CN103105472B - Method and system for detecting dissolved hydrogen in water - Google Patents
Method and system for detecting dissolved hydrogen in water Download PDFInfo
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- CN103105472B CN103105472B CN201210100436.9A CN201210100436A CN103105472B CN 103105472 B CN103105472 B CN 103105472B CN 201210100436 A CN201210100436 A CN 201210100436A CN 103105472 B CN103105472 B CN 103105472B
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Abstract
The invention provides a method and system for detecting dissolved hydrogen in water. The method comprises the following steps of: a, stabilizing the temperature of a water sample containing hydrogen between 20 DEG C and 30 DEG C; b, separating mixed gas containing the hydrogen from the water sample obtained in the step a; and c, analyzing the mixed gas obtained in the step b. The detection system disclosed by the invention is less prone to being disturbed by oxygen and flow, so that the measurement error is few.
Description
Technical field
The present invention relates to chemical industry measurement technology, particularly, relate to a kind of method and system detecting hydrogen gas dissolved water.
Background technology
In modern industry, the water and steam quality in therrmodynamic system is the key factor affecting the heat power equipment such as boiler, steam turbine safety, economical operation.Poor water quality can cause metal erosion, and corrosion product can make water quality become poorer, exacerbates metal erosion so further, and produces fouling.This kind of vicious cycle, causes heat power equipment shortening in serviceable life, causes great economic loss and potential safety hazard.
In order to prevent the corrosion and scaling of boiler and therrmodynamic system equipment, water and steam quality should reach certain standard.See whether it meets standard, instrument or chemical analysis method will be adopted to measure various water and steam quality, and take necessary measure according to measurement result.
Oligodynamical hydrogen analytical equipment can hydrogen content in METHOD FOR CONTINUOUS DETERMINATION steam, so that check and judge that whether steam quality is deteriorated, and can judge the variation tendency of corroding in therrmodynamic system.Instrument can on-line checkingi accurately and reliably for this, prevents the corrosion of the therrmodynamic system such as boiler and steam turbine equipment, ensures its safe operation.
Instrument measurement is that its corresponding for measured parameter measuring unit standard volume compares by method by experiment, and then draws numerical value, and the device realizing this comparison is exactly measurement instrument.
Oligodynamical hydrogen analytical equipment can hydrogen content in METHOD FOR CONTINUOUS DETERMINATION steam, it can not obtain scarce chemical instruments in industry, it for the water and steam quality in supervision therrmodynamic system, detect corrosion rate trend, judge pollution source, prevent fouling and salification, guarantee heat power equipment safety and economic operation and extension device time between overhauls(TBO) and serviceable life from all playing an important role.
At present, the domestic like product also not having oligodynamical hydrogen analytical equipment, and external product many employings determination of electrode, use result according to user, have the following disadvantages:
1, due to the interference by oxygen with by flow effect, measure and there is error;
2, regularly need to change film and electrolytic solution, and maintenance increases, maintenance cost is high;
3, electrode vulnerable to pollution, electrode life is shorter, and renewal cost is higher.
Summary of the invention
An object of the present invention is to provide a kind of method detecting hydrogen gas dissolved water.
Another object of the present invention is to provide the system detecting hydrogen gas dissolved water.
One aspect of the present invention provides a kind of method detecting hydrogen gas dissolved water, and the method comprises the following steps: a. first by the temperature stabilization of the water sample containing hydrogen at 20-30 DEG C; B. the mixed gas containing hydrogen is isolated in the water sample obtained by step a; C. the mixed gas that step b obtains is analyzed.
Preferably, in described step a: first the water sample containing hydrogen is passed through thermostatic water-jacket, by the temperature stabilization of water sample at 25 DEG C.
Preferably, in described step b, the water sample that step a obtains enters vacuum separation room, and in vacuum separation room, isolate mixed gas and remaining water sample, and remaining water sample is flowed out from water sample outlet by overflow groove.
Preferably, described vacuum separation room is for vacuumizing water pump or the described vacuum separation room vacuum separation room for being combined by separation bell jar, both Venturi tubes.
Preferably, in described step c, the mixed gas obtained by step b detects the content of hydrogen in heat conductometer.
Preferably, the reference elements of described heat conductometer and measuring sensor are all placed in the gas of saturation water, and described heat conductometer is wrapped in thermostatic water-jacket.
The present invention additionally provides a kind of system realizing described method on the other hand, this system comprises with lower component: sample water inlet, thermostatic water-jacket, draft tube, vacuum separation room, overflow groove, heat conductometer, air saturator and water sample outlet, described sample water inlet is connected to the inlet end of vacuum separation room by thermostatic water-jacket, draft tube is connected to vacuum separation room, gas outlet end in vacuum separation room is connected to one end of heat conductometer, liquid outlet end in vacuum separation room is connected to water sample outlet by overflow groove, the other end of heat conductometer is connected with air saturator, and described thermostatic water-jacket parcel vacuum separation room, heat conductometer and air saturator.
Preferably, this system comprises with lower component: valve and flowmeter, it is characterized in that, described sample water inlet is connected by pipeline with valve inlet, valve export is connected by pipeline with flowmeter entrance, flowmeter outlet is connected to the inlet end of vacuum separation room by thermostatic water-jacket, draft tube is connected to vacuum separation room, the gas outlet end of vacuum separation room is connected to one end of heat conductometer, the liquid outlet end of vacuum separation room is connected to water sample outlet by overflow groove, the other end of heat conductometer is connected with air saturator, and described thermostatic water-jacket parcel vacuum separation room, heat conductometer and air saturator.
Preferably, this system also comprises zero correction valve, and described zero correction valve is connected to described thermostatic water-jacket for controlling vacuum separation room.
Preferably, described system also comprises faraday's electrolytic cell, and one end of described faraday's electrolytic cell is connected to flowmeter outlet, and the other end of faraday's electrolytic cell is connected to the water inlet end of thermostatic water-jacket.
Preferably, described system also comprises constant current groove, and the outlet of described valve is also connected to one end of constant current groove by pipeline, and is connected to water sample outlet by the other end of constant current groove by pipeline.
Air saturator of the present invention is the water pot filling water, and this water pot is not connected with air, is connected to the other end of heat conductometer by cotton pipe.
Beneficial effect of the present invention is: the measurement range of dissolved hydrogen analytical equipment of the present invention can be refined to 0-20 micrograms per litre, and measuring accuracy can reach positive and negative 0.2 micrograms per litre.And detection system of the present invention is not easy the interference being subject to oxygen and flow, and measuring error is little.
Accompanying drawing explanation
Fig. 1 represents the structural drawing of the embodiment of the present invention 1 system.
Fig. 2 represents the structural drawing of the embodiment of the present invention 2 system.
Fig. 3 represents the vacuum separation room be made up of Venturi tube, separation chamber's bell jar of the present invention.
Embodiment
Following examples are only for explaining the present invention, and can not be used for limiting the present invention, the modification made in scope, replacement, change are all in protection scope of the present invention.
Embodiment 1
See Fig. 1, the present invention detects the system of dissolved hydrogen in water and comprises sample water inlet 1, valve 2, constant current groove 3, flowmeter 4, thermostatic water-jacket 5, draft tube 11, vacuum separation room 6, heat conductometer 7, air saturator 8 and water sample outlet 9.
Sample water inlet 1 is connected by pipeline with the inlet end of valve 2, the endpiece of valve 2 exports 9 with constant current groove 3 and water sample successively by pipeline and is connected, another endpiece of valve 2 is connected with the entrance of flowmeter 4, and the outlet of flowmeter 4 is connected to the entrance of vacuum separation room 6 by thermostatic water-jacket 5, an outlet of vacuum separation room 6 is connected with water sample outlet 9 by overflow groove 10 by pipeline, another outlet of vacuum separation room 6 is connected to one end of heat conductometer 7, and the other end of heat conductometer 7 connects air saturator 8.Draft tube 11 is connected to vacuum separation room 6, and the vacuum separation room 6 in the present embodiment, heat conductometer 7, air saturator 8 and draft tube 11 wrapped up by thermostatic water-jacket 5.
Embodiment 2
See Fig. 2, the present embodiment is close with embodiment 1, system unlike the present embodiment also comprises faraday's electrolytic cell 12 and zero correction valve 13, and faraday's electrolytic cell 12 is placed between the outlet of flowmeter 4 and the entrance of thermostatic water-jacket 5, and zero correction valve 13 is placed in thermostatic water-jacket downstream.
Embodiment 3
Fig. 3 represents vacuum separation room of the present invention, this vacuum separation room by Venturi tube 100 be separated bell jar 200 and form, be separated bell jar 200 and cover on outside Venturi tube 100, Venturi tube comprises liquid-inlet end 101, liquid outlet end 102 and gas vent 103.
Embodiment 4
the detection of hydrogen gas dissolved water
See Fig. 1, Fig. 1 is the flow process composition structural drawing of system according to a first embodiment of the present invention, containing hydrogen water sample first from sample water inlet 1 through needle valve 2, sample is divided into two parts, a part enters the constant current groove 3 providing certain pressure, and discharged by water sample outlet 9, another part is successively through flowmeter 4 and thermostatic water-jacket 5, constant temperature water sample passes through thermostatic water-jacket 5 by the temperature stabilization of water sample at 25 degrees Celsius, water sample enters vacuum separation room 6 by thermostatic water-jacket 5, now the zero correction valve of vacuum separation room is in closure state, fresh air in saturation water sucks in vacuum separation room 6 by draft tube 11, the separation chamber that vacuum separation room in the present embodiment combines for the separation bell jar shown in embodiment 3 and Venturi tube, the liquid-inlet end 101 that air enters Venturi tube 100 is brought in current, because the flow velocity of water sample in Venturi tube is very fast, so the mixed gas in water sample is constantly separated with water, isolated water enters overflow groove 10 from the liquid outlet end 102 of Venturi tube, discharge from water sample outlet 9.Overflow groove in the present embodiment is the tank filling water, combines, combined, thus achieve the object be separated under vacuum condition between water and gas by overflow groove with the bell jar that is separated outside Venturi tube with the bell jar 200 that is separated of Venturi tube outer 100.Then be diffused into around the measuring sensor of heat conductometer 7 from the isolated mixed gas of gas vent 103 of the Venturi tube of vacuum separation room, enter heat conductometer 7 to detect, the temperature of heat conductometer 7 is 25 degrees Celsius, heat conductometer directly connects air saturator 8, air saturator in the present embodiment is the water pot filling water, this water pot does not contact with the air in the external world, is connected to one end of heat conductometer by cotton pipe.Due to the effect that Venturi tube vacuumizes, gas in air saturator and liquid can be brought in heat conductometer, vacuum separation room 6 in the present embodiment, draft tube 11, heat conductometer 7 and air saturator 8 are all wrapped in thermostatic water-jacket 5, so their temperature is identical with the temperature of thermostatic water-jacket 5.
While air and hydrogen are diffused into heat conductometer, gas in air saturator 8 and water also form water vapor and enter in heat conductometer, because heat conductometer 7 temperature is 25 degree, so reference elements and measuring sensor are all full of by the saturated gas in air saturator in saturated water vapour.Because water vapor can affect measurement result, so the reference elements in heat conductometer and measuring sensor are all immersed in saturated gas, like this reference elements and measuring sensor are produced to the impact of equivalent, be unlikely to make the electric bridge of heat conductometer to produce uneven.
Read the reading of heat conductometer detecting electrode, thus calculate the hydrogen content in water sample.
Embodiment 5
the determination at heat conductometer zero point
See Fig. 2, when determining analytical equipment zero point, now the zero correction valve 13 of vacuum separation room 6 is in opening.
Water sample first from sample water inlet 1 through needle valve 2, sample is divided into two parts, a part enters the constant current groove 3 providing certain pressure, another part enters in thermostatic water-jacket 5 through flowmeter 4 and faraday's electrolytic cell 12 successively, the temperature of thermostatic water-jacket 5 remains on 25 degrees Celsius, therefore the temperature of water sample is also in this temperature, by draft tube 11 to vacuum separation room insufflation gas, vacuum separation room in the present invention is by being separated bell jar and Venturi tube forms, vacuum separation room 6 zero correction valve 13 be in state at zero point, now separation chamber 6 is in the state of closedown, the gas of water sample and saturation water is directly discharged to water sample outlet 9 from thermostatic water-jacket 5 by overflow groove 10 and discharges, oxygen diffusion in water sample is in heat conductometer 7, the temperature of heat conductometer remains on 25 degrees Celsius, heat conductometer directly connects air saturator 8, water and air is filled in the space of air saturator.
While oxygen diffusion to heat conductometer, in air saturator 8 gas and water also form saturation water gas and enter in heat conductometer 7, because heat conductometer temperature is 25 DEG C, thus reference elements and measuring sensor be all full of at the gas of saturation water.Because the water sample in the present embodiment is not separated, so the numerical value shown in heat conductometer should be corrected to zero.
Embodiment 6
heat conductometer is corrected by faraday's electrolytic cell
When correcting heat conductometer 7, the general water sample adopted not containing hydrogen, the zero correction valve 13 now controlling vacuum separation room 6 is in closed condition.
See Fig. 2, the process flow diagram of present system, containing hydrogen water sample first from sample water inlet 1 through needle valve 2, sample is divided into two parts, a part enters the constant current groove 3 providing certain pressure, and discharged by water sample outlet 9, another part enters faraday's electrolytic cell 12 by flowmeter 4, by the DC current of 2mA between faraday's electrolytic cell 12, hydrogen is produced from one of them electrode, with the water sample of hydrogen through thermostatic water-jacket 5, thermostatic water-jacket 5 by the temperature stabilization of water sample at 25 degrees Celsius, water sample enters vacuum separation room by thermostatic water-jacket 5, and (the vacuum separation room in the present embodiment is by being separated bell jar, Venturi tube forms) 6, air is brought in current through one end of vacuum separation room 6, because the flow velocity of water sample in Venturi tube is very fast, so the air in water sample is constantly separated with water with the mixed gas of hydrogen, isolated water is by overflow groove 10, discharge from water sample outlet 9.Then be diffused into around the measuring sensor of heat conductometer 7 from the mixed gas of the isolated air in separation chamber 6 and hydrogen, enter heat conductometer 7 to detect, the temperature of heat conductometer is 25 degrees Celsius, and heat conductometer 7 directly connects air saturator 8, fills water and air in the space of air saturator.Heat conductometer in the present embodiment and air saturator are all wrapped in thermostatic water-jacket, so their temperature and the temperature close of thermostatic water-jacket.
While air and hydrogen are diffused into heat conductometer, gas in air saturator and water also form water vapor and enter in heat conductometer, because heat conductometer temperature is 25 degrees Celsius, so reference elements and measuring sensor are all full of by the saturated gas in air saturator in saturated water vapour.Because water vapor can affect measurement result, so the reference elements in heat conductometer and measuring sensor are all immersed in saturated gas, like this reference elements and measuring sensor are produced to the impact of equivalent, be unlikely to make the electric bridge of heat conductometer to produce uneven.Now, due to the hydrogen that the hydrogen recorded in heat conductometer obtains from electrolysis in faraday's electrolytic cell, so the amounts of hydrogen of the amounts of hydrogen of the Current calculation that can be passed through by faraday's electrolytic cell and the display of heat conductometer reading is compared, thus correct the reading of heat conductometer by the amounts of hydrogen calculated.
Such as, the electric current of the 2mA passed through for the present invention, the flow of water sample is 210ml, and the hydrogen recruitment of now heat conductometer display should be: Δ H
2=630*A/V and Δ H
2=630*2/210=6 micrograms per litre, Δ H in formula
2represent the recruitment of hydrogen, unit: micrograms per litre, A represents Faradaic current, unit: mA, V represent water sample flow, unit: ml, and the reading calculated by faraday's electrolytic cell corrects the reading of heat conductometer.
Claims (6)
1. detect a method for hydrogen gas dissolved water, the method comprises the following steps:
A. first by the temperature stabilization of the water sample containing hydrogen at 20-30 DEG C;
B. the mixed gas containing hydrogen is isolated in the water sample obtained by step a;
C. the mixed gas that step b obtains is analyzed;
Wherein in described step a: first the water sample containing hydrogen is passed through thermostatic water-jacket, by the temperature stabilization of water sample at 25 DEG C;
Wherein in described step b, the water sample that step a obtains enters vacuum separation room, and in vacuum separation room, isolate mixed gas and remaining water sample, and remaining water sample is flowed out from water sample outlet by overflow groove;
Wherein said vacuum separation room is for vacuumizing water pump or the described vacuum separation room vacuum separation room for being combined by separation bell jar, both Venturi tubes;
Wherein in described step c, the mixed gas obtained by step b detects the content of hydrogen in heat conductometer;
The reference elements of described heat conductometer and measuring sensor are all placed in the gas of saturation water, and described heat conductometer is wrapped in thermostatic water-jacket.
2. one kind realizes the system of method described in claim 1, this system comprises with lower component: sample water inlet, thermostatic water-jacket, draft tube, vacuum separation room, overflow groove, heat conductometer, air saturator and water sample outlet, it is characterized in that, described sample water inlet is connected to the inlet end of vacuum separation room by thermostatic water-jacket, draft tube is connected to vacuum separation room, gas outlet end in vacuum separation room is connected to one end of heat conductometer, liquid outlet end in vacuum separation room is connected to water sample outlet by overflow groove, the other end of heat conductometer is connected with air saturator, and described thermostatic water-jacket parcel vacuum separation room, heat conductometer and air saturator.
3. system according to claim 2, this system also comprises: valve and flowmeter, it is characterized in that, described sample water inlet is connected by pipeline with valve inlet, valve export is connected by pipeline with flowmeter entrance, and flowmeter outlet is connected to the inlet end of vacuum separation room by thermostatic water-jacket.
4. system according to claim 3, wherein, this system also comprises zero correction valve, and described zero correction valve is connected to described thermostatic water-jacket for controlling vacuum separation room.
5. system according to claim 3, wherein this system also comprises faraday's electrolytic cell, and one end of described faraday's electrolytic cell is connected to flowmeter outlet, and the other end of faraday's electrolytic cell connects the water inlet end of thermostatic water-jacket.
6. system according to claim 3, wherein this system also comprises constant current groove, and the outlet of described valve is also connected to one end of constant current groove by pipeline, and is connected to water sample outlet by the other end of constant current groove by pipeline.
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| CN201210100436.9A CN103105472B (en) | 2012-04-06 | 2012-04-06 | Method and system for detecting dissolved hydrogen in water |
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| CN201210100436.9A CN103105472B (en) | 2012-04-06 | 2012-04-06 | Method and system for detecting dissolved hydrogen in water |
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| CN103105472B true CN103105472B (en) | 2015-05-27 |
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| CN102128894A (en) * | 2010-12-29 | 2011-07-20 | 北京华电云通电力技术有限公司 | Online analytical chromatograph and chromatographic detection method for gases in insulating oil |
| JP2014010092A (en) * | 2012-07-02 | 2014-01-20 | Shimadzu Corp | Gas analyzer |
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2012
- 2012-04-06 CN CN201210100436.9A patent/CN103105472B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101183087A (en) * | 2007-12-27 | 2008-05-21 | 中国计量科学研究院 | Trace quantity dissolved oxygen instrument test calibration system and calibrate method thereof |
| CN201382948Y (en) * | 2009-04-16 | 2010-01-13 | 杭州申昊信息科技有限公司 | Online monitoring system of gas in transformer oil |
| CN101539551A (en) * | 2009-04-23 | 2009-09-23 | 思源电气股份有限公司 | Transformer oil chromatographic detection system and detection method thereof |
| CN201811936U (en) * | 2010-03-18 | 2011-04-27 | 中国船舶重工集团公司第七一八研究所 | Self-starting hydrogen concentration measuring device for nuclear power station |
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| JP2014010092A (en) * | 2012-07-02 | 2014-01-20 | Shimadzu Corp | Gas analyzer |
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