CN102698715A - Fixed film for synchronously enriching phosphorus and sulphur and manufacturing method for fixed film - Google Patents
Fixed film for synchronously enriching phosphorus and sulphur and manufacturing method for fixed film Download PDFInfo
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- CN102698715A CN102698715A CN201210208540XA CN201210208540A CN102698715A CN 102698715 A CN102698715 A CN 102698715A CN 201210208540X A CN201210208540X A CN 201210208540XA CN 201210208540 A CN201210208540 A CN 201210208540A CN 102698715 A CN102698715 A CN 102698715A
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Abstract
The invention discloses a fixed film for synchronously enriching phosphorus and sulphur. The fixed film is a gel film manufactured after film liquid is gelatinized and is formed after grinding and ultrasonication are performed on a liquid mixture containing zirconium hydroxide hydrate powder, silver iodide particles and polyacrylamide. The manufacturing method for the fixed film comprises the following steps of: mixing the zirconium hydroxide hydrate powder and the silver iodide particles with polyacrylamide aqueous solution to obtain the liquid mixture; performing the grinding and the ultrasonication on the liquid mixture to prepare the even film liquid; adding a good amount of tetramethylethylenediamine and ammonium persulfate; then, injecting the film liquid into a glass mold; horizontally laying up the glass mold at the low temperature of 2-4 DEG C to enable zirconium hydroxide and the silver iodide particles to freely settle; and then, heating to 15+/-1 DEG C and laying up the glass mold until the film liquid is gelatinized into the film. According to the fixed film disclosed by the invention, the phosphorus and the sulphur can be synchronously enriched; the enrichment content is high; the particle size on the surface of the film is small (not greater than 5mum) and is even in distribution; and high-resolution synchronous analysis can be performed on deposits: the phosphorus and the sulphur.
Description
Technical field
The present invention relates to a kind of diffusive gradients in thin-films technology (Diffusive gradients in thin films; DGT) the fixedly film and preparation method thereof in; Be applicable to the enrichment and the analysis of p and s in the surrounding medium, relate in particular to fixedly film and preparation method thereof of synchronous enrichment p and s in a kind of water body environment analysis.
Background technology
P and s all is source of students key elements important in the water body environment.Phosphorus is the restricted element of most critical that causes body eutrophication, and the rising of The total phosphorus concentration is the first cause that causes blue-green algae undue growth and algal tufa to form; Sulphur can form odorous gas such as hydrogen sulfide under reducing environment; Cause the secondary pollution of water body; Reducible sulfur and iron can form deposition in the synchronous deposits, impel the phosphorus that is adsorbed onto on the ferriferous oxide to discharge, and further aggravate the release and the body eutrophication of phosphorus in the deposit.
At present, to the mensuration of active p and s in the water body deposit mode of mainly taking the initiative, after deposit taken out from water body, send the laboratory back to and analyze.Because deposit is in reducing environment under the natural conditions of water body, very easily change after the taking-up, causes analytical error.The present passive sampling of development technology, can with can Absorption of Phosphorus or the fixedly film of element such as sulphur insert in the deposit, in-situ enrichment phosphorus or sulphur after fixedly film takes out again, through analyzing phosphorus or the sulphur on the fixing film, obtain the information of active phosphorus in the deposit or sulphur indirectly.
Diffusive gradients in thin-films technology (Diffusive gradients in thin films; DGT) be that a kind of non-destructive, original position are obtained pollutant distribution in the deposit and active technology, can utilize fixedly film enrichment and measure deposit active phosphorus or sulphur, but at present in the DGT mensuration used fixedly film be the fixedly film of single absorption function; Promptly can only Absorption of Phosphorus or sulphur; Can not synchronous absorption and enrichment p and s, cause the assay determination inefficiency, operating cost is high simultaneously.
Summary of the invention
The present invention aims to provide fixedly film and preparation method thereof of the synchronous enrichment p and s of a kind of ability, improves the determination efficiency of active p and s in the analysis of DGT technology water body environment, reduces cost of determination simultaneously.
Above-mentioned purpose of the present invention realizes through following technical scheme:
A kind of fixedly film of synchronous enrichment p and s is characterized in that, this fixedly film be by the mixed liquor that comprises hydronium(ion) oxidation zirconium powder end, silver iodide particle and polyacrylamide, grind and the ultrasonic gel film of processing after disperseing film sol that the back forms with fixed attention.
Described fixedly film surface comprises zirconium hydroxide and silver iodide particle, particle diameter≤5 μ m.
In the described fixedly film, the weight ratio of hydronium(ion) oxidation zirconium and silver iodide is 1:0.2～0.4.
The fixedly film of described synchronous enrichment p and s adopts following method to make: with hydronium(ion) oxidation zirconium powder end and silver iodide particle and polyacrylamide solution mixing, after this mixed liquor grinding and ultrasonic dispersion, process uniform film liquid; After adding an amount of tetramethyl diethylamine and ammonium persulfate; This film liquid is injected glass mold, and horizontal positioned under 2-4 ℃ of low temperature makes after zirconium hydroxide and the free settling of silver iodide particle; Be warming up to 15 ± 1 ℃ of placements again, up to the film sol film that congeals into.
More specifically and optimally, described method may further comprise the steps:
1) the hydronium(ion) oxidation zirconium powder of 1g moisture content 50 ± 5% end and 0.2-0.4g silver iodide particle and 3～5mL, 30% polyacrylamide solution are mixed, grind with ultrasonic dispersion after make film liquid, leave standstill 5～10min removal and precipitate;
2) in the supernatant that step 1) obtains, add the ammonium persulfate of 2-4 μ L tetramethyl diethylamine (TEMED) and 50-100 μ L 10% (wt) again, inject the uniform space of thickness between two glass sheets of glass mold behind the mixing, bubble is caught up with use up;
3) glass mold horizontal positioned 30～60 minutes under 2-4 ℃ of low temperature; Make hydronium(ion) oxidation zirconium and the free settling of silver iodide particle to the bottom (then downwards one side is the fixing front of film); Be warming up to 15 ± 1 ℃ then, place more than half an hour, until the film sol film that congeals into;
4) behind the taking-up gel film, put into deionized water and soak more than 24 hours, make the fixedly film of described synchronous enrichment p and s.
Described zirconium hydroxide powder can be by following method preparation; The pH that regulates the zirconium oxychloride aqueous solution of 0.1M with 25% ammoniacal liquor reaches and is stabilized in 7.0 ± 0.2; The precipitate with deionized water that is produced is washed till does not have chlorion; Deposition after centrifugation, drying and to control its moisture content be between 50 ± 5%, grind into powder again.
Advantage of the present invention and beneficial effect comprise:
1) collocation of two kinds of adsorbents of fixedly film of the present invention is very reasonable.Fixedly film depends on the distribution of adsorbent on the film surface to the absorption property of object; Distribution density is big more, and then absorption property is strong more.If realize the function of two kinds of objects of the synchronous enrichment of a kind of fixedly film, two kinds of adsorbents that adopted all need be distributed in fixedly film surface, make adsorbent can directly touch object, produce suction-operated.The fixedly film of existing simple function mainly adopts iron hydroxide and Metsorb as the adsorbent of phosphorus, adopts the adsorbent of silver iodide as sulphur.Because the ratio of iron hydroxide and Metsorb is great, when arranging in pairs or groups, preferentially occupy fixedly film surface with silver iodide, make silver iodide can not be deposited to fixedly film surface, causing fixedly, film can not effectively adsorb sulphur.The hydronium(ion) oxidation zirconium proportion that the present invention adopted is littler than silver iodide; Be unformed powder simultaneously; When both together during sedimentation, the preferential sedimentation of silver iodide and be distributed to the surface, unformed hydronium(ion) oxidation zirconium then is distributed in the remaining surface part that is not occupied by silver iodide; Make fixedly and film surface distribute simultaneously zirconium hydroxide and silver iodide can adsorb the p and s ion simultaneously.To the optimization of hydronium(ion) oxidation zirconium and silver iodide addition, can make fixedly film zirconium hydroxide of the present invention and silver iodide reasonable in the distribution density on fixing film surface, reach the function of synchronous enrichment p and s.Fixedly film of the present invention enrichment synchronously p and s is compared with the fixedly film of existing single enrichment function, improves the efficient of enrichment and detection greatly.
2) fixedly film production process optimization of the present invention, fixedly film is all having excellent performance aspect absorption property and the physical strength.Because silver iodide have catalytic action; Fixing film production there is stronger interference effect, so the fixing conditioned disjunction parameter in the preparation method of film of the present invention, need through optimizing and control; Comprise zirconium hydroxide and silver iodide particle diameter, the temperature-time of sedimentation of film liquid and gelling etc.After above-mentioned parameter optimized, fixedly in the preparation process of film, zirconium hydroxide and silver iodide had suitable sedimentation and gelation rate in the present invention, thereby two kinds of adsorbents of formation is reasonably combined on the surface; And can keep fixedly film stable shape, and indeformable, absorbent particles does not come off, and absorption property keeps stable simultaneously, and the term of validity reached more than 2 years.
3) the present invention is after fixedly film adopts zirconium hydroxide and silver iodide to arrange in pairs or groups, and can adopt the gray scale method to analyze to the sulphur that accumulates on the fixing film.Fixedly film mainly carries out through silver iodide and the black precipitate of sulphur generation silver sulfide the absorption of sulphur; The fixing adsorbance of sulphur and fixedly between the film surface gray scale (0-255) corresponding relation is arranged on the film, the gray scale reckoning that therefore can utilize fixing film surface be the adsorbance of sulphur on the film fixedly.Above-mentioned application to sulphur gray analysis method needs fixedly the film surface to have extremely low background gray scale (< 50), and the phosphorus adsorbent background color that promptly adds can be to fixedly film surface generation interference.The maximum iron hydroxide adsorbent of current use is yellow or brown, and its background color can not satisfy the requirement of gray analysis to fixedly film surface generation interference.Zirconium hydroxide is lily, can not produce any interference to fixing film surface background gray scale.Fixedly film background gray scale of the present invention is low, the saturated gray scale of sulphur high (like Fig. 3), therefore is fit to very much the gray analysis of sulphur.Compare with traditional chemical extraction-assay method, this method can significantly improve sulphur content and analyse efficient, and operating cost is extremely low simultaneously.
4) compare with the simple function phosphorus fixing film of report, the fixedly film of synchronous enrichment p and s of the present invention has very high enrichment capacity.Preferentially in the film surface distributed, when guaranteeing sulphur enrichment capacity, the addition of silver iodide does not have significant adverse effect (referring to Fig. 2) to the phosphorus absorption property at silver iodide, phosphorus enrichment capacity (; 200 μ g P cm
-2) be respectively traditional F eO film, modified FeO film and Metsorb film 50 times, more than 14 times and 8 times.Owing to this advantage, can fixedly film of the present invention be used to analyze the eutrophic lake of high phosphorus background.
5) owing on manufacture craft, adopt to grind and measure such as ultrasonic; Zirconium hydroxide and silver iodide particle grain size very small (≤5 μ m) in the fixedly film of the present invention; And be evenly distributed; Make this fixedly film can carry out the high-resolution Synchronization Analysis of deposit p and s, spatial resolution is at 0.45 * 0.45mm
2More than.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not exceeded with the specific embodiment, but is limited claim.
Description of drawings
Electron-microscope scanning (SEM) image on Figure 1A fixedly film of the present invention surface can see that fixedly the zirconium hydroxide distribution of film surface is fine and close, the silver iodide uniform particles, and particle diameter is less than 5 μ m.
Figure 1B fixedly film of the present invention can see that at the electron-microscope scanning image that fully adsorbs sulphion caudacoria surface the silver sulfide deposit seed of generation is uniformly distributed in fixedly film surface.
The electron-microscope scanning in Fig. 1 C fixedly film of the present invention cross section and energy-spectrum scanning (EDS) image can find out that silver is more than zirconium in the distribution on fixing film surface, explain that silver iodide are deposited to preferentially that fixedly film is surperficial.
Fig. 2 the present invention fixedly film silver iodide addition to the influence of phosphorus absorption property.When the silver iodide addition when 0.2g changes to 0.4g, fixedly film to the absorption property of phosphorus with do not add silver iodide and compare and do not have notable difference.
Fixedly film that Fig. 3 different silver iodide additions of the present invention are processed surface gray scale (being the background gray scale) and the fixing surperficial grey scale change after the saturated absorption of film sulphur.When silver iodide were added into 0.2～0.4g, it is about 45 that the background gray scale is stabilized in, and the surperficial gray scale in the saturated back of sulphur is stabilized in about 200～220.
Fig. 4 fixedly film of the present invention is to the synchronous bioaccumulation efficiency curve map of p and s.
The specific embodiment
A kind of fixedly film of synchronous enrichment p and s, its preparation method is following:
The zirconium oxychloride aqueous solution pH that regulates 0.1M with 25% ammoniacal liquor reaches and is stabilized in 7.0 ± 0.2; The precipitate with deionized water that is produced is washed till does not have chlorion; Deposition is after centrifugal removal supernatant, and is dry with hair-dryer, to its moisture content be 50%; Clay into power with mortar again, obtain the hydronium(ion) oxidation zirconium powder end of moisture content 50%.
The hydronium(ion) oxidation zirconium powder of 1g moisture content 50% end and 0.3g silver iodide particle and 4mL 30% polyacrylamide solution are mixed, and after grinding and the ultrasonic dispersion, make film liquid, leave standstill 10min and remove and precipitate.The ammonium persulfate that in the supernatant of removing post precipitation, adds 3 μ L TEMED and 75 μ L 10% (wt) again, the space of the mould that two glass sheets that behind the mixing its slow injection accompanied 0.4mm, the uniform U-shaped plastic tab of thickness are fast formed; After catching up with bubble to the greatest extent, glass plate horizontal positioned half an hour under 3 ℃ of low temperature make hydronium(ion) oxidation zirconium and the free settling of silver iodide particle to the bottom, then one side is the fixing front of film downwards, is warming up to 15 ± 1 ℃ then, placement half an hour, makes the film sol film that congeals into.Then glass plate is pried open, is taken out gel film, put into deionized water and soaked 24 hours, during change water 3 times.
The SEM of prepared fixedly film and EDS image are seen Figure 1A～C, and its surperficial zirconium hydroxide and silver iodide even particle distribution are fine and close, particle diameter≤5 μ m.
With synchronously fixedly film be cut into the disk of diameter 2.5cm, put into the solution of the p and s that contains 1mg/L simultaneously, vibration is 180 minutes under the room temperature, fixedly film is to bioaccumulation efficiency curve such as Fig. 4 of p and s.Fixedly all along with duration of oscillation is increasing, and both increase trend is very similar to the enriching quantity of p and s for film, and enrichment is after 180 minutes, and fixedly film reaches 97% and 94% respectively to the bioaccumulation efficiency of p and s.
Embodiment 2
A kind of fixedly film of synchronous enrichment p and s, its preparation method is following:
The hydronium(ion) oxidation zirconium powder end for preparing moisture content 45% according to the method for embodiment 1.
The hydronium(ion) oxidation zirconium powder of 1g moisture content 45% end and 0.2g silver iodide particle and 3mL 30% polyacrylamide solution are mixed, and after grinding and the ultrasonic dispersion, make film liquid, leave standstill 10min and remove and precipitate.The ammonium persulfate that in the supernatant of removing post precipitation, adds 4 μ L TEMED and 100 μ L 10% (wt) again, the space of the mould that two glass sheets that behind the mixing its slow injection accompanied 0.4mm, the uniform U-shaped plastic tab of thickness are fast formed; After catching up with bubble to the greatest extent, glass plate horizontal positioned half an hour under 4 ℃ of low temperature make hydronium(ion) oxidation zirconium and the free settling of silver iodide particle to the bottom, then one side is the fixing front of film downwards, is warming up to 15 ± 1 ℃ then, placement half an hour, makes the film sol film that congeals into.Then glass plate is pried open, is taken out gel film, put into deionized water and soaked 24 hours, during change water 3 times.
Its surperficial zirconium hydroxide of prepared fixedly film and silver iodide even particle distribution are fine and close, particle diameter≤5 μ m.
Embodiment 3
A kind of fixedly film of synchronous enrichment p and s, its preparation method is following:
The hydronium(ion) oxidation zirconium powder end for preparing moisture content 55% according to the method for embodiment 1.
The hydronium(ion) oxidation zirconium powder of 1g moisture content 55% end and 0.4g silver iodide particle and 5mL 30% polyacrylamide solution are mixed, and after grinding and the ultrasonic dispersion, make film liquid, leave standstill 10min and remove and precipitate.The ammonium persulfate that in the supernatant of removing post precipitation, adds 2 μ L TEMED and 50 μ L 10% (wt) again, the space of the mould that two glass sheets that behind the mixing its slow injection accompanied 0.4mm, the uniform U-shaped plastic tab of thickness are fast formed; After catching up with bubble to the greatest extent, glass plate horizontal positioned half an hour under 2 ℃ of low temperature make hydronium(ion) oxidation zirconium and the free settling of silver iodide particle to the bottom, then one side is the fixing front of film downwards, is warming up to 15 ± 1 ℃ then, placement half an hour, makes the film sol film that congeals into.Then glass plate is pried open, is taken out gel film, put into deionized water and soaked 24 hours, during change water 3 times.
Its surperficial zirconium hydroxide of prepared fixedly film and silver iodide even particle distribution are fine and close, particle diameter≤5 μ m.
Claims (7)
1. the fixedly film of a synchronous enrichment p and s is characterized in that: this fixedly film be by the mixed liquor that comprises hydronium(ion) oxidation zirconium powder end, silver iodide particle and polyacrylamide, grind with ultrasonication after the gel film processed after with fixed attention of the film sol that forms.
2. the fixedly film of synchronous enrichment p and s according to claim 1 is characterized in that: described fixedly film surface comprises zirconium hydroxide and silver iodide particle, particle diameter≤5 μ m.
3. the fixedly film of synchronous enrichment p and s according to claim 1 is characterized in that: in the described fixedly film, the weight ratio of hydronium(ion) oxidation zirconium and silver iodide is 1:0.2～0.4.
4. the fixedly film of synchronous enrichment p and s according to claim 1 is characterized in that, described fixedly film adopts following method to make; With hydronium(ion) oxidation zirconium powder end and silver iodide particle and polyacrylamide solution mixing, after this mixed liquor grinding and ultrasonic dispersion, process uniform film liquid; After adding an amount of tetramethyl diethylamine and ammonium persulfate; This film liquid is injected glass mold, and horizontal positioned under 2～4 ℃ of low temperature makes after zirconium hydroxide and the free settling of silver iodide particle; Be warming up to 15 ± 1 ℃ of placements again, up to the film sol film that congeals into.
5. the preparation method of the fixedly film of the described synchronous enrichment p and s of claim 1; It is characterized in that:, after this mixed liquor grinding and ultrasonic dispersion, process uniform film liquid hydronium(ion) oxidation zirconium powder end and silver iodide particle and polyacrylamide solution mixing; After adding an amount of tetramethyl diethylamine and ammonium persulfate; This film liquid is injected glass mold, and horizontal positioned under 2～4 ℃ of low temperature makes after zirconium hydroxide and the free settling of silver iodide particle; Be warming up to 15 ± 1 ℃ of placements again, up to the film sol film that congeals into.
6. the preparation method of fixedly film according to claim 5 is characterized in that, described method may further comprise the steps:
1) the hydronium(ion) oxidation zirconium powder of 1g moisture content 50 ± 5% end and 0.2～0.4g silver iodide particle and 3～5mL, 30% polyacrylamide solution are mixed, grind with ultrasonic dispersion after make film liquid, leave standstill 5～10min removal and precipitate;
2) in the supernatant that step 1) obtains, add the ammonium persulfate of 2～4 μ L tetramethyl diethylamine (TEMED) and 50～100 μ L 10% (wt) again, inject the uniform space of thickness between two glass sheets of glass mold behind the mixing, bubble is caught up with to the greatest extent;
3) glass mold horizontal positioned 30～60min under 2～4 ℃ of low temperature; Make hydronium(ion) oxidation zirconium and the free settling of silver iodide particle to the bottom (then downwards one side is the fixing front of film); Be warming up to 15 ± 1 ℃ then, place more than half an hour, until the film sol film that congeals into;
4) behind the taking-up gel film, put into deionized water and soak more than 24 hours, make the fixedly film of described synchronous enrichment p and s.
7. according to the preparation method of claim 5 or 6 described fixedly films; It is characterized in that: described zirconium hydroxide powder is by following method preparation; The zirconium oxychloride aqueous solution that uses 25% ammoniacal liquor to regulate 0.1M is 7.0 ± 0.2 to pH, and the precipitate with deionized water that is produced is washed till no chlorion, and deposition is after centrifugation; Dry and to control its moisture content be between 50 ± 5%, grind into powder again.
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Cited By (5)
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| CN104048956A (en) * | 2013-03-12 | 2014-09-17 | 中国科学院南京地理与湖泊研究所 | Diffusive gradients in thin films (DGT) method for determination of phosphorus content on the basis of computer-imaging densitometry (CID) technology |
| CN104048924A (en) * | 2013-03-12 | 2014-09-17 | 中国科学院南京地理与湖泊研究所 | Two-dimensional high-resolution method for determination of distribution of active phosphorus in wetland soil and deposit |
| CN104043409A (en) * | 2013-03-12 | 2014-09-17 | 中国科学院南京地理与湖泊研究所 | Immobilized membrane for synchronously enriching phosphor and ferrum and preparation method thereof |
| CN108854967A (en) * | 2018-06-08 | 2018-11-23 | 中国科学院合肥物质科学研究院 | A kind of zirconium-based metallic organic framework materials UiO-66 and its application |
| CN112526011A (en) * | 2020-11-18 | 2021-03-19 | 农业农村部环境保护科研监测所 | Method for synchronously extracting and measuring concentrations of sulfate ions and sulfide ions in environmental medium based on DGT technology and application |
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| CN104048956A (en) * | 2013-03-12 | 2014-09-17 | 中国科学院南京地理与湖泊研究所 | Diffusive gradients in thin films (DGT) method for determination of phosphorus content on the basis of computer-imaging densitometry (CID) technology |
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| CN104043409A (en) * | 2013-03-12 | 2014-09-17 | 中国科学院南京地理与湖泊研究所 | Immobilized membrane for synchronously enriching phosphor and ferrum and preparation method thereof |
| CN104043409B (en) * | 2013-03-12 | 2016-08-17 | 中国科学院南京地理与湖泊研究所 | A kind of fixing film synchronizing enriched phosphorus and ferrum and preparation method thereof |
| CN104048956B (en) * | 2013-03-12 | 2016-08-17 | 中国科学院南京地理与湖泊研究所 | A kind of DGT method based on Computer-generated images densitometry technical measurement phosphorus content |
| CN104048924B (en) * | 2013-03-12 | 2017-04-19 | 中国科学院南京地理与湖泊研究所 | Two-dimensional high-resolution method for determination of distribution of active phosphorus in wetland soil and deposit |
| CN108854967A (en) * | 2018-06-08 | 2018-11-23 | 中国科学院合肥物质科学研究院 | A kind of zirconium-based metallic organic framework materials UiO-66 and its application |
| CN108854967B (en) * | 2018-06-08 | 2021-04-23 | 中国科学院合肥物质科学研究院 | Zirconium-based metal organic framework material UiO-66 and application thereof |
| CN112526011A (en) * | 2020-11-18 | 2021-03-19 | 农业农村部环境保护科研监测所 | Method for synchronously extracting and measuring concentrations of sulfate ions and sulfide ions in environmental medium based on DGT technology and application |
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Application publication date: 20121003 |