CN103499662A - Sampling analysis device and sampling analysis method for atmosphere volatile organic compounds - Google Patents
Sampling analysis device and sampling analysis method for atmosphere volatile organic compounds Download PDFInfo
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- CN103499662A CN103499662A CN201310438314.5A CN201310438314A CN103499662A CN 103499662 A CN103499662 A CN 103499662A CN 201310438314 A CN201310438314 A CN 201310438314A CN 103499662 A CN103499662 A CN 103499662A
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Abstract
The invention discloses a sampling analysis device for atmosphere volatile organic compounds. The sampling analysis device comprises a low-temperature environmental box and an atmosphere sampler, wherein low-temperature cold trap devices are arranged in the low-temperature environmental box and comprise a first cold trap, a second cold trap and a third cold trap, the first cold trap comprises a first condensation pipe and a first semiconductor chilling plate set, and a first heating wire is wound on the first condensation pipe; the second cold trap comprises a second condensation pipe and a second semiconductor chilling plate set, and a second heating wire is wound on the second condensation pipe; the third cold trap comprises a third condensation pipe and a third semiconductor chilling plate set. The invention further discloses a sampling analysis method for the atmosphere volatile organic compounds. The sampling analysis device and the sampling analysis method can meet requirements on the online monitoring of the contents of the volatile organic compounds and can be used for automatically detecting the contents of the atmosphere volatile organic compounds in an on-site and online manner.
Description
Technical field
The present invention relates to atmospheric environment checkout equipment technical field, specifically, relate to a kind of atmospheric volatile organic compounds sampling analysis device and sampling and analyzing method.
Background technology
The volatility contained in atmosphere, mostly there is the harm such as teratogenesis, carcinogenic, mutagenesis, and be the important arch-criminal of the phenomenons such as atmospheric photochemistry harm, greenhouse effect, therefore for the monitoring in time of the pollution level to atmosphere and control, atmospheric volatile organic compounds content is carried out to detecting in real time seems becomes more and more important, especially volatile organic content is carried out to on-line monitoring and become more and more important.At present, atmospheric volatile organic compounds is detected mainly and completed by stratographic analysis.Because the volatile organic matter kind in atmosphere is many, and concentration is low, must carry out enrichment concentration (the micro substance in atmospheric being become to solid-state reduced volume), just can reach the requirement that analytical instrument detects.And, for concerning volatile organic content is carried out on-line monitoring, concentration systems is had relatively high expectations, should reach following condition: do not consume cold-producing medium, the enrichment desorption rate is fast, in order to shorten the analytical cycle of monitoring automatically.
At present, the device concentrated for laboratory volatile organic matter condensation generally used liquid nitrogen refrigerating, directly liquid nitrogen sprayed in the evaporator of cold-trap outside, utilizes liquid nitrogen vaporization to absorb heat and freezed.For example in Chinese patent CN101337135, propose a kind of cryotrap, solved the consumption problem of condensing agent, and shortened concentration time.But the method liquid nitrogen consumption is large, the refrigeration cost is higher, and the liquid nitrogen field is changed simultaneously, store difficulty, and analytical cycle is long, and for operation and maintenance brings very big inconvenience, so it is not suitable for continuous on-line monitoring.And at present in technology, in cryotrap, generally use the poriness adsorbent, volatile organic matter is carried out to Rapid Thermal desorb again after cryosorption, in this process, be easy to produce cross pollution and " memory effect ".Therefore, current condensation enrichment facility and condensation method for concentration can not meet the needs to the volatile organic content on-line monitoring.In addition, use poriness adsorbent adsorbing volatilizing organic matter, desorption time is long, whole analytical cycle is lengthened, and easily between different sample analysis, produce cross-contamination issue.Have again, in atmosphere, volatile organic matter is of a great variety, when needs are used gas chromatograph to be analyzed the volatile organic content in atmosphere, need to analyze tens kinds and even hundreds of kind carbon containing class material, the gas chromatographs that the many uses of gas chromatograph at present have a capillary separation column, due to single capillary column to all volatile organic matter poor selectivity in atmosphere, cause separation efficiency low, generally need to surpass the long capillary column of 60m, could realize the separation fully to material, cause and require the requirement of system sample introduction pressure high, the shortcomings such as analytical cycle length.
Summary of the invention
First technical matters to be solved by this invention is: a kind of cold-producing medium, the enrichment desorption rate is fast and analytical cycle is short atmospheric volatile organic compounds sampling analysis device of not consuming is provided.
Second technical matters to be solved by this invention is: a kind of cold-producing medium, the enrichment desorption rate is fast and analytical cycle is short atmospheric volatile organic compounds sampling and analyzing method of not consuming is provided.
For solving above-mentioned first technical matters, technical scheme of the present invention is: a kind of atmospheric volatile organic compounds sampling analysis device comprises:
Environmental chamber at low temperature, described environmental chamber at low temperature is connected with compressor, be provided with the cryotrap device in described environmental chamber at low temperature, described cryotrap device comprises the first cold-trap, the second cold-trap and the 3rd cold-trap, described the first cold-trap comprises the first condenser pipe and the first semiconductor chilling plate group, on described the first condenser pipe, is wound with the first heater strip; Described the second cold-trap comprises the second condenser pipe and the second semiconductor chilling plate group, on described the second condenser pipe, is wound with the second heater strip; Described the 3rd cold-trap comprises the 3rd condenser pipe and the 3rd semiconductor chilling plate group, on described the 3rd condenser pipe, is wound with the 3rd 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, the second end of described the first multiport valve is connected with the carrier gas source of the gas, and the 3rd end of described the first multiport valve is connected to the entrance point of described the first condenser pipe;
The endpiece of described the first condenser pipe is connected to the 3rd end of the second multiport valve, and the first end of described the second multiport valve is connected with the entrance point of described the second condenser pipe, and the second end of described the second multiport valve is connected with the entrance point of described the 3rd condenser pipe;
The endpiece of described the second condenser pipe is connected to the 3rd end of the 3rd multiport valve, and the first end of described the 3rd multiport valve is connected with the blowback source of the gas, and the second end of described the 3rd multiport valve is connected to the first chromatographic detection input end;
The endpiece of described the 3rd condenser pipe is connected to the 3rd end of the 4th multiport valve, and the first end of described the 4th multiport valve is connected with described blowback source of the gas, and the second end of described the 4th multiport valve is connected to the second chromatographic detection input end.
Preferably, be provided with the first refrigeration cavity, the second refrigeration cavity and the 3rd refrigeration cavity in described environmental chamber at low temperature; Described the first condenser pipe and described the first heater strip are arranged in described the first refrigeration cavity, described the second condenser pipe and described the second heater strip are arranged in described the second refrigeration cavity, and described the 3rd condenser pipe and described the 3rd heater strip are arranged in described the 3rd refrigeration cavity.
Preferably, also be connected with semipermeable partition between the second end of described the second multiport valve and the entrance point of described the 3rd condenser pipe except water pipe, described semipermeable partition is provided with drying tube except the water pipe outer cover.
Preferably, also be connected with pressure valve between the entrance point of described semipermeable partition except the endpiece of water pipe and described the 3rd condenser pipe.
Preferably, described the first semiconductor chilling plate group comprises the semiconductor chilling plate be electrically connected to that fit together more than two and in parallel, described the second semiconductor chilling plate group comprises the semiconductor chilling plate be electrically connected to that fit together more than three and in parallel, and described the 3rd semiconductor chilling plate group comprises the semiconductor chilling plate be electrically connected to that fit together more than two and in parallel.
Preferably, the outside of described the first refrigeration cavity, described the second refrigeration cavity and described the 3rd refrigeration cavity is enclosed with respectively heat-insulating material.
Preferably, described the first condenser pipe, described the second condenser pipe and described the 3rd condenser pipe are the stainless steel condenser pipe.
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%.
For solving above-mentioned second technical matters, technical scheme of the present invention is: a kind of atmospheric volatile organic compounds sampling and analyzing method comprises the following steps:
A. at first start environmental chamber at low temperature, make it in refrigerating state, make the first refrigeration cavity and the first condenser pipe reach the low temperature of-40 ℃ to-50 ℃, make the second refrigeration cavity and the second condenser pipe reach the low temperature of-145 ℃ to-155 ℃, make the 3rd refrigeration cavity and the 3rd condenser pipe reach the low temperature of-55 ℃ to-65 ℃;
B. atmospheric volatile organic compounds is after the air sampler sampling, control the first multiport valve and the second multiport valve, air sampler is communicated with environmental chamber at low temperature, the first condenser pipe is communicated with the second condenser pipe, atmospheric sample is quantitatively sent in environmental chamber at low temperature by mass flowmeter, at first enter the first refrigeration cavity and carry out condensation, in atmospheric sample containing six carbon atom and above volatile organic compounds and moisture, at first be condensed in the first condenser pipe, change into solid-state; In atmospheric sample containing five carbon atoms and following volatile organic matter enter in the second condenser pipe, be converted into solid-state; And other gas in atmosphere is not condensed into solid-state, and directly emptying by the 3rd multiport valve;
C. treat that sampling reaches aequum, balance is after a period of time, control the first multiport valve, control the second multiport valve, disconnect the gas flow of mass flowmeter and the first condenser pipe, the first condenser pipe is communicated with the 3rd condenser pipe, open the first heater strip in the first refrigeration cavity, make the temperature of the first condenser pipe in the first refrigeration cavity be raised to 50 ℃, and control the first multiport valve, the carrier gas source of the gas is communicated with the first condenser pipe; Be heated to 50 ℃ in the first condenser pipe, now, water is in liquid state, and other is condensed in the volatile organic matter component in the first condenser pipe, after being heated to 50 ℃ of gasifications, transfer in gas phase, and by the carrier gas source of the gas, its purging being entered to the 3rd condenser pipe, to carry out cryogenic condensation concentrated, carrier gas is emptying by the 4th multiport valve;
D.5-10 minute after, close the second multiport valve and pressure valve, open the 3rd heater strip on the 3rd condenser pipe, make the 3rd condenser pipe be heated to 50 ℃, now the volatile organic matter in the 3rd condenser pipe all changes gaseous state into, and be written into the second chromatograph by the carrier gas source of the gas and detect analysis, complete the detection analysis containing six carbon atom and above volatile organic compounds in atmospheric sample;
E. simultaneously, sampling quantity reach set quantitatively after, control the second multiport valve, the off-state that keeps the first condenser pipe and the second condenser pipe, open the second heater strip on the second condenser pipe, make the temperature increase to 50 ℃ in the second condenser pipe, make the solid-state volatile organic matter in the second condenser pipe change gaseous state into, and be written into the first chromatograph by the carrier gas source of the gas and detect analysis, complete in atmospheric sample the detection analysis containing five carbon atoms and following volatile organic matter;
F. after completing said process, stop the refrigerating state of environmental chamber at low temperature, open the first heater strip, the second heater strip and the 3rd heater strip, make the first condenser pipe, the second condenser pipe and the 3rd condenser pipe temperature be elevated to 300 ℃, control the first multiport valve, the second multiport valve, the 3rd multiport valve and the 4th multiport valve, the blowback source of the gas is communicated with the second condenser pipe and the 3rd condenser pipe, and is communicated with the first condenser pipe, carry out the blowback cleaning, purge gas is emptying by the first multiport valve;
G. after the blowback process completes, close the first heater strip, the second heater strip and the 3rd heater strip, and reopen environmental chamber at low temperature and make it in refrigerating state, make the first refrigeration cavity, the second refrigeration cavity and the 3rd refrigeration cavity reach and set temperature, for next time sampling and condensation concentration ready.
Preferably, further comprising the steps of between step b and step c:
B1. control the first multiport valve, control the second multiport valve, disconnect the gas flow of mass flowmeter and the first condenser pipe, the first condenser pipe is communicated with except water pipe with semipermeable partition, the opening pressure valve makes semipermeable partition remove the certain malleation of maintenance in water pipe, opens the first heater strip in the first refrigeration cavity, makes the temperature of the first condenser pipe in the first refrigeration cavity be raised to 50 ℃, and control the first multiport valve, the carrier gas source of the gas is communicated with the first condenser pipe; Be heated to 50 ℃ in the first condenser pipe, now, water is in liquid state, and other is condensed in the volatile organic matter component in the first condenser pipe, after being heated to 50 ℃ of gasifications, transfer in gas phase, and by the carrier gas source of the gas, it is purged into semipermeable partition and further dewaters except in water pipe, carrier gas is emptying by the second multiport valve.
After having adopted technique scheme, the invention has the beneficial effects as follows:
1. due to atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method, employing be semiconductor refrigerating technology, and semiconductor refrigerating technology utilizes the paltie effect refrigeration of semiconductor material, does not need cold-producing medium, after energising, directly freezes.But semiconductor refrigerating has the advantages 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 the volatile organic content on-line monitoring.Therefore apply atmospheric volatile organic compounds sampling analysis device of the present invention and the sampling and analyzing method of this Refrigeration Technique, overcome traditional cryogenic condensation device due to the defect that needs liquid nitrogen refrigerating and poriness adsorbent to exist: the liquid nitrogen consumption is large, the refrigeration cost is higher, the liquid nitrogen field is changed simultaneously, stores difficulty; Poriness adsorbent heat desorption rate is slow, the residual height of component, and required purge time is long, thereby causes the shortcomings such as analytical cycle is long, can be used for the online automatic detection on the spot of atmospheric volatile organic compounds content.In addition, atmospheric volatile organic compounds sampling analysis device of the present invention in the course of the work, switch by the first multiport valve, the second multiport valve, the 3rd multiport valve and the 4th multiport valve is controlled and the setting of the first cold-trap, the second cold-trap and the 3rd cold-trap different temperatures, makes in atmosphere to enter the second chromatograph containing six carbon atom and above volatile organic matter after by the first cold-trap and the 3rd cold-trap and detect analysis.And in atmosphere, remaining volatile organic matter enters the first chromatograph after by the second cold-trap and detects analysis, and this setting can adopt capillary column of different nature and dissimilar detecting device to the first and second chromatographs, increased the responsiveness of whole analytic system to the heterogeneity volatile organic matter.
2. also be connected with semipermeable partition between the entrance point due to the second end of described the second multiport valve and described the 3rd condenser pipe except water pipe, described semipermeable partition is provided with drying tube except the water pipe outer cover.Therefore atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method combine with the semi-permeable technology of dewatering by the segmentation condensation is concentrated, make in atmosphere containing six carbon atom to containing the volatile organic matter of 12 carbon atoms through semipermeable partition during except water pipe, further remove moisture wherein, the elimination of maximum possible moisture on stratographic analysis impact, make it enter after the second chromatograph that to detect the result of analyzing more accurate.
3. because the first condenser pipe in the present invention, the second condenser pipe and the 3rd condenser pipe all adopt the stainless steel condenser pipe, therefore in condensation process, directly condensation on stainless-steel pipe of component, but not condensation on traditional poriness sorbing material, maximum possible avoided cross pollution between different analytical cycles and " memory " effect of system.
4. due to atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method, use highly purified inert gas to carry out blowback to the first condenser pipe, the second condenser pipe and the 3rd condenser pipe, and in condenser pipe containing the poriness sorbing material, purging speed is fast, greatly improved thermal desorption speed, but the self-cleaning of completion system in a short period of time, shorten analytical cycle.
The accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described:
Fig. 1 is the principle schematic of atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method;
In figure: 1, environmental chamber at low temperature; 2, the first refrigeration cavity; 21, the first condenser pipe; 22, the first heater strip; 3, the first semiconductor chilling plate group; 4, the second refrigeration cavity; 41, the second condenser pipe; 42, the second heater strip; 5, the second semiconductor chilling plate group; 6, the 3rd refrigeration cavity; 61, the 3rd condenser pipe; 62, the 3rd heater strip; 7, the 3rd semiconductor chilling plate group; 8, air sampler; 9, mass flowmeter; 10, the first multiport valve; 11, carrier gas source of the gas; 12, the second multiport valve; 13, the 3rd multiport valve; 14, the 4th multiport valve; 15, blowback source of the gas; 16, the first chromatograph; 17, the second chromatograph; 18, compressor; 19, semiconductor chilling plate; 20, semipermeable partition is except water pipe; 30, drying tube; 40, pressure valve.
Embodiment
Fig. 1 is the principle schematic of atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method, with reference to Fig. 1, atmospheric volatile organic compounds sampling analysis device of the present invention, comprise environmental chamber at low temperature 1 and air sampler 8, and air sampler 8 has dedusting function.
Environmental chamber at low temperature 1 is connected with compressor, be provided with the cryotrap device in environmental chamber at low temperature 1, the cryotrap device comprises the first cold-trap, the second cold-trap and the 3rd cold-trap, the first cold-trap comprises on the first condenser pipe 21 and the first semiconductor chilling plate group 3, the first condenser pipes 21 and is wound with the first heater strip 22; The second cold-trap comprises on the second condenser pipe 41 and the second semiconductor chilling plate group 5, the second condenser pipes 41 and is wound with the second heater strip 42; The 3rd cold-trap comprises on the 3rd condenser pipe 61 and the 3rd semiconductor chilling plate group 7, the three condenser pipes 61 and is wound with the 3rd heater strip 62.Wherein, the first condenser pipe 21, the second condenser pipe 41 and the 3rd condenser pipe 61 all adopt stainless steel material to make, and inside surface is through Passivation Treatment.So in condensation process, directly condensation on stainless-steel pipe of component, but not condensation on traditional poriness sorbing material, thermal desorption speed is fast, and " memory " effect of having avoided cross pollution and system of maximum possible.
The output terminal of air sampler 8 is connected to the input end of mass flowmeter 9, the output terminal of mass flowmeter 9 is connected to the first end of the first multiport valve 10, the 3rd end that the second end of the first multiport valve 10 is connected with carrier gas source of the gas 11, the first multiport valves 10 is connected to the entrance point of the first condenser pipe 21.
The endpiece of the second condenser pipe 41 is connected to the 3rd end of the second multiport valve 12, and the first end of the second multiport valve 12 is connected with the entrance point of the second condenser pipe 41, and the second end of the second multiport valve 12 is connected with the entrance point of the 3rd condenser pipe 61.In the present embodiment, also be connected with semipermeable partition between the second end of the second multiport valve 12 and the entrance point of the 3rd condenser pipe 61 except water pipe 20, semipermeable partition also is arranged with drying tube 30 except the outside of water pipe 20, between the entrance point of semipermeable partition except the endpiece of water pipe 20 and the 3rd condenser pipe 61, also is connected with pressure valve 40.Semipermeable partition is the Nafion semi-permeable film except water pipe 20, water is by the semi-permeable membranous wall infiltration of Nafion, and evaporation subsequently enters in surrounding air, and we call " pervaporation " to this process, played the function dewatered, the inside and outside moist gradient of pipe has driven whole process.And pressure valve 40 has kept when Nafion semipermeable partition pipe is inherent works keeping certain malleation.Make Nafion semipermeable partition pipe play good water removal effect to the volatile organic matter in atmosphere.
The endpiece of the second condenser pipe 41 is connected to the 3rd end of the 3rd multiport valve 13, and the first end of the 3rd multiport valve 13 is connected with blowback source of the gas 15, and the second end of the 3rd multiport valve 13 is connected to the detection input end of the first chromatograph 16.Atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method are used highly purified inert gas to carry out blowback to the first condenser pipe, the second condenser pipe and the 3rd condenser pipe, purging speed is fast, greatly improved thermal desorption speed, but the self-cleaning of completion system, shortened analytical cycle in a short period of time.
The endpiece of the 3rd condenser pipe 61 is connected to the 3rd end of the 4th multiport valve 14, and the first end of the 4th multiport valve 14 is connected with blowback source of the gas 15, and the second end of the 4th multiport valve 14 is connected to the detection input end of the second chromatograph 17.
The first chromatograph 16 and the second chromatograph 17 are two independently chromatograph analytic systems, in-built capillary column of different nature.The first chromatograph 16 and the second chromatograph 17 are gas chromatograph or gas chromatograph-mass spectrometer.
Be provided with the first refrigeration cavity 2, the second refrigeration cavity 4 and the 3rd refrigeration cavity 6 in environmental chamber at low temperature 1; The first condenser pipe 21 and the first heater strip 22 are arranged in the first refrigeration cavity 2, and the second condenser pipe 41 and the second heater strip 42 are arranged in the second refrigeration cavity 4; The 3rd condenser pipe 61 and the 3rd heater strip 62 are arranged in the 3rd refrigeration cavity 6.In the present embodiment, needs according to the volatile organic matter condensing temperature, the first semiconductor chilling plate group 3 comprises the semiconductor chilling plate 19 be electrically connected to that fit together more than two and in parallel, the second semiconductor chilling plate group 5 comprise that quantity fits together more than three and in parallel be electrically connected to semiconductor chilling plate 19, the three semiconductor chilling plate groups 7 comprise the semiconductor chilling plate 19 be electrically connected to that fit together more than two and in parallel.Wherein, by the first semiconductor cooling sheet group 3 processed, for the first refrigeration cavity 2, provide refrigeration, by the second semiconductor chilling plate group 5, for the second refrigeration cavity 4, provide refrigeration, by the 3rd semiconductor chilling plate group 7, for the 3rd refrigeration cavity 6, provide refrigeration.
In the present embodiment, the outside of the first refrigeration cavity 2, the second refrigeration cavity 4 and the 3rd refrigeration cavity 6 is enclosed with respectively heat-insulating material.The first multiport valve 10, the second multiport valve 12, the 3rd multiport valve 13 and the 4th multiport valve 14 are various way solenoid valve.The first condenser pipe 21, the second condenser pipe 41 and the 3rd condenser pipe 61 are straight shape, snakelike or spirality winding.
Carrier gas source of the gas 11 and blowback source of the gas 15 are the inert gas that purity is greater than 99.9%.In the present embodiment, carrier gas source of the gas 11 and blowback source of the gas 15 are the helium that purity is greater than 99.9%.Certainly, also can adopt other inert gas.Wherein, the meaning of carrier gas: in vapor-phase chromatography, mobile phase is gas, is called carrier gas.The effect of carrier gas is to enter together chromatographic column with certain flow velocity carrier band gaseous sample or the sample gas after gasification to be separated, again each component after separated being written into to detecting device is detected, finally flow out condenser system emptying or collection, carrier gas has been carrier band effect and substantially do not participate in centrifugation.
Adopt the sampling and analyzing method of atmospheric volatile organic compounds sampling analysis device of the present invention to comprise the following steps:
A. at first start environmental chamber at low temperature 1, make it in refrigerating state, make the first refrigeration cavity 2 and the first condenser pipe 21 reach the low temperature of-40 ℃ to-50 ℃, make the second refrigeration cavity 4 and the second condenser pipe 41 reach the low temperature of-145 ℃ to-155 ℃, make the 3rd refrigeration cavity 6 and the 3rd condenser pipe 61 reach the low temperature of-55 ℃ to-65 ℃;
B. atmospheric volatile organic compounds is after air sampler 8 samplings, control the first multiport valve 10 and the second multiport valve 12, air sampler 8 is communicated with environmental chamber at low temperature 1, the first condenser pipe 21 is communicated with the second condenser pipe 41, atmospheric sample is quantitatively sent in environmental chamber at low temperature 1 by mass flowmeter 9, at first enter the first refrigeration cavity 2 and carry out condensation, the boiling point containing six carbon atom and above volatile organic compounds and moisture in atmospheric sample is higher, at first be condensed in the first condenser pipe 21, change into solid-state; And the lower volatile organic matter of boiling point is mainly containing higher other volatile organic matter components such as formaldehyde, methyl alcohol and methane of content in five carbon atoms and following compound, especially atmosphere, enter in the second condenser pipe 41, be converted into solid-state; And other permanent gases in atmosphere, such as nitrogen, oxygen etc., because boiling point is lower, is not condensed into solid-state, and directly emptying by the 3rd multiport valve 13;
C. treat that sampling reaches aequum, balance is after a period of time, control the first multiport valve 10, control the second multiport valve 12, disconnect the gas flow of mass flowmeter 9 and the first condenser pipe 21, the first condenser pipe 21 is communicated with except water pipe 20 with semipermeable partition, opening pressure valve 40 makes semipermeable partition remove the certain malleation of maintenance in water pipe 20, open the first heater strip 22 in the first refrigeration cavity 2, make the temperature of the first condenser pipe 21 in the first refrigeration cavity 1 be raised to 50 ℃, and control the first multiport valve 10, carrier gas source of the gas 11 is communicated with the first condenser pipe 21; Be heated to 50 ℃ in the first condenser pipe 21, now, water is in liquid state, vapour pressure is very low, and other is condensed in the volatile organic matter component in the first condenser pipe 21, transfers in gas phase after being heated to 50 ℃ of gasifications, and by carrier gas source of the gas 11, it is purged into semipermeable partition and further dewaters except in water pipe 20, then entering the 3rd condenser tube 61, to carry out cryogenic condensation concentrated, and carrier gas is emptying by the 4th multiport valve 14;
D.5-10 minute after, close the second multiport valve 12 and pressure valve 40, open the 3rd heater strip 62 on the 3rd condenser pipe 61, make the 3rd condenser pipe 61 be heated to 50 ℃, now the volatile organic matter in the 3rd condenser pipe 61 all changes gaseous state into, and be written into the second chromatograph 17 by carrier gas source of the gas 11 and detect analysis, complete the detection analysis containing six carbon atom and above volatile organic compounds in atmospheric sample;
E. simultaneously, sampling quantity reach set quantitatively after, control the second multiport valve 12, the off-state that keeps the first condenser pipe 21 and the second condenser pipe 41, open the second heater strip 42 on the second condenser pipe 41, make the temperature increase to 50 ℃ in the second condenser pipe 41, make the solid-state volatile organic matter in the second condenser pipe 41 change gaseous state into, and be written into the first chromatograph 16 by carrier gas source of the gas 11 and detect analysis, complete in atmospheric sample the detection analysis containing five carbon atoms and following volatile organic matter;
F. after completing said process, stop the refrigerating state of environmental chamber at low temperature 1, open the first heater strip 22, the second heater strip 42 and the 3rd heater strip 62, make the first condenser pipe 21, the second condenser pipe 41 and the 3rd condenser pipe 61 temperature be elevated to 300 ℃, control the first multiport valve 10, the second multiport valve 12, the 3rd multiport valve 13 and the 4th multiport valve 14, blowback source of the gas 15 is communicated with the second condenser pipe 41 and the 3rd condenser pipe 61, and be communicated with the first condenser pipe 21, carry out the blowback cleaning, purge gas is emptying by the first multiport valve 10;
G. after the blowback process completes, close the first heater strip 22, the second heater strip 42 and the 3rd heater strip 62, and reopen environmental chamber at low temperature 1 and make it in refrigerating state, the first refrigeration cavity 2, the second refrigeration cavity 4 and the 3rd refrigeration cavity 6 are reached and set temperature, for next time sampling and condensation concentration ready.
From the above-mentioned course of work of atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method, can find out, atmospheric volatile organic compounds sampling analysis device of the present invention, what adopt is semiconductor refrigerating technology, and semiconductor refrigerating technology utilizes the paltie effect refrigeration of semiconductor material, do not need cold-producing medium, directly freeze after energising.But semiconductor refrigerating has the advantages 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.Simultaneously, the stainless-steel tube that the condenser pipe that patent of the present invention adopts is hollow, do not need to fill traditional poriness sorbing material; The refrigeration system of this technology can meet the needs to the volatile organic matter on-line real time monitoring.Therefore apply the atmospheric volatile organic compounds sampling analysis device of the present invention of this Refrigeration Technique, overcome traditional cryogenic condensation device due to the defect that needs liquid nitrogen refrigerating to exist: the liquid nitrogen consumption is large, the refrigeration cost is higher, and the liquid nitrogen field is changed simultaneously, stores difficulty; Simultaneously, the stainless-steel tube thermal desorption speed of hollow is fast, purges easily, makes the system scavenging period short, has shortened the analytical test cycle, can be used for the online automatic detection on the spot of atmospheric volatile organic compounds content.
In addition, atmospheric volatile organic compounds sampling analysis device of the present invention in the course of the work, switch by the first multiport valve 10, the second multiport valve 12, the 3rd multiport valve 13 and the 4th multiport valve 14 is controlled and the setting of the first cold-trap, the second cold-trap and the 3rd cold-trap different temperatures, makes in atmosphere to enter the second chromatograph 17 containing six carbon atom and above volatile organic matter after by the first cold-trap and the 3rd cold-trap and detect analysis.And in atmosphere, remaining volatile organic matter enters the first chromatograph 16 after by the second cold-trap and detects analysis.This shows, atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method can be divided into the volatile organic matter in atmosphere after two classes and enter respectively two chromatographs and detect analysis, and two chromatographs can adopt chromatographic column of different nature and dissimilar detecting device, improve the responsiveness of chromatograph to different volatile organic matters, and improved the detection analysis precision.
Atmospheric volatile organic compounds sampling analysis device of the present invention and sampling and analyzing method combine with the semi-permeable technology of dewatering by the segmentation condensation is concentrated, make in atmosphere containing six carbon atom and above volatile organic matter through semipermeable partition during except water pipe 20, further remove moisture wherein, eliminated the impact of moisture on stratographic analysis, the result that makes it enter the rear detection analysis of the second chromatograph 17 is more accurate.
The above is giving an example of best mode for carrying out the invention, and the part of wherein not addressing in detail is those of ordinary skills' common practise.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. an atmospheric volatile organic compounds sampling analysis device, is characterized in that, comprising:
Environmental chamber at low temperature, described environmental chamber at low temperature is connected with compressor, be provided with the cryotrap device in described environmental chamber at low temperature, described cryotrap device comprises the first cold-trap, the second cold-trap and the 3rd cold-trap, described the first cold-trap comprises the first condenser pipe and the first semiconductor chilling plate group, on described the first condenser pipe, is wound with the first heater strip; Described the second cold-trap comprises the second condenser pipe and the second semiconductor chilling plate group, on described the second condenser pipe, is wound with the second heater strip; Described the 3rd cold-trap comprises the 3rd condenser pipe and the 3rd semiconductor chilling plate group, on described the 3rd condenser pipe, is wound with the 3rd 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, the second end of described the first multiport valve is connected with the carrier gas source of the gas, and the 3rd end of described the first multiport valve is connected to the entrance point of described the first condenser pipe;
The endpiece of described the first condenser pipe is connected to the first end of the second multiport valve, and the second end of described the second multiport valve is connected with the entrance point of described the second condenser pipe, and the 3rd end of described the second multiport valve is connected with the entrance point of described the 3rd condenser pipe;
The endpiece of described the second condenser pipe is connected to the first end of the 3rd multiport valve, and the second end of described the 3rd multiport valve is connected with the blowback source of the gas, and the 3rd end of described the 3rd multiport valve is connected to the first chromatographic detection input end;
The endpiece of described the 3rd condenser pipe is connected to the first end of the 4th multiport valve, and the first end of described the 4th multiport valve is connected with described blowback source of the gas, and the second end of described the 4th multiport valve is connected to the second chromatographic detection input end.
2. atmospheric volatile organic compounds sampling analysis device as claimed in claim 1, is characterized in that: be provided with the first refrigeration cavity, the second refrigeration cavity and the 3rd refrigeration cavity in described environmental chamber at low temperature; Described the first condenser pipe and described the first heater strip are arranged in described the first refrigeration cavity, described the second condenser pipe and described the second heater strip are arranged in described the second refrigeration cavity, and described the 3rd condenser pipe and described the 3rd heater strip are arranged in described the 3rd refrigeration cavity.
3. atmospheric volatile organic compounds sampling analysis device as claimed in claim 1, it is characterized in that: also be connected with semipermeable partition between the second end of described the second multiport valve and the entrance point of described the 3rd condenser pipe except water pipe, described semipermeable partition is provided with drying tube except the water pipe outer cover.
4. atmospheric volatile organic compounds sampling analysis device as claimed in claim 3 is characterized in that: between the entrance point of described semipermeable partition except the endpiece of water pipe and described the 3rd condenser pipe, also be connected with pressure valve.
5. atmospheric volatile organic compounds sampling analysis device as claimed in claim 1, it is characterized in that: described the first semiconductor chilling plate group comprises the semiconductor chilling plate be electrically connected to that fit together more than two and in parallel, described the second semiconductor chilling plate group comprises the semiconductor chilling plate be electrically connected to that fit together more than three and in parallel, and described the 3rd semiconductor chilling plate group comprises the semiconductor chilling plate be electrically connected to that fit together more than two and in parallel.
6. atmospheric volatile organic compounds sampling analysis device as claimed in claim 2 is characterized in that: the outside of described the first refrigeration cavity, described the second refrigeration cavity and described the 3rd refrigeration cavity is enclosed with respectively heat-insulating material.
7. atmospheric volatile organic compounds sampling analysis device as claimed in claim 1, it is characterized in that: described the first condenser pipe, described the second condenser pipe and described the 3rd condenser pipe are the stainless steel condenser pipe.
8. atmospheric volatile organic compounds sampling analysis device as described as claim 1 to 7 any one, 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. adopt the sampling and analyzing method of atmospheric volatile organic compounds sampling analysis device claimed in claim 1, it is characterized in that, comprise the following steps:
A. at first start environmental chamber at low temperature, make it in refrigerating state, make the first refrigeration cavity and the first condenser pipe reach the low temperature of-40 ℃ to-50 ℃, make the second refrigeration cavity and the second condenser pipe reach the low temperature of-145 ℃ to-155 ℃, make the 3rd refrigeration cavity and the 3rd condenser pipe reach the low temperature of-55 ℃ to-65 ℃;
B. atmospheric volatile organic compounds is after the air sampler sampling, control the first multiport valve and the second multiport valve, air sampler is communicated with environmental chamber at low temperature, the first condenser pipe is communicated with the second condenser pipe, atmospheric sample is quantitatively sent in environmental chamber at low temperature by mass flowmeter, at first enter the first refrigeration cavity and carry out condensation, in atmospheric sample containing six carbon atom and above volatile organic compounds and moisture, at first be condensed in the first condenser pipe, change into solid-state; In atmospheric sample containing five carbon atoms and following volatile organic matter enter in the second condenser pipe, be converted into solid-state; And other gas in atmosphere is not condensed into solid-state, and directly emptying by the 3rd multiport valve;
C. treat that sampling reaches aequum, balance is after a period of time, control the first multiport valve, control the second multiport valve, disconnect the gas flow of mass flowmeter and the first condenser pipe, the first condenser pipe is communicated with the 3rd condenser pipe, open the first heater strip in the first refrigeration cavity, make the temperature of the first condenser pipe in the first refrigeration cavity be raised to 50 ℃, and control the first multiport valve, the carrier gas source of the gas is communicated with the first condenser pipe; Be heated to 50 ℃ in the first condenser pipe, now, water is in liquid state, and other is condensed in the volatile organic matter component in the first condenser pipe, after being heated to 50 ℃ of gasifications, transfer in gas phase, and by the carrier gas source of the gas, its purging being entered to the 3rd condenser pipe, to carry out cryogenic condensation concentrated, carrier gas is emptying by the 4th multiport valve;
D.5-10 minute after, close the second multiport valve and pressure valve, open the 3rd heater strip on the 3rd condenser pipe, make the 3rd condenser pipe be heated to 50 ℃, now the volatile organic matter in the 3rd condenser pipe all changes gaseous state into, and be written into the second chromatograph by the carrier gas source of the gas and detect analysis, complete the detection analysis containing six carbon atom and above volatile organic compounds in atmospheric sample;
E. simultaneously, sampling quantity reach set quantitatively after, control the second multiport valve, the off-state that keeps the first condenser pipe and the second condenser pipe, open the second heater strip on the second condenser pipe, make the temperature increase to 50 ℃ in the second condenser pipe, make the solid-state volatile organic matter in the second condenser pipe change gaseous state into, and be written into the first chromatograph by the carrier gas source of the gas and detect analysis, complete in atmospheric sample the detection analysis containing five carbon atoms and following volatile organic matter;
F. after completing said process, stop the refrigerating state of environmental chamber at low temperature, open the first heater strip, the second heater strip and the 3rd heater strip, make the first condenser pipe, the second condenser pipe and the 3rd condenser pipe temperature be elevated to 300 ℃, control the first multiport valve, the second multiport valve, the 3rd multiport valve and the 4th multiport valve, the blowback source of the gas is communicated with the second condenser pipe and the 3rd condenser pipe, and is communicated with the first condenser pipe, carry out the blowback cleaning, purge gas is emptying by the first multiport valve;
G. after the blowback process completes, close the first heater strip, the second heater strip and the 3rd heater strip, and reopen environmental chamber at low temperature and make it in refrigerating state, make the first refrigeration cavity, the second refrigeration cavity and the 3rd refrigeration cavity reach and set temperature, for next time sampling and condensation concentration ready.
10. the sampling and analyzing method of atmospheric volatile organic compounds sampling analysis device as claimed in claim 9, is characterized in that, further comprising the steps of between step b and step c:
B1. control the first multiport valve, control the second multiport valve, disconnect the gas flow of mass flowmeter and the first condenser pipe, the first condenser pipe is communicated with except water pipe with semipermeable partition, the opening pressure valve makes semipermeable partition remove the certain malleation of maintenance in water pipe, opens the first heater strip in the first refrigeration cavity, makes the temperature of the first condenser pipe in the first refrigeration cavity be raised to 50 ℃, and control the first multiport valve, the carrier gas source of the gas is communicated with the first condenser pipe; Be heated to 50 ℃ in the first condenser pipe, now, water is in liquid state, and other is condensed in the volatile organic matter component in the first condenser pipe, after being heated to 50 ℃ of gasifications, transfer in gas phase, and by the carrier gas source of the gas, it is purged into semipermeable partition and further dewaters except in water pipe, carrier gas is emptying by the second multiport valve.
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