CN106745451A - A kind of enrichment method of Organic Pollutants of Drinking Water - Google Patents
A kind of enrichment method of Organic Pollutants of Drinking Water Download PDFInfo
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- CN106745451A CN106745451A CN201611091122.1A CN201611091122A CN106745451A CN 106745451 A CN106745451 A CN 106745451A CN 201611091122 A CN201611091122 A CN 201611091122A CN 106745451 A CN106745451 A CN 106745451A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
The invention belongs to Environmental Health and water analysis technical field, it is related to water analysis pre-treating method, and in particular to a kind of enrichment method of Organic Pollutants of Drinking Water.This method is by three kinds of sorbing materials such as integrated XAD 2, PSDVB and coconut husk class activated carbon, and fine-tune water sample pH value, realize that trace organic pollutant in water is drunk in wide spectrum enrichment, the enriched substance for being obtained can be not only used for drinking trace organic pollutant in water analysis of spectrum, be also applied for biological effect research.The present invention compensate for the single deficiency of enriched fractions species in existing method, while water sample enriching apparatus used are simple, sorbing material is easy to get and can reuse, organic pollution huge number can be enriched with, bioaccumulation efficiency is high, and enrichment capacity is big, and the inventive method is with a wide range of applications.
Description
Technical field
The invention belongs to Environmental Health and water analysis technical field, it is related to water analysis pre-treating method, and in particular to one
Plant the enrichment method of Organic Pollutants of Drinking Water.XAD-2, PSDVB and coconut husk class activated carbon are used in series in the inventive method
Deng three kinds of sorbing materials of different characterization of adsorptions, and water sample pH value is fine-tuned, realize that underwater trace is drunk in wide spectrum enrichment organic
Pollutant.
Background technology
Data shows that the influence that organic extracts from water is polluted to health has turned into Environmental Health field and begged to be solved
Major issue.It is reported that the organic pollution that the whole world is detected in water at present is up to 2 221 kinds, wherein 765 kinds are present in drink
With in water, they some tumours may have certain relation with the mankind, it is considered to be the important chemistry of influence population health
Material.Generally acknowledge in the industry, it is characterized in the basis for carrying out drinking water safety research to understand Organic Pollutants of Drinking Water；Based on specific mesh
The qualitative, quantitative description of pollutant such as organo-chlorine pesticide, polycyclic aromatic hydrocarbon etc. is marked, is most commonly seen Organic Pollutants of Drinking Water
Character description method, but still be the integral status and feature for not knowing that water pollution, so as to find the pollution really worked
Species are other.Pollutant spectrum parsing based on biological effect is the means being taken seriously in recent years, and it can be fully understanded has
The pollutant classification and quantity of potential health hazard effect, further across the Organic Pollutants of Drinking Water of purification of water quality treatment
Concentration is low, in μ g/L and ng/L levels, therefore, efficiently, wide spectrum ground enrichment drink trace organic pollutant in water turn into drink
A major issue in water security research field water analysis.
At present, Organic Pollutants of Drinking Water beneficiation technologies are numerous, but every kind of technology can only be directed to specific organic contamination
Thing is enriched with, therefore, the organic micro-pollutant beneficiation technologies of wide spectrum are still lacked in practice.XAD-2 adsorbents are hydrophobicitys
Macropore polymer resin, its matrix is the divinyl benzene copolymer of styrene one, the nonpolar and low polar organic matter of primary attachment,
The compound such as including volatility and half volatile halogenated organic compound, phenols, polycyclic aromatic hydrocarbon, it is usually used in causing to dash forward in enrichment water
Denaturation organic compound such as MX；PS/DVB is the divinyl benzene copolymer of styrene one of 1% crosslinking, its flourishing specific surface area
Big and microcellular structure makes it have strong characterization of adsorption, can effectively adsorb polarity organic matter higher, such as carbamates agriculture
Medicine, and adsorption efficiency is more than 10 times of traditional C18 series；Activated carbon series adsorbent can extensively adsorb Organic substance in water,
Especially coconut husk class activated carbon, microcellular structure is most flourishing in all acticarbons, thus characterization of adsorption is extremely strong, not only may be used
To adsorb Direct acting mutagens in water, non-immediate mutagen in water can also be adsorbed.
Present situation based on prior art, present inventor intends a kind of wide spectrum enrichment of offer and drinks the organic dirt of underwater trace
A kind of method for contaminating thing, and in particular to three kinds of different characterization of adsorptions such as XAD-2, PSDVB and coconut husk class activated carbon that are used in series
Sorbing material, and water sample pH value is fine-tuned, realize that the enrichment method of trace organic pollutant in water is drunk in wide spectrum enrichment.
The content of the invention
It is an object of the present invention to be directed to Organic Pollutants of Drinking Water huge number, it is the characteristics of content is low and existing
Technology lacks the present situation of the organic micro-pollutant beneficiation technologies of wide spectrum, there is provided a kind of efficient, organic micro-pollutant of wide spectrum
Enrichment method, is used in series three kinds of suctions of different characterization of adsorptions such as XAD-2, PSDVB and coconut husk class activated carbon in the inventive method
Enclosure material, and water sample pH value is fine-tuned, realize that the enrichment of trace organic pollutant in water is drunk in wide spectrum enrichment.
In the inventive method, not only enriching apparatus are simple, it is adaptable to which water sample with bulk mass is enriched with, and sorbing material is easy to get simultaneously
Can reuse, can extract that organic pollutant category is numerous, extraction efficiency is high, enrichment capacity is big；What the method was obtained drinks
Water enriched substance can be not only used for Organic Pollutants of Drinking Water analysis of spectrum, be also applied for biological effect research.
The technical solution used in the present invention is：Choose three kinds of sorbing materials such as XAD-2, PS/DVB and coconut husk class activated carbon
Glass column is filled in respectively, is used to be enriched with heterogeneity organic pollution in drinking water after being concatenated design, and have through specific
Preserve stand-by after machine solvent classification wash-out.The method is particularly suitable for continuous extraction water sample up to 40L volumes.
A kind of enrichment method of Organic Pollutants of Drinking Water of the invention, it includes step：
1) filling of solid phase enriching column is activated with adsorbent；
2) solid phase enrichment system is built；
3) loading：Original water sample loading；
4) it is enriched with organic pollution：
5) wash-out and collection enriched substance：
6) concentration and preservation enriched substance ' '
More specifically, a kind of enrichment method of Organic Pollutants of Drinking Water of the invention, its step 1) solid phase enrichment
During the filling of post is activated with adsorbent：Including：
A) appropriate XAD ion exchange macroporous absorbent resins are cleaned and preserved through organic solvent, and lower end pad is transferred to before extraction
Have in the glass column (25cm × 1.5cm.i.d.) of mineral wool, the post bed upper end a small amount of mineral wool of pad, plus 200mL ultra-pure waters rinsing tree
Fat, stays a small amount of ultra-pure water in post, closes glass column lower end knob；
B) appropriate PS/DVB sorbing materials are cleaned and preserved through organic solvent, and lower end is transferred to before extraction with glass core and glass
In the glass column (25cm × 1.5cm.i.d.) of glass cotton, the post bed upper end a small amount of mineral wool of pad, plus the rinsing absorption of 200mL ultra-pure waters
Agent, stays a small amount of ultra-pure water in post, closes glass column lower end knob；
C) proper amount of active carbon is cleaned and preserved through organic solvent, and the glass column that lower end is lined with mineral wool is transferred to before extraction
In (25cm × 1.5cm.i.d.), the post bed upper end a small amount of mineral wool of pad, plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water
Yu Zhuzhong, closes glass column lower end knob；
Its step 2) structure solid phase enrichment system in, including：
The glass column lower end of XAD ion exchange macroporous absorbent resins and a special glass three-way valve inlet will be filled with
End connection, one end connects with wash-out bottle in two ports of export of glass three-way valve, and the other end is connected with a Brown Glass Brown glass bottles and jars only；Brown
Vial bottom is connected by a glass valves with PS/DVB sorbing material glass columns are filled with；The latter is same, special with one
Glass three-way valve inlet end connect, in two ports of export of glass three-way valve one end with elute bottle connect, the other end directly with fill one
The individual glass column connection for being filled with PS/DVB sorbing materials；The latter is same, and the glass three-way valve inlet end special with is connected, glass
One end connects with wash-out bottle in two ports of export of glass triple valve, and the other end is connected with a Brown Glass Brown glass bottles and jars only；Brown glass bottom of bottle
Portion is connected by a glass valves with a glass column for being filled with active carbon adsorption material is filled；The glass column lower end and a spy
System glass three-way valve inlet end connection, in two ports of export of glass three-way valve one end directly with wash-out bottle connect, the other end with
One Brown Glass Brown glass bottles and jars only connection；
Its step 3) loading in：Original water sample is flowed into the glass column of the superiors through siphonage；
Its step 4) enrichment organic pollution in, including：Original water sample is under room temperature (22 ± 2 DEG C) with certain flow rate stream
Through XAD posts, some organic micro-pollutants are adsorbed, and the water sample of filtration enters in Brown Glass Brown glass bottles and jars only, adds salt acid for adjusting pH value
To acidity；Then PS/DVB columnss in series are crossed with certain flow rate through siphonage, some organic micro-pollutants are adsorbed, filtration
Water sample enters in Brown Glass Brown glass bottles and jars only, adds NaOH to adjust pH value to alkalescence；Then made a living with certain flow rate through siphonage
Property charcoal, some organic micro-pollutants be adsorbed；
Its step 5) enriched substance wash-out with collect in, including,
A) wash-out of XAD enriched substances and collection：XAD post appropriate times first are soaked with organic solvent, then with certain flow rate
Wash-out enriched substance, eluent is collected in wash-out bottle X1；Eluted with other organic solvents again, and collect eluent；
B) wash-out of PS/DVB enriched substances and collection：PS/DVB post appropriate times first are soaked with organic solvent, then with one
Constant current speed wash-out enriched substance, eluent is collected in wash-out bottle X2；Eluted with other organic solvents again, and collect eluent；
C) wash-out of preconcentration with activated carbon thing and collection：Activated-charcoal column appropriate time first is soaked with organic solvent, then with one
Constant current speed wash-out enriched substance, eluent is collected in wash-out bottle X3；Eluted with other organic solvents again, and collect eluent；
Its step 6) enriched substance concentration with preserve in, including：All eluents are molten again with methyl alcohol after volatilizing naturally
Solution, nitrogen blows and is concentrated into appropriate volume, be transferred in teat glass, keeps in dark place at low temperature.
In the present invention, the XAD-2 solid phase columns prepare and are with activation：XAD-2 ion exchanges macroporous absorbent resin (20~60
Mesh) 4g cleans 3 times with appropriate ultra-pure water, dichloromethane, normal propyl alcohol, methyl alcohol, is then sealed in methyl alcohol successively.Post bed is upper and lower
End is lined with mineral wool.It is slow to discharge methyl alcohol but do it after resin filling.Plus 200mL ultra-pure waters rinsing resin, stay few
Amount ultra-pure water is in post.
In the present invention, the PS/DVB solid phase columns prepare and are with activation：PS/DVB sorbing materials (100~200 mesh) 4g is used
Proper amount of methanol is cleaned 1 time, is then sealed in methyl alcohol.The post bed upper end a small amount of mineral wool of pad, lower end carries glass core and mineral wool.Inhale
It is slow to discharge methyl alcohol but do it after attached dose of filling.Plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water in post.
In the present invention, the coconut husk class activated carbon solid phase column prepares and is with activation：Coconut husk class activated carbon (20~40 mesh) 2g
Use proper amount of acetone：N-hexane (1:1, V/V) soak 3~4 hours, then methyl alcohol is cleaned 2 times, and is sealed in methyl alcohol.On post bed,
Lower end is lined with mineral wool.It is slow to discharge methyl alcohol but do it after activated carbon filling.Plus 200mL ultra-pure waters rinsing resin,
A small amount of ultra-pure water is stayed in post.
In step (1) of the present invention, XAD-2 types, adsorbent amount, cleaning condition, store method, filling mode and activation
Condition is：XAD-2 ion exchanges macroporous absorbent resin (20~60 mesh) 4g successively with appropriate ultra-pure water, dichloromethane, normal propyl alcohol,
Methyl alcohol is cleaned 3 times, is then sealed in methyl alcohol.Post bed upper and lower end is lined with mineral wool.After resin filling, methyl alcohol is slowly discharged
But can not do it.Plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water in post.
In step (1) of the present invention, PS/DVB types, adsorbent amount, cleaning condition, store method, filling mode and work
Change condition is：PS/DVB sorbing materials (100~200 mesh) 4g is cleaned 1 time with proper amount of methanol, is then sealed in methyl alcohol.Post bed
The a small amount of mineral wool of upper end pad, lower end carries glass core and mineral wool.It is slow to discharge methyl alcohol but do it after adsorbent filling.
Plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water in post.
In step (1) of the present invention, activated carbon types, adsorbent amount, cleaning condition, store method, filling mode and work
Change condition is：Coconut husk class activated carbon (20~40 mesh) 2g proper amount of acetone：N-hexane (1:1, V/V) immersion 3~4 hours, then
Methyl alcohol is cleaned 2 times, and is sealed in methyl alcohol.Post bed upper and lower end is lined with mineral wool.After activated carbon filling, methyl alcohol is slowly discharged
But can not do it.Plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water in post.
In step (2) of the present invention, XAD-2 solid phases packed column and PS/DVB solid phases packed column all pass through a glass three-way valve
It is connected with Brown Glass Brown glass bottles and jars only and wash-out bottle；
In step (2), successively by XAD-2 solid phases packed column, PS/DVB solid phases packed column and coconut husk class activated carbon packed column
Connected；
In step (2), PS/DVB solid phase enriching sections are 2 glass columns of filling 4g PS/DVB of connecting.
In step (4) of the present invention, the water sample filtered through XAD-2 posts adjusts pH value with top pure grade concentrated hydrochloric acid (36%~38%)
To 2~3；
In step (4), the water sample filtered through PS/DVB posts adjusts pH value to 5~7 with top pure grade NaOH.
In step (5) of the present invention, the XAD-2 post 20mL methyl alcohol of water sample was enriched with：Acetone (7:3, V/V) 15 points are soaked
Clock, the organic pollution being then extracted with the flow velocity wash-out of 3~5mL/min simultaneously collects eluent.And repeat aforesaid operations 1
It is secondary.Afterwards, 30mL acetone is used：N-hexane (1:1, V/V) immersion XAD-2 posts 15 minutes, are then washed with the flow velocity of 3~5mL/min
The de- organic pollution being extracted simultaneously collects eluent.Finally, XAD-2 posts are soaked 15 minutes with 45mL dichloromethane, then with 3
The flow velocity organic pollution that is extracted of wash-out of~5mL/min simultaneously collects eluent；
In step (5), the PS/DVB post 20mL methyl alcohol of water sample was enriched with：Ethyl acetate (1:1, V/V) soak 15 minutes,
Then the organic pollution that is extracted with the flow velocity of 3~5mL/min wash-out simultaneously collects eluent.And repeat aforesaid operations 2 times.It
Afterwards, PS/DVB posts are soaked 15 minutes with 20mL n-hexanes, the organic contamination being then extracted with the flow velocity wash-out of 3~5mL/min
Thing simultaneously collects eluent.Finally, soak PS/DVB posts 15 minutes with 20mL dichloromethane, then washed with the flow velocity of 3~5mL/min
The de- organic pollution being extracted simultaneously is collected；
In step (5), the coconut husk class activated-charcoal column 20mL acetone of water sample was enriched with：N-hexane (1:1, V/V) 15 are soaked
Minute, the organic pollution being then enriched with the flow velocity wash-out of 3~5mL/min simultaneously collects eluent.And repeat aforesaid operations 1
It is secondary.Afterwards, coconut husk class activated-charcoal column is soaked 15 minutes with 20mL dichloromethane, it is then rich with the flow velocity wash-out of 3~5mL/min
The organic pollution of collection simultaneously collects eluent.Finally, soak coconut husk class activated-charcoal column 15 minutes with 10mL methyl alcohol, then with 3~
The flow velocity organic pollution that is enriched with of wash-out of 5mL/min simultaneously collects eluent.
In the present invention, all eluates are volatilized naturally in nonpollution environment, for dust pollutes in preventing environment, mouth of pot
Covered with aluminium foil, aluminium foil syringe needle stabs some apertures so that solvent volatilizees.Dry enriched substance is molten again with proper amount of methanol in crucible
Solution, high pure nitrogen is concentrated into lmL, is collected in glass ground joint test tube with 0.lmL/min, and sealing is kept in dark place in one 20 DEG C, 30
GC-MS analyses are completed in it.
The invention provides a kind of enrichment method of Organic Pollutants of Drinking Water.This method by integrated XAD-2,
Three kinds of sorbing materials such as PSDVB and coconut husk class activated carbon, and water sample pH value is fine-tuned, trace in wide spectrum enrichment drinking water can be realized
Amount organic pollution, the enriched substance for being obtained can be not only used for drinking trace organic pollutant in water analysis of spectrum, be also applied for biology
Learn effect study.
The inventive method has the following advantages that：
(1) after the sorbing material of three kinds of different characterization of adsorptions such as XAD-2, PSDVB and coconut husk class activated carbon is connected
For being enriched with water sample organic pollution, it is capable of achieving to be extracted to highly polar organic pollution wide spectrum from nonpolar, low polarity, and to having
Organic pollutants bioaccumulation efficiency is high, and the enriched substance for being obtained can be not only used for Organic Pollutants of Drinking Water analysis of spectrum, is also applied for life
Thing effect study；
(2) this method can be used for water sample with bulk mass, such as 40L water samples, continuous enrichment.
(3) sorbing material used by is easy to get, low cost, and can reuse, with good application value.
In order to make it easy to understand, the experiment of extracting and enriching efficiency, accompanying drawing table and embodiment below with reference to mark-on water sample are to this
The method of the enrichment Organic Pollutants of Drinking Water of invention is specifically explained.It is important to note that instantiation and attached
Chart is merely to explanation, it is clear that one of ordinary skill in the art can be right within the scope of the invention according to illustrating herein
The present invention makes various amendments and change, and these amendments and change are also included in the scope of the present invention.
Brief description of the drawings
Fig. 1 is the flow chart of water sample enrichment and eluent system.
Fig. 2 is that certain water factory dispatches from the factory that to extract sample GC/MS analysis through the difference eluting solvent enrichment of different sorbing materials total for water sample
Ion stream chromatogram；Wherein, JCBT- methyl alcohol:Acetone (7:3,v/v)；BTZJW- acetone:N-hexane (1:1,v/v)；ELJW- bis-
Chloromethanes；JCYSYZ- methyl alcohol:Ethyl acetate (1:1,v/v)；ZJW- n-hexanes；JC- methyl alcohol；YC- ethanol.
Specific embodiment
Embodiment 1
The simulation extraction ability test experiments of the inventive method：Two parts of collection Milli-Q ultra-pure waters 40L, is separately added into 20 μ
G target chemical substancess include 34 kinds of pesticides, 8 kinds of phthalates and adipic acid classes, 6 kinds of ethers, 4 kinds of phenols, more than 9 kinds
Volatility or the half volatile organic contaminants such as chlordiphenyl class, 16 kinds of multiring aromatic hydrocarbons, 4 kinds of amines.GC/MS uses full scan side
Formula carries out qualitative analysis；Retrieval spectrum storehouse：U.S. NIST standard spectrums storehouse；Using the extraction Quality Map spectral peak of every kind of material quota ion
Area, according to corresponding regression equation calculation gained concentration；
Laboratory method blank analysis：Identical Milli-Q ultra-pure waters 40L is gathered, using mutually the same with above-mentioned mark-on water sample
Treatment and GC/MS are analyzed, and detect background values；The purpose is to determine whether experimental situation, reagent and analytical instrument etc. draw
Enter target contaminant；
Bioaccumulation efficiency of the enrichment method to target compound：By XAD-2, PSDVB and three kinds of adsorption materials of coconut husk class activated carbon
The extracting and enriching system that material is composed in series is as shown in table 1 to the bioaccumulation efficiency of every kind of target compound；51 kinds of target compounds are inhaled
Attached good, bioaccumulation efficiency is more than 60%；5 kinds of target compound bioaccumulation efficiencies are between 40%~60%；Only 25 kinds target chemical combination
Thing bioaccumulation efficiency is less than 40%；
The judgement of enrichment system overload：To judge that enrichment system whether there is to overload problem, super to 40LMilli-Q
After 20 μ g target substance levels are added in pure water, by by the outflow water sample after XAD-2, PSDVB and coconut husk class preconcentration with activated carbon
Repeat carries out identical enrichment procedure through XAD-2, PSDVB and coconut husk class activated carbon extraction enrichment system, and is washed by identical
De- program elutes each adsorbent, and the eluent of collection is analyzed using identical GC/MS conditions, as a result as shown in table 2；This is
System does not exist overload problem to all target compounds.
Concrete application case：Certain city tap-water factory dispatches from the factory trace organic pollutant in water analysis of spectrum
The Shanghai City water factory output water 40L with Water of Huangpu River as water source is gathered, by means of the siphonage mistake of siphoning installation
4gXAD-2 adsorption columns, flow control is in 15-20mL/min；Appropriate 36-38% salt is added in water to excessively complete XAD-2 adsorption columns
Sour (top pure grade), 2~3 are adjusted to by water sample pH, and then the siphonage by means of siphoning installation crosses two 4gPS/DVB posts successively；To mistake
Appropriate sodium hydroxide solution is added in the water of complete PS/DVB adsorption columns, water sample pH is adjusted to 5~7, then by means of siphoning installation
Siphonage crosses 2g coconut husk class activated-charcoal columns, and the organic matter being enriched with adsorbent with eluting solvent respectively is with 3~5mL/min flow velocitys
Wash-out, eluent is volatilized naturally in crucible, and methyl alcohol is molten again, and nitrogen concentration is settled to 1mL, and -20 DEG C of sealings are kept in dark place.Every time
Instrument tuning, continuous calibration, method blank and solvent blank are carried out before sample GC/MS analyses, trace organic substance about 43 can be detected
Kind, as shown in Fig. 2 belonging to China《Standards for drinking water quality》(GB5749-2006) category has 8 kinds；
Bioaccumulation efficiency (Duplicate Samples) of the enrichment system of table 1 (XAD-2, PSDVB, activated carbon) to each target compound
The enrichment system of table 2 overload judges (Duplicate Samples)
In the above-mentioned enrichment performance test for the inventive method, trace that may be present in 81 kinds of water bodys is only have selected
Organic pollution does not represent this method and is only limitted to this 81 kinds of organic pollutions as goal in research compound, any to be familiar with
Professional and technical personnel, without departing from the scope of the present invention, does some when using the technology contents of above-mentioned elaboration
The Equivalent embodiments of equivalent variations are changed or are modified to, as long as being without departing from the technology of the present invention content and plan content, according to this
The technical spirit of invention, any simple modification, equivalent variations and the modification made to above-described embodiment, belongs to the inventive method
In the range of scheme.
Claims (21)
1. a kind of enrichment method of Organic Pollutants of Drinking Water, it is characterised in that it includes step,
1) filling of solid phase enriching column is activated with adsorbent；
2) solid phase enrichment system is built；
3) loading：Original water sample loading；
4) it is enriched with organic pollution：
5) wash-out and collection enriched substance：
6) concentration and preservation enriched substance.
2. the method as described in claim 1, it is characterised in that described step 1) include,
The glass column lower end of the XAD ion exchange macroporous absorbent resins glass three-way valve inlet end company special with will be filled with
Connect, one end is directly connected with a Brown Glass Brown glass bottles and jars only in two ports of export of glass three-way valve, the other end connects with wash-out bottle；From palm fibre
Color vial is derived a glass interface and is connected with 2 series connection glass columns for being filled with PS/DVB sorbing materials respectively, glass column
The lower end glass three-way valve inlet end special with is connected, in two ports of export of glass three-way valve one end directly with a brown
Vial is connected, and the other end connects with wash-out bottle in two ports of export of glass three-way valve；A glass is derived from Brown Glass Brown glass bottles and jars only
Interface is connected with the glass column for being filled with active carbon adsorption material, and glass column lower end connects with wash-out bottle；
Described step 2) include,
A) appropriate XAD ion exchange macroporous absorbent resins are cleaned and preserved through organic solvent, lower end is transferred to before extraction and is lined with glass
In the glass column of glass cotton, the post bed upper end a small amount of mineral wool of pad, plus ultra-pure water rinsing resin, a small amount of ultra-pure water is stayed in post, close
Glass column lower end knob；
B) appropriate PS/DVB sorbing materials are cleaned and preserved through organic solvent, and lower end is transferred to before extraction with glass core and mineral wool
Glass column in, the post bed upper end a small amount of mineral wool of pad, plus ultra-pure water rinsing adsorbent stays a small amount of ultra-pure water in post, closing glass
Glass post lower end knob.
C) proper amount of active carbon is cleaned and preserved through organic solvent, lower end is transferred to before extraction and is lined with the glass column of mineral wool, post
The bed upper end a small amount of mineral wool of pad, plus ultra-pure water rinsing resin, stay a small amount of ultra-pure water in post, close glass column lower end knob；
Described step 3) in,：Original water sample is flowed into glass column B1 through siphonage；
Described step 4) include, original water sample flows through XAD-2 posts, organic micro-pollutant quilt with certain flow rate at room temperature
Absorption, the water sample of filtration enters in Brown Glass Brown glass bottles and jars only, adds salt acid for adjusting pH value to acidity；Then through siphonage with a constant current
Speed crosses PS/DVB columnss in series, and organic micro-pollutant is adsorbed, and the water sample of filtration enters in Brown Glass Brown glass bottles and jars only, adds NaOH
Adjust pH value to alkalescence；Then activated carbon is crossed with certain flow rate through siphonage, organic micro-pollutant is adsorbed；
Described step 5) include,
A) wash-out of XAD enriched substances and collection：XAD post appropriate times first are soaked with organic solvent, is then eluted with certain flow rate
Enriched substance, eluent is collected in wash-out bottle X1；Eluted with other organic solvents again, and collect eluent；
B) wash-out of PS/DVB enriched substances and collection：PS/DVB post appropriate times first are soaked with organic solvent, then with a constant current
Speed wash-out enriched substance, eluent is collected in wash-out bottle X2；Eluted with other organic solvents again, and collect eluent；
C) wash-out of preconcentration with activated carbon thing and collection：Activated-charcoal column appropriate time first is soaked with organic solvent, then with a constant current
Speed wash-out enriched substance, eluent is collected in wash-out bottle X3；Eluted with other organic solvents again, and collect eluent；
Described step 2) include, all eluents are redissolved after volatilizing naturally with methyl alcohol, and nitrogen blows and is concentrated into appropriate volume,
It is transferred in teat glass, keeps in dark place at low temperature.
3. method according to claim 1, it is characterised in that：Three kinds of sorbing material quilts such as XAD-2, PS/DVB and activated carbon
Glass column is filled in respectively, is used to be enriched with heterogeneity organic micro-pollutant in drinking water after being concatenated design, and through specific
Preserve stand-by after organic solvent wash-out.
4. the method according to claim 1 or 2 or 3, it is characterised in that：Step 1) described in adsorbent type, adsorbent
Consumption, cleaning condition, store method, filling mode and activation condition are as follows respectively：
A) the mesh 4g of XAD-2 ion exchanges macroporous absorbent resin 20~60 is successively with appropriate ultra-pure water, dichloromethane, normal propyl alcohol, first
Alcohol is cleaned 3 times, is then sealed in methyl alcohol, and post bed upper and lower end is lined with mineral wool.After resin filling, slow discharge methyl alcohol but
Can not do it, plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water in post；
B) the mesh 4g of PS/DVB sorbing materials 100~200 is cleaned 1 time with proper amount of methanol, is then sealed in methyl alcohol.Post bed upper end pad
A small amount of mineral wool, lower end carries glass core and mineral wool.It is slow to discharge methyl alcohol but do it after adsorbent filling, plus 200mL
Ultra-pure water rinses resin, stays a small amount of ultra-pure water in post；
C) the mesh 2g proper amount of acetone of coconut husk class activated carbon 20~40：N-hexane 1:1, V/V immersion 3~4 hours, then methyl alcohol cleaning
2 times, and be sealed in methyl alcohol, post bed upper and lower end is lined with mineral wool, slow to discharge methyl alcohol but make after activated carbon filling
It is done,.Plus 200mL ultra-pure waters rinsing resin, stay a small amount of ultra-pure water in post.
5. the method according to claim 1 or 2 or 3, it is characterised in that：Step 2) in XAD-2 solid phases enriching column and PS/
DVB solid phases enriching column is connected by a glass three-way valve with Brown Glass Brown glass bottles and jars only and wash-out bottle.
6. the method according to claim 1 or 2 or 3, it is characterised in that：Step 2) in successively by XAD-2 solid phases enriching column,
PS/DVB solid phases enriching column and coconut husk class preconcentration with activated carbon post are connected.
7. the method according to claim 1 or 2 or 3, it is characterised in that：Step 2) in PS/DVB solid phases enriching section for string
2 glass columns of filling 4g PS/DVB of connection.
8. the method according to claim 1 or 2 or 3, it is characterised in that：Step 4) in through XAD-2 posts filter water sample use
Top pure grade concentrated hydrochloric acid 36%~38% adjusts pH value to 2~3.
9. the method according to claim 1 or 2 or 3, it is characterised in that：Step 4) in through PS/DVB posts filter water sample use
Top pure grade NaOH adjusts pH value to 5~7.
10. the method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in extracted water sample XAD-2 posts use
20mL methyl alcohol：Acetone 7:3, V/V immersions 15 minutes, then elute the organic pollution being extracted simultaneously with the flow velocity of 3~5mL/min
Collect.And repeat aforesaid operations 1 time.
11. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in through methyl alcohol：Acetone 7:3, V/V wash
The XAD-2 post 30mL acetone for taking off：N-hexane 1:1, V/V immersion 15 minutes, then elutes quilt with the flow velocity of 3~5mL/min
The organic pollution of extraction is simultaneously collected.
12. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in through acetone：N-hexane 1:1,V/V
The XAD-2 post 45mL dichloromethane for stripping soaks 15 minutes, then with having that the flow velocity wash-out of 3~5mL/min is extracted
Organic pollutants are simultaneously collected.
13. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in be enriched with the PS/DVB posts of water sample
Use 20mL methyl alcohol：Ethyl acetate 1:1, V/V immersion 15 minutes, the organic dirt being then enriched with the flow velocity wash-out of 3~5mL/min
Dye thing is simultaneously collected.And repeat aforesaid operations 2 times.
14. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in through methyl alcohol：Ethyl acetate 1:1,V/
The PS/DVB post 20mL n-hexanes that V is stripped soak 15 minutes, then with having that the flow velocity wash-out of 3~5mL/min is enriched with
Organic pollutants are simultaneously collected.
15. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in the PS/ that is stripped through n-hexane
DVB posts 20mL dichloromethane soaks 15 minutes, then elutes the organic pollution being enriched with simultaneously with the flow velocity of 3~5mL/min
Collect.
16. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in be enriched with water sample coconut husk class live
Property charcoal post 20mL acetone：N-hexane 1:1, V/V immersion 15 minutes, then with having that the flow velocity wash-out of 3~5mL/min is enriched with
Organic pollutants are simultaneously collected.And repeat aforesaid operations 1 time.
17. method according to claim 1 or 1 or 2 or 3, it is characterised in that：Step 5) in through acetone：N-hexane 1:1,
The coconut husk class activated-charcoal column 20mL dichloromethane that V/V is stripped soaks 15 minutes, is then eluted with the flow velocity of 3~5mL/min
The organic pollution that is extracted simultaneously is collected.
18. method according to claim 1 or 2 or 3, it is characterised in that：Step 5) in the coconut palm that is crossed through dichloromethane eluent
Shell class activated-charcoal column 10mL methyl alcohol soaks 15 minutes, the organic pollution being then extracted with the flow velocity wash-out of 3~5mL/min
And collect.
19. method according to claim 1 or 2 or 3, it is characterised in that：It is nonpolar and low in XAD-2 adsorbents absorption water
Polarity organic pollution, including it is organophosphorus pesticide, organo-chlorine pesticide, triazine, plan worm chrysanthemum ester agricultural chemicals, phenols, polycyclic
Aromatic hydrocarbons, phthalate, polychlorinated biphenyl, hormone and chemical substance in bactericide.
20. method according to claim 1 or 2 or 3, it is characterised in that：PS/DVB adsorbents effectively adsorb polarity in water
Stronger organic pollution includes moieties in phenols, multiring aromatic hydrocarbon, adipic acid class.
21. method according to claim 1 or 2 or 3, it is characterised in that：The coconut husk class acticarbon is inhaled extensively
Attached organic pollutants include multiring aromatic hydrocarbon, organophosphorus pesticide, organo-chlorine pesticide, phthalate, amine, sterol
Moieties in class.
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| CN113694885A (en) * | 2021-07-20 | 2021-11-26 | 红河学院 | Biological activated carbon-loaded hydroxyapatite composite material and application method thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108956917A (en) * | 2018-06-11 | 2018-12-07 | 安徽省佳逸环保科技有限公司 | A method of Organic Pollutants In Water concentration is detected using polymer absorbant |
| CN108956917B (en) * | 2018-06-11 | 2021-06-22 | 安徽省佳逸环保科技有限公司 | Method for detecting concentration of organic pollutants in water body by using polymer adsorbent |
| CN108837816A (en) * | 2018-07-16 | 2018-11-20 | 未名环境分子诊断（常熟）有限公司 | A kind of adsorbent material for acquisition polarity organic pollutant in water environment passive sampling |
| CN108837816B (en) * | 2018-07-16 | 2020-11-20 | 未名环境分子诊断（常熟）有限公司 | Adsorbing material for collecting polar organic pollutants in passive sampling of water environment |
| CN112014490A (en) * | 2019-05-31 | 2020-12-01 | 中国石油化工股份有限公司 | Method for separating and analyzing hydrocarbon components in hydrocarbon fuel |
| CN112014490B (en) * | 2019-05-31 | 2022-06-28 | 中国石油化工股份有限公司 | Method for separating and analyzing hydrocarbon components in hydrocarbon fuel |
| CN113694885A (en) * | 2021-07-20 | 2021-11-26 | 红河学院 | Biological activated carbon-loaded hydroxyapatite composite material and application method thereof |
| CN113694885B (en) * | 2021-07-20 | 2023-07-18 | 红河学院 | Biological active carbon loaded hydroxyapatite composite material and application method thereof |
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