CN105806821B - A kind of picric portable detector of detection - Google Patents
A kind of picric portable detector of detection Download PDFInfo
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- CN105806821B CN105806821B CN201610320846.2A CN201610320846A CN105806821B CN 105806821 B CN105806821 B CN 105806821B CN 201610320846 A CN201610320846 A CN 201610320846A CN 105806821 B CN105806821 B CN 105806821B
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- push rod
- grinding
- chamber
- pillar buoy
- picric
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- 238000001514 detection method Methods 0.000 title claims abstract description 26
- 238000000227 grinding Methods 0.000 claims abstract description 57
- 230000007246 mechanism Effects 0.000 claims abstract description 15
- 238000007789 sealing Methods 0.000 claims abstract description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 39
- 230000003287 optical effect Effects 0.000 claims description 31
- 239000002904 solvent Substances 0.000 claims description 15
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- KJUGUADJHNHALS-UHFFFAOYSA-N 1H-tetrazole Chemical compound C=1N=NNN=1 KJUGUADJHNHALS-UHFFFAOYSA-N 0.000 claims description 10
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000004140 cleaning Methods 0.000 claims description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 9
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 238000002189 fluorescence spectrum Methods 0.000 claims description 7
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 7
- JFDZBHWFFUWGJE-UHFFFAOYSA-N benzonitrile Chemical compound N#CC1=CC=CC=C1 JFDZBHWFFUWGJE-UHFFFAOYSA-N 0.000 claims description 6
- 239000011701 zinc Substances 0.000 claims description 6
- 150000008359 benzonitriles Chemical class 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 210000000476 body water Anatomy 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002253 acid Substances 0.000 abstract description 5
- 235000019658 bitter taste Nutrition 0.000 abstract description 5
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 10
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 125000004433 nitrogen atom Chemical group N* 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 150000003536 tetrazoles Chemical group 0.000 description 3
- DYSXLQBUUOPLBB-UHFFFAOYSA-N 2,3-dinitrotoluene Chemical compound CC1=CC=CC([N+]([O-])=O)=C1[N+]([O-])=O DYSXLQBUUOPLBB-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 238000012937 correction Methods 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 2
- 150000002825 nitriles Chemical class 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 2
- 239000004810 polytetrafluoroethylene Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229950002929 trinitrophenol Drugs 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 150000005184 1,3-dinitrobenzenes Chemical class 0.000 description 1
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 description 1
- AQNOYHFCRNPFGZ-UHFFFAOYSA-N 4-(4-cyanophenyl)sulfanylbenzonitrile Chemical compound C1=CC(C#N)=CC=C1SC1=CC=C(C#N)C=C1 AQNOYHFCRNPFGZ-UHFFFAOYSA-N 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000003670 easy-to-clean Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 231100000299 mutagenicity Toxicity 0.000 description 1
- 230000007886 mutagenicity Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000010363 phase shift Effects 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 230000005588 protonation Effects 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 238000011896 sensitive detection Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 125000003831 tetrazolyl group Chemical group 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 230000005945 translocation Effects 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D257/00—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms
- C07D257/02—Heterocyclic compounds containing rings having four nitrogen atoms as the only ring hetero atoms not condensed with other rings
- C07D257/04—Five-membered rings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1003—Carbocyclic compounds
- C09K2211/1007—Non-condensed systems
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1003—Carbocyclic compounds
- C09K2211/1014—Carbocyclic compounds bridged by heteroatoms, e.g. N, P, Si or B
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2211/00—Chemical nature of organic luminescent or tenebrescent compounds
- C09K2211/10—Non-macromolecular compounds
- C09K2211/1018—Heterocyclic compounds
- C09K2211/1025—Heterocyclic compounds characterised by ligands
- C09K2211/1074—Heterocyclic compounds characterised by ligands containing more than three nitrogen atoms as heteroatoms
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Molecular Biology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The present invention discloses a kind of picric portable detector of detection, pillar buoy including syringe-shaped, conical head and push rod, the conical head is equipped with the first switch of control conical head opening and closing, the push rod includes sequentially connected push rod cup, it push rod column and pleads, the push rod cup is slidably connected by sealing ring and pillar buoy inner wall, the side wall of pillar buoy is fixed with grinding mechanism, mechanism is ground to include running through the communicating pipe of pillar buoy side wall, the grinding chamber being connect with communicating pipe, it is equipped with the second switch of control communicating pipe opening and closing communicating pipe, grinding chamber includes pan feeding chamber, the funnel chamber that discharges and grinding chamber, grinding wheel is provided in grinding chamber, grinding wheel is sleeved in shaft, grinding wheel is fixedly connected with shaft, shaft and grinding cavity wall rotation connection.It is of the invention that a kind of picric portable detector of detection is provided, it can realize that the variation of fluorescence intensity before and after being adsorbed to picric acid carries out bitter taste acid molecule selective qualitative and quantitative detection, high sensitivity has good application prospect.
Description
Technical field
The present invention relates to field of environmental protection detection, especially with regard to a kind of picric portable detector of detection.
Background technology
2,4,6- trinitrophenols are a kind of nitro-aromatic compound, also referred to as picric acid, are often used to make strong
Explosive, while be also a kind of environmental contaminants.Therefore public safety problem and a kind of highly toxic environmental pollution are directed not only to
Object is present in air, seawater, soil and oil.Due to its toxicity, the presence of 2,4,6- trinitrophenols can be to human health
Greatly harm is generated, is caused serious injury especially for the circulatory system of people, liver, spleen and immune system.Also, 2,4,
6- trinitrophenols and its biodegradable product have mutagenicity and carcinogenicity, also have very big danger to aquatic organism and terrestrial
Evil.Many instrument analysis technology methods at present, including gas chromatography, Gc-mss method and surface-enhanced Raman
Spectra methods etc. can carry out 2,4,6- trinitrophenols highly sensitive detection, but be disadvantageous in that detection process
Huge instrument and equipment and complicated operating process are generally required, needs to take a substantial amount of time, it is quick to be not suitable for today's society
The demand of detection.In comparison, fluorescence chemical detection method is then a kind of more convenient, economic detection means.Therefore, it opens
It sends out one kind quickly, there is the fluorescence chemical sensor that unicity detects 2,4,6- trinitrophenols to be of great significance.
Invention content
In view of this, the present invention is in order to solve the above technical problems, provide a kind of picric portable detector of detection.
The purpose of the present invention is achieved through the following technical solutions：
A kind of picric portable detector of detection, pillar buoy, conical head and push rod including syringe-shaped, the taper
Head is equipped with the first switch of control conical head opening and closing, and the push rod includes sequentially connected push rod cup, push rod column and pleads, institute
It states push rod cup to be slidably connected by sealing ring and pillar buoy inner wall, the side wall of pillar buoy is fixed with grinding mechanism, grinding mechanism packet
The communicating pipe through pillar buoy side wall, the grinding chamber that connect with communicating pipe are included, is equipped with that communicating pipe is controlled to be opened and closed communicating pipe
Two switches, grinding chamber include pan feeding chamber, discharging funnel chamber and grinding chamber, are provided with grinding wheel in grinding chamber, grinding wheel is sleeved on shaft
On, grinding wheel is fixedly connected with shaft, and shaft and grinding cavity wall rotation connection, the end of shaft is fixedly connected with hand arm, hand
Arm is located at outside grinding chamber, and pan feeding cavity wall is equipped with opening, and opening is equipped with shutter door, and opening is other to be equipped with magnet one, in shutter door
Equipped with the magnet two with one mutual magnetic of magnet, discharging funnel chamber is located at by pan feeding chamber, pan feeding chamber, discharging funnel chamber and grinding chamber
It is interconnected；Contain acetonitrile solvent in the pillar buoy, the grinding mechanism has included chemical formula as (C14H8N8S)2The fluorescence of Zn
Sensor, wherein, C14H8N8S is two (4- (1H-TETRAZOLE -5- bases) phenyl) sulfane roots；The fluorescent optical sensor is monoclinic system,P21/mSpace group, cell parameter area=10.163 (3),b=9.353 (5),c=12.845 (3),α=γ=90 o,β=
103.673 (1) o, V=1220.97 (1)3, the pillar buoy is equipped with to clear up in pillar buoy and pushrod clip gap space
It is detained the cleaning mouth of foreign matter, cleaning mouth is equipped with internal thread, cleans and spiral cover is connected at mouth, and spiral cover is equipped with and the internal thread
The external screw thread matched, spiral cover are detachably connected with cleaning mouth.
The preparation method of the fluorescent optical sensor is, by organic compound 4, thio two benzonitriles of 4'-, sodium azide and chlorine
Change zinc to be dissolved in the mixed solvent of water and ethyl alcohol, wherein water and ethyl alcohol volume ratio are 1:1, it is stirred at room temperature to form mixed liquor
A obtains the fluorescent optical sensor after then the mixed liquor A is reacted 36 hours under hydrothermal conditions.
Preferably, the molar ratio of thio two benzonitriles of 4, the 4'-, sodium azide and zinc chloride is 2:6:1.
Preferably, the hydrothermal temperature is 140 DEG C.
Wherein, the thio two benzonitriles English of 4,4'- is 4,4'-thiodibenzonitrile, under hydrothermal conditions, is utilized
It can generate two (4- (1H-TETRAZOLE -5- bases) phenyl) sulfanes under the action of zinc ion and sodium azide, and two (4- (1H-TETRAZOLE -
5- yls) phenyl) sulfane protonation after a kind of complex can be formed with zinc ion in situ.And two (4- (1H-TETRAZOLE -5- bases) benzene
Base) tetrazole ring has abundant nitrogen-atoms in sulfane, is capable of providing lone pair electrons and 2, and 4,6- trinitrophenols pass through proton turn
Phase shift interaction.
The occupation mode of the picric portable detector of detection is, in use, by portable detector with taper
Head-up, push rod state directed downwardly is placed, and opens shutter door, and fluorescent optical sensor is placed in grinding chamber, fluorescent optical sensor by opening
Grinding chamber is reached by pan feeding chamber, hand armband is rotated and moves grinding wheel rotation, the grinding wheel of rotation grinds fluorescent optical sensor in powder
Shape, hereafter opens first switch, and will be equipped in pillar buoy the portable detector of acetonitrile solvent with taper upside down, push rod court
On mode close to acetonitrile solvent, acetonitrile solvent is sucked in pillar buoy, first switch is closed and simultaneously opens second switch, it is powdered
Fluorescent optical sensor enters in pillar buoy to be mixed with acetonitrile solvent, is hereafter closed second switch and is opened first switch, by pillar buoy
The interior portable detector equipped with acetonitrile solvent is in an inclined manner close to water body to be measured, when conical head stretches into the water body water surface to be measured
Behind lower section, push rod is pulled, by the water body sucking pillar buoy to be measured of part, hereafter rotates portable lead ion analyzer to taper
Head-up, push rod state directed downwardly, when portable lead ion analyzer be in taper head-up, push rod state directed downwardly when,
Fluorescence spectrum test is carried out to mixed liquor in pillar buoy, 2,4,6- trinitrophenol molecules are carried out using the variation of fluorescence intensity
Selective qualitative and quantitative detection.
The present invention is compared to the advantageous effect of the prior art：
The picric portable detector of detection of the present invention, toward grinding, mechanism is built into fluorescent optical sensor, and put into
Grind the fluorescent optical sensor grind into powder of mechanism, powdered fluorescent optical sensor is along entering in pillar buoy and second communicating pipe
Nitrile solvent mixes, and mixed liquor carries out fluorescence spectrum test with test substance can judge bitter taste acid content according to fluorescence intensity, side
Just it is practical, and fluorescent optical sensor is easily prepared, and reaction in-situ can occur in hydro-thermal, the fluorescence being synthesized passes
Sensor chemical stability is good.The fluorescent optical sensor of the present invention has good fluorescent characteristic, and being rich in tetrazolium ring structure has orphan
It to the nitrogen-atoms of electronics, is interacted by proton translocation, can realize the variation pair of fluorescence intensity before and after being adsorbed to picric acid
Bitter taste acid molecule carries out selective qualitative and quantitative detection, and high sensitivity has good application prospect.Pillar buoy is equipped with clear
Clean mouth, pillar buoy and the delay foreign matter in pushrod clip gap space can be cleared up by unscrewing the spiral cover of cleaning mouth, easy to clean, after being convenient for
Phase safeguards.
Description of the drawings
Using attached drawing, the invention will be further described, but the embodiment in attached drawing does not form any limit to the present invention
System.
Fig. 1 is the overall structure figure of the picric portable detector of detection of the present invention.
Fig. 2 is the fluorescent optical sensor chemical structural drawing of the present invention.
Fig. 3 is that the fluorescent optical sensor of the present invention adsorbs the fluorescence spectra of bitter taste acid molecule.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, the present invention is made below in conjunction with attached drawing and embodiment further detailed
Thin description.
Fig. 1-3 are please referred to, the embodiment of the present invention is as follows
A kind of picric portable detector of detection, pillar buoy 1, conical head 2 and push rod 3 including syringe-shaped, taper
First 2 are equipped with the first switches 4 of control conical head opening and closing, and push rod 3 includes sequentially connected push rod cup 5, push rod column 6 and pleads 7,
Push rod cup 5 is slidably connected by sealing ring 8 and 1 inner wall of pillar buoy, and the side wall of pillar buoy 1 is fixed with grinding mechanism, grinds mechanism
Including the communicating pipe 9 for running through 1 side wall of pillar buoy, the grinding chamber being connect with communicating pipe 9, communicating pipe 9 is equipped with control and opens communicating pipe 9
The second switch 10 closed, grinding chamber include pan feeding chamber 11, discharging funnel chamber 12 and grinding chamber 13, grinding wheel are provided in grinding chamber 13
14, grinding wheel 14 is sleeved in shaft 15, and grinding wheel 14 is fixedly connected with shaft 15, and shaft 14 is rotatablely connected with 13 wall of grinding chamber, is turned
The end of axis 15 is fixedly connected with hand arm 16, and hand arm 16 is located at outside grinding chamber 13, and 11 wall of pan feeding chamber is equipped with opening 17, opens
Mouth 17 is equipped with shutter door 18, and 17 side of opening is equipped with magnet 1, and shutter door 18 is equipped with the magnetic with one 19 mutual magnetic of magnet
Body 2 20, discharging funnel chamber 12 are located at by pan feeding chamber 11, and pan feeding chamber 11, discharging funnel chamber 12 and grinding chamber 13 are interconnected, column
Shape cylinder 1 is equipped with the cleaning mouth 21 for clearing up pillar buoy 1 with being detained foreign matter in 3 crack space of push rod, and cleaning mouth 21 is equipped with
Internal thread cleans and spiral cover 22 is connected at mouth 21, and spiral cover 22 is equipped with and the matched external screw thread of the internal thread, spiral cover 22 and cleaning
Mouth 21 is detachably connected；Contain acetonitrile solvent in pillar buoy 1, the grinding mechanism has included chemical formula as (C14H8N8S)2Zn's
Fluorescent optical sensor.
By thio two benzonitriles of 1mmol4,4'-, 3mmol sodium azide and 0.5mmol zinc chloride be dissolved in 10mL water and
In the mixed solution of 10mL ethyl alcohol, stirring at normal temperature 30 minutes is subsequently transferred in polytetrafluoroethylene (PTFE) autoclave, places it in
It is reacted in 140 DEG C of baking ovens 36 hours, is down to room temperature with 5 DEG C/h later and fluorescent optical sensor, yield 50.2% is obtained by filtration（It is based on
Zinc）.
Then the fluorescent optical sensor of gained is subjected to monocrystalline characterization.
The X ray diffracting data of the compound is visited on diffractometer in Bruker Smart Apex CCD faces, uses MoKαSpoke
(λ=0.71073) is penetrated, collected with ω scan modes and carries out Lp factor corrections, absorption correction uses SADABS programs.With
Then with difference Fourier method whole non-hydrogen atom coordinates are obtained, and obtain hydrogen atom with theoretical hydrogenation method in direct method solution structure
Position (C H 1.083), is modified structure with least square method.Evaluation work uses SHELXTL program bags in PC machine
It completes.Chemical structural drawing is as shown in Figure 1.
Parsing is it is found that the fluorescent optical sensor chemical formula is (C after tested14H8N8S)2Zn；Wherein, C14H8N8S is two (4-
(1H-TETRAZOLE -5- bases) phenyl) sulfane root, monoclinic system,P21/mSpace group, cell parameter area=10.163 (3),b=
9.353 (5),c=12.845 (3),α=γ=90 o,β=103.673 (1) o, V=1220.97 (1)3, Z=2.Its chemistry
Structure chart is as shown in Figure 1, wherein, 4,4'- thio two benzonitrile two (4- of in-situ preparation under the action of sodium azide and zinc ion
(1H-TETRAZOLE -5- bases) phenyl) sulfane, and two (4- (1H-TETRAZOLE -5- bases) phenyl) sulfanes have after protonating and zinc ion coordination,
The pattern and the N atoms on 4 two (4- (1H-TETRAZOLE -5- bases) phenyl) sulfanes on tetrazole ring that zinc ion takes 4 coordination, 4 face body
Coordination, and the tetrazole ring at two (4- (1H-TETRAZOLE -5- bases) phenyl) sulfane both ends also respectively with zinc ion coordination.
By in 0.001g embodiments 1 gained fluorescent optical sensor pulverize it is last be dispersed in 10mL acetonitrile solvents, so
2,4,6- trinitrophenols of addition various concentration carry out fluorescence spectrum test, excitation wavelength 338nm afterwards.Fluorescence spectra is such as
Shown in Fig. 2, from figure it will be seen that with 2, the concentration of 4,6- trinitrophenols increases to 10mM from 0, fluorescence intensity by
It gradually reduces, if moreover, addition is 2,4,6-trinitrotoluene, dinitrotoluene (DNT), 1,3- dinitrobenzenes, this kind of object of nitrobenzene
The fluorescent optical sensor fluorescence intensity of the present invention is not influenced if matter, substantially with a concentration of 0mM when it is similar, therefore fluorescence can be utilized
The variation of intensity carries out 2,4,6- trinitrophenols molecule selective qualitative and quantitative detection.
The picric portable detector of detection of the present invention, toward grinding, mechanism is built into fluorescent optical sensor, and put into
Grind the fluorescent optical sensor grind into powder of mechanism, powdered fluorescent optical sensor is along entering in pillar buoy and second communicating pipe
Nitrile solvent mixes, and mixed liquor carries out fluorescence spectrum test with test substance can judge bitter taste acid content according to fluorescence intensity, side
Just it is practical.
Finally it should be noted that above example illustrates technical scheme of the present invention rather than to the scope of the present invention
Limitation, although being explained in detail with reference to preferred embodiment to the present invention, it will be understood by those of ordinary skill in the art that,
Technical scheme of the present invention can be modified or replaced equivalently, without departing from the essence and model of technical solution of the present invention
It encloses.
Claims (4)
1. a kind of picric portable detector of detection, the pillar buoy including syringe-shaped（1）, conical head（2）And push rod（3）,
The conical head（2）It is equipped with the first switch of control conical head opening and closing（4）, the push rod（3）Including sequentially connected push rod
Head（5）, push rod column（6）With plead（7）, the push rod cup（5）Pass through sealing ring（8）With pillar buoy（1）Inner wall is slidably connected, column
Shape cylinder（1）Side wall be fixed with grinding mechanism, grinding mechanism is included through pillar buoy（1）The communicating pipe of side wall（9）With communicating pipe
（9）The grinding chamber of connection, communicating pipe（9）It is equipped with control communicating pipe（9）The second switch of opening and closing（10）, grinding chamber include pan feeding
Chamber（11）, discharging funnel chamber（12）And grinding chamber（13）, grinding chamber（13）Inside it is provided with grinding wheel（14）, grinding wheel（14）It is sleeved on and turns
Axis（15）On, grinding wheel（14）With shaft（15）It is fixedly connected, shaft（15）With grinding chamber（13）Wall is rotatablely connected, shaft（15）'s
End and hand arm（16）It is fixedly connected, hand arm（16）Positioned at grinding chamber（13）Outside, pan feeding chamber（11）Wall is equipped with opening
（17）, opening（17）It is equipped with shutter door（18）, opening（17）Side is equipped with magnet one（19）, shutter door（18）It is equipped with and magnet
One（19）The magnet two of mutual magnetic（20）, discharge funnel chamber（12）Positioned at pan feeding chamber（11）Side, pan feeding chamber（11）, go out funnel
Chamber（12）And grinding chamber（13）It is interconnected；The pillar buoy（1）Inside contain acetonitrile solvent, the grinding mechanism has included chemistry
Formula is (C14H8N8S)2The fluorescent optical sensor of Zn, wherein, C14H8N8S is (4- (1H-TETRAZOLE -5- bases) phenyl) sulfane root；It is described glimmering
Optical sensor is monoclinic system,P21/mSpace group, cell parameter area=10.163 (3),b=9.353 (5),c=12.845
(3),α=γ=90 o,β=103.673 (1) o, V=1220.97 (1)3；
It is characterized in that, the pillar buoy（1）It is equipped with to clear up pillar buoy（1）With push rod（3）It is detained in crack space different
The cleaning mouth of object（21）, clean mouth（21）Internal thread is equipped with, cleans mouth（21）Place's connection spiral cover（22）, spiral cover（22）It is equipped with
With the matched external screw thread of the internal thread, spiral cover（22）With cleaning mouth（21）It is detachably connected, the detection is picric portable
The occupation mode of formula detector is, in use, by portable detector with taper head-up, push rod state directed downwardly place, open
Shutter door is opened, fluorescent optical sensor is placed in grinding chamber by opening, fluorescent optical sensor reaches grinding chamber by pan feeding chamber, and rotation is hand
Armband moves grinding wheel rotation, and it is in powdered that the grinding wheel of rotation, which grinds fluorescent optical sensor, hereafter opens first switch, and will be portable
Detector by taper upside down, push rod upward in a manner of close to acetonitrile solvent, acetonitrile solvent is sucked in pillar buoy, closes first
It switchs and opens second switch, powdered fluorescent optical sensor enters in pillar buoy to be mixed with acetonitrile solvent, is hereafter closed second and is opened
It closes and opens first switch, the portable detector of acetonitrile solvent will be housed in an inclined manner close to water to be measured in pillar buoy
Body after conical head is stretched into below the water body water surface to be measured, pulls push rod, by the water body sucking pillar buoy to be measured of part, hereafter revolves
Turn portable detector to taper head-up, push rod state directed downwardly, when portable detector be in taper head-up, push rod court
Under state when, in pillar buoy mixed liquor carry out fluorescence spectrum test.
2. the picric portable detector of detection according to claim 1, which is characterized in that the fluorescent optical sensor
Method is, by organic compound 4, thio two benzonitriles of 4'-, sodium azide and zinc chloride are dissolved in water and the mixed solvent of ethyl alcohol is worked as
In, wherein water and ethyl alcohol volume ratio are 1:1, it is stirred at room temperature to form mixed liquor A, then by the mixed liquor A in hydro-thermal item
The fluorescent optical sensor is obtained after being reacted 36 hours under part.
3. the picric portable detector of detection according to claim 2, which is characterized in that 4, the 4'- thio two
The molar ratio of benzonitrile, sodium azide and zinc chloride is 2:6:1.
4. the picric portable detector of detection according to claim 2, it is characterised in that：The hydrothermal temperature is
140℃。
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| JP2013113953A (en) * | 2011-11-28 | 2013-06-10 | Ricoh Co Ltd | Optical sensor and image forming apparatus including the same |
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| AU2012201119A1 (en) * | 2004-06-07 | 2012-03-15 | The Charlotte-Mecklenburg Hospital Authority | Utilizing lipopolysaccharide in exhaled breath condensate to diagnose gram negative pneumonia |
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