CN109142303A - A method of detection mercury ion - Google Patents
A method of detection mercury ion Download PDFInfo
- Publication number
- CN109142303A CN109142303A CN201811081517.2A CN201811081517A CN109142303A CN 109142303 A CN109142303 A CN 109142303A CN 201811081517 A CN201811081517 A CN 201811081517A CN 109142303 A CN109142303 A CN 109142303A
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- mercury ion
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- citric acid
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- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/38—Diluting, dispersing or mixing samples
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- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
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- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Optics & Photonics (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
The invention discloses a kind of methods for detecting mercury ion, and step is: 1) obtaining solution A for citric acid and urea are soluble in water；After microwave heating, citric acid and urea dissolution, centrifugal treating prepares partial size in the carbon nano dot of 1-10nm；2) step carbon nano dot is dissolved in distilled water and is made into mass volume ratio as 0.05mg/ml carbon nanodot solution；3) prepare liquid containing mercury ion is added in carbon nanodot solution and obtains mixed solution, it is uniformly mixed, it is placed in cuvette, use Pekin-Elmer LS-55 type Fluorescence Spectrometer, fluorescence detection is carried out under the excitation wavelength of 420nm, if fluorescence relative intensity less than 780, illustrates that there are mercury ions in solution.The present invention is the fluorescent emission relied on by using good water solubility, good light stability, excitation wavelength, toxicity is low, the luminous carbon nano dot that is easy to get is as fluorescent optical sensor, realizes the detection of mercury ion.
Description
Technical field
The invention belongs to technical field of analytical chemistry more particularly to a kind of methods for detecting mercury ion.
Background technique
Mercury is a kind of high toxicity and there are fairly common heavy metals in living environment, the harm to environment and organism
It is very big.Mercury contact can cause different degrees of influence to organism, and poisonous effect can directly result in thyroid gland, liver, heart
Disease, and cause chronic mercury poisoning, nerve problems, or even cause the diseases such as hematuria, uremia.Therefore, mercury ion is detected
The research of correlation technique have very important significance.
Fluorescent optical sensor mainly utilizes hair before and after main body (luminescent material) and object (small molecule or ion) selective binding
The change (red shift or blue shift) of luminous intensity (enhance or be quenched) or luminous frequency identifies and analyzes target molecule or ion.Closely
It is highly selective due to fluorescent optical sensor over year, it is highly sensitive, good invertibity and it is easy to the features such as being miniaturized and becomes point
The research hotspot in sub- identification field.
Currently, the material of common fluorescent optical sensor includes organic fluorescent molecule, rare earth luminous complex etc., but it is common
Fluorescent material all there are some disadvantages, for example poorly water-soluble, be not easy to synthesis etc..
Nanometer carbon quantum dot belongs to luminescent nanoparticle.In recent years, due to its with good water solubility, photostability,
The properties such as the fluorescent emission that biocompatibility, excitation wavelength rely on cause extensive concern.
Summary of the invention
For the prior art, the invention proposes a kind of methods for detecting mercury ion.Mainly by utilizing fluorescence nano
Carbon quantum dot detects mercury ion, solves the problems, such as mercury ion detecting.
In order to solve the above-mentioned technical problem, a kind of method detecting mercury ion proposed by the present invention, comprising the following steps:
Step 1: obtaining solution A for citric acid and urea are soluble in water, wherein the mass volume ratio of citric acid and water is
The mass ratio of 1g/10~15ml, urea and citric acid is 2:1；It is put into micro-wave oven and heats 4-5min, citric acid and urea dissolution
Afterwards, then with the centrifuge of 18500rpm it is centrifuged 3 times, each 20min, prepares partial size in the carbon nano dot of 1-10nm；
Mass volume ratio is made into Step 2: carbon nano dot made from step 1 is dissolved in distilled water as 0.05mg/ml carbon
Nanodot solution；
Step 3: the prepare liquid containing mercury ion is added to carbon nano dot made from step 2 for 1:2 according to volume ratio
Mixed solution is obtained in solution, is uniformly mixed, is placed in cuvette, using Pekin-Elmer LS-55 type Fluorescence Spectrometer,
Fluorescence detection is carried out under the excitation wavelength of 420nm, if fluorescence relative intensity less than 780, illustrates that there are mercury ions in solution.
In carbon nano dot made from step 1, particle diameter distribution accounts for 20~30% between 5-6nm.
Compared with prior art, the beneficial effects of the present invention are:
(1) by the present invention in that with good water solubility, toxicity is low, fluorescent emission, the good light stability of excitation wavelength dependence are easy
The Illuminant nanometer carbon quantum dot obtained realizes the detection of mercury ion as fluorescent optical sensor；
(2) the method for the invention signal stabilization, system be very simple, sample is not required to pre-treatment；
(3) the method for the invention specificity is good, and sensitivity is relatively high, detection speed ratio is very fast, biological sample analysis,
And the fields such as medical diagnosis suffer from highly important meaning.
Detailed description of the invention
Fig. 1 and Fig. 2 is testing result of the detection method to mercury ion specificity；
Fig. 3, Fig. 4, Fig. 5 and Fig. 6 are influence of the ion concentration of mercury (0-10mM) to nano-sized carbon quantum dot fluorescence intensity.
Specific embodiment
Technical solution of the present invention is described in further detail in the following with reference to the drawings and specific embodiments, it is described specific
Embodiment is only explained the present invention, is not intended to limit the invention.
A kind of method detecting mercury ion proposed by the present invention, comprising the following steps:
1) preparation of carbon nano dot: 1g citric acid and 2g urea are dissolved in 10ml distilled water, is put into micro-wave oven and heats
It 4-5 minutes, is centrifuged 3 times, each 20min with the centrifuge of 18500rpm again after dissolution, the carbon for preparing partial size in 1-10nm is received
Meter Dian, wherein particle diameter distribution accounts for 25% or so between 5-6nm.If large-scale production, all raw material dosages press above-mentioned ratio
Example increase and decrease, the i.e. mass volume ratio of citric acid and water are 1g/10~15ml, and the mass ratio of urea and citric acid is 2:1.
2) carbon nano dot obtained above is dissolved in distilled water and is made into mass volume ratio and is by the preparation of carbon nanodot solution
0.05mg/ml carbon nanodot solution.
3) detection of mercury ion specificity: respectively by concentration be the 20 μ L silver ion solutions of 10mM, zinc ion solution, manganese from
Sub- solution, sodium ion solution, mercury ion solution, chromium ion solution, nickel ion solution, barium ions solution, potassium ion solution, magnesium from
Sub- solution is added in the carbon nanodot solution of 200 μ L steps 2) preparation, is sufficiently mixed, is placed in cuvette, uses Pekin-
Elmer LS-55 type Fluorescence Spectrometer, carries out fluorescence detection under the excitation wavelength of 420nm respectively.
Obtained by Fig. 1 and Fig. 2, carbon nanodot solution to silver ion, zinc ion, manganese ion, sodium ion, chromium ion, nickel ion,
Barium ions, potassium ion, the response signal of magnesium ion are low, and to the response signal of mercury ion height.
4) the 20 μ L mercury ion prepare liquids that concentration is 0-10mM the detection of mercury ion: are added to 200 μ L steps 2) respectively
In the carbon nanodot solution of preparation, it is sufficiently mixed, is placed in cuvette, using Pekin-Elmer LS-55 type Fluorescence Spectrometer,
Fluorescence detection is carried out under the excitation wavelength of 420nm respectively.
It being obtained by Fig. 3 to Fig. 6 and table 1 to table 8, there is no the positions for changing carbon nanodot emission peak for the addition of mercury ion, and
And with the increase of ion concentration of mercury, fluorescence intensity gradually weakens.
Its testing result is, if fluorescence relative intensity less than 780, illustrates that there are mercury ions in solution.
The present invention is low, easy by using good water solubility, good light stability, fluorescent emission, the toxicity of excitation wavelength dependence
The luminous carbon nano dot obtained realizes the detection of mercury ion as fluorescent optical sensor.
Table 1
Table 2
Table 3
Table 4
Table 5
Table 6
Table 7
Table 8
Although above in conjunction with attached drawing, invention has been described, and the invention is not limited to above-mentioned specific implementations
Mode, the above mentioned embodiment is only schematical, rather than restrictive, and those skilled in the art are at this
Under the enlightenment of invention, without deviating from the spirit of the invention, many variations can also be made, these belong to of the invention
Within protection.
Claims (2)
1. a kind of method for detecting mercury ion, which comprises the following steps:
Step 1: obtaining solution A for citric acid and urea are soluble in water, wherein the mass volume ratio of citric acid and water is 1g/10
The mass ratio of~15ml, urea and citric acid is 2:1；It is put into micro-wave oven and heats 4-5min, after citric acid and urea dissolution, then
It is centrifuged 3 times, each 20min with the centrifuge of 18500rpm, prepares partial size in the carbon nano dot of 1-10nm；
Mass volume ratio is made into Step 2: carbon nano dot made from step 1 is dissolved in distilled water as 0.05mg/ml carbon nanometer
Point solution；
Step 3: the prepare liquid containing mercury ion is added to carbon nanodot solution made from step 2 for 1:2 according to volume ratio
In obtain mixed solution, be uniformly mixed, be placed in cuvette, using Pekin-Elmer LS-55 type Fluorescence Spectrometer,
Fluorescence detection is carried out under the excitation wavelength of 420nm, if fluorescence relative intensity less than 780, illustrates that there are mercury ions in solution.
2. detecting the method for mercury ion according to claim 1, which is characterized in that it is characterized in that, carbon made from step 1
Particle diameter distribution accounts for 20~30% between 5-6nm in nano dot.
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| CN201811081517.2A CN109142303A (en) | 2018-09-17 | 2018-09-17 | A method of detection mercury ion |
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| CN201811081517.2A CN109142303A (en) | 2018-09-17 | 2018-09-17 | A method of detection mercury ion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988571A (en) * | 2019-04-06 | 2019-07-09 | 天津大学 | A kind of preparation of solid state fluorescence carbon quantum dot material and application |
| CN116478688A (en) * | 2023-03-16 | 2023-07-25 | 长沙矿冶院检测技术有限责任公司 | Carbon quantum dot for detecting mercury ions, synthesis method thereof, mercury ion detection kit and application thereof |
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| CN102942175A (en) * | 2012-11-23 | 2013-02-27 | 中国科学院长春光学精密机械与物理研究所 | Application of carbon nanodots as water-soluble ratiometric fluorescent probe |
| CN103834397A (en) * | 2014-03-11 | 2014-06-04 | 太原理工大学 | Method for preparing water-soluble fluorescent carbon dots |
| CN104804734A (en) * | 2015-04-01 | 2015-07-29 | 河南师范大学 | Synthesis method for sulfur-nitrogen-doped fluorescent carbon dots according to one-step microwave method |
| CN105044071A (en) * | 2015-08-18 | 2015-11-11 | 太原理工大学 | Method for detecting Hg<2+> of clean water by using nitrogen-doped carbon dots |
| CN108516533A (en) * | 2018-04-04 | 2018-09-11 | 桂林理工大学 | A kind of preparation method of hair peak green fluorescent carbon point |
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2018
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Patent Citations (5)
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| CN102942175A (en) * | 2012-11-23 | 2013-02-27 | 中国科学院长春光学精密机械与物理研究所 | Application of carbon nanodots as water-soluble ratiometric fluorescent probe |
| CN103834397A (en) * | 2014-03-11 | 2014-06-04 | 太原理工大学 | Method for preparing water-soluble fluorescent carbon dots |
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| CN105044071A (en) * | 2015-08-18 | 2015-11-11 | 太原理工大学 | Method for detecting Hg<2+> of clean water by using nitrogen-doped carbon dots |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109988571A (en) * | 2019-04-06 | 2019-07-09 | 天津大学 | A kind of preparation of solid state fluorescence carbon quantum dot material and application |
| CN109988571B (en) * | 2019-04-06 | 2022-04-19 | 天津大学 | Preparation and application of solid-state fluorescent carbon quantum dot material |
| CN116478688A (en) * | 2023-03-16 | 2023-07-25 | 长沙矿冶院检测技术有限责任公司 | Carbon quantum dot for detecting mercury ions, synthesis method thereof, mercury ion detection kit and application thereof |
| CN116478688B (en) * | 2023-03-16 | 2024-04-02 | 长沙矿冶院检测技术有限责任公司 | Carbon quantum dot for detecting mercury ions, synthesis method thereof, mercury ion detection kit and application thereof |
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