CN107930608A - A kind of dissolubility Phos, the preparation method of arsenic adsorbed film - Google Patents
A kind of dissolubility Phos, the preparation method of arsenic adsorbed film Download PDFInfo
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- CN107930608A CN107930608A CN201711111207.6A CN201711111207A CN107930608A CN 107930608 A CN107930608 A CN 107930608A CN 201711111207 A CN201711111207 A CN 201711111207A CN 107930608 A CN107930608 A CN 107930608A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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Abstract
The invention discloses the preparation method of a kind of dissolubility Phos, arsenic adsorbed film.The adsorbed film is that cerium oxide nanoparicles are dispersed in acrylamide solution, is reacted by acrylamide polymerization and is uniformly fixed on nano-particle in polyacrylamide gel.Preparation process is：Cerium oxide nanoparicles are distributed to acrylamide solution, add ammonium persulfate and tetramethylethylenediamine, injection is accompanied in two pieces of glass plates of U-shaped thin slice after mixing, at room temperature after horizontal positioned 30 minutes, open glass plate and take out gel mould, 24h is soaked in deionized water and removes unreacted reagent, gel mould is cut into diameter 2.5cm adsorbed film is made.The present invention prepares the easy to operate, reproducible of adsorbed film, and adsorbed film is big, selective good to the adsorption capacity of dissolubility Phos, arsenic, can for a long time preserve, have broad application prospects in analytical chemistry, environmental analysis field in the solution.
Description
Technical field
The invention discloses the preparation method of a kind of dissolubility Phos, arsenic adsorbed film, suitable for diffusive gradients in thin-films skill
Dissolubility Phos and arsenic in art measure water, belong to analytical chemistry, environmental science.
Background technology
One of three big nutrients necessary to phosphorus is biology.Phosphorus can excessively cause body eutrophication in water body, cause water
Middle algae excessive propagation, destroys the ecological balance of water body, threatens the life security of the mankind.Inorganic arsenic (trivalent arsenic and pentavalent arsenic) has
There are teratogenesis, carcinogenic or mutagenic effect, skin pigment metabolic disorder and a variety of diseases can be caused by drinking the water of arsenic pollution for a long time
Occur.Therefore, develop new sampling, determination techniques are monitored dissolubility Phos, arsenic in water to preserving the ecological environment and
Human life is of great significance safely.
Diffusive gradients in thin-films technology (Diffusive Gradients in Thin Films, DGT) is that a kind of original position is adopted
Sample, e measurement technology, which was proposed by Lancaster University of Britain David Williams et al. in 1994, for solubility
The measure of metal ion.DGT devices are mainly made of shell, diffusion barrier, adsorbed film.Ion in solution diffuses through diffusion
Film reaches adsorbed film, is combined with the adsorption site on adsorbed film.After diffusion reaches stable state, the ion of accumulation in adsorbed film
Quality meets Fick diffusion laws.
When adsorbed film surface ion concentration (C) is zero, the mass of ion M of accumulation and solution bulk ion are dense in adsorbed film
Spend (C0) directly proportional.Thus, it is ensured that C is zero, adsorbed film have to be larger than ion in diffusion barrier to the rate of adsorption of ion
Diffusion rate.
DGT mainly uses ion exchange resin membrane when measuring metal ion.It is presently used for the inorganic P and As determination of dissolubility
Adsorbed film have the sorbing materials such as iron oxide, sulfydryl silica gel, titanium dioxide and zirconium oxide (Zr-oxide) formed gel mould
(Zhang H,et al.,Anal.Chim.Acta,1998,370:29-38；Bennett W.W,et al.,
Anal.Chem.2011,83:8293~8299；Panther J.G,et al.Environ.Sci.Technol.,2010,44:
9419-9424；Ding S,et al.Environ.Sci.Technol.,2010,44:8169-8174；Bennett W.W,et
al.Anal.Chem.,2010,82:7401-7407；Sun Q,et al.Anal.Chem.,2014,86:3060-3067).Its
Preparation method is that the sorbing materials such as iron oxide, mercapto-functionalized silica gel, titanium dioxide and zirconium oxide are dispersed in hot acrylamide
Gel is formed in solution, after cooling, and adsorbed film is made.When sorbing material particle diameter is larger, sorbing material divides in polyacrylamide gel
Cloth is uneven；Further, since sent out between sorbing material and acrylamide solution there are density variation into material in gel process
Life is settled and is being layered.Chinese Patent Application No. 201310689076.5 discloses a kind of direct using polyacrylamide hydrogel
The method that absorption zirconium ion prepares adsorbed film.The zirconium gel mould prepared based on physisorption when in use may there are zirconium
The loss of ion, zirconium ion may enter in eluent when eluting in addition, influence follow-up Instrument measuring.Therefore, research is new
Type adsorbed film is of great significance for the new method of development DGT measure dissolubilities Phos, arsenic.
The content of the invention
The object of the present invention is to provide the preparation method of a kind of dissolubility Phos, arsenic adsorbed film.Which is by dioxy
Change cerium nano-particle to be dispersed in acrylamide solution, be uniformly fixed on nano-particle by the polymerisation of acrylamide poly-
In acrylamide gel.The adsorbed film of preparation is used for dissolubility Phos, arsenic in DGT measure water.
Technical scheme：
A kind of dissolubility Phos, the preparation method of arsenic adsorbed film, step are as follows：
The polymeric precursors of acrylamide containing 15wt.% and 1wt.%N, N- methylene-bisacrylamide are configured with deionized water
Solution, cerium oxide nanoparicles is added into polymerization premise solution, ultrasonic disperse is uniform；By with polymeric precursors liquor capacity
Than being separately added into 10wt.% ammonium persulfates and tetramethylethylenediamine for 1/54 and 1/180, after mixing, it is thin that injection accompanies U-shaped
In two pieces of glass plates of film trap, after discharging bubble, by horizontal positioned holding 30 minutes at room temperature of glass plate, glass plate is opened, is taken
Go out gel mould；24h is soaked in deionized water and removes unreacted reagent, gel mould is cut into diameter 2.5cm adsorbed film is made.
The mass ratio of the cerium oxide nanoparicles and polymeric precursors solution is 5%~20%.
The diameter of the cerium oxide nanoparicles is less than 1 micron.
The thickness of the adsorbed film is 0.2~0.8mm.
Beneficial effects of the present invention：
1. the present invention prepares dissolubility Phos, arsenic adsorbed film using cerium oxide nano materials.Compound containing cerium is main
As catalyst, also have been reported that and used cerium oxide as adsorbent, but there are no report of the ceria as DGT adsorbed films
Road.The adsorbed film can replace it has been reported that iron oxide film, titanium dioxide film and zirconium dioxide film, for DGT measure dissolve
Property Phos, arsenic.
2. the adsorbed film is big to the adsorption capacity of Phos, arsenic, it is not easy to which saturation, can extend the sampling time of DGT, obtain
Obtain lower detection sensitivity.
3. the absorption membrane preparation method is simple, reproducible, adsorbed film can preserve for a long time in the solution.
Brief description of the drawings
Fig. 1 is DGT sampling apparatuses and treats the schematic diagram that measured ion is spread in DGT devices.
Fig. 2 is cerium oxide nanoparicles/polyacrylamide gel adsorbed film digital image.
Fig. 3 is when being sampled based on cerium oxide nanoparicles/polyacrylamide gel adsorbed film DGT devices to phosphate radical
Between-mass accumulation figure.
Fig. 4 is to arsenic sampling time-tired based on cerium oxide nanoparicles/polyacrylamide gel adsorbed film DGT devices
Product Quality Map.
Fig. 5 is influence figure of the ionic strength to DGT extraction phosphate radicals.
Fig. 6 is influence figure of the ionic strength to DGT extraction arsenic.
Fig. 7 is influence figure of the solution ph to DGT extraction phosphate radicals.
Fig. 8 is influence figure of the solution ph to DGT extraction arsenic.
Fig. 9 is that DGT carries out actual field sampling determination arsenic (trivalent, pentavalent) result and active sampled result comparison diagram.
Embodiment
Measured with reference to the DGT of Dalian arsenic in water body (trivalent, pentavalent), further illustrate technical scheme
And beneficial effect.
(1) the cerous nitrate Ce (NO of 100mL 0.005mol/L3)3·6H2O ethanol solutions are with 100mL 0.2mol/L's
NaOH solution mixes, and agitated precipitation obtains glassy yellow cerium oxide nano materials, then uses ethanol and deionized water rinsing 3 respectively
Time, the precipitation of collected after centrifugation bottom, dries 12h in 100 DEG C of baking ovens.
(2) cerium dioxide nano material that (1) obtains is uniformly mixed with acrylamide solution, then by molten with acrylamide
1/54 volume ratio of liquid, 10% ammonium persulfate of addition, the tetramethylethylenediamine of 1/180 volume ratio, after mixing, after mixing
Mixed solution is slowly injected into the two glass sheets gaps for accompanying U-shaped thin slice (0.4mm), after discharging bubble, at room temperature by glass
Glass plate is horizontal positioned.After 30 minutes, glass plate is opened, takes out the polyacrylamide gel containing cerium oxide nano materials, super
24h is soaked in pure water and removes unreacted reagent.Gel is cut into the diaphragm of diameter 2.5cm, is immersed in ultra-pure water, lucifuge
Low-temperature storage, it is stand-by.
(3) will the adsorbed film assembling with DGT devices in, be respectively placed in phosphate radical and arsenic (trivalent, pentavalent) solution into
Row sampling, adsorbed film is removed, eluted with the 2.0mol/L sodium hydroxide -0.5mol/L hydrogen peroxide of 1mL after sampling,
Then measure, the results showed that, phosphate radical, the quality of arsenic ion are directly proportional to the sampling time (as shown in Figure 3, Figure 4) on adsorbed film,
Meet DGT and quantify principle.
(4) by adsorbed film assembling with DGT devices, being respectively placed in containing different sodium nitrate concentration (0~0.5mol/
L sampled, removed adsorbed film after sampling, with the 2.0mol/ of 1mL in phosphate radical and arsenic (trivalent, pentavalent) solution)
L sodium hydroxide -0.5mol/L hydrogen peroxide is eluted, and is then measured, the results showed that, in the sodium nitrate concentration, absorption
Phosphate radical, the quality of arsenic ion keep constant (as shown in Figure 5, Figure 6) on film, show the adsorbed film in sampling from the shadow of salt
Ring.
(5) will the adsorbed film assembling with DGT devices in, be respectively placed in the phosphate radical containing different pH (4.2~9.3) and
Sampled in arsenic (trivalent, pentavalent) solution, removed adsorbed film after sampling, with the 2.0mol/L sodium hydroxides of 1mL-
0.5mol/L hydrogen peroxide is eluted, and is then measured, the results showed that, in the range of the pH, phosphate radical on adsorbed film, arsenic from
The quality of son keeps constant (as shown in Figure 7, Figure 8), shows the adsorbed film in sampling from the influence of pH value of solution.
(5) adsorbed film is assembled in DGT devices, be positioned in reservoir carry out sampling 72 it is small when, after the completion of collection will
DGT devices take back laboratory, remove adsorbed film, with the 2.0mol/L sodium hydroxide -0.5mol/L hydrogen peroxide of 1mL eluted into
Row elution, then measures the concentration of arsenic in eluent with hydride generation-atomic fluorescence spectrometric, and quantifies publicity according to DGT and change
It is counted as the concentration of arsenic in water sample.While DGT is sampled, water sample is collected when 0,24,48,72 is small respectively, after taking back laboratory
With the concentration of hydride generation-atomic fluorescence spectrometric measure arsenic.As a result such as Fig. 9, DGT sampling determinations result is 1.25 μ g/L, directly
The average result for receiving collection water determination is 1.29 μ g/L, as a result basically identical.Show that the adsorbed film is functional, available for reality
Border spot sampling measure.
Claims (3)
1. a kind of dissolubility Phos, the preparation method of arsenic adsorbed film, it is characterised in that step is as follows：
The polymeric precursors that acrylamide containing 15wt.% and 1wt.%N, N- methylene-bisacrylamide are configured with deionized water are molten
Liquid, cerium oxide nanoparicles is added into polymerization premise solution, ultrasonic disperse is uniform；By with polymeric precursors liquor capacity ratio
10wt.% ammonium persulfates and tetramethylethylenediamine are separately added into for 1/54 and 1/180, after mixing, injection accompanies U-shaped thin slice
In two pieces of glass plates of groove, after discharging bubble, by horizontal positioned holding 30 minutes at room temperature of glass plate, glass plate is opened, is taken out
Gel；24h is soaked in deionized water and removes unreacted reagent, and gel is cut into circular or rectangular absorption diaphragm；
The mass ratio of the cerium oxide nanoparicles and polymeric precursors solution is 5%~20%.
2. preparation method according to claim 1, it is characterised in that the diameter of the cerium oxide nanoparicles is less than
1 micron.
3. preparation method according to claim 1 or 2, it is characterised in that the thickness of the adsorbed film is 0.2~0.8mm.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993373A (en) * | 2018-07-10 | 2018-12-14 | 广州大学 | A kind of adsorbed film and preparation method thereof of fixed thallium ion |
| CN109772278A (en) * | 2019-03-08 | 2019-05-21 | 南京大学 | A kind of synchronous fixed arsenic, antimony, adsorbed film of vanadium ion and preparation method thereof |
| CN110327875A (en) * | 2019-08-01 | 2019-10-15 | 广东维清环境工程有限公司 | A kind of preparation method for the new and effective Dephosphorization reagent being carried on zeolite |
| CN111103216A (en) * | 2019-12-27 | 2020-05-05 | 南京国兴环保产业研究院有限公司 | Film diffusion gradient DGT (differential global temperature sensor) collecting device for synchronously collecting ammonia nitrogen, nitrate nitrogen and phosphate radical in environment and production method thereof |
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| EP1069943B1 (en) * | 1998-04-06 | 2005-07-06 | Pall Corporation | Large pore volume composite mineral oxide beads, their preparation and their applications for adsorption and chromatography |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993373A (en) * | 2018-07-10 | 2018-12-14 | 广州大学 | A kind of adsorbed film and preparation method thereof of fixed thallium ion |
| CN109772278A (en) * | 2019-03-08 | 2019-05-21 | 南京大学 | A kind of synchronous fixed arsenic, antimony, adsorbed film of vanadium ion and preparation method thereof |
| CN110327875A (en) * | 2019-08-01 | 2019-10-15 | 广东维清环境工程有限公司 | A kind of preparation method for the new and effective Dephosphorization reagent being carried on zeolite |
| CN111103216A (en) * | 2019-12-27 | 2020-05-05 | 南京国兴环保产业研究院有限公司 | Film diffusion gradient DGT (differential global temperature sensor) collecting device for synchronously collecting ammonia nitrogen, nitrate nitrogen and phosphate radical in environment and production method thereof |
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