CN108554207B - Low-concentration standard gas continuous generation device and generation method thereof - Google Patents
Low-concentration standard gas continuous generation device and generation method thereof Download PDFInfo
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- CN108554207B CN108554207B CN201810616981.0A CN201810616981A CN108554207B CN 108554207 B CN108554207 B CN 108554207B CN 201810616981 A CN201810616981 A CN 201810616981A CN 108554207 B CN108554207 B CN 108554207B
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- 238000012546 transfer Methods 0.000 claims abstract description 54
- 238000009826 distribution Methods 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 3
- 238000013268 sustained release Methods 0.000 claims 2
- 239000012730 sustained-release form Substances 0.000 claims 2
- 238000007664 blowing Methods 0.000 claims 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 99
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- BGJSXRVXTHVRSN-UHFFFAOYSA-N 1,3,5-trioxane Chemical group C1OCOCO1 BGJSXRVXTHVRSN-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
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- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
- B01F23/10—Mixing gases with gases
- B01F23/19—Mixing systems, i.e. flow charts or diagrams; Arrangements, e.g. comprising controlling means
- B01F23/191—Mixing systems, i.e. flow charts or diagrams; Arrangements, e.g. comprising controlling means characterised by the construction of the controlling means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2213—Pressure
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/80—Forming a predetermined ratio of the substances to be mixed
- B01F35/83—Forming a predetermined ratio of the substances to be mixed by controlling the ratio of two or more flows, e.g. using flow sensing or flow controlling devices
Abstract
The invention discloses a low-concentration standard gas continuous generation device and a generation method thereof. Compared with the prior art, the technical scheme of the invention utilizes the mass transfer control device to control the volume of the air chamber, so that the pressure of the air chamber is stable, the standard gas with low concentration and uniform flow rate can be configured and continuously output, the air distribution operation is simple and convenient, the efficiency is high, and the stability is good.
Description
Technical Field
The invention relates to the technical field of standard gas generation, in particular to a low-concentration standard gas continuous generation device and a generation method thereof.
Background
Formaldehyde is one of the most widely existing indoor air pollutants, has caused serious environmental sanitation problem, along with the increasing understanding of people on formaldehyde, the demand for detecting indoor formaldehyde concentration is stronger, and only professional detection mechanisms can provide more accurate indoor formaldehyde concentration measurement at present, because accurate formaldehyde concentration measurement is more complicated, and the indoor formaldehyde concentration is detected by utilizing a gas sensor, although more convenient, the sensitivity, selectivity and stability requirements on the sensor are high due to the low concentration range (ppb range) of indoor formaldehyde detection, and the reliability of measurement is difficult to ensure under the condition of lacking professional maintenance. In order to obtain accurate and reliable measurement results, low-concentration formaldehyde standard gas is often required to be prepared for detecting and calibrating formaldehyde content detectors in indoor and outdoor air, and formaldehyde analysis and test methods, analysis quality control and the like are adopted
Formaldehyde is unstable in chemical property, is easily dissolved in water, is easily polymerized, and is free of formaldehyde pure products, so that a great deal of difficulty is brought to preparing formaldehyde standard gas.
The preparation method of the formaldehyde standard gas at present mainly comprises the following steps: static volume ratio mixing, dynamic flow ratio mixing, dynamic methods with diffuser pipes or permeate pipes as standard gas sources. At present, the diffusion tube using trioxymethylene as the raw material is mature in domestic application. In chinese patent application CN200610103424.6, a dynamic generation of formaldehyde standard gas using a trioxymethylene diffuser tube and a chemical cracking process is disclosed. The instrument is complex in equipment and high in price, needs professional personnel to maintain, and is difficult to popularize and use.
The micro-formaldehyde solution (1-10 ul) can be sucked by a micro-injector which is micro-upgraded in a laboratory to be diluted to a certain volume in an air bag, or formaldehyde gas with the concentration range of ppm is prepared in a container with a fixed volume, the indoor formaldehyde gas is actually detected, the required formaldehyde standard gas concentration is generally in the ppb concentration range, the requirement can be met by at least carrying out dilution operation for two times, if air distribution staff is not properly trained, the air distribution process is strictly controlled, human air distribution errors are introduced in the standard formaldehyde solution preparation, preservation, suction, transfer and gas dilution processes, and larger air distribution errors are caused, so that the method is inconvenient to popularize and use.
Another method of obtaining standard formaldehyde gas is to provide formaldehyde steel cylinder gas from qualified manufacturers, which can be used in a shelf life under the condition of low accuracy requirement, but the formaldehyde steel cylinder gas is unstable and cannot provide gas in ppb concentration range, and the transportation is inconvenient.
Disclosure of Invention
The invention aims to provide a low-concentration standard gas generating device and a generating method thereof, and the generating method has the advantages of simple equipment, low cost, convenient use, high reliability, convenient popularization and use and the like.
The invention aims to achieve the aim, and is specifically realized by the following technical scheme:
the utility model provides a low concentration standard gas continuously generating device, includes air inlet pipeline, air supply room, main air chamber and distribution pipeline, and the air supply room communicates with main air chamber through first air pump, installs pressure differential sensor in the main air chamber, and the air outlet end of main air chamber communicates with distribution pipeline through mass transfer controlling means, and air inlet pipeline communicates with air supply room and distribution pipeline respectively.
Further, the air inlet pipeline comprises a first filter, a second air pump and a flow sensor which are sequentially communicated.
Further, the air source chamber is a container filled with a fixed amount of air source solution.
Further, a second filter and a transfer air chamber are also communicated between the air source chamber and the first air pump.
Further, the mass transfer control device is a capillary tube, needle valve, inert porous gas permeable membrane, or other component made of an inert porous gas permeable material.
Further, the main air chamber is of a variable-volume air chamber structure.
Further, a movable piston or a telescopic air bag is arranged in the main air chamber.
Further, the main air chamber is an air bag made of flexible inert material.
The invention also provides a low-concentration standard gas continuous generation method using the generation device, which is simple to operate and long in gas generation duration, and comprises the following steps:
1) All purge the fixed amount air source in the air source chamber into the main air chamber through the air inlet pipeline by the clean air with known volume to obtain the target gas with known higher concentration;
2) Controlling and maintaining a constant pressure differential across the mass transfer control device through which a known higher concentration of target gas flows into the gas distribution conduit;
3) Clean gas with known flow flows into the gas distribution pipeline through the gas inlet pipeline, and the target gas with known higher concentration in the gas distribution pipeline is diluted and flows out to obtain the target gas with low concentration.
Further, in the step 2), the pressure difference between the two ends of the mass transfer control device is kept constant by measuring the pressure difference of the pressure difference sensor and feeding back and adjusting the gas volume in the main gas chamber in time.
Compared with the prior art, the technical scheme of the invention utilizes the mass transfer control device to control the volume of the air chamber, so that the pressure of the air chamber is stable, the standard gas with low concentration and uniform flow rate can be configured and continuously output, the air distribution operation is simple and convenient, the efficiency is high, and the stability is good.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present invention;
fig. 2 is a schematic structural diagram of another embodiment of the present invention.
In the figure, 1, an air inlet pipeline; 11. a first valve; 12. a first filter; 13. a second air pump; 14. a flow sensor; 15. a fourth valve; 2. an air source chamber; 21. a second valve; 22. a third valve; 3. a main air chamber; 31. an exhaust line; 32. an exhaust valve; 4. a first air pump; 5. a differential pressure sensor; 6. mass transfer control means; 7. a gas distribution pipeline; 71. an outlet valve; 8. a second filter; 9. and (5) transferring the air chamber.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples.
As shown in fig. 1, the low-concentration standard gas continuous generation device of the invention comprises a gas inlet pipeline 1, a gas source chamber 2, a main gas chamber 3 and a gas distribution pipeline 7. The air supply chamber 2 communicates with the main air chamber through a first air pump 4, preferably a second valve 21 is installed between the first air pump 4 and the main air chamber 3. A differential pressure sensor 5 is arranged in the main air chamber 3, an air outlet end of the main air chamber 3 is communicated with an air distribution pipeline 7 through a mass transfer control device 6, and the air inlet pipeline 1 is communicated with the air source chamber 2 through a first valve 11 and is communicated with the air distribution pipeline 7 through a first valve 11 and a fourth valve 15.
Preferably, the intake line 1 comprises a first filter 12, a second air pump 13 and a flow sensor 14, which are in communication in sequence. The first filter 12 is for filtering air, preferably potassium permanganate alumina particles and activated carbon particles according to a ratio of 3:1 are mixed according to the proportion.
The air source chamber 2 is a container filled with a fixed amount of air source solution, and comprises a glass bottle, a tube, a capsule and an air bag, wherein the components can be provided by a professional manufacturer, and the components are diluted into the transfer air chamber 9 by the quantitative air during air distribution. The gas concentration in the transfer chamber 9 obtained by this method is known. The target gas with known concentration is obtained in the gas source chamber 2 and the pipeline, and the target standard gas with required low concentration is obtained in the main gas chamber 3 and the distribution pipeline 7.
In the case of low gas flow rate, such as 4 hours of continuous gas consumption, the main gas chamber 3 may adopt a fixed volume gas chamber structure when the pressure change of the main gas chamber 3 is less than 5%. When the pressure change of the primary air chamber 3 is greater than 5% in one continuous use, preferably the primary air chamber 3 can adopt a structure with a fixed volume, the primary air chamber 3 can adopt a structure with a variable volume, preferably, the primary air chamber 3 can adopt a mode that a movable piston or a telescopic air bag is arranged inside, or the primary air chamber 3 is an air bag made of flexible inert materials, or a 'fish bubble' or a 'bellows' made of flexible inert materials is contained, and the primary air chamber 3 can be inflated or compressed by introducing or exhausting gas or liquid into the 'fish bubble' or the 'bellows', so as to achieve the purpose of adjusting the volume of the air chamber, and finally, the variable adjustment of the internal volume of the primary air chamber 3 is realized. Preferably, the main air chamber 3 is also connected with an exhaust pipeline 31 and an exhaust valve 32, which are used for conveniently exhausting air when the main air chamber 3 circulates air in a normal large-displacement mode or is cleaned.
As shown in fig. 2, a second filter 8 and a transfer air chamber 9 are also communicated between the air source chamber 2 and the first air pump 4. A third valve 22 is provided between the second filter 8 and the gas source chamber 2. The second filter 8 is used for removing moisture or organic vapor in the air source material of the air source chamber 2, and the transfer chamber 9 can be used as a primary distribution chamber for keeping the air stable during the transfer process of the air from the air source chamber 2 to the main chamber 3.
Preferably, mass transfer control device 6 is a capillary tube, needle valve, inert porous gas permeable membrane, or other component made of an inert porous gas permeable polymer, ceramic material. The mass transfer control device 6 is used to transfer the gas in the main gas chamber 3 at a constant flow rate into the gas distribution line 7. The gas phase mass transfer resistance can be adjusted according to actual needs, and a preferable scheme is to select a capillary tube with proper inner diameter and length for gas chromatography. According to the Bernoulli equation, when the gas phase mass transfer resistance of the mass transfer control means 6 is fixed, accurate control of the gas flow through the capillary tube can be achieved by controlling the pressure differential as long as the pressure differential across it remains constant and the gas flow through the resistance is determined.
Because the resistance of the gas distribution pipeline 7 is smaller, the pressure change at the mass transfer control device 6 is not large, so that the influence of the pressure change at the outlet of the mass transfer control device 6 on the mass transfer speed of gas can be ignored as long as the pressure in the main gas chamber 3 is controlled so that the pressure change at the outlet of the mass transfer control device 6 is far smaller than the pressure difference change at the two ends of the mass transfer control device 6, and the pressure in the main gas chamber 3 is directly measured and controlled at the moment. The gas pressure in the main gas chamber 3 can be adjusted as required, preferably in the range of 200 to 1000Pa, so that the pressure fluctuation at the outlet of the mass transfer control device 6 has less influence on the capillary mass transfer rate.
The main air chamber 3 contains a high-sensitivity differential pressure sensor 5 for measuring the differential pressure of the air at two ends of the mass transfer control device 5, thereby adjusting the pressure difference between the main air chamber 3 and the air distribution pipeline 7 to be constant. In one mode, when the pressure difference of the mass transfer control device 7 changes, the pressure difference sensor 5 is used for monitoring and feeding back the information in real time, and the piston, the telescopic air bag or the fish bubble structure of the main air chamber 3 is quickly adjusted to maintain the constant pressure difference at the two ends of the mass transfer control device 7. The method of pressurizing the main air chamber 3 can also be realized by a method of air supplementing and pressurizing by an air pump. In another way, after one continuous use of air, when the pressure change of the main air chamber 3 is less than 5%, the pressure difference change can be ignored, and the volume of the main air chamber 3 does not need to be adjusted to ensure the constant pressure difference. The dilution gas in the gas distribution pipeline 7 is carried out by the target gas flowing out of the main gas chamber 3 at a fixed flow rate, and the gas dilution ratio is calculated by the flow ratio.
An air outlet valve 71 is preferably installed on the air distribution pipeline 7, and the air outlet valve 71 is used for controlling the opening and closing of the air outlet end of the air distribution pipeline 7.
The invention also provides a low-concentration standard gas continuous generation method by using the generation device, which comprises the following steps:
step 1) all purging the fixed amount of air source in the air source chamber 2 into the main air chamber 3 through the air inlet pipeline 1 by clean air with known volume to obtain target gas with known higher concentration, in particular target gas with ppm concentration range; or the fixed amount of air source in the air source chamber 2 is completely purged into the transfer air chamber 9 through the air inlet pipeline 1 by using the known volume of clean air, the target air with the ppm concentration range is obtained, and then the target air with the ppm concentration range in the transfer air chamber 9 is transferred into the main air chamber 3 through the third valve 22 by the first air pump 4.
Step 2) controls and maintains a constant pressure differential across mass transfer control device 6, with a known higher concentration of target gas flowing through mass transfer control device 6 into gas distribution line 7. After the gas pressure in the main gas chamber 3 stabilizes, specifically, the pressure difference between the two ends of the mass transfer control device 6, the target gas flow passing through the mass transfer control device 6 is regarded as constant, and then the target gas flow output from the main gas chamber 3 into the gas distribution pipeline 7 is also constant.
Step 3) clean gas with known flow flows into the gas distribution pipeline 7 through the gas inlet pipeline 1, and the target gas with known higher concentration in the gas distribution pipeline 7 is diluted and flows out, so that the target standard gas with low concentration is continuously obtained. The first valve 11 is opened, a constant external dilution air source (generally clean air) is introduced into the distribution pipeline 7, and the outlet valve 23 communicated with the distribution pipeline 7 is opened, so that the ppb level target gas can be obtained.
In step 2), maintaining the pressure differential across the mass transfer control device 6 constant is accomplished by differential pressure measurement by the differential pressure sensor 5 and timely feedback and adjustment of the gas volume in the main gas chamber 3.
The following is a method of using the apparatus of the present invention, specifically taking the formulation of 100ppb formaldehyde gas as an example:
example 1
Step 1) the air source chamber 1 selects a formaldehyde metering tube prepared from 5 microliters of 2.8% formaldehyde solution, and flushes the formaldehyde metering tube into the main air chamber 3 with 1 liter of clean air;
and 2) controlling the pressure of the main air chamber 3 within the range of 1.02-1.1 kPa to control the air flow rate passing through the mass transfer control device 6 to be 0.2ml/min, and preparing the formaldehyde gas with about 100ppm, wherein the specific concentration is calculated by the formaldehyde content of the quantitative pipe and the volume of the diluent gas.
Step 3) selecting clean air as diluent gas, diluting the formaldehyde gas which is transferred by taking a capillary as a mass transfer control device 6 in a gas distribution pipeline 7 at a flow rate of 200ml/min, and obtaining the formaldehyde gas with a concentration of about 100ppb after dilution.
Under the condition of the distribution parameters, the continuous gas consumption is carried out for 4 hours, the change of the air pressure in the main air chamber 3 is less than 5%, and the stability of the distribution can be ensured.
Example two
Step 1) a formaldehyde metering tube prepared from 5. Mu.l of a 7% formaldehyde solution was selected and flushed with 5L of clean air through a second filter 8 into a transfer chamber 9 to obtain 50ppm formaldehyde gas. By controlling the third valve 22, the exhaust valve 32 and the first air pump 4, 50ppm of formaldehyde gas in the transfer air chamber 9 is transferred to the main air chamber 3, wherein the volume of the main air chamber 3 is preferably 100-200 ml.
Step 2) controlling the gas pressure in the main gas chamber 3, preferably 200-1000 Pa, so that the mass transfer rate of the gas passing through the capillary tube as the mass transfer control device 6 is controlled at 1ml/min, the capillary tube size is fixed, and the relation between the pressure and the flow is determined by a standard curve, which is calibrated in advance before the equipment leaves the factory.
Step 3) selecting clean air as diluent gas, diluting the formaldehyde gas which is transferred by taking a capillary as a mass transfer control device 6 in a gas distribution pipeline 7 at a flow rate of 500ml/min, and obtaining the formaldehyde gas with the concentration of about 100ppb after dilution.
If the volume of the main air chamber 3 is 200ml, the main air chamber 3 is full of air for continuous air supply for about 3 hours at a time according to the air distribution parameters, and the application requirements of most customers can be met.
The gas distribution device can be simplified according to the gas utilization accuracy, for example, the size of a proper gas chamber is selected, so that the pressure change of a main gas chamber is ensured to be less than 5% in the gas utilization time, and the gas chamber with a fixed volume can be selected to simplify the design on the premise of ensuring certain gas distribution accuracy. If the gas distribution parameters are adopted, the volume of the main gas chamber 11 can be about 1.5L to ensure the gas utilization accuracy for 1 hour.
The smaller air outlet amount can be controlled by adjusting the resistance of the mass transfer control device 6 and the pressure difference between two ends of the mass transfer control device, the volume of the main air chamber 3 can be further reduced, for example, the air outlet amount of 0.1ml/min is matched with the volume of 150ml of the main air chamber, and correspondingly, the volume of the transfer air chamber 9 can be reduced, so that the portable equipment can be manufactured.
The specific embodiments of the present invention are intended to be illustrative, rather than limiting, of the invention, and modifications thereof will be suggested to persons skilled in the art to which the present invention pertains without inventive contribution, as desired, after having read the present specification, but are to be protected by the patent law within the scope of the appended claims.
Claims (7)
1. The low-concentration standard gas continuous generation device is characterized by comprising an air inlet pipeline (1), an air source chamber (2), a main air chamber (3) and an air distribution pipeline (7), wherein the air source chamber is communicated with the main air chamber through a first air pump (4), a differential pressure sensor (5) is arranged in the main air chamber, an air outlet end of the main air chamber is communicated with the air distribution pipeline (7) through a mass transfer control device (6), and the air inlet pipeline is respectively communicated with the air source chamber and the air distribution pipeline;
the mass transfer control device (6) is a capillary tube, a needle valve, an inert porous ventilated membrane or other parts made of inert porous ventilated materials;
the main air chamber is of an air chamber structure with variable volume; the pressure difference of the two ends of the mass transfer control device (6) is kept constant by measuring the pressure difference of the pressure difference sensor and feeding back and adjusting the gas volume in the main gas chamber (3) in time.
2. The low concentration standard gas continuous generating apparatus according to claim 1, wherein the intake pipe includes a first filter (12), a second air pump (13) and a flow sensor (14) which are sequentially communicated.
3. The low concentration standard gas sustained release apparatus of claim 1, wherein the gas source chamber is a container containing a fixed amount of gas source solution.
4. The low-concentration standard gas continuous generation device according to claim 1, wherein a second filter (8) and a transfer air chamber (9) are further communicated between the air source chamber and the first air pump.
5. The low concentration standard gas continuous generating apparatus according to claim 1, wherein a movable piston or a telescopic airbag is provided in the main gas chamber.
6. The low concentration standard gas sustained release apparatus of claim 1, wherein the main gas chamber is an air bag made of a flexible inert material.
7. A method for continuously generating a low concentration standard gas using the generating apparatus according to any one of claims 1 to 6, comprising the steps of:
1) completely blowing a fixed amount of air source in an air source chamber (2) into a main air chamber (3) by clean air with a known volume through an air inlet pipeline (1) to obtain target gas with a known higher concentration;
2) Controlling and maintaining the pressure difference across the mass transfer control means (6) constant, the known higher concentration target gas flowing through the mass transfer control means (6) into the gas distribution line (7);
3) Clean gas with known flow rate flows into the gas distribution pipeline (7) through the gas inlet pipeline (1), and target gas with known higher concentration in the gas distribution pipeline (7) is diluted and flows out, so that low-concentration target standard gas is continuously obtained.
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| JP2011230062A (en) * | 2010-04-28 | 2011-11-17 | Kawata Mfg Co Ltd | Apparatus for producing ozone water |
| CN202315847U (en) * | 2011-11-05 | 2012-07-11 | 内蒙古科技大学 | Simple air distribution device |
| CN203422675U (en) * | 2013-07-25 | 2014-02-05 | 上海上计群力分析仪器有限公司 | Dynamic trace gas concentration distributing apparatus |
| CN104807968A (en) * | 2015-05-11 | 2015-07-29 | 杭州北辰光电技术有限公司 | Gas sensor and identification and calibration method thereof |
| CN204911266U (en) * | 2015-07-14 | 2015-12-30 | 山西新华化工有限责任公司 | Normal atmospheric temperature is in liquid gaseous reference material down and takes place system |
| CN204832124U (en) * | 2015-08-11 | 2015-12-02 | 昆山禾信质谱技术有限公司 | Quasi -state distribution appearance based on mass spectrum feedback |
| CN107715711A (en) * | 2017-08-28 | 2018-02-23 | 深圳市好美达科技有限公司 | Proof-spirit gas generation apparatus |
| CN107694359A (en) * | 2017-10-25 | 2018-02-16 | 中国原子能科学研究院 | A kind of preparation facilities and preparation method of hydrogen deuterium Standard Gases |
| CN208852714U (en) * | 2018-06-15 | 2019-05-14 | 上海雷密传感技术有限公司 | A kind of low concentration calibrating gas continues generating device |
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