CN106442515A - Simple and low-cost silver ion visual quantitative detection method - Google Patents
Simple and low-cost silver ion visual quantitative detection method Download PDFInfo
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- CN106442515A CN106442515A CN201611039050.6A CN201611039050A CN106442515A CN 106442515 A CN106442515 A CN 106442515A CN 201611039050 A CN201611039050 A CN 201611039050A CN 106442515 A CN106442515 A CN 106442515A
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000001514 detection method Methods 0.000 title claims abstract description 16
- 230000000007 visual effect Effects 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 22
- 239000007864 aqueous solution Substances 0.000 claims abstract description 21
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims description 11
- 239000004033 plastic Substances 0.000 claims description 4
- 229920003023 plastic Polymers 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 3
- CMZYGFLOKOQMKF-UHFFFAOYSA-N 1-(3,5-dimethylphenyl)-3,5-dimethylbenzene Chemical group CC1=CC(C)=CC(C=2C=C(C)C=C(C)C=2)=C1 CMZYGFLOKOQMKF-UHFFFAOYSA-N 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- HFACYLZERDEVSX-UHFFFAOYSA-N benzidine Chemical compound C1=CC(N)=CC=C1C1=CC=C(N)C=C1 HFACYLZERDEVSX-UHFFFAOYSA-N 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 5
- 239000011259 mixed solution Substances 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 3
- 229910052709 silver Inorganic materials 0.000 abstract description 2
- 239000004332 silver Substances 0.000 abstract description 2
- 230000002596 correlated effect Effects 0.000 abstract 1
- 238000011897 real-time detection Methods 0.000 abstract 1
- -1 silver ions Chemical class 0.000 abstract 1
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 4
- 239000008346 aqueous phase Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 229910021642 ultra pure water Inorganic materials 0.000 description 3
- 239000012498 ultrapure water Substances 0.000 description 3
- UAIUNKRWKOVEES-UHFFFAOYSA-N 3,3',5,5'-tetramethylbenzidine Chemical compound CC1=C(N)C(C)=CC(C=2C=C(C)C(N)=C(C)C=2)=C1 UAIUNKRWKOVEES-UHFFFAOYSA-N 0.000 description 2
- 208000035126 Facies Diseases 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 239000012496 blank sample Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 241000669244 Unaspis euonymi Species 0.000 description 1
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 238000013507 mapping Methods 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 238000012123 point-of-care testing Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910001961 silver nitrate Inorganic materials 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
- Optical Measuring Cells (AREA)
Abstract
The invention discloses a simple and low-cost silver ion visual quantitative detection method. The method adopts an organic solvent which can be mutually soluble with water and has density more than 1g/mL at the temperature of 25 DEG C for dissolving 3,3',5'5'-tetramethyl benzidine (TMB). When aqueous solution containing silver ions is dropwise added into TMB solution, Ag<+> quickly oxidizes TMB to generate blue quinoid benzidine. As the adopted organic solvent can be taken as a bicolour layering intelligent regulator, a unique bicolour mixed solution which is blue at the upper layer and colourless at the lower layer is obtained finally; meanwhile, the length of the blue solution is positively correlated with concentration of Ag<+>, so that quantitative detection on Ag<+> at micromole level can be realized by visualizing and observing with naked eyes and measuring the length of the blue solution. According to the method disclosed by the invention, a Ag<+> detection process is extremely simple, an operator not trained professionally can carry out an experiment, more importantly, a quantitative signal can be read without using instrument or equipment, and on-site analysis and real-time detection on a sample can be realized while analysis cost is greatly reduced.
Description
Technical field
The invention belongs to heavy metal ion chemical sensitisation detection technique field and in particular to a kind of simple low cost silver from
Specific item regards quantitative detecting method.
Background technology
Silver ion（Ag+）It is widely used in photography, image, electrical equipment, medicine and other fields.But Ag+Ion can be rich by food chain
Combine in human body, the activity of high concentration this kind of heavy metal ion energy destructive enzyme, and can be with the amine of various metabolite, imidazoles, carboxylic
The functional groups such as base combine, and have a strong impact on, damage the health of the mankind, even result in death.Ag traditional at present+Detection by quantitative side
Method mainly includes atom and ultraviolet absorption spectroscopy, fluorescent spectrometry, mass spectrography, electrochemical sensor method, ion selectivity electricity
Pole method etc..However, there is analysis cost to some extent relatively in these methods based on spectrogrph, mass spectrograph and electrochemical electrode
The loaded down with trivial details instrument price that is time-consuming, requiring higher professional skill to operator, used of high, analysis process is expensive and volume is huge
Greatly, cannot be used for field assay and instant detection（Point-of-Care Testing）Deng series of problems.
Content of the invention
The purpose of the present invention is for the deficiencies in the prior art, provides a kind of silver ion of simple low cost visually quantitatively to examine
Survey method.
The thinking of the present invention：Silver ion in research display aqueous solution（Ag+）Can be by 3,3', 5,5'- tetramethyl benzidine
（TMB）Colorimetric probe Quick Oxidation generates quinoid benzidine product, obtains the blue aqueous solution of color even.Use in the present invention
Miscible with water and density is more than 1 g/mL（25℃）Organic solvent dissolving TMB probe.When by Ag+Aqueous solution Deca enters such
When in TMB solution, there is a certain degree of exchange, Ag in the solute in two kinds of solution+Quick Oxidation TMB generates quinoid benzidine.
Because this quinoid benzidine product is more likely to be formed in aqueous phase, finally give colourless double of upper strata blueness-lower floor of uniqueness
Mixture of colours solution.Upper strata is mainly the less aqueous phase of density, and because assuming blueness containing quinoid benzidine product；Lower floor is main
For the organic faciess that density is larger, and because not having quinoid benzidine product or this production concentration too low and present colourless.Even more important
, institute using organic solvent can be further used as double-colored layering Intelligent adjustment agent." intelligent " refers to Ag+The increasing of concentration
Greatly, in the double-colored mixed solution ultimately forming, the length of colored solutions increases therewith.Therefore, do not needing using any specialty instrument
The length in the case of device or equipment, observing, measuring colored solutions only by macroscopic visual can achieve Ag+Quantitation inspection
Survey.
Concretely comprise the following steps：
Step one, will contain Ag+Aqueous solution be added drop-wise to equipped with 3,3', 5,5'- tetramethyl benzidine（TMB）The transparent examination of solution
Guan Zhong.
Step 2, length, the size of this length and the Ag of cuvette blue solution at the middle and upper levels is observed, measured to macroscopic visual+Concentration is proportionate, that is, complete Ag+Visual detection by quantitative.
Described containing Ag+Aqueous solution in Ag+For target analytes or produced by chemical reaction and biological respinse two
Level analyte.
The solvent of described 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions is organic solvent, and this organic solvent is miscible with water and 25
DEG C lower density is more than 1g/mL.
Described cuvette is the graduated cuvette of outer wall or outer wall does not have graduated cuvette, cuvette
Material is plastics or glass；When the outer wall of cuvette has scale, the length measuring cuvette blue solution at the middle and upper levels is
Completed by directly reading the scale on the cuvette outer wall related to blue solution length；When the outer wall of cuvette does not have
When having scale, the length of blue solution is to measure examination on cuvette outer wall by using ruler at the middle and upper levels to measure cuvette
In pipe, the length of blue solution is completing.
With existing Ag+Ion quantitative detecting method is compared, and the present invention has the prominent advantages that：1）Ag+Detection process is extremely
Simply, non-pro operator also can carry out experiment；2）Do not use any instrument or equipment, only by using ruler
Measure colored solutions length from test tube outer wall or directly read the scale the test tube outer wall related to colored solutions length
Carry out quantifiable signal reading, also enable the field assay of sample and instant detection while very big reduction analysis cost；3）
New method can directly be applied to Ag in various samples in the fields such as environmental monitoring, food safety, medical research+Analyte or
Simple, economical, quick, special for other target analytes such as the protein of secondary analysis thing, nucleic acid with this metal ion
Portable qualitative and quantitative detection, has broad application prospects.
Brief description
Fig. 1 is the principle of the simply visual quantitative detecting method of silver ion of low cost in Example 1 and Example 2 of the present invention
Schematic diagram.
In figure labelling：1- cuvette；The scale of 2- cuvette outer wall；The colourless formamide solvent of 3-；4-3,3',5,
5'- tetramethyl benzidine solute；The colourless aqueous solvent of 5-；6-Ag+Solute；7- quinoid benzidine；8- contains the indigo plant of quinoid benzidine
Color solution；9- does not contain the colourless solution of quinoid benzidine；10- naked eyes.
Fig. 2 is to analyze 1 mM in the embodiment of the present invention 1 to contain Ag+Aqueous solution when acquired results and blank sample（Do not contain
Ag+Ultra-pure water）The comparison diagram of acquired results.
Fig. 3 is that in the embodiment of the present invention 2, the silver ion visual quantitative detecting method analysis using simple low cost is a series of
The Ag of variable concentrations+Gained blue solution length during aqueous solution（Scale value on test tube outer wall）With Ag+The Log value of concentration（Log
(C Ag+)）Between working curve.
Specific embodiment
Following examples will be further described to the present invention, but not thereby limiting the invention.
Embodiment 1:
The present embodiment is analyzed 1 mM using the visual quantitative detecting method of silver ion of simply low cost and is contained Ag+Aqueous solution（A）
And blank sample（Without the ultra-pure water of Ag+, B）.
Specific implementation process is as follows：
As shown in figure 1, the concretely comprising the following steps of the present embodiment：Step one, by 50 μ L 1 mM silver nitrate（AgNO3）Aqueous solution Deca
To equipped with 100 μ L 2.5 mM TMB solution（By can prepare Methanamide miscible with water, that 25 DEG C of lower densities are 1.134 g/mL）
Outer wall graduated plastic, transparent test tube in；Step 2, macroscopic visual is observed, is directly read and blue solution in cuvette
Scale, the size of this length and Ag on the related cuvette outer wall of length+Concentration is proportionate, that is, complete Ag+Visually fixed
Amount detection.
Dummy, i.e. ultra-pure water are tested and analyzed according to identical step（Resistivity is 18.2 M Ω cm）, and visually
Observe the color change of solution in test tube.Figure it is seen that obtain during detection dummy is water white solution.
This is because there is not Ag in dummy+, so not having the quinoid benzidine product of blueness to generate.On the other hand, when detection 1
MM contains Ag+Aqueous solution when, can substantially observe colourless double-colored of upper strata blueness-lower floor defining uniqueness in test tube
Mixed solution.This is because working as Ag+When aqueous solution Deca enters in TMB solution, there is certain journey in the solute in two kinds of solution
The exchange of degree, Ag+Quick Oxidation TMB generates quinoid benzidine.Because this quinoid benzidine product is more likely to shape in aqueous phase
Become, finally give the colourless double-colored mixed solution of upper strata blueness-lower floor.Upper strata is mainly the less aqueous phase of density, and because containing
Quinoid benzidine product and assume blueness；Lower floor is mainly the larger organic faciess of density, and because do not have quinoid benzidine product or
This production concentration is too low and presents colourless.Contrast and experiment in Fig. 2 shows, the visual quantitative detecting method of silver ion conscientiously may be used
OK.
Embodiment 2:
The present embodiment is 62.5 μM ~ 4 mM using the silver ion visual quantitative detecting method analytical concentration scope of simply low cost
Ag+Aqueous solution.
Specific implementation process is as follows：
As shown in figure 1, detecting each Ag in the present embodiment+The concretely comprising the following steps of aqueous solution：Step one, by a certain for 50 μ L concentration
AgNO3Aqueous solution is added drop-wise to containing 100 μ L 2.5 mM TMB solution（By can miscible with water, 25 DEG C of lower densities be 1.134 g/
The Methanamide of mL is prepared）Outer wall graduated plastic, transparent test tube in；Step 2, macroscopic visual observe, directly read with thoroughly
Scale on the related cuvette outer wall of blue solution length in bright test tube.By all Ag+The colored solutions length of aqueous solution
Value（I.e. scale value on cuvette outer wall）To Ag+The Log value of concentration（Log(C Ag+)）Mapping（Fig. 3）, that is, complete Ag+Mesh
Depending on detection by quantitative.
From the figure 3, it may be seen that with Ag+The increase of concentration, the length value of blue solution in corresponding test tube（I.e. outside cuvette
Scale value on wall）It is gradually increased.This is because, work as Ag+When concentration is larger, the oxidable more TMB of this metal ion generates
The blue quinoid benzidine product of larger concentration, directly shows the blue solution in test tube with larger lengths.Additionally, Fig. 3
Display, the length value of blue solution（Scale value on cuvette outer wall）With Ag+The Log value of concentration（Log(C Ag+)）62.5
μM ~ 4 mM in the range of assume good linear relationship.
Claims (1)
1. a kind of visual quantitative detecting method of silver ion of simple low cost is it is characterised in that concretely comprise the following steps：
Step one, will contain Ag+Aqueous solution be added drop-wise to equipped with 3,3', in the cuvette of 5,5'- tetramethyl biphenyl amine aqueous solution；
Step 2, length, the size of this length and the Ag of cuvette blue solution at the middle and upper levels is observed, measured to macroscopic visual+Concentration
It is proportionate, that is, complete Ag+Visual detection by quantitative；
Described containing Ag+Aqueous solution in Ag+Two fraction produced for target analytes or by chemical reaction and biological respinse
Analysis thing；
The solvent of described 3,3', 5,5'- tetramethyl biphenyl amine aqueous solutions be organic solvent, this organic solvent miscible with water and 25 DEG C at
Density is more than 1g/mL；
Described cuvette is the graduated cuvette of outer wall or outer wall does not have graduated cuvette, the material of cuvette
It is plastics or glass；When the outer wall of cuvette has scale, the length of blue solution is to pass through at the middle and upper levels to measure cuvette
Directly read scale on the cuvette outer wall related to blue solution length to complete；When the outer wall of cuvette is not carved
When spending, the length of blue solution is to measure in test tube on cuvette outer wall by using ruler at the middle and upper levels to measure cuvette
The length of blue solution is completing.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106932389A (en) * | 2017-03-28 | 2017-07-07 | 桂林理工大学 | Nm of gold Two-dimensional Liquid without spectrometer compares color quantitative analysis method |
| CN108693175A (en) * | 2017-04-07 | 2018-10-23 | 南京大学 | A method of copper ion is detected using high-throughput photoelectric colorimetry |
| CN109490384A (en) * | 2017-09-11 | 2019-03-19 | 中国科学院理化技术研究所 | A kind of working electrode and electrochemical sensor can be used for selective enumeration method silver ion |
| CN110243776A (en) * | 2019-06-21 | 2019-09-17 | 福建中医药大学 | Improve reaction microenvironment using lauryl sodium sulfate and carries out that silver ion is qualitative and the detection method of quantitative detection |
| CN110579469A (en) * | 2019-09-29 | 2019-12-17 | 桂林理工大学 | Instrument-free quantitative detection method for divalent mercury ions |
| CN112285099A (en) * | 2020-09-23 | 2021-01-29 | 嘉兴学院 | Visual hydrogel sensor and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106932389A (en) * | 2017-03-28 | 2017-07-07 | 桂林理工大学 | Nm of gold Two-dimensional Liquid without spectrometer compares color quantitative analysis method |
| CN108693175A (en) * | 2017-04-07 | 2018-10-23 | 南京大学 | A method of copper ion is detected using high-throughput photoelectric colorimetry |
| CN108693175B (en) * | 2017-04-07 | 2021-07-30 | 南京大学 | Method for detecting copper ions by adopting high-throughput photoelectric colorimetric method |
| CN109490384A (en) * | 2017-09-11 | 2019-03-19 | 中国科学院理化技术研究所 | A kind of working electrode and electrochemical sensor can be used for selective enumeration method silver ion |
| CN109490384B (en) * | 2017-09-11 | 2021-04-02 | 中国科学院理化技术研究所 | Working electrode and electrochemical sensor for selectively detecting silver ions |
| CN110243776A (en) * | 2019-06-21 | 2019-09-17 | 福建中医药大学 | Improve reaction microenvironment using lauryl sodium sulfate and carries out that silver ion is qualitative and the detection method of quantitative detection |
| CN110579469A (en) * | 2019-09-29 | 2019-12-17 | 桂林理工大学 | Instrument-free quantitative detection method for divalent mercury ions |
| CN112285099A (en) * | 2020-09-23 | 2021-01-29 | 嘉兴学院 | Visual hydrogel sensor and preparation method and application thereof |
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| Publication number | Publication date |
|---|---|
| CN106442515B (en) | 2019-10-11 |
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Application publication date: 20170222 Assignee: GUILIN VEIRUN MEDICAL TECHNOLOGY Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2023980046003 Denomination of invention: A Simple Visual Quantitative Detection Method for Silver Ions Granted publication date: 20191011 License type: Common License Record date: 20231108 |