CN109632402A - A kind of novel thermal desorption adsorption tube - Google Patents
A kind of novel thermal desorption adsorption tube Download PDFInfo
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- CN109632402A CN109632402A CN201910064551.7A CN201910064551A CN109632402A CN 109632402 A CN109632402 A CN 109632402A CN 201910064551 A CN201910064551 A CN 201910064551A CN 109632402 A CN109632402 A CN 109632402A
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- adsorption tube
- thermal desorption
- novel thermal
- desorption adsorption
- activated carbon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2273—Atmospheric sampling
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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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- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention discloses a kind of novel thermal desorption adsorption tube, filler uses the extensive activated carbon fibre of industrial application, belongs to atmosphere environment supervision technical field.The VOCs monitoring method system surrounding air toxic organic compound measuring method TO-17 that novel thermal desorption adsorption tube of the invention is released according to Environmental Protection Agency is designed; it can effectively acquire Volatile Organohalides, be significantly higher than Tenax TA pipe to the collecting efficiency of VHCs.The present invention can replace Tenax TA pipe as VOCs sample and acquire adsorption tube, for the sampling analysis of VHCs in atmosphere, the concentration level of VHCs in effective Evaluation Environment air.
Description
Technical field
The present invention relates to a kind of novel thermal desorption adsorption tubes, and in particular to a kind of atmosphere VOCs sample acquisition adsorption tube belongs to
In atmosphere environment supervision technical field.
Background technique
Volatile organic matter (VOCs) refers to that fusing point is lower than room temperature and volatility of the boiling point between 50 DEG C~260 DEG C is organic
The general name of compound.VOCs can trigger a series of environment such as global warming, stratospheric ozone depletion and photochemical fog and ask
Topic has become one of the problem of global environmental pollution improvement.Document " Journal of Hazardous
Materials.2017,338:102-123 " point out most of VOCs for example aldehydes, aromatic compound, polycyclic aromatic hydrocarbon, halogenated hydrocarbons,
Alcohols and ketone etc. all have high toxicity and carcinogenicity, can enter human body by approach such as breathing, skin contact and diet
Human health is influenced, it is carcinogenic to cause acute poisoning, slow poisoning even teratogenesis.In addition, the content of VOCs has been considered in atmosphere
It is therefore to be particularly important to the monitoring of VOCs in atmosphere in Evaluation Room with the important parameter of ambient outdoor air quality.Greatly
The concentration of VOCs is generally in μ g/m in gas3Level, such as room air VOCs concentration is in 1-100 μ g/m3, general outdoor environment sky
Gas VOCs concentration is in 1-10 μ g/m3, VOCs complicated component, reactivity with higher, therefore it is required that sampling and pretreatment skill
Art must be simple and fast, efficient, pollution-free.
The common atmosphere VOCs method of sampling mainly has adsorption tube sampling, airbag method and stainless cylinder of steel method.Different adopts
The advantages of quadrat method has its own and limitation have specific applicability.Document " Science of The Total
Environment.2017,599-600:1718-1727 " and document " Analytical Chemistry.2012,84:4126-
4139 " are referred to the advantages of airbag method, stainless cylinder of steel method and adsorption tube sample and disadvantage.Airbag method and stainless cylinder of steel it is owned by France in
Full impingement needs to guarantee that container is pollution-free, and the sample resting period is short, and target substance is adsorbable in airbag or sample can
Inner wall needs specific pre-concentration process when causing the loss of target substance, and analyzing, cumbersome.And adsorption tube samples
It is a kind of active sampling method, adsorption tube is connected with air sampler, and sampler makes surrounding air with the shape of negative pressure by aspiration pump
Formula is by adsorption tube, and polluter is enriched on the filler of adsorption tube in this process, to realize the acquisition of sample.Cause
This, adsorption tube sampling can effectively collect low concentration VOCs, can be effectively enriched with to pollutant, reduce target substance
Loss, big air sample amount can be stored, have the characteristics that high sensitivity, detection limit are low, and it is small to adsorb pipe size, conveniently takes
Band has become one of the common method for collecting and analyzing VOCs in air.
Adsorption tube performance depends primarily on it and loads material, document " Anal Bioanal Chem.2002,373:490-
500 " propose the primary condition that absorption is enriched with and the adsorbent material of thermal desorption should meet: 1) being effectively enriched with target analytes；2)
Target analytes can complete fast desorption.Tenax TA is atmosphere VOCs sample collection analysis, widely used commercialization absorption
One of material, entitled poly- 2, the 6- diphenyl p-phenylene of chemistry, is a kind of Linear Polymer polymer, background value is low, purity
It is high and not easily run off, keep its very widely used.Tenax TA is a kind of hydrophobic adsorbent material, and specific surface area is about
35m2/G, VOCs of the adsorbable boiling spread at 100~400 DEG C, adsorbable number of types of substance, but it is not suitable for height and waves
The Volatile Organohalides such as volatile material, such as vinyl chloride, chloroform, chloroform of the boiling point lower than 80 DEG C.TenaxTA material belongs to
Imported material, price costly, using it are offered as the import adsorption tube of adsorbent material in 700~1600 yuan/root or so,
And Tenax TA pipe price substantially 100~200 yuan/root of domestic supply.When needing to carry out big model to VOCs in surrounding air
When enclosing analysis, needs to buy a large amount of adsorption tube and sampled, higher operating costs.
Volatile Organohalides (VHCs) are a kind of important trace materials in atmosphere VOCs.Document " Environmental Pollution and Control
.2016,38 (10): 72-78 " points out that the VHCs in atmosphere is mainly derived from artificial process, such as chloroform, vinyl chloride are weights
The chemical reagent wanted and the important source material and intermediate of organic synthesis industry；Fluorochlorohydrocarbon class and its substitute are widely used in
The industries such as industry, medical treatment, daily necessities；Trichloro ethylene, tetrachloro-ethylene are mainly used for dry-cleaning industry in China.Document " Chinese environmental
Scientific .2018,38 (1): 14~25 " refer to that VHCs can participate in atmospheric photochemical reaction and destroy ozone layer formation greenhouse effects.
VHCs in human body can long-term accumulated, generate " three cause " effect, as document " Mutation research.2007,636 (1-3):
178-242 " points out that chloroform, carbon tetrachloride etc. have been shown to have carcinogenic and mutagenic effect.It is therefore desirable to Evaluation Environment skies
The concentration level of VHCs in gas reduces human health risk.But VHCs of the Tenax TA pipe to boiling spread lower than 100 DEG C is adopted
Sample efficiency is bad, can not effectively analyze VHCs in the concentration level of environment.It is good therefore, it is necessary to design a kind of adsorption-desorption performance
Novel adsorption pipe, can effectively adsorb that boiling point is lower, VHCs of high volatile, make up the deficiency of Tenax TA pipe, and
With lower use cost.
The problem of in terms of present invention mainly solves adsorption tubes to the absorption property of VHCs and use cost.Adsorption tube of the present invention
Load the more activated carbon fibre (Activated carbon fiber, ACF) of material selection industrial application.ACF has good
Good absorption property: 1) hole is based on micropore, large amount of adsorption；2) acidproof, hot, alkali, 350 DEG C or less are stabilized；3) it adsorbs
Speed is fast, easily reaches adsorption equilibrium；4) adsorption efficiency is unrelated with the concentration of adsorbate, more effective to low concentration adsorbate；5) it solves
Suction rate is fast, regeneration efficiency is high.At present common ACF include: viscose base ACF, polyacrylonitrile-radical ACF, phenolic resin base ACF with
And asphaltic base ACF, compared to other ACF, the cost of material of Viscose-based ACF is low, and manufactured activated carbon fibre specific surface area is larger,
Absorption property is good.The relevant parameter of ACF is as follows in the present invention: viscose activated carbon fibers, and filament diameter 6.5~
13.0denier, 0.04~0.10g/cm of bulk density3, loss on drying 25~30%, ignition point >=500 DEG C, specific surface area >
900m20.60~1.23cm of/g, Kong Rong3/ g, pore-size distribution: 2nm is hereinafter, 65~90%；2~50nm, 10~35%；50nm with
On, 3~8%, pH6.0~7.0, ash content≤5% inhales iodine number (liquid phase) > 800, and material is revived from Jiangsu leads to the limited public affairs of carbon fiber
Department.Using business adsorption tube Tenax TA pipe as control adsorption tube, the relevant parameter of Tenax TA pipe is as follows: 200mg, and 60/
80 mesh, specific surface area 35m2·g-1, adsorption tube material stainless steel, Beijing Hua Yisan spectrometer device Co., Ltd.
Summary of the invention
The problem of in terms of the present invention is based on adsorption tubes to the absorption property of VHCs and use cost, propose a kind of novel heat
Adsorption tube is desorbed.
Technical solution of the present invention:
A kind of novel thermal desorption adsorption tube, including quartz ampoule tube body 1, activation steel wire 2, activated carbon fibre 3 and silica wool
4；Activation steel wire 2, activated carbon fibre 3 and 4 three of silica wool are filled in quartz ampoule tube body 1, during activated carbon fibre 3 is located at
Between, both ends are followed successively by silica wool 4 and steel wire 2.
The quartz ampoule tube body 1 is quartz material, internal diameter 4mm, outer diameter 6mm, wall thickness 1mm；
The amount of fill of the silica wool 4 is 10~20mg, and filling length is 6mm, each 3mm in the both ends of activated carbon fibre 3；
The filling length of the activated carbon fibre 3 is 32mm, amount of fill 90mg；
The activation steel wire 2 is 100 mesh.
The absorption property of ACF adsorption tube of the present invention is assessed: 1) aging of adsorption tube: its process is the High Purity Nitrogen of 20ml/min
Gas (99.99%) constantly purges adsorption tube under 280 DEG C of hot conditions, and aging 2h, the purpose is to remove the sky in ACF adsorption tube
White pollutant reduces the background value of ACF adsorption tube.It is sealed after aging using PTFE seal head, marks the purging direction of adsorption tube,
It is saved under the conditions of 4 DEG C, for use.2) preparation of VOCs gas: 5 μ l 25mg/LVOCs mixed solutions are injected filled with high pure nitrogen
Airbag in, be heat-treated 2h at 60 DEG C, guarantee that the target substance being added volatilizees completely in airbag, restore to room temperature, for use.3)
Analog sample collection process: adsorption tube one end is connected with gas airbag (purging front end) using silicone tube, one end is adopted with atmosphere
Sample device (purging rear end) is connected, and the constant current flow velocity of 0.15ml/min, the acquisition of simulated environment air sample is arranged.4) sample analysis is surveyed
It is fixed: the sample ACF adsorption tube of acquisition is analyzed by thermal desorptioner-gas chromatography-mass spectrum (TD-GC-MS).Tenax TA
Pipe carries out identical operation processing, carries out absorption property comparison with ACF adsorption tube.ACF adsorption tube Performance Evaluation is mainly according to often
The temperature absorption thermal desorption rate of recovery, calculating process are the chromatographic peak face that sample adsorption tube room temperature heat of adsorption desorbs target substance
Long-pending the ratio between the chromatographic peak area that the acquisition of blank adsorption tube is directly added into equal amount target substance.
Beneficial effects of the present invention: the background material of ACF adsorption tube is pyrolyzed the absorption of VHCs without VHCs, ACF adsorption tube
It sucks back yield and is integrally significantly higher than Tenax TA pipe.ACF adsorption tube to trans-1,2-dichloroethylene, 1,1- dichloroethanes, cis- 1,
2- dichloroethylene, chloroform, 1,1,1- trichloroethanes, a bromodichloromethane, chlorodibromomethane, glycol dibromide, 1,
The bromo- 3- chloropropane of 2- bis-, chlordene -1,3- butadiene this ten kinds of VHCs the absorption thermal desorption rate of recovery be respectively 88 ± 8%, 86 ±
8%, 39 ± 3%, 83 ± 8%, 119 ± 12%, 91 ± 10%, 96 ± 12%, 106 ± 13%, 72 ± 4% and 36 ± 1%.
And Tenax TA pipe is followed successively by 3 ± 0%, 11 ± 2%, 12 ± 2%, 26 ± 4%, 36 to the adsorption-desorption rate of recovery of these substances
± 4%, 86 ± 4%, 82 ± 1%, 77 ± 0%, 30 ± 5% and 35 ± 4%.As can be seen that ACF adsorption tube can replace
Tenax TA pipe acquires adsorption tube as VOCs sample, and for the sampling analysis of VHCs in atmosphere, and its preparation process is simple,
Cost is relatively low.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of ACF thermal desorption adsorption tube.
In figure: 1 quartz ampoule tube body；2 activation steel wires；3 activated carbon fibre；4 silica wools.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
A kind of VHCs is selected, chloroform (CAS 67-66-3) passes through atmosphere using ACF adsorption tube, Tenax TA pipe
Sampler contains the VOCs gas of chloroform with the flow velocity acquisition 4L of 0.15L/min, is enriched with to chloroform.By gas
Acquire the ACF sample cell obtained, Tenax TA sample cell is analyzed by TD-GC-MS combined instrument.Measurement result is as follows: ACF
It is 26 ± 4% to the sampling efficiency of chloroform that adsorption tube, which is 83 ± 8%, Tenax TA pipe to the sampling efficiency of chloroform,.
Embodiment 2
A kind of VHCs is selected, chlorodibromomethane (CAS 124-48-1) is passed through using ACF adsorption tube, Tenax TA pipe
Air sampler contains the VOCs gas of chlorodibromomethane with the flow velocity of 0.15L/min acquisition 4L, to chlorodibromomethane into
Row enrichment.The ACF sample cell of gas collecting acquisition, TenaxTA sample cell are analyzed by TD-GC-MS combined instrument.Measurement
As a result as follows: ACF adsorption tube is 96 ± 12%, Tenax TA pipe to chlorodibromomethane to the sampling efficiency of chlorodibromomethane
Sampling efficiency be 82 ± 1%.
Embodiment 3
A kind of VHCs is selected, a bromodichloromethane (CAS 75-27-4) is passed through using ACF adsorption tube, Tenax TA pipe
Air sampler contains the VOCs gas of a bromodichloromethane with the flow velocity of 0.15L/min acquisition 4L, to a bromodichloromethane into
Row enrichment.The ACF sample cell of gas collecting acquisition, Tenax TA sample cell are analyzed by TD-GC-MS combined instrument.It surveys
It is as follows to determine result: ACF adsorption tube is 91 ± 10%, Tenax TA pipe to monobromo dichloromethane to the sampling efficiency of a bromodichloromethane
The sampling efficiency of alkane is 86 ± 4%.
Claims (9)
1. a kind of novel thermal desorption adsorption tube, which is characterized in that the novel thermal desorption adsorption tube includes quartz ampoule tube body
(1), steel wire (2), activated carbon fibre (3) and silica wool (4) are activated；Activate steel wire (2), activated carbon fibre (3) and quartz
Cotton (4) three is filled in quartz ampoule tube body (1), and activated carbon fibre (3) is located at centre, both ends be followed successively by silica wool (4) and
It activates steel wire (2).
2. novel thermal desorption adsorption tube according to claim 1, which is characterized in that the quartz ampoule tube body (1) is stone
English material, internal diameter 4mm, outer diameter 6mm, wall thickness 1mm.
3. novel thermal desorption adsorption tube according to claim 1 or 2, which is characterized in that the filling of the silica wool (4)
Amount is 10~20mg, and filling length is 6mm, each 3mm in both ends of activated carbon fibre (3).
4. novel thermal desorption adsorption tube according to claim 1 or 2, which is characterized in that the activated carbon fibre (3)
Filling length is 32mm, amount of fill 90mg.
5. novel thermal desorption adsorption tube according to claim 3, which is characterized in that activated carbon fibre (3) are filled out
Dress length is 32mm, amount of fill 90mg.
6. according to claim 1, novel thermal desorption adsorption tube described in 2 or 5, which is characterized in that the activation steel wire (2)
For 100 mesh.
7. novel thermal desorption adsorption tube according to claim 3, which is characterized in that the activation steel wire (2) is 100
Mesh.
8. novel thermal desorption adsorption tube according to claim 4, which is characterized in that the activation steel wire (2) is 100
Mesh.
9. one kind is used to adsorb trans-1,2-dichloroethylene, 1,1- dichloroethanes, cis- 1,2- dichloroethylene, chloroform, 1,1,
1- trichloroethanes, a bromodichloromethane, chlorodibromomethane, glycol dibromide, the bromo- 3- chloropropane of 1,2- bis-, chlordene -1,3-
The novel thermal desorption adsorption tube of the halogenated hydrocarbons such as butadiene.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113521957A (en) * | 2021-07-19 | 2021-10-22 | 华电智控（北京）技术有限公司 | Filling method and filling device for VOCs-enriched adsorption tube |
| CN117427458A (en) * | 2023-12-20 | 2024-01-23 | 南京市计量监督检测院 | VOCs waste gas treatment system and method |
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| CN117427458A (en) * | 2023-12-20 | 2024-01-23 | 南京市计量监督检测院 | VOCs waste gas treatment system and method |
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