CN109141987A - The device and method for extracting volatile materials in water - Google Patents
The device and method for extracting volatile materials in water Download PDFInfo
- Publication number
- CN109141987A CN109141987A CN201811066772.XA CN201811066772A CN109141987A CN 109141987 A CN109141987 A CN 109141987A CN 201811066772 A CN201811066772 A CN 201811066772A CN 109141987 A CN109141987 A CN 109141987A
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- Prior art keywords
- helium
- volatile materials
- water sample
- water
- trap
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Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
Abstract
The device and method of volatile materials in a kind of extraction water, the device includes aerating system, condensing reflux system and trapping cold-trap system, the aerating system, the condensing reflux system and the trapping cold-trap system are in turn connected to form access, the aerating system is for being passed through helium in the water sample containing volatile materials, the property of will volatilize substance is from water phase stripping to gas phase, the condensing reflux system is used to for the vapor come out with helium together stripping being condensed back in the water sample, the volatile materials come out by stripping then enters the trapping cold-trap system with helium, the nuclei of condensation are provided in the trapping cold-trap system, the volatile materials come out for collecting capture by stripping.Volatile materials stripping in water sample can effectively be come out and pass through trapping cold-trap by the present invention collects these volatile materials.It can use the risk of toxicity for the volatile materials that the present invention effectively assesses in water sample.
Description
Technical field
The present invention relates to water treatment field, specifically a kind of device and method for extracting volatile materials in water.
Background technique
There are a variety of volatile materials in industrial wastewater, sanitary sewage.Meanwhile in order to ensure drinking water water supply security, work
Industry discharge of wastewater safety and reduction reclaimed water reuse risk, during water process, commonly using oxidation/disinfection etc.
Reason method.Some toxic volatile materials are generated however, not can avoid during processing.Currently, for assessing water sample poison
Property, the sample-pretreating method taken can not be collected into volatile materials.For example, Solid Phase Extraction is enrichment water sample and its warp
The common pre-treating method of product is generated after the processing such as peroxidating/disinfection, however, in the process by solid phase extraction concentration sample
In, nitrogen, which is blown, can lose most of volatile product (haloform etc.), cause Toxicity of Water Samples risk assessment relatively low.
In order to assess the toxicity of volatile materials in water sample, drinking water, the safety of recycled water after processing are ensured, and
The risk of toxicity for reducing industrial wastewater needs device and method appropriate and effectively collects volatile materials in water sample, with
Just assessment is made to its risk of toxicity.
Summary of the invention
It is a primary object of the present invention to overcome the deficiencies of the prior art and provide a kind of dress for extracting volatile materials in water
It sets and method.
To achieve the above object, the invention adopts the following technical scheme:
The device of volatile materials in a kind of extraction water, including aerating system, it is condensed back system and trapping cold-trap system,
The aerating system, the condensing reflux system and the trapping cold-trap system are in turn connected to form access, the aerating system
For being passed through helium in the water sample containing volatile materials, the property of will volatilize substance is described to be condensed back to from water phase stripping to gas phase
Streaming system is used to for the vapor come out with helium together stripping being condensed back in the water sample, the volatility come out by stripping
Substance then enters the trapping cold-trap system with helium, is provided with the nuclei of condensation in the trapping cold-trap system, for collecting capture
The volatile materials come out by stripping.
Preferably, the aerating system includes the heating device for heating the water sample.
Preferably, the aerating system includes the agitating device for stirring the water sample.
Preferably, the agitating device is constant temperature blender with magnetic force.
Preferably, the aerating system includes the three-necked bottle for holding water sample, wherein a neck is for being passed through helium, it is another
Neck is for being connected to the condensing reflux system, and third neck is for being arranged temperature sensor.
Preferably, the aerating system includes the flowmeter for monitoring the charge flow rate of helium.
Preferably, the helium gas flow of the aerating system input is controlled in 0.2L/min-1L/min, the mixing control of water sample
Speed is controlled in 600-1000rmp, the temperature of water sample at 24-40 DEG C.
Preferably, the condensing reflux system includes condenser pipe, helium transfer tube and low-temperature cooling fluid circulating pump, described
The both ends of helium transfer tube are separately connected the aerating system and the trapping cold-trap system, and the condenser pipe covers in a sealing fashion
Outside the helium transfer tube, the cooling passage for surrounding the helium transfer tube is formed, the low-temperature cooling fluid circulating pump is used
In entering coolant recirculation pump in the cooling passage, keep the vapor in the helium transfer tube cold by the coolant liquid
It is solidifying to flow back into the water sample.
Preferably, the helium transfer tube is spiral element.
Preferably, the condensing reflux system controls cooling temperature at 0 DEG C or so.
Preferably, the trapping cold-trap system includes inner tube and covers the outer tube outside said inner tube in a sealing fashion, described
The nuclei of condensation are placed between inner tube and the outer tube, said inner tube is connected to the condensing reflux system, and said inner tube is described outer
The inside of pipe is connected to the outer tube, and the outer tube is equipped with helium exit passageway.
Preferably, the bottom seal of said inner tube, and said inner tube is equipped on the peripheral wall close to the bottom and uniformly divides
The aperture of cloth.
Preferably, the nuclei of condensation are to be filled in trash ice between said inner tube and the outer tube.
Preferably, the outer tube is arranged in liquid nitrogen.
A kind of method of volatile materials in extraction water, uses the device to extract the volatile materials in water.
The invention has the following beneficial effects:
The present invention provides a kind of device and method for extracting volatile materials in water, can generate after water process to water sample
Volatile materials be collected, be convenient for toxicity assessment.The inventive system comprises aerating system, be condensed back system and
Cold-trap system is trapped, the aerating system, the condensing reflux system and the trapping cold-trap system are in turn connected to form access,
When work, helium is passed through in the water sample containing volatile materials by the aerating system, the property of will volatilize substance from water phase stripping to
Gas phase, the vapor come out with helium together stripping is condensed back in the water sample by the condensing reflux system, by stripping
Volatile materials out then enters the trapping cold-trap system with helium, is collected by the nuclei of condensation in the trapping cold-trap system
The volatile materials that capture is come out by stripping.The present invention can effectively come out the volatile materials stripping in water sample as a result,
And these volatile materials are collected by trapping cold-trap.It can use the present apparatus and effectively assess water sample and give birth to during the treatment
At volatile materials risk of toxicity.
Detailed description of the invention
Fig. 1 is the overall structure diagram of the volatile materials extraction element of an embodiment of the present invention.
Fig. 2 is outer tube, inner tube and its assembling schematic diagram of the trapping cold-trap in an embodiment of the present invention.
Fig. 3 is the arresting efficiency figure that an embodiment of the present invention trapping makes an addition to the volatile materials in water sample.
Fig. 4 is the stripping part accounting figure that an embodiment of the present invention trapping makes an addition to the volatile materials in water sample.
Fig. 5 is the volatile toxic substance that an embodiment of the present invention traps that sewage generates after processing, and is carried out
Toxotest, obtained cytotoxicity dosage-effect curve figure.
Chief component symbol description:
Specific embodiment
It elaborates below to embodiments of the present invention.It is emphasized that following the description is only exemplary,
The range and its application being not intended to be limiting of the invention.
Refering to fig. 1 and Fig. 2, in one embodiment, a kind of device extracting volatile materials in water, including aeration system
System is condensed back system and trapping cold-trap system, the aerating system, the condensing reflux system and the trapping cold-trap system
It is in turn connected to form access, the aerating system is for being passed through helium in the water sample containing volatile materials, the property of will volatilize object
From water phase stripping to gas phase, the condensing reflux system is used to for the vapor come out with helium together stripping being condensed back to matter
In the water sample, the volatile materials come out by stripping then enters the trapping cold-trap system, the trapping cold-trap system with helium
The nuclei of condensation are provided in system, the volatile materials come out for collecting capture by stripping.
In a preferred embodiment, the aerating system includes the heating device for heating the water sample.
In a preferred embodiment, the aerating system includes the agitating device for stirring the water sample.By described
Agitating device stirs water sample, and water sample is made adequately to be mixed and be aerated.
Refering to fig. 1, in a more preferred embodiment, the agitating device is constant temperature blender with magnetic force 2.Temperature constant magnetic stirring
Device 2 can be used for stirring and heating water sample, and volatile materials is made to be easier to be come out by stripping.
Refering to fig. 1, in a preferred embodiment, the aerating system includes the three-necked bottle 4 for holding water sample, three-necked bottle
4 neck is for being passed through helium, and another neck is for being connected to the condensing reflux system, and third neck is for being arranged temperature sensor 3.
In a preferred embodiment, the aerating system includes the flowmeter for monitoring the charge flow rate of helium.Flow
Meter may be provided on the helium air inlet 1 of three-necked bottle, for the flow of air inlet 1 to be monitored and controlled.
In a preferred embodiment, the helium gas flow of the aerating system input is controlled in 0.2L/min-1L/min, water sample
Mixing control speed in 600-1000rmp, the temperature of water sample is controlled at 24-40 DEG C.At normal atmospheric pressure, the boiling point of water is
100 DEG C, when water is below boiling point, water can also slowly flash to vapor.
Refering to fig. 1, in a preferred embodiment, the condensing reflux system includes condenser pipe 6, helium transfer tube and low
Warm coolant recirculation pump 5, the both ends of the helium transfer tube are separately connected the aerating system and the trapping cold-trap system, institute
It states condenser pipe 6 to cover in a sealing fashion outside the helium transfer tube, forms the cooling passage for surrounding the helium transfer tube, institute
Low-temperature cooling fluid circulating pump 5 is stated for entering coolant recirculation pump in the cooling passage, is made by the coolant liquid described
Vapor in helium transfer tube is condensed back in the water sample.
Refering to fig. 1, helium transfer tube passes through the connection trapping cold-trap system of connecting tube 7.In a preferred embodiment, the helium
Gas transfer tube uses spiral element.
In a preferred embodiment, the condensing reflux system controls cooling temperature at 0 DEG C or so, is effectively condensed back
The vapor produced by boasting with helium.
Referring to Fig.2, in a preferred embodiment, the trapping cold-trap system includes inner tube 11 and is covered in a sealing fashion in institute
The outer tube 10 outside inner tube 11 is stated, the nuclei of condensation are placed between said inner tube 11 and the outer tube 10, said inner tube 11 is connected to described
Condensing reflux system, said inner tube 11 are connected in the inside of the outer tube 10 with the outer tube 10, and the outer tube 10 is equipped with helium
Exit passageway.
Referring to Fig.2, in a more preferred embodiment, the bottom seal of said inner tube 11, and said inner tube 11 is close to institute
The peripheral wall for stating bottom is equipped with equally distributed aperture.
In a preferred embodiment, the nuclei of condensation are to be filled in trash ice between said inner tube 11 and the outer tube 10.
Refering to fig. 1, in a preferred embodiment, the outer tube is arranged in liquid nitrogen container 8, immerses in liquid nitrogen, so that described
Trapping cold-trap system collects volatile materials at low ambient temperatures.
In a specific embodiment, aerating system is adopted using the 2L three-necked bottle for holding water sample, the trapping cold-trap system
With inner and outer pipe structure, outer pipe outside diameter 29mm, height 330mm, outer tube is equipped with helium exit passageway, inner tube top half internal diameter
8mm, length 50mm, middle section internal diameter 14mm, length 165mm, lower half portion internal diameter 10mm, length 150mm, inner tube top is set
There is rubber plug, for sealing the junction of inner and outer tubes, guarantees that the air-tightness of cold-trap, bottom of inner tube are sealed, but around uniformly
Punching, makes helium uniform air distribution.Trash ice is filled between inner and outer pipe as the nuclei of condensation, packing volume 10-15mL, for trapping
The volatile materials produced by boasting by helium.
In another embodiment, a method of extracting volatile materials in water, use waving for aforementioned any embodiment
Volatile material extraction element extracts the volatile materials in water.
In certain embodiments, volatile materials collection device includes air inlet 1, constant temperature blender with magnetic force 2, temperature
Sensor 3, the three-necked bottle 4 of 2L, low-temperature cooling fluid circulating pump 5, condenser pipe 6, connecting tube 7 and liquid nitrogen container 8, wherein in liquid nitrogen container 8
It is provided with trapping cold-trap 9, trapping cold-trap 9 includes outer tube 10 and inner tube 11 again.Helium is passed into three necks of 2L by air inlet 1
In bottle, constant temperature blender with magnetic force is stirred and is heated to the water sample in three-necked bottle, the volatility come out by helium gas jet stripping
Substance and vapor flow back by condensing tube condensation, and vapor flows back into three-necked bottle, and volatile materials passes through with helium gas jet
Connecting tube enters in trapping cold-trap, and volatile materials can be become trapped on the nuclei of condensation in cold-trap.
Included the following steps: using the detailed process that the collection device of the embodiment of the present invention collects volatile materials in water sample
The high purity water of 10-15mL is frozen into ice cube and is crushed, is filled between the inner and outer tubes of trapping cold-trap.By rubber plug
Set on inner pipe, seals the junction of inner and outer pipe, guarantees the air-tightness of trapping cold-trap, and cold-trap is placed in liquid nitrogen and is carried out
Pre-cooling.
Coolant temperature used in condensing reflux system is adjusted to 0 DEG C or so, is run using low-temperature cooling fluid circulating pump
Condenser system.
The 2L water sample for containing volatile materials is placed in three-necked bottle, and is put into stirring rotator, constant temperature blender with magnetic force
Revolving speed is adjusted to 850rmp, and water temperature is adjusted to 40 DEG C.
Etc. after water sample temperature reach target temperature and stablize, water sample is aerated by air inlet, is furnished with before air inlet
Flowmeter, flowmeter are set as 1L/min, aeration time 5h.
In the 5h of aeration, pay attention to check package unit whether gas leakage.When device gas leakage, all scholars can be smeared in air-leak section
Woods.
In embodiment, wherein the outer pipe outside diameter 29mm of the trapping cold-trap, height 330mm, it is logical that outer tube is equipped with helium outlet
Road, inner tube top half internal diameter 8mm, length 50mm, middle section internal diameter 14mm, length 165mm, lower half portion internal diameter 10mm,
Length 150mm, inner tube top are equipped with rubber plug, for sealing cold-trap, bottom of inner tube sealing, but the uniformly punching around, make gas distribution
Uniformly.
Below by way of specific example, the present invention will be described in detail to the trapping effect and water sample of volatile materials through locating
After reason, the risk of toxicity of the volatile toxic substance of generation.
Example one: adding volatile organic matter into water sample, verifies this device to the stripping effect of volatile materials, and
Trap effect.
Added volatile organic matter is chloroform, bromodichloromethane, dichlorodibromomethane, bromoform, two chloroethenes
Nitrile and dibromo-acetonitrile.The concentration of each substance of addition is 200ug/L or so, volume of water sample 2L.It is carried out using this device
Aeration, helium flow velocity are 1L/min, and constant temperature blender with magnetic force revolving speed is set as 850rmp, and water sample temperature is set as 40 DEG C, fills out in cold-trap
Condensation Assessment of Nuclear Volume 15mL filled or so, aeration time 5h.Cold-trap is placed in room temperature after aeration to melt, is aerated by measurement
Before, after aeration, and in trapping cold-trap each volatile materials concentration, calculate accounting f (%) of each substance by stripping, and return
Yield (%), calculation formula is as follows:
F (%)={ [c (before aeration)-c (after aeration)]/c (before aeration) } × 100
The rate of recovery (%)={ c (trapping cold-trap)/[c (before aeration)-c (after aeration)] } × 100
Such as Fig. 4 and Fig. 5, haloform can be blown out 99%-100%, can substantially be come out by complete stripping, and
The rate of recovery of cold trap trapping is in 60%-70%；Two chloroacetonitriles come out 94% by stripping, and the rate of recovery 63%, dibromo-acetonitrile is blown
45% is taken off, the rate of recovery 25%.Prove that this device is effective to volatile materials stripping, collection in water sample.
Example two: collecting the volatile products of generation using sewage after processing, and evaluates its cytotoxicity.
Used sewage (secondary effluent), measuring its water quality indicator is ammonia nitrogen concentration 0.90mg/L, DOC concentration
5.52mg/L, pH 7.01, water sample are handled using chlorination, and the disinfectant that when chlorination uses is liquor natrii hypochloritis, dosage
For 40mg-Cl2/ L reacts 12h under dark condition.The volatility that water sample generates after chlorination is handled is collected using this device
Substance, helium flow velocity 0.2L/min, constant temperature blender with magnetic force revolving speed are set as 850rmp, and water sample temperature is set as 24 DEG C, when aeration
Between 5h, the condensation Assessment of Nuclear Volume filled in cold-trap is 10mL.Water sample after aeration is passed through into solid phase extraction concentration, is obtained non-volatile
Substance.The volatile materials that nonvolatile matter and trapping cold-trap are collected is subjected to cytotoxicity test (using Chinese storehouse simultaneously
Mouse gonad cell is detected using ATP and carries out cell survival test), obtained measuring effect curve is as shown in Figure 5.
As shown in Figure 5, when being concentrated 68 times, the survival rate of cell is the volatile materials that cold-trap is collected into
66.7%, illustrate that this covering device can effectively trap the sterilized rear volatile materials generated of actual water sample.
The above content is combine it is specific/further detailed description of the invention for preferred embodiment, cannot recognize
Fixed specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs,
Without departing from the inventive concept of the premise, some replacements or modifications can also be made to the embodiment that these have been described,
And these substitutions or variant all shall be regarded as belonging to protection scope of the present invention.
Claims (10)
1. a kind of device for extracting volatile materials in water, which is characterized in that including aerating system, be condensed back system and trapping
Cold-trap system, the aerating system, the condensing reflux system and the trapping cold-trap system are in turn connected to form access, described
Aerating system is for being passed through helium in the water sample containing volatile materials, and the property of will volatilize substance is from water phase stripping to gas phase, institute
Condensing reflux system is stated for the vapor come out with helium together stripping to be condensed back in the water sample, is come out by stripping
Volatile materials then enter the trapping cold-trap system with helium, be provided with the nuclei of condensation in the trapping cold-trap system, be used for
Collect the volatile materials that capture is come out by stripping.
2. device as described in claim 1, which is characterized in that the aerating system includes the heating for heating the water sample
Device.
3. device as claimed in claim 1 or 2, which is characterized in that the aerating system includes for stirring the water sample
Agitating device, it is preferable that the agitating device is constant temperature blender with magnetic force.
4. device as described in any one of claims 1 to 3, which is characterized in that the aerating system includes for holding water sample
Three-necked bottle, a neck of the three-necked bottle uses for being passed through helium, another neck for being connected to the condensing reflux system, third neck
In setting temperature sensor.
5. such as the described in any item devices of Claims 1-4, which is characterized in that the aerating system includes for monitoring helium
Charge flow rate flowmeter.
6. such as device described in any one of claim 1 to 5, which is characterized in that the helium gas flow control of the aerating system input
System is in 0.2L/min-1L/min, and in 600-1000rmp, the temperature of water sample is controlled at 24-40 DEG C the mixing control speed of water sample.
7. such as device as claimed in any one of claims 1 to 6, which is characterized in that the condensing reflux system includes condenser pipe, helium
Gas transfer tube and low-temperature cooling fluid circulating pump, the both ends of the helium transfer tube are separately connected the aerating system and described catch
Collect cold-trap system, the condenser pipe is covered in a sealing fashion outside the helium transfer tube, is formed around the helium transfer tube
Cooling passage, the low-temperature cooling fluid circulating pump is for entering coolant recirculation pump in the cooling passage, by described
Coolant liquid is condensed back to the vapor in the helium transfer tube in the water sample；Preferably, the helium transfer tube is
Spiral element；Preferably, the condensing reflux system controls cooling temperature at 0 DEG C or so.
8. device as described in any one of claim 1 to 7, which is characterized in that the trapping cold-trap system include inner tube and with
Sealing means cover the outer tube outside said inner tube, and the nuclei of condensation, said inner tube connection are placed between said inner tube and the outer tube
The condensing reflux system, said inner tube are connected in the inside of the outer tube with the outer tube, and the outer tube is exported equipped with helium
Access；Preferably, the bottom seal of said inner tube, and said inner tube close to the bottom peripheral wall on be equipped with it is equally distributed
Aperture；Preferably, the outer tube is arranged in liquid nitrogen.
9. device as claimed in claim 8, which is characterized in that the nuclei of condensation be filled in said inner tube and the outer tube it
Between trash ice.
10. a kind of method for extracting volatile materials in water, which is characterized in that using as described in any one of claim 1 to 9
Device extracts the volatile materials in water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811066772.XA CN109141987A (en) | 2018-09-13 | 2018-09-13 | The device and method for extracting volatile materials in water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811066772.XA CN109141987A (en) | 2018-09-13 | 2018-09-13 | The device and method for extracting volatile materials in water |
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| Publication Number | Publication Date |
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| CN109141987A true CN109141987A (en) | 2019-01-04 |
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ID=64825077
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811066772.XA Pending CN109141987A (en) | 2018-09-13 | 2018-09-13 | The device and method for extracting volatile materials in water |
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| CN (1) | CN109141987A (en) |
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| CN111077096A (en) * | 2019-12-20 | 2020-04-28 | 山东大学 | Utilize equipment of ultraviolet detection technique on-line measuring volatile fatty acid |
| CN115253357A (en) * | 2022-06-13 | 2022-11-01 | 湖北中烟工业有限责任公司 | High-efficient condensation enrichment device |
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| CN115253357A (en) * | 2022-06-13 | 2022-11-01 | 湖北中烟工业有限责任公司 | High-efficient condensation enrichment device |
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