CN108362814A - A kind of adsorbable organic halogen detection method - Google Patents
A kind of adsorbable organic halogen detection method Download PDFInfo
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- CN108362814A CN108362814A CN201711494642.1A CN201711494642A CN108362814A CN 108362814 A CN108362814 A CN 108362814A CN 201711494642 A CN201711494642 A CN 201711494642A CN 108362814 A CN108362814 A CN 108362814A
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Abstract
The invention discloses a kind of adsorbable organic halogen detection method, including adsorption step, combustion step, detecting step, wherein adsorption step is：Use the organohalogen compound in activated carbon adsorption water sample to be measured；Combustion step is：Activated carbon after absorption is placed in the oxygen bomb of calorimeter and carries out oxygen-enriched combusting, the organic halogen being adsorbed in combustion process on activated carbon is oxidized to hydrogen halides, and the absorbing liquid being placed in the oxygen bomb absorbs；Detecting step is：After the completion of burning, quantitative adsorption liquid is taken, uses the content of ion-chromatographic determination organic halogen.The lower calorimeter of use cost of the present invention burns to the activated carbon after absorption instead of combustion furnace in the prior art, greatly reduces testing cost.
Description
Technical field
The present invention relates to field of water quality detection more particularly to a kind of adsorbable organic halogen detection methods.
Background technology
AOX indicates that adsorbable organic halogen, the principle for detecting AOX in water at present are with organic halogen in activated carbon adsorption water
Then the activated carbon of the upper organic matter of absorption is put into high temperature furnace and burns, decomposes, being converted into hydrogen halides through alkaline water by plain compound
Solution absorbs, with chromatography of ions separation determination.
But existing detection method has the following disadvantages：
(1) existing detection device especially high temperature furnace is expensive, considerably increases the cost of detection；
(2) rate of recovery of organic halogen is low；
(3) NO when detecting3 -The interference of absorption peak is larger；
(4) when activated carbon adsorption, speed is more difficult to control, and manual operation is more inconvenient.
Invention content
For overcome the deficiencies in the prior art, the purpose of the present invention is to provide a kind of adsorbable organic halogens of low cost
Detection method.
The purpose of the present invention adopts the following technical scheme that realization：
A kind of adsorbable organic halogen detection method, including
Adsorption step：Use the organohalogen compound in activated carbon adsorption water sample to be measured；
Combustion step：Activated carbon after absorption is placed in the oxygen bomb of calorimeter and carries out oxygen-enriched combusting, is inhaled in combustion process
The absorbing liquid for investing the organic halogen on activated carbon and being oxidized to hydrogen halides, and be placed in the oxygen bomb absorbs；
Detecting step：After the completion of burning, quantitative adsorption liquid is taken, uses the content of ion-chromatographic determination organic halogen.
The lower calorimeter of use cost of the present invention replaces combustion furnace in the prior art to carry out the activated carbon after absorption
Burning, greatly reduces testing cost.
Further, the activated carbon in the adsorption step passes through activation process, and activated carbon processing step is：After grinding
Cocoanut active charcoal 1~3h is impregnated in hydrogenperoxide steam generator, then at 450~500 DEG C heat 4h obtain modified activated carbon.
The adsorption capacity that activated carbon can be improved using hydrogenperoxide steam generator processing activated carbon, to be conducive to improve the accurate of detection
Degree.
Further, in the activated carbon processing step, the mass percentage concentration of the hydrogenperoxide steam generator is 15~
30%.
Further, in the activated carbon processing step, the activated carbon after grinding crosses 100~150 mesh sieve.
Further, in the adsorption step, by peristaltic pump so that water sample to be measured with constant flow rate by being equipped with activity
The adsorption tube of charcoal.The flow velocity of water sample to be measured is controlled using peristaltic pump, the degree of automation of detection is improved, reduces people
Work operates the error brought, and is conducive to the accuracy for improving detection.
Further, there is washing step between the adsorption step and the combustion step：Take sodium nitrate solution with 2~
The flow velocity of 3ml/min washs the activated carbon in the adsorption step, washes away sodium nitrate with pure water again later.
Optionally, there is washing step between the adsorption step and the combustion step：Take leacheate with 2~3ml/
The flow velocity of min washs the activated carbon in the adsorption step.
Further, it is specifically included in the combustion step
Fill sample step：Activated carbon after absorption is placed in the sample bowl of calorimeter oxygen bomb, while in the lower section of sample bowl
Place absorbing liquid；
Inflation/deflation step：Pure oxygen is injected into the oxygen bomb, so that pressure in the oxygen bomb is reached 2.8~3MPa, then uses
Means of deflation discharges the gas in the oxygen bomb, repeats abovementioned steps 2 times, and after the 3rd injection pure oxygen, pressure is tieed up in the oxygen bomb
It holds in 2.8~3.0MPa, forms oxygen-enriched low nitrogen environment in the oxygen bomb at this time；
Lighting up procedure：So that activated carbon is burnt in the sample bowl by igniter, activity is adsorbed in combustion process
Organic halogen on charcoal is oxidized to hydrogen halides, and is absorbed by the absorbing liquid in the oxygen bomb.
In the present invention, by being repeatedly oxygenated into the oxygen bomb so that most of air in sample jar is discharged, from
And the oxygen-enriched environment of low nitrogen is formd, NO when advantageously reducing activated carbon burning3 -Generation, to reduce NO in spectrogram3 -It is right
The interference of neighbouring absorption peak, improves the accuracy of detection.
Compared with prior art, the beneficial effects of the present invention are：The lower calorimeter of use cost replaces expensive
Combustion furnace burns, and when burning, is sealed environment in oxygen bomb, and the product hydrogen halides after organic halogen burning can be placed in
Absorbing liquid in oxygen bomb fully absorbs, and ensures the accuracy of detection；The inflatable characteristic of calorimeter oxygen bomb is utilized simultaneously, for activity
Charcoal manufactures the oxygen-enriched burning situation of low nitrogen, NO when reducing burning3 -Generation, and then improve the accuracy of detection.
Description of the drawings
Fig. 1 is the collection of illustrative plates obtained using sulfate by ion chromatography after method using the present invention is burnt.
Fig. 2 is after the method provided using standard HJ/T 83-2001 is burnt, to be obtained using sulfate by ion chromatography
Collection of illustrative plates.
Specific implementation mode
In the following, in conjunction with attached drawing and specific implementation mode, the present invention is described further, it should be noted that not
Under the premise of conflicting, new implementation can be formed between various embodiments described below or between each technical characteristic in any combination
Example.
The detection method of adsorbable organic halogen can refer to the professional standard HJ/T 83-2001 of environmental protection, the prior art
In, in order to carry out combustion step, it is designed with dedicated combustion furnace, however dedicated combustion furnace is expensive, considerably increases inspection
Survey cost so that detection method is not easy to promote.
To solve the above problems, the present invention provides a kind of adsorbable organic halogen detection method of low cost, including it is following
Step
Adsorption step：Use the organohalogen compound in activated carbon adsorption water sample to be measured；
Combustion step：Activated carbon after absorption is placed in the oxygen bomb of calorimeter and carries out oxygen-enriched combusting, is inhaled in combustion process
The absorbing liquid for investing the organic halogen on activated carbon and being oxidized to hydrogen halides, and be placed in the oxygen bomb absorbs；
Detecting step：After the completion of burning, quantitative adsorption liquid is taken, uses the content of ion-chromatographic determination organic halogen.
The present invention completes combustion step using calorimeter in the prior art, since the oxygen bomb of calorimeter can ensure activity
Charcoal burns in sealed environment, it is also ensured that absorbing liquid fully absorbs combustion product, therefore it is completely alternative existing
Combustion furnace, and the price of calorimeter will well below dedicated combustion furnace in the prior art, thus greatly reduce detection at
This so that detection method of the invention is easy to spread.
Further, in order to improve the adsorption capacity of activated carbon, the activated carbon in adsorption step is by pretreatment, activated carbon
Processing step be：Activated carbon after grinding is impregnated into 1~3h in hydrogenperoxide steam generator, is then heated at 450~500 DEG C
4h obtains modified activated carbon.
The processing step of activated carbon is specially：After commercially available cocoanut active charcoal is ground, 100~150 mesh sieve is crossed, matter is used
It measures the hydrogenperoxide steam generator that percentage concentration is 15~30% and impregnates 1~3h, Muffle furnace is used after taking-up, is added at 450~500 DEG C
3~5h of heat, is cooled to room temperature, spare.
Further, the water sample to be measured in adsorption step is also to be acquired and pre-process according to HJ/T 83-2001.
Further, in adsorption step, by peristaltic pump so that water sample to be measured is passed through with constant flow rate equipped with activated carbon
Adsorption tube.Adsorption tube is the glass column that both ends are blocked with silica wool, and the modified activated carbon of 45~55mg is loaded in adsorption tube, is taken
The water sample of 250ml is placed in beaker, using peristaltic pump, flows through adsorption tube with water sample with the speed of 2~3ml/min, and accurately remember
The volume for recording trickle, to calculate the volume of activated carbon adsorption.
Further, in adsorption step, water sample to be measured is after the adsorption tube, using sodium nitrate cleaning solution to the suction
Attached pipe is washed.Specifically, the sodium nitrate solution of 20ml is washed into the adsorption tube, Zhi Houyong with the speed of 2~3ml/min
Pure water is with speed detergent active 10~30min of charcoal of 2~3L/min, to wash away sodium nitrate.Alternatively, leacheate can also be used directly
It is washed, without being washed with water after leacheate washing.The ingredient of leacheate can be selected according to actual conditions, leacheate
Ingredient be common knowledge for those skilled in the art, the present invention do not limit.
Further, it burns step and specifically includes following steps
Fill sample step：Activated carbon after absorption is placed in the sample bowl of calorimeter oxygen bomb, while in the lower section of sample bowl
Place absorbing liquid；
Inflation/deflation step：Pure oxygen is injected into the oxygen bomb, so that pressure in the oxygen bomb is reached 2.8~3.0MPa, then makes
The gas in the oxygen bomb is discharged with means of deflation, repeats abovementioned steps 2 times, after the 3rd injection pure oxygen, pressure in the oxygen bomb
2.8~3.0MPa is maintained, forms oxygen-enriched low nitrogen environment in the oxygen bomb at this time；
Lighting up procedure：So that activated carbon is burnt in the sample bowl by igniter, activity is adsorbed in combustion process
Organic halogen on charcoal is oxidized to hydrogen halides, and is absorbed by the absorbing liquid in the oxygen bomb.
Further, it fills in sample step, the absorbing liquid being put into the oxygen bomb is the boron of 10ml, concentration 0.0025mol/L
Sand solution.
Embodiment 1
Activated carbon is modified by following steps：After commercially available cocoanut active charcoal is ground, 100-150 mesh sieve is crossed,
The hydrogenperoxide steam generator that use quality percentage concentration is 15~30% impregnates 2h, Muffle furnace is used after taking-up, at 450~500 DEG C
Lower heating 4h, is cooled to room temperature, spare.
The adsorbable organic halogen content in water sample is detected by following steps:
A. water sample is acquired and is pre-processed according to HJ/T 83-2001；
B. it takes 250ml water samples to be placed in beaker, using peristaltic pump, so that sample is flowed through with the speed of 2~3ml/min and be loaded with about
The adsorption tube of the modified activated carbon of 50mg, accurate to record trickle volume, it is to make a living to deduct the water column volume after adsorption tube
Property charcoal absorption volume；
C. 20ml sodium nitrate cleaning solutions are taken, adsorption column is washed with the flow velocity of 2~3ml/min, uses pure water with 2~3L/ later
Speed detergent active 10~30min of charcoal of min, to wash away sodium nitrate.
D. the activated carbon after absorption is poured into the sample bowl of calorimeter oxygen bomb, while takes the absorbing liquid of 10ml
(0.0025mol/L borax solns) is placed in oxygen bomb；
E. pure oxygen is injected in calorimeter sample oxygen bomb, so that pressure in oxygen bomb is reached 2.8~3.0MPa, is released using means of deflation
Gas in oxygen bomb is put, is repeated 2 times, after the 3rd injection pure oxygen, pressure maintains 2.8~3.0MPa in oxygen bomb, at this time shape in oxygen bomb
At the environment of oxygen-enriched low nitrogen；
F. igniter lights the activated carbon in sample bowl, when activated carbon burns, adsorbs AOX oxidations point on it
Solution, is converted into hydrogen halides, and absorbed by absorbing liquid；
G. after the completion of burning, absorbing liquid is taken out from oxygen bomb, and a certain amount of absorbing liquid is taken to be detached with the chromatography of ions
It measures.
Fig. 1 is the collection of illustrative plates obtained using sulfate by ion chromatography after method using the present invention is burnt.Fig. 2 is to adopt
After being burnt with the standard HJ/T 83-2001 method provided, the collection of illustrative plates that is obtained using sulfate by ion chromatography.Comparison diagram 1 with
Fig. 2 is can be found that：Using method provided by the invention, NO in test result3 -Concentration it is extremely low, test result will not be caused to do
It disturbs；And in standard method, NO3 -Concentration is higher, can be to neighbouring Br-Peak test result impacts, this is mainly standard method
In, when nitrogen combustion, is aoxidized, and NO is generated2, NO is generated after being absorbed3 -, to generate interference to result.As shown in Figure 1, this hair
Br after bright method absorbs-Measured value is 0.122mg/L, and uses standard method, since there are NO3 -Interference, Br-Measured value is obviously small
In the measured value of the present invention, only 0.081mg/L.It is possible thereby to which detection method using the present invention can reduce NO3 -Interference,
Reduce Br-Test error.
In addition, the present invention also compare modified activated carbon (namely hydrogenperoxide steam generator treated activated carbon) with it is unmodified
The rate of recovery of the activated carbon to organic halogen in water.The step of being provided according to embodiment 1, using the parachlorophenol of the 1.0mg/L containing chlorine
Titer is analyzed.Table 1 is the comparison of modified activated carbon and the unmodified activated carbon rate of recovery.
1 two kinds of preconcentration with activated carbon performances of table compare
Table 1 the experimental results showed that, the rate of recovery of modified activated carbon is substantially improved than the rate of recovery of unmodified activated carbon.
This may be to increase activated carbon surface acidic functionality since hydrogen peroxide oxidation modification can reduce the isoelectric point of activated carbon, to
Improve the surface hydrophilicity of activated carbon.In addition, the method that hydrogen peroxide is modified, the NO dissolved out in activated carbon3 -Equal impurity are less, can save
Complicated elution link is gone, experimental work amount is reduced.
In addition, the present invention is also compared when being adsorbed using modified activated carbon, different sample injection methods are to the organic halogen rate of recovery
Influence.In the prior art frequently with two kinds of sample injection methods be logical nitrogen adsorption and simple absorption, in standard HJ/T 83-
It is described in 2001, and will not be described here in detail.Table 2 is listed respectively using peristaltic pump absorption (present invention), logical nitrogen adsorption (standard
HJ/T 83-2001), simple absorption (standard HJ/T 83-2001) three kinds of input modes by water sample (1.0mg/L containing chlorine to chlorine
Phenol Standard liquid) flow through the rate of recovery of organic halogen after activated carbon.
2 three kinds of absorption input modes of table compare
Table 2 the experimental results showed that, the rate of recovery of the rate of recovery and logical nitrogen adsorption adsorbed using peristaltic pump is closer to,
90% or more, meet requirement of experiment, and deviation is smaller.Compared with simple suction type in national standard method, peristaltic pump absorption
Preci-sion and accuracy be improved to some extent, this is mainly due to peristaltic pump sample introduction speed is more uniform, be conducive to
The absorption of AOX.
In addition, peristaltic pump absorption compared with logical nitrogen adsorption mode, without using nitrogen, and is not necessarily to customize adsorbent equipment,
It is more economical and practical, in addition, automatic sampling when peristaltic pump suction type realizes unattended, reduces labor intensity.
The above embodiment is only the preferred embodiment of the present invention, and the scope of protection of the present invention is not limited thereto,
The variation and replacement for any unsubstantiality that those skilled in the art is done on the basis of the present invention belong to institute of the present invention
Claimed range.
Claims (8)
1. a kind of adsorbable organic halogen detection method, which is characterized in that including
Adsorption step：Use the organohalogen compound in activated carbon adsorption water sample to be measured；
Combustion step：Activated carbon after absorption is placed in the oxygen bomb of calorimeter and carries out oxygen-enriched combusting, is adsorbed in combustion process
Organic halogen on activated carbon is oxidized to hydrogen halides, and the absorbing liquid being placed in the oxygen bomb absorbs；
Detecting step：After the completion of burning, quantitative adsorption liquid is taken, uses the content of ion-chromatographic determination organic halogen.
2. adsorbable organic halogen detection method according to claim 1, which is characterized in that the work in the adsorption step
Property charcoal pass through activation process, activated carbon processing step is：Cocoanut active charcoal after grinding impregnates in hydrogenperoxide steam generator to 1~
Then 3h heats 4h at 450~500 DEG C and obtains modified activated carbon.
3. adsorbable organic halogen detection method according to claim 2, which is characterized in that the activated carbon processing step
In, the mass percentage concentration of the hydrogenperoxide steam generator is 15~30%.
4. adsorbable organic halogen detection method according to claim 2, which is characterized in that the activated carbon processing step
In, the cocoanut active charcoal after grinding crosses 100~150 mesh sieve.
5. adsorbable organic halogen detection method according to claim 1, which is characterized in that in the adsorption step, lead to
Crossing peristaltic pump makes water sample to be measured pass through activated carbon with constant flow rate.
6. adsorbable organic halogen detection method according to claim 1, which is characterized in that the adsorption step with it is described
There is washing step between combustion step：Sodium nitrate solution is taken to wash the work in the adsorption step with the flow velocity of 2~3ml/min
Property charcoal, washes away sodium nitrate with pure water again later.
7. adsorbable organic halogen detection method according to claim 1, which is characterized in that the adsorption step with it is described
There is washing step between combustion step：Leacheate is taken to wash the activity in the adsorption step with the flow velocity of 2~3ml/min
Charcoal.
8. according to any adsorbable organic halogen detection methods of claim 1-7, which is characterized in that the combustion step
In specifically include
Fill sample step：Activated carbon after absorption is placed in the sample bowl of calorimeter oxygen bomb, while being placed in the lower section of sample bowl
Absorbing liquid；
Inflation/deflation step：Pure oxygen is injected into the oxygen bomb, pressure in the oxygen bomb is made to reach 2.8~3MPa, then using deflation
Device discharges the gas in the oxygen bomb, repeats abovementioned steps 2 times, and after the 3rd injection pure oxygen, pressure maintains in the oxygen bomb
2.8~3.0MPa forms oxygen-enriched low nitrogen environment at this time in the oxygen bomb；
Lighting up procedure：So that activated carbon is burnt in the sample bowl by igniter, is adsorbed on activated carbon in combustion process
Organic halogen be oxidized to hydrogen halides, and absorbed by the absorbing liquid in the oxygen bomb.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112505204A (en) * | 2020-12-16 | 2021-03-16 | 中煤浙江检测技术有限公司 | Organic halogen extracting solution and method for detecting adsorbable organic halogen in soil |
| 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 |
| CN114486868A (en) * | 2021-11-26 | 2022-05-13 | 云南大地丰源环保有限公司 | Quick identification method for halogen elements |
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| CN114486868A (en) * | 2021-11-26 | 2022-05-13 | 云南大地丰源环保有限公司 | Quick identification method for halogen elements |
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