CN105148847B - A kind of easily dynamic heavy metal adsorption combination phase gel mould and preparation method thereof - Google Patents
A kind of easily dynamic heavy metal adsorption combination phase gel mould and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of easily dynamic heavy metal adsorption combination phase gel mould and preparation method thereof, (1) by sulfhydryl modified sepiolite particle and acrylamide gel solution by weight 1:5~1:10 mix, and absolute ethyl alcohol is added after stirring makes sulfhydryl modified sepiolite particle be uniformly dispersed；(2) 10% ammonium persulfate solution and tetramethylethylenediamine are added in mixed solution obtained above；(3) suspension is rapidly injected in glass guide channel after low temperature ultrasonic 13 minutes, is covered with glass cover-plate and be transferred to 4 10 DEG C of low temperature incubator cultures 20 40 minutes, constant temperature and humidity incubator is moved to after culture and cultivates 1h under the conditions of 42 DEG C.Gel mould provided by the invention can not only have higher adsorbance, more preferable dissociation effect with heavy metal Cu, Zn, Pb, Cd, Ni, Fe, Mn, Al, Hg etc., and material therefor is cheap and easy to get, be advantageous to popularization and application of the DGT technologies in China.
Description
Technical field
The present invention relates to be applied to film gradient in the surrounding medium A+E such as a kind of water body, soil and deposit
Combination phase gel mould of diffusion technique (Diffusive gradients in thin films, DGT) and preparation method thereof, especially
It is a kind of based on the DGT combination phase preparation methods that sulfhydryl modified sepiolite is easy dynamic heavy-metal adsorption material.
Background technology
With the rapid development of industrialization and urbanization, heavy metal pollution of soil turns into the protrusion environment that can not be ignored and asked
Topic.China arable land is extremely serious by heavy metal pollutions such as Cd, As, Pb, Hg, Zn.It not only produces harm to ecological environment, influences
Biological growth and development, but also human body can be entered by food chain, jeopardize existence and the health of the mankind.Cadmium rice, arsenic poison,
The heavy metal pollutions such as blood lead endanger common in recent years all reports, " minamata disease " and " Itai-itai diseases " be ascertained respectively by heavy metal Hg with
Cd pollutions cause, and heavy metal pollution problem causes the common concern of countries in the world.Toxicity master of the heavy metal contaminants to biology
Its occurrence patterns rather than total amount are depended on, so the biologically effective state content of heavy metal can be effective in measure soil media
Ground is monitored to heavy metal in environment.
DGT technologies are film diffusion (the Diffusive gradients in thin- based on Fick's first law
Films, DGT) technology.It is a kind of new passive sampling technology in situ, can be enriched with monitored material, and can be according to monitored
The available state concentration of the material in the enriching quantity quantitative determination environment of material, is that element morphology ideal at present is gathered and divided
The method of analysis.The core of the technology mainly mutually and with reference to phase two parts is made up of diffusion, and diffusion is mutually the quantitative base of DGT technologies
Plinth, the effect with reference to phase are that coordination diffuses through the ion come, make diffusion phase with reducing to minimum with reference to alternate concentration of metal ions.
With reference to the functional group that can provide coordinated electronic in mutually its molecular structure containing some, these functional groups can send out with heavy metal ion
Raw complexation reaction, by by diffusion barrier diffuse through come adsorption of metal ions on its surface.It is but selected in traditional DGT technologies
There is the problems such as price is high, hardly possible is bought, versatility is bad and measurement effect is bad in combination phase material, causing can not be extensive
Ground carries out popularization and application.
The content of the invention
Present invention aims to overcome that in place of the deficiencies in the prior art, there is provided a kind of easily dynamic heavy metal adsorption combination is mutually coagulated
The preparation method of glued membrane, it is that one kind based on sulfhydryl modified sepiolite is easy dynamic heavy-metal adsorption material, sulfydryl of the invention changes
Property sepiolite combination phase gel mould can not only easily distinguish positive and negative, and may also reach up the height of heavy metal available state
Adsorbance, and there is the characteristics of cheap, to be easy to get, easily promote.
The present invention realizes that the technical scheme of purpose is：
A kind of easily dynamic heavy metal adsorption combination phase gel mould, by DGT technologies by spread mutually diffuse through come a huge sum of money
Category ion is rapidly adsorbed on its surface.It is characterized in that：The material for capturing heavy metal ion is sulfhydryl modified sepiolite, passes through third
Gel mould is made in sulfhydryl modified sepiolite powder by acrylamide gel solution.
By sulfhydryl modified sepiolite particle and acrylamide gel solution by weight 1:5~1:10 mix, then by volume
Than V (absolute ethyl alcohol)：V (acrylamide gel)=7:500, V (ammonium persulfates)：V (acrylamide gel)=3:500 add respectively
Enter absolute ethyl alcohol and 10% (g/100ml) ammonium persulfate solution, tetramethylethylenediamine (TEMED), volume V are added after mixing
(TEMED):V (acrylamide gel)=3:2000.Suspension is rapidly injected after low temperature ultrasonic 1-3 minutes certain thickness
In glass guide channel, it is about that 0.25mm non-solubility solid colorfuls haydite is used to indicate gel positive and negative then to add several particle diameters, it
Constant temperature and humidity incubator is moved to after 4-10 DEG C of low temperature incubator culture 20-40 minute is transferred to after being covered afterwards with glass cover-plate
1h is cultivated under the conditions of 42 DEG C.Then take out and be placed in ultra-pure water, gel is taken out after 30 minutes, water is changed in 24 hours at least three times
DGT combination phases are made.The combination prepared is mutually cut into the shape of needs, assembling and analysis for DGT determination techniques.
Described sulfhydryl modified sepiolite particle is that top pure grade sepiolite is scattered in deionized water, forms sepiolite and hangs
Turbid；Then sepiolite suspension is put on dispersion machine, with 12000 revs/min of speed high-speed stirred 5-10 minutes, formed
Sepiolite gel；And mercaptopropyl trimethoxysilane is added into sepiolite gel under the conditions of high-speed stirred, continue high-speed stirring
Mix to form sulfydryl modification sepiolite gel rubber system；By gel rubber system at 80 DEG C constant temperature 24-36 hours；Finally by gel from system
Middle taking-up, dried under the conditions of 65 DEG C, sulfydryl modification sepiolite particle is obtained after grinding.
A kind of easily dynamic heavy metal adsorption combination phase gel mould, sulfhydryl modified sepiolite is uniform-distribution with gel mould
Grain, the preparation method of the sulfhydryl modified sepiolite particle are：
(1) the acidification of sepiolite：Natural sepiolite is put in 15% HCl and soaks 24h-48h, is rushed with MQ water
It is washed till pH value no longer to change, obtains the sepiolite of top pure grade；
(2) grafting is handled：The top pure grade sepiolite of purification is scattered in deionized water, forms sepiolite suspension；
(3) sepiolite suspension, with 12000 revs/min of speed high-speed stirred 5-10 minutes, forms sea on dispersion machine
Afrodite gel；And mercaptopropyl trimethoxysilane is added into sepiolite gel under the conditions of high-speed stirred, continue high-speed stirred
Form sulfydryl modification sepiolite gel rubber system；
By gel rubber system at 80 DEG C constant temperature 24-36 hours；Finally gel is taken out from system, under the conditions of 65 DEG C
Drying, sulfydryl modification sepiolite is obtained after grinding.
A kind of preparation method of easily dynamic heavy metal adsorption combination phase gel mould, step are as follows：
(1) by sulfhydryl modified sepiolite particle and acrylamide gel solution by weight 1:5~1:10 mix, after stirring
Adding absolute ethyl alcohol makes sulfhydryl modified sepiolite particle be uniformly dispersed；
(2) 10% ammonium persulfate solution and tetramethylethylenediamine added in the mixed solution of above-mentioned system；
(3) suspension is rapidly injected in glass guide channel after low temperature ultrasonic 1-3 minutes, is covered with glass cover-plate and be transferred to 4-
10 DEG C of low temperature incubator culture 20-40 minutes, constant temperature and humidity incubator is moved to after culture and cultivates 1h under the conditions of 42 DEG C；
(4) take out and be placed in ultra-pure water after constant temperature and humidity culture terminates, take out gel after placing 30 minutes, changed in 24 hours
DGT combination phases are at least made in water three times；
Moreover, acrylamide gel solution acrylamide containing 15wt% and 0.3wt% crosslinking agents.
Moreover, the acrylamide gel solution manufacturing method is：Gel cross-linkage agent is soluble in water, water is added afterwards,
Mixture is shaken up, weighs acrylamide, is dissolved in water, forms acrylamide solution, by acrylamide solution and crosslinking
Agent mixes together, shakes up and produces；By crosslinking agent：Weight ratio=1 of water：50 is soluble in water by gel cross-linkage agent, afterwards according to
Crosslinking agent：Weight ratio=1 of water：158 add water, crosslinking agent：Weight ratio=1 of acrylamide：50, acrylamide：The weight of water
Measure ratio=1：2.5.
Moreover, the preparation method of the crosslinking agent is：The molten solution into boiling water of agarose is kept for 80 DEG C；By sodium borohydride
It is dissolved in 3.5mol/L sodium hydroxide solution, then adds above-mentioned agarose solution and be stirred continuously；10wt% is added after 30min
Sodium hydroxide solution, allyl glycidyl ether is added dropwise in 15min, reacts 1h, 60 DEG C is cooled to, with 4mol/L vinegar
Acid modulation is neutral, is cleaned with acetone, is put in vacuum drying chamber, dries, grind under the conditions of 60 DEG C；The agarose:The weight of boiling water
Measure ratio=1:49, sodium borohydride:Weight ratio=10 of agarose：599, sodium hydroxide:Sodium borohydride weight=5：6；Hydroxide
Sodium solution:Boiling water volume ratio=10:49, allyl glycidyl ether:Volume ratio=5 of boiling water:98.
Moreover, described sulfhydryl modified sepiolite is to be scattered in by purified sepiolite in deionized water, Hai Pao is formed
Stone suspension；Then sepiolite suspension is put on dispersion machine, with 12000 revs/min of speed high-speed stirred 5-10 minutes,
Form sepiolite gel；And mercaptopropyl trimethoxysilane is added into sepiolite gel under the conditions of high-speed stirred, continue high
Speed stirring forms sulfydryl modification sepiolite gel rubber system；By gel rubber system at 80 DEG C constant temperature 24-36 hours；Finally by gel from
Take out in system, dried under the conditions of 65 DEG C, sulfydryl modification sepiolite is obtained after grinding.
Moreover, the absolute ethyl alcohol：Acrylamide gel liquor capacity ratio is 7:500.
Moreover, the ammonium persulfate solution：Acrylamide gel liquor capacity ratio is 3:500；The tetramethylethylenediamine:
Acrylamide gel liquor capacity ratio is 3:2000.
Moreover, it is about 0.25mm non-solubility solid colorful haydites that several particle diameters are added in the glass guide channel of the step (3)
For indicating gel positive and negative, covered again with glass cover-plate afterwards.
The advantages and positive effects of the present invention are：
1st, gel mould provided by the invention can not only have more with heavy metal Cu, Zn, Pb, Cd, Ni, Fe, Mn, Al, Hg etc.
High adsorbance, more preferable dissociation effect, and material therefor is cheap and easy to get, is advantageous to popularization and application of the DGT technologies in China.
Gel mould provided by the invention is especially suitable for the extraction detection for doing mercury, and gel mould can not be used made of chelex100 resins
In easy dynamic Hg extraction.
2nd, the sulfydryl (- HS) in the sulfhydryl modified sepiolite of main sorbing material in gel mould provided by the invention can be inhaled
Attached heavy metal ion, stronger complexing occurs with heavy metal ion, complex compound is stablized to obtain in generation.By sulfhydryl modified sepiolite
As the heavy metal available state in DGT combination phase material determination of the environment, comparatively ideal effect can be reached.
3rd, gel mould provided by the invention overcomes traditional combination using sulfhydryl modified sepiolite as DGT combination phase materials
The shortcomings of phase material price is high, hardly possible is bought, poor universality and adsorption effect are bad.
4th, the absorption raw material of gel mould provided by the invention is the sepiolite of lighter in weight, by accompanying drawing 1 as can be seen that sea
Afrodite be distributed in gel more uniformly, the proportion of existing sorbing material is larger, the distribution in gel mould be extremely difficult to as
This is uniform, on the one hand uneven consequence influences accuracy of detection, on the one hand the adsorbance of reduction film, and the lightweight of the application offer
Sepiolite overcomes these shortcomings well, reaches optimal Detection results.
5th, the gel mould that the application provides adds sepiolite dispersant absolute ethyl alcohol in preparation process, and applicant is making
Attempted to be added without the case of absolute ethyl alcohol at the beginning of standby, it is found that sepiolite can condense together, it is impossible to disperseed in gel mould, effect
Fruit is undesirable；Other dispersants were also attempted in application, using the alcohols of different carbon chain lengths, it is found that its dispersion effect is bad,
The alcohols even having can also influence the polymerization of gel, and the absorption of heavy metal is also poor, therefore the present invention recommends nothing
Water-ethanol.
6th, the gel mould that the application provides uses top pure grade Hai Pao, sepiolite has been carried out into acidification, after processing
PH to sepiolite is stable, and acidified sepiolite can remove metal impurities therein (content is few) completely, effectively
Ensure the accuracy of testing result.
Brief description of the drawings
Fig. 1-1 is the cross section of sulfhydryl modified sepiolite combination phase gel under microscope, it can be seen that sulfhydryl modified modification
Sepiolite particle is deposited in the side with reference to phase gel entirely；
Fig. 1-2 is the studded one side of sulfydryl combination phase gel, it can be seen that sulfhydryl modified sepiolite particle distribution is equal
Even densification；
Fig. 2-1 and Fig. 2-2 is the combination phase gel mould under microscope.Wherein Fig. 2-1 is to be covered with sulfhydryl modified sepiolite
The one side of grain, it can be seen that particle is uniformly distributed in the side.And Fig. 2-2 be backwards to studded one side, by with figure
Whether it is studded one side that the definition of 2-1 contrast addition colored ceramic particles can clearly be told.
Embodiment
Embodiments of the invention are described in detail below, it is necessary to which explanation, the present embodiment is narrative, is not limited
, it is impossible to protection scope of the present invention is limited with this.
A kind of preparation method of easily dynamic heavy metal adsorption combination phase gel mould, step are as follows：
First, prepared by modified agarose
In the molten boiling water to 490ml of 10g agaroses, solution is kept for 80 DEG C.1.67g sodium borohydrides are dissolved in 3.5mol/L
10ml sodium hydroxide solution, then add above-mentioned agarose solution and be stirred continuously.100ml 10% hydrogen-oxygen is added after 30min
Change sodium solution.25ml allyl glycidyl ethers are added dropwise in 15min, react 1h.60 DEG C are cooled to, with 4mol/L acetic acid
Modulation is neutral.Cleaned 5 times with acetone, be put in vacuum drying chamber, dry, grind under the conditions of 60 DEG C.
2nd, the preparation of acrylamide gel solution
1.8g gel cross-linkages agent (modified agarose) is weighed, is dissolved in 90ml water, adds 285mlMQ water afterwards, will
Mixture shakes up.90g acrylamides are weighed, are dissolved in 225ml water, acrylamide solution are formed, by acrylamide solution
Mix, shake up with said mixture, be stored in standby in 4 DEG C of refrigerators.
3rd, the preparation of sulfhydryl modified sepiolite
Top pure grade sepiolite is scattered in deionized water, forms sepiolite suspension；Then sepiolite suspension is dividing
Dissipate on machine, with 12000 revs/min of speed high-speed stirred 5-10 minutes, form sepiolite gel；And under the conditions of high-speed stirred
Mercaptopropyl trimethoxysilane is added into sepiolite gel, continues high-speed stirred and forms sulfydryl modification sepiolite gel rubber system；
By gel rubber system at 80 DEG C constant temperature 24-36 hours；Finally gel is taken out from system, dried under the conditions of 65 DEG C, is ground
Obtain sulfydryl modification sepiolite afterwards.
Sepiolite used is top pure grade, and molecular structure belongs to 2:1 layer of chain transiens structure, chemical formula：Mg8(H2O)4
[Si6O16]2(OH)4·8H2O.Its preparation method concretely comprises the following steps：(1) acidification of sepiolite.By natural sepiolite (mark
Quasicrystal chemical formula：Mg8(H2O)4[Si6O16]2(OH)4·8H2O) it is put in 15% HCl and soaks 24h-48h, is rinsed with MQ water
No longer change to pH value, obtain the sepiolite of top pure grade；(2) grafting is handled.The sepiolite (top pure grade) of purification is scattered in
In ionized water, sepiolite suspension is formed；Then sepiolite suspension is on dispersion machine, with 12000 revs/min of speed at a high speed
5-10 minutes are stirred, form sepiolite gel；And mercapto propyl group trimethoxy is added into sepiolite gel under the conditions of high-speed stirred
Base silane, continue high-speed stirred and form sulfydryl modification sepiolite gel rubber system；By gel rubber system, constant temperature 24-36 is small at 80 DEG C
When；Finally gel is taken out from system, dried under the conditions of 65 DEG C, sulfydryl modification sepiolite is obtained after grinding.It is described to adopt
Sulfhydryl modified sepiolite is that the grafting modified mesh sieve particle diameter of mistake 200 of mercaptopropyl trimethoxysilane is small after sour purification process
In 74 μm of fine grained.
4th, the preparation of the DGT combination phases of easy dynamic heavy-metal adsorption material
By sulfhydryl modified sepiolite particle and acrylamide gel solution by weight 1:5~1:10 mix, and are sufficiently stirred
Particle is set to be uniformly dispersed after adding absolute ethyl alcohol afterwards, V (absolute ethyl alcohol)：V (acrylamide gel)=7:500.Then add
10% (g/100ml) ammonium persulfate solution, volume are V (ammonium persulfate)：V (acrylamide gel)=3:500；And add four
Methyl ethylenediamine (TEMED), volume are V (TEMED):V (acrylamide gel)=3:2000.After low temperature ultrasonic 1-3 minutes
Suspension is rapidly injected in certain thickness glass guide channel, it is about 0.25mm non-solubility solid colorfuls then to add several particle diameters
Haydite is used to indicate gel positive and negative, and 4-10 DEG C of low temperature incubator culture 20-40 minute is transferred to after being covered afterwards with glass cover-plate
Constant temperature and humidity incubator is moved to afterwards cultivates 1h under the conditions of 42 DEG C.Then take out and be placed in ultra-pure water, taken after 30 minutes
Go out gel, water is changed in 24 hours DGT combination phases are at least made three times.
DGT combination phases prepare instantiation：The sulfhydryl modified sepiolites of 1g are weighed, are put it into beaker, add 10ml
Acrylamide gel solution, is uniformly mixed with glass bar.Blend compounds head dropper adds 140 μ l absolute ethyl alcohols, changes sulfydryl
Property sepiolite particle fully scatters in gel solution.Then add 10% ammonium persulfate solution and 15 μ l tetramethyls that 60 μ l now match somebody with somebody
Base ethylenediamine (TEMED), is stirred continuously, and suspension is rapidly injected into certain thickness glass guide channel after low temperature ultrasonic 1-3 minutes
Interior, it is about that 0.25mm non-solubility solid colorfuls haydite is used to indicate gel positive and negative then to add several particle diameters, uses glass afterwards
Glass cover plate is moved to constant temperature and humidity incubator in 42 DEG C after 4-10 DEG C of low temperature incubator culture 20-40 minute is transferred to after covering
Under the conditions of cultivate 1h.Then take out and be placed in ultra-pure water, gel is taken out after 30 minutes, water is changed in 24 hours and is at least made three times
DGT combination phases.
(4) the image of obtained sulfydryl combination phase gel mould under the microscope is shown in Fig. 1-2, the sulfhydryl modified sea in its surface
Afrodite even particle distribution is fine and close, and particle diameter is less than 74 μm.
5th, elute
The elution process for combining the combination phase gel mould of heavy metal is：Using 3M HNO3Elution 24 hours, eluting rate reaches
80%.
Claims (5)
- A kind of 1. preparation method of easily dynamic heavy metal adsorption combination phase gel mould, it is characterised in that：Step is as follows：(1) by sulfhydryl modified sepiolite particle and acrylamide gel solution by weight 1:5~1:10 mix, and are added after stirring Absolute ethyl alcohol makes sulfhydryl modified sepiolite particle be uniformly dispersed；(2) 10% ammonium persulfate solution and tetramethylethylenediamine added in the mixed solution of above-mentioned system；(3) suspension is rapidly injected in glass guide channel after low temperature ultrasonic 1-3 minutes, is covered with glass cover-plate and be transferred to 4-10 DEG C Low temperature incubator culture 20-40 minutes, constant temperature and humidity incubator is moved to after culture and cultivates 1h under the conditions of 42 DEG C；(4) take out and be placed in ultra-pure water after constant temperature and humidity culture terminates, take out gel after placing 30 minutes, water is changed in 24 hours extremely It is few that DGT combination phases are made three times；The preparation method of the sulfhydryl modified sepiolite particle is：(1) the acidification of sepiolite：Natural sepiolite is put in 15% HCl and soaks 24h-48h, with MQ water rinse to PH value no longer changes, and obtains the sepiolite of top pure grade；(2) grafting is handled：The top pure grade sepiolite of purification is scattered in deionized water, forms sepiolite suspension；(3) sepiolite suspension, with 12000 revs/min of speed high-speed stirred 5-10 minutes, forms sepiolite on dispersion machine Gel；And mercaptopropyl trimethoxysilane is added into sepiolite gel under the conditions of high-speed stirred, continue high-speed stirred and formed Sulfydryl modification sepiolite gel rubber system；By gel rubber system at 80 DEG C constant temperature 24-36 hours；Finally gel is taken out from system, dried under the conditions of 65 DEG C It is dry, obtain sulfydryl modification sepiolite after grinding；The acrylamide gel solution manufacturing method is：Gel cross-linkage agent is soluble in water, water is added afterwards, and mixture is shaken It is even, acrylamide is weighed, is dissolved in water, forms acrylamide solution, acrylamide solution and crosslinking agent are mixed one Rise, shake up and produce；By crosslinking agent：Weight ratio=1 of water：50 is soluble in water by gel cross-linkage agent, afterwards according to crosslinking agent：Water Weight ratio=1：158 add water, crosslinking agent：Weight ratio=1 of acrylamide：50, acrylamide：Weight ratio=1 of water：2.5；The gel cross-linkage agent is modified agarose, and preparation method is as follows：The molten solution into boiling water of agarose is kept for 80 DEG C；Sodium borohydride is dissolved in 3.5mol/L sodium hydroxide solution, so After add above-mentioned agarose solution and be stirred continuously；10wt% sodium hydroxide solution is added after 30min, is added dropwise in 15min Allyl glycidyl ether, 1h is reacted, cools to 60 DEG C, modulated neutrality with 4mol/L acetic acid, cleaned with acetone, be put in vacuum Drying box, dry under the conditions of 60 DEG C, grind；The agarose:Weight ratio=1 of boiling water:49, sodium borohydride:The weight of agarose Measure ratio=10：599, sodium hydroxide:Sodium borohydride weight=5：6；Sodium hydroxide solution:Boiling water volume ratio=10:49, pi-allyl Glycidol ether:Volume ratio=5 of boiling water:98.
- 2. the preparation method of easily dynamic heavy metal adsorption combination phase gel mould according to claim 1, it is characterised in that：Institute The sulfhydryl modified sepiolite stated is to be scattered in by purified sepiolite in deionized water, forms sepiolite suspension；Then will Sepiolite suspension is put on dispersion machine, with 12000 revs/min of speed high-speed stirred 5-10 minutes, forms sepiolite gel； And mercaptopropyl trimethoxysilane is added into sepiolite gel under the conditions of high-speed stirred, continue high-speed stirred formation sulfydryl and repair Adorn sepiolite gel rubber system；By gel rubber system at 80 DEG C constant temperature 24-36 hours；Finally gel is taken out from system, 65 Dried under the conditions of DEG C, sulfydryl modification sepiolite is obtained after grinding.
- 3. the preparation method of easily dynamic heavy metal adsorption combination phase gel mould according to claim 1, it is characterised in that：Institute State absolute ethyl alcohol：Acrylamide gel liquor capacity ratio is 7:500.
- 4. the preparation method of easily dynamic heavy metal adsorption combination phase gel mould according to claim 1, it is characterised in that：Institute State ammonium persulfate solution：Acrylamide gel liquor capacity ratio is 3:500；The tetramethylethylenediamine:Acrylamide gel is molten Liquid volume ratio is 3:2000.
- 5. the preparation method of easily dynamic heavy metal adsorption combination phase gel mould according to claim 1, it is characterised in that： It is about that 0.25mm non-solubility solid colorfuls haydite is used to indicate gel just that several particle diameters are added in the glass guide channel of the step (3) Reverse side, covered again with glass cover-plate afterwards.
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| Heavy Metal Adsorption by Functionalized Clays;RAFAEL CELIS;《Environ. Sci. Technol.》;20000922;第34卷(第21期);第4593-4599页 * |
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| CN105148847A (en) | 2015-12-16 |
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