CN104931488B - A method of based on indicator array detection anion - Google Patents
A method of based on indicator array detection anion Download PDFInfo
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Abstract
The present invention relates to a kind of method based on indicator array detection anion, the detection for a variety of anion in water.In the case where organic dyestuff concentration is certain, the chelate of different colours gradient is obtained by the way that different amounts of same metal ion species are added, builds the sensor array being made of the metallo-chelate of various concentration；The principle that generation complex compound is even further reacted in precipitation reaction can occur with metal by anion in aqueous solution, metal ion is cemented out from coloured chelate, generates color change.Since different anions are different from the reaction equilibrium constant of same indicator, to achieve the purpose that distinguish to anion.It in this way, can be rapidly to S in water2‑, F‑, Cl‑, Br‑, I‑, CrO4 2‑, PO4 3‑, C2O4 2‑Whether anion is quickly judged beyond national sewage or drinking water discharge standard.Using mathematical statistics methods such as clustering and principal component analysis, qualitative or sxemiquantitative analysis is carried out to unknown anion.
Description
Technical field
The present invention relates to sensor array, specifically a kind of single organic dyestuff chelates various concentration metal ion structure
Method at colorimetric sensor array for a variety of Anionic recognitions in water.
Background technology
Anion occupies basic effect in life system, environmental system and Chemical Manufacture.As China industrializes
The living standard of the quickening of process, the people improves year by year, and the environmental pollution thus caused has become country and public's common concern
The problem of, the threat that anionic pollutant constitutes human health among these can not be ignored.These anionic pollutants mainly wrap
Include cyanide, sulfide, sulfate, chloride, fluoride, iodide, nitrite etc..Nonferrous metallurgy, steel and aluminium processing,
Coke, synthetic lucite, ceramics, electronics, plating, chemical fertilizer, the waste water of insecticide factory, agrochemical all there may be it is a large amount of these
Pollutant.Wherein fluorine ion is a kind of anion to life system important.It is well known that human body intake is suitable
Fluorine ion can pre- anti-caries, prevent osteoporosis.However excessive intake fluorine ion can lead to fluorine poisoning, cause bone
Fluorine osteosclerosis, sclerotin are hardened, osteoproliferation, make Bones and joints limitation of activity, or even paralysis, completely lose labour capacity.
Conventional Anionic recognition method includes at present：Chromatography, electrochemical process, fluorescence method, Flow Injection Analysis, ion color
Spectrometry, spectrophotometry etc..The universal cost of these methods is higher, needs large-scale instrument and skilled operator, and generally exist
Spot sampling is then delivered to laboratory and carries out off-line analysis, and there are time-consuming, analytical procedure is complicated, analytical instrument is expensive, sampling frequency
The shortcomings of rate is low and sample is not easy to maintain.Meanwhile although many detection methods can detect the anion contamination of low concentration
Object, but for the detection of true water body, the detection especially in the case of having other ion interferences seems unable to do what one wishes.At some
In the case of, it needs to know environmental pollution situation in time, to formulate corresponding treatment Countermeasures rapidly.In face of these problems, most manage
The solution thought is exactly detection in real time in situ.
Scientists have done a large amount of research and probe to the detection of the site environment of anionic pollutant and have worked, and are based on optics
Principle, electrochemical principle, the different types of sensor such as function nano material come into being.Among these, photochemistry colorimetric method
Because its is easy to operate, extensive concern of low cost and by scientists.Various indicator and with single-minded selective
Fluorescent reagents are come out one after another, and the appearance of these indicator is the Site Detection of anion and grinding for anion portable detector
Hair has established certain basis.And different anionic pollutants become the interference that intersects of indicator and inevitably ask
Topic.Therefore there is array analysis method.The prior art proposes that a kind of sensor of array is used for the analysis of anion（In
State's patent, application number：201110367842.7）, but in order to improve the resolving ability of array, in sensor array design process
In a large amount of indicator must be explored and be screened, that is, take and laborious.It is well known that in traditional Optical Sensor Array
In, a kind of indicator is intended only as a sensing unit and obtains the front and back colouring information of its reaction, this may cause a large amount of useful
Information is lost in interactive process, and therefore, the reaction equilibrium constant between each indicator and analyte is studied, foundation
The differential responses equilibrium constant distinguishes anion, can simplify setting for sensor array to avoid the screening of a large amount of indicator
Meter saves cost, improves efficiency.
Invention content
Based on above problem, it is of the same race with single organic dyestuff chelating various concentration that the purpose of the present invention is to provide one kind
Metal forms method of the array for a variety of trace anion detections in water.
To achieve the above object, the technical solution adopted by the present invention is：
Indicator array includes two or more indicator solutions；The indicator solution is by same organic dyestuff
It is reacted with same metal ion-chelant, the concentration of wherein organic dyestuff is identical, and the concentration of metal ion is different, thus
Form multiple indicator；The anion is S2-,F-,Cl-,Br-,I-,PO4 3-,C2O4 2-And CrO4 2-In one kind.
The method includes steps in detail below：
1）The structure of indicator array：
Organic dyestuff is dissolved in water-containing organic solvent, and a concentration of 1 × 10-6~5 × 10-5M；The metal reacted with it
Deionized water solution a concentration of 1 × 10-6~5 × 10-4M is mixed with organic dyestuff in different proportions, and molar ratio is 1:
10~200:Between 1, two or more indicator solutions are obtained；Each indicator solution takes same volume to be respectively placed in bottom
In transparent container, indicator array is constituted；
2) foundation of anion " fingerprint databases "：
Into each indicator solution of step 1) be added certain volume anion standard solution, after mixing in solution the moon from
The concentration of son is respectively S2-(3.0×10-5M), F-(5.6×10-4M), Cl-(7.05×10-3M), Br-(5.0×10-5M), I-
(5.0×10-5M), PO4 3-(1.0×10-4M), CrO4 2-(2.88x10-5M), C2O4 2-(5×10-4M)], these concentration are corresponding
It is respective anionic in state sewage emission standard or the upper concentration of tap water examination criteria；Anion is sent out with organic dyestuff
Raw displacement reaction, causes indicator to generate the variation of color；
It is imaged by color-image forming apparatus, acquires each indicator solution and the color before and after anionic reactive, it is right
Color is digitized processing, and image is corresponding red before and after obtaining indicator reaction（R）, it is green（G）, it is blue（B）Value, will scheme after reaction
The rgb value of picture subtracts the rgb value of image before reaction, obtains the Δ R of " subtractive image ", Δ G and Δ B, and structure anion refers at this
Show " fingerprint databases " under agent solution；
3) anionic water solution example detects：
It is added and step 2 in each indicator solution obtained to step 1)）The anionic water solution example of same volume；
According to step 2）The Δ R of the method extraction " subtractive image ", Δ G and Δ B values, obtain unknown anionic water solution example
" finger-print "；
Using mathematical statistics method, the spectrum data of sample and the database of " fingerprint databases " are contrasted, to right
Anionic water solution example carries out qualitative or sxemiquantitative analysis.
The organic dyestuff is 4-2- thiazoles resorcinol, 4- (2- pyridylazos) resorcinol, 5- dimethylamine -2-（2-
Azo pyridine）Phenol, 2- (3,5- bis- Bromo-2-pyridylazo) -5- diethylamino phenols, the black T of cadmium, (5- is bromo- by 1,3- diamino -4-
Any one of 2- pyridylazos) benzene, rose-red argentum reagent or antipyrine.
The metal ion is any one of copper, mercury, lead, nickel, cadmium or silver.
The organic solvent is any one or more in ethyl alcohol, acetone, acetonitrile, n-butanol, tetrahydrofuran or ether.
The volume ratio that the anion standard solution is mixed with indicator solution is 1:10~1:500；The anionic water
The volume ratio that solution example is mixed with indicator solution is 1:10~1:500.The mathematical statistics is will be right after image digitazation
Data clusters are analyzed or principal component analytical method, using Matlab, MVSP（Multi-Variate Statistic
Package）、SPSS（Statistical Package for the Social Sciences）In statistical software it is a kind of into
Row analysis.
The invention has the advantages that:
1. anion color developing detection relative difficulty, on the basis of being mainly mostly based on hydrogen bond because of its reaction, active force
It is very weak.The application of indicator displacement reaction will be golden by means of stronger precipitation and complexing between anion and metal ion
Belong to ion to cement out from chelate, so that chelate color is generated variation, largely improve the spirit of Anionic recognition
Sensitivity.
2. the mode of film scanning effectively overcomes shadow caused by the reflective and shadow of generally existing in solution imaging process
It rings, the solution imaging photograph of color stable homogeneous can be obtained.
3. it is different using the reaction equilibrium constant between different anion and metallo-chelate, with the same of various concentration
Indicator forms sensor array, and color change when each sensing unit is reacted with the same anion of same concentration is not
Together so that each anion corresponds to its unique dactylogram.
4. indicator can be reflected with generated color change after anionic reactive by digitized form, it is
Quantitative and semi-quantitative analysis provides basis, while being conducive to the Mathematical Statistics Analysis of database, therewith for each anion structure
Corresponding finger-print.
5. comparing more traditional array approach, generally requires multiple metal ions and multiple organic dyestuff, process are numerous
Miscellaneous, it is only necessary to a metal ion species and a kind of organic dyestuff for this method, avoid the screening of big dosis indicators, simplify array
The design of sensor, saves cost, improves efficiency.
Description of the drawings
Fig. 1 is the response that indicator replaces 6 × 28 kinds of anion of array pair of colorimetric sensor；
Fig. 2 is the clustering under indicator displacement colorimetric sensor 6 × 2 array pair, 8 kinds of anion certain concentrations, and
The classification analysis of unknown anion.
Specific implementation mode
The method includes steps in detail below：
1）The structure of indicator array：Organic dyestuff（4-2- thiazoles resorcinol, 4- (2- pyridylazos) resorcinol,
5- dimethylamine -2-（2- azo pyridines）Phenol, 2- (3,5- bis- Bromo-2-pyridylazo) -5- diethylamino phenols, cadmium black T, 1,3- bis-
Any one of amino -4- (5- Bromo-2-pyridylazos) benzene, rose-red argentum reagent or antipyrine）It is dissolved in aqueous organic molten
Agent（Any one or more in ethyl alcohol, acetone, acetonitrile, n-butanol, tetrahydrofuran or ether）In, a concentration of 1 × 10-6~
5×10-5M；The metal ion reacted with it（Any one of copper, mercury, lead, nickel, cadmium or silver）Concentration of aqueous solution is 1 × 10-6~
5×10-4M is mixed with organic dyestuff in different proportions, and molar ratio is 1:10~200:Between 1, two or two are obtained
A agent solution indicated above；Each indicator solution takes same volume to be respectively placed in the transparent container in bottom, constitutes indicator battle array
Row；
2) foundation of anion " fingerprint databases "：Into each indicator solution of step 1) be added certain volume the moon from
Substandard solution, the concentration of anions is respectively S after mixing2-(3.0×10-5M), F-(5.6×10-4M), Cl-(7.05
×10-3M), Br-(5.0×10-5M), I-(5.0×10-5M), PO4 3-(1.0×10-4M), CrO4 2-(2.88x10-5M), C2O4 2-
(5×10-4M)；Anion occurs displacement with organic dyestuff and reacts, and indicator is caused to generate the variation of color；
It is imaged by color-image forming apparatus, acquires each indicator solution and the color before and after anionic reactive, it is right
Color is digitized processing, and image is corresponding red before and after obtaining indicator reaction（R）, it is green（G）, it is blue（B）Value, will scheme after reaction
The rgb value of picture subtracts the rgb value of image before reaction, obtains the Δ R of " subtractive image ", Δ G and Δ B, and structure anion is dense at this
" fingerprint databases " under degree；
3) anionic water solution example detects：
It is added and step 2 in each indicator solution obtained to step 1)）The anionic water solution example of same volume；
According to step 2）The Δ R of the method extraction " subtractive image ", Δ G and Δ B values, obtain unknown anionic water solution example
" finger-print "；
Using mathematical statistics method（Any one of Matlab, MVSP, SPSS）, by the spectrum data of sample and " fingerprint
The database of spectrum library " contrasts, to carry out qualitative or sxemiquantitative analysis to anionic water solution example.
Embodiment 1：
1）The structure of indicator array：Organic dyestuff 2- (bis- Bromo-2-pyridylazos of 3,5-) -5- diethylamino phenols are dissolved in
1:In 1 ethanol/water, after mercury metal ionic reaction, organic dyestuff a concentration of 5 × 10-6M；Metal ion mercury a concentration of 1 × 10-5, 2 × 10-5, 3 × 10-5, 4 × 10-5, 5 × 10-5, 6 × 10-5, 7 × 10-5, 8 × 10-5, 9 × 10-5, 1 × 10-4, 2 × 10-4, 5
×10-4M obtains 12（6×2）A indicator solution；Each indicator solution takes 180 μ L to be respectively placed in the transparent container in bottom
In, constitute indicator array；
2) foundation of anion " fingerprint databases "：18 μ L anion marks are added into each indicator solution of step 1)
Quasi- solution, the concentration of anions is respectively S after mixing2-(3.0×10-5M), F-(5.6×10-4M), Cl-(7.05×
10-3M), Br-(5.0×10-5M), I-(5.0×10-5M), PO4 3-(1.0×10-4M), CrO4 2-(2.88x10-5M), C2O4 2-(5
×10-4M)；Anion occurs displacement with organic dyestuff and reacts, and indicator is caused to generate the variation of color（Fig. 1）；As shown in Figure 1,
Via Photoshop softwares, by equal proportion enhancing, (in order to facilitate observation of, color gamut extends generated color change from 8-23
To 0-255).Software processing is only to show the power of color change, is had no effect on after each anion digitlization " finger-print "
Numerical value.It is that it effectively carries out area it will be evident that 8 kinds of anion respectively illustrate its exclusive " finger-print " from figure
Divide and lays a good foundation.
It is imaged by color-image forming apparatus, acquires each indicator solution and the color before and after anionic reactive, it is right
Color is digitized processing, and image is corresponding red before and after obtaining indicator reaction（R）, it is green（G）, it is blue（B）Value, will scheme after reaction
The rgb value of picture subtracts the rgb value of image before reaction, obtains the Δ R of " subtractive image ", Δ G and Δ B, and structure anion is dense at this
" fingerprint databases " under degree；
3) anionic water solution example detects：
The anionic water solution example of 18 μ L is added in each indicator solution obtained to step 1)；
According to step 2）The Δ R of the method extraction " subtractive image ", Δ G and Δ B values, it is water-soluble to obtain unknown anion
" finger-print " of liquid sample；
Using mathematical statistics method SPSS, the spectrum data of sample and the database of " fingerprint databases " are contrasted, from
And qualitative or sxemiquantitative analysis is carried out to anionic water solution example, show that unknown anion is fluorine ion, and have reached
Or beyond the normal concentration in " fingerprint databases "（Fig. 2）；As shown in Fig. 2, each anion carries out 5 parallel tests, sensing
The excellent reproducibility of device ensures that 5 groups of parallel tests of same anion are classified as one kind well；Meanwhile establish it is each it is cloudy from
After sub-figure in the Basis of Database of " finger-print ", the response of various dimensions so that 8 kinds of anion are effectively distinguished each other.
Unknown anion and fluorine ion have immediate European square away from, it is fluorine ion to show unknown anion most possibly, and
Its concentration has been approached or is more than concentration of the fluorine ion in " finger-print ".
Claims (6)
1. a kind of method based on indicator array detection anion, it is characterised in that：Indicator array includes two or two
Agent solution indicated above；The indicator solution is reacted by same organic dyestuff with same metal ion-chelant, wherein
The concentration of organic dyestuff is identical, and the concentration of metal ion is different, and multiple indicator are consequently formed；The anion is S2-,
F-,Cl-,Br-,I-,PO4 3-,C2O4 2-And CrO4 2-In one kind；
The method includes steps in detail below：
1) structure of indicator array：
Organic dyestuff is dissolved in water-containing organic solvent, and a concentration of 1 × 10-6~5 × 10-5M；The metal ion water reacted with it
Solution concentration is 1 × 10-6~5 × 10-4M is mixed with organic dyestuff in different proportions, and molar ratio is 1:10~
200:Between 1, two or more indicator solutions are obtained；It is transparent that each indicator solution takes same volume to be respectively placed in bottom
Container in, constitute indicator array；
2) foundation of anion " fingerprint databases "：
Certain volume anion standard solution, anions after mixing are added into each indicator solution of step 1)
Concentration is respectively 3.0 × 10-5The S of M2-, 5.6 × 10-4The F of M-, 7.05 × 10-3The Cl of M-, 5.0 × 10-5The Br of M-, 5.0 × 10-5The I- of M, 1.0 × 10-4The PO of M4 3-, 2.88 × 10-5The CrO of M4 2-, 5 × 10-4The C of M2O4 2-；Anion metathesis goes out in indicator
Metal ion, cause indicator generate color variation；
It is imaged by color-image forming apparatus, each indicator solution and the color before and after anionic reactive is acquired, to color
It is digitized processing, image corresponding red (R), green (G), blue (B) value before and after indicator reaction are obtained, by image after reaction
Rgb value subtracts the rgb value of image before reaction, obtains the Δ R of " subtractive image ", Δ G and Δ B, structure anion is in the indicator
" fingerprint databases " under solution；
3) anionic water solution example detects：
The anionic water solution example with step 2) same volume is added in each indicator solution obtained to step 1)；According to
The Δ R of method extraction " subtractive image " described in step 2), Δ G and Δ B values, obtain " referring to for unknown anionic water solution example
Line collection of illustrative plates "；
Using mathematical statistics method, the spectrum data of sample and the database of " fingerprint databases " are contrasted, to the moon from
Sub- aqueous sample carries out qualitative or sxemiquantitative analysis.
2. according to the method for claim 1, it is characterised in that：The organic dyestuff is 4-2- thiazoles resorcinol, 4- (2-
Pyridylazo) resorcinol, 5- dimethylamine -2- (2- azo pyridines) phenol, 2- (bis- Bromo-2-pyridylazos of 3,5-) -5- diethyls
Any in amino phenols, cadmium black T, 1,3- diamino -4- (5- Bromo-2-pyridylazos) benzene, rose-red argentum reagent or antipyrine
Kind.
3. according to the method for claim 1, it is characterised in that：The metal ion is in copper, mercury, lead, nickel, cadmium or silver
It is any.
4. according to the method for claim 1, it is characterised in that：The organic solvent be ethyl alcohol, acetone, acetonitrile, n-butanol,
Any one or more in tetrahydrofuran or ether.
5. according to the method for claim 1, it is characterised in that：What the anion standard solution was mixed with indicator solution
Volume ratio is 1:10~1:500；The volume ratio that the anionic water solution example is mixed with indicator solution is 1:10~1:
500。
6. according to the method for claim 1, it is characterised in that：The mathematical statistics is will to gather to data after image digitazation
Alanysis or principal component analytical method are analyzed using a kind of in Matlab, MVSP, SPSS statistical software.
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| US10890574B2 (en) * | 2018-11-05 | 2021-01-12 | Hach Company | Digestion of lead(0) and subsequent colorimetric detection of lead(II) |
| CN109520984B (en) * | 2018-12-06 | 2021-04-06 | 南通中国科学院海洋研究所海洋科学与技术研究发展中心 | Method for rapidly detecting sulfate reducing bacteria in seawater environment |
| CN112268899B (en) * | 2020-10-15 | 2022-11-04 | 成都中医药大学 | Method for rapidly identifying fritillaria medicinal materials |
| CN113466225B (en) * | 2021-06-30 | 2023-06-02 | 宁波市中医院 | Method for identifying radix ophiopogonis production area |
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