CN109001260A - A kind of detection method of nitro arene explosive substance - Google Patents
A kind of detection method of nitro arene explosive substance Download PDFInfo
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- CN109001260A CN109001260A CN201710421526.0A CN201710421526A CN109001260A CN 109001260 A CN109001260 A CN 109001260A CN 201710421526 A CN201710421526 A CN 201710421526A CN 109001260 A CN109001260 A CN 109001260A
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/041—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body
Abstract
The present invention relates to the sensing detection methods of a kind of pair of nitro arene explosive substance.For the compound film gas transducer that this method uses molecular engram polymeric membrane and semiconductor material to modify for detection device, characteristic is there is the trace hole for capableing of selective absorption nitro arene explosive substance molecule in its surface layer film.When nitro arene explosive substance molecule occupies trace hole, it will limit oxygen molecule and reach bottom film, weaken response intensity.This method is exactly can generate the oxygen molecule of high-responsivity with semiconductor material as the practical object with sensor response, sensor is related with the quantity that trace hole is occupied to the size of oxygen response numerical value, i.e., positive correlation is presented with the concentration of nitro arene explosive substance in environment.Detection method principle according to the present invention is simple, is easily achieved and is widely applied, it can be achieved that quick to nitro arene explosive substance, sensitive, accurate detection, can be expected to be employed flexibly for the quick detection of various public place blended explosive materials.
Description
Technical field
Invention is related to live quick, sensitive, the accurate detection method of a kind of pair of trace nitro arene explosive substance.The party
Method uses molecular engram to polymerize film modified semiconductors coupling film sensors for detection device, and the compound film bottom of the sensor is
N-type semiconductor (stannic oxide, di-iron trioxide etc.) film, surface layer are using resorcinol as function monomer, with three nitre of triamido
Base benzene is pseudo- template molecule, the molecular engram polymeric membrane that electropolymerization is formed.The detection method with semiconductor material at high temperature with
Oxygen reaction in air changes into basic testing principle to occur resistance value, is aided with molecular imprinting technology, so that the party
Method can have specific recognition capability to nitro arene explosive substance.
Background technique
Stride forward the new century, human civilization has a higher development, but terrorist activity there is no the arrival with the new millennium and
It disappears, instead more frequently.In terrorist activity, explosion is still the major way that terrorist uses, and terrorist utilizes
Various latent explosives are extorted under false pretense, are hijacked a plane, the terrified tragic event such as manufacture fatal crass, train explosion.In order to avoid these
The generation of tragedy event and guarantee people life property safety, the public places such as airport, harbour, railway station must be able to effectively look into
Latent explosive in luggage and package out.Nitro arene explosive substance such as 2,4,6- trinitrotoluene (TNT) is because of its prestige of exploding
Power is greatly and cheap, is often used by terrorist, and most of explosives all contain nitro-aromatic compound.Currently,
The detection of trace nitro arene explosive substance can pass through electrochemical method, ion mobility spectrometry, bio-sensing method and optics
Method etc. carry out, but its there are detection sensitivities it is low, equipment manufacturing cost is expensive the deficiencies of.Therefore, exploitation has fast response time, spirit
Sensitivity is high, detection range is wide, good, low in energy consumption, the low-cost explosives detection methods of recognition performance are particularly necessary.
Semiconductor gas sensor is the detecting element being made by Metal oxide semiconductor gas-sensitiveness material, from come out with
Come, with its simple, low in cost, fast response time of production, long service life and to imflammable gas and certain toxic gases
The advantages that sensitivity with higher and be used widely, become that yield in the world is maximum, most widely used sensor.
Trace detection technology based on resistor-type semiconductor gas sensor is fast-developing, is the trace detection of nitro arene explosive substance
Provide new idea and method.But using single metal oxide as the semiconductor gas sensor of gas sensitive for
The responsiveness of nitro-aromatic compound is low and poor selectivity, and it is impossible to meet trace nitro-aromatic classes under actual environment to explode
The detection of object.
Molecular imprinting technology can be artificial synthesized to the selective molecularly imprinted polymer of template molecule (MIPs).Due to
MIPs and template molecule have the relationship of " lock-key ", have highly selective and high-intensitive (organic solvent-resistant, acid and alkali-resistance, i.e. resistance to
Heat) the advantages of.It due to its enrichment to trace materials, is rapidly developed in recent years, is widely used to various fields,
Brilliant performance is especially shown in the separation of substance, enrichment, purifying and sensor field.The basic principle of molecular engram be
In decentralized medium (usually weakly polar organic solvent) appropriate, template molecule and function monomer rely on mutual covalent bond
Active force progress is pre-assembled, or relies on mutual noncovalent interaction power (hydrogen bond, ion exchange, electrostatic attraction, Van der Waals
Power, hydrophobic effect, metal-chelating and space steric effect etc.) self assembly is carried out, form stable reversible compound;Crosslinking is added
After agent, under initiator initiation, it polymerize through the effects of light, heat or electric field, being formed has rigidity and flexible porous three
Stereo function polymeric material is tieed up, template-monomer compound is fixed in the polymer.Finally by removing template molecule, thus
Acquisition has the function of the three-dimensional cavity complementary with the size of template molecule, shape and functional group and as derived from function monomer
Residue is the MIPs of binding site.In medium appropriate, when this molecularly imprinted polymer encounters template molecule or template point again
When the analogue of son, it will occur the recognition reaction of specificity.
Detection method of the present invention combines molecular imprinting technology and semiconductor gas sensor realize for
The detection of nitro arene explosive substance.This method will polymerize film modified composite membrane semiconductor gas sensor using molecular engram
For detection device, the surface layer of related compound film sensors is using resorcinol as function monomer, with photoacoustic spectroscopy
For the molecular engram polymeric membrane that pseudo- template molecule, electropolymerization are formed, the characteristic of the polymeric membrane is to exist quick-fried with nitro-aromatic class
The memory hole that fried object matches, the memory hole can be by hydrogen bond action, electrostatic attractions with the suction of pi-pi accumulation selective action
Attached nitro arene explosive substance, including triamido trinitro- (TATB), 2,4,6-trinitrotoluene (TNT), 2,4- dinitro first
Benzene, para-nitrotoluene and trinitrophenol (TNP), and polymeric membrane of such explosive molecule by surface layer is hindered, and in air
The small oxygen of molecular structure can directly reach the bottom of electrode by memory hole;The sensor bottom is n-type semiconductor (dioxy
Change tin, di-iron trioxide etc.) film, for reacting with the oxygen penetrated from surface layer film, in no nitro arene explosive substance
In the presence of, a large amount of oxygen molecule can penetrate surface layer film, and aoxidize at 200 ~ 400 DEG C with n-type semiconductor metal
Object surface contacts and fixes the electronics in semiconductor near surface conduction band, so that the resistance of sensor entirety increased dramatically;When the biography
When sensor is exposed in environment existing for nitro arene explosive substance, nitro arene explosive substance molecule can occupy the print of surface layer film
Mark hole, so that oxygen molecule is difficult to reach underlying n-type semiconductive thin film by surface layer film and generates reaction, semiconductor surface
Fixed major part electronics comes back in conduction band, so that sensor overall electrical resistance reduces.The size of resistance reduction numerical value
It is related with the quantity in occupied trace hole, i.e., positive correlation is presented with the concentration of nitro arene explosive substance in environment.It should
Detection method be exactly by this principle detected indirectly, using can with semiconductor material generate high-responsivity oxygen molecule as
Reality reacts object with sensor, according to sensor before and after the environment being exposed to containing nitro arene explosive substance for oxygen
The knots modification of response intensity to reflect indirectly the concentration of nitro arene explosive substance.
Summary of the invention
The object of the present invention is to provide a kind of detection methods of nitro arene explosive substance.
A kind of detection method of nitro arene explosive substance provided by the invention, comprising the following steps:
(1) metal-oxide film is formed on interdigital electrode surface using the method for sputtering, obtains semiconductor gas sensor;
(2) one layer of molecular imprinted polymer membrane is modified on step (1) described colorimetric sensor films using the method for electropolymerization, it
The step of passing through elution afterwards obtains molecular engram and polymerize film modified semiconductor gas sensor;
(3) step (2) described sensor is placed among blank environment and is reacted, initial resistivity value is obtained, later by step
(2) sensor is placed among the nitro arene explosive substance environment of at least five kinds of various concentrations and is reacted, and obtains response electricity
Resistance value;
(4) according to the ratio of initial resistivity value and response resistance value, step (2) sensor is obtained to the nitro of various concentration
The response intensity of arene explosive substance, and then obtain the response intensity of step (2) described sensor and the nitre of the various concentration
Standard curve between base arene explosive substance;
(5) being placed in environment to be measured for step row (2) described sensor is obtained into the reality of step (2) sensor into reaction
Border responds resistance value, then according to initial resistivity value obtained by step (3), obtains step (2) described sensor for environment to be measured
Response intensity, it is bent according to the standard between the nitro arene explosive substance of the response intensity and the various concentration later
Line up to nitro arene explosive substance in environment to be measured concentration;
In above-mentioned method, step (1) described metal oxide isγ-Fe2O3、SnO2、ZnO、TiO2Or In2O3, partial size
Range is 10nm ~ 10 μm;
In above-mentioned method, step (1) and (2) described semiconductor film thickness range are 20nm ~ 50 μm, and molecular engram polymerize film thickness
Spending range is 10nm ~ 1 μm;
In above-mentioned method, for electropolymerization described in step (2) using cyclic voltammetry, function monomer is resorcinol, mould
Plate molecule is photoacoustic spectroscopy (concentrated sulfuric acid predissolve), and the concentration range of resorcinol is 3 × 10-5~3×10-2mol/ L,
The concentration range of photoacoustic spectroscopy is 1 × 10-5~1×10-2mol/ L, solvent are phosphate buffer, the potential windows of polymerization
Mouth is 0.0 ~ 0.8V, and scanning circle number range is 50 ~ 300 circles;
In above-mentioned method, using cyclic voltammetry, eluent is NaOH aqueous solution, dense for elution described in step (2)
Degree range is 0.1 ~ 0.8mol/L, and the potential window of elution is -0.5 ~ 0.5V, and scanning circle number range is 10 ~ 50 circles;
In above-mentioned method, step (3), (4) and (5) nitro arene explosive substance is photoacoustic spectroscopy, 2,4,6-
Trinitrotoluene, 2,4-DNT, para-nitrotoluene and 2,4,6- trinitrophenol;
In above-mentioned method, the time range of step (3) and (5) described reaction is 0.5min ~ 120min, the temperature range of reaction
It is 200 ~ 450 DEG C;
In above-mentioned method, in blank environment described in step (3) and (5) and environment to be measured the volume fraction of oxygen be 15% ~
25%。
It polymerize film modified semiconductors coupling film sensors detection nitro virtue using molecular engram the present invention provides a kind of
The method of hydro carbons explosive.The method overcome conventional semiconductors gas sensors to nitro arene explosive substance poor selectivity,
The low disadvantage of responsiveness reaches ppb magnitude to nitro arene explosive substance detection sensitivity.This method testing goal be not for
The differentiation above nitro arene explosive substance, but the response of indifference level signal is generated to the above explosive, it is used for Environmental Trace
The detection of nitro arene explosive substance, to judge in environment with the presence or absence of latent explosive.
Detailed description of the invention
Fig. 1 is the detection that molecular engram polymerize film modified composite membrane semiconductor gas sensor in the embodiment of the present invention 1
Schematic illustration.
Fig. 2 is that 2,4,6- trinitrotoluene concentration polymerize film modified composite membrane with molecular engram in the embodiment of the present invention 1
Standard curve between semiconductor gas sensor response intensity.
Fig. 3 is that photoacoustic spectroscopy concentration polymerize film modified composite membrane half with molecular engram in the embodiment of the present invention 2
Standard curve between conductor gas sensor response intensity.
Fig. 4 is that 2,4-DNT concentration polymerize film modified composite membrane half with molecular engram in the embodiment of the present invention 3
Standard curve between conductor gas sensor response intensity.
Fig. 5 is that para-nitrotoluene concentration polymerize film modified compound film semiconductor with molecular engram in the embodiment of the present invention 4
Standard curve between gas sensor response intensity.
Fig. 6 is that trinitrophenol concentration polymerize film modified compound film semiconductor with molecular engram in the embodiment of the present invention 5
Standard curve between gas sensor response intensity.
Specific embodiment
Technical solution of the present invention is further illustrated now in conjunction with attached drawing and specific embodiment, but the present invention not only limits
In embodiment disclosed below.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is unless otherwise specified that analysis is pure.
The proportion of No. 1 liquid as used in the following examples is NH4OH:H2O2:H2O=1:2:5(volume ratio);No. 2 liquid
Proportion is HCl:H2O2:H2O=1:2:8(volume ratio).
Embodiment 1:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using metallic zinc simple substance as target, zinc oxide semi-conductor gas sensor (ZnO/ is prepared by reaction gas of oxygen
IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are 5cm.
By containing 3 × 10-5 Mol/L resorcinol and 1 × 10-5 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) in cyclic voltammetry molecular engram polymeric membrane is prepared on the surface ZnO/IE,
Electropolymerizatioconditions conditions are 200 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 40 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane zinc oxide semi-conductor gas sensor (MIP/ZnO/IE).
MIP/ZnO/IE is placed among blank environment, 30min is reacted at 350 DEG C, records the resistance of sensor at this time,
Obtain initial resistivity value;Later by MIP/ZnO/IE be placed in preparation standard 2,4,6- trinitrotoluene gaseous environment (concentration according to
It is secondary be 10,50,100,250,500ppb) in, react 30min at 350 DEG C, obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/ZnO/IE is obtained to the 2,4,6- of various concentration
The response intensity of trinitrotoluene, and then obtain the response intensity and 2, the 4,6- tri- of the various concentration of the MIP/ZnO/IE
Standard curve between nitrotoleune;
The MIP/ZnO/IE is placed in environment to be measured and is reacted, the real response resistance of the MIP/ZnO/IE is obtained
Value, then according to initial resistivity value, obtaining the MIP/ZnO/IE is 1.38 for the response intensity of environment to be measured, later basis
Standard curve between the 2,4,6-trinitrotoluene of the response intensity and the various concentration to get in environment to be measured 2,
The concentration of 4,6- trinitrotoluene is 100ppb.
Embodiment 2:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance zinc metal as target, zinc oxide semi-conductor gas sensor (ZnO/ is prepared by reaction gas of oxygen
IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are 5cm.
By containing 3 × 10-4 Mol/L resorcinol and 1 × 10-4 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) in cyclic voltammetry molecular engram polymeric membrane is prepared on the surface ZnO/IE,
Electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.2M NaOH solution from 0.5 to 0.5V, scanning circle number is 30 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane zinc oxide semi-conductor gas sensor (MIP/ZnO/IE).
MIP/ZnO/IE is placed among blank environment, 40min is reacted at 300 DEG C, records the resistance of sensor at this time,
Initial resistivity value is obtained, MIP/ZnO/IE is placed in the standard photoacoustic spectroscopy gaseous environment of preparation later, and (concentration is successively
For 10,50,100,250,500ppb) in, 40min is reacted at 300 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/ZnO/IE is obtained to the triamido of various concentration
The response intensity of trinitrobenzen, and then obtain the response intensity of the MIP/ZnO/IE and three nitre of triamido of the various concentration
Standard curve between base benzene;
The MIP/ZnO/IE is placed in environment to be measured and is reacted, the real response resistance of the MIP/ZnO/IE is obtained
Value, then according to initial resistivity value, obtaining the MIP/ZnO/IE is 2.3 for the response intensity of environment to be measured, later basis
Standard curve between the photoacoustic spectroscopy of the response intensity and the various concentration is to get three ammonia in environment to be measured
The concentration of base trinitrobenzen is 150ppb.
Embodiment 3:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance zinc metal as target, zinc oxide semi-conductor gas sensor (MIP/ is prepared by reaction gas of oxygen
ZnO/IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are 5cm.
By containing 6 × 10-5 Mol/L resorcinol and 2 × 10-5 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) in prepared on the surface MIP/ZnO/IE with cyclic voltammetry molecular engram polymerization
Film, electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then lead to
The potential window elution in 0.1M NaOH solution from 0.5 to 0.5V is crossed, scanning circle number is 15 circles, to wash away the template of insertion
Molecule obtains molecular engram and polymerize film modified composite membrane zinc oxide semi-conductor gas sensor (MIP/ZnO/IE).
MIP/ZnO/IE is placed among blank environment, 50min is reacted at 200 DEG C, records the resistance of sensor at this time,
Initial resistivity value is obtained, MIP/ZnO/IE is placed in the standard 2 of preparation later, (concentration is successively for 4- dinitrotoluene (DNT) gaseous environment
For 10,50,100,250,500ppb) in, 50min is reacted at 200 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/ZnO/IE is obtained to 2, the 4- bis- of various concentration
The response intensity of nitrotoleune, and then obtain the response intensity of the MIP/ZnO/IE and 2, the 4- dinitro of the various concentration
Standard curve between toluene;
The MIP/ZnO/IE is placed in environment to be measured and is reacted, the real response resistance of the MIP/ZnO/IE is obtained
Value, then according to initial resistivity value, obtaining the MIP/ZnO/IE is 1.53 for the response intensity of environment to be measured, later basis
Standard curve between 2, the 4- dinitrotoluene (DNT) of the response intensity and the various concentration is to get in environment to be measured 2,4-
The concentration of dinitrotoluene (DNT) is 100ppb.
Embodiment 4:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance zinc metal as target, zinc oxide semi-conductor gas sensor (MIP/ is prepared by reaction gas of oxygen
ZnO/IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are 5cm.
By containing 6 × 10-5 Mol/L resorcinol and 2 × 10-5 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) in prepared on the surface MIP/ZnO/IE with cyclic voltammetry molecular engram polymerization
Film, electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then lead to
The potential window elution in 0.1M NaOH solution from 0.5 to 0.5V is crossed, scanning circle number is 15 circles, to wash away the template of insertion
Molecule obtains molecular engram and polymerize film modified composite membrane zinc oxide semi-conductor gas sensor (MIP/ZnO/IE).
MIP/ZnO/IE is placed among blank environment, 50min is reacted at 200 DEG C, records the resistance of sensor at this time,
Obtain initial resistivity value, later by MIP/ZnO/IE be placed in preparation standard para-nitrotoluene gaseous environment (concentration is followed successively by 10,
50,100,250,500ppb) in, 50min is reacted at 200 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/ZnO/IE is obtained to various concentration to nitro
The response intensity of toluene, and then obtain between the response intensity of the MIP/ZnO/IE and the para-nitrotoluene of the various concentration
Standard curve;
The MIP/ZnO/IE is placed in environment to be measured and is reacted, the real response resistance of the MIP/ZnO/IE is obtained
Value, then according to initial resistivity value, obtaining the MIP/ZnO/IE is 1.72 for the response intensity of environment to be measured, later basis
Standard curve between the para-nitrotoluene of the response intensity and the various concentration to get in environment to be measured to nitro first
The concentration of benzene is 200ppb.
Embodiment 5:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance zinc metal as target, zinc oxide semi-conductor gas sensor (MIP/ is prepared by reaction gas of oxygen
ZnO/IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are 5cm.
By containing 6 × 10-5 Mol/L resorcinol and 2 × 10-5 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) in prepared on the surface MIP/ZnO/IE with cyclic voltammetry molecular engram polymerization
Film, electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then lead to
The potential window elution in 0.1M NaOH solution from 0.5 to 0.5V is crossed, scanning circle number is 15 circles, to wash away the template of insertion
Molecule obtains molecular engram and polymerize film modified composite membrane zinc oxide semi-conductor gas sensor (MIP/ZnO/IE).
MIP/ZnO/IE is placed among blank environment, 50min is reacted at 200 DEG C, records the resistance of sensor at this time,
Obtain initial resistivity value, later by MIP/ZnO/IE be placed in preparation standard trinitrophenol gaseous environment (concentration is followed successively by 10,
50,100,250,500ppb) in, 50min is reacted at 200 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/ZnO/IE is obtained to the trinitro- of various concentration
The response intensity of phenol, and then obtain between the response intensity of the MIP/ZnO/IE and the trinitrophenol of the various concentration
Standard curve;
The MIP/ZnO/IE is placed in environment to be measured and is reacted, the real response resistance of the MIP/ZnO/IE is obtained
Value, then according to initial resistivity value, obtaining the MIP/ZnO/IE is 1.92 for the response intensity of environment to be measured, later basis
Standard curve between the trinitrophenol of the response intensity and the various concentration is to get trinitrobenzen in environment to be measured
The concentration of phenol is 100ppb.
Embodiment 6:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance ferrous metal as target, di-iron trioxide semiconductor gas sensor is prepared by reaction gas of oxygen
(γ-Fe2O3/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing
For 5cm.
By containing 6 × 10-4 Mol/L resorcinol and 2 × 10-4 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry existγ-Fe2O3Molecular engram polymerization is prepared on the surface /IE
Film, electropolymerizatioconditions conditions are 250 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then lead to
The potential window elution in 0.1M NaOH solution from 0.5 to 0.5V is crossed, scanning circle number is 25 circles, to wash away the template of insertion
Molecule obtains molecular engram and polymerize film modified composite membrane di-iron trioxide semiconductor gas sensor (MIP/γ-Fe2O3/
IE).
By MIP/γ-Fe2O3/ IE is placed among blank environment, reacts 50min at 200 DEG C, record sensor at this time
Resistance obtains initial resistivity value, and the standard 2,4,6-trinitrotoluene gaseous environment that MIP/ZnO/IE is placed in preparation later is (dense
Degree is followed successively by 10,50,100,250,500ppb) in, 50min is reacted at 200 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/ is obtainedγ-Fe2O3/ IE to the 2 of various concentration,
The response intensity of 4,6- trinitrotoluenes, and then obtain the MIP/γ-Fe2O3The response intensity of/IE and the various concentration
Standard curve between 2,4,6- trinitrotoluene;
By the MIP/γ-Fe2O3/ IE, which is placed in environment to be measured, to be reacted, and the MIP/ is obtainedγ-Fe2O3The reality of/IE
It responds resistance value and obtains the MIP/ then according to initial resistivity valueγ-Fe2O3/ IE for environment to be measured response intensity, it
Afterwards according to the standard curve between the 2,4,6-trinitrotoluene of the response intensity and the various concentration to get ring to be measured
The concentration of 2,4,6- trinitrotoluene in border.
Embodiment 7:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance tin metal as target, tin oxide semiconductor gas sensor is prepared by reaction gas of oxygen
(SnO2/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are
5cm。
By containing 6 × 10-4 Mol/L resorcinol and 3 × 10-4 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry in SnO2/ IE prepares molecular engram polymeric membrane on surface,
Electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 15 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane tin oxide semiconductor gas sensor (MIP/SnO2/ IE).
By MIP/SnO2/ IE is placed among blank environment, and 50min is reacted at 400 DEG C, records the electricity of sensor at this time
Resistance, obtains initial resistivity value, the standard 2,4,6-trinitrotoluene gaseous environment that MIP/ZnO/IE is placed in preparation later is (dense
Degree is followed successively by 10,50,100,250,500ppb) in, 50min is reacted at 400 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/SnO is obtained2/ IE to the 2,4 of various concentration,
The response intensity of 6- trinitrotoluene, and then obtain the MIP/SnO2The 2,4 of the response intensity of/IE and the various concentration,
Standard curve between 6- trinitrotoluene;
By the MIP/SnO2/ IE, which is placed in environment to be measured, to be reacted, and the MIP/SnO is obtained2The real response resistance of/IE
Value, then according to initial resistivity value, obtains the MIP/SnO2/ IE for environment to be measured response intensity, later according to
Response intensity and the various concentration 2,4,6-trinitrotoluene between standard curve to get in environment to be measured 2,4,6-
The concentration of trinitrotoluene.
Embodiment 8:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance tin metal as target, tin oxide semiconductor gas sensor is prepared by reaction gas of oxygen
(SnO2/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are
5cm。
By containing 6 × 10-3Mol/L resorcinol and 3 × 10-3 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry in SnO2/ IE prepares molecular engram polymeric membrane on surface,
Electropolymerizatioconditions conditions are 250 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 25 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane tin oxide semiconductor gas sensor (MIP/SnO2/ IE).
By MIP/SnO2/ IE is placed among blank environment, and 100min is reacted at 300 DEG C, records the electricity of sensor at this time
Resistance, obtains initial resistivity value, MIP/ZnO/IE is placed in the standard 2,4,6-trinitrotoluene gaseous environment (concentration of preparation later
It is followed successively by 10,50,100,250,500ppb) in, 100min is reacted at 300 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/SnO is obtained2/ IE to the 2,4 of various concentration,
The response intensity of 6- trinitrotoluene, and then obtain the MIP/SnO2The 2,4 of the response intensity of/IE and the various concentration,
Standard curve between 6- trinitrotoluene;
By the MIP/SnO2/ IE, which is placed in environment to be measured, to be reacted, and the MIP/SnO is obtained2The real response resistance of/IE
Value, then according to initial resistivity value, obtains the MIP/SnO2/ IE for environment to be measured response intensity, later according to
Response intensity and the various concentration 2,4,6-trinitrotoluene between standard curve to get in environment to be measured 2,4,6-
The concentration of trinitrotoluene.
Embodiment 9:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance titanium as target, titanium oxide semiconductor gas sensor is prepared by reaction gas of oxygen
(TiO2/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are
5cm。
By containing 3 × 10-4 Mol/L resorcinol and 1 × 10-4 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry in TiO2/ IE prepares molecular engram polymeric membrane on surface,
Electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 15 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane titanium oxide semiconductor gas sensor (MIP/TiO2/ IE).
By MIP/TiO2/ IE is placed among blank environment, and 70min is reacted at 250 DEG C, records the electricity of sensor at this time
Resistance, obtains initial resistivity value, MIP/ZnO/IE is placed in the standard 2,4,6-trinitrotoluene gaseous environment (concentration of preparation later
It is followed successively by 10,50,100,250,500ppb) in, 70min is reacted at 250 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/TiO is obtained2/ IE to the 2,4 of various concentration,
The response intensity of 6- trinitrotoluene, and then obtain the MIP/TiO2The 2,4 of the response intensity of/IE and the various concentration,
Standard curve between 6- trinitrotoluene;
By the MIP/TiO2/ IE, which is placed in environment to be measured, to be reacted, and the MIP/TiO is obtained2The real response resistance of/IE
Value, then according to initial resistivity value, obtains the MIP/TiO2/ IE for environment to be measured response intensity, later according to
Response intensity and the various concentration 2,4,6-trinitrotoluene between standard curve to get in environment to be measured 2,4,6-
The concentration of trinitrotoluene.
Embodiment 10:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance titanium as target, titanium oxide semiconductor gas sensor is prepared by reaction gas of oxygen
(TiO2/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are
5cm。
By containing 3 × 10-5 Mol/L resorcinol and 1 × 10-5 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry in TiO2/ IE prepares molecular engram polymeric membrane on surface,
Electropolymerizatioconditions conditions are 200 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 20 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane titanium oxide semiconductor gas sensor (MIP/TiO2/ IE).
By MIP/TiO2/ IE is placed among blank environment, and 40min is reacted at 320 DEG C, records the electricity of sensor at this time
Resistance, obtains initial resistivity value, MIP/ZnO/IE is placed in the standard 2,4,6-trinitrotoluene gaseous environment (concentration of preparation later
It is followed successively by 10,50,100,250,500ppb) in, 40min is reacted at 320 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/TiO is obtained2/ IE to the 2,4 of various concentration,
The response intensity of 6- trinitrotoluene, and then obtain the MIP/TiO2The 2,4 of the response intensity of/IE and the various concentration,
Standard curve between 6- trinitrotoluene;
By the MIP/TiO2/ IE, which is placed in environment to be measured, to be reacted, and the MIP/TiO is obtained2The real response resistance of/IE
Value, then according to initial resistivity value, obtains the MIP/TiO2/ IE for environment to be measured response intensity, later according to
Response intensity and the various concentration 2,4,6-trinitrotoluene between standard curve to get in environment to be measured 2,4,6-
The concentration of trinitrotoluene.
Embodiment 11:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance indium metal as target, indium oxide semiconductor gas sensor is prepared by reaction gas of oxygen
(In2O3/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are
5cm。
By containing 8 × 10-4 Mol/L resorcinol and 4 × 10-4 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry in In2O3/ IE prepares molecular engram polymeric membrane on surface,
Electropolymerizatioconditions conditions are 150 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 15 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane indium oxide semiconductor gas sensor (MIP/In2O3/ IE).
By MIP/In2O3/ IE is placed among blank environment, and 30min is reacted at 400 DEG C, records the electricity of sensor at this time
Resistance, obtains initial resistivity value, MIP/ZnO/IE is placed in the standard 2,4,6-trinitrotoluene gaseous environment (concentration of preparation later
It is followed successively by 10,50,100,250,500ppb) in, 30min is reacted at 400 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/In is obtained2O3/ IE to the 2,4 of various concentration,
The response intensity of 6- trinitrotoluene, and then obtain the MIP/In2O3The 2,4 of the response intensity of/IE and the various concentration,
Standard curve between 6- trinitrotoluene;
By the MIP/In2O3/ IE, which is placed in environment to be measured, to be reacted, and the MIP/In is obtained2O3The real response electricity of/IE
Resistance value obtains the MIP/In then according to initial resistivity value2O3/ IE for environment to be measured response intensity, later according to institute
Standard curve between the 2,4,6-trinitrotoluene of the response intensity and the various concentration stated to get in environment to be measured 2,4,
The concentration of 6- trinitrotoluene.
Embodiment 12:
It takes commercially available interdigital electrode (IE) to be boiled with No. 1 liquid to boiling, outwells raffinate, repeat 3 times, be washed with deionized water, repeat 3 times;
It is boiled 3 minutes with No. 2 liquid, outwells raffinate, repeated 3 times, be washed with deionized water, repeated 3 times;It is dried after cleaning with infrared lamp
And as substrate, using simple substance indium metal as target, indium oxide semiconductor gas sensor is prepared by reaction gas of oxygen
(In2O3/ IE), system-based vacuum is 6.0 × 10 in preparation process−5Pa, radio-frequency power 100W, target and substrate spacing are
5cm。
By containing 9 × 10-4 Mol/L resorcinol and 3 × 10-4 (concentrated sulfuric acid is pre-dissolved mol/L photoacoustic spectroscopy
Solution) phosphate buffer solution (pH=7.0) middle cyclic voltammetry in In2O3/ IE prepares molecular engram polymeric membrane on surface,
Electropolymerizatioconditions conditions are 200 circle of scanning under conditions of scanning speed is 50mV/s in the potential range of 0.0 ~ 0.8V.Then by
Potential window elution in 0.1M NaOH solution from 0.5 to 0.5V, scanning circle number is 20 circles, to wash away the template point of insertion
Son obtains molecular engram and polymerize film modified composite membrane indium oxide semiconductor gas sensor (MIP/In2O3/ IE).
By MIP/In2O3/ IE is placed among blank environment, and 60min is reacted at 300 DEG C, records the electricity of sensor at this time
Resistance, obtains initial resistivity value, MIP/ZnO/IE is placed in the standard 2,4,6-trinitrotoluene gaseous environment (concentration of preparation later
It is followed successively by 10,50,100,250,500ppb) in, 60min is reacted at 300 DEG C;Obtain corresponding response resistance value.
According to the ratio of initial resistivity value and response resistance value, the MIP/In is obtained2O3/ IE to the 2,4 of various concentration,
The response intensity of 6- trinitrotoluene, and then obtain the MIP/In2O3The 2,4 of the response intensity of/IE and the various concentration,
Standard curve between 6- trinitrotoluene;By the MIP/In2O3/ IE, which is placed in environment to be measured, to be reacted, and is obtained described
MIP/In2O3The real response resistance value of/IE obtains the MIP/In then according to initial resistivity value2O3/ IE is for ring to be measured
The response intensity in border, later according to the standard between the 2,4,6-trinitrotoluene of the response intensity and the various concentration
Curve to get 2,4,6-trinitrotoluene in environment to be measured concentration.
Claims (8)
1. a kind of detection method of nitro arene explosive substance, comprising the following steps:
(1) metal-oxide film is formed on interdigital electrode surface using the method for sputtering, obtains semiconductor gas sensor;
(2) one layer of molecular imprinted polymer membrane is modified on step (1) described colorimetric sensor films using the method for electropolymerization, it
It polymerize film modified semiconductor gas sensor by affording molecular engram afterwards;
(3) step (2) described sensor is placed among blank environment and is reacted, initial resistivity value is obtained, later by step
(2) sensor is placed among the nitro arene explosive substance environment of at least five kinds of various concentrations and is reacted, and obtains response electricity
Resistance value;
(4) according to the ratio of initial resistivity value and response resistance value, step (2) sensor is obtained to the nitro of various concentration
The response intensity of arene explosive substance, and then obtain the response intensity of step (2) described sensor and the nitre of the various concentration
Standard curve between base arene explosive substance;
(5) step (2) described sensor is placed in environment to be measured and is reacted, obtain the reality of step (2) sensor
Resistance value is responded, then according to initial resistivity value obtained by step (3), obtains step (2) described sensor for environment to be measured
Response intensity, later according to the standard curve between the nitro arene explosive substance of the response intensity and the various concentration
Up to the concentration of nitro arene explosive substance in environment to be measured.
2. according to the method described in claim 1, it is characterized by: in step (1), the metal oxide isγ-Fe2O3、
SnO2、ZnO、TiO2Or In2O3, particle size range is 10nm ~ 10 μm.
3. according to the method described in claim 1, it is characterized by: in step (1) and (2), the semiconductor film thickness range
It is 20nm ~ 50 μm, molecular engram polymeric film thicknesses range is 10nm ~ 1 μm.
4. according to the method described in claim 1, it is characterized by: the electropolymerization is using cyclic voltammetric in step (2)
Method, function monomer are resorcinols, and template molecule is photoacoustic spectroscopy, and the concentration range of resorcinol is 3 × 10-5~3×
10-2 Mol/L, the concentration range of photoacoustic spectroscopy are 1 × 10-5~1×10-2 Mol/L, solvent are phosphate buffers, are gathered
The potential window of conjunction is 0.0 ~ 0.8V, and scanning circle number range is 50 ~ 300 circles.
5. according to the method described in claim 1, it is characterized by: the elution is using cyclic voltammetric in step (2)
Method, eluent are NaOH aqueous solution, and concentration range is 0.1 ~ 0.8mol/L, and the potential window of elution is -0.5 ~ 0.5V, scanning
Circle number range is 10 ~ 50 circles.
6. according to the method described in claim 1, it is characterized by: the nitro-aromatic class is quick-fried in step (3), (4) and (5)
Fried object is photoacoustic spectroscopy, 2,4,6- trinitrotoluene, 2,4-DNT, para-nitrotoluene and 2,4,6- trinitro-
Phenol.
7. according to the method described in claim 1, it is characterized by: in step (3) and (5), the time range of the reaction is
0.5min ~ 120min, the temperature range of reaction are 200 ~ 450 DEG C.
8. according to the method described in claim 1, it is characterized by: in step (3) and (5), the blank environment and to be measured
The range of the volume fraction of oxygen is 15% ~ 25% in environment.
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