CN1911498A - Capillary tube array photo catalysis reactor and its preparation and application - Google Patents
Capillary tube array photo catalysis reactor and its preparation and application Download PDFInfo
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- CN1911498A CN1911498A CN 200610029643 CN200610029643A CN1911498A CN 1911498 A CN1911498 A CN 1911498A CN 200610029643 CN200610029643 CN 200610029643 CN 200610029643 A CN200610029643 A CN 200610029643A CN 1911498 A CN1911498 A CN 1911498A
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Abstract
The capillary array photocatalytic reactor and its making process and application belong to the field of nanometer semiconductor material photocatalytic reactor technology. The capillary array photocatalytic reactor of the present invention has capillary array with nanometer TiO2 film attached to the inner walls for photocatalytic reaction. The capillary array photocatalytic reactor has the advantages of no pulverizing and loss of the photocatalyst, great contact area between the reacted liquid and the photocatalyst, high light source utilization rate, high photocatalytic efficiency, capacity of detecting micro amount of sample, etc. The present invention also provides method of utilizing the photocatalytic reactor in detecting COD value of water sample.
Description
Technical field
The present invention relates to a kind of capillary tube array photo catalysis reactor and preparation thereof and application, definitely say, relate to a kind of capillary array nano-TiO
2Film light catalytic reactor and preparation thereof and application, the technical field of genus nano semiconductor material photo catalysis reactor and preparation and application.
Background technology
Photo catalysis reactor is the place that light-catalyzed reaction takes place, and designs reactor efficient, easy to use the scientific research and the practical application of light-catalyzed reaction had a very important role.Since the eighties in 20th century, the nano semiconductor material multiphase photocatalysis obtains increasing the concern at field of environment protection.Light-catalyzed reaction at room temperature just can be carried out deep reaction, the thorough mineralising of multiple organic pollution is removed, particularly, be considered to an extremely promising environmental pollution advanced purification technology showing outstanding ability aspect the removal of the poisonous and harmful substance of bio-refractory.In view of photocatalysis has broad prospect of application and huge social economic benefit in various fields such as environmental protection, clear energy sources, national defense and military, health care, construction material, auto industry, household electric appliances, textile industries; paid much attention to; scientific circles, government department and business circles have dropped into a large amount of funds and research effort; carry out catalytic base theory, application technology exploitation and through engineering approaches research, make photocatalysis become one of domestic and international most active research field in recent years.
The place that photo catalysis reactor takes place as light-catalyzed reaction, its designing requirement efficiently utilizes energy of light source and easy to use.In the liquid phase light-catalyzed reaction, existing way according to catalyst, roughly can be divided into rotating plasma precursor reactant device, fixed bed reactors and fluidized-bed reactor three classes, wherein the fixed bed reactors kind is more, can be divided into types such as film-type, packed bed type and carrier light-conducting type again.Above mentioned various reactor all has advantage and purpose of design separately, but also has shortcomings such as, catalyst not high to the energy of light source utilization rate and reactant liquor contact area be little.
At present, the mensuration of COD (COD) mostly adopts potassium bichromate circumfluence method, i.e. standard law.This method have measurement result accurately, high repeatability and other advantages, but consume a large amount of concentrated sulfuric acids and expensive silver sulfate, in order to eliminate the interference of chlorion, also need to add the very big mercuric sulfate of toxicity and sheltered, and Specimen eliminating needs a large amount of return times.In addition, when measuring low-pollution water sample such as surface water, drinking water etc., potassium dichromate method sensitivity is on the low side.Therefore when detecting oligosaprobic water sample, China recommends to use the permanganate indices method, but there are a little less than the oxidability shortcomings such as accuracy of measurement difference again in this method.
Summary of the invention
For overcoming the above-mentioned drawback of background technology effectively, first technical problem that the present invention will solve is to release a kind of capillary tube array photo catalysis reactor.This reactor mainly has the following advantages: not efflorescence of photochemical catalyst, do not run off; The contact area of reactant liquor and catalyst is big; The utilization rate height of light source, the photocatalysis efficiency height; Can detect micro-example; Can implement online detection to sample.
The technical scheme that the present invention solves the problems of the technologies described above employing is: the photo catalysis reactor of being released contains capillary 1, ultraviolet lamp tube 2, last polyfluortetraethylene pipe 30, following polyfluortetraethylene pipe 31, goes up round tray 40, following round tray 41, feed tube 5, drain pipe 6 and support 7, capillary 1 is a quartz capillary, and the inwall of capillary 1 has depended on nano-TiO
2Film, the core of two round trays has center hole, ultraviolet lamp tube 2 is inserted in the center hole of two pallets, two round trays are fixed on the support 7 in their the card circle center line connecting with them parallel to each other and support 7 parallel modes, two polyfluortetraethylene pipes are ring tubes of hollow, the mode that last polyfluortetraethylene pipe 30 overlaps with the center of circle of last round tray 40 with its center of circle is fixed on the lower surface of round tray 40, the mode that following polyfluortetraethylene pipe 31 overlaps with the center of circle of following round tray 41 with its center of circle is fixed on down the upper surface of round tray 41, capillary 1 is evenly distributed on, following polyfluortetraethylene pipe 30, on 31, keep between capillary and the capillary being parallel to each other and respectively with last, following polyfluortetraethylene pipe 30, the mode of 31 internal communication is connected across, following polyfluortetraethylene pipe 30, between 31, feed tube 5 and drain pipe 6 are respectively to be connected with last polyfluortetraethylene pipe 30 with following polyfluortetraethylene pipe 31 with the mode of following polyfluortetraethylene pipe 31 and last polyfluortetraethylene pipe 30 internal communication.
Reactor of the present invention is further characterized in that the power of ultraviolet lamp tube 2 and the centre wavelength of luminescent spectrum are respectively 11W and 253.7nm.
Being further characterized in that of reactor of the present invention, the internal diameter of capillary 1 and external diameter are respectively 250-560 μ m and 380-690 μ m.
Being further characterized in that of reactor of the present invention, the radical of capillary 1 are 20-80.
Second technical problem that the present invention will solve provides the preparation method of described reactor.
The technical scheme that the present invention addresses the above problem employing is: a kind of preparation method of capillary tube array photo catalysis reactor is characterized in that the concrete operations step:
The first step prepares inwall and is attached with nano-TiO
2The capillary 1 of film
The ratio of the amount of substance of each component of preparation is Ti (i-OC earlier
3H
7)
4: H
2O: C
2H
5OH: HNO
3=1: 1: 10: 0.2 TiO
2Colloidal sol is then with the TiO for preparing
2Colloidal sol is pressed in the capillary 1 with the nitrogen pressure device, behind the coating 2h, in room temperature gelation 1h, with nitrogen unnecessary gel is blown out under the condition of ice bath again, with capillary 1 calcining 1h under 500 ℃, obtains inwall and is attached with nano-TiO
2The capillary 1 of film, standby;
Second step was opened capilar bore, fluid hole, inlet opening and installation drain pipe 6, feed tube 5
On upper and lower polyfluortetraethylene pipe 30,31, evenly leave capilar bore, the aperture is more bigger than the external diameter of capillary 1, the number in hole equates with the radical of capillary 1, on upper and lower polyfluortetraethylene pipe 30,31, leave fluid hole and inlet opening respectively again, the aperture of fluid hole and inlet opening is more bigger than the external diameter of drain pipe 6 and feed tube 5, drain pipe 6 and feed tube 5 are inserted fluid hole and inlet opening respectively, with the epoxy resin shutoff go out, feed tube 6,5 and go out, slit between the inlet opening;
The 3rd step was opened center hole
Core at upper and lower round tray 40,41 is left center hole, and the center hole slightly larger in diameter is in the external diameter of ultraviolet lamp tube 2;
Fixing upper and lower polyfluortetraethylene pipe 30,31 of the 4th step
Upper and lower polyfluortetraethylene pipe 30,31 is separately fixed at the lower surface of round tray 40 and the upper surface of following round tray 41, and upper and lower polyfluortetraethylene pipe 30,31 keeps concentric with upper and lower round tray 40,41 respectively;
Fixing upper and lower round tray 40,41 of the 5th step
Mode so that the card of upper and lower round tray 40,41 keeps with one heart and parallel and upper and lower polyfluortetraethylene pipe 30,31 is relative is fixed on upper and lower round tray 40,41 on the support 7;
The 6th step was installed capillary array
The capillary 1 that each root first step is made is connected across in the capilar bore of upper and lower polyfluortetraethylene pipe 30,31 correspondences, and with the slit between epoxy resin shutoff capillary 1 and the capilar bore;
The 7th step was installed ultraviolet lamp tube 2
The 3rd technical problem that the present invention will solve provides the COD value that detects water body water sample to be measured with photo catalysis reactor of the present invention.For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of method that detects the COD value of water body water sample to be measured with capillary tube array photo catalysis reactor, this method needs to implement in the photocatalysis detection architecture that contains photo catalysis reactor, peristaltic pump, sampling valve, flow fluid reservoir, fluorescence detector and waste liquid reservoir, it is characterized in that, photo catalysis reactor is a capillary tube array photo catalysis reactor, the concrete operations step:
The configuration of first step flow fluid
Flow fluid is the Ce (SO of the 3.0 μ mol/L of adjusting pH to 1.2
4)
2Solution, flow fluid via hole diameter are the membrane filtration of 0.22 μ m, remove the suspended particulate that wherein may exist, and prevent to stop up sampling valve, are stored in then in the flow fluid reservoir;
The drafting of the second step COD working curve
Flow fluid flows through sampling valve under the pressure of peristaltic pump, flow velocity is 0.2-0.5ml/min, with the titer of glucose solution as COD, by sampling valve the glucose standard liquid injection sampling valve and the flow fluid of variable concentrations are mixed, flow into together in the described photo catalysis reactor, carry out light-catalyzed reaction under the irradiation of ultraviolet lamp tube 2, Ce is measured by fluorescence detector in the reaction back
4+The absorption photometric value, again with Ce
4+The changing value Δ A of absorption photometric value and the mapping of standard C OD value, obtain the working curve of COD value;
The mensuration of the 3rd step water body water sample COD value to be measured
With the glucose standard liquid in second step of water body water sample replacement to be measured, with measured Ce
4+The working curve demarcated of the changing value substitution of absorption photometric value, obtain the COD value of water body water sample to be measured.
The method that detects the COD value of water body water sample to be measured with reactor of the present invention is further characterized in that, detects Ce in second step
4+The maximum absorption wavelength of absorption photometric value be 320nm.
A kind of method that detects the COD value of water body water sample to be measured with capillary tube array photo catalysis reactor, this method needs to implement in the photocatalysis detection architecture that contains photo catalysis reactor, peristaltic pump, sampling valve, flow fluid reservoir, waste liquid reservoir and fluorescence detector, it is characterized in that, photo catalysis reactor is a capillary tube array photo catalysis reactor, the concrete operations step:
The configuration of first step flow fluid
Flow fluid is the K of the 10mmol/L of adjusting pH to 0.5
2Cr
2O
7Solution, flow fluid via hole diameter are the membrane filtration of 0.22 μ m, remove the suspended particulate that wherein may exist, and prevent to stop up sampling valve, are stored in then in the flow fluid reservoir;
The drafting of the second step COD working curve
Flow fluid flows through sampling valve under the pressure of peristaltic pump, flow velocity is 0.2-0.5ml/min, with the titer of glucose solution as COD, by sampling valve the glucose standard liquid injection sampling valve and the flow fluid of variable concentrations are mixed, flow into together in the described photo catalysis reactor, carry out light-catalyzed reaction under the irradiation of ultraviolet lamp tube 2, Cr is measured by fluorescence detector in the reaction back
3+The absorption photometric value, again with Cr
3+The changing value Δ A of absorption photometric value and the mapping of standard C OD value, obtain the working curve of COD value;
The mensuration of the 3rd step water body water sample COD value to be measured
With the glucose standard liquid in second step of water body water sample replacement to be measured, with measured Cr
3+The working curve demarcated of the changing value substitution of absorption photometric value, obtain the COD value of water body water sample to be measured.
The method that detects the COD value of water body water sample to be measured with reactor of the present invention is further characterized in that, Cr in second step
3+The maximum absorption wavelength of absorption photometric value be 610nm.
The operation principle of capillary tube array photo catalysis reactor
Inwall capillaceous in the capillary array reactor is attached with nano-TiO
2Film.TiO
2Under illumination condition, absorb luminous energy, when the energy of light source greater than TiO
2During energy gap between conduction band and valence band, electronics just can produce corresponding hole in valence band simultaneously from valence to conduction band, promptly generates electron-hole pair, and the pollutant that is adsorbed in the surface is directly carried out oxidation, or the OH of oxidized surface absorption
-, the hydrogen-oxygen hydroxyl radical free radical OH of generation strong oxidizing property, with the organic pollution oxidation, but light induced electron that is produced and hole are more compound than being easier to again, make catalytic efficiency lower.
Among the present invention, the employed Ce of flow fluid (IV) or Cr (VI) and TiO
2Can form collaboration system, Ce (IV) or Cr (VI) are as TiO
2The acceptor of light induced electron is absorbed in the light induced electron that its surface produces, and oneself is reduced to Ce
3+Or Cr
3+TiO
2The light induced electron that the surface produces is absorbed by Ce (IV) or Cr (VI), has suppressed the compound of photohole and electronics, makes the pollutant in the more effective oxidation water body of photohole, thereby has improved the photocatalysis efficiency of system, simultaneously Ce
4+Or Cr
3+The change in concentration value and the COD value in the water body linear relationship is arranged.Therefore by measuring Ce
4+Or Cr
3+The variable quantity of absorption photometric value, the quantitative value of COD in the water body just.
Compare with background technology, the present invention has the following advantages:
1, the reactor among the present invention, is compared with traditional photo catalysis reactor as the place that reaction takes place with capillary array, and bigger illuminating area and response area is provided, and has obtained higher photocatalysis efficiency.
2, capillary tube array photo catalysis reactor of the present invention is wide to the mensuration range of linearity of the COD in the water body, detectability is low, can obtain measurement result more fast, the minute of single sample only needs 5～10min, compare with the 2h digestion time of conventional method, shortened greatly and cleared up the required time of sample.
3, capillary tube array photo catalysis reactor of the present invention has been realized the room temperature measuring of COD in the water body, need not provide short its of high temperature to clear up.
4, capillary tube array photo catalysis reactor of the present invention can not cause secondary pollution to environment.
5, capillary tube array photo catalysis reactor of the present invention is easy and simple to handle, detects with low cost.
Description of drawings
Fig. 1 is the structural representation of capillary tube array photo catalysis reactor of the present invention, and wherein 1 is capillary, the 2nd, and ultraviolet lamp tube, the 30th, last polyfluortetraethylene pipe, the 31st, following polyfluortetraethylene pipe, the 40th, last round tray, the 41st, following round tray, the 5th, feed tube, the 6th, drain pipe, the 7th, support.Ultraviolet lamp tube 2 is positioned at the reactor middle body, and inwall adheres to nano-TiO
2The array of the capillary 1 of film is looped around around the ultraviolet lamp tube 2 and is fixed on the polyfluortetraethylene pipe, and capillary 1 inside is the place of light-catalyzed reaction.
Fig. 2 is the workflow schematic diagram that capillary tube array photo catalysis reactor of the present invention is used to detect the system of water body water sample COD value to be measured.Whole detection system contains flow fluid reservoir, peristaltic pump, sampling valve, capillary tube array photo catalysis reactor, fluorescence detector and waste liquid reservoir.What wherein frame of broken lines was interior is exactly capillary tube array photo catalysis reactor of the present invention.Flow fluid flows through sampling valve after peristaltic pump pressurization, in sampling valve and water body water sample to be measured mix, enter capillary tube array photo catalysis reactor together, carry out in this reactor that light-catalyzed reaction is laggard goes into the optics detector.
The specific embodiment
All embodiment all operate according to the operating procedure of the described method of summary of the invention.
The preparation of embodiment 1 capillary tube array photo catalysis reactor
Below only enumerate technical data and index that each step relates to:
In the first step, the internal diameter of capillary 1, external diameter, radical and length are respectively 560 μ m, 690 μ m, 30 and 15cm.In second step, the bore of upper and lower polyfluortetraethylene pipe 30,31 is 1.5mm, and the external diameter of upper and lower polyfluortetraethylene pipe 30,31 is 11cm.In the 3rd step, upper and lower round tray the 40, the 41st, back degree and diameter are respectively the lucite disk of 3mm and 12cm.In the 4th step, the distance between last polyfluortetraethylene pipe 30 and the following polyfluortetraethylene pipe is 15cm.In the 6th step, the radical of capillary 1 is 30 in the capillary array.In the 7th step, the power of ultraviolet lamp tube 2 and the centre wavelength of luminescent spectrum are respectively 11w and 253.7nm.
In the first step, flow fluid is that pH is the K of 0.5 10mmol/L
2Cr
2O
7Solution.In second step, the flow velocity of flow fluid is 0.3m L/min, and the glucose standard liquid of variable concentrations is injected in the reactor by sampling valve, after light-catalyzed reaction finishes, in 610nm place measurement Cr
3+The changing value of absorption photometric value, quantitatively high pollution COD in water body value.Its working curve is y=0.009x+0.0699, wherein the corresponding Cr of y and x difference
3+The changing value of absorption photometric value and measured COD value, measurement category is 10.0～500mg/L.In the 3rd step, water body water sample to be measured is taken from a domestic sewage factory in Shanghai City, measures Cr
3+The changing value of absorption photometric value is 1.462, obtains the COD value and is 154.7mg/L.
Two of the method that COD detects in the embodiment 3 capillary tube array photo catalysis reactors realization water body: to the detection of low COD value sample
In the first step, flow fluid is that the pH value is the Ce (SO of 1.2 3.0 μ mol/L
4)
2Solution.In second step, the flow velocity of flow fluid is 0.5mL/min, and the glucose standard liquid of variable concentrations is injected in the reactor by sampling valve, after light-catalyzed reaction finishes, in 320nm place measurement Ce
4+The changing value of absorption photometric value, quantitatively the COD value in the low-pollution water body.Its working curve is y=0.2384x+0.0293, wherein the corresponding Ce of y and x difference
4+The changing value of absorption photometric value and measured COD value, measurement category is 1.0～12mg/L.In the 3rd step, water body water sample to be measured is taken from the life running water in Shanghai City, measures Ce
4+The changing value of absorption photometric value is 0.578, obtains the COD value and is 2.3mg/L.
In sum, the present invention has released a kind of capillary tube array photo catalysis reactor and preparation and application.The capillary tube array photo catalysis reactor of developing among the present invention, photocatalysis efficiency height, simple to operation can be applied to detect the COD value in the water body, realized under the room temperature detection to the COD value.
Claims (10)
1, a kind of capillary tube array photo catalysis reactor, it is characterized in that, contain capillary (1), ultraviolet lamp tube (2), last polyfluortetraethylene pipe (30), following polyfluortetraethylene pipe (31), last round tray (40), following round tray (41), feed tube (5), drain pipe (6) and support (7), capillary (1) is a quartz capillary, the inwall of capillary (1) has depended on the nano TiO 2 film, the core of two round trays has center hole, ultraviolet lamp tube (2) is inserted in the center hole of two pallets, two round trays are fixed on the support (7) with their the circle center line connecting mode parallel with support (7) so that their card is parallel to each other, two polyfluortetraethylene pipes are ring tubes of hollow, the mode that last polyfluortetraethylene pipe (30) overlaps with the center of circle of last round tray (40) with its center of circle is fixed on the lower surface of round tray (40), the mode that following polyfluortetraethylene pipe (31) overlaps with the center of circle of following round tray (41) with its center of circle is fixed on down the upper surface of round tray (41), capillary (1) is evenly distributed on, following polyfluortetraethylene pipe (30,31) on, keep between capillary and the capillary being parallel to each other and respectively with last, following polyfluortetraethylene pipe (30,31) mode of internal communication is connected across, following polyfluortetraethylene pipe (30,31) between, feed tube (5) is connected with last polyfluortetraethylene pipe (30) with following polyfluortetraethylene pipe (31) in the mode with following polyfluortetraethylene pipe (31) and last polyfluortetraethylene pipe (30) internal communication respectively with drain pipe (6).
2, capillary tube array photo catalysis reactor according to claim 1 is characterized in that, the power of ultraviolet lamp tube (2) and the centre wavelength of luminescent spectrum are respectively 11W and 253.7nm.
3, capillary tube array photo catalysis reactor according to claim 1 is characterized in that, the internal diameter of capillary (1) and external diameter are respectively 250-560 μ m and 380-690 μ m.
4, capillary tube array photo catalysis reactor according to claim 1 is characterized in that, the radical of capillary (1) is 20-80.
5, capillary tube array photo catalysis reactor according to claim 1, it is characterized in that, the power and the centre wavelength of ultraviolet lamp tube (2) are respectively 11W and 253.7nm, and the internal diameter of capillary (1) and external diameter are respectively 250-560 μ m and 380-690 μ m, and the radical of capillary (1) is 20-80.
6, a kind of preparation method of capillary tube array photo catalysis reactor is characterized in that, the concrete operations step:
The first step prepares inwall and is attached with nano-TiO
2The capillary of film (1)
The ratio of the amount of substance of each component of preparation is Ti (i-OC earlier
3H
7)
4: H
2O: C
2H
5OH: HNO
3=1: 1: 10: 0.2 TiO
2Colloidal sol is then with the TiO for preparing
2Colloidal sol is pressed in the capillary (1) with the nitrogen pressure device, behind the coating 2h, in room temperature gelation 1h, with nitrogen unnecessary gel is blown out under the condition of ice bath again, with capillary (1) calcining 1h under 500 ℃, obtains inwall and is attached with nano-TiO
2The capillary of film (1), standby;
Second step was opened capilar bore, fluid hole, inlet opening and installation drain pipe (6), feed tube (5)
On upper and lower polyfluortetraethylene pipe (30,31), evenly leave capilar bore, the aperture is more bigger than the external diameter of capillary (1), the number in hole equates with the radical of capillary (1), on upper and lower polyfluortetraethylene pipe (30,31), leave fluid hole and inlet opening respectively again, the aperture of fluid hole and inlet opening is more bigger than the external diameter of drain pipe (6) and feed tube (5), drain pipe (6) and feed tube (5) are inserted fluid hole and inlet opening respectively, with the epoxy resin shutoff go out, feed tube (6,5) and go out, slit between the inlet opening;
The 3rd step was opened center hole
Core at upper and lower round tray (40,41) is left center hole, and the center hole slightly larger in diameter is in the external diameter of ultraviolet lamp tube (2);
Fixing upper and lower polyfluortetraethylene pipe (30,31) of the 4th step
Upper and lower polyfluortetraethylene pipe (30,31) is separately fixed at the lower surface of round tray (40) and the upper surface of following round tray (41), and upper and lower polyfluortetraethylene pipe (30,31) keeps concentric with upper and lower round tray (40,41) respectively;
Fixing upper and lower round tray (40,41) of the 5th step
Card with upper and lower round tray (40,41) keeps with one heart and the relative mode of parallel and upper and lower polyfluortetraethylene pipe (30,31), and upper and lower round tray (40,41) is fixed on the support (7);
The 6th step was installed capillary array
The capillary (1) that each root first step is made is connected across in the corresponding capilar bore of upper and lower polyfluortetraethylene pipe (30,31), and with the slit between epoxy resin shutoff capillary (1) and the capilar bore;
The 7th step was installed ultraviolet lamp tube (2)
Ultraviolet lamp tube (2) is inserted the circular hole of upper and lower round tray (40,41) from top to bottom, obtain capillary tube array photo catalysis reactor.
7, a kind of method that detects the COD value of water body water sample to be measured with capillary tube array photo catalysis reactor, this method needs to implement in the photocatalysis detection architecture that contains photo catalysis reactor, peristaltic pump, sampling valve, flow fluid reservoir, fluorescence detector and waste liquid reservoir, it is characterized in that, photo catalysis reactor is a capillary tube array photo catalysis reactor, the concrete operations step:
The configuration of first step flow fluid
Flow fluid is the Ce (SO of the 3.0 μ mol/L of adjusting pH to 1.2
4)
2Solution, flow fluid via hole diameter are the membrane filtration of 0.22 μ m, remove the suspended particulate that wherein may exist, and prevent to stop up sampling valve, are stored in then in the flow fluid reservoir;
The drafting of the second step COD working curve
Flow fluid flows through sampling valve under the pressure of peristaltic pump, flow velocity is 0.2-0.5ml/min, with the titer of glucose solution as COD, by sampling valve the glucose standard liquid injection sampling valve and the flow fluid of variable concentrations are mixed, flow into together in the described photo catalysis reactor, carry out light-catalyzed reaction under the irradiation of ultraviolet lamp tube (2), Ce is measured by fluorescence detector in the reaction back
4+The absorption photometric value, again with Ce
4+The changing value Δ A of absorption photometric value and the mapping of standard C OD value, obtain the working curve of COD value;
The mensuration of the 3rd step water body water sample COD value to be measured
With the glucose standard liquid in second step of water body water sample replacement to be measured, with measured Ce
4+The working curve demarcated of the changing value substitution of absorption photometric value, obtain the COD value of water body water sample to be measured.
8, according to claim 7ly detect the method for the COD value of water body water sample to be measured, it is characterized in that, detect Ce in second step with capillary tube array photo catalysis reactor
4+The maximum absorption wavelength of absorption photometric value be 320nm.
9, a kind of method that detects the COD value of water body water sample to be measured with capillary tube array photo catalysis reactor, this method needs to implement in the photocatalysis detection architecture that contains photo catalysis reactor, peristaltic pump, sampling valve, flow fluid reservoir, waste liquid reservoir and fluorescence detector, it is characterized in that, photo catalysis reactor is a capillary tube array photo catalysis reactor, the concrete operations step:
The configuration of first step flow fluid
Flow fluid is the K of the 10mmol/L of adjusting pH to 0.5
2Cr
2O
7Solution, flow fluid via hole diameter are the membrane filtration of 0.22 μ m, remove the suspended particulate that wherein may exist, and prevent to stop up sampling valve, are stored in then in the flow fluid reservoir;
The drafting of the second step COD working curve
Flow fluid flows through sampling valve under the pressure of peristaltic pump, flow velocity is 0.2-0.5ml/min, with the titer of glucose solution as COD, by sampling valve the glucose standard liquid injection sampling valve and the flow fluid of variable concentrations are mixed, flow into together in the described photo catalysis reactor, carry out light-catalyzed reaction under the irradiation of ultraviolet lamp tube (2), Cr is measured by fluorescence detector in the reaction back
3+The absorption photometric value, again with Cr
3+The changing value Δ A of absorption photometric value and the mapping of standard C OD value, obtain the working curve of COD value;
The mensuration of the 3rd step actual water sample COD value
With the glucose standard liquid in second step of actual water sample replacement, with measured Cr
3+The working curve demarcated of the changing value substitution of absorption photometric value, obtain the COD value of water body water sample to be measured.
10, according to claim 9ly detect the method for the COD value of water body water sample to be measured, it is characterized in that Cr in second step with capillary tube array photo catalysis reactor
3+The maximum absorption wavelength of absorption photometric value be 610nm.
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| JP4560164B2 (en) * | 2000-02-03 | 2010-10-13 | 旭化成ケミカルズ株式会社 | Microbial production of glycine |
| CN100368799C (en) * | 2005-05-26 | 2008-02-13 | 上海交通大学 | Photoelectrocatalysis method for determining chemical oxygen demand |
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2006
- 2006-08-01 CN CNB2006100296434A patent/CN100404123C/en not_active Expired - Fee Related
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| CN101786803A (en) * | 2010-03-02 | 2010-07-28 | 常州龙腾太阳能热电设备有限公司 | Method for coating multiple compound high anti-reflection films on inner surface and outer surface of glass tube with length/aperture ratio greater than 30 |
| CN101786803B (en) * | 2010-03-02 | 2012-06-20 | 常州龙腾太阳能热电设备有限公司 | Method for coating multiple compound high anti-reflection films on inner surface and outer surface of glass tube with length/aperture ratio greater than 30 |
| CN104837559A (en) * | 2012-10-09 | 2015-08-12 | Jn迈德西斯私人有限公司 | Improved device and method for sample separation |
| CN104837559B (en) * | 2012-10-09 | 2018-11-16 | 嘉恩生物科技有限公司 | Improved device and method for sample separation |
| CN106053436A (en) * | 2016-05-13 | 2016-10-26 | 东南大学 | Liquid phase photocatalysis test device |
| CN108786687A (en) * | 2017-05-02 | 2018-11-13 | 上海交通大学 | Photochemical reaction system based on micro- Chemical Engineering Technology |
| CN111790335A (en) * | 2019-04-08 | 2020-10-20 | 上海交通大学 | Ultraviolet photochemical reactor device based on continuous flow technology |
| CN112604616A (en) * | 2020-11-17 | 2021-04-06 | 华东师范大学 | Automatic control system and method for continuous synthesis of microchemical reaction and online monitoring |
| CN113230992A (en) * | 2021-04-30 | 2021-08-10 | 山东优检生物技术有限公司 | Reactor capable of controllably loading multiple catalytic materials, coating device and preparation method |
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