CN106525999B - Gas gas-chromatography detection method - Google Patents
Gas gas-chromatography detection method Download PDFInfo
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- CN106525999B CN106525999B CN201610853018.5A CN201610853018A CN106525999B CN 106525999 B CN106525999 B CN 106525999B CN 201610853018 A CN201610853018 A CN 201610853018A CN 106525999 B CN106525999 B CN 106525999B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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Abstract
The invention discloses a kind of gas gas-chromatography detection methods, it is detected using multifunctional gas detection system, including baking oven, gas chromatograph, baking oven is connected with baking oven air inlet pipe, baking oven air inlet pipe is protruded into baking oven and is connect at least one airbag air inlet pipe, airbag escape pipe corresponding with airbag air inlet pipe is additionally provided in baking oven, airbag air inlet pipe can be connect with airbag escape pipe with airbag, airbag escape pipe is connected to baking oven escape pipe, baking oven escape pipe stretches out baking oven and branches into the first bronchus and the second bronchus, first bronchus is connect with aspiration pump, second bronchus is connect with gas chromatograph, gas chromatograph is also connect with aspiration pump by third bronchus, the tracheae stretched out from aspiration pump protrudes into exhaust gas cup；Specifically comprise the following steps: 1) to connect airbag and detection system installation；2) baking oven is opened, airbag is heated；3) gas enters gas chromatograph and is detected.Testing result is accurate and reliable, easy to operate, and batch test efficiency is high.
Description
Technical field
The invention belongs to field of gas detection, and in particular to a kind of gas gas-chromatography detection method.
Background technique
Atmosphere organic pollutant is many kinds of, complicated composition, and organic pollutant category contained by different industries, disparity items is not
One, and analysis method cannot be exhaustive with pollutant emission standard, therefore often with volatile organic matter (VOCs), general volatile
The comprehensive evaluation factor as organic pollutant such as organic matter (TVOC) or non-methane total hydrocarbons (NMHC).Usual gas detection
Object is exhaust gas, room air, surrounding air etc..State Ministry of Environmental Protection is " about further strengthening new period environmental monitoring work
Opinion " and " Supreme People's Court, the Supreme People's Procuratorate are about handling environmental pollution criminal case law of application saliva some problem
Explain " indicate monitoring data as basis and the environmental pollution criminal case evidence for formulating Environment Protection Policy and measure respectively
Importance.As it can be seen that guarantee monitoring data accuracy be realize environmental supervision and administration work legalization, quantification, it is scientific and
The top priority of monitoring data " quasi-, fast, complete " target.
Existing frequently-used gas detection method has gas chromatography etc., the target pair in using gas chromatography measurement gas
As Shi Faxian, there is larger range fluctuation or larger exceptional value in the target substance concentration of chronicity monitoring site, such as in gas sample
Methane concentration is higher than total hydrocarbon concentration, and the total hydrocarbon peak peak shape of gas sample is abnormal, hangover, bifurcated or multiple peaks occurs, goes out on void column
The principle of one total hydrocarbon peak contradicts.Under the premise of excluding operating condition and oxygen peak and interfering, when reason mostlys come from sampling not
Particulate filter or mineral wool are installed, power device cross-reference is sampled, does not take and is protected from light measure transport, instrument system is dirty
Dye, calibration curve draw that effect is poor, and Quality Control measure is not complete, and sampling container cleaning effect is bad or saves improper, half volatile and has
Machine object, which is adsorbed on sampling container wall, leads to testing result inaccuracy etc..Major part influence factor therein can be according to the rule of national standard
Model operation or Quality Control measure are eliminated, and sampling container cleanliness integrates the influence of quantitative and result judgement to target compounds only
There has been no efficient and practicable solutions.
Currently, gas to be checked frequently with collection container be aluminum-plastic composite membrane, Devex film, Tedlar (PVF) film,
Teflon (FEP) film, Fluode (PCTFE) film gas sampling bag and Su Ma tank etc., collection container is at high cost, if disposable
It is then at high cost and increase environmental pollution.Therefore, collection container is typically repeated use, and needing to clean before use prevents last time from collecting
Gas residual contamination next time detection.The cleaning method being often used at present is the multiple weight by high pure nitrogen or de- hydrocarbon air
It resets and brings cleaning airbag, but this method purification capacity is weak, cleaning effect is poor and there are limitations, and it is low, dry to be only applicable to concentration
Disturb the few sample airbag cleaning of object.Since waste gas sample is in higher temperatures, humidity and pressure environment, some easily vaporized liquid
State hydro carbons, difficult volatility and the high component of chemical activity are easily collected in airbag with air-flow, when environment temperature reduces suddenly
It is adsorbed on airbag inner wall, conventional cleaning method is difficult to wash the substance being adsorbed on airbag inner wall.
Summary of the invention
The purpose of the present invention is providing in view of the above problems, one kind is easy to use, operates easy, result accurately and reliably gas
Body gas-chromatography detection method.
Technical solution used for the above purpose is: a kind of gas gas-chromatography detection method, use are multi-functional
Gas detecting system is detected, and the multifunctional gas detection system includes baking oven, gas chromatograph, and the baking oven is connected with
Baking oven air inlet pipe, the baking oven air inlet pipe are protruded into baking oven and are connect at least one airbag air inlet pipe, be additionally provided in baking oven and
The corresponding airbag escape pipe of the airbag air inlet pipe, airbag air inlet pipe can removably connect with the airbag escape pipe with airbag
It connects, the airbag escape pipe is connected to baking oven escape pipe, and the baking oven escape pipe stretches out baking oven and branches into the first bronchus and the
Two bronchuses, first bronchus are connect with aspiration pump, and second bronchus is connect with the gas chromatograph, gas phase color
Spectrometer is also connect with aspiration pump by third bronchus, and the tracheae stretched out from aspiration pump protrudes into exhaust gas cup；The baking oven into
Tracheae, airbag escape pipe, baking oven escape pipe, is provided with valve on the first bronchus at airbag air inlet pipe；
Specifically comprise the following steps:
1) baking oven air inlet pipe, airbag air inlet pipe, the valve on airbag escape pipe are closed, by equipped under test gas airbag with
Airbag air inlet pipe and airbag the escape pipe installation of multifunctional gas detection system connect；
2) baking oven is opened, airbag is heated；
3) after heating, airbag escape pipe, the valve on baking oven escape pipe is opened, the valve on the first bronchus is closed
Door allows the gas in airbag to enter gas chromatograph and is detected.
Preferably, the airbag is polyvinyl fluoride airbag, in the step 2) temperature setting of baking oven (1) be 60~
100 DEG C, heating time is 8~10 minutes.Polyvinyl fluoride airbag property is stablized, and is not easy to gaseous contamination to be measured, source is wide.
Preferably, the multifunctional gas detection system further includes gas cylinder, the baking oven air inlet pipe and the gas
Bottle connection.Gas cylinder can be selected as gas source or the other gas sources of selection according to actual needs, gas cylinder is easy to use, easily moves
It is dynamic.
Further, air intake branch is additionally provided in the baking oven, described air intake branch one end is connected to baking oven air inlet pipe,
The other end is connected to baking oven escape pipe.Inert gas can be allowed to pass through from air intake branch after carrying out wasted nickel catalyst or washing bag,
And then baking oven escape pipe, the first bronchus are cleaned, it avoids remaining in gas organic substance influence exhaust gas next time inspection therein
It surveys.
In above-mentioned detection method, the advanced row gas piping before having detected a sample and having carried out next sample detection
Cleaning: opening baking oven air inlet pipe, so that the inert gas of external source connection successively passes through baking oven air inlet pipe, air intake branch, baking oven and goes out
Tracheae, the first bronchus, aspiration pump, finally enter in exhaust gas cup, that is, complete gas piping cleaning.
Preferably, the baking oven air inlet pipe, airbag air inlet pipe, airbag escape pipe, baking oven escape pipe, first gas
The tracheae that pipe, the second bronchus, third bronchus, air intake branch and aspiration pump stretch out is stainless steel material and passes through inertia
Processing, material are easy to get, durable, safety.
In the above-mentioned technical solutions, several airbag air inlet pipe, each airbag air inlet pipe have been arranged in parallel in the baking oven
It is correspondingly arranged on an airbag escape pipe, all airbag escape pipes are connected with baking oven escape pipe again after being arranged in parallel, airbag air inlet
Pipe with being capable of a detachably connected airbag between corresponding airbag escape pipe.One baking oven can connect multiple arranged side by side simultaneously
Airbag, multiple airbags can once be cleaned；When carrying out gas detection, first multiple airbags are put into baking oven simultaneously
It connects together, then different airbags is successively detected by the valve operation on pipeline.
The beneficial effects of the present invention are: the multifunctional gas detection system used is easy to use, operation is easy, by gas
Body heats airbag before entering gas chromatograph detection, and the organic matter of half volatile in gas is avoided to be adhered to airbag
It not can enter gas chromatograph on inner wall and cause the inaccuracy of testing result；The system can also carry out the airbag of recycling
Cleaning before sampling avoids cross contamination caused by airbag is reused.Using the method for the present invention, testing result accurately may be used
It leans on, operation is easy, and can carry out batch detection, saves manpower, improves working efficiency.
Detailed description of the invention
Fig. 1 is multifunctional gas detection system structure used in the present invention.
Specific embodiment
Embodiment one, building multifunctional gas detection system
Building a kind of multifunctional gas detection system as shown in Figure 1, mainly by baking oven 1, gas chromatograph 2, aspiration pump
10, gas cylinder 13 forms, and baking oven air inlet pipe 3 is connect with gas cylinder 13.Gas cylinder can be selected according to actual needs as gas source or choosing
Other gas sources are selected, gas cylinder is easy to use, easily moves.Baking oven 1 is connected with baking oven air inlet pipe 3, and baking oven air inlet pipe 3 protrudes into baking oven
It is connect in 1 with several airbag air inlet pipe 4, airbag escape pipe 5 corresponding with airbag air inlet pipe 4 is additionally provided in baking oven 1, owned
Airbag escape pipe 5 is connected with baking oven escape pipe 6 again after being arranged in parallel, energy between airbag air inlet pipe 4 and corresponding airbag escape pipe 5
Enough detachably connected airbags.Multiple airbags arranged side by side can be connected in one baking oven simultaneously, it once can be to multiple
Airbag is cleaned；When carrying out gas detection, first multiple airbags are put into baking oven and are connected together, then by pipeline
Valve operation different airbags are successively detected.
Baking oven escape pipe 6 stretches out baking oven 1 and branches into the first bronchus 7 and the second bronchus 8, the first bronchus 7 and pumping
10 connection of pump, the second bronchus 8 connect with gas chromatograph 2, gas chromatograph 2 pass through third bronchus 9 also with aspiration pump 10
Connection, the tracheae stretched out from aspiration pump 10 protrude into exhaust gas cup 11.
Air intake branch 12 is additionally provided in baking oven 1,12 one end of air intake branch is connected to baking oven air inlet pipe 3, the other end and baking
Case escape pipe 6 is connected to.Inert gas can be allowed to pass through from air intake branch after carrying out wasted nickel catalyst or washing bag, and then to baking oven
Escape pipe, the first bronchus, the second bronchus, the gas passage in gas chromatograph, third bronchus are cleaned, and are avoided residual
Organic substance influence wasted nickel catalyst next time being left in them.
Baking oven air inlet pipe 3, airbag escape pipe 5, baking oven escape pipe 6, is provided on the first bronchus 7 airbag air inlet pipe 4
Valve.Cleaning airbag, gas detection, the clean different function template in gas passage can be selected according to different needs, using not
The selection of gas passage is realized with the valve on pipeline.Valve in baking oven air inlet pipe 3 is gas flow control valve, can basis
Need adjusting gas flow.
Gas chromatograph 2 is ten logical sampling valve gas chromatographs.Gas chromatograph usually have ten logical sampling valves and six lead into
Two kinds of sample valve, two sampling valves are then needed if it is six-way injection valve, logical then only need one if it is ten.Selection ten lead into
The gas chromatograph of sample valve, the second bronchus need to be only connected to a ten logical sampling valves.
7, second baking oven air inlet pipe 3, airbag air inlet pipe 4, airbag escape pipe 5, baking oven escape pipe 6, the first bronchus gas
The tracheae that pipe 8, third bronchus 9, air intake branch 12 and aspiration pump 10 stretch out is stainless steel material and by inertization,
Material is easy to get, durable, safety.
Embodiment two, gas detection
Gas is detected using the multifunctional gas detection system in embodiment one:
The airbag (for polyvinyl fluoride airbag) 5 for being collected under test gas is taken, test object is non-methane total hydrocarbons, is pressed
It is operated according to following steps:
1) baking oven air inlet pipe 3 is opened, makes the nitrogen in gas cylinder 13 successively by adjusting the valve on each gas piping
By baking oven air inlet pipe 3, air intake branch 12, baking oven escape pipe 6, the first bronchus 7, aspiration pump 10, exhaust gas cup is finally entered
In 11, that is, complete gas piping cleaning.
2) baking oven air inlet pipe 3, airbag air inlet pipe 4, the valve on airbag escape pipe 5 are closed, 5 of under test gas will be equipped with
Airbag is connected with the airbag air inlet pipe 4 of multifunctional gas detection system and the installation of airbag escape pipe 5 respectively.
3) baking oven 1 is opened, temperature setting is 80 DEG C, and (according to polyvinyl fluoride airbag property, temperature setting is 60~100 DEG C equal
Can), heating is carried out 8~10 minutes to airbag.
4) after heating, the airbag escape pipe 5 connected on one of airbag, the valve on baking oven escape pipe 6 are opened,
The valve on the first bronchus 7 is closed, gas chromatograph 2 is opened, so that the gas in airbag enters gas chromatograph 2 and examined
It surveys.
5) after having detected a sample, gas piping is cleaned according to the method in step 1), then according to step
4) detection of next airbag is carried out.
6) step 5) is repeated, until having detected all airbags to be measured.
In this detection, the operation of gas chromatograph and parameter setting reference standard HJ/T38-1999.
Embodiment three, airbag cleaning
Used airbag saves after being cleaned with the multifunctional gas detection system in embodiment one for next time
The acquisition of sample, cleaning method carry out in accordance with the following steps:
Will clean polyvinyl fluoride airbag two nozzles respectively with the airbag air inlet pipe 4 in baking oven, airbag escape pipe 5
Connection reaches 80 DEG C of setting value (according to polyvinyl fluoride airbag property, temperature setting is 60~100 DEG C) to oven temperature,
Then heating 3~10 minutes opens aspiration pump 10 and enters the gas extraction in airbag in exhaust gas cup 11, is filled with into airbag
Nitrogen continues 80 DEG C and heats 3~10 minutes.Then it under the conditions of 80 DEG C, opens gas cylinder 13, adjust the valve on each gas piping
Door, so that nitrogen finally enters exhaust gas cup 11 followed by airbag, baking oven escape pipe 6, the first bronchus 7, aspiration pump 10
In, it maintaining nitrogen purge 3~10 minutes, can be clean by the residuals in used airbag.
For the airbag after cleaning, is inspected by random samples according to the method in embodiment two, target substance or detection is not detected
As a result as cleaning up lower than detection limit.
The gas in airbag is drained and can be saved backup to airbag with aspiration pump 10 after having cleaned.
Claims (3)
1. a kind of gas gas-chromatography detection method, which is characterized in that it is detected using multifunctional gas detection system, it is described
Multifunctional gas detection system includes baking oven (1), gas chromatograph (2), gas cylinder (13), the baking oven (1) be connected with baking oven into
Tracheae (3), the baking oven air inlet pipe (3) connect with the gas cylinder (13), and baking oven air inlet pipe (3) protrudes into baking oven (1) and at least
Piece airbag air inlet pipe (4) connection, baking oven (1) is interior to be additionally provided with airbag escape pipe corresponding with airbag air inlet pipe (4)
(5), airbag air inlet pipe (4) can be detachably connected with airbag with the airbag escape pipe (5), the airbag escape pipe (5)
It is connected to baking oven escape pipe (6), the baking oven escape pipe (6) stretches out baking oven (1) and branches into the first bronchus (7) and second gas
It manages (8), first bronchus (7) connect with aspiration pump (10), second bronchus (8) and the gas chromatograph (2)
Connection, gas chromatograph (2) are also connect with aspiration pump (10) by third bronchus (9), the tracheae stretched out from aspiration pump (10)
It protrudes into exhaust gas cup (11)；The baking oven air inlet pipe (3), airbag air inlet pipe (4), airbag escape pipe (5), baking oven escape pipe
(6), valve is provided on the first bronchus (7)；Air intake branch (12), the air intake branch are additionally provided in baking oven (1)
(12) one end is connected to baking oven air inlet pipe (3), and the other end is connected to baking oven escape pipe (6)；Baking oven (1) is inner be arranged in parallel it is several
A airbag air inlet pipe (4), each airbag air inlet pipe (4) are correspondingly arranged on an airbag escape pipe (5), all airbag escape pipes
(5) it connects again with baking oven escape pipe (6) after being arranged in parallel, it can between airbag air inlet pipe (4) and corresponding airbag escape pipe (5)
A detachably connected airbag；
Specifically comprise the following steps:
1) baking oven air inlet pipe (3), airbag air inlet pipe (4), the valve on airbag escape pipe (5) are closed, it will be equipped under test gas
The airbag air inlet pipe (4) and airbag escape pipe (5) installation of airbag and multifunctional gas detection system connect；
2) baking oven (1) is opened, airbag is heated；
3) after heating, airbag escape pipe (5), the valve on baking oven escape pipe (6) is opened, is closed on the first bronchus (7)
Valve, allow the gas in airbag to enter gas chromatograph (2) and detected；Next sample is carried out having detected a sample
The cleaning of advanced row gas piping before detecting: opening baking oven air inlet pipe (3), so that the inert gas of external source connection is successively by drying
Case air inlet pipe (3), air intake branch (12), baking oven escape pipe (6), the first bronchus (7), aspiration pump (10), finally enter exhaust gas
In cup (11), that is, complete gas piping cleaning.
2. gas gas-chromatography detection method according to claim 1, which is characterized in that the airbag is polyvinyl fluoride gas
Bag, the temperature setting of baking oven (1) is 60~100 DEG C in the step 2), and heating time is 8~10 minutes.
3. gas gas-chromatography detection method according to claim 1 or 2, which is characterized in that the baking oven air inlet pipe
(3), airbag air inlet pipe (4), airbag escape pipe (5), baking oven escape pipe (6), the first bronchus (7), the second bronchus (8),
The tracheae that three bronchuses (9), air intake branch (12) and aspiration pump (10) stretch out is stainless steel material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610853018.5A CN106525999B (en) | 2016-09-27 | 2016-09-27 | Gas gas-chromatography detection method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610853018.5A CN106525999B (en) | 2016-09-27 | 2016-09-27 | Gas gas-chromatography detection method |
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| CN106525999A CN106525999A (en) | 2017-03-22 |
| CN106525999B true CN106525999B (en) | 2019-03-26 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108692887A (en) * | 2018-05-17 | 2018-10-23 | 合肥国轩高科动力能源有限公司 | A kind of device for detecting lithium ion battery airtightness |
| CN108828172A (en) * | 2018-06-21 | 2018-11-16 | 中国计量科学研究院 | The calibration method and device of total organic carbon analyzer |
| CN109655564A (en) * | 2019-01-18 | 2019-04-19 | 武汉市天虹仪表有限责任公司 | A kind of two-way continuous sample introduction device and method |
| JP7349621B2 (en) * | 2019-09-13 | 2023-09-25 | 株式会社テクロム | Sampling bag cleaning method, sampling bag cleaning device, and liquids used in the method and device |
| CN112763635B (en) * | 2019-10-21 | 2022-03-22 | 中昊晨光化工研究院有限公司 | Gas chromatographic column, application and low-boiling-point fluorine-containing compound separation method |
| CN112268288A (en) * | 2020-10-16 | 2021-01-26 | 重庆渝久环保产业有限公司 | Waste gas detection system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103698164B (en) * | 2013-12-31 | 2016-09-07 | 宁波环测实验器材有限公司 | VOC fills gas production system |
| CN204101337U (en) * | 2014-08-15 | 2015-01-14 | 奇鼎科技股份有限公司 | Automatic gas gathers apparatus for temporary storage |
| CN204101524U (en) * | 2014-09-22 | 2015-01-14 | 山西潞安环保能源开发股份有限公司 | A kind of proving installation of simulating coal mine gob injecting CO 2 fire extinguishing |
| CN204255916U (en) * | 2014-11-07 | 2015-04-08 | 中国石油天然气股份有限公司 | Gas chromatograph |
| CN204594943U (en) * | 2015-05-02 | 2015-08-26 | 苏州索泰检测技术服务有限公司 | A kind of VOC pick-up unit for automobile green reclaim |
| CN105675358A (en) * | 2016-01-27 | 2016-06-15 | 上海杰诺质量检测技术有限公司 | VOC (volatile organic compound) sampling system |
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