CN105223256A - A kind of Karl Fischer coulometric determination crude oil, tar water-containing measuring instrument - Google Patents
A kind of Karl Fischer coulometric determination crude oil, tar water-containing measuring instrument Download PDFInfo
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- CN105223256A CN105223256A CN201510714860.6A CN201510714860A CN105223256A CN 105223256 A CN105223256 A CN 105223256A CN 201510714860 A CN201510714860 A CN 201510714860A CN 105223256 A CN105223256 A CN 105223256A
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Abstract
A kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument relate to electron chemistry analytical instrument, be made up of nitrogen storage tank, stepper motor, needle-valve, mass flowmeter, solenoid valve, metal bath gasification unit, cassette coulometry electrolytic cell and control module, the valve rod of needle-valve is connected with the pto of stepper motor, and nitrogen storage tank, needle-valve, mass flowmeter, solenoid valve, metal bath gasification unit and cassette coulometry electrolytic cell successively pipeline connect; Control module connects with stepper motor, mass flowmeter, solenoid valve, metal bath gasification unit and cassette coulometry electrolytic cell circuit respectively.The method that the present invention adopts is not directly inject in electrolytic cell by sample, but adopt metal bath gasification unit to be heated by sample, with high pure nitrogen, the moisture content in sample is blown in electrolytic cell, the impurity avoided in crude oil or tar forms oil film parcel to electrolysis electrode and potential electrode, make the shortcoming that reagent lost efficacy, improve the utilization factor of reagent.
Description
Technical field
The present invention relates to electron chemistry analytical instrument, refer more particularly to and be applicable to crude oil, a kind of Karl Fischer coulometric determination crude oil of Tar use, tar water-containing measuring instrument.
Background technology
What traditional crude-oil water-content determiner adopted is the way of distillation, needs to distill a lot of samples, condensation, recovery collect moisture content, measure the moisture content in crude oil or tar.Process of the test is more loaded down with trivial details, and the result of metering, because be the graduated cylinder metering with 5 milliliters, so result is rough calculation, is not very accurate.Since Karl Fischer coulometric determination trace water analyzer occurs, people carry out determination of moisture according to GB/T11146 and crude oil moisture determination method Karl_Fischer method standard again, directly crude oil or tar are injected in electrolytic cell bottle in this standard, electrolytic solution and sample is made to participate in reacting, thus calculating water-retention value, but due to crude oil or tarry impurities many, oil film parcel is formed to electrolysis electrode and potential electrode, reagent was easily lost efficacy.
Summary of the invention
The present invention is exactly to overcome the problems referred to above, provides a kind of Karl Fischer coulometric determination crude oil, tar water-containing measuring instrument.
A kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument, be made up of nitrogen storage tank, stepper motor, needle-valve, mass flowmeter, solenoid valve, metal bath gasification unit, cassette coulometry electrolytic cell and control module, the valve rod of needle-valve is connected with the pto of stepper motor, and nitrogen storage tank, needle-valve, mass flowmeter, solenoid valve, metal bath gasification unit and cassette coulometry electrolytic cell successively pipeline connect; Control module connects with stepper motor, mass flowmeter, solenoid valve, metal bath gasification unit and cassette coulometry electrolytic cell circuit respectively.
As a further improvement on the present invention, the top of metal bath gasification unit is provided with sample injection port, bottom is provided with nitrogen inlet, inside is provided with metal bath heating module; Nitrogen inlet connects with electromagnetic valve pipeline, and metal bath heating module connects with control module circuit.
As a further improvement on the present invention, cassette coulometry electrolytic cell comprises electrolytic cell bottle, electrolysis electrode and potential electrode, electrolysis electrode and potential electrode are all fixed in electrolytic cell bottle, Liquid sample introduction mouth, gas access and gas vent is provided with above this electrolytic cell bottle, gas access connects with metal bath gasification unit pipeline, and electrolysis electrode, potential electrode all connect with control module circuit.
As a further improvement on the present invention, gas vent is connected with drying tube.
As a further improvement on the present invention, nitrogen storage tank, stepper motor, needle-valve, mass flowmeter, solenoid valve, metal bath gasification unit and control module are all located in a casing, and this casing is provided with display, and this display connects with control module circuit.
A kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument, the method adopted is not directly inject in electrolytic cell by sample, but adopt metal bath gasification unit to be heated by sample, with high pure nitrogen, the moisture content in sample is blown in electrolytic cell, the impurity avoided in crude oil or tar forms oil film parcel to electrolysis electrode and potential electrode, make the shortcoming that reagent lost efficacy, and improve the utilization factor of reagent.
Accompanying drawing explanation
Accompanying drawing 1 ~ accompanying drawing 2 is the structural drawing of a kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument;
Accompanying drawing 3 is the structural drawing of metal bath gasification unit of a kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument;
Accompanying drawing 4 is the structural drawing of casing of a kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument;
Accompanying drawing 5 is the module map of a kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument.
Embodiment
Below in conjunction with accompanying drawing to a kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument, be described further:
A kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument are made up of nitrogen storage tank 1, stepper motor 2, needle-valve 3, mass flowmeter 4, solenoid valve 5, metal bath gasification unit 6, cassette coulometry electrolytic cell 7 and control module 8.
Wherein, the valve rod of needle-valve 3 is connected with the pto of stepper motor 2, and control module 8 controls the gas flow of needle-valve 3 by control step motor 2.
In this device, nitrogen storage tank 1, needle-valve 3, mass flowmeter 4, solenoid valve 5, metal bath gasification unit 6 and cassette coulometry electrolytic cell 7 successively pipeline connect, circuit ingredient is connected with stepper motor 2, mass flowmeter 4, solenoid valve 5, metal bath gasification unit 6 and cassette coulometry electrolytic cell 7 circuit respectively by control module 8 to form, metal bath gasification unit 6, the top of metal bath gasification unit 6 is provided with sample injection port 9, bottom is provided with nitrogen inlet 10, inside is provided with metal bath heating module; Nitrogen inlet 10 connects with solenoid valve 5 pipeline, and metal bath heating module connects with control module 8 circuit.
Namely cassette coulometry electrolytic cell 7 is converted by ready-made karl Fischer micro-water analyzer, such as use the WA-1C type micro-water analyzer of acrylonitrile by Coulometry moisture, it mainly comprises electrolytic cell bottle 12, electrolysis electrode 13 and potential electrode 14, electrolysis electrode 13 and potential electrode 14 are all fixed in electrolytic cell bottle 12, Liquid sample introduction mouth 15 is provided with above this electrolytic cell bottle 12, gas access 16 and gas vent 18, gas access 16 connects with metal bath gasification unit 6 pipeline, for passing into the mixed gas of nitrogen and steam, gas vent 18 is connected with drying tube 19, air for unnecessary nitrogen and former electrolytic cell bottle 12 inside is discharged, electrolysis electrode 13, potential electrode 14 all connects with control module 8 circuit.
This device outside is provided with casing 11, casing 11 is installed display 17, and is provided with external keyboard, and keyboard and display 17 connect with control module 8 circuit respectively.
A kind of Karl Fischer coulometric determination crude oil of the present invention, tar water-containing measuring instrument, its concrete using method is as follows:
Nitrogen storage tank 1 is for storing and discharging the nitrogen dewatered, nitrogen is successively by needle-valve 3 and mass flowmeter 4, control module 8 is adjusted by the Real-Time Monitoring feedback of mass flowmeter 4 pairs of flows and then the flow of opening and closing degree to nitrogen of control needle-valve 3, nitrogen enters solenoid valve 5 after mass flowmeter 4, this solenoid valve 5 is T-valve, two outlet one is communicated with the nitrogen inlet 10 below metal bath gasification unit 6, another is provided with drain, when detection does not prepare completely or after completing, drain side opened by solenoid valve 5, nitrogen is discharged by drain.
Before carrying out determination of moisture work, in cassette coulometry electrolytic cell 7 and electrolysis electrode 13, inject the reagent mixed with the pyridine, methyl alcohol etc. that are filled with sulphuric dioxide by dominant iodine, then carry out self-inspection and demarcation.
Start instrument and wait for that in electrolytic cell 7, state reaches equilibrium state, makes metal bath gasification unit 6 reach preset temperature, after passing into nitrogen, controls needle-valve 3 make nitrogen flow rate reach setting value with stepper motor 2, take a certain amount of testing sample (crude oil or tar etc., 2g ~ 3g), inject metal bath gasification unit 6, in metal bath gasification unit 6 testing sample, moisture flashes off, keypad starts to analyze, switching solenoid valve 5 makes nitrogen be blown into metal bath gasification unit 6, drive aqueous vapor is blown into cassette coulometry electrolytic cell 7 li, until the measuring state limit-up of cassette coulometry electrolytic cell 7, switching solenoid valve 4 is to drain, guide unnecessary nitrogen to discharge and terminate to purge, electrolysis electrode 13 starts electrolysis, last control module 8 calculates water-retention value according to consumed electricity and is presented on display 17.
Claims (5)
1. a Karl Fischer coulometric determination crude oil, tar water-containing measuring instrument, by nitrogen storage tank (1), stepper motor (2), needle-valve (3), mass flowmeter (4), solenoid valve (5), metal bath gasification unit (6), cassette coulometry electrolytic cell (7) and control module (8) are formed, it is characterized in that the valve rod of needle-valve (3) is connected with the pto of stepper motor (2), nitrogen storage tank (1), needle-valve (3), mass flowmeter (4), solenoid valve (5), metal bath gasification unit (6) and cassette coulometry electrolytic cell (7) successively pipeline connect, control module (8) connects with stepper motor (2), mass flowmeter (4), solenoid valve (5), metal bath gasification unit (6) and cassette coulometry electrolytic cell (7) circuit respectively.
2. a kind of Karl Fischer coulometric determination crude oil according to claim 1, tar water-containing measuring instrument, is characterized in that the top of metal bath gasification unit (6) is provided with sample injection port (9), bottom is provided with nitrogen inlet (10), inside is provided with metal bath heating module; Nitrogen inlet (10) connects with solenoid valve (5) pipeline, and metal bath heating module connects with control module (8) circuit.
3. a kind of Karl Fischer coulometric determination crude oil according to claim 1, tar water-containing measuring instrument, it is characterized in that cassette coulometry electrolytic cell (7) comprises electrolytic cell bottle (12), electrolysis electrode (13) and potential electrode (14), electrolysis electrode (13) and potential electrode (14) are all fixed in electrolytic cell bottle (12), this electrolytic cell bottle (12) top is provided with Liquid sample introduction mouth (15), gas access (16) and gas vent (18), gas access (16) connects with metal bath gasification unit (6) pipeline, electrolysis electrode (13), potential electrode (14) all connects with control module (8) circuit.
4. a kind of Karl Fischer coulometric determination crude oil according to claim 3, tar water-containing measuring instrument, is characterized in that gas vent (18) is connected with drying tube (19).
5. a kind of Karl Fischer coulometric determination crude oil according to claim 1, tar water-containing measuring instrument, it is characterized in that nitrogen storage tank (1), stepper motor (2), needle-valve (3), mass flowmeter (4), solenoid valve (5), metal bath gasification unit (6) and control module (8) are all located in a casing (11), this casing (11) is provided with display (17), this display (17) connects with control module (8) circuit.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201510714860.6A CN105223256A (en) | 2015-10-29 | 2015-10-29 | A kind of Karl Fischer coulometric determination crude oil, tar water-containing measuring instrument |
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| CN201510714860.6A CN105223256A (en) | 2015-10-29 | 2015-10-29 | A kind of Karl Fischer coulometric determination crude oil, tar water-containing measuring instrument |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110596354A (en) * | 2019-11-04 | 2019-12-20 | 云南电网有限责任公司电力科学研究院 | Device and method for detecting moisture content in hydrogen oil |
| CN110850024A (en) * | 2018-08-21 | 2020-02-28 | 中国计量科学研究院 | Water detection calibration system, detection model establishing method and water detection method |
| CN114166686A (en) * | 2021-12-02 | 2022-03-11 | 襄阳九鼎昊天环保设备有限公司 | Detection system and detection method for tar content in coke oven gas |
Citations (5)
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| CN1680810A (en) * | 2004-04-07 | 2005-10-12 | 董慧茹 | Method and device for improving Karl Fischer water content determination |
| CN102937618A (en) * | 2012-10-26 | 2013-02-20 | 河北省电力公司电力科学研究院 | Post-desulphurization flue gas moisture content determination method and apparatus |
| CN103380370A (en) * | 2011-02-18 | 2013-10-30 | 京都电子工业株式会社 | Karl fischer titrator and karl fischer titration method |
| CN104569113A (en) * | 2015-01-27 | 2015-04-29 | 上海化工研究院 | Hot gas flow dissociation dewatering indirect Karl-Fischer-process analysis device |
| CN205049514U (en) * | 2015-10-29 | 2016-02-24 | 大庆市日上仪器制造有限公司 | Ka erfeixiu coulometry crude oil, moisture measuring device of tar |
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2015
- 2015-10-29 CN CN201510714860.6A patent/CN105223256A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN1680810A (en) * | 2004-04-07 | 2005-10-12 | 董慧茹 | Method and device for improving Karl Fischer water content determination |
| CN103380370A (en) * | 2011-02-18 | 2013-10-30 | 京都电子工业株式会社 | Karl fischer titrator and karl fischer titration method |
| CN102937618A (en) * | 2012-10-26 | 2013-02-20 | 河北省电力公司电力科学研究院 | Post-desulphurization flue gas moisture content determination method and apparatus |
| CN104569113A (en) * | 2015-01-27 | 2015-04-29 | 上海化工研究院 | Hot gas flow dissociation dewatering indirect Karl-Fischer-process analysis device |
| CN205049514U (en) * | 2015-10-29 | 2016-02-24 | 大庆市日上仪器制造有限公司 | Ka erfeixiu coulometry crude oil, moisture measuring device of tar |
Non-Patent Citations (1)
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| 贾桂敏: "液态烃微量水份测定中进样方式的研究", 《现代科学仪器》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110850024A (en) * | 2018-08-21 | 2020-02-28 | 中国计量科学研究院 | Water detection calibration system, detection model establishing method and water detection method |
| CN110596354A (en) * | 2019-11-04 | 2019-12-20 | 云南电网有限责任公司电力科学研究院 | Device and method for detecting moisture content in hydrogen oil |
| CN114166686A (en) * | 2021-12-02 | 2022-03-11 | 襄阳九鼎昊天环保设备有限公司 | Detection system and detection method for tar content in coke oven gas |
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Application publication date: 20160106 |