CN102068954A - Method and device for photocatalytic reaction - Google Patents
Method and device for photocatalytic reaction Download PDFInfo
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- CN102068954A CN102068954A CN2009102382654A CN200910238265A CN102068954A CN 102068954 A CN102068954 A CN 102068954A CN 2009102382654 A CN2009102382654 A CN 2009102382654A CN 200910238265 A CN200910238265 A CN 200910238265A CN 102068954 A CN102068954 A CN 102068954A
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Abstract
The invention provides a photocatalytic reaction method, comprising the steps of: atomizing a solution or suspension containing a photocatalyst and a reactant to form mist; and leading the mist to be subjected to photocatalytic reaction by utilizing a light source. The invention also provides a photocatalytic reaction device, which comprises a reaction vessel, an atomizer arranged inside or outside the reaction vessel, a condensation sleeve communicated with the reaction vessel, and the light source used for photocatalytic reaction. By means of the method and the device, a gas-liquid interface is enlarged by changing the form of water, i.e. atomizing the liquid-phase solution of the catalyst, so as to reduce the escape path of hydrogen gas and effectively inhibit the occurrence of reverse reaction, meanwhile, because the scattering probability of light in the mist is increased and the effective absorption is enhanced, the light utilization rate and the catalytic efficiency of the photocatalyst are greatly improved.
Description
Technical field
The present invention relates to a kind of method and device that is used for light-catalyzed reaction, more specifically, relate to a kind of method and device that is used for photocatalytic hydrogen production by water decomposition and photocatalysis degradation organic contaminant.
Background technology
The energy and environment problem is that human society is realized two major issues that sustainable development must solve.At present, along with the exhaustion day by day of fossil energy and being on the rise of environmental problem, seeking the renewable new forms of energy of cleanliness without any pollution and the degraded of pollutant and reduce discharging extremely urgent.
In many new forms of energy, solar energy is subjected to extensive concern with its inexhaustible absolute predominance.In solar utilization technique, photocatalytic hydrogen production by water decomposition and photocatalysis degradation organic contaminant have great significance.Hydrogen Energy is a kind of cleaning, efficient, safety, can store, can transport, the reproducible energy, is the ideal substitute of fossil energy.Compare with traditional fossil feedstock hydrogen manufacturing, utilize solar energy and photochemical catalyst, realize that photocatalytic hydrogen production by water decomposition is the hydrogen manufacturing approach that cleans the most.Photocatalysis degradation organic contaminant is that photochemical catalyst is power with solar energy, is nontoxic small-molecule substance with poisonous and hazardous organic pollution oxidation Decomposition, make it can safety dumping in natural environment.In above-mentioned photocatalytic process, the operation principle of photochemical catalyst is that its absorption energy is excited greater than the photon of its energy gap, produce electron hole pair, electronics and hole are transported to catalyst surface, generate hydrogen and oxygen or generation with the material generation redox reaction that is adsorbed in catalyst surface and have the free radical of strong oxidizing property with organic pollution oxidative degradation.Such photochemical catalyst mostly is Powdered, generally is it to be dispersed to form suspension in the aqueous systems when characterizing photocatalysis efficiency, carries out catalytic reaction under illumination.Mainly be to improve photocatalysis efficiency at present: 1) improve the light absorption that is subjected to the energy gap restriction by following two kinds of approach; 2) suppress the compound of light induced electron hole.But for the absorptivity that how to improve light and suppress that back reaction (hydrogen of generation generates water with oxygen reaction) studies less.
(Catalysis Letters 1995 34:245-249) finds during to the influencing of photochemical catalyzing hydrogen generation efficiency at the research direction of illumination people such as S.Tabata, and light source is more than 10 times of hydrogen output from bottom incident from the hydrogen output of reactor head incident; People such as H.Kominami (Phys.Chem.Chem.Phys.2001,3:4102-4106) contrast light source incident from the side and also obtained similar result during from the hydrogen output of top incident, this explanation hydrogen mainly is to overflow from the water layer of gas-liquid interface part, and the hydrogen of liquid internal is owing to will just can enter gas phase through relatively long distance, the probability that back reaction takes place increases greatly, and is very limited to the contribution of actual hydrogen output.As seen this liquid phase suspension system is severely limited the output of hydrogen, even the hydrogen production efficiency of catalyst itself is very high, also have only hydrogen in the water layer of gas-liquid interface part to escape into and be collected utilization in the gas phase, and the hydrogen of liquid internal and oxygen major part consume because of compound, thereby influence hydrogen generation efficiency.In addition, the light transmission of liquid phase suspension is better, and the transmission and going out from liquid phase suspension of quite a few light is arranged, and can not effectively be absorbed by catalyst, and lower to the utilization rate of light, this has also just reduced photocatalysis efficiency.
Summary of the invention
Therefore, the light-catalyzed reaction method that the objective of the invention is to overcome prior art can not effectively suppress back reaction and the lower problem of light utilization efficiency, proposes higher light-catalyzed reaction method of a kind of effective inhibition back reaction and light utilization efficiency and the device that is used for this method.
To achieve these goals, the photocatalytic reaction device that the invention provides a kind of light-catalyzed reaction method and be used for this method.Wherein, light-catalyzed reaction method of the present invention comprises the steps:
The solution or the suspension atomization that 1, will contain photochemical catalyst and reactant form fog;
2, the fog generation light-catalyzed reaction that utilizes light source that step 1 is obtained.
According to method provided by the invention, wherein, described solution or suspension are to contain the reactant of light-catalyzed reaction and the solution or the suspension of photochemical catalyst, for example, for the reaction of photochemical catalyzing, described solution or suspension can be the aqueous solution or the suspension that contains the photochemical catalyst that is used for decomposition water; For the reaction of photocatalysis degradation organic contaminant, described solution or suspension can be for containing the photochemical catalyst that is used for degradable organic pollutant and the aqueous solution of organic pollution.
According to method provided by the invention, wherein, described photochemical catalyst can be any photochemical catalyst that is used for light-catalyzed reaction.In some embodiments of the present invention, this photochemical catalyst can or be used for the photochemical catalyst of photocatalysis degradation organic contaminant for the photochemical catalyst of hydrogen production by water decomposition.The example of such catalyst comprises, but be not limited to: metal oxide, metal sulfide, titanate, niobates, tantalates, tungstates, vanadate, zirconates, gallate, germanate, indate, stannate, stibate and by wherein several composite catalysts of forming or solid solution catalyst, and the above-mentioned catalyst of mix (metal-doped, nonmetal doping, metal and nonmetal codope) and support in the above-mentioned catalyst of co-catalyst one or more.
According to method provided by the invention, wherein, the method for described atomizing can be any method that makes the atomization of liquid of the prior art, for example, can use conventional ultrasonic atomizer, centrifugal turntable atomizer or other atomizing means to make described solution atomization.
According to method provided by the invention, wherein, described light source can be used for the light source of light-catalyzed reaction for any routine, for example, can be in xenon lamp, mercury lamp, halogen tungsten lamp, LED lamp and the sunshine one or more.According to method provided by the invention, wherein, utilize light source to make the method for described fog generation light-catalyzed reaction light source can be placed the optional position of fog, also light source can be placed the fog outside.
Method of the present invention can also be included in the process of light-catalyzed reaction, takes a sample, and analyzes the degree of carrying out of light-catalyzed reaction.Described sampling had both comprised takes a sample to reactant, also comprises product is taken a sample, and also comprises the mixture of reactant and product is taken a sample.Under the preferable case, determine the mode and the time of sampling according to concrete light-catalyzed reaction.For example, in the reaction of photochemical catalyzing, can every 0.1-20 hour to the gas sample in the reaction system, carry out chromatography, judge whether reaction finishes; In the reaction of photocatalysis degradation organic contaminant, can get the 0.5-10 ml soln every 5-120 minute and analyze, finish up to reaction.
In addition, according to the needs of concrete light-catalyzed reaction, method of the present invention can also comprise that the reaction vessel to holding described solution and/or described fog carries out vacuum pumping.
According to said method provided by the invention, the present invention also provides a kind of photocatalytic reaction device that is used for this method, and this device comprises:
Reaction vessel;
Place this reaction vessel interior or outside atomizer;
The condensation sleeve pipe that is connected with this reaction vessel; And
The light source that is used for light-catalyzed reaction.
According to device of the present invention, wherein, described reaction vessel can be the container that can be used for light-catalyzed reaction of any routine.According to concrete light-catalyzed reaction, described reaction vessel can be airtight (decompression or normal pressure), also can airtight (normal pressure) of right and wrong.There is no particular limitation to described reaction container materials in the present invention, and under the preferable case, for the ease of the state of observing response system, described reaction container materials is preferably glass, for the light-catalyzed reaction under the radiation of visible light, more preferably Pyrex glass; For the light-catalyzed reaction under the UV-irradiation, more preferably quartz glass.
Described atomizer be used for will contain the solution or the suspension atomization of reactant and photochemical catalyst form fog, there is no particular limitation to the kind of atomizer and model in the present invention, for example, can be the ultrasonic atomizer that is purchased, centrifugal turntable atomizer etc.Described atomizer can place the inside of reaction vessel, also can place the outside of reaction vessel.Wherein, when placing reaction vessel interior, described atomizer can contact with the inner bottom surface of reaction vessel, also can not contact, as long as this atomizer all is arranged in described solution or floating suspension; When placing reaction vessel outside, described atomizer can contact with the outer bottom surface of reaction vessel, perhaps and the distance between the outer bottom surface of reaction vessel make the liquid in the reaction vessel to atomize, but, in order to make atomizer reach best atomizing effect, under the preferable case, when placing reaction vessel outside, atomizer contacts with the outer bottom surface of reaction vessel.
Described condenser jacket pipe is used for fog is condensed into the droplet condensing reflux to reaction vessel, can be the condensation sleeve pipe with water inlet and delivery port of any routine.About the quantity of condensation sleeve pipe, there is no particular limitation in the present invention, can be preferably 1-4, for example, can be 2.
According to device provided by the invention, wherein, described light source can be used for the light source of light-catalyzed reaction for any routine, for example, but is not limited to: xenon lamp, mercury lamp, halogen tungsten lamp, LED lamp and sunshine.
Device provided by the invention can also comprise and is used to take out the sampling portion of sample segment to analyze, thereby determine the degree that light-catalyzed reaction is carried out.The present invention is not particularly limited the quantity and the position of described sampling portion, can determine according to different light-catalyzed reactions.For example, for the reaction of photochemical catalyzing, described sampling portion can be positioned at the outlet top of condenser pipe, can directly link to each other with condenser pipe or link to each other with condenser pipe by conduit; For the reaction of photocatalysis degradation organic contaminant, analyze owing to need to take out fluid sample, therefore described sampling portion can be positioned at bottom one side of reaction vessel, device for example shown in Figure 2, wherein 5 ' is sampling portion.
In addition, according to the needs of concrete light-catalyzed reaction, device of the present invention can also comprise vacuum extractor.
Need to prove, those skilled in the art can expect that by reading the disclosed content of the application the application of light-catalyzed reaction method provided by the invention and device is not limited only to conventional light-catalyzed reaction, but also can be applied to association areas such as the purification of air and chemical defence.
In light-catalyzed reaction method provided by the invention, change the form of water by atomizing, because fog is made up of a large amount of droplets, each droplet the inside all is mixed with catalyst, the surface of each droplet all is a gas-liquid interface, atomizing by the liquid solution with catalyst like this increases gas-liquid interface, reduces the distance that hydrogen is selected, thereby has suppressed the generation of back reaction effectively; In addition, because the scattering probability of light in fog increases, effectively absorb enhancing, thereby greatly improved the utilization rate of light and the catalytic efficiency of photochemical catalyst.In sum, method and apparatus provided by the invention compared with prior art, advantage mainly is:
1, improved the absorption of photochemical catalyst to light;
2, suppressed the generation of back reaction in the light-catalyzed reaction;
3, improved the efficient of light-catalyzed reaction effectively.
Description of drawings
Below, describe embodiment of the present invention in conjunction with the accompanying drawings in detail, wherein:
Fig. 1 is the schematic representation of apparatus that is used for photocatalytic hydrogen production by water decomposition of embodiment 1;
Fig. 2 is the schematic representation of apparatus that is used for photocatalysis degradation organic contaminant of embodiment 2;
Fig. 3 is the schematic representation of apparatus that is used for photocatalytic hydrogen production by water decomposition of embodiment 3.
The specific embodiment
Below in conjunction with the specific embodiment the present invention is further described in detail, the embodiment that provides is only in order to illustrate the present invention, rather than in order to limit the scope of the invention.
Present embodiment is used for illustrating the application in the reaction of photochemical catalyzing of the method for light-catalyzed reaction of the present invention and device.
The device that uses in the present embodiment as shown in Figure 1, this device comprises 1 reaction vessel, 2 ultrasonic atomizers, 3 condensation sleeve pipes, 4 light sources, 5-7 three-way valve, 8 four way valves, 9-10 gas-chromatography interface, 11 vavuum pump interfaces (5-10 can being referred to as " sampling portion ").Wherein, two adjacent Zhi Tonglian of four way valve 8 are logical, and and three-way valve 7 between glass tube constitute the quantitative sampling ring, the adjacent Zhi Tonglian of two other of four way valve 8 is logical, is connected with gas-chromatography with 10 through gas-chromatography interface 9.Rotation four way valve 8 can make the quantitative sampling ring be communicated with chromatogram or disconnect, and when being in off-state, opens valve 7, and gas can diffuse in the quantitative sampling ring by valve 7; When being in connected state, the gas in the quantitative sampling ring can be brought into chromatogram (this moment, valve 7 was closed), the composition of real-time analysis gas and content by carrier gas.Vavuum pump (omitting among the figure) can be to whole device or only the quantitative sampling ring is vacuumized.Wherein, reaction vessel 1 is a silica glass material.
Concrete operating procedure is as follows:
1) with 0.3g TiO
2, 200ml H
2O, 0.3g C
2H
2O
4H with 240ul 0.01g/mL
2PtCl
6Solution joins in the reaction vessel shown in Figure 11;
2) mercury lamp of 500W is installed in the position of power supply shown in Figure 14, opens the recirculated cooling water in the condensation sleeve pipe 3, the temperature of cooling water is 10-13 ℃;
3) swivel tee valve 6 and 7 makes sampling portion full-mesh, and rotary four-way valve 8, and the quantitative sampling ring is not communicated with chromatogram, opens vavuum pump and vacuumizes, and reaches 10Pa up to vacuum;
4) swivel tee valve 5 gradually slowly reduces the reaction vessel internal gas pressure, treat that vacuum reaches 10Pa after, swivel tee valve 6 makes and closes between vavuum pump and the whole device, closes vavuum pump then;
5) open the power switch of ultrasonic atomizer 2, make the atomization of liquid in the reaction vessel 1;
6) open the power switch of mercury lamp, carry out the photochemical catalyzing reaction;
7) after reaction is carried out 2 hours, swivel tee valve 7 is closed it, and rotary four-way valve 8 makes the quantitative sampling ring be communicated with chromatogram, carries out analytical test with chromatogram, and rotary four-way valve 8 disconnected quantitative sampling ring and chromatogram after test finished;
8) after reaction finishes, close the power switch of ultrasonic atomizer 2 and mercury lamp, and close cooling water, the air pressure in the recovery device is to normal pressure.
Comparative Examples 1
This Comparative Examples is the contrast of embodiment 1, is used to measure the hydrogen output of the photochemical catalyzing reaction of not using atomizer.
Carry out the photochemical catalyzing reaction according to the method identical with embodiment 1, different is, does not comprise ultrasonic atomizer in the device of this Comparative Examples, does not comprise the operation of using ultrasonic atomizer in operating procedure.
Measure by the following method " hydrogen output ": at first demarcate amounts of hydrogen with gas-chromatography and the hydrogen peak area that records with chromatogram between the standard relationship curve, according to value pairing amounts of hydrogen in above-mentioned standard relationship curve of the hydrogen peak area that in the real reaction process, obtains, draw actual hydrogen output then.The test result of embodiment 1 and Comparative Examples 1 is listed in the table 1.
Table 1
| Difference | Hydrogen output (10 -3mol) | |
| |
Use ultrasonic atomizer | 54.5 |
| Comparative Examples 1 | Do not use ultrasonic atomizer | 5.1 |
Present embodiment is used for illustrating the application in the reaction of photocatalysis degradation organic contaminant of the method for light-catalyzed reaction of the present invention and device.
The device that uses in the present embodiment as shown in Figure 2, this device comprises 1 ' reaction vessel, 2 ' ultrasonic atomizer, 3 ' condensation sleeve pipe, 4 ' light source, 5 ' sampling portion and 6 ' sampling portion lid.Wherein, reaction vessel 1 ' links to each other with atmosphere by condensation sleeve pipe 3 ', with needed oxygen in the postreaction process; Be added with a sampling portion lid 6 ' in the sampling portion 5 ', be used for preventing the effusion of atomized drop.Wherein reaction vessel 1 ' is a silica glass material.
Concrete operating procedure is as follows:
1) with 25mg TiO
2With 50ml 2 * 10
-5The rhodamine B solution of m/l joins in the reaction vessel 1 ' shown in Figure 2;
2) the 150W mercury lamp is installed in the position of power supply 4 ' shown in Figure 2, opens the recirculated cooling water in the condensation sleeve pipe 3 ', the temperature of cooling water is 10-13 ℃;
3) open the power switch of ultrasonic atomizer 2 ', with the atomization of liquid in the reaction vessel;
4) open the power switch of mercury lamp, carry out the reaction of photocatalysis degradation organic contaminant;
5) every the 15min timing sampling, earlier sampling portion lid 6 ' is taken off during sampling, the liquid in that sampling portion 5 ' locates to take out 3mL covers sampling portion lid 6 ' then.The sample that takes out is carried out centrifugation, get supernatant liquor, measure the absorbance of this clear liquid with ultraviolet-uisible spectrophotometer, to calculate the degradation rate of pollutant;
6) close the power switch of ultrasonic atomizer 2 ' and mercury lamp after reaction finishes, stop logical cooling water.
Comparative Examples 2
This Comparative Examples is the contrast of embodiment 2, is used to measure the degradation rate of the photocatalysis degradation organic contaminant reaction of not using atomizer.
Carry out the photocatalysis degradation organic contaminant reaction according to the method identical with embodiment 2, different is, does not comprise ultrasonic atomizer in the device of this Comparative Examples, does not comprise the operation of using ultrasonic atomizer in operating procedure.Test result is listed in table 2.
Calculate " degradation rate " by following method: measure initial 2 * 10 respectively with ultraviolet-uisible spectrophotometer
-5The absorbance of the stillness of night that M rhodamine B solution and timing sampling obtain is respectively A
oAnd A, because the absorbance of rhodamine B and the pass between the concentration are linear in this concentration range, i.e. A
o/ C
o=A/C is so degradation rate is: (1-A/A
o) * 100%.
Table 2
Present embodiment is used for illustrating the application in the reaction of photochemical catalyzing of the method for light-catalyzed reaction of the present invention and device.
The device that uses in the present embodiment as shown in Figure 3, this device comprises 1 " reaction vessel, 2 " ultrasonic atomizer, 3 " condensation sleeve pipe, 4 " light source, 5 "-7 " three-way valve, 8 " four way valve, 9 "-10 " gas-chromatography interface, 11 " vavuum pump interface (can be "-10 " be referred to as " sampling portion ") with 5.Wherein, ultrasonic atomizer 2 " with reaction vessel 1 " outer bottom surface contact; Four way valve 8 " two adjacent Zhi Tonglian logical, and and three-way valve 7 " between glass tube constitute quantitative sampling ring, four way valve 8 " two other adjacent Zhi Tonglian logical, through 9 " with 10 " be connected with gas-chromatography.Rotate four way valve 8 " the quantitative sampling ring is communicated with chromatogram or disconnects, when being in off-state, open valve 7 ", gas can be by valve 7 " diffuse in the quantitative sampling ring; When being in connected state, the gas in the quantitative sampling ring can be brought into chromatogram (this moment valve 7 " close), the composition of real-time analysis gas and content by carrier gas.Vavuum pump (omitting among the figure) can be to whole device or only the quantitative sampling ring is vacuumized.Wherein, reaction vessel 1 " be silica glass material.
Concrete operating procedure is as follows:
1) with 0.3g TiO
2, 200ml H
2O, 0.3g C
2H
2O
4H with 240ul 0.01g/mL
2PtCl
6Solution joins reaction vessel shown in Figure 31 " in;
2) mercury lamp with 500W is installed in power supply shown in Figure 34 " the position, open condensation sleeve pipe 3 " in recirculated cooling water, the temperature of cooling water is 10-13 ℃;
3) the swivel tee valve 6 " and 7 ", make sampling portion full-mesh, and rotary four-way valve 8 ", the quantitative sampling ring is not communicated with chromatogram, open vavuum pump and vacuumize, reach 10Pa up to vacuum;
4) swivel tee valve 5 gradually ", the reaction vessel internal gas pressure is slowly reduced, treat that vacuum reaches 10Pa after, swivel tee valve 6 ", make and close between vavuum pump and the whole device, close vavuum pump then;
5) open ultrasonic atomizer 2 " power switch, make reaction vessel 1 " in the atomization of liquid;
6) open the power switch of mercury lamp, carry out the photochemical catalyzing reaction;
7) after reaction is carried out 2 hours, swivel tee valve 7 " it is closed, rotary four-way valve 8 " the quantitative sampling ring is communicated with chromatogram, carry out analytical test with chromatogram, rotary four-way valve 8 after test finishes " quantitative sampling ring and chromatogram are disconnected;
8) after reaction finishes, close ultrasonic atomizer 2 " and the power switch of mercury lamp, and close cooling water, the interior air pressure of recovery device is to normal pressure.
Comparative Examples 3
This Comparative Examples is the contrast of embodiment 3, is used to measure the hydrogen output of the photochemical catalyzing reaction of not using atomizer.
Carry out the photochemical catalyzing reaction according to the method identical with embodiment 3, different is, does not comprise ultrasonic atomizer in the device of this Comparative Examples, does not comprise the operation of using ultrasonic atomizer in operating procedure.Test result is listed in table 3.
The computational methods of " hydrogen output " in the table 3 are identical with embodiment 1.
Table 3
| Difference | Hydrogen output (10 -3mol) | |
| |
Use ultrasonic atomizer | 54.1 |
| Comparative Examples 3 | Do not use ultrasonic atomizer | 5.0 |
By the data in table 1, table 2 and the table 3 as can be seen, the method of light-catalyzed reaction provided by the invention and device atomize by the liquid solution with catalyst and increase gas-liquid interface, reduce the distance that hydrogen is overflowed, suppressed the generation of back reaction effectively, simultaneously because the scattering probability increase of light in fog, effectively absorb enhancing, thereby greatly improved the utilization rate of light and the catalytic efficiency of photochemical catalyst.
Claims (10)
1. the method for a light-catalyzed reaction is characterized in that, this method comprises the steps: 1, will contain the solution or the suspension atomization of photochemical catalyst and reactant, forms fog; 2, the fog generation light-catalyzed reaction that utilizes light source that step 1 is obtained.
2. method according to claim 1, wherein, described solution or suspension are the aqueous solution or the suspension that contains photochemical catalyst; Perhaps, described solution or suspension are the aqueous solution or the suspension that contains photochemical catalyst and organic pollution.
3. method according to claim 1 and 2, wherein, described photochemical catalyst is selected from metal oxide, metal sulfide, titanate, niobates, tantalates, tungstates, vanadate, zirconates, gallate, germanate, indate, stannate, stibate and by wherein several composite catalysts of forming or solid solution catalyst, and has the above-mentioned catalyst of metal and/or nonmetal doping and support in the above-mentioned catalyst of co-catalyst one or more.
4. according to any described method among the claim 1-3, wherein, the method for described atomizing is for using atomizer with described solution or suspension atomization.
5. according to any described method among the claim 1-4, wherein, this method also is included in the process of light-catalyzed reaction, the sample analysis light-catalyzed reaction carry out degree.
6. a device that is used for light-catalyzed reaction is characterized in that, this device comprises:
Reaction vessel;
Place this reaction vessel interior or outside atomizer;
The condensation sleeve pipe that is connected with this reaction vessel; And
The light source that is used for light-catalyzed reaction.
7. device according to claim 6, wherein, described reaction vessel is made by Pyrex glass or quartz glass.
8. according to claim 6 or 7 described devices, wherein, described atomizer is ultrasonic atomizer and/or centrifugal turntable atomizer.
9. according to any described device among the claim 6-8, wherein, described light source is one or more in xenon lamp, mercury lamp, halogen tungsten lamp, LED lamp and the sunshine.
10. according to any described device among the claim 6-9, wherein, this device also comprises and is used to take out the sampling portion of sample segment to analyze.
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