CN201965043U - Sampling tube and sampling enriching and thermal desorbing device for atmospheric trace volatile organic compounds - Google Patents

Sampling tube and sampling enriching and thermal desorbing device for atmospheric trace volatile organic compounds Download PDF

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Publication number
CN201965043U
CN201965043U CN2010205808801U CN201020580880U CN201965043U CN 201965043 U CN201965043 U CN 201965043U CN 2010205808801 U CN2010205808801 U CN 2010205808801U CN 201020580880 U CN201020580880 U CN 201020580880U CN 201965043 U CN201965043 U CN 201965043U
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China
Prior art keywords
sampling pipe
sampling
liang
interface
way valve
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Expired - Lifetime
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CN2010205808801U
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关亚风
彭虹
沈铮
吴大朋
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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Abstract

The utility model relates to the analysis of gases, in particular to a sampling tube and a sampling, enriching and thermal desorbing device for atmospheric trace volatile organic compounds; the sampling tube is a glass tube or a quartz tube which is internally and sequentially filled with carbon molecule sieves TDX-01, graphitized carbon black STH-2 and Tenax-TA. The utility model uses three different adsorbing agents as a mixed adsorbing agent which is suitable for both polar components and nonpolar components and can realize the overall enrichment on a sample in a wide boiling range. A first-stage thermal desorption instrument of the utility model is directly connected with a sampling opening of a gas chromatograph on line; and the sample directly enters the chromatograph by primary thermal desorption, so that a secondary freezing focusing device is not needed, thereby reducing the analysis cost and increasing the detection sensitivity.

Description

Sampling pipe and Atmospheric Trace volatile organic matter sampling-enrichment-thermal analysis apparatus
Technical field
The utility model relates to the analysis of gas, specifically is meant a kind of sampling pipe and Atmospheric Trace volatile organic matter sampling-enrichment-thermal analysis apparatus.
Background technology
(Volatile Organic Compounds is the important pollutant of a class in the atmosphere VOCs) to volatile organic matter, and ecologic environment system and human health are had serious harm.VOCs illumination down easily with atmosphere in the OH free radical reaction and oxidative degradation through a series of atmospheric photochemical reactions generation photo-chemical smogs, causes serious secondary pollution, be one of key precursor thing of atmosphere combined pollution.VOCs easily enters human body by respiratory tract, alimentary canal and skin and produces harm, and long term exposure has three to cause effect in VOCs to human body, also is the one of the main reasons that produces the sick Building syndrome.At present countries in the world have all increased VOCs in monitoring project because VOCs has source, kind and concentration range very widely, set up a kind of blanket method to its carry out fast, high-sensitivity analysis and detection, significant.
One of gordian technique that detects volatile organic matter in the air is the pretreatment technology of air sample, wherein absorption concentrates/thermal desorption technology acquisition widespread use, and the EPA of American National Environmental Protection Agency ambient air standard TO-17, China's national standard " IAQ (indoor air quality) standard " (GB/T18883-2002) are clearly stipulated to adopt " pyrolysis is analysed " method to detect volatile organic matter in the air.Standard method commonly used can only detect the volatile organic matter of particular polarity in the atmosphere and boiling spread, is difficult to realize the comprehensive enrichment to extensive characteristic range sample.Usually because pyrolysis is analysed is a slow process, cause thermal desorption component peaks broadening, sampling volume big, be difficult to be complementary with capillary chromatographic column, need cold-trap to the freezing again focusing of thermal desorption component or carry out secondary concentration, increased the complicacy of device.
The utility model content
The purpose of this utility model is to provide a kind of sampling pipe and the application in the analysis of trace volatile organic matter in atmosphere, by using mixed adsorbent and one-level pyrolysis to analyse, with the volatile organic matter of opposed polarity and different boiling scope in the gas chromatograph coupling assay determination simultaneously air.
For achieving the above object, device of the present utility model is:
A kind of sampling pipe, described sampling pipe are filled with glass tube or the quartz ampoule of carbonaceous molecular sieve TDX-01, Graphon STH-2 and Tenax-TA for inner order;
In the described sampling pipe, filler is by mass ratio: carbonaceous molecular sieve TDX-01: Graphon STH-2: Tenax-TA=(1.8-2.5): (4.6-6.3): (0.7-1.1).
Described sampling pipe is the application in the analysis of trace volatile organic matter in atmosphere, carries out the sampling-enrichment-pyrolysis of trace volatile organic matter in the atmosphere and analyses;
Atmospheric Trace volatile organic matter sampling-enrichment-thermal analysis apparatus: be that adsorbent is filled in the sampling pipe with carbonaceous molecular sieve TDX-01, Graphon STH-2 and Tenax-TA respectively successively from left to right; The right-hand member of atmosphere from sampling pipe fed, and the trace volatile organic matter in the atmosphere is adsorbed in the sampling pipe; Place pyrolysis to analyse instrument sampling pipe and carry out a pyrolysis and analyse, volatile organic matter directly enters gas chromatograph with carrier gas and carries out compartment analysis.
Pyrolysis is analysed instrument and is analysed instrument for the one-level pyrolysis, and two two position four-way valves of being analysed stove and two ends series connection by pyrolysis constitute;
The sampling pipe pyrolysis of packing into is analysed in the stove, one end of sampling pipe links to each other with an interface of second liang of position four-way valve by second connecting line, second interface of second liang of position four-way valve links to each other by interface of first connecting line and first liang of position four-way valve, and second interface of first liang of position four-way valve connects sample gas;
The other end of sampling pipe links to each other with an interface of the 3rd liang of position four-way valve by the 3rd connecting line, and second interface of the 3rd liang of position four-way valve is carried gas;
The 3rd interface of second liang of position four-way valve links to each other the detecting device in another termination gas chromatograph of capillary chromatographic column by the 4th connecting line with capillary chromatographic column one end in the gas chromatograph.
Sampling pipe carries out blowback by carrier gas before heating is resolved, air and moisture in the sampling pipe are discharged with carrier gas.
Described one-level thermal analysis apparatus is in heating resolving, and sampling pipe places pyrolysis to analyse in the instrument, the obstructed over-sampling pipe of carrier gas, after the pyrolysis eutectoid temperature reaches 280 ℃~310 ℃, switch two position four-way valves, make carrier gas blowback sampling pipe, volatile organic matter enters gas chromatograph with carrier gas.
Described one-level thermal analysis apparatus is connected with the gas chromatograph injection port is online, directly enters gas chromatograph after volatile organic matter is analysed by a pyrolysis and carries out compartment analysis.
The utility model is compared with existing atmosphere VOCs sampling-enrichment-thermal analysis apparatus, and following advantage is arranged:
1. the utility model adopts the filler of three sections heterogeneitys and structure, comprise carbonaceous molecular sieve, Graphon and organic porous polymer polymer absorbant, enrichment polarity and nonpolar volatile organic matter are applied widely simultaneously, guarantee that sample collecting is complete.
2. the one-level thermal analysis apparatus that adopts of the utility model is connected with gas chromatograph is online, and directly entering gas chromatograph after volatile organic matter is analysed by a pyrolysis carries out compartment analysis, has improved the sensitivity of sample analysis.
3. device described in the utility model can make capillary chromatographic column keep composing the resolution characteristic at peak under the condition of no cold-trap to freezing focusing of thermal desorption component and secondary parsing, and especially the light constituent to low boiling, high volatility can not cause the peak broadening.
Description of drawings
Fig. 1 is one-level thermal analysis apparatus of the present utility model and gas chromatograph on-line coupling figure.1,3,7 is first, second, third liang of position four-way valve; 2,4,6,9 is first, second, third, fourth connecting line; 8 analyse stove for pyrolysis, in sampling pipe 5 is housed; 10 is capillary chromatographic column; 11 is detecting device; 12 is gas chromatograph; 17 is sample gas; 18 are carrier gas.
Fig. 2 is the sampling pipe synoptic diagram.13 is carbonaceous molecular sieve TDX-01, and 14 is Graphon STH-2, and 15 is Tenax-TA, and 16 is glass or quartz fibre.
Fig. 3 is the spectrogram that C2 among the utility model embodiment 3~C7 hydrocarbon standard specimen is analyzed.
Embodiment
Embodiment 1
Preparation to sampling pipe described in the utility model is described.
(1) filling of adsorbent: 49mg TDX-01,118mg STH-2,22mg Tenax-TA are loaded in proper order in the quartz ampoule of 2mm I.D. * 4mm O.D. * 15cm, separate with a small amount of glass fibre between the filler.As shown in Figure 2.
(2) sampling pipe is aging: sampling pipe heating that will be populated under the 50mL/min high pure nitrogen is protected, is warming up to 320 ℃ with 10 ℃/min speed from 40 ℃, and kept 30 minutes.
Embodiment 2
On-line coupling to device described in the utility model and gas chromatograph is described.
As shown in Figure 1, the sampling pipe pyrolysis of packing into is analysed in the stove, one end of sampling pipe links to each other with an interface of second liang of position four-way valve by second connecting line, second interface of second liang of position four-way valve links to each other by interface of first connecting line and first liang of position four-way valve, and second interface of first liang of position four-way valve connects sample gas;
The other end of sampling pipe links to each other with an interface of the 3rd liang of position four-way valve by the 3rd connecting line, and second interface of the 3rd liang of position four-way valve is carried gas;
The 3rd interface of second liang of position four-way valve links to each other the detecting device in another termination gas chromatograph of capillary chromatographic column by the 4th connecting line with capillary chromatographic column one end in the gas chromatograph.
During collected specimens, valve 1, valve 3 and valve 7 are positioned at position shown in Figure 1, and sample gas enters sampling pipe 5 through connecting line 2,4, volatile matter in the sample gas is adsorbed the agent enrichment, all the other components are through connecting line 6 emptying, and the sampling flow velocity is 80mL/min, and sampling volume is 250mL.After sampling is finished, transfer valve 1 and valve 7, carrier gas is carried out blowback to sampling pipe 5, and the moisture in the sampling pipe 5 is discharged with carrier gas.Transfer valve 7, carrier gas this moment is without sampling pipe 5, heat hot is resolved stove 8, when pyrolysis is analysed after furnace temperature reaches 280 ℃~310 ℃, transfer valve 3 and valve 7, the thermal desorption component enters gas chromatograph 12 with the carrier gas by connecting line 6,4,9,, obtains detecting on detecting device 11 through temperature programme after capillary chromatographic column 10 separates.
Embodiment 3
Select the representation compound C2~C7 hydrocarbon samples of volatile organic matter in the air, concentration is 20ppb (v/v), measures according to the step of embodiment 2, and analysis result is seen Fig. 3.
The alundum (Al PLOT post of 30m * 0.53mm i.d.; Split sampling not; Nitrogen is done carrier gas, constant voltage 30kPa; 33 ℃ of initial column temperatures keep 2min, are raised to 100 ℃ with the speed of 20 ℃/min, keep 7min, and the speed with 20 ℃/min is raised to 180 ℃ again, keeps 10min.150 ℃ of injector temperatures; 250 ℃ of fid detector temperature.
Chromatographic peak 1~17 is followed successively by among the figure: ethane, ethene, propane, propylene, isobutane, normal butane, acetylene, anti--the 2-butylene, 1-butylene, suitable-the 2-butylene, cyclopentane, n-pentane, 1,3-butadiene, anti--the 2-amylene, cyclohexane, 3-methylpentane, normal heptane.Adopt sampling pipe of the present utility model, enrichment when having realized wide boiling spread and opposed polarity sample is analysed directly by a pyrolysis and to be analyzed, and has reduced analysis cost, has improved detection sensitivity.

Claims (4)

1. sampling pipe is characterized in that: described sampling pipe is filled with glass tube or the quartz ampoule of carbonaceous molecular sieve TDX-01, Graphon STH-2 and Tenax-TA for inner order.
2. sampling pipe as claimed in claim 1 is characterized in that: in the described sampling pipe, filler is by mass ratio: carbonaceous molecular sieve TDX-01: Graphon STH-2: Tenax-TA=(1.8-2.5): (4.6-6.3): (0.7-1.1).
3. Atmospheric Trace volatile organic matter sampling-enrichment-thermal analysis apparatus is characterized in that:
Be that adsorbent is filled in the sampling pipe with carbonaceous molecular sieve TDX-01, Graphon STH-2 and Tenax-TA respectively successively from left to right.
4. device as claimed in claim 3 is characterized in that: pyrolysis is analysed instrument and is analysed instrument for the one-level pyrolysis, and two two position four-way valves of being analysed stove and two ends series connection by pyrolysis constitute;
Sampling pipe (5) pyrolysis of packing into is analysed in the stove (8), one end of sampling pipe (5) links to each other with an interface of second liang of position four-way valve (3) by second connecting line (4), second interface of second liang of position four-way valve links to each other by (1) interface of first connecting line (2) and first liang of position four-way valve, and second interface of first liang of position four-way valve (1) connects sample gas (17);
The other end of sampling pipe (5) links to each other with an interface of the 3rd liang of position four-way valve (7) by the 3rd connecting line (6), and second interface of the 3rd liang of position four-way valve (7) is carried gas (18);
The 3rd interface of second liang of position four-way valve links to each other the detecting device (11) in another termination gas chromatograph (12) of capillary chromatographic column (10) by the 4th connecting line (9) with capillary chromatographic column (10) one ends in the gas chromatograph (12).
CN2010205808801U 2010-10-27 2010-10-27 Sampling tube and sampling enriching and thermal desorbing device for atmospheric trace volatile organic compounds Expired - Lifetime CN201965043U (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103018376A (en) * 2012-11-27 2013-04-03 张勇 Gas sampling device
CN103212250A (en) * 2013-04-24 2013-07-24 清华大学 Combined type helium gas filtering sampling device for gas cooled reactor and installation method of device
CN103234778A (en) * 2013-04-19 2013-08-07 中国地质科学院水文地质环境地质研究所 Device for enriching semi-volatile organic compounds in underground water
CN105651910A (en) * 2014-12-03 2016-06-08 中国科学院大连化学物理研究所 Enrichment-thermal desorption-chromatography separating unit
CN106568876A (en) * 2016-11-16 2017-04-19 上海化工研究院 Multistage through-flow adsorption type sampling apparatus for GC-MS (Gas Chromatography-Mass Spectrometer)-headspace analysis
CN109030661A (en) * 2018-09-10 2018-12-18 广东金发科技有限公司 A kind of polycarbonate volatile matter test method
CN109870341A (en) * 2017-12-01 2019-06-11 中国科学院大连化学物理研究所 Volatile organic matter original position cold-trap enrichment-Thermal desorption sample pretreatment device
CN111983103A (en) * 2020-09-01 2020-11-24 中国科学院华南植物园 Volatile substance real-time collection and online analysis device

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103018376A (en) * 2012-11-27 2013-04-03 张勇 Gas sampling device
CN103234778A (en) * 2013-04-19 2013-08-07 中国地质科学院水文地质环境地质研究所 Device for enriching semi-volatile organic compounds in underground water
CN103234778B (en) * 2013-04-19 2014-12-03 中国地质科学院水文地质环境地质研究所 Device for enriching semi-volatile organic compounds in underground water
CN103212250A (en) * 2013-04-24 2013-07-24 清华大学 Combined type helium gas filtering sampling device for gas cooled reactor and installation method of device
CN103212250B (en) * 2013-04-24 2015-02-18 清华大学 Combined type helium gas filtering sampling device for gas cooled reactor and installation method of device
CN105651910A (en) * 2014-12-03 2016-06-08 中国科学院大连化学物理研究所 Enrichment-thermal desorption-chromatography separating unit
CN106568876A (en) * 2016-11-16 2017-04-19 上海化工研究院 Multistage through-flow adsorption type sampling apparatus for GC-MS (Gas Chromatography-Mass Spectrometer)-headspace analysis
CN109870341A (en) * 2017-12-01 2019-06-11 中国科学院大连化学物理研究所 Volatile organic matter original position cold-trap enrichment-Thermal desorption sample pretreatment device
CN109030661A (en) * 2018-09-10 2018-12-18 广东金发科技有限公司 A kind of polycarbonate volatile matter test method
CN111983103A (en) * 2020-09-01 2020-11-24 中国科学院华南植物园 Volatile substance real-time collection and online analysis device

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