CN108414490A - Fluorescence gel test paper and fluorescence colloidal sol, and preparation method and application - Google Patents
Fluorescence gel test paper and fluorescence colloidal sol, and preparation method and application Download PDFInfo
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- CN108414490A CN108414490A CN201810242093.7A CN201810242093A CN108414490A CN 108414490 A CN108414490 A CN 108414490A CN 201810242093 A CN201810242093 A CN 201810242093A CN 108414490 A CN108414490 A CN 108414490A
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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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- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention discloses a kind of preparation methods of fluorescence gel test paper, include the following steps：Step 1：By organic ligand DDT and Cd (NO3)2Mixing, is used in combination DMF to dissolve；Step 2：It is added in baking oven and toasts, the gel colloidal of semi-solid state is made.Step 3：After taking-up, gel colloidal dilution is prepared into colloidal sol, and load on paper material, obtains fluorescence gel test paper.The present invention also provides a kind of fluorescence gel test paper and its applications.The present invention also provides a kind of fluorescence colloidal sols and preparation method and application.The raw material of the present invention is easy to get, and production method is easy, and fluorescence gel test paper is not affected by the external environment, can long-term preservation.Detection speed of the present invention is fast, and Nitroaromatic explosive solution is added dropwise or Ethanol activation is added dropwise after wiping the sample for having explosive, after fluorescence gel test paper is done, puts the change in fluorescence for visually observing test paper in the UV lamp, whether contains explosive in judgement sample.
Description
Technical field
The present invention relates to a kind of Test papers, and in particular to a kind of fluorescence for quickly detecting Nitroaromatic explosive is solidifying
Glue test paper and the preparation method and application thereof further relates to fluorescence colloidal sol and preparation method and application, belongs to explosive detection analysis
Technical field.
Background technology
Nitroaromatic explosive is a kind of common dangerous explosive, to national security and people's lives in the attack of terrorism
Bring great threat.In addition to this, it during the production and transportation of explosive, is also easy to penetrate into soil and underground
In water, become the carcinogenic substance highly toxic to the mankind, when people suck such compound, hepatic disease, regeneration barrier can be caused
The diseases such as impenetrability anaemia and cataract are caused greatly to negatively affect, also be caused great harm to the health of the common people to environment.
Therefore, it is most important to study influence of micro- trace explosive to environment.
In addition, such harmful influence requires to detect whenever and wherever possible at the scene, the shorter the response time the better, and detection mode also requires
It is quick rapid.Therefore, development is quick, convenient, and the method for inexpensive detection Nitroaromatic explosive is increasingly by researcher
Concern.
Fluorescence detection method often uses detection method as a kind of effective nitro explosive, has high sensitivity, stablizes
The advantages such as property height, however traditional fluorescence detection method needs instrument to detect, it is expensive, it is inconvenient to use, there is certain office
It is sex-limited.Fluorescence gel test paper have it is easy to carry, phenomenon is apparent, fast response time, the advantages such as at low cost, it is only necessary to which one is portable
Ultraviolet lamp can be carried out the real-time naked eyes quickly identification at scene, be paid high attention to by researcher.However, current Chinese patent
Nitro explosive Test paper disclosed in document CN106596493A and CN107167462A, CN107286327A, is supported on
Fluorescent material on test paper is mostly the fluorescent material of solubility, is easily transferred in detection process in aqueous phase system or organic phase
And causing the loss or dilution of material, the fluorescence intensity for be easy to causeing test paper itself weakens, to reduce the sensitivity of its test paper.
And the synthesis technology of fluorescent material is complex, super more step, and the structure of fluorescent ligand is also very complicated, after synthesis
The operations such as reason purifying are all pretty troublesome, these all constrain the application of fluorescent test paper.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of inspections of the fluorescence gel of quick detection Nitroaromatic explosive
Test paper and the preparation method and application thereof, fluorescence gel test paper load fluorescent material be a kind of highly stable colloid, not by
The influence of any environment does not dissolve in water phase or organic phase, and preparation is very simple, and raw material is easy to get, fluorescence intensity in detection process
Remained unchanged with sensitivity, overcome the limitation of traditional nitro benzene class explosive detection, be used for trinitrobenzen, dinitrobenzene,
Picric acid, the detection of a variety of explosives such as trinitrotoluene.
In order to solve the above technical problems, the present invention uses following technical scheme：
A kind of preparation method of fluorescence gel test paper, includes the following steps：
Step 1：By bis- (1H-TETRAZOLE -5- the bases) -2H-1,2,3- triazoles hydrates of organic ligand 4,5- (referred to as DDT)
With Cd (NO3)2Mixing, is used in combination DMF to dissolve；
Step 2：It is added in baking oven and toasts, the gel colloidal of semi-solid state is made.
Step 3：After taking-up, gel colloidal dilution is prepared into colloidal sol, and load on paper material, it is solidifying to obtain fluorescence
Glue test paper.
Further scheme is：
In step 1, organic ligand DDT and Cd (NO3)2Mixed molar ratio is 1:1 to 1:2.5.
Further scheme is：
When the amount of DDT is not more than 200 milligram hours in step 1, the amount of DMF dissolvings is not more than 0.5 milliliter；Wherein, 0.4 milli
It is upgraded to optimum solvent amount.
Further scheme is：
In step 2, the temperature of baking oven is 60 DEG C -100 DEG C, and baking time is 20min -40min.
Further scheme is：
In step 2, the temperature of baking oven is 80 DEG C, baking time 30min.
Further scheme is：
In step 3, collosol concentration is 1.0M -0.01M.
Further scheme is：
In step 3, collosol concentration 0.1M.
Further scheme is：
In step 3, paper material is more filter paper, filters paper or papery non-woven fabrics, and mode of loading is to filter or impregnate, and is born
After being downloaded on paper material, dry at room temperature.
The present invention also provides a kind of fluorescence gel test paper, prepared by the preparation method of fluorescence gel test paper above-mentioned
It obtains.
It is micro for Nitroaromatic explosive in solution or solid the present invention also provides the application of fluorescence gel test paper
Detection, the nitrobenzene are trinitrobenzen, dinitrobenzene, picric acid, trinitrotoluene.
Further scheme is：
Detection includes：
First, fluorescence gel test paper is placed under ultraviolet lamp and sees whether to send out bluish violet fluorescence, if any then illustrating test paper
Effectively, it can directly use；
Secondly, according to the difference of sample to be tested, different detection methods is selected；
When sample to be tested is solution, testing sample solution is taken to drip on fluorescence gel test paper, or by fluorescence gel test paper
It is immersed in testing sample solution, stands 5s, take out fluorescence gel test paper, after fluorescence gel test paper is done, put in the UV lamp
The change in fluorescence of test paper is visually observed, if Fluorescence-quenching has occurred in test paper, is exploded containing nitrobenzene in judgement sample
Object does not contain explosive if test paper does not have fluorescent quenching in judgement sample.
When sample to be tested is solid, after test paper is used for wiping and being stained with the sample of explosive, several drop ethyl alcohol work are added dropwise
Change, after fluorescence gel test paper is done, the change in fluorescence for visually observing test paper in the UV lamp is put, if fluorescent quenching has occurred in test paper
Phenomenon then contains Nitroaromatic explosive in judgement sample, if test paper does not have fluorescent quenching, explosion is not contained in judgement sample
Object.
On this basis, the present invention also provides a kind of fluorescence colloidal sols and preparation method and application.
A kind of preparation method of fluorescence colloidal sol, it is characterised in that include the following steps：
Step 1：By bis- (1H-TETRAZOLE -5- the bases) -2H-1,2,3- triazoles hydrates (DDT) of organic ligand 4,5- and Cd
(NO3)2Mixing, is used in combination DMF to dissolve；
Step 2：It is added in baking oven and toasts, the gel colloidal of semi-solid state is made.
Step 3：After taking-up, fluorescence colloidal sol is prepared in gel colloidal dilution.
The application of fluorescence colloidal sol is for use as quickly detecting the fluorescence chemical sensor of Nitroaromatic explosive, i.e., will
This gel is diluted to colloidal sol, and the solution of Nitroaromatic explosive or solid are added in colloidal sol, is shone in ultraviolet lamp according to colloidal sol
Fluorescence color variation under penetrating, or the case where colloid quenches is detected using sepectrophotofluorometer, to which whether identification contains
There is Nitroaromatic explosive.
Explosive fluorescent optical sensor, is detected using luminoscope, can quickly obtain the picric Testing and appraisal of 1ppb.
The beneficial effects of the present invention are：
1, raw material of the invention is easy to get, and production method is easy, and the fluorescent material of fluorescence gel test paper load is a kind of colloid,
Property stablize, be not affected by the external environment, can long-term preservation, be used as fluorescence indicator, can avoid by solvent, acid-base property is to glimmering
The influence of test paper autofluorescence strength reduction caused by the influence of luminescent material.
2, detection speed of the present invention is fast, and Nitroaromatic explosive solution is added dropwise or second is added dropwise after wiping the sample for having explosive
Alcohol activates, and after fluorescence gel test paper is done, the change in fluorescence for visually observing test paper in the UV lamp is put, if fluorescence has occurred in test paper
Quenching then contains Nitroaromatic explosive in judgement sample, if test paper does not have fluorescent quenching, is not contained in judgement sample
Explosive.The detection that naked eyes are observed that is limited down to 10-6M。
Description of the drawings
Fig. 1 is the synthetic route chart that the embodiment of the present invention one prepares organic ligand DDT；
Fig. 2 is the photo figure for the fluorescence gel that the embodiment of the present invention one is prepared.It can be seen that (a) figure on the left side, is solid
(b) figure of gel, the right shows the gel under ultra violet lamp, sends out strong bluish violet fluorescence.
Fig. 3 is the fluorescence gel test paper photo figure that the embodiment of the present invention one is prepared.It can be seen that (a) figure above, for certainly
Gel test paper under right light, (b) figure below show the test paper under ultra violet lamp, send out strong bluish violet fluorescence.
Fig. 4 is that the embodiment of the present invention one is quickly identified using fluorescence gel test paper p-nitrophenyl class explosive picric acid
Photo figure；It can be seen that (a) figure above, after picric acid is added dropwise, the gel test paper under natural light, (b) figure below shows this
Test paper sends out bluish violet fluorescence under ultra violet lamp, and as bitter taste acid concentration reduces, Quenching of fluorescence degree reduces.
Fig. 5 is that the embodiment of the present invention two is quickly known using fluorescence gel test paper p-nitrophenyl class explosive trinitrobenzen
Other photo figure；It can be seen that (a) figure above, after trinitrobenzen is added dropwise, the gel test paper under natural light, (b) figure below is shown
Show that the test paper under ultra violet lamp, sends out bluish violet fluorescence, as trinitrobenzen concentration reduces, Quenching of fluorescence degree subtracts
It is small.
Fig. 6 is that the embodiment of the present invention three is quickly known using fluorescence gel test paper p-nitrophenyl class explosive dinitrobenzene
Other photo figure；It can be seen that (a) figure above, after dinitrobenzene is added dropwise, the gel test paper under natural light, (b) figure below is shown
Show that the test paper under ultra violet lamp, sends out bluish violet fluorescence, as dinitrobenzene concentration reduces, Quenching of fluorescence degree subtracts
It is small.
Fig. 7 is that the embodiment of the present invention four is carried out quickly using fluorescence gel test paper p-nitrophenyl class explosive trinitrotoluene
The photo figure of identification；It can be seen that (a) figure above, after trinitrotoluene is added dropwise, the gel test paper under natural light, (b) below
Figure shows that the test paper under ultra violet lamp, sends out bluish violet fluorescence, as trinitrotoluene concentration reduces, Quenching of fluorescence journey
Degree reduces.
Specific implementation mode
Embodiment one
A kind of preparation method of fluorescence gel test paper, includes the following steps：
Step 1：The preparation of organic ligand DDT：
As shown in Fig. 1,2H- (1,2,3) triazole -4,5- dintrile, sodium azide and zinc chloride are soluble in water.It will clarify molten
Liquid is heated to reflux 3 hours, is then cooled to room temperature, and concentrated hydrochloric acid is added while 0 DEG C cooling.Suction strainer removes precipitation, thick to produce
Object water, ethyl alcohol and ether washing, obtain bis- (1H-TETRAZOLE -5- the bases) -2H-1 of 4,5-, 2,3- triazole hydrates.
Step 2：The preparation of fluorescent colloid：
At room temperature by DDT (102.5mg, 5 × 10-4) and Cd (NO M3)2·4H2O (154mg, 5 × 10-4M) it is dissolved in DMF
In (0.5mL), it is subsequently placed in 80 DEG C 15 minutes, obtains the translucent colloidal sol of high viscosity, then by obtained material with DMF (4.5mL)
Dilution is to obtain oenothera biennis yellow transparent solution, and as shown in Fig. 2, a is the fluorescence gel figure under solar illumination, b in wherein Fig. 2
For the fluorescence gel figure under UV Light.
Step 3：Filter paper or cotton swab are put into sol-gel, are then dried at room temperature for, obtains can be used for explosive
Gel test paper.As shown in Fig. 3, a is the fluorescence gel test paper under solar illumination wherein in Fig. 3, and b is under UV Light
Fluorescence gel test paper.
Step 4:The filter paper prepared is used for picric detection, as shown in figure 4, wherein a is fluorescence under solar illumination
Gel test paper quickly identifies picric acid b is that fluorescence gel test paper quickly identifies picric acid under UV Light.
Embodiment two
A kind of preparation method of fluorescence gel test paper, includes the following steps：
Step 1：The preparation of organic ligand DDT：
By 2H- (1,2,3) triazole -4,5- dintrile, sodium azide and zinc chloride are soluble in water.Clear solution is heated to reflux
It 3 hours, then cools to room temperature, and concentrated hydrochloric acid is added while 0 DEG C cooling.Suction strainer removes precipitation, crude product with water, ethyl alcohol
It is washed with ether, obtains bis- (1H-TETRAZOLE -5- the bases) -2H-1 of 4,5-, 2,3- triazole hydrates.
Step 2：The preparation of fluorescent colloid：
At room temperature by DDT (205mg, 1 × 10-3) and Cd (NO M3)2·4H2O (600mg, 2 × 10-3M) it is dissolved in DMF
In (1.0mL), it is subsequently placed in 80 DEG C 20 minutes, obtains the translucent colloidal sol of high viscosity, it is then that obtained material is dilute with DMF (9mL)
It releases to obtain oenothera biennis yellow transparent solution.
Step 3：Filter paper or cotton swab are put into sol-gel, are then dried at room temperature for, obtains can be used for explosive
Gel test paper.
Step 4:The filter paper prepared is used for the detection of trinitrobenzen, as shown in figure 5, wherein a is glimmering under solar illumination
Light gel test paper quickly identifies trinitrobenzen b is that fluorescence gel test paper quickly identifies trinitrobenzen under UV Light.
Embodiment three
A kind of preparation method of fluorescence gel test paper, includes the following steps：
Step 1：The preparation of organic ligand DDT：
By 2H- (1,2,3) triazole -4,5- dintrile, sodium azide and zinc chloride are soluble in water.Clear solution is heated to reflux
It 3 hours, then cools to room temperature, and concentrated hydrochloric acid is added while 0 DEG C cooling.Suction strainer removes precipitation, crude product with water, ethyl alcohol
It is washed with ether, obtains bis- (1H-TETRAZOLE -5- the bases) -2H-1 of 4,5-, 2,3- triazole hydrates.
Step 2：The preparation of fluorescent colloid：
At room temperature by DDT (156mg, 5.5 × 10-4) and Cd (NO M3)2·4H2O (400mg, 1.5 × 10-3M it) is dissolved in
In DMF (1.0mL), it is subsequently placed in 80 DEG C 20 minutes, obtains the translucent colloidal sol of high viscosity, then by obtained material with DMF (9mL)
Dilution is to obtain oenothera biennis yellow transparent solution.
Step 3：Filter paper or cotton swab are put into sol-gel, are then dried at room temperature for, obtains can be used for explosive
Gel test paper.
Step 4:The filter paper prepared is used for the detection of dinitrobenzene, as shown in fig. 6, a is that fluorescence is solidifying under solar illumination
Glue test paper paradinitrobenzene quickly identifies that b is that fluorescence gel test paper paradinitrobenzene quickly identifies under UV Light.
Example IV
A kind of preparation method of fluorescence gel test paper, includes the following steps：
Step 1：The preparation of organic ligand DDT：
By 2H- (1,2,3) triazole -4,5- dintrile, sodium azide and zinc chloride are soluble in water.Clear solution is heated to reflux
It 3 hours, then cools to room temperature, and concentrated hydrochloric acid is added while 0 DEG C cooling.Suction strainer removes precipitation, crude product with water, ethyl alcohol
It is washed with ether, obtains bis- (1H-TETRAZOLE -5- the bases) -2H-1 of 4,5-, 2,3- triazole hydrates.
Step 2：The preparation of fluorescent colloid：
At room temperature by DDT (156mg, 5.5 × 10-4) and Cd (NO M3)2·4H2O (400mg, 1.5 × 10-3M it) is dissolved in
In DMF (1.0mL), it is subsequently placed in 80 DEG C 20 minutes, obtains the translucent colloidal sol of high viscosity, then by obtained material with DMF (9mL)
Dilution is to obtain oenothera biennis yellow transparent solution.
Step 3：Filter paper or cotton swab are put into sol-gel, are then dried at room temperature for, obtains can be used for explosive
Gel test paper.
Step 4:The filter paper prepared is used for the detection of trinitrotoluene, as shown in Figure 7.Wherein a is under solar illumination
Fluorescence gel test paper paradinitrobenzene quickly identifies that b is that fluorescence gel test paper paradinitrobenzene quickly identifies under UV Light.
Although reference be made herein to invention has been described for explanatory embodiment of the invention, and above-described embodiment is only this hair
Bright preferable embodiment, embodiment of the present invention are not limited by the above embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other modification and implementations, these modifications and implementations will be fallen in principle disclosed in the present application
Within scope and spirit.
Claims (10)
1. a kind of preparation method of fluorescence gel test paper, it is characterised in that include the following steps：
Step 1：By organic ligand 4, bis- (1H-TETRAZOLE -5- the bases) -2H-1 of 5-, 2,3- triazole hydrates, i.e. DDT and Cd (NO3)2
Mixing, is used in combination DMF to dissolve；
Step 2：It is added in baking oven and toasts, the gel colloidal of semi-solid state is made；
Step 3：After taking-up, gel colloidal dilution is prepared into colloidal sol, and load on paper material, obtains fluorescence gel examination
Paper.
2. the preparation method of fluorescence gel test paper according to claim 1, it is characterised in that：
In step 1, organic ligand DDT and Cd (NO3)2Mixed molar ratio is 1:1 to 1:2.5.
3. the preparation method of fluorescence gel test paper according to claim 1, it is characterised in that：
In step 1, when the amount of DDT is not more than 200 milligram hours, the amount of DMF dissolvings is not more than 0.5 milliliter；
In step 2, the temperature of baking oven is 60 DEG C -100 DEG C, and baking time is 20min -40min；
In step 3, collosol concentration is 1.0M -0.01M.
4. the preparation method of fluorescence gel test paper according to claim 3, it is characterised in that：
In step 1, when the amount of DDT is not more than 200 milligram hours, the amount of DMF dissolvings is 0.4 milliliter；
In step 2, the temperature of baking oven is 80 DEG C, baking time 30min；
In step 3, collosol concentration 0.1M.
5. the preparation method of fluorescence gel test paper according to claim 1, it is characterised in that：
In step 3, paper material is more filter paper, filters paper or papery non-woven fabrics, and mode of loading is to filter or impregnate, and is loaded to
After on paper material, dry at room temperature.
6. a kind of fluorescence gel test paper is the preparation by the fluorescence gel test paper described in claim 1 to 5 any claim
What method was prepared.
7. the application of fluorescence gel test paper described in claim 6 is for the micro inspection of Nitroaromatic explosive in solution or solid
It surveys, nitrobenzene is trinitrobenzen, dinitrobenzene, picric acid, trinitrotoluene.
8. the application of fluorescence gel test paper according to claim 7, it is characterised in that：
Detection process includes：
First, fluorescence gel test paper is placed under ultraviolet lamp and sees whether to send out bluish violet fluorescence, if any then illustrating that test paper has
Effect, can directly use；
Secondly, according to the difference of sample to be tested, different detection methods is selected；
When sample to be tested is solution, testing sample solution is taken to drip on fluorescence gel test paper, or fluorescence gel test paper is impregnated
In testing sample solution, 5s is stood, takes out fluorescence gel test paper, after fluorescence gel test paper is done, puts naked eyes in the UV lamp
The change in fluorescence of observation test paper contains Nitroaromatic explosive if Fluorescence-quenching has occurred in test paper in judgement sample, if
Test paper does not have fluorescent quenching, then explosive is not contained in judgement sample.
When sample to be tested is solid, after test paper is used for wiping and being stained with the sample of explosive, a few drop Ethanol activations are added dropwise, it will
After fluorescence gel test paper is dry, the change in fluorescence for visually observing test paper in the UV lamp is put, if Fluorescence-quenching has occurred in test paper,
Then contain Nitroaromatic explosive in judgement sample, if test paper does not have fluorescent quenching, explosive is not contained in judgement sample.
9. a kind of preparation method of fluorescence colloidal sol, it is characterised in that include the following steps：
Step 1：By bis- (1H-TETRAZOLE -5- the bases) -2H-1,2,3- triazoles hydrates of organic ligand 4,5- and Cd (NO3)2According to rubbing
You are than being 1:1 to 1:2.5 mixing are used in combination the DMF no more than 0.5 milliliter to dissolve；
Step 2：It is added in baking oven and toasts, the temperature of baking oven is 60 DEG C -100 DEG C, and baking time is 20min -40min, is made
The gel colloidal of semi-solid state；
Step 3：After taking-up, fluorescence colloidal sol, collosol concentration 0.1M is prepared in gel colloidal dilution.
10. a kind of application of fluorescence colloidal sol, it is characterised in that be for use as quickly detecting the Fluoresceinated of Nitroaromatic explosive
Sensor is learned, i.e., the solution of Nitroaromatic explosive or solid are added in fluorescence colloidal sol, according to fluorescence colloidal sol in ultraviolet lamp
The lower fluorescence color variation of irradiation, or the case where colloid quenches is detected using sepectrophotofluorometer, to identify whether
Contain Nitroaromatic explosive.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109870417A (en) * | 2019-04-13 | 2019-06-11 | 中国科学院新疆理化技术研究所 | A kind of comparator gel and preparation method thereof quickly detecting non-standard explosion raw material urea |
| CN109870417B (en) * | 2019-04-13 | 2021-07-02 | 中国科学院新疆理化技术研究所 | Colorimetric gel for rapidly detecting non-standard explosive raw material urea and preparation method thereof |
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