CN205003116U - Novel gaseous karl fischer moisture appearance - Google Patents
Novel gaseous karl fischer moisture appearance Download PDFInfo
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- CN205003116U CN205003116U CN201520788109.6U CN201520788109U CN205003116U CN 205003116 U CN205003116 U CN 205003116U CN 201520788109 U CN201520788109 U CN 201520788109U CN 205003116 U CN205003116 U CN 205003116U
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Abstract
The utility model provides a pair of novel gaseous karl fischer moisture appearance, it uses the response coefficient that matches with the sample to rectify high accuracy mass flow controller, realizes accurate measurement sample size. Ensure to liquefy compressed gas with the cooler and in higher temperature gasification postcooling to room temperature, eliminate the degree of accuracy that the sample high temperature influence mass flow controller measurement, adopt quick -operation joint and carrier gas to sweep the replacement and advance kind pipeline, ensure to eliminate the interference between the sample and make the titrator obtain lower blank value, adopt the long blast pipe of taking the check valve, prevent that the air from flowing back and air moisture permeates the influence to testing. Sample waste gas is directional to be discharged, and safety ring protects, adopts multiple airtight isolation, controls the titrator effectively and not influenced by the external environment condition, improve equipment's detection limit and the repeatability of improving the analysis data.
Description
Technical field
The utility model relates to electrochemical technical field in physico-chemical analysis, is specially a kind of new gas karl Fischer Moisture Meter, and it mainly solves the technical matters of the Measurement accuracy measuring micro-moisture in liquified compressed gas or gas.
Background technology
Karl_Fischer method is proposed by karl Fischer nineteen thirty-five, is divided into volumetric method and coulometry according to its titration mode.Coulometry is more suitable for measuring low moisture sample, its principle is that the Ka Shi reagent in the electrolytic cell of instrument injects moisture sample when reaching balance, water participates in the redox reaction of iodine, sulphuric dioxide, deposit in case at pyridine and methyl alcohol, generate hydroiodic acid, pyridine and methylsulfuric acid pyridine, the iodine consumed produces at anode electrolysis, thus redox reaction is constantly carried out, till moisture all exhausts, according to Faraday's laws of electrolysis, the electricity direct proportionality consumed when electrolysis generation iodine is same electrolysis.
Existing Karl_Fischer method measures micro-moisture in easily gasify sample or gaseous sample and has the following disadvantages:
(1) conventionally, the titration cup measurement result affected by environment fluctuation of titrator is very large, and measure very low content moisture (≤10ppm) especially, measurement result repeatability is very poor.
(2) according to GB/T3727 or GB/T6023 standard, weigh with balance, determine sample introduction quality, when this is for mensuration liquified compressed gas sample (as propylene liguid, liquefied gas), gasification easily produces condensate water near steel cylinder, affects precise.
(3) existing karl Fischer Moisture Meter measures components be soluble in the sample of karl Fischer reagent, and may occur air suck-back phenomenon, this has obvious impact to determination of trace water.
(4) single hole sample feeding pipe sample introduction is not suitable for fast flow velocity sample introduction because affecting by absorption efficiency, the detection limit of have the greatest impact sample size and practical methods.
(5) with GB and Wan Tong 875, during sample introduction, sample gasification efficiency affects greatly by temperature and sample composition, and the sample gasification repeatability that boiling point is higher is poor, and result reappearance is also very poor.
For solving each above technical matters, the utility model provides a kind of new gas karl Fischer Moisture Meter, its structure is simple, easy to use, reliable, it is affected by environment and cannot Accurate Determining traces of moisture that the utility model overcomes test process, by high-temperature electric heated gas heats coil pipe, sample rapid flash is gasified, and sample entrapped moisture is imported in titration cell by gas absorption pipe.Sample introduction is even, reaction of moisture in sample is fallen up hill and dale fast.It is mainly applicable to gaseous state or can normal temperature gasification sample in determination of trace water (< 0.1%).
Summary of the invention
For above-mentioned situation, for solving the defect of prior art, the object of the utility model just there is provided a kind of new gas karl Fischer Moisture Meter, it comprises main case, titrator, sample vaporization module, carrier gas purge assembly and sample introduction module, it is characterized in that, all parts or assembly are all arranged in described main case, and wherein, described sample vaporization module comprises by sampling thief, needle valve, gasifying heater and refrigeratory; Described carrier gas purge assembly comprises carrier gas source of the gas, dry-run protection device, T-valve and rapid-acting coupling, wherein, described carrier gas source of the gas is connected with one end of described dry-run protection device, the other end of described dry-run protection device connects a valve port of described T-valve, two other valve port of described T-valve is also connected with the four-way valve of described rapid-acting coupling and sample introduction module; Described sample introduction module comprise four-way valve, displacement gas outlet, mass flow controller, insertion titrator titration cup in gas absorption pipe and gas outlet, wherein, valve port on described four-way valve is connected to the refrigeratory of displacement gas outlet, mass flow controller and described sample vaporization module, be connected with described needle valve after described refrigeratory connects described gasifying heater, mass flow controller is communicated with the gas absorption pipe in the titration cup of described titrator, and the titration cup of described titrator is also provided with gas outlet.
Further, as preferably, it also comprises temperature controller, data acquisition and control module, closed bin and drying agent, wherein, described temperature controller is connected with the gasifying heater of sample vaporization module, and for controlling the temperature of the gasifying heater of described sample vaporization module, described data acquisition and control module and described sample introduction module communicate to connect, be provided with drying agent in described closed bin, described titrator is placed in described closed bin.
Further, as preferably, the gasifying heater of described sample vaporization module comprises gas-heated coil pipe and electric heating cover, and described gas-heated coil pipe is arranged in described electric heating cover.
Further, as preferably, described refrigeratory is air-cooled cooler or water-cooling cooler.
Further, as preferably, insert in the titration cup of titrator after described gas absorption pipe employing hard tube and bubbler are closely connected.
Further, as preferably, described gas outlet is that flexible pipe is drawn, and is connected with retaining valve on the pipeline of gas outlet, channels in titration cup to prevent Air Reverse.
The beneficial effects of the utility model:
(1) response coefficient of the utility model with sample match corrects high precision mass flow controller, realizes accurate-metering sample size.
(2) the utility model refrigeratory guarantees that liquified compressed gas is cooled to room temperature after higher temperature gasification, eliminates the too high accuracy affecting mass flow controller metering of sample temperature.
(3) the utility model adopts the switching mode of minimal dead volumes, realizes carrier gas and replaces pipeline quickly and efficiently.
(4) the utility model adopts rapid-acting coupling and carrier gas purge displacement sample introduction pipeline, guarantees that sample introduction pipeline has lower blank value.
(5) the utility model adopts micro pores attract technology, improves efficiency and sample introduction efficiency that karl Fischer absorbs moisture in gas.
(6) the utility model adopts the long gas outlet of band retaining valve, prevents air return and air moisture infiltration on the impact of test.The discharge of sample waste gas orientation, safety and environmental protection.
(7) the utility model adopts multiple airtight isolation, effectively controls titrator not by external environment influence, improves the detection limit of equipment and improves the repeatability analyzing data.
Accompanying drawing explanation
The structural representation of a kind of new gas karl Fischer Moisture Meter that Fig. 1 provides for the utility model.
Wherein, in figure, 1-carrier gas source of the gas 2-dry-run protection device 3-T-valve 4-rapid-acting coupling 5-needle valve 6-gasifying heater 7-refrigeratory 8-four-way valve 9-mass flow controller 10-titrator 11-gas absorption pipe 12-gas outlet 13-replaces gas outlet 14-temperature controller 15-main case 16-data acquisition and control module 17-closed bin 18-drying agent.
Embodiment
Below in conjunction with accompanying drawing, the utility model is described further.
As shown in Figure 1, the utility model provides a kind of new gas karl Fischer Moisture Meter, it comprises main case 15, sample vaporization module, carrier gas purge assembly and sample introduction module, described sample vaporization module, carrier gas purge assembly and sample introduction module are all arranged in described main case 15, wherein, described sample vaporization module comprises by sampling thief, needle valve 5, gasifying heater 6 and refrigeratory 7; Described carrier gas purge assembly comprises carrier gas source of the gas 1, dry-run protection device 2, T-valve 3 and rapid-acting coupling 4, wherein, described carrier gas source of the gas 1 is connected with one end of described dry-run protection device 2, the other end of described dry-run protection device 2 connects a valve port of described T-valve 3, two other valve port of described T-valve 3 is also connected with the four-way valve 8 of described rapid-acting coupling 4 and sample introduction module; Described sample introduction module comprise four-way valve 8, displacement gas outlet 13, mass flow controller 9, insert titrator titration cup in gas absorption pipe 11 and gas outlet 12, wherein, valve port on described four-way valve 8 is connected to the refrigeratory 7 of displacement gas outlet 13, mass flow controller 9 and described sample vaporization module, described refrigeratory 7 is connected with described gasifying heater 6 after connecting described needle valve 5, mass flow controller 9 is communicated with the gas absorption pipe 11 in the titration cup of described titrator 10, and the titration cup of described titrator 10 is also provided with gas outlet 12.
In the present embodiment, the utility model also comprises temperature controller 14, data acquisition and control module 16, closed bin 17 and drying agent 18, wherein, described temperature controller 14 is connected with the gasifying heater of sample vaporization module, for controlling the temperature of the gasifying heater of described sample vaporization module, described data acquisition and control module 16 communicates to connect with described sample introduction module, and be provided with drying agent 18 in described closed bin 17, described titrator 10 is placed in described closed bin 18.
In addition, the gasifying heater of described sample vaporization module comprises gas-heated coil pipe and electric heating cover, and described gas-heated coil pipe is arranged in described electric heating cover.Refrigeratory is air-cooled cooler or water-cooling cooler.Gas absorption pipe inserts in the titration cup of titrator after adopting hard tube and bubbler to be closely connected.Gas outlet is that flexible pipe is drawn, and is connected with retaining valve on the pipeline of gas outlet, channels in titration cup to prevent Air Reverse.
The utility model in use, first carrier gas purge:
The carrier gas that carrier gas source of the gas 1 flows out carries out further depth drying by pipeline to dry-run protection device 2; guarantee that its moisture is enough spent (lower than 1ug/L); through T-valve 3; a direction connects four-way valve 8; another direction connects self-sealing fast joint 4; when carrier gas is communicated with four-way valve 8, the abundant dry sample introduction module of carrier gas and titration assembly or fully dry displacement gas outlet 13.When carrier gas is communicated with rapid-acting coupling 4, carrier gas can abundant drying, gasifying assembly.Fully dry through two, guarantee that the blank moisture of system is negligible for sample.
Sample displacement:
The sampling thief that sample is housed is connected with vaporization module by pipeline, sample regulates suitable flow through needle valve 5, guarantee that the sample flowing through needle valve 5 can change into gaseous state by quick air in gasifying heater 6, through subcooler 7, gas temperature is cooled to room temperature (less than 50 degree), then is connected with four-way valve 8.Discharged by the displacement gas outlet 13 of four-way valve 8 after sample gasification.
Sample feeding:
After sample is fully replaced, switch four-way valve 8 to sample introduction state, sample flows through mass flow controller 9 through four-way valve 8, with constant flow rate uniformly across gas absorption pipe 11, in sample, moisture karl Fischer reagent that is abundant and titrator 10 reacts, and unreacted gas is discharged by gas outlet 12.The gross mass of sample water is calculated by electricity.The quality of the water after deduction blank and sample quality (sampling volume according to mass flow controller calculates) ratio are exactly the moisture of sample.
The response coefficient of the utility model with sample match corrects high precision mass flow controller, realizes accurate-metering sample size.Guarantee that liquified compressed gas is cooled to room temperature after higher temperature gasification with refrigeratory, eliminate the too high accuracy affecting mass flow controller metering of sample temperature.Adopt the switching mode of minimal dead volumes, realize carrier gas and replace pipeline quickly and efficiently.Adopt rapid-acting coupling and carrier gas purge displacement sample introduction pipeline, guarantee that sample introduction pipeline has lower blank value.Adopt micro pores attract technology, improve efficiency and sample introduction efficiency that karl Fischer absorbs moisture in gas.Adopt the long gas outlet of band retaining valve, prevent air return and air moisture infiltration on the impact of test.The discharge of sample waste gas orientation, safety and environmental protection.Adopt multiple airtight isolation, effectively control titrator not by external environment influence, improve the detection limit of equipment and improve the repeatability analyzing data.
Claims (6)
1. a new gas karl Fischer Moisture Meter, it comprises main case, sample vaporization module, carrier gas purge assembly, sample introduction module and titrator, it is characterized in that, described sample vaporization module, carrier gas purge assembly and sample introduction module are all arranged in described main case, wherein, described sample vaporization module comprises by sampling thief, needle valve, gasifying heater and refrigeratory; Described carrier gas purge assembly comprises carrier gas source of the gas, dry-run protection device, T-valve and rapid-acting coupling, wherein, described carrier gas source of the gas is connected with one end of described dry-run protection device, the other end of described dry-run protection device connects a valve port of described T-valve, two other valve port of described T-valve is also connected with the four-way valve of described rapid-acting coupling and sample introduction module; Described sample introduction module comprise four-way valve, displacement gas outlet, mass flow controller, insertion titrator titration cup in gas absorption pipe and gas outlet, wherein, valve port on described four-way valve is connected to the refrigeratory of displacement gas outlet, mass flow controller and described sample vaporization module, be connected with described needle valve after described refrigeratory connects described gasifying heater, mass flow controller is communicated with the gas absorption pipe in the titration cup of described titrator, and the titration cup of described titrator is also provided with gas outlet.
2. a kind of new gas karl Fischer Moisture Meter according to claim 1, it is characterized in that, it also comprises temperature controller, data acquisition and control module, closed bin and drying agent, wherein, described temperature controller is connected with the gasifying heater of sample vaporization module, for controlling the temperature of the gasifying heater of described sample vaporization module, described data acquisition and control module and described sample vaporization module, described sample introduction module communicates to connect, Automated condtrol is realized by software programming, drying agent is provided with in described closed bin, described titrator is placed in described closed bin.
3. a kind of new gas karl Fischer Moisture Meter according to claim 2, it is characterized in that, the gasifying heater of described sample vaporization module comprises gas-heated coil pipe and electric heating cover, and described gas-heated coil pipe is arranged in described electric heating cover.
4. a kind of new gas karl Fischer Moisture Meter according to claim 1, it is characterized in that, described refrigeratory is air-cooled cooler or water-cooling cooler.
5. a kind of new gas karl Fischer Moisture Meter according to claim 1, is characterized in that, described gas absorption pipe inserts in the titration cup of titrator after adopting hard tube and bubbler to be closely connected.
6. a kind of new gas karl Fischer Moisture Meter according to claim 1, is characterized in that, described gas outlet is that flexible pipe is drawn, and is connected with retaining valve on the pipeline of gas outlet, channels in titration cup to prevent Air Reverse.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201520788109.6U CN205003116U (en) | 2015-10-12 | 2015-10-12 | Novel gaseous karl fischer moisture appearance |
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| CN201520788109.6U CN205003116U (en) | 2015-10-12 | 2015-10-12 | Novel gaseous karl fischer moisture appearance |
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| CN205003116U true CN205003116U (en) | 2016-01-27 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109682986A (en) * | 2019-02-18 | 2019-04-26 | 哈尔滨天龙仪器制造有限公司 | A kind of device for sampling quantitative gas capable of washing |
| CN110146607A (en) * | 2019-05-06 | 2019-08-20 | 北京水木滨华科技有限公司 | The quantitative detecting method of micro-moisture in a kind of organic system |
| 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 |
| CN112505242A (en) * | 2020-12-24 | 2021-03-16 | 红宝丽集团泰兴化学有限公司 | Method for measuring moisture in oxide |
| CN114894960A (en) * | 2022-05-25 | 2022-08-12 | 重庆康普化学工业股份有限公司 | Method for detecting KOH moisture content |
-
2015
- 2015-10-12 CN CN201520788109.6U patent/CN205003116U/en not_active Expired - Fee Related
Cited By (7)
| 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 |
| CN110850024B (en) * | 2018-08-21 | 2021-11-09 | 中国计量科学研究院 | Water detection calibration system, detection model establishing method and water detection method |
| CN109682986A (en) * | 2019-02-18 | 2019-04-26 | 哈尔滨天龙仪器制造有限公司 | A kind of device for sampling quantitative gas capable of washing |
| CN110146607A (en) * | 2019-05-06 | 2019-08-20 | 北京水木滨华科技有限公司 | The quantitative detecting method of micro-moisture in a kind of organic system |
| CN110146607B (en) * | 2019-05-06 | 2020-05-15 | 北京水木滨华科技有限公司 | Quantitative detection method for trace moisture in organic system |
| CN112505242A (en) * | 2020-12-24 | 2021-03-16 | 红宝丽集团泰兴化学有限公司 | Method for measuring moisture in oxide |
| CN114894960A (en) * | 2022-05-25 | 2022-08-12 | 重庆康普化学工业股份有限公司 | Method for detecting KOH moisture content |
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| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| DD01 | Delivery of document by public notice | ||
| DD01 | Delivery of document by public notice |
Addressee: Wang Zhigang Document name: Notification of Termination of Patent Right |
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| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160127 Termination date: 20211012 |