CN109001169A - A kind of developing latent finger printss and chemical residual object detecting method based on up-conversion nanoparticles - Google Patents
A kind of developing latent finger printss and chemical residual object detecting method based on up-conversion nanoparticles Download PDFInfo
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- CN109001169A CN109001169A CN201810647184.9A CN201810647184A CN109001169A CN 109001169 A CN109001169 A CN 109001169A CN 201810647184 A CN201810647184 A CN 201810647184A CN 109001169 A CN109001169 A CN 109001169A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 52
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 31
- 239000000126 substance Substances 0.000 title claims abstract description 18
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 claims abstract description 28
- 229960002715 nicotine Drugs 0.000 claims abstract description 28
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 12
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 235000019504 cigarettes Nutrition 0.000 claims description 13
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 9
- 229910052740 iodine Inorganic materials 0.000 claims description 9
- 239000011630 iodine Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000004519 grease Substances 0.000 claims description 8
- 230000000391 smoking effect Effects 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 5
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 5
- 150000002910 rare earth metals Chemical class 0.000 claims description 5
- 238000004088 simulation Methods 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910009523 YCl3 Inorganic materials 0.000 claims description 4
- 239000005030 aluminium foil Substances 0.000 claims description 4
- 229910052796 boron Inorganic materials 0.000 claims description 4
- 238000011088 calibration curve Methods 0.000 claims description 4
- 238000005336 cracking Methods 0.000 claims description 4
- 238000004090 dissolution Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 229910052710 silicon Inorganic materials 0.000 claims description 4
- 239000010703 silicon Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- CKLHRQNQYIJFFX-UHFFFAOYSA-K ytterbium(III) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Yb+3] CKLHRQNQYIJFFX-UHFFFAOYSA-K 0.000 claims description 4
- PCMOZDDGXKIOLL-UHFFFAOYSA-K yttrium chloride Chemical compound [Cl-].[Cl-].[Cl-].[Y+3] PCMOZDDGXKIOLL-UHFFFAOYSA-K 0.000 claims description 4
- 239000012491 analyte Substances 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 238000004851 dishwashing Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 210000001061 forehead Anatomy 0.000 claims description 3
- 239000003446 ligand Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 238000000859 sublimation Methods 0.000 claims description 3
- 230000008022 sublimation Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 claims description 2
- 238000003776 cleavage reaction Methods 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000007017 scission Effects 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims 1
- GRONZTPUWOOUFQ-UHFFFAOYSA-M sodium;methanol;hydroxide Chemical compound [OH-].[Na+].OC GRONZTPUWOOUFQ-UHFFFAOYSA-M 0.000 claims 1
- 230000008859 change Effects 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 230000006872 improvement Effects 0.000 description 9
- 238000003384 imaging method Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000005284 excitation Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 238000012067 mathematical method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 244000061176 Nicotiana tabacum Species 0.000 description 1
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
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- 238000007796 conventional method Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- -1 disc Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 230000003862 health status Effects 0.000 description 1
- 230000036571 hydration Effects 0.000 description 1
- 238000006703 hydration reaction Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 210000001595 mastoid Anatomy 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
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- 235000009566 rice Nutrition 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
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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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- Health & Medical Sciences (AREA)
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- Analytical Chemistry (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Optics & Photonics (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
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- Measurement Of The Respiration, Hearing Ability, Form, And Blood Characteristics Of Living Organisms (AREA)
Abstract
The invention discloses a kind of developing latent finger printss based on up-conversion nanoparticles and chemical residual object detecting methods, the up-conversion nanoparticles NaYF including hexagonal structure4:Yb3+/Tm3+Preparation prepares latent fingerprint sample, the formation of complex, latent fingerprint shows, and the present invention uses up-conversion nanoparticles, interfere fingerprint small, faster, background interference is small for color speed, does not destroy the potential information of latent fingerprint, the DNA identification of latent fingerprint is not influenced, synthesis, detection process are without any side effects, and it is obvious that nicotine images change in fluorescence, high sensitivity, detection device is portable, and the used equipment of entire detection is all portable moveable, it is convenient for carrying, the scene of progress is detected on the spot.
Description
Technical field
The invention belongs to detection technique fields, and in particular to a kind of up-conversion nanoparticles are for showing latent fingerprint and chemistry
Remaining method.
Background technique
Fingerprint is the tangible evidence of a most useful type, in particular to the mastoid process decorative pattern of human hands skin surface,
It is typical inhereditary feature.Line as a kind of material evidence be known as " first of evidence " be throughout the world recognized by, be widely used in investigating and seizing
Case, certification criminal.How to be found on the miscellaneous object in scene of a crime, show and collect it, be the pass that fingerprint utilizes
Key problem.Up to the present, the detection method of fingerprint is varied, and various imaging techniques are constantly progressive.However, current
Most of detection methods can only accurately detect finger print information, and cannot detect the other information on fingerprint simultaneously, and this is logical
It is often the evidence of of great value crime.The specificity information of human body physical sign is usually contained in fingerprint, such as personal favourite hobby, body
Health status etc..And by these features, it can contribute to reduce the field of investigation, more accurate investigate.And instantiated
Nicotine can learn the tobacco smoking status of individual, have great meaning to locking suspect.
Rare earth up-conversion luminescence nanomaterial is a kind of rare earth doped element, issues visible light under near infrared light excitation
Fluorescent material.Optical stability is good, material non-toxic, for a long time the stable luminescence under strong light or exciting light irradiation, flicker free, no
Easy photodissociation and photobleaching, excitation light source are the near-infrared of 980nm, and high energy radiation is avoided to destroy fingerprint lines, and upper conversion is received
On rice ions binding to fingerprint imaging, background interference can reduce.NaYF4:Yb3+/Tm3+Nanoparticle has fluorescence in 450nm,
It can be used as and show light source and show latent fingerprint, material synthesis method is simple and to show process fast.
Summary of the invention
Aiming at the problems existing in the prior art, the purpose of the present invention is be based on NaYF4:Yb3+/Tm3+Upper conversion nano grain
The application of the developing latent finger printss and chemical residual analyte detection of son, NaYF4:Yb3+/Tm3+Nanoparticle good dispersion, background interference
It is small, fluorescence intensity is high, glass, silicon wafer, stainless steel, aluminium foil, disc and the potential blood fingerprint of ceramic tile surface can be shown.I2Steam is smoked
Under steaming, it may make with NaYF4:Yb3+/Tm3+Nanoparticle fluorescence be obviously reduced.Observing the same of clearly fingerprint lines
When, nicotine content detected also by calibration curve method.The present invention is achieved by the following technical solutions:
The invention discloses a kind of developing latent finger printss based on up-conversion nanoparticles and chemical residual object detecting method, packets
Include following steps:
The up-conversion nanoparticles NaYF of hexagonal structure4:Yb3+/Tm3+Preparation:
It is raw material using rare earth-iron-boron, oleic acid is ligand, and oleic acid or 1- octadecylene are mixed solvent, using classical height
Warm cleavage method prepares the rare earth upconversion nano particle of hexagonal structure；Six side UCNPs fluorescence properties are good；
It prepares latent fingerprint sample: with placing a finger on the cigarette lighted, finger gently being pressed in fingerprint carrier surface, table
Face can leave potential fingerprint trace, obtain the fingerprint sample containing different content nicotine；
The formation of complex: elemental iodine being placed in the same container where carrier, 30min is stood, so that fingerprint
Sample adequately distils, and can shorten sublimation time with heating；
Latent fingerprint shows: a small amount of up-conversion nanoparticles being taken to be covered on the surface of fingerprint sample, NaYF4:Yb3+/Tm3+On
The fluorescence of conversion nanoparticles is absorbed by complex, and in fingerprint ridge region, nicotine is more, and fluorescence is weaker, to reach
Show the purpose of nicotine to fluorescence, it is capable of taking pictures at this time to carry out leaving and taking finger print data.
As a further improvement, rare earth-iron-boron of the present invention is preferably YCl3, YbCl3, TmCl3Or its hydration
Object.
As a further improvement, the method specifically includes following steps:
1), the up-conversion nanoparticles NaYF of hexagonal structure4:Yb3+/Tm3+Preparation
Classical high temperature pyrolytic cracking preparation, YCl3, YbCl3, TmCl3It is added in there-necked flask, by 6mlOA, 15mlODE points
It is not added in there-necked flask, vacuumizes, lead to nitrogen temperature to 160 DEG C of dissolutions, be down to 18-25 DEG C, be added dropwise containing NH4F and
The CH of NaOH3OH solution, stirs evenly, and leads to nitrogen temperature to 310 DEG C of 1-2h, is cooled to room temperature, ethyl alcohol centrifuge separation is added to collect
Product, it is dry；
2) fingerprint residues, are detected
It is washed away with dish washing liquid and is remained on hand, smeared grease, light cigarette later, finger is placed in the top that cigarette goes out smog
Smoking state is simulated, then finger is gently pressed in fingerprint carrier surface, surface can leave potential fingerprint trace, obtain containing not
With the fingerprint sample of content nicotine；
3), complex is formed
By I2Simple substance is placed in reaction in closed container and elemental iodine is sufficiently reacted, and is put into fingerprint sample, reacts
30min, so that fingerprint sample adequately distils, which can shorten elemental iodine with the methods of heating and distil the reaction time；Reaction
30min guarantees reaction sufficiently, and in small closed container, a few minutes can see apparent reaction, and 30min is anti-in order to guarantee
That answers is complete；
4) residue, is detected
By ready-made up-conversion nanoparticles physical attachment in fingerprint sample, with the laser irradiation of 980nm, with intelligent hand
The tools such as machine are taken pictures, by the softwares such as matlab calculate, calculate shape, the profile of fingerprint, for the point on fingerprint come
The statistics for carrying out brightness calculates, and obtains an average value, can reduce random error, increases accuracy, distinguishes fingerprint and uses simultaneously
Its mathematical method calculates brightness, and the more of nicotine content in fingerprint are finally judged by calibration curve method according to the height of brightness
It is few, further judge the personal feature of fingerprint owner；It is low with the laser illumination energy of 980nm, fingerprint is not damaged, it is invisible
Light, background interference is small, is taken pictures with tools such as smart phones, and mobile phone is easy to use, and equipment is simply portable.
As a further improvement, smearing grease in step 2) of the present invention is to secrete grease by contact forehead
Mode has just washed clean finger and has been difficult to leave the trace of clear fingerprint, needed the grease of a little forehead that could make fingerprint more
Clearly, this step is the conventional method of latent fingerprint production.
As a further improvement, finger is placed in the top simulation that cigarette goes out smog in step 2) of the present invention
Smoking state 3 seconds to 2 minutes；Time of contact is longer, and flue gas is attached to more on fingerprint, and nicotine content is bigger, for bright
Degree variation influences also bigger, easier differentiation.
As a further improvement, finger is placed in the top simulation that cigarette goes out smog in step 2) of the present invention
Smoking state 10 seconds to 1 minute；There is no the brightness of nicotine most bright if it is full value, accomplishes that 30s or so is exactly probably 2/3
The brightness of left and right, it is very sensitive.Possible signal intensity is not obvious enough within former seconds, 10s or so it has been seen in that compare detail that
Change.
As a further improvement, in step 4) of the present invention, physical attachment be include being sprinkling upon above or with washing
Ear ball purging.
Methanol is removed as a further improvement, leading to nitrogen in step 1) of the present invention and being first warming up to 65-80 DEG C at a slow speed,
It is rapidly heated again after methanol eliminates to 310 DEG C, is usually first set to 80 DEG C, methanol is evaporated completely, then logical nitrogen temperature arrives
310 DEG C, mainly prevent reaction from influencing fastly on the upper conversion particles fluorescent effect for being finally synthesizing out very much.
As a further improvement, fingerprint carrier of the present invention is glass, silicon wafer, stainless steel, aluminium foil, disc or porcelain
Any one in brick.
The invention has the benefit that
1, the present invention uses up-conversion nanoparticles, small to fingerprint interference, and faster, background interference is small for color speed.
2, the potential information of latent fingerprint is not destroyed, does not influence the DNA identification of latent fingerprint.
3, synthesis, detection process are without any side effects.
4, nicotine imaging change in fluorescence is obvious, high sensitivity.Detection device is portable.The used equipment of entire detection is all
Be it is portable moveable, be convenient for carrying, the scene of progress is detected on the spot.
6, time of developing is shorter (30min), can directly be detected after ligand compound, it was therefore concluded that.
Detailed description of the invention
Fig. 1, NaYF4:Yb3+/Tm3+The transmission electron microscope picture of nanoparticle；
Fig. 2, NaYF4:Yb3+/Tm3+The fluorescence spectrum of nanoparticle；
Fig. 3, NaYF4:Yb3+/Tm3+Show latent fingerprint and the comparison diagram containing different nicotine residues.
Specific embodiment
The present invention is the NaYF of rare earth doped element T m4:Yb3+/Tm3+The application of up-conversion nanoparticles, NaYF4:Yb3+/
Tm3+Method for showing latent fingerprint and chemical residue, detailed process is as follows:
It prepares latent fingerprint sample: with placing a finger on the cigarette lighted, controlling time of contact, finger is gently pressed in glass
Any fingerprints carrier surface such as glass, silicon wafer, stainless steel, aluminium foil, disc, ceramic tile, surface can leave potential fingerprint trace, obtain
Fingerprint sample containing different content nicotine；The formation of complex: same container elemental iodine being placed in where carrier
In, 30min is stood, so that fingerprint sample adequately distils, sublimation time can be shortened with heating.Latent fingerprint shows: taking a small amount of
Up-conversion nanoparticles are covered on the surface of fingerprint sample, NaYF4:Yb3+/Tm3+The fluorescence of up-conversion nanoparticles is by coordinationization
It closes object to absorb, in fingerprint ridge region, nicotine is more, and fluorescence is weaker.To achieve the purpose that fluorescence shows nicotine, this
When, it is capable of taking pictures to carry out leaving and taking finger print data.
Fig. 1 is the electromicroscopic photograph hexagonal phase of the up-conversion nanoparticles of high temperature pyrolytic cracking preparation, form as can be seen；
The fluorescence spectrum of the up-conversion nanoparticles of Fig. 2 preparation；As seen from the figure: the up-conversion nanoparticles of preparation have relatively strong
Fluorescence, bands of a spectrum in visible-range only have a strong signal, bands of a spectrum are single, and miscellaneous peak is few, upper high conversion efficiency, equally
Signal is stronger under exciting light, and compound particle is high-quality, there is fluorescence in blue wavelength range, is that up-conversion nanoparticles fingerprint is residual
Excess detection provides possibility.
Fig. 3 is NaYF4:Yb3+/Tm3+Show latent fingerprint and the comparison diagram containing different nicotine residues, left figure is not have
Fingerprint existing for nicotine, right figure are the fingerprint containing nicotine, as seen from the figure: without fingerprint existing for nicotine
Sample, imaging is very limpid in sight, and the fingerprint sample containing nicotine, then brightness is very dark, and brightness change is very bright
It is aobvious, by quantifying the variation of this brightness, we may determine that the nicotine content contained in fingerprint number.
Technical solution of the present invention is further described below by specific embodiment:
Embodiment 1:
1), the up-conversion nanoparticles NaYF of hexagonal structure4:Yb3+/Tm3+Preparation
Classical high temperature pyrolytic cracking preparation, by the YCl of 1mmol3YbCl3TmCl3=79.5:20:0.5 is added to three mouthfuls
In bottle, 6mlOA, 15mlODE are added separately in there-necked flask, vacuumized, led to nitrogen temperature to 160 DEG C of dissolutions, be down to 18-25
DEG C, it is added dropwise containing NH4Methanol solution (the CH for the 10ml that F and NaOH are added to3OH), ultrasonic dissolution obtains solution 2, by solution 2
It is added dropwise in there-necked flask, 30min is mixed, lead to nitrogen temperature, here, 65-80 DEG C has methanol and evaporates,
It is enriched in surge flask, pours into discarded bottle after the completion of reaction, be then warming up to again to 310 DEG C of 1-2h, be cooled to room temperature, add
Product is collected in ethyl alcohol centrifuge separation, dry；
2) fingerprint residues, are detected
It is washed away with dish washing liquid and is remained on hand, smeared grease, light cigarette later, finger is placed in the top that cigarette goes out smog
Smoking state is simulated, then finger is gently pressed in fingerprint carrier surface, surface can leave potential fingerprint trace, obtain containing not
With the fingerprint sample of content nicotine；
3), complex is formed
By I2Simple substance is placed in reaction in closed container and elemental iodine is sufficiently reacted, and is put into fingerprint sample, reacts
30min, so that fingerprint sample adequately distils, which can shorten elemental iodine with the methods of heating and distil the reaction time；Reaction
30min guarantees reaction sufficiently, and in small closed container, a few minutes can see apparent reaction, and 30min is anti-in order to guarantee
That answers is complete；
4) residue, is detected
By ready-made up-conversion nanoparticles physical attachment in fingerprint sample, with the laser irradiation of 980nm, with intelligent hand
The tools such as machine are taken pictures, by the softwares such as matlab calculate, calculate shape, the profile of fingerprint, for the point on fingerprint come
The statistics for carrying out brightness calculates, and obtains an average value, can reduce random error, increases accuracy, distinguishes fingerprint and uses simultaneously
Its mathematical method calculates brightness, and the more of nicotine content in fingerprint are finally judged by calibration curve method according to the height of brightness
It is few, further judge the personal feature of fingerprint owner；It is low with the laser illumination energy of 980nm, fingerprint is not damaged, it is invisible
Light, background interference is small, is taken pictures with tools such as smart phones.
The above is not limitation of the present invention, it should be pointed out that: those skilled in the art are come
It says, under the premise of not departing from essential scope of the present invention, several variations, modifications, additions or substitutions can also be made, these improvement
It also should be regarded as protection scope of the present invention with retouching.
Claims (9)
1. a kind of developing latent finger printss and chemical residual object detecting method based on up-conversion nanoparticles, which is characterized in that including
Following steps:
The up-conversion nanoparticles NaYF of hexagonal structure4:Yb3+/Tm3+Preparation:
It is raw material using rare earth-iron-boron, oleic acid is ligand, and oleic acid or 1- octadecylene are mixed solvent, using classical high warm
Cleavage method prepares the rare earth upconversion nano particle of hexagonal structure；
It prepares latent fingerprint sample: with placing a finger on the cigarette lighted, finger gently being pressed in fingerprint carrier surface, surface meeting
Potential fingerprint trace is left, the fingerprint sample containing different content nicotine is obtained；
The formation of complex: elemental iodine being placed in the same container where carrier, 30min is stood, so that fingerprint sample
Adequately distillation can shorten sublimation time with heating；
Latent fingerprint shows: a small amount of up-conversion nanoparticles being taken to be covered on the surface of fingerprint sample, NaYF4:Yb3+/Tm3+Upper conversion
The fluorescence of nanoparticle is absorbed by complex, and in fingerprint ridge region, nicotine is more, and fluorescence is weaker, to reach glimmering
Light shows the purpose of nicotine, capable of taking pictures at this time to carry out leaving and taking finger print data.
2. the developing latent finger printss and chemical residual object detecting method according to claim 1 based on up-conversion nanoparticles,
It is characterized in that, the rare earth-iron-boron is preferably YCl3, YbCl3, TmCl3Or its hydrate.
3. the developing latent finger printss and chemical residual object detecting method according to claim 1 based on up-conversion nanoparticles,
It is characterized in that, specifically comprising the following steps:
1), the up-conversion nanoparticles NaYF of hexagonal structure4:Yb3+/Tm3+Preparation
Classical high temperature pyrolytic cracking preparation, YCl3, YbCl3, TmCl3It is added in there-necked flask, 6mlOA, 15mlODE is added respectively
Enter into there-necked flask, vacuumize, leads to nitrogen temperature to 160 DEG C of dissolutions, be down to 18-25 DEG C, be added dropwise containing NH4F's and NaOH
Methanol (CH3OH) solution stirs evenly, and leads to nitrogen temperature to 310 DEG C of 1-2h, is cooled to room temperature, ethyl alcohol centrifuge separation is added to collect
Product, it is dry；
2) fingerprint residues, are detected
It is washed away with dish washing liquid and is remained on hand, smeared grease, light cigarette later, finger is placed in the top simulation that cigarette goes out smog
Smoking state, then finger is gently pressed in fingerprint carrier surface, surface can leave potential fingerprint trace, obtain containing containing difference
Measure the fingerprint sample of nicotine；
3), complex is formed
By I2Simple substance is placed in reaction in closed container and elemental iodine is sufficiently reacted, and is put into fingerprint sample, reacts 30min, so that
Fingerprint sample adequately distils, which can shorten elemental iodine with the methods of heating and distil the reaction time；
4) residue, is detected
By ready-made up-conversion nanoparticles physical attachment in fingerprint sample, with the laser irradiation of 980nm, with smart phone etc.
Tool is taken pictures, and is calculated by softwares such as matlab, is calculated shape, the profile of fingerprint, carry out for the point on fingerprint
The statistics of brightness calculates, and obtains an average value, can reduce random error, increases accuracy, distinguishes fingerprint and is counted simultaneously with it
Method calculates brightness, finally according to the height of brightness judged by calibration curve method nicotine content in fingerprint number,
Further judge the personal feature of fingerprint owner.
4. the developing latent finger printss and chemical residual object detecting method according to claim 3 based on up-conversion nanoparticles,
It is characterized in that, smearing grease in the step 2) is in such a way that contact forehead secretes grease.
5. the developing latent finger printss and chemical residual object detecting method according to claim 3 based on up-conversion nanoparticles,
It is characterized in that, finger is placed in top simulation smoking state 30 seconds to 2 minutes that cigarette goes out smog in the step 2).
6. the developing latent finger printss and chemical residual object detecting method according to claim 3 based on up-conversion nanoparticles,
It is characterized in that, finger is placed in top simulation smoking state 10 seconds to 1 minute that cigarette goes out smog in the step 2).
7. the developing latent finger printss and chemical residual object detecting method according to claim 3 based on up-conversion nanoparticles,
It is characterized in that, in the step 4), physical attachment be include being sprinkling upon above or being purged with ear washing bulb.
8. the developing latent finger printss and chemical residual object detecting method according to claim 3 based on up-conversion nanoparticles,
It is characterized in that, leading to nitrogen in the step 1) is first warming up at a slow speed 65-80 DEG C except methanol, quickly risen again after methanol eliminates
Temperature is to 310 DEG C.
9. the developing latent finger printss and chemical residual analyte detection according to claim 1 or 2 or 3 based on up-conversion nanoparticles
Method, which is characterized in that the fingerprint carrier is any one in glass, silicon wafer, stainless steel, aluminium foil, disc or ceramic tile.
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