CN1967218A - Colorimetric detection and analysis method for Hg2+ ion - Google Patents
Colorimetric detection and analysis method for Hg2+ ion Download PDFInfo
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- CN1967218A CN1967218A CN 200510125522 CN200510125522A CN1967218A CN 1967218 A CN1967218 A CN 1967218A CN 200510125522 CN200510125522 CN 200510125522 CN 200510125522 A CN200510125522 A CN 200510125522A CN 1967218 A CN1967218 A CN 1967218A
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Abstract
The invention relates to the supramolecular colorimetric sensor technology, specifically refers to: in the colorful charge-transfer complexes solution, adding analyte solution, through the solution color change to detect the analyte. The method uses two-pyrrole-methane as electron donor, the quinones as the electron acceptor in polar solution to take place electronic transfer, forming colored charge transfer complexes detection solution. Mercury salt analyte is made to a certain concentration solution, mixed a certain volume of this solution with the same volume of the detection solution, the solution color changed significantly, and other metal ion compounds unable disturbing the Hg2+ ion detection. The invention has very specific colorimetric recognition ability to two price mercuric salt, and the invention has convenient solution preparation, simple colorimetric detection operation, quick colorimetric reaction color-change speed, and can complete the colorimetric detection of the analyte in a short time.
Description
Technical field
The present invention relates to a kind of colorimetric qualitative detection analytical approach at mercury ion.
Technical background
Along with the progress in development of science and technology and epoch, the protection of environment for human survival has caused people's attention more and more with improvement.The protection of earth water environment, the sustainable development of environment for human survival is had higher requirement to the relevant environment quality.But according to the update statistics, the content of mercury has more improved 3 times in water, soil, the atmosphere at present, and well-known, mercury pollution has great harm to the mankind.
The Hg of solubilised state
2+Having higher chemical activity, is the main existence form that enters pollutant in the natural water body, and its compound has higher water-soluble, also is the hinge that various mercury shapes transform.
Mercury is a kind of high toxicity heavy metal element that causes the body irreversible damage, Hg
2+Easily combining with protein that contains sulfydryl and enzyme, cause interior tens of kinds of enzyme deactivations of body or film dysfunction, is the basis of mercury toxic action thereby cause cellular damage; Hg
2+Can destroy the structural intergrity of DNA by combining with amino, hydroxyl, phosphate and nucleic acid component complexing such as base.Yet human body can't be drained the Trace Mercury of food chain or the accumulation of other approach by the metabolism of self, and the Trace Mercury accumulation will directly cause diseases such as heart, liver, thyroid gland, even cause nerve problems and chronic mercury poisoning.Therefore, mercury is paid close attention to by people the pollution of environment always, need be strict controlled in certain content range.High in developed countries such as the U.S., Japan, and proposed very strict control requirement to the degree of concern of mercury, mercury has been listed in main test item or preferentially monitored the blacklist of pollutant.
At present, the assay determination of mercury compounds generally is to adopt atomic emission spectrometry (inductively coupled plasma atomic emission spectrum); Atomic absorption spectrography (AAS) (cold vapor atomic absorbs spectrophotometric spectra, Electrothermal Atomic Absorption spectrophotometric spectra); Atomic fluorescence spectrometry (two pass atom fluorescent luminosity method, mobile injection of hydride atomic fluorescence spectrometry); Spectrophotometric method methods such as (chromogenic reagent photometry, dynamics spectrophotometric method).
Design a kind of system or synthetic compound as acceptor, utilize it to discern certain important functional group or biological micromolecule with special construction.Method the most attractive makes up and uses colorimetric sensor exactly in this technical field.In our known colorimetric sensor, host molecule as sensor is connected with a receptor site and a hyperchromic group by covalent bond, when receptor site and guest molecule are had an effect, hyperchromic group on the host molecule will produce change color, but this detection substantially all is to occur in the non-polar solvent.We find that the charge-transfer complex that quinone and two pyrroles's methane constitute also can be used in colorimetric detection, it is in 1: 1 the water/acetonitrile mixed solution or organic solvent that this electric charge transfering system can stably be present in volume ratio, and this provides advantageous environment for detecting water-soluble substances.Use the detector probe of charge-transfer complex as high selectivity, the change color visual by naked eyes optionally detects Hg
2+Utilize charge-transfer complex colorimetric detection Hg
2+At present no pertinent literature report.
Summary of the invention
Purpose of the present invention is exactly for a kind of new Hg is provided
2+The high selectivity of ion detection, convenient and simple analytical approach.
Thinking of the present invention is that the requirement analytical approach is easy and simple to handle, and the selectivity height is not finished the qualitative analysis of sample at short notice by macroscopic change color by instrument.
The present invention realizes by following measure:
A kind of Hg
2+The colorimetric detection and analysis method of ion is characterized in that this method may further comprise the steps:
A, use two pyrroles's methane and quinoness as solvent, are made the detectable of blue charge-transfer complex as phenyl compound with acetonitrile; Wherein two pyrroles's methane are selected from a kind of in dihydroxy two pyrroles's methane, dimethyl two pyrroles's methane, diethyl two pyrroles's methane, cyclohexyl two pyrroles's methane, the cyclopentyl two pyrroles's methane, quinones selects 7 for use, 7,8,8-four cyano quinone bismethane (TCNQ);
B, make detection liquid, Hg with dissolved in distilled water mercury salt to be measured
2+Concentration be 5.0 * 10
-3-5.0 * 10
-4M;
C, with Hg
2+The detection liquid that ion detection reagent is identical with volume mixes, and mixed liquor has blueness to become colorless.
At Hg
2+In the ion detection reagent, the concentration of two pyrroles's methane is 0.001-0.00025M, and the concentration of quinones is 1.0 * 10
-4M-1.0 * 10
-5M.
When containing other metal cation in detecting liquid, change color does not take place in detectable.
We have made contrast test with analytical instrument:
Under same condition, with the Hg of respective concentration
2+Solion is made reference, with the absorbance variation at ultraviolet-visible spectrophotometric determination 613nm wavelength place in solution.In detecting liquid, add Hg
2+Deionized water solution, complex disappears at the absorption peak at 613nm place.
The present invention has following substantive distinguishing features:
1. the present invention need not Hg
2+Ion carries out special processing, Hg
2+The aqueous solution of ion just can satisfy the requirement that detects.
2. detection liquid used in the present invention can mix with arbitrary proportion mutually with water, and solution mixes the back does not have wild effect generations such as precipitation.
3. Hg used in the present invention
2+Ion detection reagent, its process for preparation is simple, can be positioned in the refrigerator standby after preparation finishes.
4. the present invention is characterized in that this detection method not by any instrument, detects measured matter by macroscopic change color.
5. the present invention is easy fast, just can detect measured object by change color in several minutes.
Description of drawings
Fig. 1 is for using Hg
2+Ion detection reagent detects the ultraviolet spectrogram of phenylamino.
Fig. 2 is for using Hg
2+But ion detection reagent detects the colorimetric view of phenylamino.
Scheming Chinese and English primary and secondary represents respectively: blank (A), cadmium nitrate (B), zinc nitrate (C), chromic nitrate (D), barium nitrate (E), silver nitrate (F), magnesium sulphate (G), plumbi nitras (H), mercuric nitrate (I), common salt (J), potassium bromide (K), lime chloride (L), aluminum chloride (M).
Embodiment
Embodiment 1
Carry out the preparation of detectable: in dissolve measuring bottle, accurately take by weighing a certain amount of 7,7,8,8-four cyano quinone bismethane (concentration 1.0 * 10
-4M) and a certain amount of dimethyl two pyrroles's methane (concentration 1.0 * 10
-3M), it is fixed molten to add the acetonitrile dissolving, and solution becomes after the mazarine stand-by.This dark blue solution is for detecting Hg
2+The detectable of ion.
Carry out Hg
2+The preparation of ion detection liquid: take by weighing following 11 kinds of metal cation salts (potassium bromide, sodium chloride, lime chloride, magnesium sulphate, aluminum chloride, chromic nitrate, cadmium nitrate, zinc nitrate, silver nitrate, plumbi nitras, barium nitrate) and mercuric nitrate respectively in different test tubes, the distilled water that pipettes 10ml with transfer pipet is 5.0 * 10 after the dissolving in the test tube that slaine and mercuric nitrate are housed respectively
-3The solution of M.
Carry out Hg
2+The detection of ionic compound: with the metallic ion aqueous solution of 2ml respectively with TCNQ-dimethyl two pyrroles's methane (TCNQ=1.0 * 10 of 2ml
-4M, dimethyl two pyrroles's methane=1.0 * 10
-3M) detection agent mixes, and observes the change color of different metal solion, and the gained result as shown in Figure 2.
Embodiment 2
Carry out the preparation of detectable: in dissolve measuring bottle, accurately take by weighing a certain amount of 7,7,8,8-four cyano quinone bismethane (concentration 1.0 * 10
-4M) and a certain amount of dihydroxymethyl two pyrroles's methane (concentration 1.0 * 10
-3M), it is fixed molten to add the acetonitrile dissolving, and solution becomes after the mazarine stand-by.This dark blue solution is for detecting Hg
2+The detectable of ion.
Carry out Hg
2+The preparation of ion detection liquid: take by weighing following 11 kinds of metal cation salts (potassium bromide, sodium chloride, lime chloride, magnesium sulphate, aluminum chloride, chromic nitrate, cadmium nitrate, zinc nitrate, silver nitrate, plumbi nitras, barium nitrate) and mercuric nitrate respectively in different test tubes, the distilled water that pipettes 10ml with transfer pipet is 5.0 * 10 after the dissolving in the test tube that slaine and mercuric nitrate are housed respectively
-3The solution of M.
Carry out Hg
2+The detection of ionic compound: with the metallic ion aqueous solution of 2ml respectively with TCNQ-dimethyl two pyrroles's methane (TCNQ=1.0 * 10 of 2ml
-4M, dimethyl two pyrroles's methane=1.0 * 10
-3M) detection agent mixes, and observes the change color of different metal solion, and the gained result as shown in Figure 2.
Under same condition, make reference with the metal ion solution of respective concentration, change with the absorbance of ultraviolet-visible spectrophotometric determination at 613nm wavelength place.Measured result adds Hg as shown in Figure 1 in detecting liquid
2+Deionized water solution, complex disappears at the absorption peak at 613nm place.
Embodiment 3
Carry out the preparation of detectable: in dissolve measuring bottle, accurately take by weighing a certain amount of 7,7,8,8-four cyano quinone bismethane (concentration 1.0 * 10
-4M) and a certain amount of diethyl two pyrroles's methane (concentration 1.0 * 10
-3M), it is fixed molten to add the acetonitrile dissolving, and solution becomes after the mazarine stand-by.This dark blue solution is for detecting Hg
2+The detectable of ion.
Carry out Hg
2+The preparation of ion detection liquid: take by weighing following 11 kinds of metal cation salts (potassium bromide, sodium chloride, lime chloride, magnesium sulphate, aluminum chloride, chromic nitrate, cadmium nitrate, zinc nitrate, silver nitrate, plumbi nitras, barium nitrate) and mercuric nitrate respectively in different test tubes, the distilled water that pipettes 10ml with transfer pipet is 5.0 * 10 after the dissolving in the test tube that slaine and mercuric nitrate are housed respectively
-3The solution of M.
Carry out Hg
2+The detection of ionic compound: with the metallic ion aqueous solution of 2ml respectively with TCNQ-diethyl two pyrroles's methane (TCNQ=1.0 * 10 of 2ml
-4M, diethyl two pyrroles's methane=1.0 * 10
-3M) detection agent mixes, and observes the change color of different metal solion, and the gained result as shown in Figure 2.
Embodiment 4
Carry out the preparation of detectable: in dissolve measuring bottle, accurately take by weighing a certain amount of 7,7,8,8-four cyano quinone bismethane (concentration 1.0 * 10
-4M) and a certain amount of cyclohexyl two pyrroles's methane (concentration 1.0 * 10
-3M), it is fixed molten to add the acetonitrile dissolving, and solution becomes after the mazarine stand-by.This dark blue solution is for detecting Hg
2+The detectable of ion.
Carry out Hg
2+The preparation of ion detection liquid: take by weighing following 11 kinds of metal cation salts (potassium bromide, sodium chloride, lime chloride, magnesium sulphate, aluminum chloride, chromic nitrate, cadmium nitrate, zinc nitrate, silver nitrate, plumbi nitras, barium nitrate) and mercuric nitrate respectively in different test tubes, the distilled water that pipettes 10ml with transfer pipet is 5.0 * 10 after the dissolving in the test tube that slaine and mercuric nitrate are housed respectively
-3The solution of M.
Carry out Hg
2+The detection of ionic compound: with the metallic ion aqueous solution of 2ml respectively with TCNQ-cyclohexyl two pyrroles's methane (TCNQ=1.0 * 10 of 2ml
-4M, cyclohexyl two pyrroles's methane=1.0 * 10
-3M) detection agent mixes, and observes the change color of different metal solion, and the gained result as shown in Figure 2.
Embodiment 5
Carry out the preparation of detectable: in dissolve measuring bottle, accurately take by weighing a certain amount of 7,7,8,8-four cyano quinone bismethane (concentration 1.0 * 10
-4M) and a certain amount of cyclopentyl two pyrroles's methane (concentration 1.0 * 10
-3M), it is fixed molten to add the acetonitrile dissolving, and solution becomes after the mazarine stand-by.This dark blue solution is for detecting Hg
2+The detectable of ion.
Carry out Hg
2+The preparation of ion detection liquid: take by weighing following 11 kinds of metal cation salts (potassium bromide, sodium chloride, lime chloride, magnesium sulphate, aluminum chloride, chromic nitrate, cadmium nitrate, zinc nitrate, silver nitrate, plumbi nitras, barium nitrate) and mercuric nitrate respectively in different test tubes, the distilled water that pipettes 10ml with transfer pipet is 5.0 * 10 after the dissolving in the test tube that slaine and mercuric nitrate are housed respectively
-3The solution of M.
Carry out Hg
2+The detection of ionic compound: with the metallic ion aqueous solution of 2ml respectively with TCNQ-cyclopentyl two pyrroles's methane (TCNQ=1.0 * 10 of 2ml
-4M, cyclopentyl two pyrroles's methane=1.0 * 10
-3M) detection agent mixes, and observes the change color of different metal solion, and the gained result as shown in Figure 2.
Claims (3)
1, a kind of Hg
2+The colorimetric detection and analysis method of ion is characterized in that this method may further comprise the steps:
A, use two pyrroles's methane and quinoness as solvent, are made the detectable of blue charge-transfer complex as phenyl compound with acetonitrile; Wherein two pyrroles's methane are selected from a kind of in dihydroxy two pyrroles's methane, dimethyl two pyrroles's methane, diethyl two pyrroles's methane, cyclohexyl two pyrroles's methane, the cyclopentyl two pyrroles's methane, and quinones selects 7,7,8 for use, 8-four cyano quinone bismethane;
B, make detection liquid, Hg with dissolved in distilled water mercury salt to be measured
2+Concentration be 5.0 * 10
-3-5.0 * 10
-4M;
C, with Hg
2+The detection liquid that ion detection reagent is identical with volume mixes, and mixed liquor has blueness to become colorless.
2, as claims 1 said method, the concentration that it is characterized in that two pyrroles's methane is 0.001-0.00025M.
3, as claims 1 said method, the concentration that it is characterized in that quinones is 1.0 * 10
-4M-1.0 * 10
-5M.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101255225A CN100451628C (en) | 2005-11-17 | 2005-11-17 | Colorimetric detection and analysis method for Hg2+ ion |
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|---|---|---|---|
| CNB2005101255225A CN100451628C (en) | 2005-11-17 | 2005-11-17 | Colorimetric detection and analysis method for Hg2+ ion |
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| Publication Number | Publication Date |
|---|---|
| CN1967218A true CN1967218A (en) | 2007-05-23 |
| CN100451628C CN100451628C (en) | 2009-01-14 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101871165A (en) * | 2010-06-17 | 2010-10-27 | 浙江大学 | Method for preparing anionic colorimetric sensing cellulosic material |
| CN102207465A (en) * | 2010-12-17 | 2011-10-05 | 西北师范大学 | Use of substituted mercaptothiodiazole compound in colorimetric identification of Hg<2+> |
| CN102374986A (en) * | 2010-08-13 | 2012-03-14 | 国家纳米科学中心 | Method for detecting mercury ions by using surface modified gold nano particles |
| CN103983637A (en) * | 2014-05-21 | 2014-08-13 | 成都理工大学 | Method for in-situ detecting Hg<2+> in water sample through photocatalysis visible manner |
| CN105092501A (en) * | 2015-09-23 | 2015-11-25 | 成都艾比科生物科技有限公司 | Method for determining mercury content in rapeseed oil |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2742863B1 (en) * | 1995-12-22 | 1998-03-06 | Instruments Sa | DEVICE AND METHOD FOR INTRODUCING A SAMPLE FOR ANALYTICAL ATOMIC SPECTROMETRY FOR THE CONCOMITANT MERCURY ANALYSIS |
| CN1210556C (en) * | 2001-06-05 | 2005-07-13 | 中国科学院生态环境研究中心 | Mecury compound testing strip based on enzyme inhibiting reaction |
| GB0305602D0 (en) * | 2003-03-12 | 2003-04-16 | Univ Strathclyde | Indicator |
| CN1687752A (en) * | 2005-04-29 | 2005-10-26 | 农业部环境保护科研监测所 | Test paper for detecting heavy metal mercury rapidly, preparation method and application |
-
2005
- 2005-11-17 CN CNB2005101255225A patent/CN100451628C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101871165A (en) * | 2010-06-17 | 2010-10-27 | 浙江大学 | Method for preparing anionic colorimetric sensing cellulosic material |
| CN101871165B (en) * | 2010-06-17 | 2012-01-25 | 浙江大学 | Method for preparing anionic colorimetric sensing cellulosic material |
| CN102374986A (en) * | 2010-08-13 | 2012-03-14 | 国家纳米科学中心 | Method for detecting mercury ions by using surface modified gold nano particles |
| CN102207465A (en) * | 2010-12-17 | 2011-10-05 | 西北师范大学 | Use of substituted mercaptothiodiazole compound in colorimetric identification of Hg<2+> |
| CN103983637A (en) * | 2014-05-21 | 2014-08-13 | 成都理工大学 | Method for in-situ detecting Hg<2+> in water sample through photocatalysis visible manner |
| CN105092501A (en) * | 2015-09-23 | 2015-11-25 | 成都艾比科生物科技有限公司 | Method for determining mercury content in rapeseed oil |
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| Publication number | Publication date |
|---|---|
| CN100451628C (en) | 2009-01-14 |
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Granted publication date: 20090114 Termination date: 20111117 |