CN102928365A - Dynamic calibrating device and method in process of measuring micro-moisture in gas by using optical method - Google Patents
Dynamic calibrating device and method in process of measuring micro-moisture in gas by using optical method Download PDFInfo
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- CN102928365A CN102928365A CN2012104184147A CN201210418414A CN102928365A CN 102928365 A CN102928365 A CN 102928365A CN 2012104184147 A CN2012104184147 A CN 2012104184147A CN 201210418414 A CN201210418414 A CN 201210418414A CN 102928365 A CN102928365 A CN 102928365A
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Abstract
The invention relates to a dynamic calibrating device and a dynamic calibrating method in a process of measuring micro-moisture in gas by using an optical method. The dynamic calibrating device comprises a gas steel bottle, an adjusting valve, a main flow meter, a low-temperature water washing pipe, a sample switching valve, an optical moisture measuring meter, a reversing valve and a low-temperature gas moisture absorption pipe-Kari Fischer titration cell, and further comprises a bypass adjusting valve and a bypass flow meter; the bypass adjusting valve and the bypass flow meter are connected in series, and are connected in parallel at the both ends of the low-temperature water washing pipe. The dynamic calibrating method comprises the following steps of: sequentially introducing gas into a photo-acoustic spectrometry moisture meter and the gas moisture absorption pipe-Kari Fischer titration cell which are connected in series; and measuring the water containing amount in the gas through the gas moisture absorption pipe-Kari Fischer titration cell, so as to calibrate the photo-acoustic spectrometry moisture meter. Compared with the prior art, the dynamic calibrating device and method provided by the invention can use the photo-acoustic spectrometry moisture meter and the gas moisture absorption pipe-Kari Fischer titration cell in series, and can be used for calibrating while testing; and the dynamic calibrating device and the dynamic calibrating method can be used for adjusting the micro-moisture content in the gas and has the advantages of good operability and the like.
Description
Technical field
The present invention relates to a kind of mensuration of minor amount of water, especially relate to the dynamic calibrating method in the micro-moisture process in a kind of optical method mensurated gas composition.
Background technology
Infra-red sepectrometry detects the gas ultimate principle: utilize material that the selectivity of the electromagnetic radiation in infrared light district is absorbed to carry out structure analysis and to a method of the qualitative and quantitative analysis of the compound of various absorption infrared lights.The molecule of tested gaseous matter only absorbs the infrared spectrum consistent with its molecular vibration, rotational frequency under infrared radiation.Infrared spectrum is analyzed, can be carried out qualitative analysis to gaseous matter.Exist many atomic groups in the compound molecule, after each atomic group is excited, all can produce eigen vibration, its vibration frequency also must be reflected on the infrared absorption spectrum.But various atomic groups in the authenticating compound also can carry out quantitative test accordingly.
Photocaustic spectroscopy detects the gas ultimate principle: the monochromatic light with the adjustable system of a beam intensity shines on the sample that is sealed in the photoacoustic cell, absorption of sample luminous energy, and to discharge the mode de excitation of heat energy, the heat energy that discharges makes sample and surrounding medium periodically heat by the modulating frequency generation of light, thereby cause medium to produce the periodic pressure fluctuation, this pressure surge can detect with sensitive microphone or piezoelectric ceramic microphone, and obtains photoacoustic signal, optoacoustic effect that Here it is by amplification.If the incident monochromatic wavelength is variable, then can measure the photoacoustic signal collection of illustrative plates that becomes with wavelength, Here it is optoacoustic spectroscopy.If incident light is to focus on the pencil light form and move by the x-y axle scan mode of sample, then can be recorded to photoacoustic signal with the variation of sample position, Here it is photoacoustic imaging technology.
This photocaustic spectroscopy can be used for measuring the strong or opaque sample of light scattering that traditional spectroscopic methodology is difficult to measure, such as gel, and colloidal sol, powder, Biosamples etc. are applied to physics at present, chemistry, the fields such as biomedicine and environmental protection.Also can be used for detecting micro-moisture content in the gas.For further promoting the application in the micro-moisture assay field in gas of this detection method, these two kinds of methods all need the gas of known moisture levels to demarcate, and are to select preferably and utilize classical karl Fischer method to the definite value of moisture in the gas.
The karl Fischer method is called for short Fei Xiufa, is the capacity analysis method of the mensuration moisture of nineteen thirty-five karl Fischer (Karl Fischer) proposition.Fei Xiufa measures in all kinds of chemical methodes of substance moisture content,, the most accurately method the most single-minded to water.Though belong to classical way but through in recent years improving, improved accuracy, enlarged measurement range, be listed in the standard method of determination of moisture in many materials.
Divide titrimetry and two kinds of methods of coulomb electric charge method.Be applicable to the mensuration of water cut in many mineral compounds and the organic compound.It is the classical way of universally acknowledged mensuration substance moisture content content.But the moisture in Fast Measurement liquid, the solid matter is the most single-minded, chemical method the most accurately, the industry standard analytical approach of using for Global Access.Be widely used in the units such as oil, chemical industry, electric power, medicine, pesticide industry and universities and colleges' scientific research.
Summary of the invention
Purpose of the present invention is exactly to provide a kind of operability good for the defective that overcomes above-mentioned prior art existence, accurately and reliably dynamic calibration apparatus and the method in the micro-moisture process in the optical method mensurated gas composition.
Purpose of the present invention can be achieved through the following technical solutions: the dynamic calibration apparatus in a kind of optical method mensurated gas composition in the micro-moisture process, it is characterized in that, comprise the gas bomb, variable valve, main flow meter, low temperature washing pipe, sample transfer valve, optics moisture teller, reversal valve and the cryogenic gas moisture absorption pipe-karl Fischer titration cell that connect successively, also comprise bypass valve and bypass flow meter, after bypass valve and the series connection of bypass flow meter, be connected in low temperature washing pipe two ends in parallel.
Described cryogenic gas moisture absorption pipe-karl Fischer titration cell comprises titration bottle, magnetic agitation external member, in the described titration bottle absorption liquid is housed, the titration bottleneck is inserted with sample introduction liquid pipe, karl Fischer reagent titrating head, the bleeder pipe with retaining valve, electrode and sample draft tube, described titration bottle is provided with cooling coil outward, is connected with liquid coolant in the cooling coil.
Described magnetic agitation external member comprises drive motor, magnet, magnetic stirring bar, and described magnet is fixed on the drive motor, and described magnetic stirring bar places the titration bottle bottom, and titration bottle places on the magnet.
The described sample introduction liquid pipe mouth of pipe is with the biscuiting ceramics, and this biscuiting ceramics makes gas bloat with tiny bubble, increases the bubble ratio surface area, improves the efficient of micro-moisture in the absorption liquid absorption of gases.
Described cryogenic gas moisture absorption pipe-Ka Erfei body titration cell and low temperature washing Guan Jun places constant temperature oven, also is provided with refrigeration compressor in the constant temperature oven, makes temperature stabilization in the constant temperature oven in zero degree or subzero.
A kind ofly use described device to carry out the dynamic calibrating method in the micro-moisture process in the optical method mensurated gas composition, the method is to make gas successively by optoacoustic spectroscopy moisture teller and the gas moisture absorption tube-karl Fischer titration cell of series connection, demarcates the optoacoustic spectroscopy moisture teller by the water cut that gas moisture absorption tube-karl Fischer titration cell is measured in the gas.
Described method specifically may further comprise the steps:
(1) in cooling coil, inputs liquid coolant, open refrigeration compressor and magnetic agitation external member, so that the temperature stabilization of constant temperature oven is in zero degree or subzero;
(2) in low temperature washing pipe, add pure water, be used for increasing micro-moisture at dry gas;
(3) treat after the temperature constant, open gas bomb, variable valve, main flow meter, bypass valve, bypass flow meter and optics moisture teller, the nitrogen that flow out this moment from steel cylinder will contain micro-moisture, and its moisture is directly read by the optics moisture teller;
(4) treat after the optics moisture teller stable reading, exhaust switched in cryogenic gas moisture absorption pipe-karl Fischer titration cell, add in advance an amount of moisture absorption liquid, and the titration blank value, record the time and the flow that absorb moisture content gas, calculate gas volume;
(5) above-mentioned moisture absorption liquid is carried out the karl Fischer titration, and measure the titration equivalent weight of karl Fischer reagent with pure water, draw moisture data in the gas of being measured by the karl Fischer method, with the nominal data of these data as step (3) optics moisture teller;
(6) obtain the gas of different in moisture content by regulating bypass valve and bypass flow meter, treat after the optics moisture teller stable reading, exhaust switched in cryogenic gas moisture absorption pipe-karl Fischer titration cell, add in advance an amount of moisture absorption liquid, and titration blank value, record the time and the flow that absorb moisture content gas, calculate gas volume, be used for the demarcation of optics moisture teller;
(7) demarcate when finishing, close gas cylinder, power supply and various valve.
The present invention utilizes moisture absorption pipe and karl Fischer titration cell to demarcate the optoacoustic spectroscopy moisture teller that is used for mensurated gas composition micro-moisture content, for realizing that the method comprises device and has: valve, flowmeter, optoacoustic spectroscopy moisture teller and gas moisture absorption tube-karl Fischer titration cell etc.Thereby solve existing optoacoustic spectroscopy moisture teller and demarcate hard problem.The present invention has the use of connecting with gas moisture absorption tube-karl Fischer titration cell of optoacoustic spectroscopy moisture teller, and synchronism is good; Micro-moisture content in the adjustable gas, the advantages such as good operability.
Compared with prior art, the present invention has the following advantages:
1) can use online, the optoacoustic spectroscopy moisture teller is connected with gas moisture absorption tube-karl Fischer titration cell, and namely gaseous sample passes through both successively, and synchronism is good.
2) micro-moisture content in the adjustable gas, good operability.
3) karl Fischer mensuration is integrated with moisture absorbing device, and is simple in structure.
4) adopt low temperature environment to carry out moisture absorption, efficient is high.
Description of drawings
Fig. 1 is the structural representation of system of the present invention;
Fig. 2 is cryogenic gas moisture in Fig. 1 system-karl Fischer method titration cell partial schematic diagram.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
Embodiment 1:
The present invention makes gas successively by optoacoustic spectroscopy moisture teller and the gas moisture absorption tube-karl Fischer titration cell of series connection, demarcates the optoacoustic spectroscopy moisture teller by the water cut that gas moisture absorption tube-karl Fischer titration cell is measured in the gas;
System schematic such as Fig. 1, comprise the gas bomb 1, variable valve 2, main flow meter 3, low temperature washing pipe 4, sample transfer valve 7, optics moisture teller 9, reversal valve 11, the cryogenic gas moisture absorption pipe-karl Fischer titration cell 8 that connect successively, also comprise bypass valve 5 and bypass flow meter 6, be connected in parallel on low temperature washing pipe 4 two ends after bypass valve 5 and 6 series connection of bypass flow meter, cryogenic gas moisture absorption pipe-karl Fischer titration cell 8 and low temperature washing pipe 4 all place constant temperature oven, also are provided with refrigeration compressor 10 in the constant temperature oven.
Described cryogenic gas moisture absorption pipe-karl Fischer titration cell structure as shown in Figure 2, comprise titration bottle, magnetic agitation external member, absorption liquid 8-5 is housed in the described titration bottle, the titration bottleneck is inserted with sample introduction liquid pipe 8-6, karl Fischer reagent titrating head 8-7, the bleeder pipe 8-8 with retaining valve, electrode 8-9 and sample draft tube 8-10, described titration bottle is provided with cooling coil 8-11 outward, be connected with liquid coolant 8-4 in the cooling coil 8-11, liquid coolant 8-4 is for can make the temperature of titration bottle maintain zero degree or sub-zero liquid, such as water, kerosene etc.The described sample introduction liquid pipe 8-6 mouth of pipe is with biscuiting ceramics 8-12, and this biscuiting ceramics 8-12 makes gas bloat with tiny bubble, increases the bubble ratio surface area, improves the efficient of micro-moisture in the absorption liquid absorption of gases.
Described magnetic agitation external member comprises drive motor 8-1, magnet 8-2, magnetic stirring bar 8-3, and described magnet 8-2 is fixed on the drive motor 8-1, and described magnetic stirring bar 8-3 places the titration bottle bottom, and titration bottle places on the magnet 8-2.
Use said apparatus to carry out the dynamic calibration in the micro-moisture process in the optical method mensurated gas composition, concrete steps are as follows:
Step (1) adds liquid coolant 8-4 in cooling coil 8-11, open refrigeration compressor 10 and magnetic agitation external member, so that the temperature stabilization of constant temperature oven is in zero degree or subzero.
Step (2) adds pure water in low temperature washing pipe 4, be used for increasing micro-moisture at drying nitrogen.
Step (3) is treated after the temperature constant, opens gas bomb 1, variable valve 2, main flow meter 3, bypass valve 5, bypass flow meter 6 and optics moisture teller 9.The nitrogen that flow out this moment from steel cylinder will contain micro-moisture, and its moisture can directly be read by optics moisture teller 9.
Step (4) is treated after optics moisture teller 9 stable reading, exhaust is switched to an amount of moisture absorption liquid of adding in cryogenic gas moisture absorption pipe-karl Fischer titration cell 8, and titration blank value, record the time and the flow that absorb moisture content gas, can calculate gas volume according to the two.
Step (5) is carried out the karl Fischer titration to above-mentioned moisture absorption liquid, and measures the titration equivalent weight of karl Fischer reagent with pure water, calculates moisture in the gas of being measured by the karl Fischer method.These data can be used as the nominal data of step (3) optics moisture teller 9.
Step (6) obtains the gas of different in moisture content by regulating bypass valve 5 and bypass flow meter 6, treat after optics moisture teller 9 stable reading, exhaust is switched to an amount of moisture absorption liquid of adding in cryogenic gas moisture absorption pipe-karl Fischer titration cell 8, and titration blank value, record the time and the flow that absorb moisture content gas, can calculate gas volume according to the two, be used for the demarcation of optics moisture teller 9.
Step (7) is demarcated when finishing, and closes gas cylinder, power supply and various valve.
Those of ordinary skill in the art will be appreciated that, above embodiment illustrates the present invention, and be not to be used as limitation of the invention, as long as in connotation scope of the present invention, all will drop in claims scope of the present invention variation, the modification of the above embodiment.
Claims (7)
1. the dynamic calibration apparatus in the micro-moisture process in the optical method mensurated gas composition, it is characterized in that, comprise the gas bomb, variable valve, main flow meter, low temperature washing pipe, sample transfer valve, optics moisture teller, reversal valve and the cryogenic gas moisture absorption pipe-karl Fischer titration cell that connect successively, also comprise bypass valve and bypass flow meter, after bypass valve and the series connection of bypass flow meter, be connected in low temperature washing pipe two ends in parallel.
2. the dynamic calibration apparatus in the micro-moisture process in a kind of optical method mensurated gas composition according to claim 1, it is characterized in that, described cryogenic gas moisture absorption pipe-karl Fischer titration cell comprises titration bottle, magnetic agitation external member, in the described titration bottle absorption liquid is housed, the titration bottleneck is inserted with sample introduction liquid pipe, Ka Erfei body reagent titrating head, the bleeder pipe with retaining valve, electrode and sample draft tube, described titration bottle is provided with cooling coil outward, is connected with liquid coolant in the cooling coil.
3. the dynamic calibration apparatus in the micro-moisture process in a kind of optical method mensurated gas composition according to claim 2, it is characterized in that, described magnetic agitation external member comprises drive motor, magnet, magnetic stirring bar, described magnet is fixed on the drive motor, described magnetic stirring bar places the titration bottle bottom, and titration bottle places on the magnet.
4. the dynamic calibration apparatus in the micro-moisture process in a kind of optical method mensurated gas composition according to claim 2, it is characterized in that, the described sample introduction liquid pipe mouth of pipe is with the biscuiting ceramics, this biscuiting ceramics makes gas bloat with tiny bubble, increase the bubble ratio surface area, improve the efficient of micro-moisture in the absorption liquid absorption of gases.
5. the dynamic calibration apparatus in the micro-moisture process in a kind of optical method mensurated gas composition according to claim 1, it is characterized in that, described cryogenic gas moisture absorption pipe-karl Fischer titration cell and low temperature washing Guan Jun place constant temperature oven, also be provided with refrigeration compressor in the constant temperature oven, make temperature stabilization in the constant temperature oven in zero degree or subzero.
6. a use such as any described device of claim 1-5 carry out the dynamic calibrating method in the micro-moisture process in the optical method mensurated gas composition, the method is to make gas successively by optoacoustic spectroscopy moisture teller and the gas moisture absorption tube-karl Fischer titration cell of series connection, demarcates the optoacoustic spectroscopy moisture teller by the water cut that gas moisture absorption tube-karl Fischer titration cell is measured in the gas.
7. the dynamic calibrating method in the micro-moisture process in a kind of optical method mensurated gas composition according to claim 6 is characterized in that described method specifically may further comprise the steps:
(1) in cooling coil, inputs liquid coolant, open refrigeration compressor and magnetic agitation external member, so that the temperature stabilization of constant temperature oven is in zero degree or subzero;
(2) in low temperature washing pipe, add pure water, be used for increasing micro-moisture at dry gas;
(3) treat after the temperature constant, open gas bomb, variable valve, main flow meter, bypass valve, bypass flow meter and optics moisture teller, the nitrogen that flow out this moment from steel cylinder will contain micro-moisture, and its moisture is directly read by the optics moisture teller;
(4) treat after the optics moisture teller stable reading, exhaust switched in cryogenic gas moisture absorption pipe-karl Fischer titration cell, add in advance an amount of moisture absorption liquid, and the titration blank value, record the time and the flow that absorb moisture content gas, calculate gas volume;
(5) above-mentioned moisture absorption liquid is carried out the karl Fischer titration, and measure the titration equivalent weight of karl Fischer reagent with pure water, draw moisture data in the gas of being measured by the karl Fischer method, with the nominal data of these data as step (3) optics moisture teller;
(6) obtain the gas of different in moisture content by regulating bypass valve and bypass flow meter, treat after the optics moisture teller stable reading, exhaust switched in cryogenic gas moisture absorption pipe-karl Fischer titration cell, add in advance an amount of moisture absorption liquid, and titration blank value, record the time and the flow that absorb moisture content gas, calculate gas volume, be used for the demarcation of optics moisture teller;
(7) demarcate when finishing, close gas cylinder, power supply and various valve.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149169A (en) * | 2013-02-28 | 2013-06-12 | 山东大学 | Trace water detecting device by taking water inside component of optical fiber gas sensor as reference |
| 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 |
| CN112557482A (en) * | 2020-11-17 | 2021-03-26 | 四川佳士特环境检测有限公司 | Method for measuring trace moisture in liquefied methane chloride |
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| US20080093555A1 (en) * | 2006-09-29 | 2008-04-24 | N.V. Organon | Method to determine water content in a sample |
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| CN202256237U (en) * | 2011-08-05 | 2012-05-30 | 郑州光力科技股份有限公司 | Measurement instrument for trace water in oil |
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| US20040241863A1 (en) * | 2001-08-22 | 2004-12-02 | Frawley Nile N | Method and apparatus for determination of water and for normal phase liquid chromatography |
| US20080093555A1 (en) * | 2006-09-29 | 2008-04-24 | N.V. Organon | Method to determine water content in a sample |
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| VIKRAM KESTENS ET.AL: "Online measurement of water content in candidate reference materials by AOTF-NIR using pork meat calibrants controlled by Karl Fischer titration", 《FOOD CHEMISTRY》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103149169A (en) * | 2013-02-28 | 2013-06-12 | 山东大学 | Trace water detecting device by taking water inside component of optical fiber gas sensor as reference |
| CN103149169B (en) * | 2013-02-28 | 2015-08-26 | 山东大学 | Utilize the method that the calibration system of trace aqueous vapor pick-up unit is demarcated device inside water |
| CN112557482A (en) * | 2020-11-17 | 2021-03-26 | 四川佳士特环境检测有限公司 | Method for measuring trace moisture in liquefied methane chloride |
| 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 |
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Address after: 200062 room 2004-C, Wuning Road, Shanghai, Putuo District, 509 Co-patentee after: Shanghai Chemical Research Institute Co., Ltd. Patentee after: Shanghai Tianke Chemical Detection Co., Ltd. Address before: 200062 room 2004-C, Wuning Road, Shanghai, Putuo District, 509 Co-patentee before: Shanghai Research Institute of Chemical Industry Patentee before: Shanghai Tianke Chemical Detection Co., Ltd. |
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Address after: 200062 6th Floor, 252 Building, 345 Yunling East Road, Putuo District, Shanghai Co-patentee after: Shanghai Chemical Research Institute Co., Ltd. Patentee after: Shanghai Chemical Institute Testing Co., Ltd. Address before: 200062 2004-C room, No. 509, Wuning Road, Shanghai, Putuo District Co-patentee before: Shanghai Chemical Research Institute Co., Ltd. Patentee before: Shanghai Tianke Chemical Detection Co., Ltd. |