CN104614432A - Single organic matter standard gas concentration detecting device and method - Google Patents
Single organic matter standard gas concentration detecting device and method Download PDFInfo
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- CN104614432A CN104614432A CN201510021063.XA CN201510021063A CN104614432A CN 104614432 A CN104614432 A CN 104614432A CN 201510021063 A CN201510021063 A CN 201510021063A CN 104614432 A CN104614432 A CN 104614432A
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Abstract
The invention discloses a single organic matter standard gas concentration detecting device and method which are used for solving the problem about organic gas concentration analysis in the standard gas production process. The single organic matter standard gas concentration detecting device comprises a gas-liquid phase balance device and a photoelectrocatalysis COD (chemical oxygen demand) measuring device, wherein in the gas-liquid phase balance device, to-be-detected gas enters a prepared standard solution through a valve, a gas pressure relief valve and a sand core filter plate to form small bubbles, and the concentration of organic matters in a liquid phase gradually get stable in the rising process of the bubbles in the liquid; in the photoelectrocatalysis COD measuring device, a TiO2 working electrode is irradiated by ultraviolet light, the organic matters in the liquid phase are oxidized through photoelectrocatalysis, coulomb electric charge is calculated through light current measurement, and a value of COD in the liquid is obtained. The concentration of the organic matters in the liquid is calculated according to an organic matter molecular formula, and the concentration of organic gas in gas is obtained in combination of the henry's law.
Description
Technical field
The present invention relates to organism gas detection field, specifically a kind of pick-up unit of single organism gas concentration and method.
Background technology
At present, in the production run of gas, analysis is carried out to the concentration of organic gas in gas and is significant.For single volatile organic gas analytical approach of concentration in gas the most frequently used have vapor-phase chromatography (GC), gas chromatography-mass spectrography (GC-MS), its detection will experience sampling, pre-service and quantitative test three processes.There is complicated operation, spended time length, some component difficulty separation, need to make the problems such as relevant criterion curve in advance in these detection methods.The technology of liquid phase photoelectrocatalysis mensuration chemical oxygen demand (COD) (COD) obtains and develops fast in recent years, and the reaction of the method photoelectrocatalysis is carried out in thin-layer microreactor, take Titanium as anode, with the TiO of Titanium body surface
2nano-pipe array thin film is photocatalyst, and Pt does electrode, and saturated calomel electrode is reacted as contrast electrode.Such as, Chinese patent CN1696684 discloses " photoelectrocatalysis measures the method for chemical oxygen demand (COD) ", and this patent has made TiO by oneself
2film, and prepared at the aqueous solution Anodic Oxidation containing hydrofluorite, high temperature sintering by metal titanium sheet, obtain film product integrated with Titanium, then by measuring coulomb electric charge value determination COD value when water sample catalytic organism is complete in thin-layer microreactor.But the method is only suitable for measuring organic content in liquid phase, still cannot solve for the problem analysis measuring organic concentration in gas.To this, Chinese patent CN101915791A discloses " a kind of method and apparatus detecting total organic content of gas ", its way utilizes photocatalysis phase transfer device that organism in gas is transferred to liquid phase by gas phase, photoelectrocatalysis COD determinator detects organic content in liquid phase, but accurate analysis can not be carried out to the concentration of organic gas, and need organism in gas phase all to transfer in liquid phase to analyze.
Summary of the invention
The object of this invention is to provide a kind of pick-up unit and method of single organism gas concentration, to solve prior art Problems existing.
In order to achieve the above object, the technical solution adopted in the present invention is:
A pick-up unit for single organism gas concentration, is characterized in that: comprise gas-liquid phase equilibrium device, photoelectrocatalysis COD determinator, and connects the peristaltic pump of gas-liquid phase equilibrium device, photoelectrocatalysis COD determinator, wherein:
Described gas-liquid phase equilibrium device comprises thermostat, and the gas-liquid phase equilibrium tank be placed in thermostat, standard solution is filled in gas-liquid phase equilibrium tank, gas-liquid phase equilibrium tank top is set to tank mouth, and blocking has rubber plug in tank mouth, air induction conduit is inserted with in rubber plug, outtake tube, air induction conduit lower end stretches to below gas-liquid phase equilibrium tank internal standard liquid level of solution, and be provided with core filter plate in air induction conduit lower end, thermostat side side wall upper part is provided with air intake valve, air induction conduit upper end is communicated to air intake valve by gas pressure reducer, more than gas-liquid phase equilibrium tank internal standard liquid level of solution is stretched in outtake tube lower end, thermostat opposite side side wall upper part is provided with valve of giving vent to anger, outtake tube upper end is communicated to valve of giving vent to anger,
Described photoelectrocatalysis COD determinator comprises the reactive tank of sealing, reactive tank one end is communicated with connecting line, peristaltic pump is arranged on connecting line, connecting line penetrates the thermostat in gas-liquid phase equilibrium device and is communicated to gas-liquid phase equilibrium tank one side lower part, the reactive tank other end is provided with draining valve, reactive tank inside groove top is provided with ultraviolet source, reactive tank internal groove bottom is provided with working electrode, contrast electrode, to electrode, in reactive tank cell body, voltage source is set, the negative pole of voltage source with to Electrode connection, the positive pole of voltage source is connected with contrast electrode, the positive pole of voltage source is also connected with working electrode by the electrochemical workstation be arranged on outside reactive tank, form voltage source, working electrode, contrast electrode, to the three-electrode system of electrode, described electrochemical workstation, peristaltic pump control end is connected with the data processing equipment of outside respectively.
The pick-up unit of described a kind of single organism gas concentration, is characterized in that: described standard solution is NaNO
3solution, its concentration is 2mol/L, and pH value NaOH solution is adjusted to 8 ~ 9.
The pick-up unit of described a kind of single organism gas concentration, is characterized in that: described working electrode take Titanium as anode, with metallic titanium matrix surface TiO
2nano-pipe array thin film is photocatalyst; Prepare with Pt metal electrode, contrast electrode is prepared with Ag/AgCl.
A kind of single organism gas concentration detection method, is characterized in that: comprise the following steps:
(1), within specified temperatures, gas to be measured is input in the gas-liquid phase equilibrium tank of gas-liquid phase equilibrium device with standard atmospheric pressure; Gas to be measured enters the standard solution of configuration, and form micro-bubble, in the process risen in the solution, organism concentration in the liquid phase reaches stable gradually;
(2), get quantitative organic concentration in gas-liquid phase equilibrium tank to reach stable solution carry out chemical oxygen demand (COD) measurement in photoelectrocatalysis COD determinator;
(3), in photoelectrocatalysis COD determinator, organic cod value in solution is calculated according to coulomb electric charge Q; By organic molecule formula and COD value, obtain organic concentration in solution; Under the environment of specified temp and inorganic standard electrolyte solution, the Henry's constant of organic gas is certain value, therefore can obtain the concentration of organic gas in gas to be measured.
In the present invention in photoelectrocatalysis COD determinator, when UV-irradiation, organic gas is at TiO
2oxidation reaction is there is in nanometer pipe array electrode reactor.When after organism oxidized dose of mineralising, by obtaining coulomb electric charge Q to the data acquisition process of electric current, Faraday's law is utilized to obtain COD value.
The inventive method and the photoelectrocatalysis COD determination part described in Chinese patent CN101915791A divide similar, and what it measured is organic content in gas, and the method for employing is that gas is transferred to liquid phase, then measures; What the inventive method adopted is principles of vapor liquid equilibrium, does not need gas all to transfer in liquid phase.
Compared with prior art, tool has the following advantages in the present invention: the detection method and the device that the invention provides and prepared a kind of single organism gas concentration, the method and apparatus structure is simple, performance is good, cost is low, detection is fast.The present invention utilizes principles of vapor liquid equilibrium and photoelectrocatalysis COD measuring principle, and organism in gas phase is measured indirectly in the liquid phase.The present invention, compared with traditional chromatographic detection, does not need complicated operating process; Compared with photocatalysis phase transfer of technology, do not need organism to be transferred to completely liquid phase and measure.
Accompanying drawing explanation
Fig. 1 is apparatus of the present invention structural representation.
Embodiment
As shown in Figure 1, a kind of pick-up unit of single organism gas concentration, comprises gas-liquid phase equilibrium device, photoelectrocatalysis COD determinator, and connects the peristaltic pump 8 of gas-liquid phase equilibrium device, photoelectrocatalysis COD determinator, wherein:
Gas-liquid phase equilibrium device comprises thermostat 5, and the gas-liquid phase equilibrium tank 6 be placed in thermostat 5, standard solution is filled in gas-liquid phase equilibrium tank 6, gas-liquid phase equilibrium tank 6 top is set to tank mouth, and blocking has rubber plug in tank mouth, air induction conduit 3-1 is inserted with in rubber plug, outtake tube 3-2, air induction conduit 3-1 lower end stretches to below gas-liquid phase equilibrium tank 6 internal standard liquid level of solution, and be provided with core filter plate 7 in air induction conduit 3-1 lower end, thermostat 5 side side wall upper part is provided with air intake valve 1, air induction conduit 3-1 upper end is communicated to air intake valve 1 by gas pressure reducer 2, outtake tube 3-2 stretches into lower end more than gas-liquid phase equilibrium tank 6 internal standard liquid level of solution, thermostat 5 opposite side side wall upper part is provided with valve 4 of giving vent to anger, outtake tube 3-2 upper end is communicated to valve 4 of giving vent to anger,
Photoelectrocatalysis COD determinator comprises the reactive tank 9 of sealing, reactive tank 9 one end is communicated with connecting line, peristaltic pump 8 is arranged on connecting line, connecting line penetrates the thermostat 5 in gas-liquid phase equilibrium device and is communicated to gas-liquid phase equilibrium tank 6 one side lower part, reactive tank 9 other end is provided with draining valve 14, reactive tank 9 inside groove top is provided with ultraviolet source 10, reactive tank 9 internal groove bottom is provided with working electrode 11, contrast electrode 12, to electrode 13, in reactive tank 9 cell body, voltage source 15 is set, the negative pole of voltage source 15 is connected with to electrode 13, the positive pole of voltage source 15 is connected with contrast electrode 12, the positive pole of voltage source 15 is also connected with working electrode 11 by the electrochemical workstation 16 be arranged on outside reactive tank 9, form voltage source 15, working electrode 11, contrast electrode 12, to the three-electrode system of electrode 13, electrochemical workstation 16, peristaltic pump 8 control end is connected with the data processing equipment 17 of outside respectively.
Standard solution is NaNO
3solution, its concentration is 2mol/L, and pH value NaOH solution is adjusted to 8 ~ 9.
Working electrode 11 take Titanium as anode, with metallic titanium matrix surface TiO
2nano-pipe array thin film is photocatalyst; To electrode 13 with Pt metal preparation, contrast electrode 12 is prepared with Ag/AgCl.
A kind of single organism gas concentration detection method, comprises the following steps:
(1), within specified temperatures, gas to be measured is input in the gas-liquid phase equilibrium tank of gas-liquid phase equilibrium device with standard atmospheric pressure; Gas to be measured enters the standard solution of configuration, and form micro-bubble, in the process risen in the solution, organism concentration in the liquid phase reaches stable gradually;
(2), get quantitative organic concentration in gas-liquid phase equilibrium tank to reach stable solution carry out chemical oxygen demand (COD) measurement in photoelectrocatalysis COD determinator;
(3), in photoelectrocatalysis COD determinator, organic cod value in solution is calculated according to coulomb electric charge Q; By organic molecule formula and COD value, obtain organic concentration in solution; Under the environment of specified temp and inorganic standard electrolyte solution, the Henry's constant of organic gas is certain value, therefore can obtain the concentration of organic gas in gas to be measured.
Specific embodiment:
Under the control of thermostat 5, gas-liquid phase equilibrium device is in 25 DEG C of environment, in gas-liquid phase equilibrium device, gas-liquid phase equilibrium tank 6 adopts the material not easily adsorbed to make, consider solution height, gas-liquid phase equilibrium tank is made as high about 30cm, diameter is 3.5cm, be about 5cm place at gas-liquid phase equilibrium tank one side bottom and get the aperture of 6mm for sampling, at tank mouth place except being inserted into airway 3-1, the place of outtake tube 3-2, all the other places are with rubber stopper seal, air induction conduit 3-1, outtake tube 3-2 diameter gets 1cm, it is wherein the core filter plate 7 made with sintered glass bottom air induction conduit 3-1, it is used for micro-bubble to increase the contact area of gas and liquid.That hold in gas-liquid phase equilibrium tank 6 is the NaNO of special 2mol/L
3solution, is modulated into 8 ~ 9 with NaOH solution by pH, and the height in gas-liquid phase equilibrium tank 6 is about about 20cm, and the height that air induction conduit 3-1 stretches into liquid level is about about 10cm, and outtake tube 3-2 at ullage, and leads to emission-control equipment.In photoelectrocatalysis COD Analytical system, reactive tank 9 (volume is about 60mm × 30mm × 5mm) adopts encapsulation process, and its top, with glass capsulation, is equipped with ultraviolet source 10 (wavelength is 365nm, and power is 4 watts) on the upside of glass.Be equipped with thief hatch and draining valve 14 respectively in reactive tank 9 both sides, thief hatch is communicated to the aperture of gas-liquid phase equilibrium tank 6 one side bottom by the connecting line being provided with peristaltic pump 8.Bottom reactive tank 9, be provided with working electrode 11, take Titanium as anode, with metallic titanium matrix surface TiO
2nano-pipe array thin film is photocatalyst, does to make contrast electrode 12 to electrode 13, Ag/AgCl with Pt metal, and Electrode connection is to electrochemical workstation 16, and consider ability to bear and the reaction speed of working electrode, generally choosing bias voltage size is 0.5 ~ 1.0V.
First open peristaltic pump 8, get quantitative titer to reactive tank 9.Open ultraviolet source 10, electrochemical workstation 16 gathers without titer blank photocurrent i during organism
blank, when reaction reaches stable, data processing equipment 17 pairs of current differential process obtain Q
blank.Close peristaltic pump valve 6, open air intake valve 1 and valve 4 of giving vent to anger, will treat that the gas (as ethane in nitrogen) of concentration analysis passes into standard NaNO
3solution, controls the stable input of gas with gas pressure reducer 2.Continue to pass into 3 ~ 5 minutes, close air intake valve 1 and valve 4 of giving vent to anger, open peristaltic pump 8 and carry out quantitative sampling.Along with the time passing into gas is elongated, gas-liquid levels off to balance gradually, after each quantitative sampling, is measured by photoelectrocatalysis COD determinator, and the COD value recorded more and more levels off to certain certain value.
After liquid phase reaches balance, open peristaltic pump 8 and sample, control to adopt liquid volume.Treat that liquid acquisition is complete, enter into reactive tank 9 containing organic solution to be measured, close peristaltic pump 8, turn on violet source 10 lamp and start to irradiate working electrode, TiO
2nanotube reaction zone starts to carry out oxidation reaction, meanwhile, due to the traction of bias voltage, forms photocurrent i
total, gathered by electrochemical workstation 16 pairs of electric currents, data processing equipment 17 pairs of photocurrents carry out differential process, will obtain coulomb electric charge:
Q＝∫(i
total-i
blank)dt (1-1)
There is certain error in this electricity, can make corresponding Error processing according to actual conditions.
So COD value is:
Wherein, COD-chemical oxygen demand (COD); F is Faraday constant, F=96487C/mol; V amasss for adopting liquid.Organism concentration in the solution (calculating for ethane) can be calculated below according to chemical oxygen demand (COD):
Wherein
for the substance withdrawl syndrome (mol/L) of ethane in water sample.The concentration that can be obtained organic ethane in gas by formula the Ideal-Gas Equation and Henry's law is:
In formula, H is the Henry's constant of ethane 25 DEG C time, H=5.57 × 10
4pam
3/ mol, P are standard atmospheric pressure.Because whether uncertain gas-liquid balances, can gather several times, when measured value is tending towards certain certain value more.Above with C in nitrogen
2h
6for example, different gaseous solute Henry's constants is different, and can measure temperature is in advance 25 DEG C, and solute is the Henry's constant of special sodium nitrate solution, carries out calibration process.
Claims (4)
1. a pick-up unit for single organism gas concentration, is characterized in that: comprise gas-liquid phase equilibrium device, photoelectrocatalysis COD determinator, and connects the peristaltic pump of gas-liquid phase equilibrium device, photoelectrocatalysis COD determinator, wherein:
Described gas-liquid phase equilibrium device comprises thermostat, and the gas-liquid phase equilibrium tank be placed in thermostat, standard solution is filled in gas-liquid phase equilibrium tank, gas-liquid phase equilibrium tank top is set to tank mouth, and blocking has rubber plug in tank mouth, air induction conduit is inserted with in rubber plug, outtake tube, air induction conduit lower end stretches to below gas-liquid phase equilibrium tank internal standard liquid level of solution, and be provided with core filter plate in air induction conduit lower end, thermostat side side wall upper part is provided with air intake valve, air induction conduit upper end is communicated to air intake valve by gas pressure reducer, more than gas-liquid phase equilibrium tank internal standard liquid level of solution is stretched in outtake tube lower end, thermostat opposite side side wall upper part is provided with valve of giving vent to anger, outtake tube upper end is communicated to valve of giving vent to anger,
Described photoelectrocatalysis COD determinator comprises the reactive tank of sealing, reactive tank one end is communicated with connecting line, peristaltic pump is arranged on connecting line, connecting line penetrates the thermostat in gas-liquid phase equilibrium device and is communicated to gas-liquid phase equilibrium tank one side lower part, the reactive tank other end is provided with draining valve, reactive tank inside groove top is provided with ultraviolet source, reactive tank internal groove bottom is provided with working electrode, contrast electrode, to electrode, in reactive tank cell body, voltage source is set, the negative pole of voltage source with to Electrode connection, the positive pole of voltage source is connected with contrast electrode, the positive pole of voltage source is also connected with working electrode by the electrochemical workstation be arranged on outside reactive tank, form voltage source, working electrode, contrast electrode, to the three-electrode system of electrode, described electrochemical workstation, peristaltic pump control end is connected with the data processing equipment of outside respectively.
2. the pick-up unit of a kind of single organism gas concentration according to claim 1, is characterized in that: described standard solution is NaNO
3solution, its concentration is 2mol/L, and pH value NaOH solution is adjusted to 8 ~ 9.
3. the pick-up unit of a kind of single organism gas concentration according to claim 1, is characterized in that: described working electrode take Titanium as anode, with metallic titanium matrix surface TiO
2nano-pipe array thin film is photocatalyst; Prepare with Pt metal electrode, contrast electrode is prepared with Ag/AgCl.
4., based on a single organism gas concentration detection method for pick-up unit described in claim 1, it is characterized in that: comprise the following steps:
(1), within specified temperatures, gas to be measured is input in the gas-liquid phase equilibrium tank of gas-liquid phase equilibrium device with standard atmospheric pressure; Gas to be measured enters the standard solution of configuration, and form micro-bubble, in the process risen in the solution, organism concentration in the liquid phase reaches stable gradually;
(2), get quantitative organic concentration in gas-liquid phase equilibrium tank to reach stable solution carry out chemical oxygen demand (COD) measurement in photoelectrocatalysis COD determinator;
(3), in photoelectrocatalysis COD determinator, organic cod value in solution is calculated according to coulomb electric charge; By organic molecule formula and COD value, obtain organic concentration in solution; Under the environment of specified temp and inorganic standard electrolyte solution, the Henry's constant of organic gas is certain value, therefore can obtain the concentration of organic gas in gas to be measured.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107138111A (en) * | 2017-05-23 | 2017-09-08 | 郑州轻工业学院 | A kind of carbon dioxide catalytic reduction reaction device |
| CN108318530A (en) * | 2018-03-20 | 2018-07-24 | 郑州轻工业学院 | A kind of device detecting formaldehyde gas concentration based on photocatalysis |
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| CN101915791A (en) * | 2010-07-09 | 2010-12-15 | 中国科学院广州能源研究所 | Method and device for detecting total organic content of gas |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107138111A (en) * | 2017-05-23 | 2017-09-08 | 郑州轻工业学院 | A kind of carbon dioxide catalytic reduction reaction device |
| CN107138111B (en) * | 2017-05-23 | 2019-02-22 | 郑州轻工业学院 | A kind of carbon dioxide catalytic reduction reaction device |
| CN108318530A (en) * | 2018-03-20 | 2018-07-24 | 郑州轻工业学院 | A kind of device detecting formaldehyde gas concentration based on photocatalysis |
| CN108318530B (en) * | 2018-03-20 | 2023-09-26 | 郑州轻工业大学 | Device based on photocatalysis detects formaldehyde gas concentration |
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Application publication date: 20150513 |