CN103755997A - Preparation method and application of metal cation modified sodium alginate microsphere - Google Patents
Preparation method and application of metal cation modified sodium alginate microsphere Download PDFInfo
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- CN103755997A CN103755997A CN201310719441.2A CN201310719441A CN103755997A CN 103755997 A CN103755997 A CN 103755997A CN 201310719441 A CN201310719441 A CN 201310719441A CN 103755997 A CN103755997 A CN 103755997A
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Abstract
The invention discloses a preparation method and application of a metal cation modified sodium alginate microsphere in the technical fields of analysis and detection. The preparation method comprises the steps: with a CaCl2 solution as a crosslinking agent, dispersing a sodium alginate solution into the CaCl2 solution to obtain a sodium alginate microsphere; placing the sodium alginate microsphere into a GaCl3 solution or ZrCl4 solution to sufficiently react, and then, transferring the sodium alginate microsphere into an acetate buffer solution to obtain the metal cation modified sodium alginate microsphere; and finally, packing by using a wet process to obtain a packed column based on the modified sodium alginate microsphere. By using the preparation method, the existence of inorganic As (III) with a clear toxic effect in actual complex sample systems such as natural water, seawater and the like can be effectively analyzed.
Description
The application is that application number is 201110020757.3, the applying date is 2011.1.19, and denomination of invention is dividing an application of the arsenic compartment analysis packed column preparation method > > of < < based on modified sodium alginate microballoon.
Technical field
What the present invention relates to is a kind of method of analyzing monitoring technical field, is specially a kind of arsenic compartment analysis packed column preparation method based on metallic cation modified sodium alginate microballoon.
Background technology
Along with modern industrial and agricultural production development, the arsenic pollution problem serious threat human health day by day causing due to nature and human factor.Recently, in conjunction with the relevant drinking water quality standard regulation of American National environment administration (EPA), in China's water quality standard, total arsenic content has been revised as 10ngmL
-1.But because arsenic belongs to abnormal element, in natural stream networks, mainly with the arsenite (As (III)) of inorganic form and arsenate, (As (V) exists arsenic, wherein the environmental ecology toxicological effect of inorganic As (III) is much larger than inorganic As (V), on the morbidity impact of local arseniasis obviously, there is clear and definite carcinogenic toxicity.Therefore, cheap, the easy and simple to handle inorganic arsenic effectively of development cost compartment analysis packed column system, effectively to analyze inorganic As (III) content in the actual sample systems such as natural water, seawater, for arsenic pollution situation in science early warning environment, promote China's environmental monitoring level, conscientiously ensure people ' s health safety, obviously have important practical application of significance.Current paper data-searching result shows, Turkey Mustafa Tuzen study group utilizes it to test indoor biological culture extract and modifies after packed column, according to biological solanine composition in corresponding extract as avtive spot, trivalent arsenic in the separated natural water of selective enrichment under neutrallty condition, follow-up combination atomic spectrograph, effectively in compartment analysis natural water, inorganic trivalent arsenic and pentavalent arsenic exist, correlative study paper is to be entitled as " Selective speciation and determination of inorganic arsenic in water, food and biological samples " be published in " Food and Chemical Toxicology " (food and chemical toxicology, 2010, 48 volumes, the page number 41 – 46).But it is worthy of note, corresponding biological culture extract preparation process complexity is loaded down with trivial details, meanwhile, in concentration and separation operating process, harsh for the physico-chemical parameter conditional request of detection sample solution to be analyzed.
Sodium alginate (C
6h
7o
8na) n is mainly comprised of Lalgine sodium salt, it is as natural polysaccharide carbohydrate, it is a kind of macromolecular material with good thickening property, film-forming properties, stability, flocculence, chelating and Biosafety consistency, utilize calcium chloride as linking agent, can form and there is highly cross-linked cancellated sodium alginate micro ball, the follow-up ion exchange process that passes through, the different metal positively charged ions such as Fe (III) are introduced containing in Ca (II) sodium alginate micro ball structure, to prepare metallic cation modified sodium alginate microballoon.Because the metallic cations such as corresponding Fe (III) can be used as avtive spot, with thering is different selective coordination keying actions between inorganic As (III), pentavalent As (V), therefore, based on modified sodium alginate microballoon, can further develop and provide that preparation process is easy, with low cost, environmental friendliness is without the arsenic compartment analysis packed column of the advantages such as laboratory secondary pollution, effectively to meet actual analysis monitoring technical field needs.
Summary of the invention
The present invention is directed to prior art above shortcomings, a kind of arsenic compartment analysis packed column preparation method based on modified sodium alginate microballoon is provided, the packed column that the metallic cation modified sodium alginate microballoon of take is matrix, in conjunction with metallic cation with the coordination keying action that can provide between the arsenate chemical group of lone-pair electron structure, with fractionation by adsorption inorganic arsenic chemicals optionally, follow-up with corresponding analysis and detecting instrument coupling, the inorganic As (III) in the actual complex sample systems such as natural water, seawater scientificlly and effectively to analyze with clear and definite toxic action exists.
The present invention is achieved by the following technical solutions, and the present invention is with CaCl
2solution, as linking agent, is scattered in CaCl by sodium alginate soln
2in solution, obtain sodium alginate micro ball; Sodium alginate micro ball is placed in to FeCl
3solution, GaCl
3solution or ZrCl
4in solution, fully after reaction, be transferred in acetate buffer solution, obtain metallic cation modified sodium alginate microballoon, finally by wet method dress post, obtain the packed column based on modified sodium alginate microballoon.
The weight percent concentration of described sodium alginate soln is 1.0-3.0wt%;
Described CaCl
2the volumetric molar concentration of solution is 0.01-1.0mol/L;
Described dispersion refers to: adopt peristaltic pump, under 1.0-3.0mL/min flow velocity, sodium alginate soln is dropwise splashed into CaCl
2in solution, also at room temperature place 3 days.
Described FeCl
3the volumetric molar concentration of solution is 0.01-0.15mol/L;
The pH of described acetate buffer solution is 4.0;
Described dress post refers to: through wet method, metallic cation modified sodium alginate microballoon is packed in the pillar of silica glass, stainless steel or tetrafluoroethylene material, it is cotton and sealed at both ends that two ends are filled with Arsenic-free glass, obtains the packed column based on modified sodium alginate microballoon.
The invention has the advantages that: based on metallic cation modified sodium alginate microballoon, be column material first, arsenic compartment analysis packed column is prepared in development.It is easy, with low cost that this packed column system has preparation process, and environmental friendliness is avoided the advantages such as laboratory secondary pollution.
Embodiment
Below embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
1., take 2g without arsenic sodium alginate powder powder solid in 250mL beaker, add the pure water of 100mL mass spectrum, be placed in (60 ± 5 ℃ of bath temperatures, power 100W) concussion 6h in ultrasonator, it is fully dissolved, obtains 2%(weight percent) sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL0.1mol/LCaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.1mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 2.5%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=95%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 2
1., according to step in example 1,1. configure sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL0.01mol/LCaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.1mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 1.5%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 3
1., according to step in example 1,1. configure sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL1.0mol/L CaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.1mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 1.5%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 4
1., take 1g without arsenic sodium alginate powder powder solid in 250mL beaker, add the pure water of 100mL mass spectrum, be placed in (60 ± 5 ℃ of bath temperatures, power 100W) concussion 6h in ultrasonator, it is fully dissolved, obtains 3%(weight percent) sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 3mL/min flow velocity, dropwise splash into 500mL0.1mol/LCaCl
2in solution, be cross-linked and obtain diameter 4mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.1mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 4mm, iron level 1.5%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 5
1., take 3g without arsenic sodium alginate powder powder solid in 250mL beaker, add the pure water of 100mL mass spectrum, be placed in (60 ± 5 ℃ of bath temperatures, power 100W) concussion 6h in ultrasonator, it is fully dissolved, obtains 3%(weight percent) sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 3mL/min flow velocity, dropwise splash into 500mL0.1mol/LCaCl
2in solution, be cross-linked and obtain diameter 4mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.02mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 4mm, iron level 1.0%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=85%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 6
1., according to step in example 1,1. configure sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL0.1mol/L CaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.01mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 1.5%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 7
1., according to step in example 1,1. configure sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL0.1mol/LCaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.15mol/L FeCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and ferric ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 1.5%(weight percent), sorrel Fe (III) modified sodium alginate microballoon;
4., Fe (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 8
1., according to step in example 1,1. configure sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL0.1mol/LCaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.1mol/L GaCl be housed
3in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and trivalent gallium ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 1.5%(weight percent), sorrel Ga (III) modified sodium alginate microballoon;
4., Ga (III) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 9
1., according to step in example 1,1. configure sodium alginate soln;
2., make 1. sodium alginate soln by peristaltic pump, under 2mL/min flow velocity, dropwise splash into 500mL0.1mol/LCaCl
2in solution, be cross-linked and obtain diameter 2mm, white sodium alginate micro ball, is dispersed in corresponding CaCl
2in solution, at room temperature place 3 days (20 ℃ ± 5 ℃);
3., the sodium alginate micro ball 2. obtaining is cleaned repeatedly with the pure water of mass spectrum after, be submerged into 250mL0.1mol/L ZrCl be housed
4in the glass beaker of solution, under 100r/min condition, shaking table vibration is 3 days, and tetravalence zirconium ion is incorporated in sodium alginate micro ball structure as avtive spot.With the pure water of mass spectrum, repeatedly clean afterwards, to supernatant liquor, be neutral, corresponding sodium alginate micro ball is moved in 250mL pH=4 acetate buffer solution, continuation is shaking table vibration 12h under 100r/min, prepare diameter 2mm, iron level 1.5%(weight percent), sorrel Zr (IV) modified sodium alginate microballoon;
4., Zr (IV) the modified sodium alginate microballoon 5.0g for preparing in taking 3., with wet method dress post, packing column internal diameter into is 0.8cm, length is in the filling separator column of tetrafluoroethylene material of 15.0cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
5., the filling separator column obtaining in is 4. connected with peristaltic pump.Pass through peristaltic pump, make 4.0mL, the water sample solution that contains 100 μ g/LAs (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and the analytical results of corresponding atomic spectrograph shows: the inorganic As (V) in corresponding water sample solution is adsorbed (adsorption efficiency >=90%) by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out and fills separator column and obtain analyzing and testing exactly.
Embodiment 10
1., according to the 1. 2. 3. 4. step preparation filling separator column based on Fe (III) modified sodium alginate microballoon in example 1;
2., take 5.0g modified sodium alginate microballoon, with wet method dress post, packing column internal diameter into is 0.8cm, in the separated packed column of the glass material that length is 15cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
3., the filling separator column obtaining in is 2. connected with peristaltic pump.Pass through peristaltic pump, the mixing water sample solution that makes 4.0mL contain 100 μ g/L As (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and follow-up atomic spectrograph analytical results shows: in corresponding water sample solution, inorganic As (V) is adsorbed (adsorption efficiency >=95%) by selectivity in post; In corresponding water sample solution, inorganic As (III) non-selectivity in packed column retains, and directly flows out cylinder and obtain accurate analysis to detect.
Embodiment 11
1., according in example 1 1. 2. 3. step prepare Fe (III) modified sodium alginate microballoon;
2., take modified sodium alginate microballoon 5.0g, with wet method dress post, packing column internal diameter into is 0.8cm, in the separated packed column of the stainless steel that length is 15cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
3., corresponding filling separator column is connected with peristaltic pump.Pass through peristaltic pump, the mixing water sample solution that makes 4.0mL contain 100 μ g/L As (V) and 20 μ g/L As (III) flows through packed column with flow velocity 1.2mL/min, the sample solution after post is flow through in collection, and follow-up atomic spectrograph analytical results shows: in corresponding water sample solution, inorganic As (V) is adsorbed (adsorption efficiency >=95%) by selectivity in post; In corresponding water sample solution, inorganic As (III) non-selectivity in filling separator column retains, and directly flows out cylinder and obtain accurate analysis to detect.
Embodiment 12
1., according in example 1 1. 2. 3. step prepare based on Fe (III) modified sodium alginate microballoon;
2., take modified sodium alginate microballoon 5.0g, with wet method dress post, packing column internal diameter into is 0.8cm, in the separated packed column of the tetrafluoroethylene that length is 15cm, it is cotton that a little Arsenic-free glass is filled at post two ends, screws post two ends nut, stand-by;
3., corresponding filling separator column is connected with peristaltic pump.By peristaltic pump, make the seawater sample solution that 4.0mL contains 100 μ g/L As (V) and 20 μ g/L As (III) (take artificial seawater as background, artificial seawater formula: 26.726g/L NaCl, 2.260g/L MgCl
2, 3.248g/L MgSO
4, 1.153g/L CaCl
2, 0.198g/L NaHCO
30.721g/L KCl) with flow velocity 1.2mL/min, flow through packed column, the sample solution after post is flow through in collection, and follow-up atomic spectrograph analytical results shows: in corresponding seawater sample solution, inorganic As (V) is adsorbed (adsorption efficiency>=95%) by selectivity in post; In corresponding water sample solution, inorganic As (III) non-selectivity in filling separator column retains, and directly flows out cylinder and obtain accurate analysis to detect.
Claims (10)
1. a preparation method for metallic cation modified sodium alginate microballoon, is characterized in that, with CaCl
2solution, as linking agent, is scattered in CaCl by sodium alginate soln
2in solution, obtain sodium alginate micro ball; Sodium alginate micro ball is placed in to GaCl
3solution or ZrCl
4in solution, fully after reaction, be transferred in acetate buffer solution, obtain metallic cation modified sodium alginate microballoon.
2. the preparation method of metallic cation modified sodium alginate microballoon according to claim 1, is characterized in that, described sodium alginate soln weight percent concentration is 1.0-3.0wt%.
3. the preparation method of metallic cation modified sodium alginate microballoon according to claim 2, is characterized in that, described CaCl
2the volumetric molar concentration of solution is 0.01-1.0mol/L.
4. the preparation method of metallic cation modified sodium alginate microballoon according to claim 3, is characterized in that, described GaCl
3the concentration of solution is 0.01-0.15mol/L.
5. the preparation method of metallic cation modified sodium alginate microballoon according to claim 3, is characterized in that, described ZrCl
4the concentration of solution is 0.01-0.15mol/L.
6. according to the preparation method of the metallic cation modified sodium alginate microballoon described in claim 1-5 any one, it is characterized in that, described dispersion balling-up process refers to: adopt peristaltic pump, under 1.0-3.0mL/min flow velocity, sodium alginate soln is dropwise splashed into CaCl
2in solution, also at room temperature place 3 days.
7. the preparation method of metallic cation modified sodium alginate microballoon according to claim 6, is characterized in that, the pH of described acetate buffer solution is 4.0.
8. an application for metallic cation modified sodium alginate microballoon, is characterized in that: using metallic cation modified sodium alginate microballoon as column material, prepare arsenic compartment analysis packed column, and for arsenic compartment analysis;
The preparation of described metallic cation modified sodium alginate microballoon: with CaCl
2solution, as linking agent, is scattered in CaCl by sodium alginate soln
2in solution, obtain sodium alginate micro ball; Sodium alginate micro ball is placed in to GaCl
3solution or ZrCl
4in solution, fully after reaction, be transferred in acetate buffer solution, obtain metallic cation modified sodium alginate microballoon.
9. the application of metallic cation modified sodium alginate microballoon according to claim 8, it is characterized in that, described for arsenic compartment analysis, refer to: the arsenic compartment analysis packed column obtaining is connected with peristaltic pump, pass through peristaltic pump, make water sample solution stream cross packed column, collect and flow through the sample solution after post, adopt atomic spectrograph analysis: the inorganic As (V) in corresponding water sample solution is adsorbed by selectivity in post; Inorganic As (III) in corresponding water sample solution non-selectivity in filling separator column retains, and directly flows out arsenic compartment analysis packed column and obtains analyzing and testing exactly.
10. the application of metallic cation modified sodium alginate microballoon according to claim 8 or claim 9, it is characterized in that, the described arsenic compartment analysis packed column of preparing refers to: through wet method, metallic cation modified sodium alginate microballoon is packed in the pillar of silica glass, stainless steel or tetrafluoroethylene material, it is cotton and sealed at both ends that two ends are filled with Arsenic-free glass, obtains the packed column based on modified sodium alginate microballoon.
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| CN107573457A (en) * | 2017-08-30 | 2018-01-12 | 广州大学 | A kind of poly- N N-isopropylacrylamides of stephanoporate interpenetrating network/alginic acid zirconium gel ball and its preparation method and application |
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| CN104922933A (en) * | 2014-03-19 | 2015-09-23 | 中国科学院生态环境研究中心 | Inorganic arsenic separation method |
| CN106290346A (en) * | 2016-09-29 | 2017-01-04 | 浙江达美生物技术有限公司 | Mensuration reagent of superoxide dismutase and preparation method thereof |
| CN108905983A (en) * | 2018-07-19 | 2018-11-30 | 浙江工业大学 | A kind of preparation method of the Beta-cyclodextrin-based material of sodium alginate-for handling intermetallic composite coating waste water |
| CN109261138A (en) * | 2018-10-29 | 2019-01-25 | 浙江理工大学 | It is a kind of for heavy metal ion adsorbed ultrabranching polyamide modified sodium alginate microballoon and preparation method thereof |
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| KR100709557B1 (en) * | 2007-01-02 | 2007-04-20 | 한국과학기술연구원 | Method for fabrication of granular zirconium nano-mesostructure |
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| CN103736298A (en) | 2014-04-23 |
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