CN107976343A - The capturing device of freon in a kind of water - Google Patents
The capturing device of freon in a kind of water Download PDFInfo
- Publication number
- CN107976343A CN107976343A CN201711429677.7A CN201711429677A CN107976343A CN 107976343 A CN107976343 A CN 107976343A CN 201711429677 A CN201711429677 A CN 201711429677A CN 107976343 A CN107976343 A CN 107976343A
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- China
- Prior art keywords
- freon
- tube
- capturing device
- trap tube
- water
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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
- G01N1/2294—Sampling soil gases or the like
Abstract
The invention belongs to technical field of measurement and test.Otherness using different packing materials to the physisorption of freon component, by Proper Match, realizes effective trapping to freon component.The capturing device of freon in water of the present invention, it is made of sequentially connected control valve, flowmeter, purifier, emptying device, trap tube, gas emission device and sample conveying tube, the interior subsection filling mass ratio of trap tube (9) is the filler material of TENAX40%~60%, porasil C20%~40% and porapak Q10%~30%；Populated trap tube is under the effect of 20~60mL/min nitrogen, more than 200 DEG C heat treatment more than 12h；Sample purge pond (5) are connected between flowmeter and gas emission device.The device, simple in structure, Applicable temperature scope is wide, easy to operate, it can be achieved that the absorption fully effective to freon component, compared with the prior art in single filler absorption, there is more preferable adsorption effect, be suitable for the trapping of freon in water.
Description
Technical field
The invention belongs to technical field of measurement and test, is related to gas analysis measuring technology, more particularly to Freon gas trapping skill
Art.
Background technology
Freon, be by the general name of artificial synthesized fluorine chloromethane and fluorine chloric ethane, it is most common to have a fluorine trichlorine
Methane (F-11), dichlorodifluoromethane (F-12) and trifluorotrichloroethane (F-113) etc., it is low boiling point, volatile, it is widely used in system
Cooling system, foaming agent, cleaning agent etc..Freon is notable to environmental hazard, can cause ozone layer depletion, aggravates greenhouse effects.
The detection of freon is widely paid close attention in fields such as atmospheric environment science, environmental protections in air and water body.
Since freon content is horizontal for trace even ultra trace in air and water body, to ensure analysis result accurately and reliably, freon
Detection usually require by enrichment obtain the sample of enough contents, can meet instrument test limit requirement.At present, in the world
Generally using the freon in purge and trap device enrichment air and water body, then using gas-chromatography-electron capture detection
(GC-ECD), gas-chromatography-hydrogen flameionization (GC-FID) and the methods of gas chromatography-mass spectrum (GC-MS) method, are examined
Survey.Purge and trap device is made of several parts such as blow device, purifier, capturing device, desorption apparatus, wherein, trapping dress
Put the accuracy that middle freon absorption efficiency seriously affects test result.
For the trap tube packing material of freon, mainly there are the porasil C (porous silica bead C), porapak T (porous
Property polymer microballoon T), porapak Q (porapak Q), TENAX (poly- 2,6- diphenyl p-phenylene resin), carbon
Sieve etc..Trap tube mainly has the different materials such as nylon tube, copper pipe, capillary, stainless steel tube, quartz glass tube, polyfluortetraethylene pipe
Matter.The packing material of different cultivars, different types of trapping column produce trapping temperature, resolution temperature and arresting efficiency different
Influence.
Due to freon complicated components, boiling point is different, is filled out at present using undressed trapping column and one-component
Fill that material capture effect is poor, report is had no specifically for the capturing device of freon component.
The content of the invention
The purpose of the present invention is aim to solve the problem that the problem of freon adsorption effect in the presence of the prior art is poor, there is provided one
Kind is directed to the capturing device of multicomponent freon, improves the arresting efficiency of freon.
The object of the present invention is achieved like this：Using different packing materials to the physisorption of freon component
Otherness, by Proper Match, realizes effective trapping to freon component.
The capturing device of freon in water of the present invention, by sequentially connected control valve, flowmeter, purifier,
Emptying device, trap tube, gas emission device and sample conveying tube composition, it is characterised in that：Subsection filling quality in trap tube 9
Than the filler material for TENAX (40%~60%), porasil C (20%~40%) and porapak Q (10%~30%)；Fill out
The trap tube substituted the bad for the good is under the effect of (20~60) mL/min nitrogen, more than 200 DEG C heat treatment more than 12h；Flowmeter and tail gas row
Put and sample purge pond 5 is connected between device.
The capturing device of freon in water of the present invention, by sequentially connected control valve, flowmeter, purifier,
Emptying device, trap tube, gas emission device and sample conveying tube composition, it is characterised in that：The trap tube for 1/8 inch~
1/4 inch of 316L stainless steel tube, fills length (40~80) cm.
The capturing device of freon in water of the present invention, by sequentially connected control valve, flowmeter, purifier,
Emptying device, trap tube, gas emission device and sample conveying tube composition, it is characterised in that：The pipeline inner wall and valve of flowmeter
Door nickel plating, range (10~100) mL/min.
The capturing device of freon in water of the present invention, by sequentially connected control valve, flowmeter, purifier,
Emptying device, trap tube, gas emission device and sample conveying tube composition, it is characterised in that：Connecting line inner wall and interface plating
Nickel.
The capturing device of freon in water of the present invention, by sequentially connected control valve, flowmeter, purifier,
Emptying device, trap tube, gas emission device and sample conveying tube composition, it is characterised in that：All valves are bipolar stainless
Steel pressure reducing valve or needle valve, independently of one another.
The capturing device of freon in water of the present invention, by sequentially connected control valve, flowmeter, purifier,
Emptying device, trap tube, gas emission device and sample conveying tube composition, it is characterised in that：Purifier is 3A with drier
Molecular sieve or anhydrous calcium chloride.
The capturing device of freon, simple in structure in water of the present invention, and Applicable temperature scope is wide, easy to operate, can
Realize the absorption fully effective to freon component, compared with the prior art in single filler absorption, there is preferably absorption
Effect, is suitable for the trapping of freon in water.
Brief description of the drawings
Freon capturing device structure diagram in Fig. 1 water
Embodiment
Technical scheme is described further below by way of specific embodiment.But not as to protection domain
Limitation.
Embodiment 1
Trap tube is 1/4 inch of 316L stainless steel tube, fill length 40cm, packing material according to TENAX60%,
The mass ratio of porasil C20% and porapak Q20% subsection filling in order, populated trap tube is in 30mL/min nitrogen
Under gas effect, 220 DEG C of conditions are heat-treated 12h；
Scavenging conduit, as purging tube chamber, is tightly connected, maximum using pyrex using polytetrafluoroethylene sealing gasket
Pressure-resistant is 1MPa；
Purifier is filling anhydrous calcium chloride in U-shaped glass drying tube；
Flow is calculated as gas electronic flowmeter, 0~100mL/min；
Temperature range be respectively semiconductor refrigerating instrument (- 32 DEG C of lowest refrigerating temperature) and electric heater unit (4 DEG C/s of heating rate,
300 DEG C of maximum temperature)；
Gas chromatograph Agilent 7890A, chromatographic column：GS-GASPRO(60m×0.32mm×0.25μm).
Gas chromatographic detection condition such as embodiment 1.
In a kind of water freon capturing device structure as shown in Figure 1, by high pure nitrogen 1, pressure reducing valve 2, needle valve A3, stream
Gauge 4, sample purge pond 5, purifier 6, threeway A7, air bleeding valve A8, trap tube 9, warm bath 10, sample conveying tube 11, threeway
B12, air bleeding valve B13, needle valve B14, gas chromatograph 15 form, and each component links in order successively, purifier 6 and threeway
The a positions of A7 are connected, and air bleeding valve A8 is connected with the b positions of threeway A7, and 9 one end of trap tube is connected with the c positions of threeway A7, and trap tube 9 is another
One end is connected with a positions of threeway B12, and trap tube 9 is placed in warm bath 10.
Pipeline purging is carried out with high pure nitrogen first before trapping, closes air bleeding valve A8, needle valve B14, opens carrier gas system
With the every other valve of pipeline, flowmeter 4 is fed to through pressure reducing valve 2, needle valve A3 at high pure nitrogen 1, into sample purge
Pond 5, it is 40mL/min to control gas flow, and trap tube 9 is reached through threeway A7 after purified device 6, by sample conveying tube 11,
Threeway B12, air bleeding valve B13 are discharged, and whole purge continues 3min, close pressure reducing valve 2, needle valve A3 completes pipeline purging.
Trap tube 9 is placed in the semiconductor refrigerating instrument (warm bath 10) being used as, controls and absorb temperature for -30 DEG C.Sample is put
After entering sample purge pond, pressure reducing valve 2, needle valve A3 are opened, high pure nitrogen 1 is fed to flowmeter 4 through pressure reducing valve 2, needle valve A3,
Into sample purge pond 5, it is 40mL/min to control gas flow, and trap tube 9, control are reached through threeway A7 after purified device 6
It is -30 DEG C, time 10min to absorb temperature, is discharged by sample conveying tube 11, threeway B12, air bleeding valve B13, waits to be completely exhausted out
After continue to purge 2min, close pressure reducing valve 3, needle valve A3, and air bleeding valve B13.
Freon thermal desorption：Trap tube 9 is placed in the electric heater unit of warm bath 10, and it is 160 DEG C to control desorption temperature, parsing
Time 3min.Pressure reducing valve 2, needle valve A3, needle valve B14 are opened, high pure nitrogen 1 is fed through pressure reducing valve 2, needle valve A3 threeways 7
To flowmeter 4, into sample purge pond 5, it is 40mL/min to control gas flow, reaches and catches through threeway A7 after purified device 6
Collector 9, enters gas chromatograph 15 by sample conveying tube 11, threeway B12, needle valve B14.
Using 1 × 10-12Freon solution carries out add-back yield experiment to sample in mol/mol methanol, and the rate of recovery is
98.3%, it was demonstrated that adsorption effect is good.
Embodiment 2
Trap tube 9 is 1/8 inch of 316L stainless steel tube, fill length 50cm, packing material according to TENAX45%,
The mass ratio of porasil C25% and porapak Q30% subsection filling in order.Populated trap tube is in 40mL/min
Under nitrogen effect, 200 DEG C of conditions are heat-treated 12h.Pipeline purging, freon cold trapping, freon are carried out according to 1 flow of embodiment
Thermal desorption and detection, using 1 × 10-12Freon solution carries out add-back yield experiment, the rate of recovery to sample in mol/mol methanol
For 96.7%, it was demonstrated that adsorption effect is good.
Embodiment 3
Trap tube 9 is 1/4 inch of 316L stainless steel tube, fill length 40cm, packing material according to TENAX50%,
The ratio of porasil C40% and porapak Q10% subsection filling in order.Populated trap tube is in 40mL/min nitrogen
Under effect, 200 DEG C of conditions are heat-treated 12h.Pipeline purging, freon cold trapping, freon pyrolysis are carried out according to 1 flow of embodiment
Inhale and detect, using 1 × 10-12Freon solution carries out add-back yield experiment to sample in mol/mol methanol, and the rate of recovery is
100.3%, it was demonstrated that adsorption effect is good.
Embodiment 4
Trap tube 9 is 1/8 inch of 316L stainless steel tube, fill length 80cm, packing material according to TENAX40%,
The ratio of porasil C32% and porapak Q28% subsection filling in order.Populated trap tube is in 40mL/min nitrogen
Under effect, 200 DEG C of conditions are heat-treated 13h.Pipeline purging, freon cold trapping, freon pyrolysis are carried out according to 1 flow of embodiment
Inhale and detect, using 1 × 10-12Freon solution carries out add-back yield experiment to sample in mol/mol methanol, and the rate of recovery is
98.1%, it was demonstrated that adsorption effect is good..
Comparative example
Trap tube 9 is 1/8 inch of 316L stainless steel tube, fills length 80cm, packing material porasil C100% fillings.
For populated trap tube under the effect of 40mL/min nitrogen, 200 DEG C of conditions are heat-treated 12h.Pipeline is carried out according to 1 flow of embodiment
Purging, freon cold trapping, freon thermal desorption and detection, using 1 × 10-12Freon solution is to sample in mol/mol methanol
Add-back yield experiment is carried out, the rate of recovery 46.2%, adsorption effect is worse than multi-component filler..
Claims (6)
1. the capturing device of freon in a kind of water, by sequentially connected control valve, flowmeter, purifier, emptying device,
Trap tube, gas emission device and sample conveying tube composition, it is characterised in that：The interior subsection filling mass ratio of trap tube (9) is
TENAX：40%~60%, porasil C：20%~40% and porapak Q：10%~30% filler material；
Populated trap tube is under the effect of 20mL/min~60mL/min nitrogen, more than 200 DEG C heat treatment more than 12h；Flow
Sample purge pond (5) are connected between meter and gas emission device.
2. the capturing device of freon in water according to claim 1, it is characterised in that：The trap tube (12) is 1/8
Inch~1/4 inch of 316L stainless steel tube, filling length 40cm~80cm.
3. the capturing device of freon in the water according to 1 or 2 any one of claim, it is characterised in that：Flowmeter
Pipeline inner wall and valve nickel plating, range 10mL/min~100mL/min.
4. the capturing device of freon in the water according to 1 or 2 any one of claim, it is characterised in that：Connecting line
Inner wall and interface nickel plating.
5. the capturing device of freon in the water according to 1 or 2 any one of claim, it is characterised in that：All valves
It is bipolar stainless steel pressure reducing valve or needle valve, independently of one another.
6. the capturing device of freon in the water according to 1 or 2 any one of claim, it is characterised in that：Purifier
It is 3A molecular sieves or anhydrous calcium chloride with drier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711429677.7A CN107976343A (en) | 2017-12-26 | 2017-12-26 | The capturing device of freon in a kind of water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711429677.7A CN107976343A (en) | 2017-12-26 | 2017-12-26 | The capturing device of freon in a kind of water |
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| Publication Number | Publication Date |
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| CN107976343A true CN107976343A (en) | 2018-05-01 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201711429677.7A Pending CN107976343A (en) | 2017-12-26 | 2017-12-26 | The capturing device of freon in a kind of water |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110879281A (en) * | 2018-09-05 | 2020-03-13 | 中国科学院地理科学与资源研究所 | Method for determining age of underground water |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102466636A (en) * | 2010-11-09 | 2012-05-23 | 国家海洋局第一海洋研究所 | Device for detecting marine volatile sulfur compounds with ultraviolet fluorescence method and manufacture method of device |
| CN102650623A (en) * | 2011-02-28 | 2012-08-29 | 国家海洋局第一海洋研究所 | Device for detection of low-concentration Freon in seawater and production method thereof |
-
2017
- 2017-12-26 CN CN201711429677.7A patent/CN107976343A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102466636A (en) * | 2010-11-09 | 2012-05-23 | 国家海洋局第一海洋研究所 | Device for detecting marine volatile sulfur compounds with ultraviolet fluorescence method and manufacture method of device |
| CN102650623A (en) * | 2011-02-28 | 2012-08-29 | 国家海洋局第一海洋研究所 | Device for detection of low-concentration Freon in seawater and production method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张栋 等: "海水中氟利昂检测技术及示踪研究进展", 《海洋环境科学》 * |
| 张栋: "大气和水体中痕量氟利昂检测方法的研究", 《中国优秀硕士学位论文全文数据库（电子期刊）工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110879281A (en) * | 2018-09-05 | 2020-03-13 | 中国科学院地理科学与资源研究所 | Method for determining age of underground water |
| CN110879281B (en) * | 2018-09-05 | 2024-02-13 | 中国科学院地理科学与资源研究所 | Method for determining age of underground water |
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Application publication date: 20180501 |