CN103439153B - Atmosphere volatile organic compound condensation and concentration sampling device and method - Google Patents
Atmosphere volatile organic compound condensation and concentration sampling device and method Download PDFInfo
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Abstract
The invention discloses an atmosphere volatile organic compound condensation and concentration sampling device which comprises a low-temperature environmental cabinet and an atmosphere sampler, wherein a low-temperature cold trap device is arranged in the low-temperature environmental cabinet, and comprises a first-stage cold trap and a second-stage cold trap, the first-stage cold trap comprises a first condensation pipe and a first semiconductor chilling plate group, a first heating wire is wound on the first condensation pipe, the second-stage cold trap comprises a second condensation pipe and a second semiconductor chipping plate group, and a second heating wire is wound on the second condensation pipe. The invention also discloses an atmosphere volatile organic compound condensation and concentration sampling method. The atmosphere volatile organic compound condensation and concentration sampling device and method disclosed by the invention are capable of meeting the demand on online automatic monitoring of the content of a volatile organic compound, and can be used in on-site online automatic monitoring of the content of the atmosphere volatile organic compound.
Description
Technical field
The present invention relates to atmospheric environment checkout equipment technical field, specifically, relate to a kind of atmosphere volatile organic compound condensation and concentrate sampler and sampling method.
Background technology
The volatile organic matter contained in air, there is the harm such as teratogenesis, carcinogenic, mutagenesis mostly, and be the important arch-criminal of the phenomenons such as atmospheric photochemistry harm, greenhouse effect, therefore in order to the timely Inspect and control of the pollution level of air, volatile organic content in air is carried out to detecting in real time seems becomes more and more important, on-line monitoring is carried out to volatile organic content especially in the wild and become more and more important.At present, detect to have come mainly through stratographic analysis to the volatile organic matter in air.Because the volatile organic matter kind in air is more, and concentration is low, must carry out enrichment concentration, just can reach the requirement that analytical instrument detects.And for concerning volatile organic content online auto monitoring, require higher to concentration systems, following condition should be reached: do not consume cold-producing medium, enrichment desorption rate is fast, to shorten the analytical cycle of monitoring automatically.
At present, the device concentrated for laboratory volatile organic matter condensation generally uses liquid nitrogen refrigerating, namely directly liquid nitrogen is sprayed in the evaporator of cold-trap outside, utilizes liquid nitrogen vaporization to absorb heat and freezes.Such as, propose a kind of cryotrap in Chinese patent CN101337135, solve the consumption problem of condensing agent, and shorten concentration time.But the method liquid nitrogen consumption is large, refrigeration cost is higher, and liquid nitrogen field is changed simultaneously, and store difficulty, and analytical cycle is long, for operation and maintenance brings very big inconvenience, therefore it is not suitable for the continuous on-line monitoring in field.And at present generally use poriness adsorbent in cryotrap in technology, Rapid Thermal desorb again after cryosorption is carried out to volatile organic matter, in this process, is easy to produce cross pollution and " memory effect ".Therefore, current condensation enrichment facility and condensation method for concentration can not meet the needs to volatile organic content on-line monitoring.In addition, use poriness adsorbent volatile organic matter, desorption time is long, and whole analytical cycle is lengthened, and easily between different sample analysis, produces cross-contamination issue.
Summary of the invention
First technical matters to be solved by this invention is: provide a kind of and do not consume cold-producing medium, enrichment desorption rate is fast and analytical cycle is short atmosphere volatile organic compound condensation concentrates sampler.
Second technical matters to be solved by this invention is: provide a kind of and do not consume cold-producing medium, enrichment desorption rate is fast and analytical cycle is short atmosphere volatile organic compound condensation concentration sampling method.
For solving above-mentioned first technical matters, technical scheme of the present invention is: a kind of atmospheric volatile organic compounds cryogenic condensation enrichment facility, comprising:
Environmental chamber at low temperature, described environmental chamber at low temperature is connected with compressor, cryotrap device is provided with in described environmental chamber at low temperature, described cryotrap device comprises first order cold-trap and second level cold-trap, described first order cold-trap comprises the first condenser pipe and the first semiconductor chilling plate group, and described first condenser pipe is wound with the first heater strip; Described second level cold-trap comprises the second condenser pipe and the second semiconductor chilling plate group, and described second condenser pipe is wound with the second heater strip;
Air sampler, the output terminal of described air sampler is connected to the input end of mass flowmeter, the output terminal of described mass flowmeter is connected to the first end of the first multiport valve, second end of described first multiport valve is connected with carrier gas source of the gas, and the three-terminal link of described first multiport valve is to the entrance point of described first condenser pipe;
The endpiece of described first condenser pipe is connected with the entrance point of described second condenser pipe, the endpiece of described second condenser pipe is connected to the first end of the second multiport valve, second end of described second multiport valve is connected with blowback source of the gas, and the three-terminal link of described second multiport valve is to chromatographic detection input end.
Preferably, the first refrigeration cavity and the second refrigeration cavity is provided with in described environmental chamber at low temperature; Described first condenser pipe and described first heater strip are arranged in described first refrigeration cavity, and described second condenser pipe and described second heater strip are arranged in described second refrigeration cavity.
Preferably, described first semiconductor chilling plate group comprises the semiconductor chilling plate of electrical connection that two or more fits together and in parallel, described second semiconductor chilling plate group comprise more than three fit together and the semiconductor chilling plate of electrical connection in parallel.
Preferably, described first refrigeration cavity and described second refrigeration cavity are enclosed with heat-insulating material respectively.
Preferably, described first condenser pipe and described second condenser pipe are stainless steel condenser pipe.
Preferably, described air sampler is the air sampler with dedusting function.
Preferably, described first multiport valve and described second multiport valve are various way solenoid valve.
Preferably, described carrier gas source of the gas and described blowback source of the gas are the inert gas that purity is greater than 99.9%.
Preferably, described chromatograph is gas chromatograph or gas chromatograph-mass spectrometer.
For solving above-mentioned second technical matters, technical scheme of the present invention is: a kind of atmospheric volatile organic compounds cryogenic condensation concentration sampling method, comprises the following steps:
A. first start environmental chamber at low temperature, make it be in refrigerating state, make the first refrigeration cavity and the first condenser pipe reach the low temperature of-40 DEG C to-50 DEG C, make the second refrigeration cavity and the second condenser pipe reach the low temperature of-145 DEG C to-155 DEG C;
B. atmospheric volatile organic compounds is after air sampler sampling, open the first multiport valve, air sampler is communicated with environmental chamber at low temperature, atmospheric sample is quantitatively sent in environmental chamber at low temperature by mass flowmeter, first enter the first refrigeration cavity and carry out condensation, contain six carbon atom and above compound and moisture in atmospheric sample are condensed in the first condenser pipe, change into liquid or solid-state; Containing five carbon atoms and following compound in atmospheric sample, enter in the second condenser pipe and be converted into liquid state or solid-state, and other gas in air, be not condensed into liquid or solid-state, and directly emptying by the second multiport valve;
C. to be sampled reach aequum after, control the first multiport valve, the gas disconnecting mass flowmeter and the first condenser pipe flows, open the first heater strip in the first refrigeration cavity, the temperature of the first condenser pipe in the first refrigeration cavity is made to be raised to 10 DEG C, and control the first multiport valve, carrier gas source of the gas is communicated with the first condenser pipe; Be heated to 10 DEG C in first condenser pipe, now, water is in liquid state; and other are condensed in the volatile organic components in the first condenser pipe; after heating and gasifying, become gas phase, and purged by carrier gas source of the gas and carry out cryogenic condensation into the second condenser pipe and concentrate, carrier gas is emptying by the second multiport valve;
Minute d.5-10 after; open the second heater strip on the second condenser pipe; the second condenser pipe is made to be heated to 30-40 DEG C; control the second multiport valve; second condenser pipe is communicated with chromatograph; now volatile organic components changes gaseous state into, and carries it into chromatograph by carrier gas source of the gas and carry out quantitative test measurement;
E. after completing said process; stop the refrigerating state of environmental chamber at low temperature; open the first heater strip and the second heater strip; the first condenser pipe and the second condenser pipe temperature is made to be elevated to 300 DEG C; control the second multiport valve, blowback source of the gas is communicated with the second condenser pipe, carries out blowback cleaning; running time is 5-10 minute, and purge gas is emptying by the first multiport valve;
F., after blowback process completes, the first heater strip and the second heater strip is closed.
After have employed technique scheme, the invention has the beneficial effects as follows:
1. because atmosphere volatile organic compound condensation of the present invention concentrates sampler and sampling method, employing be semiconductor refrigerating technology, and semiconductor refrigerating technology utilizes the paltie effect of semiconductor material to freeze, and does not need cold-producing medium, direct refrigeration after energising.Semiconductor refrigerating has can the advantage such as continuous cooling, fast, the shockproof noise of refrigerating speed, life-span be long, convenient for installation and maintenance, can also realize accurate refrigeration, automatic controlling system process of refrigerastion easy to use.The refrigeration system of this technology can meet in the wild to the needs of volatile organic content on-line monitoring.Therefore the atmosphere volatile organic compound condensation of the present invention applying this Refrigeration Technique concentrates sampler, overcome the defect that traditional cryogenic condensation device exists owing to needing liquid nitrogen: liquid nitrogen consumption is large, refrigeration cost is higher, liquid nitrogen field is changed simultaneously, store difficulty, can be used for the online automatic detection on the spot of atmospheric volatile organic compounds content.
2. because the first condenser pipe in the present invention and the second condenser pipe are stainless steel condenser pipe.Therefore in condensation process, component directly condensation on stainless-steel pipe, but not condensation on traditional sorbing material, thermal desorption speed is fast, shortens analytical test period distances, and maximum possible avoid cross pollution and memory effect.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described:
Fig. 1 is the principle schematic that atmosphere volatile organic compound condensation of the present invention concentrates sampler;
In figure: 1, environmental chamber at low temperature; 2, the first refrigeration cavity; 3, the first condenser pipe; 4, the first heater strip; 5, the first semiconductor chilling plate group; 6, the second refrigeration cavity; 7, the second condenser pipe; 8, the second heater strip; 9, the second semiconductor chilling plate group; 10, air sampler; 11, mass flowmeter; 12, the first multiport valve; 13, carrier gas source of the gas; 14, the second multiport valve; 15; Blowback source of the gas; 16, chromatograph; 17, compressor; 18, semiconductor chilling plate.
Embodiment
Fig. 1 is the principle schematic that atmosphere volatile organic compound condensation of the present invention concentrates sampler, with reference to Fig. 1, atmosphere volatile organic compound condensation of the present invention concentrates sampler, and comprise environmental chamber at low temperature 1 and air sampler 10, air sampler 10 has dedusting function.
Environmental chamber at low temperature 1 is connected with compressor, cryotrap device is provided with in environmental chamber at low temperature 1, cryotrap device comprises first order cold-trap and second level cold-trap, and first order cold-trap comprises on the first condenser pipe 3 and the first semiconductor chilling plate group 5, first condenser pipe 3 and is wound with the first heater strip 4; Second level cold-trap comprises on the second condenser pipe 7 and the second semiconductor chilling plate group 9, second condenser pipe 7 and is wound with the second heater strip 8.Wherein, the first condenser pipe 3 and the second condenser pipe 7 all adopt stainless steel material to make, and inside surface is through Passivation Treatment.Therefore in condensation process, component directly condensation on stainless-steel pipe, but not condensation on traditional sorbing material, thermal desorption speed is fast, shortens analytical cycle, and maximum possible avoid cross pollution and memory effect.
The output terminal of air sampler 10 is connected to the input end of mass flowmeter 11, the output terminal of mass flowmeter 11 is connected to the first end of the first multiport valve 12, second end of the first multiport valve 12 is connected with the entrance point of three-terminal link to the first condenser pipe 3 of carrier gas source of the gas 13, first multiport valve 12.
The endpiece of the first condenser pipe 3 is connected with the entrance point of the second condenser pipe 7, the endpiece of the second condenser pipe 7 is connected to the first end of the second multiport valve 14, second end of the second multiport valve 14 is connected with the detection input end of three-terminal link to chromatograph 16 of blowback source of the gas 15, second multiport valve 14.Chromatograph 16 is gas chromatograph or gas chromatograph-mass spectrometer.
The first refrigeration cavity 2 and the second refrigeration cavity 6 is provided with in environmental chamber at low temperature 1; First condenser pipe 3 and the first heater strip 4 are arranged in the first refrigeration cavity 2, and the second condenser pipe 7 and the second heater strip 8 are arranged in the second refrigeration cavity 6.In the present embodiment, according to the needs of condensing temperature, semiconductor chilling plate 18, the second semiconductor chilling plate group 9 that first semiconductor chilling plate group 5 comprises electrical connection that two or more fits together and in parallel comprise more than three fit together and electrical connection in parallel semiconductor chilling plate 18.Wherein, by the first semiconductor cooling sheet group 5 processed for the first refrigeration cavity 2 provides refrigeration, by the second semiconductor chilling plate group 9 for the second refrigeration cavity 6 provides refrigeration.
In the present embodiment, the first refrigeration cavity 2 and the second refrigeration cavity 6 are enclosed with heat-insulating material respectively.First multiport valve 12 and the second multiport valve 14 are various way solenoid valve.First condenser pipe and the second condenser pipe are straight shape, snakelike or spirality.
Carrier gas source of the gas and blowback source of the gas are the inert gas that purity is greater than 99.9%.In the present embodiment, carrier gas source of the gas and blowback source of the gas are the helium that purity is greater than 99.9%.Certainly, other inert gas can also be adopted.Wherein, the meaning of carrier gas: in vapor-phase chromatography, mobile phase is gas, is called carrier gas.The effect of carrier gas enters chromatographic column together with certain flow velocity carrier band gaseous sample or the sample gas after gasification to be separated, again each component after separated is loaded into detecting device to detect, finally flow out condenser system emptying or collection, carrier gas has been carrier band effect and has not participated in centrifugation.
In the present embodiment, the course of work utilizing atmosphere volatile organic compound condensation of the present invention to concentrate sampler is:
A. first start environmental chamber at low temperature 1, make it be in refrigerating state, make the first refrigeration cavity 2 and the first condenser pipe 3 reach the low temperature of-40 DEG C to-50 DEG C; The second refrigeration cavity 6 and the second condenser pipe 7 is made to reach the low temperature of-145 DEG C to-155 DEG C;
B. atmospheric volatile organic compounds is after air sampler 10 is sampled, open the first multiport valve 12, air sampler 10 is communicated with environmental chamber at low temperature 1, atmospheric sample quantitatively to send in environmental chamber at low temperature 1 by mass flowmeter 11, first enter the first refrigeration cavity 2 and carry out condensation, in atmospheric sample containing six carbon atom and above compound and moisture boiling point higher, be first condensed in the first condenser pipe 3, change into liquid or solid-state; And the volatile organic matter that boiling point is lower; mainly containing five carbon atoms and following compound; other volatile organic matters such as formaldehyde, methyl alcohol and methane that especially in air, content is higher; enter in the second condenser pipe 7 and be converted into liquid state or solid-state; and other permanent gases in air, such as nitrogen, oxygen etc., because boiling point is lower; be not condensed into liquid or solid-state, and directly emptying by the second multiport valve 14;
C. to be sampled reach aequum after, control the first multiport valve 12, the gas disconnecting mass flowmeter 11 and the first condenser pipe 3 flows, open the first heater strip 4 in the first refrigeration cavity 2, the temperature of the first condenser pipe 3 in the first refrigeration cavity 2 is made to be raised to 10 DEG C fast, and control the first multiport valve 12, carrier gas source of the gas 13 is communicated with the first condenser pipe 3; 10 DEG C are heated in first condenser pipe 3; now; water is in liquid state; vapour pressure is very low; and other are condensed in the volatile organic components in the first condenser pipe 3; after heating and gasifying, become gas phase, and purged by the carrier gas of carrier gas source of the gas 13 and carry out cryogenic condensation into the second condenser pipe 7 and concentrate, carrier gas is emptying by the second multiport valve 14;
Minute d.5-10 after; open the second heater strip 8 on the second condenser pipe 7; the second condenser pipe 7 is made to be heated to 30-40 DEG C; control the second multiport valve 14; second condenser pipe 7 is communicated with chromatograph 16; now volatile organic components changes gaseous state into, and carries it into chromatograph 16 by carrier gas source of the gas 13 and carry out quantitative test measurement;
E. after completing said process; stop the refrigerating state of environmental chamber at low temperature 1; open the first heater strip 4 and the second heater strip 8; the first condenser pipe 3 and the second condenser pipe 7 temperature is made to be elevated to 300 DEG C; control the second multiport valve 14, blowback source of the gas 15 is communicated with the second condenser pipe 7, carries out blowback cleaning; running time is 5-10 minute, and purge gas is emptying by the first multiport valve 12;
F. after blowback process completes, close the first heater strip 4 and the second heater strip 8, and again make environmental chamber at low temperature 1 be in refrigerating state, make the first refrigeration cavity 2 and the second refrigeration cavity 6 reach design temperature, for sampling next time is ready.
The above-mentioned course of work of sampler is concentrated as can be seen from atmosphere volatile organic compound condensation of the present invention, atmosphere volatile organic compound condensation of the present invention concentrates sampler, what adopt is semiconductor refrigerating technology, and semiconductor refrigerating technology utilizes the paltie effect of semiconductor material to freeze, do not need cold-producing medium, directly freeze after energising.Semiconductor refrigerating has can the advantage such as continuous cooling, fast, the shockproof noise of refrigerating speed, life-span be long, convenient for installation and maintenance, can also realize accurate refrigeration, automatic controlling system process of refrigerastion easy to use.The refrigeration system of this technology can meet the needs to volatile organic content on-line real time monitoring.Therefore the atmosphere volatile organic compound condensation of the present invention applying this Refrigeration Technique concentrates sampler, overcome the defect existed owing to needing liquid nitrogen refrigerating of traditional cryogenic condensation device: liquid nitrogen consumption is large, refrigeration cost is higher, liquid nitrogen field is changed simultaneously, store difficulty, can be used for the online automatic detection on the spot of atmospheric volatile organic compounds content.In addition, condenser pipe of the present invention is not containing the stainless-steel tube of poriness sorbing material, and thermal desorption speed is fast, shortens the analytical test cycle, and maximum possible avoid cross pollution and memory effect.
The above is the citing of best mode for carrying out the invention, and the part wherein do not addressed in detail is the common practise of those of ordinary skill in the art.Protection scope of the present invention is as the criterion with the content of claim, and any equivalent transformation carried out based on technology enlightenment of the present invention, also within protection scope of the present invention.
Claims (10)
1. atmosphere volatile organic compound condensation concentrates a sampler, it is characterized in that, comprising:
Environmental chamber at low temperature, described environmental chamber at low temperature is connected with compressor, cryotrap device is provided with in described environmental chamber at low temperature, described cryotrap device comprises first order cold-trap and second level cold-trap, described first order cold-trap comprises the first condenser pipe and the first semiconductor chilling plate group, and described first condenser pipe is wound with the first heater strip; Described second level cold-trap comprises the second condenser pipe and the second semiconductor chilling plate group, and described second condenser pipe is wound with the second heater strip;
Air sampler, the output terminal of described air sampler is connected to the input end of mass flowmeter, the output terminal of described mass flowmeter is connected to the first end of the first multiport valve, second end of described first multiport valve is connected with carrier gas source of the gas, and the three-terminal link of described first multiport valve is to the entrance point of described first condenser pipe;
The endpiece of described first condenser pipe is connected with the entrance point of described second condenser pipe, the endpiece of described second condenser pipe is connected to the first end of the second multiport valve, second end of described second multiport valve is connected with blowback source of the gas, and the three-terminal link of described second multiport valve is to chromatographic detection input end.
2. atmosphere volatile organic compound condensation as claimed in claim 1 concentrates sampler, it is characterized in that: be provided with the first refrigeration cavity and the second refrigeration cavity in described environmental chamber at low temperature; Described first condenser pipe and described first heater strip are arranged in described first refrigeration cavity, and described second condenser pipe and described second heater strip are arranged in described second refrigeration cavity.
3. atmosphere volatile organic compound condensation as claimed in claim 1 concentrates sampler, it is characterized in that: described first semiconductor chilling plate group comprises the semiconductor chilling plate of electrical connection that two or more fits together and in parallel, described second semiconductor chilling plate group comprise more than three fit together and the semiconductor chilling plate of electrical connection in parallel.
4. atmosphere volatile organic compound condensation as claimed in claim 2 concentrates sampler, it is characterized in that: described first refrigeration cavity and described second refrigeration cavity are enclosed with heat-insulating material respectively.
5. atmosphere volatile organic compound condensation as claimed in claim 1 concentrates sampler, it is characterized in that: described first condenser pipe and described second condenser pipe are stainless steel condenser pipe.
6. atmosphere volatile organic compound condensation as claimed in claim 1 concentrates sampler, it is characterized in that: described air sampler is the air sampler with dedusting function.
7. atmosphere volatile organic compound condensation as claimed in claim 1 concentrates sampler, it is characterized in that: described first multiport valve and described second multiport valve are various way solenoid valve.
8. the atmosphere volatile organic compound condensation as described in any one of claim 1 to 7 concentrates sampler, it is characterized in that: described carrier gas source of the gas and described blowback source of the gas are the inert gas that purity is greater than 99.9%.
9. atmosphere volatile organic compound condensation as claimed in claim 8 concentrates sampler, it is characterized in that: described chromatograph is gas chromatograph or gas chromatograph-mass spectrometer.
10. adopt atmosphere volatile organic compound condensation according to claim 1 to concentrate the sampling method of sampler, it is characterized in that, comprise the following steps:
A. first start environmental chamber at low temperature, make it be in refrigerating state, make the first refrigeration cavity and the first condenser pipe reach the low temperature of-40 DEG C to-50 DEG C, make the second refrigeration cavity and the second condenser pipe reach the low temperature of-145 DEG C to-155 DEG C;
B. atmospheric volatile organic compounds is after air sampler sampling, open the first multiport valve, air sampler is communicated with environmental chamber at low temperature, atmospheric sample is quantitatively sent in environmental chamber at low temperature by mass flowmeter, first enter the first refrigeration cavity and carry out condensation, contain six carbon atom and above compound and moisture in atmospheric sample are condensed in the first condenser pipe, change into liquid or solid-state; Containing five carbon atoms and following compound in atmospheric sample, enter in the second condenser pipe and be converted into liquid state or solid-state, and other gas in air, be not condensed into liquid or solid-state, and directly emptying by the second multiport valve;
C. to be sampled reach aequum after, control the first multiport valve, the gas disconnecting mass flowmeter and the first condenser pipe flows, open the first heater strip in the first refrigeration cavity, the temperature of the first condenser pipe in the first refrigeration cavity is made to be raised to 10 DEG C, and control the first multiport valve, carrier gas source of the gas is communicated with the first condenser pipe; Be heated to 10 DEG C in first condenser pipe, now, water is in liquid state; and other are condensed in the volatile organic components in the first condenser pipe; after heating and gasifying, become gas phase, and purged by carrier gas source of the gas and carry out cryogenic condensation into the second condenser pipe and concentrate, carrier gas is emptying by the second multiport valve;
Minute d.5-10 after; open the second heater strip on the second condenser pipe; the second condenser pipe is made to be heated to 30-40 DEG C; control the second multiport valve; second condenser pipe is communicated with chromatograph; now volatile organic components changes gaseous state into, and carries it into chromatograph by carrier gas source of the gas and carry out quantitative test measurement;
E. after completing said process; stop the refrigerating state of environmental chamber at low temperature; open the first heater strip and the second heater strip; the first condenser pipe and the second condenser pipe temperature is made to be elevated to 300 DEG C; control the second multiport valve, blowback source of the gas is communicated with the second condenser pipe, carries out blowback cleaning; running time is 5-10 minute, and purge gas is emptying by the first multiport valve;
F., after blowback process completes, the first heater strip and the second heater strip is closed.
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