CN108287148A - A kind of mercury ion sensor, preparation method and application - Google Patents
A kind of mercury ion sensor, preparation method and application Download PDFInfo
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- CN108287148A CN108287148A CN201711306708.XA CN201711306708A CN108287148A CN 108287148 A CN108287148 A CN 108287148A CN 201711306708 A CN201711306708 A CN 201711306708A CN 108287148 A CN108287148 A CN 108287148A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/55—Specular reflectivity
- G01N21/552—Attenuated total reflection
- G01N21/553—Attenuated total reflection and using surface plasmons
- G01N21/554—Attenuated total reflection and using surface plasmons detecting the surface plasmon resonance of nanostructured metals, e.g. localised surface plasmon resonance
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Abstract
The present invention discloses a kind of mercury ion sensor, preparation method and application, and preparation method includes the following steps：A, molybdenum disulfide nano material is dissolved in organic solvent first, obtains molybdenum disulfide solution, a concentration of 0.01 10mg/ml；B, surface plasmon resonance chip is immersed in the molybdenum disulfide solution, soaking time is 0.01 48 hours, then removes the molybdenum disulfide not adsorbed, finally obtains mercury ion sensor.The present invention makes full use of molybdenum disulfide nano material and the stronger interaction of mercury ion, and when, there are when mercury ion, SPR spectroscopy curve being made to move right in surface plasmon resonance (SPR) sensor chip surface solution, realization quantitatively detects mercury ion.By the present invention in that with molybdenum disulfide material, increase the sensitivity of mercury ion, and reduces detectable limit.
Description
Technical field
The present invention relates to mercury ion detecting technical field more particularly to a kind of mercury ion sensor, preparation method and applications.
Background technology
Mercury ion is a kind of huge heavy metal ion of toxicity, and it can be enriched in human body, is caused a variety of serious
Disease, it is even more serious to the body harm of pregnant woman and fetus etc., develop a kind of effective method, to detect in food and drinking water
Ion concentration of mercury have very important significance.
In the prior art, the technical method for detecting mercury ion is mainly：The technologies such as ICP-MS, fluorescence, atomic emissions, it is existing
Main problem existing for technology is：(1) of high cost, (2) sensitivity is low, and (3) are extremely difficult to lower detectable limit.
Therefore, the existing technology needs to be improved and developed.
Invention content
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of mercury ion sensor, preparation methods
And application, it is intended to solve the problems, such as that existing detection method sensitivity is low, be difficult to reach lower detectable limit.
Technical scheme is as follows：
A kind of preparation method of mercury ion sensor, wherein include the following steps：
A, molybdenum disulfide nano material is dissolved in organic solvent first, obtains molybdenum disulfide solution, a concentration of 0.01-
10mg/ml；
B, surface plasmon resonance chip is immersed in the molybdenum disulfide solution, soaking time is
0.01-48 hours, the molybdenum disulfide not adsorbed then is removed, finally obtains mercury ion sensor.
The preparation method of the mercury ion sensor, wherein the organic solvent is ethyl alcohol.
The preparation method of the mercury ion sensor, wherein in the step B, do not inhaled using deionized water removal
Attached molybdenum disulfide.
The preparation method of the mercury ion sensor, wherein the molybdenum disulfide nano material is prepared as follows：
Ammonium thiomolybdate powder is added in dimethyl formamide solution, when then reacting one section under predetermined temperature
Between, it is finally cleaned and is evaporated to obtain molybdenum disulfide nano material powder.
The preparation method of the mercury ion sensor, wherein in the step A, ultrasound is carried out to molybdenum disulfide solution
Dispersion, the molybdenum disulfide solution after being disperseed.
The preparation method of the mercury ion sensor, which is characterized in that the surface plasmon resonance core
Piece is prepared as follows：
It is coated with golden film in glass or quartz surfaces.
The preparation method of the mercury ion sensor, wherein the golden film thickness is 20-60 nanometers.
A kind of mercury ion sensor, wherein be made of any one of them preparation method as above.
A kind of application of mercury ion sensor as described above, wherein by the mercury ion sensor application in detection mercury
Ion concentration.
The application of the mercury ion sensor, wherein the solution containing mercury ion is added to and is sensed equipped with mercury ion
In the sample cell of device, and the test surfaces plasmon resonance curve of spectrum, determine the variation of resonance peak, it is true according to the variation
Determine ion concentration of mercury.
Advantageous effect：The present invention makes full use of molybdenum disulfide nano material and the stronger interaction of mercury ion, works as surface
There are when mercury ion in plasmon resonance (SPR) sensor chip surface solution, SPR spectroscopy curve is made to move right, realized
Quantitatively detect mercury ion.By the present invention in that with molybdenum disulfide material, increase the sensitivity of mercury ion, and reduces detection pole
Limit.
Description of the drawings
Fig. 1 is the transmission electron micrograph of molybdenum disulfide nano material of the present invention.
Fig. 2 is various concentration (10 of the present invention-12-10-6M the corresponding SPR spectroscopy curve graph of mercury ion solution).
Fig. 3 is various concentration (10 of the present invention-12-10-6M mercury ion solution testing result figure).
Fig. 4 is response variable quantity schematic diagram of the mercury ion sensor to different metal ions signal of the present invention.
Specific implementation mode
The present invention provides a kind of mercury ion sensor, preparation method and application, for make the purpose of the present invention, technical solution and
Effect is clearer, clear, and the present invention is described in more detail below.It should be appreciated that specific embodiment described herein
It is only used to explain the present invention, be not intended to limit the present invention.
A kind of preparation method of mercury ion sensor provided by the present invention comprising following steps：
S1, molybdenum disulfide nano material is dissolved in organic solvent first, obtains molybdenum disulfide solution, a concentration of 0.01-
10mg/ml；
S2, surface plasmon resonance chip is immersed in the molybdenum disulfide solution, soaking time is
0.01-48 hours, the molybdenum disulfide not adsorbed then is removed, finally obtains mercury ion sensor.
Surface plasmon resonance (Surface Plasmon Resonance, SPR) sensor is a kind of by spectrum song
The sensing technology of variations in refractive index in detection solution is realized in the variation of line, and the quantitative detection to molecules in solution may be implemented,
Have the characteristics that monitor in real time, quickly detects, is of low cost.
But for mercury ion sensor field, due to the limitation of sensitivity, the detection to metal mercury ions is difficult reality
The existing technical indicators such as higher sensitivity and relatively low detectable limit.The present invention by performing creative labour select molybdenum disulfide come pair
Spr sensor chip is handled.The molybdenum disulfide is basic as material important in two-dimentional transition-metal sulphides
Structure is made of sandwich tri- atomic layers of sandwich S-Mo-S combined closely, and wherein Mo atoms are in molecular layer centre position, and two
A S atom is in both ends.Sulphur atom can be effectively combined with mercury ion, and molybdenum disulfide can be as spr sensor chip
Sensitive layer has the advantages that ultra-sensitivity and ultralow detectable limit to realize the detection to mercury ion.
Specifically, the molybdenum disulfide nano material is prepared as follows：
Ammonium thiomolybdate powder is added in dimethyl formamide solution, when then reacting one section under predetermined temperature
Between, it is finally cleaned and is evaporated to obtain molybdenum disulfide nano material powder.
For example, ammonium thiomolybdate powder is added in dimethyl formamide solution using chemical method, reaction kettle is then used
Under the high temperature conditions (being more than 180 degree) reaction a period of time (such as 10 hours or more), then clean, such as carried out using ethyl alcohol
Cleaning, is then evaporated to obtain molybdenum disulfide nano material powder, naturally it is also possible to other drying modes, such as vacuum be used to do
Dry, freeze-drying etc..The molybdenum disulfide nano material prepared using chemical method is two sulphur of superstructure for having larger interlamellar spacing
Change molybdenum nano material, can preferably play it and interact with mercury ion.
Specifically, in the step S1, molybdenum disulfide nano material is dissolved in organic solvent first, obtains molybdenum disulfide
Solution, a concentration of 0.01-10mg/ml.The molybdenum disulfide nano material that will be prepared is dissolved in organic solvent, is disperseed
The good molybdenum disulfide solution of property.Its concentration is preferably 0.01-10mg/ml, such as can be 1mg/ml.The organic solvent is excellent
It is selected as ethyl alcohol, other common organic solvents, such as methanol, propyl alcohol etc. can also be used certainly.Of course for obtain dispersibility more
Good molybdenum disulfide solution can carry out ultrasonic disperse after the molybdenum disulfide nano material that will be prepared is dissolved in organic solvent,
Molybdenum disulfide solution after being disperseed.
Specifically, in the step S2, surface plasmon resonance chip is immersed in the molybdenum disulfide
In solution, soaking time is 0.01-48 hours, for example, surface plasmon resonance chip can be put into SPR samples
Pond, then molybdenum disulfide solution is passed through SPR sample cells, to carry out immersion treatment.After the completion of immersion, removed using deionized water
The molybdenum disulfide solution not adsorbed is removed, that is, removes extra molybdenum disulfide solution.
Preferably, the surface plasmon resonance chip is prepared as follows：
It is coated with golden film in glass or quartz surfaces.It is furthermore preferred that the golden film thickness is 20-60 nanometers, such as golden film
Thickness is 40 nanometers.
The present invention also provides a kind of mercury ion sensor preferred embodiments, use any one of them preparation method as above
It is made.
The present invention also provides a kind of applications of mercury ion sensor, by the mercury ion sensor application in detection mercury ion
Concentration.
Preferably, the solution containing mercury ion is added in the sample cell equipped with mercury ion sensor, and test surfaces
The plasmon resonance curve of spectrum determines the variation of resonance peak, and ion concentration of mercury is determined according to the variation.
For example, the sequence according to ion concentration of mercury from low to high, by the solution containing mercury ion be passed through successively equipped with mercury from
In the sample cell of sub- sensor, and impregnate 0.01-24 hours, such as 5 hours；To utilize mercury ion sensor test surface etc.
From the plasmon resonance curve of spectrum, the variation of resonance peak is determined, ion concentration of mercury is determined according to the variation.Particular by point
The variable quantity for analysing SPR spectroscopy resonance curve resonance angle, realizes that the mercury ion in the quantitative detection solution of ultralow detectable limit is dense
Degree.
Be exactly using molybdenum disulfide and mercury ion in the sensing process of the present invention with the principle compared with strong interaction, mercury from
Son is easily adsorbed on molybdenum disulfide surface, when in spr sensor chip surface solution there are when mercury ion, can and curing molybdenum materials
The sulphur atom of material combines, and SPR spectroscopy curve is made to move right, and realization quantitatively detects mercury ion.The mercury ion sensor of the present invention
With ultralow detectable limit, it is able to detect that ion concentration of mercury is 10-12M。
One specific example is as follows：
1) preparation of molybdenum disulfide nano material
Ammonium thiomolybdate powder is added in dimethyl formamide solution using chemical method, then uses reaction kettle 200
It is reacted 14 hours under degrees celsius, is evaporated to obtain molybdenum disulfide nano material powder after cleaning using ethyl alcohol, transmitted electron is aobvious
Micro mirror test chart is as shown in Figure 1.
2) assembling of the molybdenum disulfide nano material on spr sensor chip surface
Molybdenum disulfide powder prepared by chemical method is dissolved in ethanol solution, the curing of favorable dispersibility is obtained by ultrasound
Molybdenum solution, by concentration respectively 0.01,1, the molybdenum disulfide solution of 10mg/ml be passed through corresponding sample cell, molybdenum disulfide solution point
Not after SPR chip surfaces assemble 0.1,1,48 hour, unassembled molybdenum disulfide is flushed to using deionized water.
3) mercury ion of various concentration is detected
Respectively a concentration of 10-12-10-6The mercury ion solution of M each leads into sample cell according to low concentration to high concentration, point
Not Ce Shi SPR spectroscopy curve, the corresponding SPR spectroscopy curve of various concentration referring to Fig. 2, analysis SPR spectroscopy curve resonance angle to
The situation of change moved right realizes the Sensitive Detection of various concentration mercury ion solution referring to Fig. 3.
4) to the specific test of mercury ion sensing
Respectively other different metal ion (Fe are detected using the mercury ion sensor for being assembled with molybdenum disulfide2+,Fe3+,
Sn2+,Co2+,Pb2+,Zn2+,Cu2+,Mg2+,Ca2+), in the case of same concentrations, referring to Fig. 4, it is assembled with the mercury of molybdenum disulfide
Ion transducer illustrates in the present invention 10 times or more that mercury ion signal response variable quantity is the response of other metal ion signals
Mercury ion sensor have good specificity.
The present invention is led to by spr sensor chip surface-assembled molybdenum disulfide material, can sensitively detect mercury ion
The variation for crossing the formant of analysis SPR spectroscopy curve, quantitatively detects the concentration of mercury ion, and the lowest detection limit is 10-12M has
Very high sensing specificity.The result shows that the method can solve to reduce asking for mercury ion detecting limit difficulty at present really
Topic.The detection method is simple, economical, efficient, has preferable application prospect.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of mercury ion sensor, which is characterized in that include the following steps：
A, molybdenum disulfide nano material is dissolved in organic solvent first, obtains molybdenum disulfide solution, a concentration of 0.01-10mg/
ml；
B, surface plasmon resonance chip is immersed in the molybdenum disulfide solution, soaking time 0.01-48
Hour, the molybdenum disulfide not adsorbed then is removed, mercury ion sensor is finally obtained.
2. the preparation method of mercury ion sensor according to claim 1, which is characterized in that the organic solvent is second
Alcohol.
3. the preparation method of mercury ion sensor according to claim 1, which is characterized in that in the step B, using going
Ionized water removes the molybdenum disulfide not adsorbed.
4. the preparation method of mercury ion sensor according to claim 1, which is characterized in that the molybdenum disulfide nano material
Material is prepared as follows：
Ammonium thiomolybdate powder is added in dimethyl formamide solution, a period of time is then reacted under predetermined temperature,
It is finally cleaned and is evaporated to obtain molybdenum disulfide nano material powder.
5. the preparation method of mercury ion sensor according to claim 1, which is characterized in that in the step A, to two sulphur
Change molybdenum solution and carries out ultrasonic disperse, the molybdenum disulfide solution after being disperseed.
6. the preparation method of mercury ion sensor according to claim 1, which is characterized in that the surface phasmon is total
Vibration sensor chip is prepared as follows：
It is coated with golden film in glass or quartz surfaces.
7. the preparation method of mercury ion sensor according to claim 6, which is characterized in that the golden film thickness is 20-
60 nanometers.
8. a kind of mercury ion sensor, which is characterized in that be made of such as claim 1~7 any one of them preparation method.
9. a kind of application of mercury ion sensor as claimed in claim 8, which is characterized in that answer the mercury ion sensor
For detecting ion concentration of mercury.
10. the application of mercury ion sensor according to claim 9, which is characterized in that add the solution containing mercury ion
Enter into the sample cell equipped with mercury ion sensor, and the test surfaces plasmon resonance curve of spectrum, determines resonance peak
Variation determines ion concentration of mercury according to the variation.
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| CN112964676A (en) * | 2020-12-22 | 2021-06-15 | 燕山大学 | Surface plasmon resonance sensor chip and preparation method and application thereof |
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