CN102854054A - Quick sample injection and metering digestion reaction device for detecting COD (chemical oxygen demand) - Google Patents

Quick sample injection and metering digestion reaction device for detecting COD (chemical oxygen demand) Download PDF

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Publication number
CN102854054A
CN102854054A CN2012103472518A CN201210347251A CN102854054A CN 102854054 A CN102854054 A CN 102854054A CN 2012103472518 A CN2012103472518 A CN 2012103472518A CN 201210347251 A CN201210347251 A CN 201210347251A CN 102854054 A CN102854054 A CN 102854054A
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China
Prior art keywords
metering
sample
pool
valve
reflux
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Pending
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CN2012103472518A
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Chinese (zh)
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张荣标
王中鑫
楚孔旭
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Jiangsu University
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Jiangsu University
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Abstract

The invention discloses a quick sample injection and metering digestion reaction device for detecting COD (chemical oxygen demand) in water samples. Each sample injection gas pump is connected to the upper portion of a sample pool, the bottom of the sample pool is connected to the top of a reflux pool positioned below the sample pool, a vent duct and a pressurizing pipeline are respectively arranged on two sides of the top of the reflux pool, a vent valve is disposed on the vent duct, the reflux pool is connected with a reflux gas pump by the pressurizing pipeline, a reflux gas pump valve is arranged on the pressurizing pipeline, the bottom of the reflux pool is connected to the upper side of the sample pool by a reflux pipe, a reflux valve is disposed on the reflux pipe, a metering funnel is arranged in an inner cavity of the reflux pool, the lower end of the metering funnel extends out of the reflux pool and is connected with a digestion reaction flask, a metering valve is arranged at the lower end of the metering funnel, and is closed when reagents in the sample pool are metered, and the vent valve is closed when the reflux gas pump works; a circle of electric heating sheets encircles the outer edge of the digestion reaction flask; and a semiconductor refrigerator is arranged above the digestion reaction flask. The quick sample injection and metering digestion reaction device has the advantage that processes including extracting water samples, filling oxidants and catalysts for digestion, digestion heating and the like are controlled automatically.

Description

Reaction unit is cleared up in a kind of fast sample metering for the COD detection
Technical field
The present invention relates to a kind of for water sample COD(chemical oxygen demand (COD)) the sample introduction metering that detects clears up reaction unit.
Background technology
At present, the digestion process of chemical digesting method COD detecting instrument commonly used is divided into manually and automatic two kinds both at home and abroad, manually clear up and be generally used for laboratory COD and measure, need manually to add the used reagent of digestion process, then will clear up test tube and be placed in the heating arrangement and clear up.The manual procedure complex steps, digestion time is long; The fluid transport mode that automatic digestion process is used generally is to adopt peristaltic pump as delivery means, peristaltic pump is delivered to liquid the reaction bulb from container bottle by the extruding pump line, but peristaltic pump is very low to the transfer efficiency of liquid, and long-term use is easily aging, affects transfer efficiency.Easy residual liquid forms dirt in the pipe, affects fluid transport and measuring accuracy, finally affects the COD testing result.
Summary of the invention
For the weak point that COD detecting instrument digestion instrument commonly used exists, the purpose of this invention is to provide a kind ofly measure accurately, fast sample metering that transfer efficiency is high clears up reaction unit.
The technical scheme that the reaction unit employing is cleared up in a kind of fast sample metering for the COD detection provided by the invention is: the sample introduction air pump connects sample cell top, the sample cell bottom connects the top of the backflow pool that is positioned at the sample cell below by pipeline, sampling valve is set in the middle of pipeline, both sides, backflow pool top are provided with ventilating duct and capstan, the first breather valve is set on the ventilating duct, backflow pool is connected to the backflow air pump by capstan, the backflow air pump valve is set on the capstan, the backflow pool bottom is connected to the sample cell top by recirculatory pipe, reverse flow valve is set on the recirculatory pipe, in the backflow pool inner chamber measuring hoper is set, the lower end of measuring hoper is stretched out outside the backflow pool and is connected and clears up reaction bulb, the measuring hoper lower end is provided with metering valve, and metering valve cut out when the reagent in the sample cell was measured, and the first breather valve is closed during the work of backflow air pump; Outside one corral of clearing up reaction bulb has electric heating piece.
The described reaction bulb of clearing up carries 3-6 sample feeding pipe, each sample feeding pipe with is connected the measuring hoper of a correspondence and connects, finish simultaneously metering and sample introduction that the 3-6 kind is cleared up reagent.
The described reaction bulb top of clearing up arranges semiconductor cooler.
Beneficial effect of the present invention is as follows:
1, apparatus of the present invention can realize fully automatically control, clear up used oxygenant and catalyzer from extracting water sample to adding, and clear up heating etc. and realize automatically control fully, and process is simple and convenient.
2, than the digestion instrument that adopts peristaltic pump to transmit and measure, apparatus of the present invention adopt the conical hopper First Astronautic Research Institute for Measurement and Test to survey water sample and agents useful for same, measure more accurate.
3, than the digestion instrument that adopts cooling water circulation to cool off, apparatus of the present invention adopt semiconductor cooler to clear up cooling, and semiconductor cooler heat absorption and radiating effect are obvious, and be more obvious than cooling water temperature effect, and structure is simpler.
4, overflow unnecessary reagent in apparatus of the present invention metering process and be back in the sample injection bottle by pressurization, do not cause any waste, reduced pollution, reduced cost.
Description of drawings
Fig. 1 is the one-piece construction figure of apparatus of the present invention;
Among the figure: 1. sample introduction air pump; 2. sample cell; 3. reverse flow valve; 4. backflow air pump; 5. backflow air pump valve; 6. sampling valve; 7. breather valve; 8. metering valve; 9. temperature sensor; 10. clear up reaction bulb; 11. semiconductor cooler; 12. sample feeding pipe; 13. measuring hoper; 14. electric heating piece; 15. go out the sample pipe valve; 16. backflow pool; 17. recirculatory pipe; 18. breather valve; 19. sampling valve; 20 sample introduction metering sections; 21. clear up reactive moieties.
Embodiment
Referring to Fig. 1, apparatus of the present invention comprise sample introduction metering section 20 and clear up reactive moieties 21 two parts.Sample introduction metering section 20 mainly comprises sample cell 2, sample introduction air pump 1, adds compression pump 4, backflow pool 16, recirculatory pipe 17, reverse flow valve 3, measuring hoper 13, sampling valve 6, breather valve 7, breather valve 18 and metering valve 8.Wherein, sample introduction air pump 1 connects sample cell 2 tops, and backflow pool 16 is positioned at sample cell 2 belows, and sample cell 2 bottoms connect backflow pool 16 tops by pipeline, and in the middle of pipeline sampling valve 6 are set.Both sides, backflow pool 16 top are provided with ventilating duct and capstan, at ventilating duct breather valve 7 are installed, and the effect of ventilation duct is to keep backflow pool 16 inner and outer air pressures to equate.Backflow pool 16 is connected to backflow air pump 4 by capstan, and installs back gas pump valve 5 at capstan.The bottom of backflow pool 16 is connected to sample cell 2 tops by recirculatory pipe 17, at recirculatory pipe 17 reverse flow valve 3 is installed.In backflow pool 16 inner chambers measuring hoper 13 is set, measuring hoper 13 is taper, and it is outer and connect and clear up and clear up reaction bulb 10 in the reactive moieties 21 that backflow pool 16 is stretched out in the lower end of measuring hoper 13, and measuring hoper 13 inner chambers are cleared up reaction bulb 10 inner chambers and communicated.Be provided with metering valve 8 in measuring hoper 13 lower ends.Backflow pool 16 is designed to a side can Unclosing structure, is convenient to measuring hoper 13 is changed, and selects different measuring hopers 13 according to metering volume.Measuring hoper 13 minimum metering volume can reach 1ml, and volume is less, and the consumption of reagent is fewer, thereby can reduce cost, and reduce to pollute.
Breather valve 18 is installed at sample cell 2 tops, sample cell 2 inside are communicated with ambient atmosphere, the effect of this breather valve 18 is after metering is finished, open this breather valve 18, make the pressure in the sample cell 2 be unlikely to too large, thereby make the reagent in the backflow pool 16 return smoothly sample cell 2, reduce the power consumption of backflow air pump 4.When the reagent in the sample cell 2 is measured, this metering valve 8 cuts out, reagent in the sample cell 2 splashes in the measuring hoper 13 under pressure, after measuring hoper 13 is full of, unnecessary reagent spills in the backflow pool 16, can take full advantage of each and clear up agents useful for same, not cause any waste.Breather valve 7 is closed when 4 work of backflow air pump, backflow air pump 4 has double action, at first be to backflow pool 16 interior pressurizations the reagent of 13 li of measuring hopers to be pressed into to clear up in the reaction bulb 10, backflow pool 16 interior unnecessary reagent can be depressed in the sample cell 2 by recirculatory pipe 17 simultaneously.
Clearing up reactive moieties 21 comprises and clears up reaction bulb 10, temperature sensor 9, semiconductor cooler 11, electric heating piece 14, sample feeding pipe 19 and go out sample pipe valve 15.Wherein, going out sample pipe valve 15 is installed in and clears up the going out on the sample pipe of reaction bulb 10 bottoms; Clear up reaction bulb 10 and carry sample feeding pipe 12, sampling valve 19 is installed on the sample feeding pipe 12; The lower end of measuring hoper 13 is connected to the sample feeding pipe 12 of clearing up reaction bulb 10 by rubber tube, clear up reaction bulb 10 total 3-6 sample feeding pipes 12, each sample feeding pipe 12 connects with the measuring hoper 13 of in the sample introduction metering section 20 of a correspondence, can finish simultaneously metering and sample introduction that the 3-6 kind is cleared up reagent.Clear up reaction bulb 10 tops cooling device is set, cooling device adopts semiconductor cooler 11, and this semiconductor cooler 11 is schistose textures, has tow sides, the one side heat absorption, and the one side heat release, the two sides temperature difference maintains about 60 degree.Clear up reactive moieties 21 and seal, cool off clearing up reaction bulb 10 tops, can reduce the pressure in the bottle, prevent from clearing up reactive moieties 21 blasts.Adopt electric heating pieces 14 to heat clearing up reaction bulb 10, electric heating piece 14 is trapped among outside one circle of clearing up reaction bulb 10, a temperature sensor 9 in the middle embedding of electric heating piece 14, and this temperature sensor 9 is used for Real-Time Monitoring and clears up temperature in the reaction bulb 10, and digestion condition is maintained about 165 ℃.
The specific works process of apparatus of the present invention is as follows: at first be that the required reagent of clearing up is measured: before device is started working, all valves all are in closed condition, during device work, at first open sampling valve 6, start simultaneously sample introduction air pump 1, sample introduction air pump 1 is to sample cell 2 interior pressurizations, reagent in the sample cell 2 splashes into the measuring hoper 13 in the backflow pool 16 under pressure, behind the certain hour, closes sample introduction air pump 1, measuring hoper 13 is full of, and the reagent that overflows flows in the backflow pool 16.After metering process is finished, the reagent that measures to be transferred to and clear up in the reaction bulb 10, at this moment, open metering valve 8, sampling valve 19 and backflow air pump valve 5, start simultaneously backflow air pump 4, clear up in the reaction bulb 10 by to backflow pool 16 interior pressurizations the reagent in the measuring hoper 13 being pressed into, after reagent in the measuring hoper 13 transfers, close metering valve 8 and sampling valve 19, open reverse flow valve 3 and breather valve 18, the reagent that overflows in the backflow pool 16 returns sample cell 2 from recirculatory pipe 17 under pressure.After sample introduction and reflux course were finished, closing volume air pump 4, reverse flow valve 3 and backflow air pump valve 5 were opened breather valve 7 simultaneously, made backflow pool 16 internal gas pressures be down to standard atmospheric pressure.Then, begin the reagent of clearing up in the reaction bulb 10 is cleared up electric conduction backing 14 power supplys, to clearing up reaction bulb 10 heating, temperature sensor 9 Real-Time Monitorings on the electric heating piece 14 temperature in the bottle, when temperature reaches 165 ℃, cut off electric heating piece 14 power supplys, stopped heating; When temperature in the bottle was lower than 165 ℃, electric conduction backing 14 power supplys heated clearing up reaction bulb 10 again, thereby the temperature of clearing up in the reaction bulb 10 are maintained about 165 ℃ all the time.When clearing up, start the semiconductor cooler 11 clear up above the reaction bulb 10, ceaselessly absorb heat in semiconductor cooler 11 inboards, the water vapor of clearing up reaction bulb 10 interior tops is cooled off, make and clear up reaction bulb 10 interior pressure and be unlikely to too large and blast, the ceaselessly heat release of semiconductor cooler 11 outsides, the temperature difference of inside and outside both sides maintains about 60 ℃.Digestion time at first cuts off electric heating piece 14 power supplys after finishing, and stops the device heating.Semiconductor cooler 11 works on a period of time, makes to clear up reacted solution and be cooled to as early as possible room temperature.Cooling is opened sample output valve 15 after finishing, and the water sample after will clearing up transfers to the detection that pick-up unit carries out the COD value.

Claims (6)

1. reaction unit is cleared up in a fast sample metering that is used for the COD detection, sample introduction air pump (1) connects sample cell (2) top, it is characterized in that: sample cell (2) bottom connects the top of the backflow pool (16) that is positioned at sample cell (2) below by pipeline, sampling valve (6) is set in the middle of pipeline, backflow pool (16) both sides, top are provided with ventilating duct and capstan, the first breather valve (7) is set on the ventilating duct, backflow pool (16) is connected to backflow air pump (4) by capstan, backflow air pump valve (5) is set on the capstan, backflow pool (16) bottom is connected to sample cell (2) top by recirculatory pipe (17), reverse flow valve (3) is set on the recirculatory pipe (17), in backflow pool (16) inner chamber measuring hoper (13) is set, the lower end of measuring hoper (13) is stretched out outside the backflow pool (16) and is connected and clears up reaction bulb (10), and measuring hoper (13) lower end is provided with metering valve (8); Metering valve (8) cuts out during to the metering of the reagent in the sample cell (2), and the first breather valve (7) is closed during backflow air pump (4) work; Outside one corral of clearing up reaction bulb (10) has electric heating piece (14).
2. reaction unit is cleared up in a kind of fast sample metering for the COD detection according to claim 1, it is characterized in that: clear up reaction bulb (10) and carry 3-6 sample feeding pipe (12), each sample feeding pipe (12) with is connected the measuring hoper (13) of a correspondence and connects, finish simultaneously metering and sample introduction that the 3-6 kind is cleared up reagent.
3. reaction unit is cleared up in a kind of fast sample metering for the COD detection according to claim 1, and it is characterized in that: sample cell (2) top is equipped with the second breather valve (18).
4. reaction unit is cleared up in a kind of fast sample metering for the COD detection according to claim 1, and it is characterized in that: backflow pool (16) is an openable structure in side.
5. reaction unit is cleared up in a kind of fast sample metering for the COD detection according to claim 1, it is characterized in that: clear up reaction bulb (10) top semiconductor cooler (11) is set.
6. reaction unit is cleared up in a kind of fast sample metering for the COD detection according to claim 1, it is characterized in that: be embedded with temperature sensor (9) in the middle of the electric heating piece (14).
CN2012103472518A 2012-09-19 2012-09-19 Quick sample injection and metering digestion reaction device for detecting COD (chemical oxygen demand) Pending CN102854054A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104049093A (en) * 2014-06-17 2014-09-17 江苏大学 Numerical-control dosing metering pump for detecting COD (chemical oxygen demand) and metering method
CN104713994A (en) * 2013-12-16 2015-06-17 恩德莱斯和豪瑟尔测量及调节技术分析仪表两合公司 Analytical device for determining a digestion parameter of a liquid sample
CN105004687A (en) * 2015-07-16 2015-10-28 江苏大学 Constant-volume liquid feeding metering method and device for COD detection
CN105158432A (en) * 2015-09-30 2015-12-16 成都源溢科技有限公司 Automatic online detecting device for hydrochemical oxygen demand
CN105158488A (en) * 2015-06-23 2015-12-16 中山欧麦克仪器设备有限公司 Rapid COD detector and preparation method for reagent thereof
CN105973687A (en) * 2016-06-13 2016-09-28 山东思睿环境设备科技有限公司 High temperature and high pressure digestion system with quadruple safety protection
CN114252569A (en) * 2020-09-24 2022-03-29 运泽惠通(北京)技术有限公司 Application flow path for water treatment or detection

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104713994A (en) * 2013-12-16 2015-06-17 恩德莱斯和豪瑟尔测量及调节技术分析仪表两合公司 Analytical device for determining a digestion parameter of a liquid sample
US10295458B2 (en) 2013-12-16 2019-05-21 Endress+Hauser Conducta Gmbh+Co. Kg Analytical device for determining a digestion parameter of a liquid sample
CN104049093A (en) * 2014-06-17 2014-09-17 江苏大学 Numerical-control dosing metering pump for detecting COD (chemical oxygen demand) and metering method
CN104049093B (en) * 2014-06-17 2016-03-02 江苏大学 The numerical control dosing volume pump detected for COD and metering method
CN105158488A (en) * 2015-06-23 2015-12-16 中山欧麦克仪器设备有限公司 Rapid COD detector and preparation method for reagent thereof
CN105004687A (en) * 2015-07-16 2015-10-28 江苏大学 Constant-volume liquid feeding metering method and device for COD detection
CN105004687B (en) * 2015-07-16 2017-07-18 江苏大学 A kind of constant volume feed liquor metering method and device for COD detections
CN105158432A (en) * 2015-09-30 2015-12-16 成都源溢科技有限公司 Automatic online detecting device for hydrochemical oxygen demand
CN105973687A (en) * 2016-06-13 2016-09-28 山东思睿环境设备科技有限公司 High temperature and high pressure digestion system with quadruple safety protection
CN114252569A (en) * 2020-09-24 2022-03-29 运泽惠通(北京)技术有限公司 Application flow path for water treatment or detection

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Application publication date: 20130102