the absorbance ratio A of solution ultra-violet absorption spectrum
700/ A
520concentration with judgement thiocyanate.
4. according to described in claim 1 or 2 or 3
take nm of gold as colour developing probe thiocyanate rapid assay methodsit is characterized in that used nm of gold adopts the method preparation of sodium citrate reduction gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution that adds rapidly 3 milliliters of 0.1g/L, reaction solution is from the light yellow claret that becomes, after continuing to reflux 15 minutes, reaction solution is naturally cooled to room temperature and forms nm of gold.
5. according to claim 1
take nm of gold as colour developing probe thiocyanate rapid assay methodsit is characterized in that 5:1 mixes by nano-Au solution with containing variable concentrations thiocyanate salt solution by volume, adding 0.2 milliliter of sulfuric acid solution to make to mix sulfuric acid final concentration in rear solution is 8 mmol/L, places 5-8 minute for 30 ℃, visualization color characteristic or mensuration absorbance ratio A
700/ A
520, when visualization color characteristic, along with the increase of thiocyanate concn, the color of nm of gold becomes purple-aubergine-redness from blueness gradually, and the detection of visualization is limited to 1 μ mol/L; When measuring absorbance ratio A
700/ A
520time, the absorbance ratio A along with the increase of thiocyanate concn
700/ A
520reduce gradually Δ A within the scope of 0.25 ~ 2 μ mol/L
700/ A
520linear with thiocyanate concn, detect and be limited to 0.14 μ mol/L.
6. according to claim 1
take nm of gold as colour developing probe thiocyanate rapid assay methods, it is characterized in that used nm of gold particle diameter is 13 nm, concentration is 3.2 nmol/L.
7. according to claim 5
take golden nanometer particle as colour developing probe thiocyanate rapid assay methodsit is characterized in that 5:1 by volume mixes by nano-Au solution with containing the testing sample thiocyanate salt solution of variable concentrations, adding 0.2 milliliter of sulfuric acid solution to make to mix sulfuric acid final concentration in rear solution is 8 mmol/L, places 5 minutes visualization color characteristic or mensuration absorbance ratio A for 30 ℃
700/ A
520concentration with judgement thiocyanate.
8. according to claim 7
take golden nanometer particle as colour developing probe thiocyanate rapid assay methods, the volume that it is characterized in that thiocyanate salt solution and nano-Au solution is 0.05 milliliter and 0.25 milliliter.
9. one kind
take the method for nm of gold thiocyanate in colour developing probe Fast Measurement water sample, comprise the steps: that in the water sample of 10 milliliters, adding ethylenediamine tetraacetic acid to make to mix ethylenediamine tetraacetic acid final concentration in rear solution is 1 mmol/L, after 0.22 μ m membrane filtration, obtains sample solution; After adding 0.05 milliliter of above-mentioned sample solution and 0.2 milliliter of sulfuric acid to make to mix in 0.25 milliliter of nm of gold, in solution, sulfuric acid final concentration is 8 mmol/L, places 5 minutes then visualization change color or mensuration absorbance ratio A for 30 ℃
700/ A
520, according to solution colour and color standards series of comparisons or undertaken quantitatively by absorbance ratio typical curve, obtain
thiocyanate ion content in water sample.
10. according to claim 9
take the method for nm of gold thiocyanate in colour developing probe Fast Measurement water sampleit is characterized in that used nm of gold adopts the method preparation of following sodium citrate reduction gold chloride, the chlorauric acid solution of 1 milliliter of 0.1 g/L is dissolved in 100 ml waters, reflux heating boils the rear citric acid three sodium solution that adds rapidly 3 milliliter of 0.1 g/L, reaction solution is from the light yellow claret that becomes, after continuing to reflux 15 minutes, reaction solution is naturally cooled to room temperature and forms nm of gold.
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| CN201310124281.7A CN103207160B (en) | 2013-04-11 | 2013-04-11 | Rapid determination method for thiocyanate with nanogold as coloring probe |
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|---|---|---|---|
| CN201310124281.7A CN103207160B (en) | 2013-04-11 | 2013-04-11 | Rapid determination method for thiocyanate with nanogold as coloring probe |
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| CN103207160B true CN103207160B (en) | 2014-12-10 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104990915A (en) * | 2015-06-24 | 2015-10-21 | 南昌大学 | Method for detecting thiocyanate ions based on gold nanoparticle visualization |
| CN109705292B (en) * | 2019-01-23 | 2021-05-18 | 济南大学 | Organic silicon polymer fluorescent probe for detecting thiocyanate radical and synthesis and application thereof |
| CN110132953A (en) * | 2019-05-20 | 2019-08-16 | 齐鲁工业大学 | A kind of gold nanoparticle and its preparation method and application of asparatate modification |
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