CN104048930B - Synchronization acquisition method of active phosphorus and iron in deposit - Google Patents

Synchronization acquisition method of active phosphorus and iron in deposit Download PDF

Info

Publication number
CN104048930B
CN104048930B CN201310078099.2A CN201310078099A CN104048930B CN 104048930 B CN104048930 B CN 104048930B CN 201310078099 A CN201310078099 A CN 201310078099A CN 104048930 B CN104048930 B CN 104048930B
Authority
CN
China
Prior art keywords
iron
phosphorus
film
fixing film
deposit
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201310078099.2A
Other languages
Chinese (zh)
Other versions
CN104048930A (en
Inventor
丁士明
陈义飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanjing Institute of Geography and Limnology of CAS
Original Assignee
Nanjing Institute of Geography and Limnology of CAS
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanjing Institute of Geography and Limnology of CAS filed Critical Nanjing Institute of Geography and Limnology of CAS
Priority to CN201310078099.2A priority Critical patent/CN104048930B/en
Publication of CN104048930A publication Critical patent/CN104048930A/en
Application granted granted Critical
Publication of CN104048930B publication Critical patent/CN104048930B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

A synchronization acquisition method of active phosphorus and iron in a deposit is disclosed; the principle of diffusive gradients in thin films (DGT) can be used, a fixing film and a diffusion film which are capable of performing phosphorus and iron synchronous enrichment are combined into a DGT acquisition device, the DGT acquisition device is put into the deposit for 2-6 days, active phosphorus and iron ions in the deposit pass through the diffusion film in a way of free diffusion, and then are acquired by the fixing film; after the DGT acquisition device is taken out, accumulation contents of phosphorus and iron on the fixing film can be respectively analyzed by use of a slicing-two step extraction-micro amount colorimetric method, and contents of the active phosphorus and iron in the deposit can be calculated by use of the Fick's first law of diffusion.

Description

The synchronous obtaining method of active phosphorus and iron in a kind of deposit
Technical field
The present invention relates to a kind of synchronous obtaining method to active phosphorus and iron in the surrounding mediums such as soil, deposit, can use The migratory activity of active phosphorus and iron, biological effectiveness, pollution risk and the Transport And Transformation relation of the two etc. in surrounding medium A+E.
Background technology
Diffusive gradients in thin-films (Diffusive Gradients in Thin Films, DGT) technology is a kind of new form Analytical technology, is mainly grown up in the mid-90 in last century by Lancaster university of Britain Davison and Zhang etc..Should Technology is based on ion diffusion principle, by object ion in the diffusion defining diffusion layer and association process research, obtains Ion activated information in media as well.The device of DGT determination techniques is made up of fixed bed and diffusion layer superposition, and ion is with diffused sheet Formula passes through diffusion layer, immediately fixed layer capture, and forms linear gradient distribution on diffusion layer, and it is near fixing film one end Ion concentration is maintained zero, contacts the concentration (C of one end with mediumDGT) be:
In above formula, M is accumulation (the mol cm of ion on fixing film-2), Δ g is thickness of diffusion layer (cm), DgExist for ion Diffusion rate (cm in diffusion barrier2s-1), t is diffusion time (s).CDGTStanding time section by DGT analysis obtain average Concentration (mol L-1).
Ion transfer in DGT diffusion process and actual environment and bioadsorption processes have comparativity, and this technology is As a kind of new morphological analysis means, gradually it is applied in water body, upper earth and deposit, research object is from conventional metal Element expands to yttrium and nonmetalloid etc..
At present, diffusive gradients in thin-films technology (DGT) has been applied to obtain the active phosphorus in deposit or iron content, does not also have Have and develop into the synchronous method obtaining phosphorus and iron.Because deposit has the special heterogeneity of highly significant, respectively obtain phosphorus and Iron content, does not only exist the deficiencies such as acquisition efficiency is low, cost is high, simultaneously because Existential Space dislocation, to the investigation of both sides relation Bring difficulty.
Content of the invention
It is an object of the invention to provide in a kind of deposit active phosphorus and iron synchronous obtaining method, the method be based on film Diffusion gradient (DGT) know-why, using the fixing film that can synchronously absorb phosphorus and iron, the synchronous active phosphorus obtaining in deposit Content and space distribution information with iron.
The above-mentioned purpose of the present invention is achieved through the following technical solutions:
The synchronous obtaining method of a kind of deposit active phosphorus and iron, it is characterised in that utilizing diffusive gradients in thin-films principle, is adopted Synchronously it is enriched with fixing film with phosphorus-iron and forms DGT device with diffusion barrier, put it into the work extracting in core sediments in deposit Property phosphorus and ferrous ion, in deposit, active phosphorus and ferrous ion pass through diffusion barrier in free diffusing mode, synchronous by fixing film Capture;To fix after film takes out, analyze amassing of phosphorus and iron on fixing film respectively using section-two step extractions-microcolorimetric methods Tired amount, is calculated the content of active phosphorus and iron in deposit according to Fick first diffusion law.
Described phosphorus-iron is synchronously enriched with fixing film, is by comprising hydronium(ion) zirconium oxide, Chelex-100 cation exchange tree The film forming sol of fat and polyacrylamide coagulates the gel film made;Fixing film surface depositing zirconium hydroxides and Chelex-100 sun Ion exchange resin.In described fixing film, the weight of hydronium(ion) zirconium oxide and Chelex-100 cationic ion-exchange resin is than for 1 : 0.6~1.
The fixing film that described phosphorus-iron is synchronously enriched with adopts following methods to make:By hydronium(ion) Zirconium oxide powder and Chelex-100 cationic ion-exchange resin and polyacrylamide solution are sufficiently mixed, and make uniform one-tenth film liquid, add appropriate After tetramethyl diethylamine and ammonium persulfate, by this one-tenth film liquid implantation glass mould, horizontal positioned under 2-4 DEG C of low temperature so that After zirconium hydroxide and Chelex-100 cationic ion-exchange resin free settling, then it is warming up to 45 ± 5 DEG C of placements, until film forming sol Congeal into film.
Described diffusion barrier, is to be made up of the polyacrylamide gel of moisture content 95%, thickness 0.4-1.2 millimeter it Between.
In the synchronous obtaining method of described deposit active phosphorus and iron, standing time in deposit for the DGT device is 2-6 days.
In the synchronous obtaining method of described deposit active phosphorus and iron, extract the active phosphorus in core sediments and ferrous iron After ion, on fixing film, the accumulation of phosphorus and iron is obtained using the method for section-two step extraction-microcolorimetric, and method is will be solid Determine the section that film is cut into strip or bulk by one-dimensional (vertical or horizontal) or two dimension (horizontal × vertical) direction, first use HNO3Solution Extract the iron that every piece of fixing film section (strip or bulk) above accumulates, then use and deoxygenate the section of every piece of water washing fixing film, then use NaOH solution extracts the accumulation phosphorus in every piece of fixing film section.In extract, the mensure of iron adopts Phen development process, and phosphorus is surveyed Surely adopt molybdenum blue colorimetric method, carry out colorimetric analysis with microplate spectrophotometer.
Described deposit active phosphorus and iron acquisition methods, specifically include following steps:
(1) phosphorus-iron is synchronously enriched with the preparation of fixing film:By the hydronium(ion) Zirconium oxide powder of 1g moisture content 50 ± 5% and 3~ Grind after the mixing of 5mL30% polyacrylamide solution, add the stirring of 0.6~1gChelex-100 cationic ion-exchange resin all Even, obtain into film liquid;Add the ammonium persulfate of 4~8 μ L tetramethyl diethylamine (TEMED) and 12~16 μ L10% (wt), mix Afterwards in space in uniform thickness between two glass sheets of implantation glass mould, bubble is caught up with to the greatest extent;Glass mold is under 2-4 DEG C of low temperature Horizontal positioned is more than half an hour, makes hydronium(ion) zirconium oxide and Chelex-100 Particle free is deposited to bottom and (is simultaneously downwards then The front of fixing film), then heat to 45 ± 5 DEG C, place more than half an hour, the film until film forming sol congeals into;Take out gel thin After film, put in deionized water and soak more than 24 hours, described phosphorus-iron is obtained and is synchronously enriched with fixing film;
(2) DGT device assembling:By phosphorus-iron, synchronously the fixing film of enrichment, diffusion barrier, nitrocellulose filter are sequentially overlapped rear group Dress up DGT device;
(3) nitrogen charging:DGT device is put in the container filling deionized water, is filled with pure nitrogen gas in water and removes DGT device In the oxygen that contains;
(4) DGT device is placed:DGT device is inserted perpendicularly in deposit, retains 3-5cm and be exposed in overlying water, place After 2-6 days, take out phosphorus-iron and be synchronously enriched with fixing film mark depositions-overlying water termination;
(5) fixing film section:Film will be fixed and take out fixation from device, to part below fixing film water/sediment interface, It is cut into the section of strip or bulk with slicer by one-dimensional (vertical or horizontal) or two dimension (horizontal × vertical) direction;
(6) iron extracts:After section, all fixing films are cut into slices and choose successively in centrifuge tube, then add to each centrifuge tube Appropriate 1M HNO3Solution, stands 16 hours;
(7) phosphorus extracts:The fixing film section having been extracted iron is chosen, and with deoxygenating water washing 2h, then is reentered into new In centrifuge tube, add appropriate 1M NaOH solution, stand 16 hours;
(8) ferrous colorimetric analysis:Draw appropriate stripping liquid from each centrifuge tube of step (6) micro- to 96 hole elisa Plates Kong Zhong, determines suitable extension rate, sequentially adds nitrite ion (nonyl phenol) and reducing agent, then 35 DEG C of constant temperature colour developings 30min, is then read the light absorption value of each micropore under 520nm wavelength, deducts this micropore by microplate spectrophotometer The absorbance of stripping liquid in each micropore is obtained after blank absorbency;
(9) phosphorus colorimetric analysis:Draw appropriate stripping liquid to 96 new hole elisa Plates from each centrifuge tube of step (7) In micropore, determine suitable extension rate, sequentially add 2M H2SO4Neutralization NaOH, is subsequently adding molybdenum blue colorimetric method nitrite ion, will Microwell plate after colour developing is put into after being centrifuged off bubble in centrifuge, then 35 DEG C of constant temperature colour developing 1h, then passes through microwell plate light splitting Photometer reads the light absorption value of each micropore under 700nm wavelength, obtains each micropore after the blank absorbency deducting this micropore The absorbance of middle stripping liquid;
(10) data processing:
Respectively the absorbance of stripping liquid is converted into the concentration of iron and phosphorus in stripping liquid according to iron or phosphorus development criteria curve, According to formula below, concentration conversion is become the accumulation of iron or phosphorus in every piece of fixing film section:
M=CV × 10-6
In above formula, C is the concentration of iron or phosphorus in each stripping liquid, and unit is μ g/L;V is the volume of stripping liquid, and unit is μ L;M is the accumulation of iron or phosphorus in every piece of fixing film section, and unit is μ g;
Further according to Fick First Law, the accumulation of iron or phosphorus is converted into iron or active phosphorus in deposit on corresponding section Content:
In above formula, Δ g is diffusion film thickness, and unit is cm;DgFor iron ion (Fe (- II)) or phosphate anion in diffusion Diffusion coefficient in film, unit is cm2/s;A is the area of fixing film section, and unit is cm2;T is standing time, and unit is the second, CDGTFor the concentration of active phosphorus or iron, unit is μ g/L;
Finally, according to each position in core sediments for the fixing film section, C can be madeDGTOne-dimensional or Two dimensional Distribution Figure.
Advantages of the present invention and beneficial effect include:
1. obtain content and the space distribution information of deposit active phosphorus and iron using a device simultaneously.DGT of the present invention Device applies the fixing film that can synchronously absorb phosphorus and iron, after putting it into deposit, can obtain the work of deposit simultaneously Property phosphorus and iron, by analyzing the fixed amount of phosphorus and iron on same fixing film, the content of synchronization gain deposit active phosphorus and iron and Space distribution information.
2. can scene in situ, nondestructive acquisition deposit active phosphorus and iron.At present to deposit active phosphorus and iron Acquisition, the overwhelming majority adopt destructive method, after deposit is taken out, by the methods such as chemical extraction obtain active phosphorus and Iron.Because deposit is chronically at reducing environment, inevitable oxidation by air after taking-up, causes sediment properties to occur very big Change, thus the active phosphorus that obtain of analysis and iron information have very large deviation.DGT device can directly be rendered to existing by the present invention , due to employing the passive acquiring technology of DGT, during acquisition, in device, it is heavy not destroy for deposit active phosphorus and iron Passive diffusion Long-pending thing reset condition, the therefore active phosphorus of acquisition and iron information are true and reliable.
3. the acquisition time of deposit active phosphorus and iron is short, and mensuration program is simply efficient.Traditional deposit passively obtains Take technology, such as Diffusion of interstitial water bascule etc., 20 days about are needed to the acquisition time of sediment phosphorus and iron.Using the present invention Method, the acquisition time only needs 2-6 days.After device takes out from deposit, using section-two step extraction-microcolorimetric methods When phosphorus on fixing film and iron are analyzed, disposably can process 96 section sample, each article colorimetric measures only needs 2 Minute.The operation sequence of above-mentioned analysis method is very simple, compared with traditional phosphorus, iron colorimetric estimation method, collects data Efficiency exceeds two orders of magnitude.
4. due in the inventive method DGT device obtain active phosphorus and iron using a fixing film simultaneously it is ensured that phosphorus and The spatial information of iron is derived from same position, it is to avoid the spatial offset currently being caused due to the asynchronous acquisition of element.Due to deposition Thing has the special heterogeneity of height, ferrophosphorus spatial information uniformity for investigate the two relation it is critical that.
Describe the present invention with reference to specific embodiment.Protection scope of the present invention is not to be embodied as Mode is limited, but is defined in the claims.
Brief description
Fig. 1 DGT know-why schematic diagram.
The DGT performance test that Fig. 2 the inventive method synchronously obtains to phosphorus in solution and iron.According to DGT principle, when DGT dress Put the object accumulation of acquisition and target concentration in solution is linearly incremented by, and during with theoretical calculation, then show this dress Put the requirement meeting DGT performance test.As illustrated, in the inventive method, phosphorus (Fig. 2A) and iron (Fig. 2 B) that DGT device obtains Accumulation and their concentration in the solution all assume straight line to be increased, and and theoretical calculation, show this device can be used for phosphorus and The DGT of iron synchronously obtains.
Taihu Lake Sediment section active phosphorus and the one-dimensional distribution map of iron that Fig. 3 is obtained by the inventive method, spatial discrimination Rate is 1mm.It is seen that deposit active phosphorus and iron have the phenomenon of synchronous rising in local location.
Specific embodiment
With example, the inventive method is further illustrated below in conjunction with the accompanying drawings.
DGT device in the inventive method is put in Lake Taihu deposit, takes out after 48 hours, transport experiment back Room, is analyzed to the phosphorus on fixing film and iron, is obtained in core sediments by the accumulation conversion of phosphorus and iron on fixing film The content of active phosphorus and iron and spatial distribution.
Described method concrete operations comprise the following steps:
(1) phosphorus-iron is synchronously enriched with the preparation of fixing film:By the hydronium(ion) Zirconium oxide powder of 1g moisture content 50 ± 5% and 3~ 5mL30% polyacrylamide solution mixes, and grinds, and adds the stirring of 0.6-1gChelex-100 cationic ion-exchange resin all Even, obtain into film liquid;Add the ammonium persulfate of 4-8 μ L tetramethyl diethylamine (TEMED) and 12-16 μ L10% (wt), after mixing In space in uniform thickness between two glass sheets of implantation glass mould, bubble is caught up with to the greatest extent;Glass mold water under 2-4 DEG C of low temperature Placing flat is more than half an hour, makes hydronium(ion) zirconium oxide and Chelex-100 Particle free is deposited to bottom (then one side is solid downwards Determine the front of film), then heat to 45 ± 5 DEG C, place more than half an hour, the film forming until film liquid is gelled;After taking out gel film, Put in deionized water and soak more than 24 hours, described phosphorus-iron is obtained and is synchronously enriched with fixing film.
(2) DGT device assembling:By phosphorus-iron, synchronously the fixing film of enrichment, diffusion barrier, nitrocellulose filter are sequentially overlapped rear group Dress up DGT device.
(3) nitrogen charging:DGT device is put in the container filling deionized water, is filled with pure nitrogen gas in water and removes DGT device In the oxygen that contains.
(4) DGT device is placed:DGT device is inserted perpendicularly in deposit, retains 3-5cm and be exposed in overlying water, place After 2-6 days, take out phosphorus-iron and be synchronously enriched with fixing film mark depositions-overlying water termination.
(5) fixing film section:Film will be fixed and take out fixation from device, to part below fixing film water/sediment interface, It is cut into the section of strip or bulk with slicer by one-dimensional (vertical) or two dimension (horizontal × vertical) direction.
(6) iron extracts:After section, fixing to all strips or square film section is chosen in centrifuge tube successively, then to every Individual centrifuge tube adds appropriate 1M HNO3Solution, stands 16 hours.
(7) phosphorus extracts:The section having been extracted iron is chosen, and adds and deoxygenates water washing 2h, then is reentered into new centrifugation Guan Zhong, adds appropriate 1M NaOH solution, stands 16 hours.
(8) ferrous colorimetric analysis:Draw appropriate stripping liquid from each centrifuge tube of step (6) micro- to 96 hole elisa Plates Kong Zhong, determines suitable extension rate, sequentially adds nitrite ion (nonyl phenol) and reducing agent, then 35 DEG C of constant temperature colour developings 30min, is then read the light absorption value of each micropore under 520nm wavelength, deducts this micropore by microplate spectrophotometer The absorbance of stripping liquid in each micropore is obtained after blank absorbency.
(9) phosphorus colorimetric analysis:Draw appropriate stripping liquid micro- to 96 new hole elisa Plates from each centrifuge tube of step (7) Kong Zhong, determines suitable extension rate, sequentially adds 2M H2SO4Neutralization NaOH, is subsequently adding nitrite ion, by the micropore after colour developing Plate is put into after being centrifuged off bubble in centrifuge, then 35 DEG C of constant temperature colour developing 1h, then passes through microplate spectrophotometer in 700nm Read the light absorption value of each micropore under wavelength, after the blank absorbency deducting this micropore, obtain the extinction of stripping liquid in each micropore Degree.
(10) data processing:
Respectively the absorbance of stripping liquid is converted into the concentration of iron and phosphorus in stripping liquid according to iron and phosphorus development criteria curve, According to formula below, concentration conversion is become the accumulation of iron and phosphorus in each strip or the fixing film of square:
M=CV × 10-6
In above formula, C is the concentration of iron or phosphorus in each micropore stripping liquid, and unit is μ g/L;V is the volume of stripping liquid, single Position is μ L;M is the accumulation of iron or phosphorus in every piece of section, and unit is μ g;
Further according to Fick First Law, the accumulation of iron or phosphorus is converted into the content of active iron or phosphorus in corresponding deposit:
In above formula, Δ g is diffusion film thickness, and unit is cm;DgFor iron ion (Fe (- II)) or phosphate anion in diffusion Diffusion coefficient in film, unit is cm2/s;A is the area of strip or square, and unit is cm2;T is standing time, and unit is the second, CDGTFor the concentration of active phosphorus or iron, unit is μ g/L.
Finally, according to each position in core sediments for the fixing film section, make CDGTOne-dimensional or Two dimensional Distribution Figure.

Claims (8)

1. the synchronous obtaining method of a kind of deposit active phosphorus and iron, it is characterised in that utilizing diffusive gradients in thin-films principle, adopts Phosphorus-iron is synchronously enriched with fixing film and forms DGT device with diffusion barrier, puts it into the activity extracting in core sediments in deposit Phosphorus and ferrous ion, in deposit, active phosphorus and ferrous ion pass through diffusion barrier in free diffusing mode, are synchronously caught by fixing film Obtain;The accumulation of phosphorus and iron on fixing film after film taking-up will be fixed, is analyzed respectively using section-two step extraction-microcolorimetric methods Amount, is calculated the content of active phosphorus and iron in deposit according to Fick first diffusion law;
Described phosphorus-iron is synchronously enriched with fixing film, be by comprise hydronium(ion) zirconium oxide, Chelex-100 cationic ion-exchange resin and The film forming sol of polyacrylamide coagulates the gel film made, surface depositing zirconium hydroxides and Chelex-100 cation exchange tree Fat.
2. the synchronous obtaining method of deposit active phosphorus according to claim 1 and iron it is characterised in that described phosphorus- Iron is synchronously enriched with fixing film, and the weight of hydronium(ion) zirconium oxide and Chelex-100 cationic ion-exchange resin ratio is for 1: 0.6~1.
3. the synchronous obtaining method of deposit active phosphorus according to claim 1 and 2 and iron is it is characterised in that described Phosphorus-iron is synchronously enriched with fixing film and adopts following methods to make:By hydronium(ion) Zirconium oxide powder and Chelex-100 cation exchange Resin and polyacrylamide solution are sufficiently mixed, and make uniform one-tenth film liquid, add appropriate tetramethyl diethylamine and persulfuric acid After ammonium, by this film liquid implantation glass mould, horizontal positioned under 2~4 DEG C of low temperature is so that zirconium hydroxide and Chelex-100 are positive After ion exchange resin free settling, then it is warming up to 45 ± 5 DEG C of placements, until film forming sol congeals into film.
4. the synchronous obtaining method of deposit active phosphorus according to claim 1 and iron is it is characterised in that described diffusion Film is to be made up of the polyacrylamide gel of moisture content 95%, and thickness is between 0.4~1.2 millimeter.
5. the synchronous obtaining method of deposit active phosphorus according to claim 1 and iron is it is characterised in that described DGT fills Putting standing time in deposit is 2~6 days.
6. the synchronous obtaining method of deposit active phosphorus according to claim 1 and iron is it is characterised in that described cuts The method of piece-two step extraction-microcolorimetric, is the section that fixing film is cut into strip or bulk by one-dimensional or two-dimensional directional, first Use HNO3Solution extracts the iron in every piece of fixing film section, is cut with extracting every piece of fixing film with NaOH solution again after deoxidation water washing Phosphorus on piece;In extract, the mensure of iron adopts Phen development process, and phosphorus measures and adopts molybdenum blue colorimetric method, uses microwell plate light splitting Photometer carries out colorimetric analysis.
7. the synchronous obtaining method of deposit active phosphorus according to claim 1 and iron is it is characterised in that described method Comprise the following steps:
(1) phosphorus-iron is synchronously enriched with the preparation of fixing film:By the hydronium(ion) Zirconium oxide powder of 1g moisture content 50 ± 5% and 3~ 5mL30% polyacrylamide solution mixes, and grinds, and adds the stirring of 0.6~1g Chelex-100 cationic ion-exchange resin Uniformly, obtain into film liquid;Add 12~16 μ L10wt% ammonium persulfates and 4~8 μ L tetramethyl diethylamine, implantation glass after mixing In space in uniform thickness between two glass sheets of mould, bubble is caught up with to the greatest extent;Glass mold horizontal positioned under 2~4 DEG C of low temperature More than half an hour, make hydronium(ion) zirconium oxide and Chelex-100 Particle free be deposited to bottom, then heat to 45 ± 5 DEG C, put Put half an hour more than, the film until film forming sol congeals into;After taking out gel film, put in deionized water and soak more than 24 hours, Described phosphorus-iron is obtained and is synchronously enriched with fixing film;
(2) DGT device assembling:Phosphorus-iron is synchronously assembled into after the fixing film of enrichment, diffusion barrier, nitrocellulose filter are sequentially overlapped DGT device;
(3) nitrogen charging:DGT device is put in the container filling deionized water, is filled with water in pure nitrogen gas removal DGT device and contains Some oxygen;
(4) DGT device is placed:DGT device is inserted perpendicularly in deposit, retain 3~5cm be exposed in overlying water, place 2~ After 6 days, take out phosphorus-iron and be synchronously enriched with fixing film mark depositions-overlying water termination;
(5) fixing film section:Film will be fixed and take out fixation from device, to part below fixing film water/sediment interface, with cutting Piece knife is cut into the section of strip or bulk by one-dimensional or two-dimensional directional;
(6) iron extracts:After section, all fixing films are cut into slices and choose successively in centrifuge tube, then add to each centrifuge tube appropriate 1M HNO3Solution, stands 16 hours;
(7) phosphorus extracts:The fixing film section having been extracted iron is chosen, and with deoxygenating water washing 2h, then is reentered into new centrifugation Guan Zhong, adds appropriate 1M NaOH solution, stands 16 hours;
(8) ferrous colorimetric analysis:Draw appropriate stripping liquid to 96 hole elisa Plates micropores from each centrifuge tube of step (6) In, determine suitable extension rate, sequentially add nonyl phenol nitrite ion and reducing agent, then 35 DEG C of constant temperature colour developing 30min, so Read the light absorption value of each micropore afterwards by microplate spectrophotometer under 520nm wavelength, deduct the Blank absorbance of this micropore The absorbance of stripping liquid in each micropore is obtained after value;
(9) phosphorus colorimetric analysis:Draw appropriate stripping liquid to 96 new hole elisa Plates micropores from each centrifuge tube of step (7) In, determine suitable extension rate, sequentially add 2M H2SO4Neutralization NaOH, is subsequently adding molybdenum blue colorimetric method nitrite ion, will develop the color Microwell plate afterwards is put into after being centrifuged off bubble in centrifuge, then 5 DEG C of constant temperature colour developing 1h, then passes through microplate spectrophotometer Read the light absorption value of each micropore under 700nm wavelength, after the blank absorbency deducting this micropore, obtain desorption in each micropore The absorbance of liquid;
(10) data processing:
Respectively the absorbance of stripping liquid is converted into the concentration of iron and phosphorus in stripping liquid according to iron and phosphorus development criteria curve, according to Concentration conversion is become the accumulation of iron or phosphorus in every piece of fixing film section by formula below:
M=CV×10-6
In above formula, C is the concentration of iron or phosphorus in each stripping liquid, and unit is μ g/L;V is the volume of stripping liquid, and unit is μ L;M For the accumulation of iron or phosphorus in every piece of fixing film section, unit is μ g;
Further according to Fick First Law, the accumulation of iron or phosphorus is converted into containing of iron in deposit on corresponding section or active phosphorus Amount:
In above formula, Δ g is diffusion film thickness, and unit is cm;DgFor the ferrous ion or phosphate anion diffusion system in diffusion barrier Number, unit is cm2/s;A is the area of fixing film section, and unit is cm2;T is standing time, and unit is the second, CDGTFor active phosphorus Or the concentration of iron, unit is μ g/L.
8. the synchronous obtaining method of deposit active phosphorus according to claim 7 and iron is it is characterised in that described method In, step (10) also includes, according to each position in core sediments for the fixing film section, making CDGTOne-dimensional or two-dimentional point Butut.
CN201310078099.2A 2013-03-12 2013-03-12 Synchronization acquisition method of active phosphorus and iron in deposit Expired - Fee Related CN104048930B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310078099.2A CN104048930B (en) 2013-03-12 2013-03-12 Synchronization acquisition method of active phosphorus and iron in deposit

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310078099.2A CN104048930B (en) 2013-03-12 2013-03-12 Synchronization acquisition method of active phosphorus and iron in deposit

Publications (2)

Publication Number Publication Date
CN104048930A CN104048930A (en) 2014-09-17
CN104048930B true CN104048930B (en) 2017-02-22

Family

ID=51502050

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310078099.2A Expired - Fee Related CN104048930B (en) 2013-03-12 2013-03-12 Synchronization acquisition method of active phosphorus and iron in deposit

Country Status (1)

Country Link
CN (1) CN104048930B (en)

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104614331B (en) * 2015-01-27 2017-12-22 中国环境科学研究院 The method of organophosphor and Forms of Inorganic Phosphorus in extraction simultaneously and analyzing water body deposit
CN106198319A (en) * 2016-06-23 2016-12-07 中国科学院南京地理与湖泊研究所 A kind of method based on 8 kinds of oxidized form aniones of DGT Simultaneous Determination
CN107561025A (en) * 2017-07-20 2018-01-09 武汉纺织大学 A kind of method of quantitative determination iron-oxidizing bacteria to iron oxidability
CN109126473B (en) * 2018-10-11 2020-04-17 江南大学 In-situ forward osmosis membrane pollution relieving method based on calcium and magnesium ion removal
CN109883968A (en) * 2019-03-07 2019-06-14 长江水利委员会水文局 The method for quickly testing and analyzing phosphorus in water using microplate reader microcolorimetry high-volume
CN111060511B (en) * 2020-01-10 2022-07-19 南京国兴环保产业研究院有限公司 PO-DGT combined detection device and acquisition detection method for sediment nutrients
CN111175229A (en) * 2020-01-19 2020-05-19 厦门大学 In-situ detection device for dissolved Fe (II) and S (-II) in sediment section pore water and application thereof
CN113884643A (en) * 2021-08-19 2022-01-04 河海大学 Method for evaluating phosphorus release risk of deep water reservoir surface sediment

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102507471B (en) * 2011-10-23 2014-03-19 中国科学院南京地理与湖泊研究所 Method for acquiring two-dimensional distribution of sediment dissolved reactive phosphorus (DRP)
CN102507388A (en) * 2011-10-24 2012-06-20 河海大学 Improved phosphorus fixing film used in DGT (diffusive gradients in thin films) measurement and preparation method thereof

Also Published As

Publication number Publication date
CN104048930A (en) 2014-09-17

Similar Documents

Publication Publication Date Title
CN104048930B (en) Synchronization acquisition method of active phosphorus and iron in deposit
CN103743655B (en) Method for determining inorganic arsenic in soil or water body based on diffusive gradients in thin-films technique
CN102507471B (en) Method for acquiring two-dimensional distribution of sediment dissolved reactive phosphorus (DRP)
CN101629881B (en) Phosphorus fixing film applied to diffusive gradients in thin-films measurement technology
Nelson et al. Production and pelagic dissolution of biogenic silica in the Southern Ocean
Kolev et al. Mathematical modeling of the extraction of uranium (VI) into a polymer inclusion membrane composed of PVC and di-(2-ethylhexyl) phosphoric acid
Imboden et al. Natural radon and phosphorus as limnologic tracers: Horizontal and vertical eddy diffusion in Greifensee
CN109507177A (en) A method of colour developing monitoring available phosphorus in situ is carried out based on DGT technology
CN106289940A (en) A kind of method of quick mensuration soil organic matter content
CN111060511B (en) PO-DGT combined detection device and acquisition detection method for sediment nutrients
CN102879485B (en) Application method of retention indexes in identifying adulterated starch syrup in honey
CN106198319A (en) A kind of method based on 8 kinds of oxidized form aniones of DGT Simultaneous Determination
Horowitz et al. Reference phase analysis of free and bound intracellular solutes. I. Sodium and potassium in amphibian oocytes
CN101972414A (en) Method for establishing single-gastrodia capsule fingerprint and fingerprint thereof
CN102507262B (en) Device and method for acquiring and storing sediment pore water sample
CN104048924B (en) Two-dimensional high-resolution method for determination of distribution of active phosphorus in wetland soil and deposit
CN107930608A (en) A kind of dissolubility Phos, the preparation method of arsenic adsorbed film
CN109142612A (en) The measuring method of TMSP in lithium battery electrolytes
CN102866124A (en) Method for testing Fe<3+> content of lithium iron phosphate
CN104048956B (en) A kind of DGT method based on Computer-generated images densitometry technical measurement phosphorus content
CN101303276B (en) High precision in situ acquisition and analysis method of sediment clearance phosphorus in water
CN110763776B (en) LC-HG-AFS detection method of thioarsenate
Cohn et al. Metabolism of Tissue Cultures: III. A Method for Measuring the Permeability of Tissue Cells to Solutes
CN103207104B (en) Ferro element colouring method in a kind of plant
CN105572290A (en) Detection method of contents of monophosphate, biphosphonate and fatty alcohol-polyoxyethylene ether in phosphate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20170222

CF01 Termination of patent right due to non-payment of annual fee