CN109211863A - Utilize Eu2+The method of f-f Transition Spectra detection explosive TNP - Google Patents

Utilize Eu2+The method of f-f Transition Spectra detection explosive TNP Download PDF

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CN109211863A
CN109211863A CN201811258092.8A CN201811258092A CN109211863A CN 109211863 A CN109211863 A CN 109211863A CN 201811258092 A CN201811258092 A CN 201811258092A CN 109211863 A CN109211863 A CN 109211863A
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tnp
explosive
concentration
transition
nanoparticle
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CN109211863B (en
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华瑞年
张璇
刘力涛
那立艳
张伟
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Dalian Minzu University
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Dalian Nationalities University
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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
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
    • G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material

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Abstract

The present invention provides utilize Eu2+The method that f-f Transition Spectra detects explosive TNP, is with amido modified rare earth Eu2+Application of the lower conversion nano material of dopen Nano particle in explosive detection.Under 258nm ultraviolet excitation, Eu is utilized2+The resonance energy transfer that f-f transition fluorescence intensity and TNP at the 360nm generated in host material are formed at 360nm, to Eu2+The concentration of the measurement energy quantitative detection explosive TNP of fluorescence intensity at 360nm.Eu2+F-f Transition Spectra can show stable, good testing result in explosive TNP detection, can efficiently judge that the concentration of explosive, the detection method are simple, easy to spread real-time, quickly.

Description

Utilize Eu2+The method of f-f Transition Spectra detection explosive TNP
Technical field
It the present invention relates to the use of Eu2+F-f Transition Spectra detects explosive TNP.
Background technique
Trinitrophenol (TNP) is a kind of dangerous explosive, is adversely affected to environment, therefore for micro explosion The detection and analysis of object is increasingly important, currently, the method to explosive detection mainly has chromatography, ionic migration method, Raman light Spectrometry, biosensor technique method, wherein chromatography there are equipment costly and cumbersome, complicated for operation defect.Ionic migration method is deposited Larger in complicated for operation and error, detectable limit is low.The spectrum of Raman spectroscopy is weaker, is easy to be interfered by outside, detection knot Fruit is unstable.Biosensor technique method is interfered by outside larger, and error is higher.Therefore quick and easy, stable detection The method of explosive is increasingly by the concern of those skilled in the art.
Illuminant nanometer material is converted under rare earth refers to the process of that a high-energy photons split into multiple energy photons. In general, this process can by rare earth doped, using its level structure abundant realize efficient energy transmission with Conversion.Illuminant nanometer material is converted under rare earth to be widely used in biomarker field, but is led in explosive detection It is rarely reported in domain.
Summary of the invention
For the blank for making up the prior art, the present invention provides a kind of with amido modified rare earth Eu2+The lower conversion of doping is received Application of the rice material in explosive TNP detection.
The technical scheme is that under 258nm ultraviolet excitation, Eu2+At the 360nm generated in host material F-f transition fluorescence intensity combined with absorption of the TNP at 360nm, the resonance energy transfer of formation, and the concentration of TNP With Eu2+There are linear relationships for fluorescence intensity at 360nm, to Eu2+The measurement of fluorescence intensity at 360nm can be examined quantitatively Survey the concentration of explosive TNP.Wherein the host material is amido modified rare earth Eu2+Adulterate lower conversion nano material.Such as BaAlF5、SrAlF5、BaSiF6、 KMgF3、KZnF3、LiBaF3One of.
The detection method specifically: nanoparticle and PEI are dissolved in deionized water, magnetic agitation is uniformly mixed, and is used Ethyl alcohol and deionized water are centrifuged 3-4 times, obtain the nanoparticle for being connected with PEI, the nanoparticle for being connected with PEI is dissolved in deionization In water, after magnetic agitation 4 hours, the TNP of concentration to be measured is added, stirring carries out spectral measurement after ten minutes, to mixing liquid, The intensity of detection transmitting light, passes through TNP concentration and Eu under 258nm ultraviolet excitation2+F-f transition transmitting (360nm at) by force The linear relationship presented between degree carries out quantitative detection to explosive.Nanoparticle and PEI mass ratio are 1:10.
Wherein BaAlF5: Eu2+Nanoparticle f-f transition transmitting (6P7/2→8S7/2) it can detect nanogram rank TNP, Eu2+ F-f transition emissive porwer and TNP concentration between meet linear relationship y=108341.3c-1012.5, R2=0.997.Detection It is limited to 1ng/ml.
BaSiF6: Eu2+Nanoparticle f-f transition transmitting (6P7/2→8S7/2) it can detect nanogram rank TNP, Eu2+F- Meet linear relationship y=104623.4c-265.3, R between f transition emissive porwer and TNP concentration2=0.997.Detection is limited to 3ng/ml。
In above-mentioned linear relation, y indicates corresponding spectrum integral intensity, and c is corresponding object concentration to be detected. R2Generation The fitting accuracy of table linear relationship.
The utility model has the advantages that
The present invention provides with amido modified rare earth Eu2+The lower conversion nano material of dopen Nano particle is in explosive Application in detection.Utilize Eu2+F-f Transition Spectra can show stable, good detection knot in explosive TNP detection Fruit can efficiently judge that the concentration of explosive, the detection method are simple, easy to spread real-time, quickly.
Detailed description of the invention
Fig. 1 (a) is BaAlF5: Eu2+Nanoparticle (b) BaSiF6: Eu2+Nanoparticle scanning electron microscope (SEM) photograph.
Fig. 2 coats Eu before and after PEI2+The infrared spectrogram of dopen Nano particle, wherein before and after (a) is cladding PEI BaAlF5/BaSiF6: Eu2+The infrared spectrogram of nanoparticle.It (b) is BaAlF5/BaSiF6: Eu2+The transmitting light of nanoparticle The abosrption spectrogram of spectrum and TNP.
Fig. 3 coats Eu before and after PEI2+The XRD spectrum of dopen Nano particle, wherein BaAlF before and after (a) cladding PEI5: Eu2+ The XRD spectrum of nanoparticle.(b) BaSiF before and after cladding PEI6: Eu2+The XRD spectrum of nanoparticle.
After various concentration TNP is added in Fig. 4, PEI-BaAlF5: Eu2+Nanoparticle is corrected bent in the fluorescence intensity of 360nm Line.
After various concentration TNP is added in Fig. 5, PEI-BaSiF6: Eu2+Nanoparticle is corrected bent in the fluorescence intensity of 360nm Line.
Specific embodiment
The present invention is described in detail below by specific embodiment, but is not limited the scope of the invention.Unless otherwise specified, Experimental method of the present invention is conventional method, and experiment equipment used, material, reagent etc. can chemically company be purchased It buys.
Embodiment 1
BaAlF5: Eu2+The preparation of nanoparticle
1. weighing 2mmolAlCl3·6H2O、1.92mmol BaCl2·6H2O、0.08mol EuCl2With 10mL distilled water It being dissolved in 50mL beaker, rotor is added in beaker, beaker, which is put into stirring 20min on magnetic stirring apparatus, dissolves it sufficiently, Obtain mixed solution 1..
2. weighing 2mmol NH4HF2It is dissolved in 5mL distilled water, is slowly dropped into mixed solution 1. to sufficiently dissolve In, 20min is stirred, obtains mixed solution 2..
It is heated for 24 hours for 200 DEG C 3. mixed solution is transferred in 25mL reaction kettle 2..
4. after taking out reaction kettle, being cooled to after room temperature with revolving speed 5000rpm/min centrifugation 10 minutes, abandoning supernatant, sink Starch distillation washing 4 times.After drying, constituent analysis is carried out, has obtained pure phase BaAlF known to XRD spectrum Fig. 3 (a)5: Eu2 +Nanoparticle.
BaAlF5: Eu2+The preparation of@PEI nanoparticle
1. by 0.2g BaAlF5: Eu2+Nanoparticle and 2g PEI are added in 50ml beaker, at room temperature with 10mL distilled water Magnetic agitation 4h is dissolved.
2. being centrifuged repeatedly 3 times with distilled water.The modified PEI-BaAlF in surface is obtained after drying5: Eu2+Nanoparticle.
Embodiment 2
BaSiF6:Eu2+The preparation of nanoparticle
1. weighing 2gCTAB to be dissolved in the mixed solution of 50mL hexamethylene and 2mL n-butanol, magnetic force is stirred in 60 DEG C of water-baths After mixing 30min, solution becomes pale yellow transparent shape at this time, prepares two parts of same solution.
2. respectively by 1mLBaCl2The mixed solution and 1mLH of (1mol/L) and citric acid (CA)2SiF6(10%) and CA Mixed solution is added in the resulting two parts of solution of step 1, continues to stir 30min.
3. two parts of solution are mixed, after room temperature strong stirring 1h, it is transferred to 120 DEG C of heating 12h in 100mL reaction kettle.
4. after taking out reaction kettle, being cooled to after room temperature with revolving speed 9000rpm/min centrifugation 10 minutes, abandoning supernatant, sink Starch ethyl alcohol and distillation are washed 4 times.Constituent analysis is carried out after drying, obtains pure phase known to XRD spectrum Fig. 3 (b) BaSiF6:Eu2+Nanoparticle.
BaSiF6:Eu2+The preparation of@PEI nanoparticle
1. by 0.2g BaSiF6: Eu2+Nanoparticle and 2g PEI are added in 50ml beaker, at room temperature with 10mL distilled water Magnetic agitation 4h is dissolved.
2. being centrifuged repeatedly 3 times with distilled water.The modified PEI-BaSiF in surface is obtained after drying6: Eu2+Nanoparticle.
Such as Fig. 2 (b) it is found that BaAlF5/BaSiF6:Eu2+The emission peak of nanoparticle is overlapped with the absorption peak of TNP.Due to Amino is there are extra electronics pair, and there are electron holes for the phenyl ring in TNP, therefore amino and phenyl ring can connect together concurrently Raw resonance energy transfer.The relationship between the concentration of explosive and fluorescent concentration can be analyzed according to this, to reach The purpose of accurate detection explosive concentration.
Application examples 1
BaAlF5:Eu2+The method that nanoparticle is used to detect TNP
1. taking 5mgBaAlF5:Eu2+Conversion nanoparticles under@PEI are added in the bottle containing 4ml deionized water and stir Mix 4h.
2. the TNP (original solution concentration 400ng/ml) of concentration to be measured is added, carry out gradient experiment, be separately added into 10ul, 20ul, 30ul, 40ul, 50ul TNP carry out spectral measurement to it respectively after stirring 10min.
As shown in figure 4, the intensity of spectrum can be linear with the increase of TNP concentration when the TNP of various concentration is added Weaken.
Wherein BaAlF5: Eu2+Nanoparticle f-f transition transmitting (6P7/2→8S7/2) it can detect nanogram rank TNP, Eu2+ F-f transition emissive porwer and TNP concentration between meet linear relationship y=108341.3c-1012.5, R2=0.997；Linearly In relational expression, y indicates corresponding spectrum integral intensity, and c is corresponding object concentration to be detected.R2Represent the fitting of linear relationship Accuracy.From the experimental results, BaAlF after surface modification5:Eu2+Lower conversion nanoparticles are limited to 1ng/ to the detection of TNP ml。
Application examples 2
BaSiF6:Eu2+The method that nanoparticle is used to detect TNP
1. taking 5mgBaAlF5: Eu2+Conversion nanoparticles under@PEI are added in the bottle containing 4ml deionized water and stir Mix 4h.
2. the TNP (original solution concentration 400ng/ml) of concentration to be measured is added, carry out gradient experiment, be separately added into 30ul, 40ul, 50ul, 150ul TNP carry out spectral measurement to it respectively after stirring 10min.
As shown in figure 5, the intensity of spectrum can be linear with the increase of TNP concentration when the TNP of various concentration is added Weaken.BaSiF6: Eu2+Nanoparticle f-f transition transmitting (6P7/2→8S7/2) it can detect nanogram rank TNP, Eu2+F-f jump It moves and meets linear relationship y=104623.4c-265.3, R between emissive porwer and TNP concentration2=0.997.Linear relation In, y indicates corresponding spectrum integral intensity, and c is corresponding object concentration to be detected.R2Represent the fitting accuracy of linear relationship. From the experimental results, BaSiF after surface modification6: Eu2+Lower conversion nanoparticles are limited to 3ng/ml to the detection of TNP.
The preferable specific embodiment of the above, only the invention, but the protection scope of the invention is not It is confined to this, anyone skilled in the art is in the technical scope that the invention discloses, according to the present invention The technical solution of creation and its inventive concept are subject to equivalent substitution or change, should all cover the protection scope in the invention Within.

Claims (5)

1.Eu2+Application in detection explosive TNP, which is characterized in that under 258nm ultraviolet excitation, Eu2+In host material F-f transition fluorescence intensity at the 360nm of middle generation is combined with absorption of the TNP at 360nm, and the energy resonance of formation turns It moves, to Eu2+The concentration of the measurement energy quantitative detection explosive TNP of fluorescence intensity at 360nm.
2. application according to claim 1, which is characterized in that the host material is amido modified rare earth Eu2+Doping Lower conversion nano material.
3. application according to claim 1, which is characterized in that the host material is BaAlF5、SrAlF5、BaSiF6、 KMgF3、KZnF3、LiBaF3One of.
4. utilizing Eu in a kind of application as described in claim 12+The method for detecting explosive TNP, which is characterized in that by nanoparticle Son is dissolved in deionized water with PEI, and magnetic agitation is uniformly mixed, and is centrifuged 3-4 times with ethyl alcohol and deionized water, and acquisition is connected with PEI Nanoparticle, the nanoparticle for being connected with PEI is dissolved in deionized water, after magnetic agitation 4 hours, concentration to be measured is added TNP, stirring carry out spectral measurement after ten minutes, to mixing liquid, the intensity of detection transmitting light under 258nm ultraviolet excitation, Pass through TNP concentration and Eu2+The linear relationship presented between f-f transition emissive porwer at 360nm, quantifies explosive Detection.
5. according to the method described in claim 4, it is characterized in that, the host material is BaAlF5Or BaSiF6When:
BaAlF5: Eu2+The f-f transition of nanoparticle emits detectable nanogram rank TNP, Eu2+F-f transition emissive porwer with Meet linear relationship y=108341.3c-1012.5, R between TNP concentration2=0.997；
BaSiF6: Eu2+The f-f transition of nanoparticle emits detectable nanogram rank TNP, Eu2+F-f transition emissive porwer with Meet linear relationship y=104623.4c-265.3, R between TNP concentration2=0.997；
Wherein, y indicates corresponding spectrum integral intensity, and c is corresponding object concentration to be detected, R2The fitting for representing linear relationship is quasi- Exactness.
CN201811258092.8A 2018-10-26 2018-10-26 Using Eu2+Method for detecting explosive TNP (trinitrotoluene) by f-f transition spectrum Active CN109211863B (en)

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