CN103207160A - 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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- CN103207160A CN103207160A CN2013101242817A CN201310124281A CN103207160A CN 103207160 A CN103207160 A CN 103207160A CN 2013101242817 A CN2013101242817 A CN 2013101242817A CN 201310124281 A CN201310124281 A CN 201310124281A CN 103207160 A CN103207160 A CN 103207160A
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- thiocyanate
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- gold
- milliliter
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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 the nm of gold is the quick content assaying method of thiocyanate ion of colour developing probe, belongs to analytical chemistry and field of nanometer technology.
Background technology
Nm of gold is paid close attention to widely owing to it is easy to prepare with biological functional, good biological stability and unique spectral characteristic.The surface plasma absorption band of nm of gold is positioned at the visible region of electromagnetic wave spectrum, and is subjected to the influence of the pattern of nanometer aggregation.Typical colloidal nano gold is claret, and their aggregation then presents purple or blueness, and this is due to surface plasma absorption band owing to nm of gold moves to the long wavelength.Method based on this principle of change color in the nm of gold accumulation process has been widely used in detection cell, protein, DNA, metallic ion and little molecule etc.Yet the accumulation process that should be pointed out that nm of gold is subjected to the influence of many external factor, therefore can produce the false positive signal and obtains incorrect result.In order to obtain higher selectivity and accuracy, become one based on the coloration method of anti-gathering or the nm of gold of disperseing again and well select.
Thiocyanate (SCN
-) being widely used in medicine, dyeing is in the industries such as photograph.(the CN for example because the hypertoxicity chemical constitution of its generation
-, CNCl) can cause serious environmental (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 Chromatography method, 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 directly with the nm of gold of sodium citrate reducing process preparation as the 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 to detect new method.
Summary of the invention
The nm of gold that the objective of the invention is with the preparation of sodium citrate reducing process is the colour developing probe, provides a kind of quick, safe, easy, sensitive thiocyanate to detect new method.
To achieve these goals, the present invention is by the following technical solutions:
Of the present invention a kind of
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, it is characterized in that utilizing thiocyanate 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
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, be characterized in utilizing the variation characteristic of visualization solution colour to judge the concentration of thiocyanate.
Described
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, be characterized in utilizing the absorbance ratio A of solution ultra-violet absorption spectrum
700/ A
520To judge the concentration of thiocyanate.
Described
It is the thiocyanate rapid assay methods of colour developing probe with the nm of goldBe characterized in that employed 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, the citric acid three sodium solution that the back adds 3 milliliters of 0.1g/L is rapidly boiled in the heating that refluxes, 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
It is the thiocyanate rapid assay methods of colour developing probe with the nm of goldBe characterized in by volume 5:1 with nano-Au solution and contain the variable concentrations thiocyanate salt solution mixing, add 0.2 milliliter of sulfuric acid solution and make and mix that the sulfuric acid final concentration is 8 mmol/L in the solution of back, placed 5-8 minute for 30 ℃, visualization color characteristic or measure absorbance ratio A
700/ A
520, along with the increase of thiocyanate concn, the color of nm of gold becomes purple-aubergine-redness by blueness gradually when the visualization color characteristic, and the detection of visualization is limited to 1 μ mol/L; When measuring absorbance ratio A
700/ A
520The time, the absorbance ratio A along with the increase of thiocyanate concn
700/ A
520Increase Δ A in 2.5 ~ 2 μ mol/L scopes gradually
700/ A
520Linear with thiocyanate concn, detect and be limited to 0.14 μ mol/L.
Described
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, being characterized in that employed nm of gold particle diameter is 13 nm, concentration is 3.2 nmol/L.
Described
It is the thiocyanate rapid assay methods of colour developing probe with the golden nanometer particleBe characterized in that 5:1 mixes nano-Au solution and the testing sample thiocyanate salt solution that contains variable concentrations by volume, add 0.2 milliliter of sulfuric acid solution and make and mix that the sulfuric acid final concentration is 8 mmol/L in the solution of back, placed 5 minutes for 30 ℃, visualization color characteristic or measure absorbance ratio A
700/ A
520To judge the concentration of thiocyanate.
Described
It is the thiocyanate rapid assay methods of colour developing probe with the golden nanometer particle, 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
It is the method that the colour developing probe is measured thiocyanate in the water sample fast with the nm of gold, comprise the steps: to add in 10 milliliters the water sample ethylenediamine tetraacetic acid and make and mix that the ethylenediamine tetraacetic acid final concentration is 1 mmol/L in the solution of back, behind 0.22 μ m membrane filtration, get sample solution; In 0.25 milliliter of nm of gold, add 0.05 milliliter of above-mentioned sample solution and 0.2 milliliter of sulfuric acid and make and mix that the sulfuric acid final concentration is 8 mmol/L in the solution of back, placed 5 minutes for 30 ℃, visualization change color then or measure absorbance ratio A
700/ A
520, carry out quantitatively according to solution colour and color standards series of comparisons or by the absorbance ratio typical curve, obtain
Thiocyanate ion content in the water sample
Described
It is the method that the colour developing probe is measured thiocyanate in the water sample fast with the nm of goldBe characterized in that employed 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, the citric acid three sodium solution that the back adds 3 milliliter of 0.1 g/L is rapidly boiled in the heating that refluxes, 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:
All glasswares that use in the 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, the citric acid three sodium solution that the back adds 3 milliliter of 0.1 g/L is rapidly boiled in the heating that refluxes, 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
0.05 add the nano-Au solution of 0.25 milliliter of step () preparation in the milliliter thiocyanate sample solution, add 0.20 milliliter of 20 mmol/L sulfuric acid (final concentration of sulfuric acid is 8 mmol/L in the mixed solution) then, mix the back and placed 5 minutes at 30 ℃, visualization change in color or measure 700 nm and the absorbance ratio (A at 520 nm wavelength places
700/ A
520).Carry out quantitatively according to solution colour and color standards series of comparisons or by the absorbance ratio typical curve.The detection of visualization is limited to 1 μ mol/L, and the detection that absorbance ratio is measured 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, need not further to modify, and preparation process is simply quick.
(3) the present invention is low to the processing requirements of sample, and anti-interference is good, and only need add ethylenediamine tetraacetic acid in the water sample can measure.
(4) detection speed of the present invention is fast, can finish pre-service and the detection of actual water sample in 5 minutes.
(5) detection sensitivity height of the present invention, the detection by the visual inspection change color is limited to 1 μ mol/L, and the detection that absorbance ratio is measured is limited to 0.14 μ mol/L.
Description of drawings
Fig. 1 is the uv absorption spectra of nm of gold under the 8 mmol/L sulfuric acid existence conditions.
Fig. 2 is the uv absorption spectra after nm of gold and the thiocyanate effect under the 8 mmol/L sulfuric acid existence conditions.
Fig. 3 is the absorbance ratio figure after nm of gold and the thiocyanate effect under the different aggregation inducing agent effects.
Fig. 4 is the absorbance ratio figure after nm of gold and the thiocyanate effect under the variable concentrations sulfuric acid existence condition.
Fig. 5 is that the absorbance ratio after nm of gold and the effect of variable concentrations thiocyanate is schemed over time under the 8 mmol/L sulfuric acid existence conditions.
Fig. 6 is the change color figure after nm of gold and the effect of variable concentrations thiocyanate under the 8 mmol/L sulfuric acid existence conditions.Concrete change color from left to right is shown as, and when thiocyanate not, it is blue that solution shows; When thiocyanate concn was 1 μ mol/L, solution showed purple; When thiocyanate concn is 1.5 μ mol/L, the solution displaing amaranth; When thiocyanate concn was 2 μ mol/L, it is red that solution shows.
Fig. 7 is the absorbance ratio variation diagram after nm of gold and the effect of variable concentrations thiocyanate under the 8 mmol/L sulfuric acid existence conditions.
Fig. 8 is Δ A under the 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, the citric acid three sodium solution that the back adds 3 milliliter of 0.1 g/L is rapidly boiled in the heating that refluxes, reaction solution after continuing to reflux 15 minutes, slowly is cooled to room temperature with reaction solution from the light yellow claret that becomes.The nm of gold particle diameter of gained is 13 nm, and concentration is about 3.2 nmol/L, 4 ℃ of preservations.All glasswares that use in the above process all soak through chloroazotic acid, and thoroughly clean with distilled water, dry.
Embodiment 2:
In the nm of gold that 0.25 milliliter of embodiment 1 makes, add 0.05 ml distilled water and 0.2 milliliter of sulfuric acid (the sulfuric acid final concentration is 8 mmol/L in the solution of mixing back), placed 5 minutes for 30 ℃.The nm of gold color becomes blueness by claret, absorbance ratio (A
700/ A
520) the increase (see figure 1).
Embodiment 3:
In the nm of gold that 0.25 milliliter of embodiment 1 makes, add 0.05 milliliter of thiocyanate salt solution (the thiocyanate final concentration is 2 μ mol/L in the solution of mixing back) and 0.2 milliliter of sulfuric acid (the sulfuric acid final concentration is 8 mmol/L in the solution of mixing back), placed 5 minutes for 30 ℃.The nm of gold color remains unchanged substantially, absorbance ratio (A
700/ A
520) than the little (see figure 2) of absorbance ratio of embodiment 2.
Embodiment 4:
In the nm of gold that 0.25 milliliter of embodiment 1 makes, add 0.05 milliliter of thiocyanate salt solution (the thiocyanate final concentration is 2 μ mol/L in the solution of mixing back) and 0.2 milliliter of different aggregation inducing agent (sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid, acetic acid, sodium chloride) (aggregation inducing agent final concentration is 8 mmol/L in the solution of mixing back), placed 5 minutes for 30 ℃, measure absorbance ratio A
700/ A
520The 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 that 0.25 milliliter of embodiment 1 makes, add 0.05 milliliter of thiocyanate salt solution (the thiocyanate final concentration is 2 μ mol/L in the solution of mixing back) and 0.2 milliliter of variable concentrations (the sulfuric acid final concentration is 0-10 mmol/L in the solution of mixing back) sulfuric acid, placed 5 minutes for 30 ℃, measure absorbance ratio A
700/ A
520The blank group replaces thiocyanate salt solution with distilled water.As shown in Figure 4, Δ A
700/ A
520When being 8 mmol/L, the sulfuric acid final concentration reaches maximum.
Embodiment 6:
In the nm of gold that 0.25 milliliter of embodiment 1 makes, add 0.05 milliliter of thiocyanate salt solution (the thiocyanate final concentration is respectively 0,1,2 μ mol/L in the solution of mixing back) and 0.2 milliliter of sulfuric acid (the sulfuric acid final concentration is 8 mmol/L in the solution of mixing back), placed 0.5-8 minute for 30 ℃, measure absorbance ratio A
700/ A
520The 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 (the sulfuric acid final concentration is 8 mmol/L in the solution of mixing back) that in the nm of gold that 0.25 milliliter of embodiment 1 makes, add 0.05 milliliter of variable concentrations, placed 5 minutes for 30 ℃, visualization change in color, result are as shown in Figure 6.When thiocyanate not, it is blue that solution shows; When thiocyanate concn was 1 μ mol/L, solution showed purple; When thiocyanate concn is 1.5 μ mol/L, the solution displaing amaranth; When thiocyanate concn was 2 μ mol/L, it is red that solution shows.
Embodiment 8:
In the nm of gold that 0.25 milliliter of embodiment 1 makes, add thiocyanate salt solution and 0.2 milliliter of sulfuric acid (the sulfuric acid final concentration is 8 mmol/L in the solution of mixing back) of 0.05 milliliter of variable concentrations, placed 5 minutes for 30 ℃, measure absorbance ratio A
700/ A
520As shown in Figure 7, absorbance ratio A
700/ A
520Increase with thiocyanate concn reduces, Δ A in 0.25 ~ 2 μ mol/L scope
700/ A
520With the linear (see figure 8) of thiocyanate concn, detect and be limited to 0.14 μ mol/L.
Embodiment 9:
Add ethylenediamine tetraacetic acid (the ethylenediamine tetraacetic acid final concentration is 1 mmol/L in the solution of mixing back) in 10 milliliters the water sample, behind 0.22 μ m membrane filtration, get sample solution.In the nm of gold that 0.25 milliliter of embodiment 1 makes, add 0.05 milliliter of above-mentioned sample solution and 0.2 milliliter of sulfuric acid (the sulfuric acid final concentration is 8 mmol/L in the solution of mixing back), placed 5 minutes visualization change in color or mensuration absorbance ratio A for 30 ℃
700/ A
5208 content that calculate thiocyanate in the 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 above only is preferred embodiment of the present invention, and in order to limit the present invention, all any modifications of doing within the spirit and principles in the present invention are not equal to replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. one kind
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, it is characterized in that utilizing thiocyanate 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
2. according to claim 1
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, it is characterized in that utilizing the variation characteristic of visualization solution colour to judge the concentration of thiocyanate.
3. according to claim 1
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, it is characterized in that utilizing the absorbance ratio A of solution ultra-violet absorption spectrum
700/ A
520To judge the concentration of thiocyanate.
4. according to claim 1 or 2 or 3 described
It is the thiocyanate rapid assay methods of colour developing probe with the nm of goldIt is characterized in that employed 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, the citric acid three sodium solution that the back adds 3 milliliters of 0.1g/L is rapidly boiled in the heating that refluxes, 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
It is the thiocyanate rapid assay methods of colour developing probe with the nm of goldIt is characterized in that by volume 5:1 with nano-Au solution and contain the variable concentrations thiocyanate salt solution mixing, add 0.2 milliliter of sulfuric acid solution and make and mix that the sulfuric acid final concentration is 8 mmol/L in the solution of back, placed 5-8 minute for 30 ℃, visualization color characteristic or measure absorbance ratio A
700/ A
520, along with the increase of thiocyanate concn, the color of nm of gold becomes purple-aubergine-redness by blueness gradually when the visualization color characteristic, and the detection of visualization is limited to 1 μ mol/L; When measuring absorbance ratio A
700/ A
520The time, the absorbance ratio A along with the increase of thiocyanate concn
700/ A
520Increase Δ A in 2.5 ~ 2 μ mol/L scopes gradually
700/ A
520Linear with thiocyanate concn, detect and be limited to 0.14 μ mol/L.
6. according to claim 1
It is the thiocyanate rapid assay methods of colour developing probe with the nm of gold, it is characterized in that employed nm of gold particle diameter is 13 nm, concentration is 3.2 nmol/L.
7. according to claim 5
It is the thiocyanate rapid assay methods of colour developing probe with the golden nanometer particleIt is characterized in that 5:1 mixes nano-Au solution and the testing sample thiocyanate salt solution that contains variable concentrations by volume, add 0.2 milliliter of sulfuric acid solution and make and mix that the sulfuric acid final concentration is 8 mmol/L in the solution of back, placed 5 minutes for 30 ℃, visualization color characteristic or measure absorbance ratio A
700/ A
520To judge the concentration of thiocyanate.
8. according to claim 7
It is the thiocyanate rapid assay methods of colour developing probe with the golden nanometer particle, it is characterized in that the volume of thiocyanate salt solution and nano-Au solution is preferably 0.05 milliliter and 0.25 milliliter.
9. one kind
It is the method that the colour developing probe is measured thiocyanate in the water sample fast with the nm of gold, comprise the steps: to add in 10 milliliters the water sample ethylenediamine tetraacetic acid and make and mix that the ethylenediamine tetraacetic acid final concentration is 1 mmol/L in the solution of back, behind 0.22 μ m membrane filtration, get sample solution; In 0.25 milliliter of nm of gold, add 0.05 milliliter of above-mentioned sample solution and 0.2 milliliter of sulfuric acid and make and mix that the sulfuric acid final concentration is 8 mmol/L in the solution of back, placed 5 minutes for 30 ℃, visualization change color then or measure absorbance ratio A
700/ A
520, carry out quantitatively according to solution colour and color standards series of comparisons or by the absorbance ratio typical curve, obtain
Thiocyanate ion content in the water sample
10. according to claim 9
It is the method that the colour developing probe is measured thiocyanate in the water sample fast with the nm of goldIt is characterized in that employed 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, the citric acid three sodium solution that the back adds 3 milliliter of 0.1 g/L is rapidly boiled in the heating that refluxes, 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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| CN104990915A (en) * | 2015-06-24 | 2015-10-21 | 南昌大学 | Method for detecting thiocyanate ions based on gold nanoparticle visualization |
| CN109705292A (en) * | 2019-01-23 | 2019-05-03 | 济南大学 | A kind of organosilicon macromolecule fluorescence probe detecting thiocyanate radical and its synthesis and application |
| 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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| CN109705292A (en) * | 2019-01-23 | 2019-05-03 | 济南大学 | A kind of organosilicon macromolecule fluorescence probe detecting thiocyanate radical and its synthesis and application |
| 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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| Publication number | Publication date |
|---|---|
| CN103207160B (en) | 2014-12-10 |
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