CN104614331A - Method for simultaneously extracting and analyzing forms of organic phosphorus and inorganic phosphorus in aquatic sediments - Google Patents
Method for simultaneously extracting and analyzing forms of organic phosphorus and inorganic phosphorus in aquatic sediments Download PDFInfo
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Abstract
The invention discloses a method for simultaneously extracting and analyzing forms of organic phosphorus and inorganic phosphorus in aquatic sediments, relates to the technical filed of environment, and solves the problems that the conventional phosphorus form extracting method cannot simultaneously measure the contents of the organic phosphorus and inorganic phosphorus in the aquatic sediments. The invention adopts the technical scheme as follows: mixing an aquatic sediment sample and a first extracting solution, centrifuging and filtering so as to obtain first residues and a first phosphorus extracting solution; mixing the first residues with a second extracting solution, centrifuging and filtering so as to obtain second residues and a second phosphorus extracting solution; mixing the second residues with a third extracting solution, oscillating, centrifuging and filtering so as to obtain third residues and a third phosphorus extracting solution; mixing the third residues with a fourth extracting solution, oscillating, centrifuging and filtering so as to obtain fourth residues and a fourth phosphorus extracting solution; ashing the fourth residues, mixing the ashed fourth residues with a fifth extracting solution, oscillating, centrifuging and filtering so as to obtain a fifth phosphorus extracting solution. By adopting the method, the contents of the organic phosphorus and inorganic phosphorus of different forms in the aquatic sediments can be accurately reflected.
Description
Technical field
The present invention relates to field of environmental technology, particularly relate to a kind of method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit.
Background technology
Phosphorus, as one of element crucial in freshwater lake ecosystem metabolism, is the key factor affecting lake eutrophication.After external source import is progressively controlled, in water body deposit, Endogenous Phosphorus is discharged in overlying water by effects such as the diffusion of Interstitial Water concentration difference, ion-exchange and bioturbations, maintains or deepen further the eutrophication in lake.But, be not that the phosphorus of all forms in water body deposit is all easy to be discharged in overlying water, when factors vary such as temperature, pH value, hydrodynamic condition and bioturbations, only the organic form phosphorus of the absorption of the particle surface such as activated Fe/Mn oxide, oxyhydroxide and clay mineral or co-precipitation, inorganic phosphorous spread to overlying water, and then affect the nutrition condition of water body.Therefore, in lake sediment, the form of phosphorus controls all tools be of great significance for the Transport And Transformation of phosphorus in lake, eutrphication mechanism research and eutrophication.
At present, many P form sequential extractions obtain utilization, and all achieve many achievements.Wherein, organophosphorus extracts main based on Ivanoff method, Bowman-Cole method, Golterman method, and Forms of Inorganic Phosphorus mainly contains Willimas method, Hendly method.
But the present inventor finds singlely to carry out abstraction and quantification for organophosphorus or Forms of Inorganic Phosphorus in above-mentioned extracting method, can not the content of organophosphorus and Phos in Simultaneously test water-outlet body sediment.
Summary of the invention
In view of this, the embodiment of the present invention provides a kind of method of organophosphorus and Forms of Inorganic Phosphorus in extraction simultaneously and analyzing water body sediment, and fundamental purpose is the content that simultaneously can analyze each form organophosphorus and Phos in water body deposit.
For achieving the above object, the present invention mainly provides following technical scheme:
On the one hand, embodiments provide a kind of method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit, comprise the steps:
Water body deposit sample is mixed with the first extract, vibrates, centrifugal and after filtering, obtain the first residue and the first phosphorus extract; Wherein, weakly stable state organophosphorus and weakly stable state Phos is contained in described first extract;
Described first residue is mixed with the second extract, vibrates, centrifugal and after filtering, obtain the second residue and the second phosphorus extract; Wherein, lateral reactivity Phos and lateral reactivity organophosphorus is contained in described second phosphorus extract;
Described second residue is mixed with the 3rd extract, vibrates, centrifugal and after filtering, obtain the 3rd residue and the 3rd phosphorus extract; Wherein, organophosphorus is extracted containing iron/aluminium in conjunction with state Phos and alkali in described 3rd phosphorus extract;
3rd residue is mixed with the 4th extract, vibrates, centrifugal and after filtering, obtain the 4th residue and the 4th phosphorus extract; Wherein, calcium is contained in described 4th phosphorus extract in conjunction with active organic phosphorus in state Phos and acid extractants;
By mixing with the 5th extract after the 4th residue ashing, vibrate, centrifugal and filter, obtain the 5th phosphorus extract; Wherein, residual form phosphorus is contained in described 5th phosphorus extract.
The aforesaid method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit, when the pH of described 3rd phosphorus extract is adjusted to 3.0-3.1, quiet heavy, obtain supernatant and precipitation; Wherein, active organic phosphorus in extracting containing alkali in described supernatant, extracts nonactive organophosphorus containing alkali in precipitation.
The aforesaid method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit, described first extract adopts concentration to be the ammonium chloride solution of 0.5-1mol/L;
Described second extract adopts concentration to be the sodium bicarbonate solution of 0.25-0.5mol/L;
Described 3rd extract adopts concentration to be the sodium hydroxide solution of 0.05-0.1mol/L;
Described 4th extract, the 5th extract all adopt concentration to be the HCL solution of 1-3.5mol/L.
The aforesaid method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit, also comprised before the step mixed by described first residue with the second extract: wash described first residue at least one times and by the withering step of described first residue with ultrapure water or saturated sodium chloride solution;
Also is comprised before the step that described second residue is mixed with the 3rd extract: wash described second residue at least one times and by the withering step of described second residue with ultrapure water or saturated sodium chloride solution;
Also is comprised before the step that described 3rd residue is mixed with the 4th extract: wash described 3rd residue at least one times and by the withering step of described 3rd residue with ultrapure water or saturated sodium chloride solution.
The aforesaid method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit, puts into muffle furnace ashing 2-4 hour at 500-600 DEG C by described 4th residue, then mixes with the 5th extract, vibrates, centrifugal, obtains the 5th phosphorus extract.
On the other hand, the while that embodiments of the invention providing a kind of, the method for organophosphorus and Forms of Inorganic Phosphorus in analyzing water body sediment, comprises the steps:
Adopt the method described in above-mentioned any one to extract the phosphorus of different shape in water body deposit sample, obtain the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract and the 5th phosphorus extract;
Determine iron/aluminium in the content of lateral reactivity Phos in the content of weakly stable state Phos in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract in conjunction with the content of calcium in the content of state Phos, the 4th phosphorus extract in conjunction with residual form phosphorus in the content of state Phos and the 5th phosphorus extract;
Determine the content of total phosphorus in the content of total phosphorus in the content of total phosphorus in the content of total phosphorus in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract;
Calculate the content of active organic phosphorus in acid extractants in the content of alkali extraction organophosphorus in the content of lateral reactivity organophosphorus in the content of weakly stable state organophosphorus in described first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract.
The method of organophosphorus and Forms of Inorganic Phosphorus in aforesaid Simultaneously test water body deposit, in described first phosphorus extract, the content of weakly stable state organophosphorus is the content of total phosphorus in the first phosphorus extract and the difference of weakly stable state content of inorganic phosphorus;
In described two phosphorus extracts, the content of lateral reactivity organophosphorus is the content of total phosphorus and the difference of lateral reactivity content of inorganic phosphorus in the second phosphorus extract;
In described 3rd phosphorus extract alkali extract the content of organophosphorus be the content of total phosphorus in the 3rd Phos solution in the 3rd phosphorus extract iron/aluminium in conjunction with the difference of state content of inorganic phosphorus;
In described 4th phosphorus extract, in acid extractants, the content of active organic phosphorus is the content of total phosphorus in the 4th Phos solution and the difference of calcium in conjunction with state content of inorganic phosphorus.
The method of organophosphorus and Forms of Inorganic Phosphorus in aforesaid Simultaneously test water body deposit, quiet heavy after when the pH of described 3rd phosphorus extract being adjusted to 3.0-3.1, obtain supernatant and precipitation; Wherein, during the alkali in described supernatant extracts, the content of active organic phosphorus comprises the steps:
Determine the content of the Phos in described supernatant and the content of total phosphorus;
In supernatant, the content of total phosphorus and the difference of content of inorganic phosphorus are the content of active organic phosphorus during alkali extracts.
The method of organophosphorus and Forms of Inorganic Phosphorus in aforesaid Simultaneously test water body deposit, according to alkali in described 3rd phosphorus extract extract alkali in the content of organophosphorus and described supernatant extract in the difference of active organic phosphorus, the alkali obtained in described precipitation extracts the content of nonactive organophosphorus.
Extract while the embodiment of the present invention proposes and chemical form that in analyzing water body sediment, the method for organophosphorus and Forms of Inorganic Phosphorus effectively can be separated Phos in water body deposit, organophosphorus simultaneously, and comparatively accurately reflect the content of each form organophosphorus and Phos in water body deposit, and the biological effectiveness of phosphorus and the analytical test needs of stability thereof can be taken into account.In the water body deposit that the embodiment of the present invention proposes, needed for the extraction of Paddy soil and content assaying method, sample size is little, analyzes extraction step few, decreases the loss of phosphorus in leaching process, save the time analyzing sample; The chemical reagent used in leaching process is simple and easy to get, and cost is little.
Accompanying drawing explanation
The process flow diagram of the extraction of Paddy soil in a kind of water body deposit that Fig. 1 provides for the embodiment of the present invention;
Fig. 2 is the schematic diagram of Forms of Inorganic Phosphorus distribution in one embodiment of the invention;
Fig. 3 is the schematic diagram of Organic phosphorus form distribution in another embodiment of the present invention.
Embodiment
For further setting forth the present invention for the technological means reaching predetermined goal of the invention and take and effect, below in conjunction with preferred embodiment, to a kind ofly extracting and its embodiment of method of organophosphorus and Forms of Inorganic Phosphorus, feature and effect thereof in analyzing water body sediment of proposing according to the present invention simultaneously, be described in detail as follows.
Because many P form chemical sequential methods of prior art only singlely can carry out abstraction and quantification for organophosphorus or Phos, the content of organophosphorus and Phos can not be gone out by Simultaneously test.Based on this, the present inventor proposes the abstraction and quantification method of Paddy soil in a kind of water body deposit, to realize Main Morphology and the content thereof that can distinguish organophosphorus and Phos simultaneously.
Machine phosphorus and Phos two kinds of forms are consisted predominantly of in water body deposit; Wherein, Forms of Inorganic Phosphorus is divided into: weakly stable state Phos (WA-P
i), lateral reactivity Phos (PA-P
i), iron or aluminium is in conjunction with state Phos (Fe/Al-P
i) and calcium in conjunction with state Phos (Ca-P
i).Organic phosphorus form is divided into: weakly stable state organophosphorus (WA-P
o), lateral reactivity organophosphorus (PA-P
o), middle active organic phosphorus (MA-P
o) and nonactive organophosphorus (NA-P
o).Wherein, active organic phosphorus (MA-P
o) comprise active organic phosphorus (MA in NaOH solution extraction
naOH-P
o) and hydrochloric acid extraction in active organic phosphorus (MA
hCl-P
o); Nonactive organophosphorus (NA-P
o) comprise NaOH solution and extract nonactive organophosphorus (NA
naOH-P
o) and residual form phosphorus (R-P
o).
On the one hand, embodiments of the invention propose a kind of method simultaneously extracting organophosphorus and Forms of Inorganic Phosphorus in water body deposit, comprise the steps:
1) water body deposit sample mixed with the first extract, vibrate, centrifugal and after filtering, obtain the first residue and the first phosphorus extract.
The water body deposit of this step by by sampling thief gather the sediment sample of top layer 2cm in research lake.
Preferably, this step is specially: water body deposit and the first extract are mixed to form potpourri, after regulating pH value to 7 ± 0.01 of potpourri, by potpourri at 25 DEG C after mechanical shaking extraction 2h, after the rotating speed centrifuging 10-30min of 8000-15000r/min, obtain the first residue and supernatant; The first phosphorus extract is obtained after supernatant being crossed 0.45 μm of glass fiber filter.Wherein, weakly stable state Phos (WA-P is contained in the weak first phosphorus extract that this step obtains
i) and weakly stable state organophosphorus (WA-P
o), solvent is water.
The first extract in this step is any one or a few the potpourri in ammonium chloride solution, sodium chloride solution and magnesium chloride solution.Preferred working concentration is the ammonium chloride solution of 1moL/L.
In order to accurately carry out the test of next step, with ultrapure water or saturated neutral salt solution wash the first residue at least one times after, be dried process.Preferred use saturated nacl aqueous solution.
2) the first residue mixed with the second extract, vibrate, centrifugal and after filtering, obtain the second residue and the second phosphorus extract.
This step is specially: after the 0.5-2h that vibrates with the potpourri of the second extract in the first residue, with the centrifugal 15-30min of the rotating speed of 1000-15000r/min, obtain the second residue and supernatant; The second phosphorus extract is obtained after supernatant being crossed 0.45 μm of glass fiber filter.Wherein, lateral reactivity organophosphorus (PA-P is contained in the second phosphorus extract that this step obtains
o) and lateral reactivity Phos (PA-P
i), solvent is water.
The second extract in this step is that (sequestrant comprises: disodium ethylene diamine tetraacetate, sodium citrate for sodium bicarbonate solution or sequestrant.), preferred working concentration is 0.5mol/L NaHCO
3solution.
In order to accurately carry out the test of next step, with ultrapure water or saturated sodium chloride solution wash the second residue at least one times after, be dried process.Preferred use saturated nacl aqueous solution.
3) by the second residue and the 3rd extract solution mixing, vibration, centrifugal and filter after, obtain the 3rd residue and the 3rd phosphorus extract.
Wherein, iron/aluminium is contained in the 3rd phosphorus extract in conjunction with state Phos (Fe/Al-P
i) and alkali extraction organophosphorus (alkali extraction organophosphorus comprises active organic phosphorus and alkali in alkali extraction and extracts nonactive organophosphorus).
This step is specially: add strong base solution to in the second residue after saturated nacl aqueous solution washing, the potpourri of the second residue and highly basic is vibrated after 10-20h, after the centrifugal 10-30min of the rotating speed of 8000-15000r/min, obtain the 3rd residue and supernatant.Three phosphorus extracts are obtained after supernatant being crossed 0.45 μm of glass fiber filter.
The 3rd extract in this step is sodium hydroxide solution, potassium hydroxide solution, and preferred working concentration is the sodium hydroxide solution of 0.1mol/L.If when strong base solution is the sodium hydroxide solution of 0.1mol/L, alkali extracts organophosphorus and is called that NaOH extracts organophosphorus, and NaOH extracts organophosphorus and comprises active organic phosphorus (MA in NaOH extraction
naOH-P
o) and NaOH extract nonactive organophosphorus (NA
naOH-P
o).
Preferably, in this step, after when the pH of the 3rd phosphorus extract being adjusted to 3.0-3.1 with the hydrochloric acid of 0.1mol/L, obtain supernatant and precipitation; Wherein, in precipitation, containing nonactive organophosphorus, (NaOH solution extracts nonactive organophosphorus (NA
naOH-P
o)).Obtain after adopting 0.45 μm of glass fiber filter to filter supernatant containing middle active organic phosphorus (NaOH solution extract in active organic phosphorus (MA
naOH-P
o)) extract.
In order to accurately carry out the test of next step, wash the 3rd residue at least one times with ultrapure water or saturated nacl aqueous solution.Preferred use saturated nacl aqueous solution.
4) the 3rd residue mixed with the 4th extract solution, vibrate, centrifugal and after filtering, obtain the 4th residue and the 4th phosphorus extract;
Wherein, calcium is contained in described 4th phosphorus extract in conjunction with state Phos (Ca-P
i) and acid extractants in active organic phosphorus (MA
hCl-P
o);
The 4th extract in this step is hydrochloric acid, and preferred working concentration is the hydrochloric acid solution of 1mol/L.
In order to accurately carry out the test of next step, with ultrapure water saturated sodium chloride solution washing the 4th residue at least one times after, be dried process.Preferred use saturated nacl aqueous solution.
5) the 4th residue is put into muffle furnace slag ashing 3 hours, then mixes with the 5th extract, vibrates, centrifugal and filter, obtain residual form phosphorus the 5th phosphorus extract; Wherein, main containing residual form phosphorus in the 5th phosphorus extract.
This step is specially: the 4th residue ashing process 2-4h at 500-600 DEG C in muffle furnace.After being mixed with the 5th extract by the 4th residue after ashing process, with the centrifugal 10-30min of the rotating speed of 8000-15000, obtain supernatant, supernatant obtains residue phosphorus extract after crossing 0.45 μm of glass fiber filter.Preferably, the preferred working concentration of the 5th extract in this step is the hydrochloric acid solution of 1mol/L.
The present invention is by providing the extracting method of Paddy soil in above-mentioned water body deposit, the Phos of the various forms in convenient research water body deposit and organophosphorus, and can realize measuring the Phos of various form and the content of organophosphorus in water body deposit simultaneously.
On the other hand, embodiments of the invention provide the content assaying method of Paddy soil in a kind of water body deposit, this assay method be the phosphorus of the different shape extracted based on said extracted method basis on carry out, specifically comprise the steps:
1) adopt said method to extract the phosphorus of different shape in water body deposit sample, obtain the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract and the 5th phosphorus extract;
2) iron/aluminium in the content of lateral reactivity Phos in the content of weakly stable state Phos in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract is determined in conjunction with the content of calcium in the content of state Phos, the 4th phosphorus extract in conjunction with residual form phosphorus in the content of state Phos, the 5th phosphorus extract;
3) content of total phosphorus in the content of total phosphorus in the content of total phosphorus in the content of total phosphorus in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract is determined;
4) content of active organic phosphorus in acid extractants in the content of alkali extraction organophosphorus in the content of lateral reactivity organophosphorus solution in the content of weakly stable state organophosphorus in described first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract is calculated;
Preferably, in described first phosphorus extract, the content of weakly stable state organophosphorus is the content of total phosphorus in the first phosphorus extract and the difference of weakly stable state content of inorganic phosphorus;
In described second phosphorus extract of diving, the content of lateral reactivity organophosphorus is the content of total phosphorus and the difference of lateral reactivity content of inorganic phosphorus in the second phosphorus extract;
In described 3rd phosphorus extract alkali extract the content of organophosphorus be the content of total phosphorus in the 3rd Phos solution in the 3rd phosphorus extract iron/aluminium in conjunction with the difference of state content of inorganic phosphorus;
In described 4th phosphorus extract, in acid extractants, the content of active organic phosphorus is the content of total phosphorus in the 4th Phos solution and the difference of calcium in conjunction with state content of inorganic phosphorus.
Preferably, quiet heavy after when the pH of described 3rd phosphorus extract being adjusted to 3.0-3.1, obtain supernatant and precipitation; Wherein, during the alkali in described supernatant extracts, the content of active organic phosphorus comprises the steps:
Determine the content of the Phos in described supernatant and the content of total phosphorus;
In supernatant, the content of total phosphorus and the difference of content of inorganic phosphorus are the content of active organic phosphorus during alkali extracts.
Preferably, according to alkali in described 3rd phosphorus extract extract alkali in the content of organophosphorus and described supernatant extract in the difference of active organic phosphorus, the alkali obtained in described precipitation extracts the content of nonactive organophosphorus.
Preferably, P-Mo blue spectrophotometric method is adopted to determine iron/aluminium in the content of lateral reactivity Phos in the content of weakly stable state Phos in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract respectively in conjunction with the content of calcium in the content of state Phos, the 4th phosphorus extract in conjunction with residual form phosphorus in the content of state Phos and the 5th phosphorus extract;
Preferably, the content of total phosphorus in the content of total phosphorus in total phosphorus content, the 3rd phosphorus extract in total phosphorus content in alkaline potassium per-sulfate digestion-P-Mo blue spectrophotometry first phosphorus extract, the second phosphorus extract, the 4th phosphorus extract is adopted;
Preferably, quiet heavy after when the pH of described 3rd phosphorus extract being adjusted to 3.0-3.1, adopt the content of Phos in P-Mo blue spectrophotometry supernatant, adopt the content of total phosphorus in alkaline potassium per-sulfate digestion-P-Mo blue spectrophotometry supernatant;
In addition, in said determination phosphorus extract total phosphorus step in, first the organophosphorus in extract is converted into Phos, adopts the content of total phosphorus in alkaline potassium per-sulfate digestion-P-Mo blue spectrophotometry supernatant.
In addition, utilize the data statisticss such as EXCEL, ORIGIN and analysis software, analyze its relative content and space distribution further.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
The present inventor is in Dec, 2013, and the water body deposit sample of 8 some position collection top layer 2cm in calabash shell serving as a dipper lake respectively with columnar sampler, each sampled point gathers 6 Duplicate Samples and on-the-spot mixing, 4 DEG C of preservations.Water body deposit is stored in sealed bag for subsequent use after-40 DEG C of freeze dryings, grinding, excessively 100 mesh sieves.
Above-mentioned collection 8 water body deposit samples are carried out respectively to the abstraction and quantification of Paddy soil according to following steps, the concrete process flow diagram implemented is shown in Figure 1, and detailed step is as follows:
Step 1, adds the NH that 50mL concentration is 1mol/L in 1g sediment sample
4cl solution, regulate pH to 7 ± 0.01, at 25 DEG C after mechanical shaking extraction 2h, centrifuging 20min under the rotating speed of 10000r/min, obtains the first residue and supernatant; Get after supernatant crosses 0.45 μm of glass fiber filter, obtain the first phosphorus extract, determine the weakly stable state Phos (WA-P in the first phosphorus extract
i) content and the amount of total phosphorus, obtain weakly stable state organophosphorus (WA-P in weakly stable state phosphorus extract by minusing
o) content.
Step 2, adds the saturated NaCl solution of 10mL in the first residue, and adding 50mL concentration after washing 2 times is 0.5mol/L NaHCO
3solution, vibration 1h, centrifugal 20min under the rotating speed of 5000r/min, obtains the second residue and supernatant, obtains the second phosphorus extract after supernatant being crossed 0.45 μm of glass fiber filter.Determine total phosphorus and lateral reactivity Phos (PA-P in the second phosphorus extract
i) content, obtain lateral reactivity organophosphorus (PA-P in the second phosphorus extract by minusing
o) content;
Step 3, adds the saturated NaCl solution of 10mL in the second residue, and adding 50mL concentration after washing 2 times is 0.1mol/L NaOH solution, and vibration 16h, centrifugal 20min under the rotating speed of 10000r/min, obtain the 3rd residue and supernatant; The 3rd phosphorus extract is obtained after supernatant being crossed 0.45 μm of glass fiber filter; 3rd phosphorus extract is divided into two parts.A total phosphorus and iron or the aluminium of measuring in the 3rd phosphorus extract is in conjunction with state Phos (Fe/Al-P
i), obtain the organophosphorus (NaOH-P in the 3rd phosphorus extract by minusing
o) content; Separately get the 3rd phosphorus extract 30mL, with concentration be 0.1mol/L HCl regulate pH=3.0, after producing layering, centrifugal 20min under the rotating speed of 5000r/min, measure the content of total phosphorus and Phos after the supernatant obtained being crossed 0.45 μm of filter membrane, obtain active organic phosphorus (MA in the 3rd phosphorus extract by minusing
naOH-P
o) content; Organophosphorus (NaOH-P is extracted by not regulating NaOH before pH
o) and regulate active organic phosphorus (MA in after pH=3
naOH-P
o) concentration difference can obtain NaOH extract nonactive organophosphorus (NA
naOH-P
0) content.
Step 4, the saturated NaCl solution of 10mL is added in the 3rd residue, 40 DEG C of oven dry after washing 2 times, adding 50mL concentration in the 3rd residue after drying to 0.5g is 1mol/L HCl solution vibration 16h, centrifugal 20min under the rotating speed of 10000r/min, obtain the 4th residue and supernatant, obtain the 4th phosphorus extract after supernatant being crossed 0.45 μm of glass fiber filter, in mensuration the 4th phosphorus extract, total phosphorus and calcium are in conjunction with state Phos (Ca-P
i) content, obtain active organic phosphorus (MA in hydrochloric acid extraction by minusing
hCl-P
o) content;
Step 5, the saturated NaCl solution of 10mL is added in the 4th residue, 40 DEG C of oven dry after washing 2 times, after taking 0.2g oven dry, the 4th residue is placed in crucible, and carries out ashing to the 4th residue at 550 DEG C, and adding concentration is 1mol/L HCl 20mL, centrifugal 20min under the rotating speed of 10000r/min, get after 0.45 μm of glass fiber filter crossed by supernatant and obtain the 5th phosphorus extract, measure the content of Phos in the 5th phosphorus extract, obtain residual form organophosphorus (R-P
o) content.
According to the content of Paddy soil and the quality of water body deposit sample in the volume of the Paddy soil extract of step measurements in embodiment 1, Paddy soil extract, calculate weakly stable state Phos in water body deposit, weakly stable state organophosphorus, lateral reactivity Phos, lateral reactivity organophosphorus, iron/aluminium extracts organophosphorus, calcium in conjunction with the content of active organic phosphorus in state Phos and acid extractants in conjunction with state Phos, alkali; Measurement result as shown in Figures 2 and 3.
As can be seen from Fig. 2 and Fig. 3, in the water body deposit that the embodiment of the present invention proposes, each form organophosphorus of Sequential extraction and organophosphorus are distributed with significant difference.Wherein, as shown in Figure 2.In water body deposit, Forms of Inorganic Phosphorus content is followed successively by Ca-P
i>Fe/Al-P
i>PA-P
i>WA-P
i, the relative scale of mean value is 30.45:15.97:11.25:1.00.As shown in Figure 3, in water body deposit, organic phosphorous content change is followed successively by R-P
o>NA
naOH-P
o>PA-P
o>MA
hCl-P
o>WA-P
o>MA
naOH-P
o, the relative scale of mean value is 17.98:4.81:4.49:3.99:1.27:1.00.
In addition, the embodiment of the present invention propose water body deposit in Paddy soil extraction measures total phosphorus with content assaying method with SMT method (the phosphorus detection method that European standard develops under testing council's framework), Phos is compared with the result of organophosphorus, total phosphorous recovery is between 93.34-112.10%, the Phos recovery is between 93.85-111.46%, and the organophosphorus recovery is between 76.36-119.86%.Can find out, on value, difference is less.Therefore in the water body deposit that proposes of the embodiment of the present invention, the extraction of Paddy soil and content assaying method can be widely used in separation and Extraction that is organic in fluviolacustrine deposit thing, suspension and Forms of Inorganic Phosphorus, and the relational expression of various Forms of Phosphorus can show bioavailability and the stability of sediment phosphorus preferably, to seek the P form directly affected lake eutrophication most.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (9)
1. extract a method for organophosphorus and Forms of Inorganic Phosphorus in water body deposit simultaneously, it is characterized in that, comprise the steps:
Water body deposit sample is mixed with the first extract, vibrates, centrifugal and after filtering, obtain the first residue and the first phosphorus extract; Wherein, weakly stable state organophosphorus and weakly stable state Phos is contained in described first phosphorus extract;
Described first residue is mixed with the second extract, vibrates, centrifugal and after filtering, obtain the second residue and the second phosphorus extract; Wherein, lateral reactivity Phos and lateral reactivity organophosphorus is contained in described second phosphorus extract;
Described second residue is mixed with the 3rd extract, vibrates, centrifugal and after filtering, obtain the 3rd residue and the 3rd phosphorus extract; Wherein, organophosphorus is extracted containing iron/aluminium in conjunction with state Phos and alkali in described 3rd phosphorus extract;
3rd residue is mixed with the 4th extract solution, vibrates, centrifugal and after filtering, obtain the 4th residue and the 4th phosphorus extract; Wherein, calcium is contained in described 4th phosphorus extract in conjunction with active organic phosphorus in state Phos and acid extractants;
By mixing with the 5th extract after the 4th residue ashing, vibrate, centrifugal and filter, obtain the 5th phosphorus extract; Wherein, residual form phosphorus is contained in described 5th phosphorus extract.
2. method according to claim 1, is characterized in that, when the pH of described 3rd phosphorus extract is adjusted to 3.0-3.1, quiet heavy, obtains supernatant and precipitation; Wherein, active organic phosphorus in extracting containing alkali in described supernatant, extracts nonactive organophosphorus containing alkali in precipitation.
3. method according to claim 1, is characterized in that, described first extract adopts concentration to be the ammonium chloride solution of 0.5-1mol/L;
Described second extract adopts concentration to be the sodium bicarbonate solution of 0.25-0.5mol/L;
Described 3rd extract adopts concentration to be the sodium hydroxide solution of 0.05-0.1mol/L;
Described 4th extract, the 5th extract all adopt concentration to be the HCL solution of 1-3.5mol/L.
4. method according to claim 1, it is characterized in that, is also comprised before the step that described first residue is mixed with the second extract: wash described first residue at least one times and by the withering step of described first residue with ultrapure water or saturated sodium chloride solution;
Also is comprised before the step that described second residue is mixed with the 3rd extract: wash described second residue at least one times and by the withering step of described second residue with ultrapure water or saturated sodium chloride solution;
Also is comprised before the step that described 3rd residue is mixed with the 4th extract: wash described 3rd residue at least one times and by the withering step of described 3rd residue with ultrapure water or saturated sodium chloride solution.
5. method according to claim 1, is characterized in that, described 4th residue is put into muffle furnace ashing 2-4 hour at 500-600 DEG C, then mixes with the 5th extract, vibrate, centrifugal, obtains the 5th phosphorus extract.
6. the simultaneously method of organophosphorus and Forms of Inorganic Phosphorus in analyzing water body sediment, is characterized in that, comprise the steps:
Adopt the method described in any one of claim 1-5 to extract the phosphorus of different shape in water body deposit sample, obtain the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract and the 5th phosphorus extract;
Determine iron/aluminium in the content of lateral reactivity Phos in the content of weakly stable state Phos in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract in conjunction with the content of calcium in the content of state Phos, the 4th phosphorus extract in conjunction with residual form phosphorus in the content of state Phos and the 5th phosphorus extract;
Determine the content of total phosphorus in the content of total phosphorus in the content of total phosphorus in the content of total phosphorus in the first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract;
Calculate the content of active organic phosphorus in acid extractants in the content of alkali extraction organophosphorus in the content of lateral reactivity organophosphorus in the content of weakly stable state organophosphorus in described first phosphorus extract, the second phosphorus extract, the 3rd phosphorus extract, the 4th phosphorus extract.
7. method according to claim 6, is characterized in that,
In described first phosphorus extract, the content of weakly stable state organophosphorus is the content of total phosphorus in the first phosphorus extract and the difference of weakly stable state content of inorganic phosphorus;
In described two phosphorus extracts, the content of lateral reactivity organophosphorus is the content of total phosphorus and the difference of lateral reactivity content of inorganic phosphorus in the second phosphorus extract;
In described 3rd phosphorus extract alkali extract the content of organophosphorus be the content of total phosphorus in the 3rd Phos solution in the 3rd phosphorus extract iron/aluminium in conjunction with the difference of state content of inorganic phosphorus;
In described 4th phosphorus extract, in acid extractants, the content of active organic phosphorus is the content of total phosphorus in the 4th Phos solution and the difference of calcium in conjunction with state content of inorganic phosphorus.
8. method according to claim 7, is characterized in that, quiet heavy after when the pH of described 3rd phosphorus extract being adjusted to 3.0-3.1, obtains supernatant and precipitation; Wherein, during the alkali in described supernatant extracts, the content of active organic phosphorus comprises the steps:
Determine the content of the Phos in described supernatant and the content of total phosphorus;
In supernatant, the content of total phosphorus and the difference of content of inorganic phosphorus are the content of active organic phosphorus during alkali extracts.
9. method according to claim 8, is characterized in that, according to alkali in described 3rd phosphorus extract extract alkali in the content of organophosphorus and described supernatant extract in the difference of active organic phosphorus, the alkali obtained in described precipitation extracts the content of nonactive organophosphorus.
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