CN109283024A - A kind of AOX organic halogen sample recovery method - Google Patents
A kind of AOX organic halogen sample recovery method Download PDFInfo
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- CN109283024A CN109283024A CN201810853558.2A CN201810853558A CN109283024A CN 109283024 A CN109283024 A CN 109283024A CN 201810853558 A CN201810853558 A CN 201810853558A CN 109283024 A CN109283024 A CN 109283024A
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- sample
- tube
- aox
- combustion
- organic halogen
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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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
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The present invention relates to water quality inspection technique fields, more particularly to a kind of AOX organic halogen sample recovery method, include: step S1, will be packed into Molotov cocktail by pretreated water sample, and carry out vibrating obtained activated carbon sample on the oscillator after being packed into AOX special-purpose activated charcoal in Molotov cocktail；Step S2, pre-processes combustion tube and example boat, takes out activated carbon sample and puts it into the example boat being disposed, example boat is pushed into the combustion tube of high temperature combustion furnace, so that activated carbon sample is carried out full combustion and gaseous sample is made；Gaseous sample is emitted into the air blister type absorption tube connecting with the outlet side of combustion tube and is recycled by step S3.Beneficial effect is: the present invention makes activated carbon sufficiently adsorb the water sample of acquisition using " oscillation suction type " replacement " nitrogen pressurized adsorbent ", simplifies operating process, improves working efficiency and sample recovery rate, easy to operate, highly effective.
Description
Technical field
The present invention relates to water quality inspection technique fields, and in particular to a kind of AOX organic halogen sample recovery method.
Background technique
AOX refers to absorbable halide (Absorbable Organic Halogen), AOX organic halogen (organochlorine,
Organic fluoride, organic bromine) measurement have become the important Water Quality Control Indexes of environment measuring industry.Adsorbable organic halogens
(AOX) most of is persistence organic pollutant, because it is with teratogenesis, carcinogenic and mutagenicity, it has also become an important water
Matter Con trolling index.The measurement of Adsorbable organic halogens has small-hole drilling (GB/T15959-1995) and the chromatography of ions in water
(HJ/T83-2001), two methods are required to use a core component-with precise temperature control, closed high temperature combustion furnace (temperature
Degree is set as 950 DEG C).It purchases organohalogen compounds analyzer and needs substantial contribution in laboratory.
Currently used water sample analysis method has column adsorption method, and column absorption is the sample cell that water sample is moved into adsorbent equipment
In, so that water sample is flowed through adsorption column with 2-3ml speed per minute, the organohalogen compounds in water sample are adsorbed on adsorption column, are reached
To the purpose of absorption.
Column adsorption method simplifies treatment process, and at present in many laboratories, the column adsorption method for simplifying version is all using constant
Nitrogen pressure as power, operate comparatively laborious.And it is easy to happen the reduction that will cause subsequent flow velocity when blocking and cannot fill
The problem of dividing absorption, greatly reduce analysis efficiency.
Summary of the invention
The purpose of the present invention is to solve the above problems, provide a kind of AOX organic halogen sample recovery method.
In order to achieve the above object of the invention, the invention adopts the following technical scheme:
A kind of AOX organic halogen sample recovery method, comprising:
Step S1 will be packed into Molotov cocktail by pretreated water sample, shake after being packed into AOX special-purpose activated charcoal in Molotov cocktail
It swings and carries out vibrating obtained activated carbon sample on device；
Step S2, pre-processes combustion tube and example boat, takes out what activated carbon sample and putting it into was disposed
In example boat, example boat is pushed into the combustion tube of high temperature combustion furnace, so that activated carbon sample is carried out full combustion and gas is made
Sample；
Gaseous sample is emitted into the air blister type absorption tube connecting with the outlet side of combustion tube and is returned by step S3
It receives.
Preferably, the step S2 includes step 21: the air inlet of high temperature combustion furnace and apparatus of oxygen supply are connected by pipeline
Connect, the first gas outlet and the second gas outlet of high temperature combustion furnace respectively with the first air inlet of the outer tube of combustion tube, combustion tube
Second air inlet of inner tube opens apparatus of oxygen supply and inputs oxygen progress oxygen purging into combustion tube by piping connection.
Preferably, the step S2 includes step S22: will be in the preheating zone of empty example boat push-in combustion tube and to burning
Pipe opens high temperature combustion furnace after jumping a queue, and oxygen is inputted into combustion tube by apparatus of oxygen supply.
Preferably, the step S2 further includes step S23: borax absorbing liquid is packed into air blister type absorption tube, in bubble
Gauze heat preservation is wrapped up on sebific duct between formula absorption tube and combustion tube outlet side.
Preferably, the step S2 includes step S24: will be filled in the Molotov cocktail on oscillator in such a way that filter paper filters
The activated carbon sample of adsorption sample water is divided to take out.
Preferably, stating step S2 includes step S25: the example boat in high temperature combustion furnace preheating zone is taken out, by active carbon sample
Product move into example boat, then example boat is pushed into combustion tube preheating zone and is jumped a queue to combustion tube, stop example boat in preheating zone
2min。
Preferably, the step S2 includes step S26: example boat being slowly pushed into high-temperature region and is jumped a queue, in pipe to be combusted
Example boat completely, then is withdrawn into the inlet of combustion tube and jumped a queue to combustion tube by active carbon burning, is continued by apparatus of oxygen supply
To example boat oxygen blast 4min to 5min.
Preferably, the step S3 includes: closing high temperature combustion furnace, first turns off the switch on oxygen cylinder and turns off high temperature combustion again
The flowmeter valve on furnace is burnt, absorption tube and connecting tube are removed from high temperature combustion furnace, is exported with ear washing bulb from air blister type absorption tube
End is gently blown, and is made in absorption tube and connecting tube in remaining droplet sucking air blister type absorption tube.
Preferably, the Molotov cocktail is tool plug triangle Molotov cocktail.
Preferably, the time range that the Molotov cocktail vibrates on the oscillator is 60min to 90min.
Compared with prior art, the present invention beneficial effect is: the present invention is using " oscillation suction type " replacement " nitrogen pressurization
Absorption " makes activated carbon sufficiently adsorb the water sample of acquisition, simplifies operating process, improves working efficiency and sample recovery rate, operation
It is convenient, highly effective.
In a preferred scheme, the activated carbon sample after absorption water sample of the invention is enclosed in combustion tube and carries out in advance
It in the example boat of heating, then is pushed into combustion tube, provides working efficiency, make activated carbon sample full combustion.
Detailed description of the invention
Fig. 1 is process flow chart of the invention；
Fig. 2 is the specific flow chart of step S2.
Specific embodiment
Below in conjunction with the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carry out it is clear,
It is fully described by, it is clear that described embodiment is only a part of the embodiments of the present invention, instead of all the embodiments.
Based on the embodiments of the present invention, obtained by those of ordinary skill in the art without making creative efforts all
Other embodiments shall fall within the protection scope of the present invention.
If raw material employed in the embodiment of the present invention is raw material commonly used in the art without specified otherwise, implement
Method employed in example, is the conventional method of this field.
Water sampling, active carbon equipment, bubble absorption tube, example boat, glassware and other devices as described in the examples
Tool and reagent material are all made of (HJ/T83-2001) chromatography of ions and the standard of (GB/T15959-1995) small-hole drilling is wanted
It asks.
It is as shown in Figure 1 and Figure 2: a kind of AOX organic halogen sample recovery method of the present embodiment, comprising:
Step S1 will be packed into flask by pretreated water sample, be packed into after AOX special-purpose activated charcoal in flask in oscillator
On carry out vibrating obtained activated carbon sample.
In this step S1, the Molotov cocktail is tool plug triangle Molotov cocktail, and Molotov cocktail capacity is 250ml, by 125ml by pre-
The water sample of processing is packed into Molotov cocktail, and the sample water of 125ml generally requires the AOX special-purpose activated charcoal greater than 50mg.In this implementation
In example, it is packed into the AOX special-purpose activated charcoal of 60mg in Molotov cocktail, is vibrated on electric agitator or ultrasonic oscillator, vibrates
It is more than hour to generally require one, it is preferred that allow active carbon sufficiently to adsorb water sample, duration of oscillation to improve efficiency and can guarantee
It is set as 70min.
After step S1, execute step S2: combustion tube and example boat are pre-processed, take out activated carbon sample and by its
It is put into the example boat being disposed, example boat is pushed into combustion tube preheating zone and jumps a queue to combustion tube, preheating example boat
Area stops 2min.It shifts intermediate high-temperature region onto again, so that activated carbon sample is carried out full combustion and gaseous sample is made.
Above-mentioned high temperature combustion furnace uses AOX-3 organic halogen combustion furnace, which is existing equipment.
Step S2 includes step S21, is pre-processed to combustion tube: the air inlet of high temperature combustion furnace and apparatus of oxygen supply are led to
Cross piping connection, the first gas outlet and the second gas outlet of high temperature combustion furnace respectively with the first air inlet of the outer tube of combustion tube,
By piping connection, unlatching apparatus of oxygen supply inputs oxygen progress oxygen into combustion tube and blows second air inlet of the inner tube of combustion tube
It washes.
For the oxygen used in step S21 for 99.999% purity oxygen, AOX-3 organic halogen combustion furnace right side has oxygen
Import, first by the oxygen inlet on the right side of 99.999% pure oxygen air pipe access AOX-3 organic halogen combustion furnace.AOX-3 is organic
First air inlet of the outer tube of the first gas outlet access combustion tube of halogen combustion furnace, positioned at the top of combustion tube；AOX-3 is organic
Second air inlet of the inner tube of the second gas outlet access combustion tube of halogen combustion furnace, positioned at the lower section of combustion tube；Two connections
Place is all made of band and tightens, and the entrance of big small sample is finally blocked using rubber plug.
In step 21, it is also necessary to the positive stream of oxygen pressure reducing valve and AOX-3 organic halogen combustion furnace to apparatus of oxygen supply
Meter is adjusted.In two oxygen flow meters of front setting of AOX-3 organic halogen combustion furnace, it is respectively used to detection input combustion
The oxygen flow for burning pipe inner and outer tubes, makes the oxygen blast speed in combustion tube inner tube reach 120-150ml/min；Make outside combustion tube
Oxygen blast speed in pipe reaches 40-60ml/min；Sky blows the time for 3min, to ensure combustion tube and the burning of AOX-3 organic halogen
The sebific duct of furnace outlet it is pure.
After the step S21, step S22 is executed, example boat is pre-processed: by empty example boat push-in burning
High temperature combustion furnace is opened after jumping a queue in the preheating zone of pipe and to combustion tube, oxygen is inputted into combustion tube by apparatus of oxygen supply.
In the step S22, clean empty example boat shifts combustion tube preheating zone onto, and it is organic which is located at AOX-3
At the fire door of halogen combustion furnace, after empty example boat push-in combustion tube, jump a queue combustion tube by AOX-3 organic halogen combustion furnace
Temperature be set in 950 DEG C and heat up, apparatus of oxygen supply oxygen blast into combustion tube is then turned on, to the oxygen blow duration of empty example boat
No less than 10min.
The step S2 includes step S23: being packed into 3ml borax absorbing liquid in air blister type absorption tube, absorbs in bubble type
The heat preservation of package gauze is conducive to the recycling of gaseous sample on sebific duct between pipe and combustion tube outlet side.
After the step S23, execute step S24, i.e., it will be in the Molotov cocktail on oscillator in such a way that filter paper filters
The activated carbon sample of abundant adsorption sample water takes out.
After the step S24, step S25 is executed, the example boat in high temperature combustion furnace preheating zone is taken out, by active carbon sample
Product move into example boat, then example boat is pushed into combustion tube preheating zone and is jumped a queue to combustion tube, stop example boat in preheating zone
2min。
After the step S25, step S26 is executed, example boat is slowly pushed into high-temperature region from preheating zone, in pipe to be combusted
Active carbon burning completely, then example boat is withdrawn into the inlet of combustion tube and is jumped a queue to combustion tube, by apparatus of oxygen supply after
Continue to example boat oxygen blast 4min to 5min.
In step S26, due to joined the AOX active carbon of 60mg, the active carbon just meeting in about 3min after-combustion pipe is needed
Completely, the flame of the active carbon for the combustion inner pipe that burns at this time extinguishes, so that it may judge that active carbon has burnt completely for burning.
Gaseous sample is emitted into the air blister type absorption tube connecting with the outlet side of combustion tube and is returned by step S3
It receives.
The step S3 further include: close high temperature combustion furnace, first close oxygen valve and turn off flowmeter valve.From high-temp combustion
Absorption tube and connecting tube are removed on furnace, are gently blown with ear washing bulb from air blister type absorption tube outlet end, are made absorption tube and connecting tube
In in remaining droplet sucking air blister type absorption tube.
Embodiment 2: it on the basis of embodiment 1, simplifies activated carbon purification method: being moved into clean empty example boat
The AOX special-purpose activated charcoal of 50mg, is put among the combustion tube of AOX-3 organic halogen combustion furnace.Oxygen flow meter is observed, makes to burn
The oxygen blast speed of pipe inner tube is 120-150ml/min；It is 280 DEG C that temperature, which is arranged, purifies 30min.
The present invention makes activated carbon sufficiently adsorb the water sample of acquisition using oscillation suction type, improves work efficiency, and improves
Sample recovery rate.The process of gas washing is reduced using 99.999% pure oxygen；Streamline operation improves working efficiency and matter
Amount, easy to operate, highly effective, technique meet (HJ/T83-2001) chromatography of ions and (GB/T15959-1995) microcoulomb
The requirement of method.
The present invention utilizes the configuration of existing AOX-3 organic halogen combustion furnace, can complete adsorbable organic halogen (AOX)
Measurement, and be not required to carry out existing equipment big change, reduce scrap build cost, improve the function of existing equipment, energy
Enough greatly easy operations, while sample recovery rate is improved, greatly improve working efficiency.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (10)
1. a kind of AOX organic halogen sample recovery method characterized by comprising
Step S1 will be packed into Molotov cocktail by pretreated water sample, be packed into after AOX special-purpose activated charcoal in Molotov cocktail in oscillator
On carry out vibrating obtained activated carbon sample；
Step S2, pre-processes combustion tube and example boat, takes out activated carbon sample and puts it into the sample being disposed
In boat, example boat is pushed into the combustion tube of high temperature combustion furnace, so that activated carbon sample is carried out full combustion and gaseous sample is made；
Gaseous sample is emitted into the air blister type absorption tube connecting with the outlet side of combustion tube and is recycled by step S3.
2. a kind of AOX organic halogen sample recovery method according to claim 1, which is characterized in that the step S2 packet
Include step 21: by the air inlet of high temperature combustion furnace and apparatus of oxygen supply by piping connection, the first gas outlet of high temperature combustion furnace and
Second gas outlet is connected with the second air inlet of the inner tube of the first air inlet of the outer tube of combustion tube, combustion tube by pipeline respectively
It connects, opens apparatus of oxygen supply and input oxygen progress oxygen purging into combustion tube.
3. a kind of AOX organic halogen sample recovery method according to claim 2, which is characterized in that the step S2 packet
It includes step S22: high temperature combustion furnace will be opened in the preheating zone of empty example boat push-in combustion tube and after jumping a queue to combustion tube, passed through
Apparatus of oxygen supply inputs oxygen into combustion tube.
4. a kind of AOX organic halogen sample recovery method according to claim 3, which is characterized in that the step S2 is also
Including step S23: borax absorbing liquid is packed into air blister type absorption tube, between air blister type absorption tube and combustion tube outlet side
Gauze heat preservation is wrapped up on sebific duct.
5. a kind of AOX organic halogen sample recovery method according to claim 4, which is characterized in that the step S2 packet
It includes step S24: taking the activated carbon sample of adsorption sample water abundant in the Molotov cocktail on oscillator in such a way that filter paper filters
Out.
6. a kind of AOX organic halogen sample recovery method according to claim 5, which is characterized in that stating step S2 includes
Step S25: taking out the example boat in high temperature combustion furnace preheating zone, activated carbon sample is moved into example boat, then example boat is pushed away
Enter combustion tube preheating zone and jump a queue to combustion tube, example boat is made to stop 2min in preheating zone.
7. a kind of AOX organic halogen sample recovery method according to claim 6, which is characterized in that the step S2 packet
It includes step S26: example boat being slowly pushed into high-temperature region and is jumped a queue, the active carbon burning in pipe to be combusted completely, then example boat is drawn
It returns to the inlet of combustion tube and jumps a queue to combustion tube, continued by apparatus of oxygen supply to example boat oxygen blast 4min to 5min.
8. a kind of AOX organic halogen sample recovery method according to claim 1, which is characterized in that the step S3 packet
It includes: closing high temperature combustion furnace, first turn off the switch on oxygen cylinder and turn off flowmeter valve on combustion furnace again, from high temperature combustion furnace
Absorption tube and connecting tube are removed, is gently blown, is made residual in absorption tube and connecting tube from air blister type absorption tube outlet end with ear washing bulb
In the droplet sucking air blister type absorption tube stayed.
9. a kind of AOX organic halogen sample recovery method according to claim 1-8, which is characterized in that described
Molotov cocktail is tool plug triangle Molotov cocktail.
10. a kind of AOX organic halogen sample recovery method according to claim 1-8, which is characterized in that described
The time range that Molotov cocktail vibrates on the oscillator is 60min to 90min.
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| CN201810853558.2A CN109283024A (en) | 2018-07-30 | 2018-07-30 | A kind of AOX organic halogen sample recovery method |
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| CN201810853558.2A CN109283024A (en) | 2018-07-30 | 2018-07-30 | A kind of AOX organic halogen sample recovery method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376307A (en) * | 2021-06-23 | 2021-09-10 | 国家纺织服装产品质量监督检验中心（浙江桐乡） | Method for measuring AOX content in textile by adopting oscillation extraction and ion chromatography |
| CN115343401A (en) * | 2022-07-11 | 2022-11-15 | 浙江格临检测股份有限公司 | Method for measuring adsorbable organic halogen AOX in soil and sediment |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113376307A (en) * | 2021-06-23 | 2021-09-10 | 国家纺织服装产品质量监督检验中心（浙江桐乡） | Method for measuring AOX content in textile by adopting oscillation extraction and ion chromatography |
| CN115343401A (en) * | 2022-07-11 | 2022-11-15 | 浙江格临检测股份有限公司 | Method for measuring adsorbable organic halogen AOX in soil and sediment |
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Application publication date: 20190129 |