CN101629881A - Phosphorus fixing film applied to diffusive gradients in thin-films measurement technology - Google Patents
Phosphorus fixing film applied to diffusive gradients in thin-films measurement technology Download PDFInfo
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Abstract
The invention relates to a phosphorus fixing film applied to diffusive gradients in thin-films measurement technology. A fixing film and dispersion film superposed structure is arranged in the diffusive gradients in thin-films measurement technology, ions pass through a dispersion film in a dispersion way and is captured by a fixing film immediately to form the linear gradient distribution on the dispersion film. The phosphorus fixing film capturing phosphorus ions is characterized by using zirconium dioxide powder and acrylamide as raw materials, the raw materials are uniformly mixed to form mixed solution according to the weight volume ratio of 1:1.5-1:4, the mixed solution is slowly infused into a clearance of two glass plates clamping a u-shaped plastic sheet, the glass plates are placed for 2-4h horizontally at lower temperature of 10-15 DEG C after bubbles are removed, the temperature is risen to 30-35 DEG C after the zirconium dioxide powder is freely settled so as to enable the mixed solution to be gelated to form a film, the film has higher absorption capacity ratio to phosphate radicals than the prior iron film material by at least 4 times under the condition that the pH value is 5-9, so the analysis requirement of the DGT technology to phosphorus in different environment media is completely met.
Description
Technical field
The present invention relates to the A+E of migratory activity, biological effectiveness, pollution risk etc., especially a kind of phosphorus fixing film that is applied to diffusive gradients in thin-films measurement technology to phosphorus in the surrounding mediums such as soil, sediment.
Background technology
(Diffusive Gradients in Thin Films, DGT) determination techniques is a kind of new morphological analysis technology to diffusive gradients in thin-films, is mainly grown up in the mid-90 in last century by Britain Davison of Lancaster university and Zhang etc.This technology by gradient diffusion and the association process research of object ion at the definition diffusion layer, obtains the activated information of ion in medium based on diffusion principle.DGT determination techniques device is formed (Fig. 1) by the stack of fixedly film and diffusion barrier, ion passes diffusion barrier with diffusion way, and the film that is fixed is immediately caught, and forms the linear gradient distribution on diffusion barrier, its close fixedly ion concentration of film one end is maintained zero, contacts the concentration (C of an end with medium
DGT) be:
M is accumulation (the mol cm of ion on the resin molding in the following formula
-2), ▽ g is thickness of diffusion layer (cm), D
gBe the rate of diffusion (cm of ion in diffusion barrier
2s
-1), t is diffusion time (s).C
DGTBe mean concentration (the mol cm that standing time, section obtained by the DGT analysis
-3), its variation is not only relevant with the solubilised state concentration of object ion in medium, depends on source-remittance transfer processes such as form transformation, solid-liquid exchange simultaneously.Satisfying the important prerequisite that DGT measures, is that fixedly film has sufficiently high adsorption capacity to object ion, makes in minute, and the close fixedly ion concentration of film one end is maintained zero.Because migration of the ion in DGT diffusion process and the actual environment and bioadsorption processes have comparability, this technology is as a kind of new morphological analysis means, be applied to gradually in water body, soil and the sediment, research object expands to yttrium and nonmetalloid etc. from the metallic element of routine.
Yet diffusive gradients in thin-films technology (DGT) is that the application of object is few with phosphorus, in the DGT technology fixedly film to the deficiency of phosphorus adsorption capacity, be the restriction its application bottleneck.The fixedly film that uses in the current DGT technology is made of ferric oxide particles, is configured to gel film by third rare acid amides, utilizes the absorption of ferric oxide particles to phosphorus, reaches the fixedly purpose of phosphorus.According to the report of developer Zhang etc., when environment temperature is 25 ℃, when the content of phosphorus is 0.4mg/L in the solution, to place after 24 hours, this film is saturated to phosphorus fixation.Because in a large amount of soil liquid or sediment interstitial water, the content of dissolved phosphorus is much larger than 0.4mg/L, the application of this device thereby be subjected to great restriction.This film is very easily distortion simultaneously, as after being cut into definite shape, the phenomenon that can shrink, and very easily attach to tube wall, cause analytical error.
Summary of the invention
The present invention seeks to overcome the deficiency of prior art, a kind of phosphorus fixing film that is applied to diffusive gradients in thin-films measurement technology is provided, this phosphorus fixed film has very high adsorption capacity to phosphonium ion, to solve the problem of phosphorus fixed capacity deficiency in the DGT technology.
Above-mentioned purpose of the present invention is achieved through the following technical solutions: a kind of phosphorus fixing film that is applied to diffusive gradients in thin-films measurement technology, be provided with the fixedly structure of film and diffusion barrier stack in the diffusive gradients in thin-films measurement technology, ion passes diffusion barrier with diffusion way, the film that is fixed is immediately caught, and the formation linear gradient distributes on diffusion barrier, it is characterized in that: the phosphorus fixing film of catching phosphonium ion is the material of absorption phosphorus with the zirconium dioxide, by third rare acid amides Zirconium dioxide powder is made gel film.
With Zirconium dioxide powder and acrylamide solution 1: 1.5～1: 4 mixing of pressing mass volume ratio, the ammonium persulfate that adds tetramethyl diethylamine (TEMED) and mass ratio 10% again by 1/3600～1/900 and 1/144～1/36 of acrylamide volume respectively, behind the mixing its slow injection is accompanied the two glass sheets spaces that u moulds the material thin slice, after catching up with bubble to the greatest extent, glass plate horizontal positioned 2～4 hours under 10～15 ℃ of low temperature, after treating zirconium powder free setting, be warming up to 30～35 ℃, make after the solution gel film forming, glass plate is pried open, take out gel film, put into and be cut into required form after the deionized water immersion is no less than 10 hours, be used for the assembling and the analysis of DGT determination techniques.
Said Zirconium dioxide powder is by zirconium oxychloride (ZrClO
28H
2O) aqueous solution and ammoniacal liquor mix to dispose and form, mixed solution pH reaches and is stabilized in 6～8, the precipitate with deionized water that is produced is washed 3～4 times, wash 1～2 time with 80% ethanol again, supernatant is removed in centrifugal back, with hair-dryer its water percentage is dried up between 30～60%, clay into power with mortar.
Advantage of the present invention and beneficial effect:
(1) uses new material zirconium dioxide (ZrO
2) make phosphorus fixing film, substitute traditional iron film.Zirconium dioxide (ZrO
2) be a kind of white powder material, have water insoluble, high-temperature heat-resistance, characteristics that chemical property is stable.Now be mainly used in fire resistive material and special cermacis field, ZrO
2Open report is not seen in application in the DGT technology as yet as the phosphorus sorbing material.Key is the fixedly preparation of film, is not that Zirconium dioxide powder and third rare amide solution simply are mixed into glue, need consider intensity and adsorption capacity after operability, the film forming simultaneously.Prepare fixedly film as the moistening zirconium dioxide of direct use water cut more than 95%, when addition was big slightly, because glutinousness is big, zirconium dioxide and third rare acid amides mixed liquor can not be injected in the u-shaped glass plate holder seam smoothly, therefore do not have operability; When the fixing film of the Zirconium dioxide powder preparation that directly uses white drying, although addition can be very big, the fixedly film of making does not have absorption property to phosphonium ion.We discover, when the zirconium dioxide that uses water cut 30-60% prepares fixedly film, can inject film forming smoothly, and intensity after the film forming and adsorption capacity all reach best simultaneously.
(2) adsorption capacity height.This film (pH 5～9) under environment pH condition exceeds 4 times (Fig. 2) at least than iron film, satisfies the analysis requirement of DGT in the varying environment medium fully.
(3) easy operating.This film strength and stretching, extension superior performance, indeformable, easy fracture does not stick tube wall, satisfies the different requirements of analyzing fully.
(4) combine with other materials and can be made into composite membrane.When the system film, add materials such as AgI particle, resin cation, can carry out DGT to sulphur, heavy metal plasma in the surrounding medium simultaneously and analyze.
Description of drawings
Fig. 1 is the fixedly film and the diffusion barrier overlaying structure of DGT determination techniques;
Fig. 2 is to use the adsorption capacity contrast (adsorption capacity unit weight zirconium dioxide (dry weight) in film to contain) of the fixedly film of different water cut rate zirconium dioxide preparation to phosphate radical;
Fig. 3 be under the condition of different pH zirconium film of the present invention and iron film to the adsorption capacity contrast of phosphate radical;
Fig. 4 is to use that the DGT to Taihu Lake Sediment analyzes behind the zirconium film of the present invention.
Embodiment
Referring to Fig. 1, DGT determination techniques device is made up of the stack of fixedly film and diffusion barrier, and ion passes diffusion barrier with diffusion way, and the film that is fixed is immediately caught, and forms the linear gradient distribution on diffusion barrier.
Referring to Fig. 2, as can be seen from the figure, different water cut rate zirconium dioxide film exists obviously different to the adsorption capacity of phosphate radical, though Zirconium dioxide powder has certain adsorptive power to phosphate radical, but the adsorptive power of making behind the film significantly reduces, and the adsorption capacity of the zirconium dioxide film of water percentage 50% is maximum among the three.
Referring to Fig. 3, as can be seen from Figure, no matter under which kind of pH condition, the adsorption capacity of zirconium film is all apparently higher than the iron film.PH in the natural water or the soil liquid is between 5～9 (dash area) generally.In this pH interval, the adsorption capacity of zirconium film exceeds 4 times than iron film at least.
DGT analysis with Taihu Lake Sediment phosphorus is an example below, and the present invention will be further described.
Take by weighing 19.2g ZrClO
48H
2O (analyzing pure) fully is dissolved in the 600ml deionized water, slowly adds 25% ammoniacal liquor, stirs simultaneously, reaches and is stabilized in 7.0 until pH value of solution.With deionized water precipitation is washed 4 times, remove chlorion; With 80% ethanol precipitation is washed 2 times, supernatant is removed in centrifugal back again, will precipitate water cut with hair-dryer and blow between 45～55%, clays into power with mortar.The Zirconium dioxide powder and the 3.6ml acrylamide solution that 1.8g were prepared in 1: 2 by mass volume ratio mix, the ammonium persulfate that successively adds 2 μ l TEMED and 50 μ l mass ratioes 10%, slowly inject the space of two glass sheets behind the mixing, gap thickness moulds the material thin slice by u and is controlled at 0.4mm, after catching up with bubble to the greatest extent, the glass plate horizontal positioned, temperature is controlled at 10～15 ℃, makes the powder sedimentation 2～4 hours, is warming up to 30～35 ℃ then, after treating solution solidifies, glass plate is pried open, taken out gel film, put into the deionized water soaked overnight, be cut into definite shape then, be used for the assembling and the analysis of DGT device.The DGT device that the zirconium film is housed is inserted in the Taihu Lake Sediment, placed 24 hours, take out the zirconium film, be cut into the slice of width 3～4mm, put into the 2ml centrifuge tube, add 1ml 1M NaOH solution, vibrated 6 hours, analyze phosphorus concentration in the extract with colorimetric method, be converted into the fixed amount of zirconium film, be the diffusing capacity of different sediment depth profiled deposit thing phosphorus to the DGT device.As can be seen from Figure 4, the diffusing capacity of sediment lower floor phosphorus illustrates that apparently higher than the upper strata activity of lower floor's phosphorus is higher than the upper strata.
Claims (3)
1, a kind of phosphorus fixing film that is applied to diffusive gradients in thin-films measurement technology, be provided with the fixedly structure of film and diffusion barrier stack in the diffusive gradients in thin-films measurement technology, ion passes diffusion barrier with diffusion way, the film that is fixed is immediately caught, and the formation linear gradient distributes on diffusion barrier, it is characterized in that: the phosphorus fixing film of catching phosphonium ion is the material of absorption phosphorus with the zirconium dioxide, by third rare acid amides Zirconium dioxide powder is made gel film.
2, the phosphorus fixing film that is applied to diffusive gradients in thin-films measurement technology according to claim 1, it is characterized in that Zirconium dioxide powder and acrylamide solution by 1: 1.5～1: 4 mixing of mass volume ratio, the ammonium persulfate that adds tetramethyl diethylamine TEMED and mass ratio 10% again by 1/3600～1/900 and 1/144～1/36 of acrylamide volume respectively, behind the mixing its slow injection is accompanied the two glass sheets spaces that u moulds the material thin slice, after catching up with bubble to the greatest extent, glass plate horizontal positioned 2～4 hours under 10～15 ℃ of low temperature, after treating zirconium powder free setting, be warming up to 30～35 ℃, make after the solution gel film forming, glass plate is pried open, take out gel film, be cut into required form after putting into the deionized water soaked overnight.
3, the phosphorus fixing film that is applied to diffusive gradients in thin-films measurement technology according to claim 2 is characterized in that said Zirconium dioxide powder is by zirconium oxychloride ZrClO
28H
2O aqueous solution and ammoniacal liquor mixed configuration form, and mixed solution pH reaches and is stabilized in 6～8, and the precipitate with deionized water that is produced is washed 3～4 times, wash 1～2 time with 80% ethanol again, supernatant is removed in centrifugal back, with hair-dryer its water percentage is dried up between 30～60%, clays into power with mortar.
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