CN105675599B - A kind of photochemical method of recyclable detection nitrogen oxides - Google Patents
A kind of photochemical method of recyclable detection nitrogen oxides Download PDFInfo
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Abstract
The present invention discloses a kind of photochemical method of recyclable detection nitrogen oxides, barium doping titanium dioxide nano crystalline substance solution is added in methylene blue solution and is sufficiently mixed and obtains mixed solution with water constant volume, then the optical filter of irradiation and use≤365nm wavelength filters under mercury lamp, it reacts under agitation, mixed solution takes off into colourless, obtains colourless light-catalyzed reaction system solution；The sodium nitrite standard solution of various concentration is added dropwise in above-mentioned colourless photocatalytic system solution；System becomes blue, is fitted concentration absorbance quantitative relationship equation；According to the concentration absorbance quantitative relationship equation drafted, the concentration of nitrogen oxides in sample to be tested is calculated.The detection method of the present invention has the characteristics that simple, easy to operate, at low cost；Acid photocatalytic system is constructed, detection sensitivity is high；The colourless retention time that light-catalyzed reaction system solution is placed in air is 15~30min, and accuracy is high；Recycle number >=45 time.
Description
Technical field
The invention belongs to chemical analysis test fields, and in particular to a kind of photochemistry side of recyclable detection nitrogen oxides
Method.
Background technology
Nitrogen oxides based on nitric oxide and nitrogen dioxide is the important original to form photochemical fog and acid rain
Cause.Nitrogen oxides in vehicle exhaust irradiates the react toxic smog to be formed, referred to as light with hydrocarbon through ultraviolet light
Chemical fumes.Photochemical fog has special odor, stimulates eyes, injures plant, and can reduce atmospheric visibility.In addition,
Nitrogen oxides reacts the nitric acid of generation with the water in air and nitrous acid is the ingredient of acid rain.The main source of nitrogen oxides in air
The conversion of nitrogenous compound in the burning of fossil fuel and the burning of plant and agricultural land soil and animal excrements.Greatly
Gas is precious resources for the survival of mankind, and the destruction of Atmosphere environment resource is a kind of irreversible procedure, restores good air
Quality pays more costs than Air Pollution prevention and control.It prevents and remedies pollution it is necessary to understand pollution first, correctly to understand dirt
Contaminate object from where, what ingredient is, pollutant load how many, careful, conscientious and extensive investigations are made to everything
After research, method and the measure of prevention can be just made, extensive environment measuring or monitoring will be carried out thus.With science skill
The progress of art and the tremendous development of all kinds of subjects, substance detection means are also greatly enriched and are developed, accuracy of detection and
There has also been qualitative leaps for reliability.At present, many gas detection methods have been derived according to the chemically and physically characteristic of gas.Such as
Colorimetric method：It is much like that the measuring method and chemical test paper measure liquid pH value method.Gas is passed through during measurement and has solution examination
In the colorimetric cylinder of agent, then it is tested gas and is chemically reacted with solution, solution colour can change in reaction process, different
Gas concentration solution different colors can be presented, control color table can roughly estimate the concentration and type of gas.It should
Measuring method applicability is very wide, but precision is relatively low, is suitable for some gas detections without particular instrument detection method；It is based on
Semiconductor technology sensor：The operation principle of the sensor is the chemistry based on semi-conducting material, biology and physical characteristic.So
It can be classified as chemical-sensitive semiconductor transducer, bio-sensing semiconductor transducer and physics sensitive semiconductor sensor.Its
Available for the detection of imflammable gas, for certain pernicious gases, detection limit is up to ppm stratification levels；Electrochemical sensor：Electricity
The principle of chemical sensor is based on tested gas generation oxidation or reduction reaction and generates the electricity directly proportional to gas concentration
Signal.Electrochemical sensor mensuration be at present be applied to portable gas detector in detection pernicious gas it is most common and most into
Ripe detection technique, its main feature is that it is small, power consumption is small, it is linear and reproducible, last a long time, but there are cross jamming disadvantages
End；Non-dispersion infrared absorption process：According to tested gas to the absorption characteristic of infrared light, absorbed amount of infrared light is detected, i.e.,
The parameters such as the concentration of tested gas can be calculated.This method measuring range is big, and precision is high, and can measure multiple gases simultaneously,
And there is no cross jamming effect, but involve great expense；The surface acoustic wave method and gas chromatography-mass spectrum that also latest developments are got up
Combination method, quartz resonance gas sensor mensuration etc., above-mentioned measuring method all achieves certain effect.But due to quilt
Survey gaseous species are various, and chemical property difference is very big, and a kind of instrument can be not only accurate, economical but also be quickly solved currently not yet
The test problems of specific gas, it is desirable that have the higher response sensitivity even more extremely difficult to multiple gases.
Invention content
Goal of the invention：Present invention aims in view of the deficiencies of the prior art, provide a kind of structure simplicity, quick, Gao Ling
The photochemical method of sensitivity, high specific and environmentally friendly recyclable detection nitrogen oxides.
Technical solution：A kind of photochemical method of recyclable detection nitrogen oxides of the present invention, it is characterised in that packet
Include following steps：
(1) light-catalyzed reaction system solution is prepared：The barium doping titanium dioxide nano crystalline substance of a concentration of 18~40mg/mL is molten
Liquid by volume 8~12:1 is added to and is sufficiently mixed in the methylene blue solution of 0.05mol/L~0.015mol/L and is determined with water
Hold to 15mL~35mL and obtain mixed solution, above-mentioned mixed solution is then transferred to photocatalytic system, is irradiated simultaneously under mercury lamp
It is filtered, reacted under agitation, mixed solution takes off into colourless after 3~10s, obtains colourless with the optical filter of≤365nm wavelength
Light-catalyzed reaction system solution；
(2) oxides of nitrogen gas is passed through sodium hydroxide solution, generates the sodium nitrite standard solution of various concentration, and adjusted
PH value is saved to neutrality, the salting liquid of the normal concentration is added dropwise in above-mentioned colourless light-catalyzed reaction system solution, the system
Moment becomes au bleu, and the absorption spectrum change curve of solution, is then fitted concentration-absorbance quantitative relationship after detection each group becomes basket
Equation；
(3) according to the concentration-absorbance quantitative relationship equation drafted, the concentration of nitrogen oxides in sample to be tested is calculated.
Further, the volume of barium doping titanium dioxide nano crystalline substance solution described in step (1) is 300~700 μ L.
Further, the power of mercury lamp described in step (1) is 300~500W.
In this method, the colourless retention time that step (1) the light-catalyzed reaction system solution is placed in air is 15
~30min.
Further, a concentration of 0.8~1.2mmol L of sodium hydroxide described in step (2)-1。
Further, to avoid interference of the dissolved oxygen to test system, before detection to the colourless light-catalyzed reaction
System solution and the salting liquid of the neutrality advertise method using nitrogen and remove dissolved oxygen.
Further, for gas is avoided to flow through havoc light-catalyzed reaction system solution and prevents letting nitrogen in and deoxidizing overlong time
Solution becomes blue again, influences testing result, and the air velocity that the nitrogen advertises nitrogen in method is controlled in 300~700ml min-1
In the range of.
In this method, the light-catalyzed reaction system solution recycles number >=45 time.
Advantageous effect：(1) present invention is, selection nanocrystalline based on ultraviolet excitation functional form barium doped nano titanium dioxide
Property real estate third contact of a total solar or lunar eclipse electronics, is quickly restored to colourless reduced form methylene blue by blue methylene blue solution, is added dropwise in this system
The sodium hydroxide neutral salt solution of nitrogen oxides, colourless reduced form methylene blue solution momentary recovery blue, nitrogen oxides
Concentration is bigger, and blue is deeper, measures the concentration of nitrogen oxides accordingly, which has the spies such as simple, easy to operate, at low cost
Point；(2) this method, which constructs acid photocatalytic system, is beneficial to the raising of nitrogen oxides, and further improve photochemical
The detection sensitivity of method；(3) the colourless retention time that light-catalyzed reaction system solution is placed in air in this method is 15
~30min, time period carry out the measure of nitrous oxides concentration enough, avoid detecting caused by system self-recovery blue
Error, it is ensured that the accuracy of detection；(4) this method using the methylene blue that is easy to switch between oxidation state and reduction-state as
Probe and beacon, this detection architecture can be recycled, coloration can 100% recovery, recycle number >=45 time, improve light and urge
The recycling number of agent reduces testing cost.
Description of the drawings
Fig. 1 is the structure schematic diagram that nitrogen oxides photochemical method detects in the present invention；
Fig. 2 is the abosrption spectrogram before and after light-catalyzed reaction system solution light color in embodiment 1；Wherein a is ultraviolet
Abosrption spectrogram before illumination, b are the abosrption spectrogram after ultraviolet lighting；
Fig. 3 is that reduction-state methylene blue colourless in embodiment 1 restores to absorb light to the time change of the oxidation state of blue
Spectrogram；
Fig. 4 is the absorption spectrum change curve changed in embodiment 1 with sodium nitrite concentration of standard solution；Illustration is fitting
Concentration afterwards-absorbance quantitative relationship curve, the concentration of Sodium Nitrite standard solution are followed successively by 0.05,0.1,0.5,1,5,
25,50 μm of ol L-1；
Fig. 5 is common gas in embodiment 1 to the interference block diagram of detection architecture；Wherein, interference gas is 10 times of oxygen
Gas, 100 times of sulfur dioxide, 1000 times of carbon monoxide, carbon dioxide, nitrogen, hydrogen sulfide；
Fig. 6 is cycle-index-absorbance figure of light-catalyzed reaction detection architecture in embodiment 1.
Specific embodiment
Technical solution of the present invention is described in detail below by attached drawing, but protection scope of the present invention is not limited to
The embodiment, method is conventional method unless otherwise specified in embodiment, and the reagent used is normal unless otherwise specified
It advises commercially available.
Embodiment 1：
(1) light-catalyzed reaction system solution is prepared：By 500 μ L, the barium doping titanium dioxide nano crystalline substance solution of 28.5mg/mL
It is added in the methylene blue solution of 50 μ L, 0.01mol/L to be sufficiently mixed and be settled to 25mL with water and obtains mixed solution, then
Above-mentioned mixed solution is transferred to photocatalytic system, irradiated under 300W mercury lamps and is filtered with the optical filter of 365nm wavelength, is being stirred
It is reacted under the conditions of mixing, mixed solution takes off into colourless after 5s, obtains colourless light-catalyzed reaction system solution；Take the light that part is colourless
Catalystic converter system solution observes its color-recovering time, and timing measures the change curve of m- trap at that time；
(2) oxides of nitrogen gas is passed through 1mmol L-1Sodium hydroxide solution, generate the sodium nitrite mark of various concentration
Quasi- solution, and pH value is adjusted to neutrality, the concentration of sodium nitrite standard solution is respectively 0.05,0.1,0.5,1,5,25,50 μ
mol L-1, first progress nitrogen is advertised respectively for salting liquid and colourless light-catalyzed reaction system solution to the neutrality, removes solution
Interior dissolved oxygen, nitrogen flow rate is 500ml min during nitrogen is advertised-1, then salting liquid is added dropwise to colourless photocatalysis
In reaction system solution, which becomes au bleu, and the absorption spectrum change curve of solution, then intends after detection each group becomes basket
Close concentration-absorbance quantitative relationship equation；
(3) according to the concentration-absorbance quantitative relationship equation drafted, the concentration of nitrogen oxides in sample to be tested is calculated.
Fig. 1 is the structure schematic diagram that nitrogen oxides photochemical method detects in the present invention, and this method is based on ultraviolet excitation
Functional form barium doped nano titanium dioxide is nanocrystalline, selectively generates photoelectron, quickly restores blue methylene blue solution
To colourless reduced form methylene blue, using being not easy to restore after colour fading to the principle of former blue, we construct photochemical method detection
The sodium hydroxide neutral salt solution of nitrogen oxides, colourless reduced form methylene is added dropwise in the new method of nitrogen oxides in this system
Blue solution momentary recovery blue, the concentration of nitrogen oxides is bigger, and blue is deeper, measures the concentration of nitrogen oxides accordingly；
Fig. 2 is the abosrption spectrogram before and after light-catalyzed reaction system solution light color in the present embodiment；Wherein a is ultraviolet
Abosrption spectrogram before illumination, b are the abosrption spectrogram after ultraviolet lighting；As can be seen from Figure, it is penetrated by outer illumination
Before catalysis, the light absorption to 400~700nm wave bands of mixed solution is apparent, with significantly absorption peak, solution show as indigo plant
Color；By after ultraviolet light is catalyzed, mixed solution becomes colorless, the mixed solution pair after illumination it can be seen from curve b
The light of 400~700nm wave bands does not absorb substantially, thus proves, and after ultraviolet catalytic irradiates, mixed solution do not absorb 400~
The light of 700nm wave bands, becomes colorless；
Fig. 3 is that reduction-state methylene blue colourless in the present embodiment restores to absorb light to the time change of the oxidation state of blue
Spectrogram；Reduction in Air state methylene blue need to can just be fully returned to primitive color through 480min as can be seen from Figure, preceding
20min does not see its color change visually, and nitrogen oxides can fully be reacted with reduction-state methylene blue very much in 20 minutes,
So as to avoid influence of the oxygen to test system in air；
Fig. 4 is the absorption spectrum change curve changed in the present embodiment with sodium nitrite concentration of standard solution；Illustration is intends
Concentration-absorbance quantitative relationship curve after conjunction, the concentration of Sodium Nitrite standard solution are followed successively by 0.05,0.1,0.5,1,
5,25,50 μm of ol L-1；By test result, the raising of solution absorbance sodium nitrite concentration of standard solution linearly improves, according to
Each test point can be fitted concentration-absorbance quantitative relationship equation.
Fig. 5 is common gas in the present embodiment to the interference block diagram of detection architecture；In order to prove the selectivity of this method,
We have investigated interference of the component common in flue gas to the detection architecture, the results showed that, 10 times of oxygen, 100 times of dioxy
Change sulphur, 1000 times of carbon monoxide, carbon dioxide, nitrogen, hydrogen sulfide do not form this detection architecture interference, and this method is with excellent
Good selectivity.
Fig. 6 is cycle-index-absorbance figure of light-catalyzed reaction detection architecture in embodiment 1, the results showed that 45 cycles
Still close to 100%, this method has excellent stability for the recovery of methylene blue absorbance afterwards.
Embodiment 2：
(1) light-catalyzed reaction system solution is prepared：By 300 μ L, the barium doping titanium dioxide nano crystalline substance solution of 18.5mg/mL
It is added in the methylene blue solution of 40 μ L, 0.005mol/L to be sufficiently mixed and be settled to 15mL with water and obtains mixed solution, so
Above-mentioned mixed solution is transferred to photocatalytic system afterwards, irradiated under 350W mercury lamps and is filtered with the optical filter of 254nm wavelength,
It is reacted under stirring condition, mixed solution takes off into colourless after 8s, obtains colourless light-catalyzed reaction system solution；Take part colourless
Light-catalyzed reaction system solution observes its color-recovering time, and timing measures the change curve of m- trap at that time；
(2) oxides of nitrogen gas is passed through 0.8mmol L-1Sodium hydroxide solution, generate the sodium nitrite of various concentration
Standard solution, and pH value is adjusted to neutrality, the concentration of sodium nitrite standard solution is respectively 0.05,0.1,0.5,1,5,25,50 μ
mol L-1, first progress nitrogen is advertised respectively for salting liquid and colourless light-catalyzed reaction system solution to the neutrality, removes solution
Interior dissolved oxygen, nitrogen flow rate is 300ml min during nitrogen is advertised-1, then salting liquid is added dropwise to colourless photocatalysis
In reaction system solution, which becomes au bleu, and the absorption spectrum change curve of solution, then intends after detection each group becomes basket
Close concentration-absorbance quantitative relationship equation；
(3) according to the concentration-absorbance quantitative relationship equation drafted, the concentration of nitrogen oxides in sample to be tested is calculated.
Obtained colourless light-catalyzed reaction system solution is after air is placed 25 minutes in the present embodiment, solution colour
Ability and sagacity becomes micro- blue, needs just can completely to become for 510 minutes former blue, and methylene blue absorbance after cycle detection 46 times
Recovery still close to 100%.
Embodiment 3：
(1) light-catalyzed reaction system solution is prepared：By 700 μ L, the barium doping titanium dioxide nano crystalline substance solution of 38.5mg/mL
It is added in the methylene blue solution of 60 μ L, 0.015mol/L to be sufficiently mixed and be settled to 35mL with water and obtains mixed solution, so
Above-mentioned mixed solution is transferred to photocatalytic system afterwards, irradiated under 500W mercury lamps and is filtered with the optical filter of 365nm wavelength,
It is reacted under stirring condition, mixed solution takes off into colourless after 10s, obtains colourless light-catalyzed reaction system solution；Take part colourless
Light-catalyzed reaction system solution observe its color-recovering time, and timing measures the change curve of m- trap at that time；
(2) oxides of nitrogen gas is passed through 1.2mmol L-1Sodium hydroxide solution, generate the sodium nitrite of various concentration
Standard solution, and pH value is adjusted to neutrality, the concentration of sodium nitrite standard solution is respectively 0.05,0.1,0.5,1,5,25,50 μ
mol L-1, first progress nitrogen is advertised respectively for salting liquid and colourless light-catalyzed reaction system solution to the neutrality, removes solution
Interior dissolved oxygen, nitrogen flow rate is 700ml min during nitrogen is advertised-1, then salting liquid is added dropwise to colourless photocatalysis
In reaction system solution, which becomes au bleu, and the absorption spectrum change curve of solution, then intends after detection each group becomes basket
Close concentration-absorbance quantitative relationship equation；；
(3) according to the concentration-absorbance quantitative relationship equation drafted, the concentration of nitrogen oxides in sample to be tested is calculated.
Obtained colourless light-catalyzed reaction system solution is after air is placed 15 minutes in the present embodiment, solution colour
Ability and sagacity becomes micro- blue, needs just can completely to become for 460 minutes former blue, and methylene blue absorbance after cycle detection 45 times
Recovery still close to 100%.
As described above, although the present invention has been represented and described with reference to specific preferred embodiment, must not explain
For to the limitation of itself of the invention.It, can be right under the premise of the spirit and scope of the present invention that appended claims define are not departed from
Various changes can be made in the form and details for it.
Claims (7)
1. a kind of photochemical method of recyclable detection nitrogen oxides, it is characterised in that include the following steps：
(1) by the barium doping titanium dioxide nano crystalline substance solution of a concentration of 18~40mg/mL by volume 8~12:1 is added to
Be sufficiently mixed in the methylene blue solution of 0.05mol/L~0.015mol/L and with water be settled to 15mL~35mL obtain mixing it is molten
Then above-mentioned mixed solution is transferred to photocatalytic system by liquid, the optical filter of the irradiation and use≤365nm wavelength filter under mercury lamp
Light reacts under agitation, and mixed solution takes off into colourless after 3~10s, obtains colourless light-catalyzed reaction system solution；
(2) oxides of nitrogen gas is passed through sodium hydroxide solution, generates the sodium nitrite standard solution of various concentration, and adjust pH
The salting liquid of the normal concentration is added dropwise in above-mentioned colourless light-catalyzed reaction system solution, the system moment by value to neutrality
Become au bleu, the absorption spectrum change curve of solution, is then fitted concentration-absorbance quantitative relationship side after detection each group becomes basket
Journey；
(3) according to the concentration of fitting-absorbance quantitative relationship equation, the concentration of nitrogen oxides in sample to be tested is calculated.
2. the photochemical method of recyclable detection nitrogen oxides according to claim 1, it is characterised in that：In step (1)
The volume of the barium doping titanium dioxide nano crystalline substance solution is 300~700 μ L.
3. the photochemical method of recyclable detection nitrogen oxides according to claim 1, it is characterised in that：In step (1)
The power of the mercury lamp is 300~500W.
4. the photochemical method of recyclable detection nitrogen oxides according to claim 1, it is characterised in that：In step (2)
A concentration of 0.8~1.2mmol L of the sodium hydroxide-1。
5. the photochemical method of recyclable detection nitrogen oxides according to claim 1, it is characterised in that：It is right before detection
The colourless light-catalyzed reaction system solution and the salting liquid of the neutrality advertise method using nitrogen and remove dissolved oxygen.
6. the photochemical method of recyclable detection nitrogen oxides according to claim 5, it is characterised in that：The nitrogen drum
The air velocity for blowing nitrogen in method is 300~700ml min-1。
7. the photochemical method of recyclable detection nitrogen oxides according to claim 1, it is characterised in that：Step (1) institute
That states light-catalyzed reaction system solution recycles number >=45 time.
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