CN103525424A - CdTe quantum dots, preparation method therefor and applications in detection of trace explosives - Google Patents

CdTe quantum dots, preparation method therefor and applications in detection of trace explosives Download PDF

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CN103525424A
CN103525424A CN201310515815.9A CN201310515815A CN103525424A CN 103525424 A CN103525424 A CN 103525424A CN 201310515815 A CN201310515815 A CN 201310515815A CN 103525424 A CN103525424 A CN 103525424A
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quantum dot
dinitrotoluene
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dnt
cdte quantum
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CN103525424B (en
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匡芮
赵海丽
刘一石
朱晓丽
冯攸联
闫荣金
杨文科
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Shandong Jiaotong University
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Abstract

The invention discloses CdTe quantum dots, a preparation method therefor and applications in detection of trace explosives, and belongs to the analytical chemistry and nanotechnology fields. The CdTe quantum dots are prepared from cadmium chloride, trisodium citrate, sodium tellurite, hydrazine hydrate and methionine. The quantum dots can be applied in detection of dinitrotoluene explosive. The method has high sensitivity, and dinitrotoluene with a concentration of 1.5*10<-9> mol/L can be detected.

Description

A kind of CdTe quantum dot and preparation method thereof and the application that detects trace explosive
Technical field
The present invention relates to a kind of CdTe quantum dot and preparation method thereof and the application that detects trace explosive, belong to analytical chemistry, field of nanometer technology.
Background technology
Quantum dot is called again semiconductor nanocrystal, normally by II-VI family element and III-V group element, formed, as CdTe, CdSe, CdS etc., its physical behavior, as similar to atom in optical, electrical character, therefore, be described as " artificial atom ", its surface irregularity, diameter is between 1-10nm, and its size and dimension can be controlled by reaction times, temperature, part accurately.
Compare with traditional organic dye, quantum dot has unique luminescent properties, such as the adjustable fluorescent emission of size, and narrow and symmetrical utilizing emitted light spectrum width and continuous absorption spectrum, light stability is also fabulous.By regulating different sizes, also can obtain the quantum dot of different emission.Quantum dot has caused the extensive concern of every field with its incomparable optics and electric property advantage.Nowadays, the technology of preparing of quantum dot is very ripe, and in polychrome imaging, the drug screening of biological video picture and diagnosis, medical science, obtained major progress.In recent years, quantum dot was because its highly sensitive in quantitative analysis is subject to analytical chemistry field worker's close attention.
The detection technique of explosive substance can be for very challenging fields such as nonmetallic mine detection, anti-terrorism, environmental quality monitorings, and the detection technique of explosive substance can be divided into body Detection Techniques and microscratch amount detection technique.Health check-up survey technology is expensive, sensitivity is low, equipment volume is large, in application aspect, has limitation.Compare with health check-up survey technology, microscratch amount detection technique have multi-functional integrated, reliability is high, excellent performance, can produce in batches, make explosive detection device to realize that miniaturization, cost are low, precision advantages of higher.
Nitro-aromatic compound is a class explosive substance, and residual in environment constitutes a serious threat to the mankind and vegeto-animal existence.Therefore, to it, the detection in environment has been subject to people and has more and more paid close attention to.In recent years, detect nitryl aromatic molecule obtained very large results with sensor, quenching of fluorescence material is proved and can detects explosive compound.Well-known fluorescent material is as conjugated polymers, silicon-dioxide micro-capsule, fluorescence dye, zinc (salicylic alidehyde imine) and support (TMS) molecule, trimethyl silicon based ethynyl molecule, it can perception direction of passage key bonding in solution electron deficiency nitroaromatic analyte, compare with other method, the selectivity of fluorescent method is better, sensitivity is higher, signal and parameter various.
Application number is 201210391464.0 patent, a kind of recognition detection method of nitro arene explosive substance is disclosed, utilize six kinds of fluorescence sense films of 5-dimethylamino-1-naphthalene sulfonyl modification that different diamines are connecting arm, the sense film of the same unit and fluorescence unit connecting according to different connecting arms has different quenching effects to nitro-aromatic compound, obtain the explosive substances such as dinitrotoluene (DNT) in coordinate in different zones, and then can reach the object of identification.Application number is 201310042069.6 patent, discloses a kind of dinitrotoluene (DNT) method for quick, it is characterized in that, selects as required sensing chip substrate material; In the substrate after cleaning, make metal nano array structure, obtain sensing chip; After solution to be measured is combined on above-mentioned sensing chip, after its natural air drying, puts into Raman spectrum test set and carry out in the scope of 500-2000cm-1 the Raman spectrum spectrogram that Raman spectroscopy scans obtains solution to be measured; By 1352cm in spectrum software analysis solution Raman spectrum to be measured spectrogram -1the relative intensity of characteristic peak and the linear ratio relation of 2,4-dinitrotoluene (DNT) content, and then realize 2,4-dinitrotoluene (DNT) quantitatively and qualitative detection.
Above-mentioned document is not open using quantum dot as the technical characterictic that detects nitro-aromatic compound nano material, not open using quantum dot as the technology enlightenment that detects nitro-aromatic compound yet.
Summary of the invention
One of technical assignment of the present invention is in order to make up the deficiencies in the prior art, and a kind of CdTe quantum dot is provided, and this quantum dot has the advantages such as highly sensitive, fast response time.
Two of technical assignment of the present invention is to provide the preparation method of this quantum dot, and this preparation technology is simple, and raw materials cost is low, technology maturation is reliable.
Three of technical assignment of the present invention is to provide this quantum dot and is detecting trace 2, the application of 4-dinitrotoluene (DNT).
CdTe technology of quantum dots scheme of the present invention is as follows:
1. a CdTe quantum dot, this quantum dot is comprised of the raw material of following proportioning:
Figure BSA0000096767350000021
Described hydrazine hydrate, massfraction is 85%.
2. the CdTe quantum dot as described in 1, preparation method is as follows:
(1) CdCl of 0.35mmol 25H 2o is dissolved in 150mL deionized water, under agitation, adds the trisodium citrate (Na of 0.4～0.5mmol 3c 6h 5o 72H 2o), the sodium tellurite (Na of 0.07～0.08mmol 2teO 3) and 0.4～0.45mmol hydrazine hydrate (N 2h 4h 2o), stirring at room 10min, then add 0.4～0.45mmol methionine(Met), and mixed solution is transferred in microwave reaction instrument, controlling temperature of reaction is 90～95 ℃, and power is 350-400W, and reaction times 5～10min makes CdTe quantum dot;
(2) (1) is made to CdTe quantum dot cool to room temperature, add acetone precipitation solution 10min, centrifugation obtains CdTe quantum dot powder.
3. the CdTe quantum dot as described in 1 and 2, for detection of trace 2,4-dinitrotoluene (DNT), step is as follows:
(1) in the water that is 1:1～2 in volume ratio and acetonitrile, dissolve 2,4-dinitrotoluene (DNT), make 1.5 * i0 -9mol/L～4.5 * 10 -72 of mol/L, 4-dinitrotoluene (DNT) standardized solution; CdTe quantum dot is dissolved in phosphate buffered saline buffer, makes the CdTe quantum dot solution of 0.025mg/mL;
(2) get 2 of 1mL CdTe quantum dot solution and 20uL, the standardized solution of 4-dinitrotoluene (DNT) is in 10mL colorimetric cylinder, with deionized water, be settled to 10mL, shaken up, static to 5min, this appropriate solution is transferred in quartz colorimetric utensil, use 410nm as excitation wavelength, record the funtcional relationship between the concentration of standard solution of fluorescent emission intensity and oil of mirbane, drawing standard curve;
(3) accurately take 5.000g sample, add water and the acetonitrile that 20mL, volume ratio are 1:1 to extract solution, then add 0.10g disodium ethylene diamine tetraacetate, ultrasonic 30min, room temperature is centrifugal, extracts upper strata liquid, and residue extracts once with extracting solution again, merge extracted twice liquid, filter, filtrate is revolved and steamed to dry, be settled to 1.00mL, make the sample solution of 2,4-dinitrotoluene (DNT);
(4) get 1mL CdTe quantum dot solution and 20uL2, the sample solution of 4-dinitrotoluene (DNT), is settled to 10mL with deionized water, shaken up, static to 5min, this appropriate solution is transferred in quartz colorimetric utensil, with 410nm, as excitation wavelength, record fluorescent emission intensity;
According to typical curve, calculate in sample solution 2, the concentration C of 4-dinitrotoluene (DNT), calculate recovery rate.
CdTe quantum dot as mentioned above, it is of a size of 4-6nm, and excitation wavelength is 410nm.
Described 2,4-dinitrotoluene (DNT), to CdTe quantum dot, has fluorescent quenching effect; The concentration of 2,4-dinitrotoluene (DNT) is 1.5 * 10 -9mol/L～4.5 * 10 -7within the scope of mol/L and the available the Representation Equation of relation of the fluorescence intensity of system be:
I。/ I=1.4671C 2,4-dinitrotoluene (DNT)+ 0.9740
This equation linearly dependent coefficient R 2be 0.997, the method detects and is limited to 1.5 * 10 -9mol/L.This shows, the method provides good accuracy and sensitivity to detecting 2,4-dinitrotoluene (DNT), can be used for 2 within the scope of finite concentration, the quantitative assay of 4-dinitrotoluene (DNT).
This preparation method and the outstanding feature of detection 2,4-dinitrotoluene (DNT) are:
1. the preparation of this CdTe quantum dot, owing to having used bistable agent methionine(Met) and trisodium citrate, the thiomethyl (CH of methionine(Met) 3s-), the carboxyl of amino, carboxyl and trisodium citrate can with quantum dot surface bonding, by sterically hindered and static steric hindrance, improved the dispersiveness of quantum dot, meanwhile, high price small molecules trisodium citrate can also be taken on pH buffer composition, can improve purity and the output of quantum dot.
2. this CdTe quantum-dot structure is stable, quantum point grain diameter homogeneous, and room temperature lucifuge above fluorescent stability placement half a year is good.
3. the preparation of this CdTe quantum dot, whole reaction process is carried out under atmospheric condition, and without logical nitrogen protection, technique is simple, easy to operate, and raw materials cost is low.
4. this quantum dot detects the method for 2,4-dinitrotoluene (DNT), and sample preparation is simple, easy, quick to the detection of 2,4-dinitrotoluene (DNT).The method can detect and be low to moderate 1.5 * 10 -92 of mol/L, 4-dinitrotoluene (DNT), compares with traditional method, and the method has higher sensitivity.
5. above preparation and application desired raw material all can be bought from local chemical reagents corporation.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but protection scope of the present invention is not only confined to embodiment, and the change that this field professional does technical solution of the present invention, all should belong in protection scope of the present invention.
Embodiment 1: a kind of CdTe quantum dot, and its preparation method comprises the following steps:
(1) CdCl of 0.35mmol 25H 2o is dissolved in 150mL deionized water, under agitation, adds the trisodium citrate (Na of 0.4mmol 3c 6h 5o 72H 2o), the sodium tellurite (Na of 0.07mmol 2teO 3) and 0.4mmol hydrazine hydrate (N 2h 4h 2o), stirring at room 5min, then add 0.4mmol methionine(Met), and mixed solution is transferred in microwave reaction instrument, controlling temperature of reaction is 90 ℃, and microwave power is 400W, and reaction times 10min makes CdTe quantum dot;
(2) (1) is made to CdTe quantum dot cool to room temperature, add acetone precipitation solution 10min, obtain CdTe quantum dot powder.
This CdTe quantum dot is of a size of 4nm.Under 4 ℃ of conditions, more than preserving half a year, fluorescence intensity weakens and is no more than 4%.
Embodiment 2: a kind of CdTe quantum dot, and its preparation method comprises the following steps:
(1) CdCl of 0.35mmol 25H 2o is dissolved in 150mL deionized water, under agitation, adds the trisodium citrate (Na of 0.5mmol 3c 6h 5o 72H 2o), the sodium tellurite (Na of 0.08mmol 2teO 3) and 0.45mmol hydrazine hydrate (N 2h 4h 2o), stirring at room 10min, then add 0.45mmol methionine(Met), and mixed solution is transferred in microwave reaction instrument, controlling temperature of reaction is 95 ℃, and power is 350W, and reaction times 15min makes CdTe quantum dot;
(2) (1) is made to CdTe quantum dot cool to room temperature, add acetone precipitation solution 10min, obtain CdTe quantum dot powder.
This CdTe quantum dot is of a size of 6nm.
Embodiment 3: a kind of CdTe quantum dot, and its preparation method comprises the following steps:
(1) CdCl of 0.35mmol 25H 2o is dissolved in 150mL deionized water, under agitation, adds the trisodium citrate (Na of 0.45mmol 3c 6h 5o 72H 2o), the sodium tellurite (Na of 0.075mmol 2teO 3) and 0.43mmol hydrazine hydrate (N 2h 4h 2o), stirring at room 7min, then add 0.43mmol methionine(Met), and mixed solution is transferred in microwave reaction instrument, controlling temperature of reaction is 93 ℃, and power is 370W, and reaction times 12min makes CdTe quantum dot;
(2) (1) is made to CdTe quantum dot cool to room temperature, add acetone precipitation solution 10min, obtain CdTe quantum dot powder.
This CdTe quantum dot is of a size of 5nm.
Embodiment 4: draw the typical curve that detects 2,4-dinitrotoluene (DNT), step is as follows:
(1) in the water that is 1:1 in volume ratio and acetonitrile, dissolve 2,4-dinitrotoluene (DNT), make 1.5 * 10 -9mol/L～4.5 * 10 -72 of mol/L, 4-dinitrotoluene (DNT) standardized solution; The CdTe quantum dot that embodiment 1 or embodiment 2 or embodiment 3 are made is dissolved in phosphate buffered saline buffer, makes the CdTe quantum dot solution of 0.025mg/mL;
(2) get 2 of different concns, 4-dinitrotoluene (DNT) solution joins respectively in quantum dot solution, carries out fluoroscopic examination;
(3) get 2 of 1mL CdTe quantum dot solution and 20uL, the standardized solution of 4-dinitrotoluene (DNT), in 10mL colorimetric cylinder, is settled to 10mL with deionized water, is shaken up, static to 5min, this appropriate solution is transferred in quartz colorimetric utensil, with 410nm, as excitation wavelength, excites and launch slit to be respectively 5nm, record the fluorescent emission intensity and 2 at 550nm place, funtcional relationship between 4-dinitrotoluene (DNT) concentration, draws the typical curve of concentration and its fluorescence intensity of 2,4-dinitrotoluene (DNT);
2,4-dinitrotoluene (DNT), to CdTe quantum dot, has fluorescent quenching effect, and the concentration of its fluorescence intensity of the quantum dot that embodiment 1 makes and 2,4-dinitrotoluene (DNT) is 1.5 * 10 -9mol/L～4.5 * 10 -7within the scope of mol/L, with equation, can be expressed as:
I。/ I=1.4671C 2,4-dinitrotoluene (DNT)+ 0.9740
This equation linearly dependent coefficient R 2be 0.997, the method detects and is limited to 1.5 * 10 -9mol/L.
Embodiment 5:2, the detection of 4-dinitrotoluene (DNT)
(1) soil for sample detection is taken at 2,4-dinitrotoluene (DNT) IA, accurately takes 5.000g soil, add water and the acetonitrile that 20mL, volume ratio are 1:1 to extract solution, then add 0.10g disodium ethylene diamine tetraacetate, ultrasonic 30min, room temperature is centrifugal, extracts upper strata liquid, and residue extracts once with extracting solution again, merge extracted twice liquid, filter, filtrate is revolved and steamed to dry, be settled to 1.00mL, make the sample solution of 2,4-dinitrotoluene (DNT).
(2) get that CdTe quantum dot solution that 1mL embodiment 4 (1) makes and embodiment 5 (1) make 2, the sample solution 20uL of 4-dinitrotoluene (DNT), with deionized water, be settled to 10mL, shaken up, static to 5min, this appropriate solution is transferred in quartz colorimetric utensil, with 410nm, as excitation wavelength, records fluorescent emission intensity.According to typical curve, calculate the concentration C of 2,4-dinitrotoluene (DNT), calculate recovery rate.
The CdTe quantum dot solution that adopts embodiment 1 to make, result is as shown in table 1.
Figure BSA0000096767350000051

Claims (5)

1. a CdTe quantum dot, is characterized in that, this quantum dot is comprised of the raw material of following proportioning:
Figure FSA0000096767340000011
Described hydrazine hydrate, massfraction is 85%.
2. CdTe quantum dot as claimed in claim 1, is characterized in that, its preparation method is as follows:
(1) by the CdCl of 0.35mmol 22.5H 2o is dissolved in 150mL deionized water, under agitation, adds the trisodium citrate (Na of 0.4～0.5mmol 3c 6h 5o 72H 2o), the sodium tellurite (Na of 0.07～0.08mmol 2teO 3), 0.4～0.45mmol massfraction hydrazine hydrate (N that is 85% 2h 4h 2o), stirring at room 10min, then add 0.4～0.45mmol methionine(Met), and mixed solution is transferred in microwave reaction instrument, controlling temperature of reaction is 90～95 ℃, and power is 350-400W, and reaction times 5～10min makes CdTe quantum dot;
(2) (1) is made to CdTe quantum dot cool to room temperature, add acetone precipitation solution 10min, obtain CdTe quantum dot powder.
3. CdTe quantum dot as claimed in claim 1, is characterized in that, CdTe quantum dot is for detection of 2,4-dinitrotoluene (DNT), and step is as follows:
(1) in the water that is 1:1～2 in volume ratio and acetonitrile, dissolve 2,4-dinitrotoluene (DNT), make 1.5 * 10 -9mol/L～4.5 * 10 -72 of mol/L, 4-dinitrotoluene (DNT) standardized solution; CdTe quantum dot is dissolved in phosphate buffered saline buffer, makes the CdTe quantum dot solution of 0.025mg/mL;
(2) get 2 of 1mL CdTe quantum dot solution and 20uL, the standardized solution of 4-dinitrotoluene (DNT), with deionized water, be settled to 10mL, shaken up, after static 5min, this appropriate solution is transferred in quartz colorimetric utensil, with 410nm as excitation wavelength, record the funtcional relationship between fluorescent emission intensity and 2,4-dinitrotoluene (DNT) concentration, drawing standard curve;
(3) accurately take 5.000g sample, add water and the acetonitrile that 20mL, volume ratio are 1:1 to extract solution, then add 0.10g disodium ethylene diamine tetraacetate, ultrasonic 30min, room temperature is centrifugal, extracts upper strata liquid, and residue extracts once with extracting solution again, merge extracted twice liquid, filter, filtrate is revolved and steamed to dry, be settled to 1.00mL, make the sample solution of 2,4-dinitrotoluene (DNT);
(4) get the 20uL2 that 1mL CdTe quantum dot solution that (1) make and (3) make, the sample solution of 4-dinitrotoluene (DNT), with deionized water, be settled to 10mL, shaken up, static to 5min, this appropriate solution is transferred in quartz colorimetric utensil, with 410nm, as excitation wavelength, records fluorescent emission intensity; According to typical curve, calculate the concentration C of 2,4-dinitrotoluene (DNT), calculate recovery rate.
4. the quantum dot of CdTe as claimed in claim 1, is characterized in that, described CdTe quantum dot is of a size of 4-6nm.
5. the quantum dot of CdTe as claimed in claim 1, is characterized in that, described CdTe quantum dot is limited to 1.5 * 10 to detecting of 2,4-dinitrotoluene (DNT) -9mol/L.
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