CN105242021A - Subaqueous dissolved hydrogen measuring instrument calibration device and calibration method thereof - Google Patents

Subaqueous dissolved hydrogen measuring instrument calibration device and calibration method thereof Download PDF

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CN105242021A
CN105242021A CN201510654578.3A CN201510654578A CN105242021A CN 105242021 A CN105242021 A CN 105242021A CN 201510654578 A CN201510654578 A CN 201510654578A CN 105242021 A CN105242021 A CN 105242021A
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hydrogen
water
measuring instrument
valve
dissolved hydrogen
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周海涛
马彦
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Abstract

The invention discloses a subaqueous dissolved hydrogen measuring instrument calibration device and a calibration method thereof. The device is a subaqueous dissolved hydrogen closed water circulation system controlled by a computer and includes a background hydrogen processing system, a degassing system, a flow quantity control system, a standard hydrogen generation system and a computer control system. The calibration method comprises the steps: during calibration, opening the subaqueous dissolved hydrogen measuring instrument calibration device; starting up a three-way valve, and accessing a calibrated dissolved hydrogen measuring instrument in a circulating waterway; removing gas and dissolved hydrogen in the circulating waterway; inputting parameters in the computer control system; calibrating a hydrogen sensor, and reading background hydrogen; calculating standard hydrogen by the computer control system; and calculating the subaqueous calibrated dissolved hydrogen measuring instrument. A based principle is reliable, the method is correct, and the maneuverability is high. The subaqueous dissolved hydrogen measuring instrument calculation and uncertainty evaluation in China are achieved for the first time, and a reliable technical guarantee is provided for accuracy of the subaqueous dissolved hydrogen quantity value traceability.

Description

Dissolved hydrogen measuring instrument calibrating installation and calibration steps thereof in a kind of water
Technical field
The present invention relates to measuring equipment field, specifically dissolved hydrogen measuring instrument calibrating installation and calibration steps thereof in a kind of water.
Background technology
In water, dissolved hydrogen value accurately and reliably, is the key preventing boiler, pipeline and other power-equipment burn into from monitoring corrosion activity and the leakage of genset hydrogen, has great significance to the safety and economic operation of electric boiler, nuclear power generating sets.At present, in domestic and international water, the measuring method of dissolved hydrogen all adopts dissolved hydrogen measuring instrument determination method.Although in water, dissolved hydrogen measuring instrument is simple to operate, resolution is high, reproducible, and can be arranged on pipeline dissolved hydrogen in water is carried out on-line measurement, monitored in real time, signal that is rapid, that continue is provided, but, due to calibrating installation and calibration steps, in water, the important technology index such as accuracy, repeatability of dissolved hydrogen measuring instrument, does not have corresponding detection means, cannot ensure and evaluate.
Summary of the invention
The object of the present invention is to provide and a kind ofly measure dissolved hydrogen measuring instrument calibrating installation and calibration steps thereof in accurate, workable water, to solve the problem proposed in above-mentioned background technology.
For achieving the above object, the invention provides following technical scheme:
Dissolved hydrogen measuring instrument calibrating installation in a kind of water, this device is that in computer-controlled water, dissolved hydrogen closes water circulation system, includes background hydrogen disposal system, off gas system, flow control system, standard hydrogen generation systems and computer control system; Background hydrogen disposal system comprises fabric filter, active carbon filter, dehydrogenation resin; The water delivering orifice D of background hydrogen disposal system is connected to the water inlet A of off gas system; Off gas system includes a water inlet A, exhausr port and water outlet A; Water outlet A is by pipeline connection to digital servo water pump, and digital servo exit of pump is connected to spinner-type flowmeter, and exhausr port is connected to the entrance A of multilevel water seal by pipeline, and the outlet A of multilevel water seal leads to air;
Standard hydrogen generation systems comprises Stainless Steel Shell, faraday's electrode and constant current source; The outlet of spinner-type flowmeter is connected to the water inlet D of Stainless Steel Shell by pipeline, faraday's electrode is installed on the bottom of Stainless Steel Shell; Faraday's electrode is connected with constant current source; Stainless Steel Shell upper end water delivering orifice C is connected to the water inlet B of flow cell, is provided with hydrogen sensor in flow cell, and the water outlet B of flow cell is connected a water inlet C of the first T-valve by pipeline; One end outlet B of the first T-valve is connected to by school dissolved hydrogen measuring instrument by pipeline; The other end outlet C of the first T-valve is connected with the entrance B of the second T-valve by pipeline, and one end outlet D of the second T-valve is connected with by school dissolved hydrogen measuring instrument by pipeline, and the other end outlet E of the second T-valve is connected with ebullator by pipeline; Ebullator is connected to an end entrance F of the 3rd T-valve; 3rd T-valve other end outlet G is connected to the water inlet E of background hydrogen disposal system; One end entrance H of the 3rd T-valve connects small pump, and small pump also connects pure water tank by pipeline; The gas circuit entrance of background hydrogen disposal system connects hydrogen generator by gas piping B, stop valve, gas piping A successively;
This computer control system is a microprocessor, and connects off gas system, video location monitoring system, ebullator, digital servo water pump, constant current source, small pump, the 3rd T-valve, the second T-valve, the first T-valve, hydrogen sensor successively respectively.
As the further scheme of the present invention: described fabric filter, active carbon filter, dehydrogenation resin connect successively.
The calibration steps of dissolved hydrogen measuring instrument calibrating installation in described water, comprises the following steps:
1) dissolved hydrogen measuring instrument calibrating installation in open water;
2) start T-valve accesses by school dissolved hydrogen measuring instrument in circulation waterway;
3) gas and dissolved hydrogen in circulation waterway is removed;
4) input parameter in computer control system;
5) calibrate hydrogen sensor, read background hydrogen;
6) standard hydrogen that calculates of computer control system;
7) calibrate in water by school dissolved hydrogen measuring instrument.
As the further scheme of the present invention: the parameter of input comprises flow, Faradaic current, electrolytic efficiency, faraday's electrode number.
Compared with prior art, the invention has the beneficial effects as follows:
1, the principle of foundation of the present invention is reliable, and method is correct, workable.Solve the determination of background hydrogen in calibrating installation, the determination of supporting electrolyte, the making of faraday's electrode, the control of discharge, multiple key problem in technology such as the development of background hydrogen disposal system and electronics circuit design, software programming.
2, the range ability of calibrating installation of the present invention is (0 ~ 10n) μ g/L (n >=1), the each performance parameters of device: background hydrogen is lower than 0.1 μ g/L, flow uncertainty is less than 2.9ml/min, background hydrogen uncertainty is less than 0.17 μ g/L, constant current source power supply uncertainty is less than 0.01mA, brine electrolysis efficiency is better than 98%, and uncertainty of measurement is less than 0.86%.
3, the present invention achieves calibration and the uncertainty evaluation of dissolved hydrogen measuring instrument in China's water first, range ability (0 ~ 10n) μ g/L (n >=1), uncertainty is better than 0.5 μ g/L (k=2), repeatability is less than 0.1 μ g/L, accurately provides reliable technical guarantee for dissolved hydrogen magnitude tracing in water.
Accompanying drawing explanation
Fig. 1 is structure diagram of the present invention.
Fig. 2 is each parts connection layout of the present invention.
In figure: 1-background hydrogen disposal system, 2-off gas system, 3-multilevel water seal, 4-flow control system, 6-standard hydrogen generation systems, 9-flow cell, 10-hydrogen sensor, 11-first T-valve, 12-is by school dissolved hydrogen measuring instrument, 13-second T-valve, 14-ebullator, 15-small pump, 16-stop valve, 17-hydrogen generator, 18-pure water tank, 19-the 3rd T-valve, 21-water inlet A, 22-exhausr port, 23-water outlet A, 24-fabric filter, 25-dehydrogenation resin, 26-active carbon filter, 29-computer control system, 31-entrance A, 32-exports A, 40-gas piping A, 41-digital servo water pump, 42-spinner-type flowmeter, 43-video location monitoring system, 44-gas piping B, 50-data signal line A, 51-data signal line B, 52-data signal line C, 53-data signal line D, 54-data signal line E, 55-data signal line F, 56-data signal line G, 57-data signal line H, 58-data signal line I, 59-data signal line J, 61-Stainless Steel Shell, 62-faraday electrode A, 63-faraday electrode B, 64-faraday electrode C, 65-constant current source, 91-water inlet B, 92-water outlet B, 111-water inlet C, 112-exports B, 113-exports C, 131-entrance B, 132-exports D, 133-exports E, 191-entrance F, 192-entrance H, 193-exports G, 241-water inlet E, 242-gas circuit entrance, 611-water inlet D, 612-water delivering orifice C, 2501-water delivering orifice D.
Embodiment
Below in conjunction with the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, as shown in Figure 1-2, be the connection sketch of circulation waterway of the present invention and computer system control schematic diagram and critical piece.Dissolved hydrogen measuring instrument calibrating installation in a kind of water, in computer-controlled water, dissolved hydrogen closes water circulation system, includes background hydrogen disposal system 1, off gas system 2, flow control system 4, standard hydrogen generation systems 6 and computer control system 29.
This background hydrogen disposal system 1 comprises fabric filter 24, active carbon filter 26, dehydrogenation resin 25.Fabric filter 24, active carbon filter 26, dehydrogenation resin 25 connect successively, and the water delivering orifice D2501 of dehydrogenation resin 25 is connected to the water inlet A 21 of off gas system 2.
This off gas system 2 includes a water inlet A 21, exhausr port 22 and water outlet A 23.The water inlet A 21 of off gas system 2 is connected by the water delivering orifice D2501 of pipeline with background hydrogen disposal system 1, water outlet A 23 by pipeline connection to digital servo water pump 41, digital servo water pump 41 outlet is connected to spinner-type flowmeter 42, spinner-type flowmeter 42 also connects video location monitoring system 43, and video location monitoring system 43 monitors the rotor of spinner-type flowmeter 42; Exhausr port 22 is connected to the entrance A31 of multilevel water seal 3 by pipeline, and the outlet A32 of multilevel water seal 3 leads to air.
Standard hydrogen generation systems 6 comprises Stainless Steel Shell 61, faraday's electrode A62, faraday's electrode B63, faraday's electrode C64 and constant current source 65.The outlet of spinner-type flowmeter 42 is connected to the water inlet D611 of Stainless Steel Shell 61 by pipeline, faraday's electrode A62, faraday's electrode B63, faraday's electrode C64 are installed on the bottom of Stainless Steel Shell 61.Faraday's electrode A62, faraday's electrode B63, faraday's electrode C64 are all connected with constant current source 65.Stainless Steel Shell 61 upper end water delivering orifice C612 is connected to the water inlet B 91 of flow cell 9, is provided with hydrogen sensor 10 in flow cell 9, and the water outlet B 92 of flow cell 9 is connected to a water inlet C111 of the first T-valve 11 by pipeline.One end outlet B112 of the first T-valve 11 is connected to by school dissolved hydrogen measuring instrument 12 by pipeline; The other end outlet C113 of the first T-valve 11 is connected by the entrance B131 of pipeline with the second T-valve 13, one end outlet D132 of the second T-valve 13 is connected with by school dissolved hydrogen measuring instrument 12 by pipeline, and the other end outlet E133 of the second T-valve 13 is connected with ebullator 14 by pipeline; Ebullator 14 is connected to an end entrance F191 of the 3rd T-valve 19.3rd T-valve 19 other end outlet G193 is connected to the water inlet E241 of background hydrogen disposal system 1.
Starting or close the first T-valve 11 and the second T-valve 13 can by by school dissolved hydrogen measuring instrument 12 short circuit or be communicated in the circulation waterway of device.
One end entrance H192 of the 3rd T-valve 19 connects small pump 15, and small pump 15 connects pure water tank 18 by pipeline; Start the 3rd T-valve 19 and the pure water in pure water tank 18 can be pumped into background hydrogen disposal system 1 by small pump 15.
The gas circuit entrance 242 of background hydrogen disposal system 1 connects stop valve 16 by gas piping B44, and the other end of stop valve 16 connects hydrogen generator 17 by gas piping A40.Open stop valve 16, the hydrogen produced can be injected background hydrogen disposal system 1 in hydrogen gas generation system 17.
This computer control system 29 is a microprocessor, there is control, regulate, signals collecting and Presentation Function, by data signal line A50, data signal line B51, data signal line H57, data signal line D53, data signal line E54, data signal line G56, data signal line C52, data signal line I58, data signal line J59, data signal line F55 and software simulating are to off gas system 2, video location monitoring system 43, ebullator 14, digital servo water pump 41, constant current source 65, small pump 15, 3rd T-valve 19, second T-valve 13, the control of the first T-valve 11, and read the signal of hydrogen sensor 10.
The calibration steps of dissolved hydrogen measuring instrument calibrating installation in this water: 1) dissolved hydrogen measuring instrument calibrating installation in open water; 2) start T-valve accesses by school dissolved hydrogen measuring instrument 12 in circulation waterway; 3) gas and dissolved hydrogen in circulation waterway is removed; 4) parameter such as input flow rate, Faradaic current, electrolytic efficiency, faraday's electrode number in computer control system 29; 5) calibrate hydrogen sensor 10, read background hydrogen; 6) standard hydrogen that calculates of computer control system 29; 7) calibrate in water by school dissolved hydrogen measuring instrument 12.Each performance parameters: range ability is (0 ~ 10n) μ g/L (n >=1).Each performance parameters: background hydrogen is lower than 0.1 μ g/L; Hydrogen sensor 10 aftercurrent is less than 0.1 μ g/L; Flow uncertainty is less than 2.9ml/min; Background hydrogen uncertainty is less than 0.17 μ g/L; Constant current source 65 power supply uncertainty is less than 0.01mA; Brine electrolysis efficiency is better than 98%, and uncertainty of measurement is less than 0.86%.
Range ability (0 ~ 10n) μ g/L (n >=1) of this calibrating installation, uncertainty is better than 0.5 μ g/L (k=2), and repeatability is less than 0.1 μ g/L.
Water Plays hydrogen in water in dissolved hydrogen measuring instrument calibrating installation should be;
c s=c 0+nc p(1)
In formula: c s---water Plays dissolved hydrogen, μ g/L;
C 0---background hydrogen, μ g/L;
N---faraday's electrode number, n >=1;
C p---water Plays hydrogen increment, calculates by formula (2), μ g/L.
C p = 6 × 10 7 × η · I F · q v - - - ( 2 )
In formula, F---Faraday constant, 96485.3383 ± 0.0083C/mol;
The electrolytic efficiency of η---brine electrolysis;
I---Faradaic current, mA;
Q v---circular flow, ml/min.
The invention solves the calibration to dissolved hydrogen measuring instrument in water, have rated the value uncertainty of the calibration of dissolved hydrogen in water first, provide technical guarantee accurately and reliably for dissolved hydrogen measuring instrument measurement result in water.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this instructions is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of instructions is only for clarity sake, those skilled in the art should by instructions integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.

Claims (4)

1. dissolved hydrogen measuring instrument calibrating installation in a water, this device is that in computer-controlled water, dissolved hydrogen closes water circulation system, it is characterized in that, include background hydrogen disposal system, off gas system, flow control system, standard hydrogen generation systems and computer control system;
Background hydrogen disposal system comprises fabric filter, active carbon filter, dehydrogenation resin; The water delivering orifice D of background hydrogen disposal system is connected to the water inlet A of off gas system;
Off gas system includes a water inlet A, exhausr port and water outlet A; Water outlet A is by pipeline connection to digital servo water pump, and digital servo exit of pump is connected to spinner-type flowmeter, and exhausr port is connected to the entrance A of multilevel water seal by pipeline, and the outlet A of multilevel water seal leads to air;
Standard hydrogen generation systems comprises Stainless Steel Shell, faraday's electrode and constant current source; The outlet of spinner-type flowmeter is connected to the water inlet D of Stainless Steel Shell by pipeline, faraday's electrode is installed on the bottom of Stainless Steel Shell; Faraday's electrode is connected with constant current source; Stainless Steel Shell upper end water delivering orifice C is connected to the water inlet B of flow cell, is provided with hydrogen sensor in flow cell, and the water outlet B of flow cell is connected a water inlet C of the first T-valve by pipeline; One end outlet B of the first T-valve is connected to by school dissolved hydrogen measuring instrument by pipeline; The other end outlet C of the first T-valve is connected with the entrance B of the second T-valve by pipeline, and one end outlet D of the second T-valve is connected with by school dissolved hydrogen measuring instrument by pipeline, and the other end outlet E of the second T-valve is connected with ebullator by pipeline; Ebullator is connected to an end entrance F of the 3rd T-valve; 3rd T-valve other end outlet G is connected to the water inlet E of background hydrogen disposal system; One end entrance H of the 3rd T-valve connects small pump, and small pump also connects pure water tank by pipeline; The gas circuit entrance of background hydrogen disposal system connects hydrogen generator by gas piping B, stop valve, gas piping A successively;
This computer control system is a microprocessor, and connects off gas system, video location monitoring system, ebullator, digital servo water pump, constant current source, small pump, the 3rd T-valve, the second T-valve, the first T-valve, hydrogen sensor successively respectively.
2. dissolved hydrogen measuring instrument calibrating installation in water according to claim 1, is characterized in that, described fabric filter, active carbon filter, dehydrogenation resin connect successively.
3. the calibration steps of dissolved hydrogen measuring instrument calibrating installation in the water as described in as arbitrary in claim 1-2, is characterized in that, comprise the following steps:
1) dissolved hydrogen measuring instrument calibrating installation in open water;
2) start T-valve accesses by school dissolved hydrogen measuring instrument in circulation waterway;
3) gas and dissolved hydrogen in circulation waterway is removed;
4) input parameter in computer control system;
5) calibrate hydrogen sensor, read background hydrogen;
6) standard hydrogen that calculates of computer control system;
7) calibrate in water by school dissolved hydrogen measuring instrument.
4. the calibration steps of dissolved hydrogen measuring instrument calibrating installation in water according to claim 3, it is characterized in that, the parameter of input comprises flow, Faradaic current, electrolytic efficiency, faraday's electrode number.
CN201510654578.3A 2015-10-13 2015-10-13 Subaqueous dissolved hydrogen measuring instrument calibration device and calibration method thereof Withdrawn CN105242021A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105651953A (en) * 2015-12-28 2016-06-08 周海涛 Calibration device for gauge for dissolved hydrogen in water and calibration method thereof
CN105807000A (en) * 2016-03-17 2016-07-27 山东电力研究院 Online chemical instrument standard calibration device and method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105651953A (en) * 2015-12-28 2016-06-08 周海涛 Calibration device for gauge for dissolved hydrogen in water and calibration method thereof
CN105807000A (en) * 2016-03-17 2016-07-27 山东电力研究院 Online chemical instrument standard calibration device and method

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Application publication date: 20160113