CN102494936A - Measuring cell device for trace dissolved oxygen water and device for preparing trace dissolved oxygen water - Google Patents
Measuring cell device for trace dissolved oxygen water and device for preparing trace dissolved oxygen water Download PDFInfo
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- CN102494936A CN102494936A CN2011104012432A CN201110401243A CN102494936A CN 102494936 A CN102494936 A CN 102494936A CN 2011104012432 A CN2011104012432 A CN 2011104012432A CN 201110401243 A CN201110401243 A CN 201110401243A CN 102494936 A CN102494936 A CN 102494936A
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Abstract
The invention discloses a trace dissolved oxygen electrode measuring cell, which comprises an organic glass shell cell body 1, wherein a sealing cover 2 is arranged on the upper part of the cell body 1. A plurality of round holes 5 for mounting dissolved oxygen measuring electrodes are formed in the cover according to needs of a user; oxygen electrodes coated with polytetrafluoroethylene films are inserted into the round holes 5 for sealing the holes; a ventilating nozzle 3 is formed in the cover and is connected with a ventilating tube of another prepared oxygen steel cylinder; a lower end of the ventilating nozzle 3 is connected with a plastic hose 4 with the inner diameter of about phi 2mm until the ventilating nozzle 3 is inserted to the bottom of a bottle; a ventilating nozzle 6 is formed above the cover; a lower end of the ventilating nozzle 6 is flush with an organic glass cover; a plastic tube with the inner diameter of about phi 2mm is inserted into the upper end of the ventilating nozzle 6; the ventilating nozzle 3 is used for introducing needed gases into the measuring cell; the plastic hose 4 is used for guiding the gases to the lower part of liquid; and the ventilating nozzle 6 is used for providing an air outlet to make air bubbles which are generated on the liquid level escape from the holes. Distilled water is introduced to the liquid level which is about 5mm away from the surface of the measuring cell in an electrode measuring cell body, and steel cylinder gas with different oxygen content are introduced into the cell. A measuring instrument has high precision, linearity and repeatability.
Description
Technical field
The present invention relates to a kind of measuring cell device of trace dissolved oxygen appearance water and preparation facilities of trace dissolved oxygen water of preparing, be used for precision, linearity, the reappearance of oligodynamical analyzer are tested.
Background technology
1. the present invention relates to a kind of technology for preparing trace dissolved oxygen appearance water, and its oxygen level can be prepared various concentration according to user's requirement.
2. the dissolved oxygen DO in the common water is in to be protected and state; Its content is mg/L (ppm level); But because of nuclear power plant, fuel-burning power plant, large scale integrated circuit prepare the low more good more μ g/L (ppb level) that is of oxygen level in the special place such as water, boiler feed water, this is under high-temperature and high-pressure conditions, very easily boiler, genset and auxiliary device thereof to be produced corrosion because of oxygen.Or water quality is caused the product to be processed adverse effect because of the existence of oxygen.Must carry out pre-treatment to the water before the access arrangement like this, its method is generally physical method-thermal de-aeration; Chemical deoxidization (interpolation reductive agent).Deaerating effect should have monitoring, uses the low concentration dissolved oxygen meter to carry out on-line monitoring usually.The existing how tame renowned company of dissolved oxygen meter is producing at present; Domestic also have corresponding instrument manufacturer, a supply correlate meter.But there is not a family that corresponding hypoxemia examination criteria or method can be provided.Indivedual production firms are arranged when buying instrument, so-called zero oxygen sample standard annex is provided, supply the user that instrument is carried out zero oxygen and demarcate.But this does not obtain the permission of any authoritative standard, and according to me it is carried out the full pattern analysis, and its oxygen level is also non-vanishing!
3. be example with regard to generation current factory, be: chemical method comparison method: according to GB 12157-1989 GB, carry out appearance water oxygen analysis on Content, thereby differentiate the precision of dissolved oxygen meter with colourimetry to the detection method of instrument.But this method exists very big uncertainty; Because when the oxygen content in the water reaches the μ g/L order of magnitude; Differing several ug/L is to be difficult to confirm, for example: when water oxygen level was lower than 10 μ g/L, the aberration that its chemical method produces was unable to recognize; But in fact the oxygen in the stove water is not more than 9 μ g/L by national standard, after the actual deoxygenation often between 0.5-3 μ g/L.The method of generation current factory is according to GB 12157-1989 GB, adds the accumulating experience of genset operating mode, with belonging to the quality of confirming dissolved oxygen meter qualitatively basically.But this is extremely unscientific.
4. the present invention is exactly that the very important person is for making the LDO water sample; And its oxygen level can prepare various concentration according to user's requirement, come to examine and determine effectively dissolved oxygen meter to the true precision of low concentration dissolved oxygen DO, linearity, reappearance etc. to the vital index of instrument.
5. the test stone of the domestic and international LDO appearance of just investigating is not at present also carried out effective calibration method to it.The present invention provides a brand-new standard method to this product.
Summary of the invention
1. the present invention is exactly that the very important person is for making the LDO water sample; And its oxygen content can prepare various concentration according to user's requirement, come to measure effectively dissolved oxygen meter to the true precision of low concentration dissolved oxygen DO, linearity, reappearance etc. to the vital index of instrument.
2. adopt following technical scheme (seeing accompanying drawing 1, accompanying drawing 2) for reaching above-mentioned requirements the present invention:
Accompanying drawing 1: " the trace dissolved oxygen measuring cell " explanation
Fig. 1 is a trace dissolved oxygen electrode measurement pond, and it comprises: lucite shell pond body 1, a seal cover 2 is done with same lucite in body top, pond.Processing a number on the cover mounting hole garden oxygen measuring electrode 5, a circular aperture 5 or more holes can be more, depending on the number of holes needs to determine garden, park size holes 5 may be determined according to electrode size processing, the PTFE film on the oxygen electrode package insert of the park to seal the holes 5 holes in the lid with a ventilation tipped 3, ventilation and other equipment connected to the mouth three outtakes oxygen cylinders connected; ventilation tipped 3 Connect an inner diameter of about Φ2mm bottom of the plastic hose 4, the hose line to the bottom of the bottle.Cover side opened a ventilation tipped 6, then the mouth 6 and plexiglass cover flat bottom, the upper plug straight about Φ2mm within a plastic tube.The effect that connects mouth 3 of ventilation is in the gas feeding pond with need usefulness, and the plastic flexible pipe of its lower end is that gas is directed at body below, pond.The effect that connects mouth 6 of ventilation provides a vent port, lets the bubble that produces on the liquid level from the hole, run away, and feeds distilled water to liquid level in the body of trace dissolved oxygen electrode measurement pond earlier from the about 5mm of pond face;
Accompanying drawing 2: " device of preparation trace dissolved oxygen " explanation
Steel cylinder 1 is selected for use 99.99% nitrogen to mould pipe 3 through gas pressure reducer 2 usefulness earlier to lead in the pond 4 (being the trace dissolved oxygen measuring cell of Fig. 1), regulate the size of reduction valve 2, liquid level is produced till the continuous minute bubbles.The bubble that liquid level produces can be run away from gas outlet (6 Fig. 1), its objective is the existing dissolved oxygen DO of driving away in the distilled water, because nitrogen has no and should ring oxygen electrode, replaces the dissolved oxygen DO in the water with nitrogen; Duration of ventilation shows pond body size and decide that general pond body capacity needs 1 hour approximately when 500ml, at this moment between in can oxygen in water be driven away, the cable of electrode is connected to simulating on the good dissolved oxygen DO display instrument 5 of electric Equipment Alignment;
Feed nitrogen and observe dissolved oxygen DO display instrument 5 simultaneously, its oxygen oxygen level can be run toward little direction very soon, can not down run until displayed value again, at this moment is exactly zero oxygen value.With calibrating indicating instrument to 0.0 μ g/L;
Change steel cylinder 1 into off-the-shelf low content of oxygen gas cylinder; Use with above-mentioned same method and feed measured oxygen to pond body 4; But the time need not be so much; Observe dissolved oxygen DO display instrument 5 readings simultaneously feeding this gas, until displayed value stabilize to, the oxygen level of this steel cylinder this moment and the difference of instrument displayed value are the precision of instrument.
Feed the gas of off-the-shelf other two kinds of low content of oxygen gas cylinders; Method of operating is the same; Observe dissolved oxygen DO display instrument 5 readings simultaneously feeding this gas, until displayed value stabilize to, the oxygen level of this steel cylinder this moment and the difference of instrument displayed value are the precision of instrument; Through measurement, just calculate the linearity and the precision of instrument at an easy rate to these three kinds of variable concentrations gases.
Also answer to the gas that feeds previous concentration again after feeding other concentration gases, observe the instrument displayed value, repeat to do continuously 6 times, can calculate the reappearance of this instrument with the standard mathematical algorithm.(computing formula 1.b in seeing Appendix)
The calculating of calibrating gas and dissolved oxygen concentration (computing formula 1.a in seeing Appendix)
1. by relevant national Specification, its unit is a gas phase percentage oxygen concentration in the preparation of calibrating gas.So that but its precision is a rope is former.
2. airborne oxygen concentration: be 20.95% in clean dry air; Under the virtual condition, water loading of the air between 1-3%, gets 20.7% after revising usually usually with relative humidity variations.(as wanting accurate Calculation, follow, revise after looking into absolute moisture content concentration according to temperature, relative humidity.)
3. the calculating of the oxygen concentration in feeding pond formula is:
As＝Aw×C÷Aa
In the formula: As---dissolved oxygen concentration
Aw---saturated oxygen concentration in the water under this temperature (note: saturated oxygen concentration is different in the water of different temperatures, the table 1 of seeing Appendix)
C---the degree of oxygen in the steel cylinder
Aa---airborne oxygen concentration
Contain the different preparation steel cylinder of percentage oxygen content concentration with two bottles is that example is calculated corresponding oxygen concentration at present:
A. routine: first bottle of oxygen content is 0.303%, when temperature is 25 ℃
As1＝8.24mg/L×0.00303÷0.207＝120.6μg/L
B. routine: second bottle of oxygen content is 125 * 10-6, when temperature is 25 ℃
As1＝8.24mg/L×0.000125÷0.207＝4.98μg/L
Description of drawings
Fig. 1: the measuring cell device of trace dissolved oxygen water
1. organic glass measuring cell 4. imports the conduit at the bottom of the pond with gas
2. organic glass loam cake 5. is installed the circular hole of dissolved oxygen electrode
3. air inlet introducing port 6. is because of importing the vent port of residual gas behind the gas
Fig. 2: trace dissolved oxygen water preparation apparatus
1. the measuring cell of gas storage steel cylinder 4. trace dissolved oxygen water
2. steel cylinder reduction valve 5. dissolved oxygen meter displays of giving vent to anger
3. post-decompression gas is imported the measuring cell of trace dissolved oxygen water
Embodiment
Do a trace dissolved oxygen electrode measurement pond, it comprises: lucite shell pond body 1, a seal cover 2 is done with same lucite in body top, pond.Processing a number on the cover mounting hole garden oxygen measuring electrode 5, a circular aperture 5 or more holes can be more, depending on the number of holes needs to determine garden, park size holes 5 may be determined according to electrode size processing, the PTFE film on the oxygen electrode package insert of the park to seal the holes 5 holes in the lid with a ventilation tipped 3, ventilation and other equipment connected to the mouth three outtakes oxygen cylinders connected; ventilation tipped 3 connect an inner diameter of about Φ2mm bottom of the plastic hose 4, the hose line to the bottom of the bottle.Cover side opened a ventilation tipped 6, then the mouth 6 and plexiglass cover flat bottom, the upper plug straight about Φ2mm within a plastic tube.The effect that connects mouth 3 of ventilation is that the plastic flexible pipe of its lower end is that gas is directed at the liquid below in the gas feeding pond with need usefulness.The effect that connects mouth 6 of ventilation provides a vent port, lets the bubble that produces on the liquid level from the hole, run away, and feeds distilled water to liquid level in the body of trace dissolved oxygen electrode measurement pond earlier from the about 5mm of pond face;
Use the calibrating gas steel cylinder, select for use 99.99% nitrogen to mould pipe 3 earlier and lead in the dissolved oxygen sensing pond 4 (being the trace dissolved oxygen measuring cell of Fig. 1), regulate the size of reduction valve 2, make till the continuous minute bubbles of liquid level generation through gas pressure reducer 2 usefulness.The bubble that liquid level produces can be run away from gas outlet (6 Fig. 1), its objective is the existing dissolved oxygen DO of driving away in the distilled water, because nitrogen has no and should ring oxygen electrode, replaces the dissolved oxygen DO in the water with nitrogen.Duration of ventilation shows pond body size and decides that general pond body capacity needs 1 hour approximately when 500ml; Can oxygen in water be driven away at this moment, the cable of electrode is connected to be used on the good dissolved oxygen DO display instrument 5 of the electric Equipment Alignment of simulation, feeds nitrogen and observes dissolved oxygen DO display instrument 5 simultaneously; Its oxygen oxygen level can be run toward little direction very soon; Can not down run until displayed value, at this moment be exactly zero oxygen value, with calibrating indicating instrument to 0.0 μ g/L again; Feed the gas of off-the-shelf other two kinds of low content of oxygen gas cylinders then; Method of operating is the same; Observe dissolved oxygen DO display instrument 5 readings simultaneously feeding this gas, until displayed value stabilize to, the oxygen level of this steel cylinder this moment and the difference of instrument displayed value are the precision of instrument; Through measurement, just calculate the linearity and the precision of instrument at an easy rate to these three kinds of variable concentrations gases.
Measuring accuracy and instrument linear calibration example:
1 usefulness nitrogen steel cylinder is driven away in the measuring cell behind the dissolved oxygen DO, and the dissolved oxygen DO displayed value is 0.6 μ g/L, and in Fig. 2 display instrument, the adjusting instrument zero is 0.00g/L.
2 difference aerating oxygen steel cylinders are to measuring cell, and their percentage composition is respectively: 125 * 10
-6, 252 * 10
-6, 408 * 10
-6, measurement result is shown in table 1
The liquid temperature is 24 ℃ in the pond, and this instrument is in 0-20ug/L range ability table 1
Reappearance example: see table 2
Reappearance is (with 252 * 10
-6Oxygen in the steel cylinder is tested) table 2
Follow according to formula 1 and calculate this instrument reappearance S=99.6%
Annex
1. criterion calculation formula:
A. oxygen concentration calculates formula
As＝Aw×C÷Aa…………………………………………………………(1.a)
In the formula: As---dissolved oxygen concentration
Aw---saturated oxygen concentration in the water under this temperature (note: saturated oxygen concentration is different in the water of different temperatures, the table 1 of seeing Appendix)
C---the degree of oxygen in the steel cylinder
Aa---airborne oxygen concentration
B. reappearance computing formula
In the formula: S---reappearance
Ci---the i time measured value
2. water saturation dissolved oxygen DO (normal atmosphere is depressed) concentration table (unit: mg/L) table 1 under the different temperatures
| Temperature (℃) | Concentration (mg/L) | Temperature (℃) | Concentration (mg/L) |
| 0 | 14.60 | 25 | 8.24 |
| 1 | 14.19 | 26 | 8.09 |
| 2 | 13.81 | 27 | 7.95 |
| 3 | 13.44 | 28 | 7.81 |
| 4 | 13.09 | 29 | 7.67 |
| 5 | 12.75 | 30 | 7.54 |
| 6 | 12.43 | 31 | 7.41 |
| 7 | 12.12 | 32 | 7.28 |
| 8 | 11.83 | 33 | 7.16 |
| 9 | 11.55 | 34 | 7.05 |
| 10 | 11.27 | 35 | 6.93 |
| 11 | 11.01 | 36 | 6.82 |
| 12 | 10.76 | 37 | 6.71 |
| 13 | 10.52 | 38 | 6.61 |
| 14 | 10.29 | 39 | 6.51 |
| 15 | 10.07 | 40 | 6.41 |
| 16 | 9.85 | 41 | 6.31 |
| 17 | 9.65 | 42 | 6.22 |
| 18 | 9.45 | 43 | 6.13 |
| 19 | 9.26 | 44 | 6.04 |
| 20 | 9.07 | 45 | 5.95 |
| 21 | 8.90 | 46 | 5.86 |
| 22 | 8.72 | 47 | 5.78 |
| 23 | 8.56 | 48 | 5.70 |
| 24 | 8.40 | 49 | 5.62 |
Claims (2)
1. do a trace dissolved oxygen electrode measurement pond, it comprises: lucite shell pond body 1, a seal cover 2 is done with same lucite in body top, pond.Processing a number on the cover mounting hole garden oxygen measuring electrode 5, a circular aperture 5 or more holes can be more, depending on the number of holes needs to determine garden, park size holes 5 may be determined according to electrode size processing, the PTFE film on the oxygen electrode package insert of the park to seal the holes 5 holes in the lid with a ventilation tipped 3, ventilation and other equipment connected to the mouth three outtakes oxygen cylinders connected; ventilation tipped 3 connect an inner diameter of about Φ2mm bottom of the plastic hose 4, the hose line to the bottom of the bottle.Cover side opened a ventilation tipped 6, then the mouth 6 and plexiglass cover flat bottom, the upper plug straight about Φ2mm within a plastic tube.The effect that connects mouth 3 of ventilation is that the plastic flexible pipe of its lower end is that gas is directed at the liquid below in the gas feeding pond with need usefulness.The effect that connects mouth 6 of ventilation provides a vent port, lets the bubble that produces on the liquid level from the hole, run away, and feeds distilled water to liquid level in the body of trace dissolved oxygen electrode measurement pond earlier from the about 5mm of pond face;
2. use the calibrating gas steel cylinder, select for use 99.99% nitrogen to mould pipe 3 earlier and lead in the dissolved oxygen sensing pond 4 (being the trace dissolved oxygen measuring cell of Fig. 1), regulate the size of reduction valve 2, make till the continuous minute bubbles of liquid level generation through gas pressure reducer 2 usefulness.The bubble that liquid level produces can be run away from gas outlet (6 Fig. 1), its objective is the existing dissolved oxygen DO of driving away in the distilled water, because nitrogen has no and should ring oxygen electrode, replaces the dissolved oxygen DO in the water with nitrogen.Duration of ventilation shows pond body size and decides that general pond body capacity needs 1 hour approximately when 500ml; Can oxygen in water be driven away at this moment; The cable of electrode is connected to be used on the good dissolved oxygen DO display instrument 5 of the electric Equipment Alignment of simulation, feeds nitrogen and observes dissolved oxygen DO display instrument 5 simultaneously, and its oxygen oxygen level can be very fast toward little direction race; Can not down run until displayed value, at this moment be exactly zero oxygen value again.With calibrating indicating instrument to 0.0 μ g/L; Feed the gas of off-the-shelf other two kinds of low content of oxygen gas cylinders then; Method of operating is the same; Observe dissolved oxygen DO display instrument 5 readings simultaneously feeding this gas, until displayed value stabilize to, the oxygen level of this steel cylinder this moment and the difference of instrument displayed value are the precision of instrument; Through measurement, just calculate the linearity and the precision of instrument at an easy rate to these three kinds of variable concentrations gases.
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| CN2011104012432A CN102494936A (en) | 2011-12-06 | 2011-12-06 | Measuring cell device for trace dissolved oxygen water and device for preparing trace dissolved oxygen water |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107305193A (en) * | 2016-04-19 | 2017-10-31 | 季春峰 | Trace quantity dissolved oxygen instrument on-line calibration and measuring system and method |
| CN111044589A (en) * | 2019-12-02 | 2020-04-21 | 河北冀研能源科学技术研究院有限公司 | Preparation method of zero-point correction oxygen-free water for electrodes of online dissolved oxygen meter in thermal power plant |
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| CN2692664Y (en) * | 2003-10-20 | 2005-04-13 | 中国环境科学研究院 | Small degradation meter for real-time monitoring concentration of dissolved oxygen |
| WO2007023283A2 (en) * | 2005-08-25 | 2007-03-01 | Isis Innovation Limited | Detection of oxygen, carbon dioxide and anaesthetic agents |
| WO2007029245A2 (en) * | 2005-09-07 | 2007-03-15 | Medis Technologies Ltd. | Electrochemical method and system for detection of trace explosives |
| JP2007256025A (en) * | 2006-03-22 | 2007-10-04 | Kajima Corp | Method and apparatus for detecting dissolved oxygen in underground water |
| JP2008032691A (en) * | 2006-06-29 | 2008-02-14 | Fuji Electric Systems Co Ltd | Water quality monitoring system and method |
| JP2009257854A (en) * | 2008-04-15 | 2009-11-05 | Yokogawa Electric Corp | Electrochemical sensor |
| CN201637705U (en) * | 2010-04-20 | 2010-11-17 | 贵阳学通仪器仪表有限公司 | Dual-channel online dissolved oxygen meter |
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- 2011-12-06 CN CN2011104012432A patent/CN102494936A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2692664Y (en) * | 2003-10-20 | 2005-04-13 | 中国环境科学研究院 | Small degradation meter for real-time monitoring concentration of dissolved oxygen |
| WO2007023283A2 (en) * | 2005-08-25 | 2007-03-01 | Isis Innovation Limited | Detection of oxygen, carbon dioxide and anaesthetic agents |
| WO2007029245A2 (en) * | 2005-09-07 | 2007-03-15 | Medis Technologies Ltd. | Electrochemical method and system for detection of trace explosives |
| JP2007256025A (en) * | 2006-03-22 | 2007-10-04 | Kajima Corp | Method and apparatus for detecting dissolved oxygen in underground water |
| JP2008032691A (en) * | 2006-06-29 | 2008-02-14 | Fuji Electric Systems Co Ltd | Water quality monitoring system and method |
| JP2009257854A (en) * | 2008-04-15 | 2009-11-05 | Yokogawa Electric Corp | Electrochemical sensor |
| CN201637705U (en) * | 2010-04-20 | 2010-11-17 | 贵阳学通仪器仪表有限公司 | Dual-channel online dissolved oxygen meter |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107305193A (en) * | 2016-04-19 | 2017-10-31 | 季春峰 | Trace quantity dissolved oxygen instrument on-line calibration and measuring system and method |
| CN107305193B (en) * | 2016-04-19 | 2019-06-04 | 季春峰 | Trace quantity dissolved oxygen instrument on-line calibration and measuring system and method |
| CN111044589A (en) * | 2019-12-02 | 2020-04-21 | 河北冀研能源科学技术研究院有限公司 | Preparation method of zero-point correction oxygen-free water for electrodes of online dissolved oxygen meter in thermal power plant |
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Application publication date: 20120613 |