CN107037177A - Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity - Google Patents
Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity Download PDFInfo
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- CN107037177A CN107037177A CN201610078537.9A CN201610078537A CN107037177A CN 107037177 A CN107037177 A CN 107037177A CN 201610078537 A CN201610078537 A CN 201610078537A CN 107037177 A CN107037177 A CN 107037177A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
- G01N31/223—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols
- G01N31/224—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols for investigating presence of dangerous gases
Abstract
Colorimetric gas sensor is improved by adding alkali to Cl the present invention relates to one kind2The method of detection sensitivity.Because chlorine is having H2Redox hydrolysis generation HCl and HClO can occur in the presence of O, sour generation can be detected using pH indicator, meanwhile, there are NaOH, KOH, Na2CO3、K2CO3In the presence of alkaline matter, because with above-mentioned alkaline matter acid-base reaction can occur for the acid of generation, and it is swift in response, so as to largely accelerate Cl2Redox reaction speed, while consume pH indicator local environments in alkaline matter, so as to change the pH value of indicator local environment so that the color of pH indicator changes, and improves to Cl2Detection sensitivity.In addition, pass through the addition of alkaline matter, environment residing for pH indicator can be adjusted near the catastrophe point slightly alkalescence of its color change so that when being contacted with acidic materials color change easily occurs for the color of indicator, so as to further increase detection sensitivity.
Description
Technical field
The present invention relates to the regulation of gas sensor detection sensitivity, specifically by pH
Being added in indicator can be with Cl2Occurs the alkaline matter of redox reaction, this not only can be with
Accelerate Cl2The speed of redox reaction, additionally it is possible to the immobilized pH indicator in matrix
The pH value of local environment is adjusted, so that the pH value of the immobilized indicator in matrix
Catastrophe point in color change so that indicator is to Cl2Detection sensitivity greatly improve.
Background technology
Chlorine is industrial widely used gas, and more than 60% commercial chemicals are produced at it
During to use chlorine, such as various chlorinated solvents, refrigerant, scattered propellant, detergent,
In disinfectant, the industrial production of dyestuff etc..Meanwhile, chlorine is also a kind of hypertoxic gas, even if
(it is less than 3mg/m in low concentration3) under, during human body Long Term Contact chlorine, it also can seriously stimulate people
Respiratory mucosa and eye mucous membranes, cause the pulmonary ventilation obstacle of contactee, bronchitis,
Toxic pulmonary edema and eyeball are burnt.International Health WSO announces harmless standard：In chlorine
Gas concentration is 3mg/m3Environment in time must not exceed 10min；Not as defined in China
It is respectively with chlorine maximum permissible concentration under environment：It is 3mg/m in operating environment air3,
It is 0.09mg/m in living environment3(per day).And about 9-15 is cut off from smell of the people to chlorine
mg/m3, this is significantly larger than harmless standard.Therefore, produced in industrial area or be possible to suitable
Implement real-time, detection on the spot to the chlorine in air and be very important in the living area of harm.Mesh
Before, temporarily it disclosure satisfy that above-mentioned requirements without convenient and effective laboratory analysis methodologies.
Photochemistry colorimetric method is simple to operate because of its, with low cost and extensive pass by scientists
Note.Due to Cl2With stronger oxidisability, therefore colored indicator can be aoxidized, make finger
Show that the color of agent is bleached., just can be to Cl by simple colorimetric method in theory2Enter
Row detection.But because the speed of the reaction is slower, it is relatively low to directly result in detection sensitivity, it is difficult to
Reach the test limit of international regulations.Due to Cl2Can occur in the presence of water redox
Hydrolysis generates two kinds of acid of HCl and HClO, it is possible to pass through colorimetric with pH indicator
Method is detected to it, particularly in the presence of having alkali, and HCl and HClO are sent out with alkali
Raw acid-base reaction is so as to accelerate Cl2With the redox reaction speed of water, while consuming finger
Show the alkali in agent local environment so that the pH value of indicator local environment changes, so that
Improve the detection sensitivity of indicator；In addition, being carried out by the amount of the alkaline matter to addition
Regulation, can make the pH value of indicator local environment in the catastrophe point meta-alkalescence of its color change
Near, so that the color of indicator easily changes and further improves pH indicator
To Cl2Detection sensitivity.
The content of the invention
Promoted it is an object of the invention to provide one kind by adding alkaline matter in pH indicator
Enter Cl2The progress of redox hydrolysis, by redox reaction product HCl, HClO
With the neutralization of alkaline matter, the pH value of indicator local environment is reduced, and add by adjusting
The amount of alkaline matter come control it is immobilized after indicator local environment pH value to its color change
Catastrophe point meta-alkalescence near, so as to improve indicator to Cl2Detection sensitivity method.
To achieve the above object, the technical solution adopted by the present invention is：
Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity, by adding
Can be with Cl2The alkaline matter of acid-base reaction occurs for hydrolysate HCl and HClO, and passes through
It is the indicator color that the addition of alkaline matter, which is adjusted, come the pH value after causing indicator immobilized
Near the catastrophe point of change, the pH value of indicator color change catastrophe point is A, then immobilized
The pH value of indicator local environment in matrix is A+0.01 to A+0.5, is finally prepared into
To for detecting Cl2Colorimetric gas sensor.
The solution for immobilized indicator is silica gel sol gel solution, and preparation method is：
The synthesis of silica gel collosol and gel：
Silicone agent：Ethylene glycol monomethyl ether：Propylene glycol methyl ether acetate：Organic solvent：Catalysis
Agent：Surfactant：Water is with 1：2-4：1-2：0.2-0.8：0.1-0.8：0.005
- 0.04：0.5-1 volume ratios are mixed, and 35-85 DEG C of stirring is hydrolyzed 1-8 hours, obtains silica gel
Sol gel solution.
Described silicone agent includes：Tetramethoxy-silicane, tetraethoxysilane, methyl three
Methoxy silane, MTES, normal octane triethoxysilane, (3- sulfydryls third
Base) trimethoxy silane, (3- aminopropyls) triethoxysilane, phenyl triethoxysilane, (3-
Chloropropyl) trimethoxy silane, the one or two or more kinds in trim,ethylchlorosilane；
Described organic solvent is toluene, dimethylbenzene, hexamethylene, chloroform, 1,2- bis-
Chloroethanes, tetrahydrofuran, dimethyl sulfoxide, ethanol, acetone, methanol, dimethylformamide,
One or two or more kinds in acetic acid, 1- propyl alcohol, n-hexane or acetonitrile；Catalyst is 0.1-1M
Hydrochloric acid or one kind in nitric acid or two kinds；Surfactant is lauryl sodium sulfate, 12
Sodium alkyl benzene sulfonate, cetyl trimethylammonium bromide, polysorbas20, L7001, Span 60,
One or two or more kinds in triton x-100, Span 80 and sodium carboxymethylcellulose.
The alkali for being used to adjust immobilized indicator solution pH environment is sodium hydroxide, hydroxide
One or two or more kinds in potassium, sodium carbonate, potassium carbonate, TBAH, ammoniacal liquor.
The indicator be pH indicator, including Congo red, methyl red, chlorophenol red,
Cresol red, nitro-nitrogen yellow, soap Huang, bromophenol blue, bromthymol blue, thymol blue, bromine cresols
One kind in green, bromocresol purple, m-cresol purple, methyl orange, fluorescein, alizarin or two kinds with
On.
The preparation process of the sensor is：1mL is added in 2-15mg indicator to consolidate
The solution of indicator is carried, then, the solution for adding alkaline matter adjusts the pH value of indicator,
Ultrasonic dissolution, takes solution drop coating in matrix, the lower drying at room temperature of nitrogen protection is standby；Wherein
The addition of alkaline matter is determined by the pH of indicator color change point.
The matrix for immobilized indicator is porous filter paper, nitric acid-acetic acid composite fibre
Cellulose ester film, polyvinylidene fluoride film, poly tetrafluoroethylene, and non-porous poly terephthalic acid second
One kind in diol ester film, polycarbonate membrane, polyethylene film, polychloroethylene film and polypropylene screen
Or more than two kinds.
The catastrophe point of the indicator color change refer to when pH value be more than or less than the value when,
Significant change takes place in the color of pH indicator.
The invention has the advantages that
1st, the Bio-sil colloidal sol coacervation material in the present invention can carry out effectively solid to indicator
Carry, formed after silica gel, with very big specific surface area, meanwhile, the acidproof alkali ability phase of silica gel
To relatively strong, and translucency is good, and stability is high, therefore arrives base by indicator is immobilized from the material
The specific surface area that indicator is contacted with gas can not only be increased in matter, improve what gas was detected
Sensitivity, while the stability of immobilized rear indicator can also be improved, when extending the preservation of sensor
Between, provide possibility for the commercialization of sensor.
2nd, by adding alkaline matter, Cl is accelerated2The speed of redox hydrolysis,
So that the pH value reduction of indicator local environment, causes the color of indicator to change；
By the addition for controlling alkaline matter so that the indicator local environment after immobilized is indicator
Near the catastrophe point meta-alkalescence of color change so that the minor variations of pH value and cause indicator
Color changes a lot, so as to greatly improve indicator to Cl2Detection sensitivity.
3rd, the sensor not only low cost, and simple to operate prepared using immobilized method,
It is easy to field assay to detect.
Brief description of the drawings
Fig. 1 is that indicator chlorophenol red and bromocresol purple add in for immobilized indicator solution
Enter or be added without the sensor prepared in the case of two kinds of alkaline matter with 300mL/min's
Flow velocity is passed through concentration for 10ppm, and humidity is 30% Cl2Passed in the case of sensor 3min
The response condition figure of sensor；
Fig. 2 is that indicator nitro-nitrogen yellow is added or is added without in for immobilized indicator solution
It is 10ppm that the sensor prepared in the case of two kinds of alkaline matter, which is put into equipped with concentration, wet
Spend the Cl for 30%2Closed container in 3min sensors response condition figure；
Fig. 3 is that indicator cresol red is adding alkaline matter regulation pH value to the change of indicator color
The sensor prepared in the case of the catastrophe point slight alkali environment of change is 30% to humidity, dense
The Cl spent between 3-5.5ppm2Response and standard concentration curve figure.
Embodiment
Embodiment 1
Weigh two kinds of indicator chlorophenol reds and each two parts of bromocresol purple, every part of 5mg, Ran Houxiang
1mL sol gel solutions are separately added into every part of indicator, and (preparation method of collosol and gel is：
Tetraethoxysilane：Normal octane triethoxysilane：Ethylene glycol monomethyl ether：Propylene glycol monomethyl ether acetic acid
Ester：Toluene：0.1M hydrochloric acid：Polysorbas20：Water is with 0.5：0.5：3：1.5：0.5：0.4：
0.02：1 volume ratio mixes to obtain 10mL solution, and water at normal temperature solution 16 hours obtains silica gel colloidal sol
Gel solution), in addition, adding 40 microlitres of 0.5M sodium carbonate liquor into portion, surpass
Sound dissolves, and draw each 1 microlitre of drop coating of different indicator solutions respectively with liquid-transfering gun is in aperture
On 0.22 micron of poly tetrafluoroethylene, the lower room temperature of nitrogen protection is kept in dark place, standby, takes a little
There is the film of indicator, inclosure is left in the transparent plastic capsule of air inlet/outlet, so as to can use
In Cl2The sensor of detection.A sensor prepared is taken, is obtained and sensed using scanner
The priming color picture of device, being then passed through concentration from air admission hole by 300mL/min of flow velocity is
10ppm, humidity is 30% Cl2, sensor is taken with scanner again after 3 minutes
Color；Utilize Photoshop softwares pair and Cl2The color of indicator is digitized before and after reaction,
The value after three passage digitlizations of RGB is extracted, and subtractive is carried out to the rgb value of acquisition,
So as to obtain the Cl that concentration is 10ppm2Prepared with two kinds of indicator under different pH condition
Color change value △ R, △ G and the △ B of obtained sensor, and utilize formulaCalculating obtains Cl2Color change value before and after reaction.
Its result is as shown in figure 1, from figure 1 it appears that the plus sensor that is prepared after alkali
Detection sensitivity apparently higher than not plus alkali sensor.
Embodiment 2
Two parts of indicator nitro-nitrogen yellow is weighed, then every part of 2mg distinguishes into every part of indicator
Adding 1mL sol gel solutions, (preparation method of collosol and gel is：Tetraethoxysilane：
Normal octane triethoxysilane：Ethylene glycol monomethyl ether：Propylene glycol methyl ether acetate：Chloroform：
0.1M hydrochloric acid：Neopelex：Water is with 0.5：0.5：3：1.5：0.5：0.4：
0.02：1 volume ratio mixes to obtain 10mL solution, and water at normal temperature solution 16 hours obtains silica gel colloidal sol
Gel solution), in addition, 10 microlitres of 0.1M potassium hydroxide solution is added into portion,
Ultrasonic dissolution, each 1 microlitre of drop coating of different indicator solutions is drawn with liquid-transfering gun in aperture respectively
For on 0.22 micron of poly tetrafluoroethylene, the lower room temperature of nitrogen protection is kept in dark place, so that
To available for Cl2The sensor of detection.Used time takes out sensor, and it is obtained using mobile phone photograph
Priming color picture, is then put into Cl by sensor2Concentration for 10ppm closed container in,
Taken out after 2min, carried out taking pictures again with mobile phone obtaining and Cl2Sensor after reaction
Color picture；With Photoshop softwares to sensor and Cl2Color before and after reaction enters line number
Word, extracts the rgb value after digitlization, and carries out subtractive to the rgb value of acquisition, so that
Color change value △ R, △ G, △ B before and after being reacted, then use formulaCalculating is obtained and Cl2Color change value before and after reaction, its
Color change situation is shown in Fig. 2.From figure 2 it can be seen that nitro-nitrogen yellow adds the biography that alkali is prepared
Sensor is 10ppm to concentration, is the Cl to 30%2With good response, but it is not added with alkali
Poor effect.
Embodiment 3
Indicator cresol red 5mg is weighed, 1mL collosol and gels are then added into indicator molten
(preparation method of collosol and gel is liquid：Tetraethoxysilane：Normal octane triethoxysilane：
Ethylene glycol monomethyl ether：Propylene glycol methyl ether acetate：Acetone：0.1M nitric acid：Span 80：Water with
0.5：0.6：3.5：1.4：0.45：0.35：0.03：1 volume ratio mixes to obtain 10mL solution,
Water at normal temperature solution 16 hours, obtains silica gel sol gel solution), ultrasonic dissolution uses liquid-transfering gun
1 microlitre of drop coating of indicator solution is drawn on filter paper, the lower room temperature of nitrogen protection is kept in dark place, standby
With, the filter paper for a little having indicator is taken, inclosure is left in the transparent plastic capsule of air inlet/outlet, from
And obtain can be used for Cl2The sensor of detection.The sensor prepared is taken, is obtained using scanner
The priming color picture of sensor is taken, then flow velocity is each led into from air admission hole for 300mL/min,
Concentration be 3,3.5,4.5,5,5.5ppm Cl2, again with scanner to passing after 2 minutes
Sensor carries out taking color；Utilize Photoshop softwares pair and Cl2The color of indicator before and after reaction
It is digitized, extracts the rgb value after digitlization, and subtractive is carried out to the rgb value of acquisition,
So as to obtain the Cl of various concentrations2With color change value △ R, the △ G of sensor response and
△ B, and utilize formulaCalculating obtains Cl2Face before and after reaction
Color change value.As a result as shown in figure 3, prepare sensor to concentration between 3-5.5ppm
Cl2With good linear relationship R2=0.9933.
Because chlorine is having H2Redox hydrolysis can occur in the presence of O
HCl and HClO is generated, sour generation can be detected using pH indicator, meanwhile,
There are NaOH, KOH, Na2CO3、K2CO3In the presence of alkaline matter, due to generation
With above-mentioned alkaline matter acid-base reaction can occur for acid, and be swift in response, so that largely
Accelerate Cl2Redox reaction speed, while consume pH indicator local environments in
Alkaline matter, so as to change the pH value of indicator local environment so that pH indicator
Color changes, and improves to Cl2Detection sensitivity.In addition, passing through alkaline matter
Add, the environment residing for pH indicator can be adjusted to the catastrophe point slightly alkali to its color change
Near property so that color change easily occurs when being contacted with acidic materials for the color of indicator,
So as to further increase detection sensitivity.
Claims (9)
1. add alkali to improve Colorimetric gas sensor to Cl2The method of detection sensitivity, passes through
Addition can be with Cl2The alkaline matter of acid-base reaction occurs for hydrolysate HCl and HClO, and
PH value after causing indicator immobilized by adjusting the addition of alkaline matter is the indicator
Near the catastrophe point of color change, the pH value of indicator color change catastrophe point is A, then
The pH value for the indicator local environment being immobilized in matrix be A+0.01 to A+0.5, final system
It is standby to obtain being used to detect Cl2Colorimetric gas sensor.
2. according to the method described in claim 1, it is characterised in that：It is described to be used for immobilized refer to
The solution for showing agent is silica gel sol gel solution, and preparation method is：
The synthesis of silica gel collosol and gel：
Silicone agent：Ethylene glycol monomethyl ether：Propylene glycol methyl ether acetate：Organic solvent：Catalysis
Agent：Surfactant：Water is with 1：2-4：1-2：0.2-0.8：0.1-0.8：0.005
- 0.04：0.5-1 volume ratios are mixed, and 35-85 DEG C of stirring is hydrolyzed 1-8 hours, obtains silica gel
Sol gel solution.
3. method according to claim 2, it is characterised in that：Described siloxanes examination
Agent includes：Tetramethoxy-silicane, tetraethoxysilane, MTMS, methyl three
Ethoxysilane, normal octane triethoxysilane, (3- mercaptopropyis) trimethoxy silane, (3-
Aminopropyl) triethoxysilane, phenyl triethoxysilane, (3- chloropropyls) trimethoxy silane,
One or two or more kinds in trim,ethylchlorosilane.
4. method according to claim 2, it is characterised in that：Described organic solvent
For toluene, dimethylbenzene, hexamethylene, chloroform, 1,2- dichloroethanes, tetrahydrofuran,
Dimethyl sulfoxide, ethanol, acetone, methanol, dimethylformamide, acetic acid, 1- propyl alcohol, just oneself
One or two or more kinds in alkane or acetonitrile；Catalyst is in 0.1-1M hydrochloric acid or nitric acid
It is a kind of or two kinds；Surfactant is lauryl sodium sulfate, neopelex, ten
Six alkyl trimethyl ammonium bromides, polysorbas20, L7001, Span 60, triton x-100, department
One or two or more kinds in class 80 and sodium carboxymethylcellulose.
5. according to the method described in claim 1, it is characterised in that：It is described to be used to adjust solid
Carry indicator solution pH environment alkali for sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate,
One or two or more kinds in TBAH, ammoniacal liquor.
6. according to the method described in claim 1, it is characterised in that：The indicator is pH
Indicator, including Congo red, methyl red, chlorophenol red, cresol red, nitro-nitrogen yellow, soap it is yellow,
Bromophenol blue, bromthymol blue, thymol blue, bromocresol green, bromocresol purple, m-cresol purple,
One or two or more kinds in methyl orange, fluorescein, alizarin.
7. according to the method described in claim 1, it is characterised in that：The system of the sensor
It is for process：The solution of the immobilized indicator of 1mL is added in 2-15mg indicator, so
Afterwards, the solution for adding alkaline matter adjusts the pH value of indicator, and ultrasonic dissolution takes solution to drip
It is applied in matrix, the lower drying at room temperature of nitrogen protection is standby；The addition of wherein alkaline matter is more
It is few to be determined by the pH of indicator color change point.
8. the method according to claim 1 and 7, it is characterised in that：It is described to be used for admittedly
It is porous filter paper, nitric acid-acetic acid mixed cellulose ester membrane, poly- inclined fluorine to carry the matrix of indicator
Vinyl film, poly tetrafluoroethylene, and non-porous polyethylene terephthalate film, poly- carbon
One or two or more kinds in acid esters film, polyethylene film, polychloroethylene film and polypropylene screen.
9. the method according to claim 1 or 7, it is characterised in that：The indicator
The catastrophe point of color change refer to when pH value be more than or less than the value when, the face of pH indicator
Significant change takes place in color.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610078537.9A CN107037177A (en) | 2016-02-03 | 2016-02-03 | Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610078537.9A CN107037177A (en) | 2016-02-03 | 2016-02-03 | Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity |
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| CN201610078537.9A Pending CN107037177A (en) | 2016-02-03 | 2016-02-03 | Plus alkali improves Colorimetric gas sensor to Cl2The method of detection sensitivity |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166838A (en) * | 2021-11-18 | 2022-03-11 | 潍坊易北特健康食品有限公司 | Yoghourt fermentation degree indicator and preparation method thereof |
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