CN104483278B - Ag in a kind of Visual retrieval aqueous solution+Method - Google Patents
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- CN104483278B CN104483278B CN201410759571.3A CN201410759571A CN104483278B CN 104483278 B CN104483278 B CN 104483278B CN 201410759571 A CN201410759571 A CN 201410759571A CN 104483278 B CN104483278 B CN 104483278B
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000007864 aqueous solution Substances 0.000 title claims abstract description 24
- 230000000007 visual effect Effects 0.000 title claims abstract description 22
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 47
- 238000001514 detection method Methods 0.000 claims abstract description 24
- 239000012488 sample solution Substances 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 21
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 14
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 14
- 239000000376 reactant Substances 0.000 claims abstract description 11
- 238000002835 absorbance Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000012800 visualization Methods 0.000 claims abstract description 7
- 239000003643 water by type Substances 0.000 claims abstract description 5
- 238000000862 absorption spectrum Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- 239000003086 colorant Substances 0.000 claims description 4
- -1 silver ions Chemical class 0.000 claims description 4
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 3
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 238000007689 inspection Methods 0.000 claims 1
- 238000002474 experimental method Methods 0.000 description 20
- 230000000694 effects Effects 0.000 description 5
- 239000000523 sample Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 210000001124 body fluid Anatomy 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 230000036737 immune function Effects 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 210000001835 viscera Anatomy 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
Disclosed herein is Ag in a kind of Visual retrieval aqueous solution+Method, be characterized in that, detected according to the following steps：（1）Set up and determine Ag+Quantitative and visualization half-quantitative detection standard：Change value (the △ of color comparison picture and absorbanceA) and Ag+Linear equation between concentration is：△A=0.2171lgc+1.8453；（2）Ag in detection sample solution+：By volume, 14.7 parts of redistilled waters are taken in conical flask, 1.0 parts of amino black 10B, 2.0 parts of Ag under thermostat water bath, stirring condition, are sequentially added+Sample solution, 0.3 part of NaBH4Solution and 2 parts of BR cushioning liquid.And the color of reactant liquor is recorded by digital camera, it is seen that and the absorbance of spectrophotometer sample solution, then compare with color comparison picture, or silver ion content in sample solution is calculated according to linear equation.
Description
Technical field
The invention belongs to chemical field, and in particular to Ag in a kind of Visual retrieval aqueous solution+Method.
Background technology
Silver is one of important trace element that needed by human body is wanted, Ag+The ferment of vigor effect in germ body can be slackened, is entered
And can effectively prevent the patience of germ；In addition have been reported that mentioning silver ion affects the immunologic function of human body, as Ag in body fluid+Content
When declining 0.001, the probability of happening of numerous disease can be dramatically increased, the Ag of excess+Injury effect can be produced to body also, especially
The eyes and internal organ of its harm people, because the Ag of excess+Can deposit in brain, liver, kidney, lung, bone etc..Therefore with people
Ag in the directly related material of class+Detection have important practical significance.The method of conventional detection micro silver ion has at present：
Spectroscopic methodology, mass spectrography, electrochemical method etc..Wherein, the probe used in spectroscopic methodology mainly has novel nano-material, semiconductor amount
Sub- select, develop the color with decolourant etc..In these methods, realize that Silver detection can due to facilitating implementation using colour developing and decolourant
Concerned depending on changing.But the sensitivity of the detection of such detection method is changed high not enough at present.Hence set up new highly sensitive
The method of Visual retrieval silver ion is significant.
Content of the invention
Present invention seek to address that the deficiency of prior art detection method, there is provided Ag in a kind of Visual retrieval aqueous solution+'s
Method.
The technical solution used in the present invention is：Ag in a kind of Visual retrieval aqueous solution+Method, it is characterized in that, with ammonia
The black 10B of base is developer, using variable concentrations Ag+Catalysis NaBH4Reduction amino black 10B obtains different colours and visible absorbance is strong
The reactant liquor of degree, realizes to Ag in the aqueous solution+Accurate quantitative analysis or visualization half-quantitative detection.
Ag in the described Visual retrieval aqueous solution+Method, be to be detected according to the following steps：
（1）Set up and determine Ag+Quantitative and visualization half-quantitative detection standard：
NaBH is catalyzed using variable concentrations Ag+4Reduction amino black 10B obtains the reactant liquor of different colours, by digital phase
In the presence of machine record variable concentrations silver ion, the color of reactant liquor, obtains color comparison picture；Scanned using visible spectrophotometer
The absorption spectrum of 400-700 nm scopes, and make visible absorption spectra figure；And by calculating variable concentrations silver ion in 616 nm
After the absorbance at place deducts blank absorbance, the change value (△ of absorbance is obtainedA) and concentration of silver ions（C represents that sample is molten
The concentration of liquid, unit are mol/L) between linear equation be：△A=0.2171lgc+1.8453；
（2）Ag in detection sample solution+：
By volume, 14.7 parts of redistilled waters are taken in container, in thermostat water bath, is sequentially added under stirring condition
1.0 parts of amino black 10B, 2.0 parts of Ag+Sample solution, 0.3 part of NaBH4Solution and 2 parts of BR cushioning liquid, using visible spectrum
Instrument scans the absorption spectrum of 400-700 nm wavelength bands, and the color by digital camera record reactant liquor, then with color
Movement images are compareed, or according to linear equation determination sample solution, so as to draw silver ion content in sample solution.
The pH value that reaction is controlled using BR cushioning liquid.
When in detection sample solution have Ni2+, Pb2+When, EDTA is added, Ni is eliminated2+, Pb2+To Ag+The impact of detection.
The initial concentration of the amino black 10B that testing conditions are used is 5.0 × 10-4M, NaBH4The initial concentration of solution is
0.1 M, BR cushioning liquid pH=7.96；Blank replaces Ag using secondary water+Solution is reacted.
Testing conditions optimize as a result, the optium concentration of the amino black 10B be 2.5 × 10-5M, NaBH4Solution
Optium concentration is 1.5 × 10-3Optimal pH=7.96 of M, BR cushioning liquid, 60 min of stirring reaction at 60 DEG C.
After condition optimizing, Ag+The minimal detectable concentration of solution is 5.0 × 10-9M, the determined silver ion range of linearity is：
5.0×10-95.0 × 10-7M.
The present invention adopts the amino black 10B of good water solubility for developer, NaBH4And Ag+In the presence of common, 60 DEG C of reactions 60
After min, it is possible to achieve Ag in accurate quantitative analysis and the visualization half-quantitative detection aqueous solution+.In the method and prior art other
Visual retrieval Ag+Method is compared, with the advantage such as sensitivity is high, selective good.
Description of the drawings
Fig. 1 is Ag in the Visual retrieval aqueous solution+UV-visible absorption spectrum（A）And linear graph（B）, illustration is right
The solution picture that answers；
Fig. 2 is Ag+NaBH is catalyzed with part common metal ion4Reduction amino black 10B contrast block diagrams.
Specific embodiment
With reference to specific experiment example and accompanying drawing, the present invention is described in further detail.
Experiment 1：Set up the visualization half-quantitative detection standard for determining silver ion
Contain Ag+The preparation of standard liquid：
Ag+The preparation of standard liquid：Weigh 0.0849 g AgNO3Solid prepare 50 mL, 0.01 M containing Ag+Solution,
Then 5.0 × 10 are diluted to-3M、5.0×10- 5M and 5.0 × 10-7The Ag of M+Standard liquid.
By volume, 14.7 parts of redistilled waters are taken in container, in thermostat water bath, is sequentially added under stirring condition
1.0 parts of amino black 10B, 2.0 parts contain Ag+Standard liquid, 0.3 part of NaBH4Solution and 2 parts of BR cushioning liquid, using visible ray
Spectrometer scans the absorption spectrum of 400-700 nm wavelength bands, and records the color of reactant liquor by digital camera.
According to the method described above, Ag is determined+Concentration is respectively 5.0 × 10-9M, 1.0 × 10-8M, 2.5 × 10-8M, 5 ×
10-8M, 7.5 × 10-8M, 1.0 × 10-7M, 5.0 × 10-7The absorption spectrum of standard liquid system during M, makes visible suction
Receive spectrogram (see Fig. 1 (A)).1-8 in figure： Ag+Concentration is respectively：0, 5.0×10-9M, 1.0 × 10-8M, 2.5 × 10-8
M, 5.0 × 10-8M, 7.5 × 10-8M, 1.0 × 10-7M, 5.0 × 10-7M.
Experiment finds：The color of solution presents regular change (inserting in see Fig. 1 (A) with the increase of concentration of silver ions
Figure).And find that the color of solution presents regular change (see the illustration in Fig. 1 (A)) with the increase of concentration of silver ions.Visually
Change detection Ag+Concentration range is 5.0 × 10- 9～5.0×10-7Equation of linear regression in M is：△A=0.2171lgc+
1.8453.(△AFor the change value of absorbance, c represents Ag in sample solution+Concentration, unit is mol/L)；Experiment can have
Ag in the effect detection aqueous solution+Least concentration up to 5.0 × 10-9M, and coefficient R2=0.9930, as a result such as Fig. 1 (B).
Experiment 2：Detection Ag+Sample solution
Ag+The detection of sample solution：By volume, 14.7 parts of redistilled waters are taken in container, in thermostat water bath,
1.0 parts of amino black 10B, 2.0 parts of Ag are sequentially added under stirring condition+Sample solution, 0.3 part of NaBH4Solution and 2 parts of BR bufferings
Solution, the absorption spectrum that 400-700 nm wavelength bands are scanned using visible spectrophotometer, and reactant liquor is recorded by digital camera
Color, then compare with visible absorption spectra figure, or according to linear equation determination sample solution, so as to draw sample solution
Middle silver ion content.
According to linear relationship, three Ag are determined+Sample solution, the rate of recovery of measure are more than 95%（It is shown in Table 1）, this is described
Method has preferable actual application value.
The measurement result of 1. synthetic sample of table
| Sample sequence number | Concentrations/molL-1 | Actual concentrations/molL-1 | The rate of recovery/% |
| 1 | 4.780×10-8 | 5.000×10-8 | 95.60 |
| 2 | 4.934×10-8 | 5.000×10-8 | 98.69 |
| 3 | 4.8308×10-8 | 5.000×10-8 | 96.62 |
Experiment 3：According to the method in experiment 1, in Ag+Ultimate density be 5.0 × 10-8Under the conditions of M, determine in solution
Amino black 10B ultimate densities are respectively 1.25 × 10-5M, 1.875 × 10-5M, 2.5 × 10-5M, 3.125 × 10-5M, 3.75
×10-5During M, to Ag in the Visual retrieval aqueous solution+Impact.Experiment shows：When in final solution, amino black 10B concentration is
2.5×10-5During M, UV absorption strength difference is maximum.
Experiment 4：According to the method in experiment 1, in Ag+Ultimate density be 5.0 × 10-8Under the conditions of M, NaBH is determined4Most
Final concentration is respectively 0.5 mM, 1.0 mM, 1.5 mM, 2.0 mM, during 2.5 mM, to Ag in the Visual retrieval aqueous solution+Shadow
Ring.Experiment shows：Work as NaBH4Concentration when being 1.5 mM, ultraviolet absorptivity difference is maximum.
Experiment 5：According to the method in experiment 1, in Ag+Ultimate density be 5.0 × 10-8Under the conditions of M, water-bath temperature is determined
30 DEG C of degree, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, to Ag in the Visual retrieval aqueous solution when 80 DEG C+Impact.Experiment shows：Work as water
When bath temperature is 60 DEG C, ultraviolet absorptivity difference is maximum.
Experiment 6：According to the method in experiment 1, in Ag+Ultimate density be 5.0 × 10-7Under the conditions of M, 15min is determined,
To Ag in the Visual retrieval aqueous solution when 30min, 45min, 60min, 75min, 90min+Impact.Experiment shows：Work as reaction
When time is 60min, ultraviolet absorptivity difference is maximum.
Experiment 7：In order to further optimize Ag in the Visual retrieval aqueous solution+When pH conditions, we select BR buffering molten
The pH value of hydraulic control system reaction.And in Ag+Initial concentration be 5.0 × 10-7Under the conditions of M, pH=6.80 is determined, 7.24,
To Ag in the Visual retrieval aqueous solution when 7.96,8.69,9.62+Impact.Test result indicate that：The ultraviolet suction as pH=7.96
Luminosity difference is maximum.
Experiment 8：Under cushioning liquid existence condition, Ag is determined respectively+Amino black 10B is urged with some common metal ions
Change the contrast of fading effect, metal ion initial concentration used is 5.0 × 10-7M.Experimental result is shown in Fig. 2.As a result show：
Ni2+, Pb2+To Ag+Detection have a large effect, but add EDTA successfully eliminate Ni2+, Pb2+Impact, and do not affect
To Ag+Detection results.
Also, it should be noted the specific experiment example of the present invention is used only to exemplary illustration, and limit never in any form
Determine protection scope of the present invention, the person skilled of this area can be improved according to some explanations above-mentioned or be changed, but
All these improvements and changes should all belong to the protection domain of the claims in the present invention.
Claims (6)
1. Ag in a kind of Visual retrieval aqueous solution+Method, with amino black 10B as developer, using variable concentrations Ag+Catalysis
NaBH4Reduction amino black 10B obtains the reactant liquor with different colours and absorption spectrum, realizes to Ag in the aqueous solution+Visualization
Quantitative determination, is characterized in that, be detected according to the following steps：
（1）Set up and determine Ag+Visualization quantitative measurement standard：
Using variable concentrations Ag+Catalysis NaBH4Reduction amino black 10B obtains the reactant liquor of different colours, is recorded by digital camera
The color of reactant liquor in the presence of variable concentrations silver ion, obtains color comparison picture；400-700 is scanned using visible spectrophotometer
The absorption spectrum of nm scopes, and make abosrption spectrogram；And by calculating absorbance button of the variable concentrations silver ion at 616 nm
After except blank absorbance, change value D of absorbance is obtainedAWith the linear equation between concentration of silver ions c it is：DA=
0.2171lgc+1.8453；
（2）Ag in detection sample solution+：
By volume, 14.7 parts of redistilled waters are taken in container, in thermostat water bath, under stirring condition, 1.0 is sequentially added
Part amino black 10B, 2.0 parts of Ag+Sample solution, 0.3 part of NaBH4Solution and 2 parts of BR cushioning liquid, are swept using visible spectrophotometer
The absorption spectrum of 400-700 nm wavelength bands, and the color by digital camera record reactant liquor is retouched, is then compared with color
Image contrast, or according to linear equation determination sample solution, so as to draw silver ion content in sample solution.
2. Ag in the Visual retrieval aqueous solution according to claim 1+Method, it is characterized in that, using BR cushioning liquid controls
The pH value of system reaction.
3. Ag in the Visual retrieval aqueous solution according to claim 1+Method, it is characterized in that, when in detection sample solution
There is Ni2+, Pb2+When, EDTA is added, Ni is eliminated2+, Pb2+To Ag+The impact of detection.
4. Ag in the Visual retrieval aqueous solution according to claim 2+Method, it is characterized in that, the amino black 10B's
Initial concentration is 5.0 × 10-4M, NaBH4The initial concentration of solution is 0.1 M, BR cushioning liquid pH=7.96；Blank uses two
Secondary water replaces containing Ag+Solution reacted.
5. Ag in the Visual retrieval aqueous solution according to claim 2+Method, it is characterized in that, the amino black 10B's
Optium concentration is 2.5 × 10-5M, NaBH4The optium concentration of solution is 1.5 × 10-3The Optimal pH of M, BR cushioning liquid=
60 min of stirring reaction at 7.96,60 DEG C.
6. Ag in the Visual retrieval aqueous solution according to claim 1+Method, it is characterized in that, Ag+The minimum inspection of solution
It is 5.0 × 10 to survey concentration-9M, the determined silver ion range of linearity is：5.0×10-95.0 × 10-7M.
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| JP2000055901A (en) * | 1998-08-12 | 2000-02-25 | Seiken:Kk | Simple measurement method of silver ion concentration |
| CN102516978A (en) * | 2011-11-18 | 2012-06-27 | 厦门大学 | Molecular probe for detecting mercury ions and silver ions in water and preparation method thereof |
| CN103772318A (en) * | 2014-01-22 | 2014-05-07 | 天津希恩思生化科技有限公司 | Organic compound for measuring content of metal ions in water environment and application of organic compound |
| CN104101577A (en) * | 2014-08-05 | 2014-10-15 | 贵州大学 | Ag+ or F- determining method by adopting rate absorption spectrophotometry |
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2014
- 2014-12-12 CN CN201410759571.3A patent/CN104483278B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000055901A (en) * | 1998-08-12 | 2000-02-25 | Seiken:Kk | Simple measurement method of silver ion concentration |
| CN102516978A (en) * | 2011-11-18 | 2012-06-27 | 厦门大学 | Molecular probe for detecting mercury ions and silver ions in water and preparation method thereof |
| CN103772318A (en) * | 2014-01-22 | 2014-05-07 | 天津希恩思生化科技有限公司 | Organic compound for measuring content of metal ions in water environment and application of organic compound |
| CN104101577A (en) * | 2014-08-05 | 2014-10-15 | 贵州大学 | Ag+ or F- determining method by adopting rate absorption spectrophotometry |
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| Title |
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| 典型中成药中Cu2+的可视化数值分析法;詹蕾 等;《中国科学:化学》;20111231;第41卷(第6期);第1044-1050页 * |
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