CN109632448A - A kind of concentration and separation method of colloid phosphorus in soil - Google Patents
A kind of concentration and separation method of colloid phosphorus in soil Download PDFInfo
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- CN109632448A CN109632448A CN201811428937.3A CN201811428937A CN109632448A CN 109632448 A CN109632448 A CN 109632448A CN 201811428937 A CN201811428937 A CN 201811428937A CN 109632448 A CN109632448 A CN 109632448A
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- phosphorus
- colloid
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4055—Concentrating samples by solubility techniques
Abstract
The invention discloses a kind of concentration and separation method of colloid phosphorus in soil, this method mainly comprises the steps that S1: weighing the soil sample of sieving in conical flask, adds deionized water, extracts；S2: extraction supernatant is centrifuged 10~12min in advance at 3000~3500g to remove bulky grain, and the supernatant after taking pre- centrifugation is filtered with 1 μm of miillpore filter, collects all filtrates after discarding primary filtrate；S3: above-mentioned filtrate is put into the super filter tube of 3KDa, and 30~40min of ultracentrifugation under 4000g takes supernatant；Wherein supernatant is the true dissolved phosphorus component for removing gel component, and ultrafiltration bottom of the tube is water diffusivity colloid phosphorus concentrate.The present invention provides a kind of simple and effective colloid phosphorus to be concentrated and separated method, is improved traditional Gravity Separation and field flow separation method, greatly simplifies colloid phosphorus measurement analytical procedure, shortens minute.
Description
Technical field
The invention belongs to soil nutrients to monitor field, be related to colloid knot in a kind of method concentration and separation soil using ultrafiltration
Close the new method of phosphorus.
Background technique
Phosphorus is important one of bioactive elemements, and soil phophorus library not only directly affects soil fertility and agricultural production, and also because
Phosphorus levels cause water eutrophication problem to take place frequently and cause environmental area and social extensive concern.In recent years,
With a large amount of investments of chemical fertilizer, the P elements in soil are largely accumulated, research shows that the cumulant of soil phophorus is considerably beyond making
The demand of object.Traditional view think the loss of phosphorus in soil mainly due to chemical fertilizer application result in dissolved phosphorus in soil with
Rainwater and irrigation water and flow into water body.But recent studies indicate that, migration from soil phosphorus to water body actually with soil
Earth colloid phosphorus particle is closely related.Soil colloid is particle of the partial size between 1nm to 1 μm, generally includes iron, alumina
The inorganic colloid of the mineral compositions such as object, clay mineral, the organic colloids such as organic macromolecule, microorganism and mineral and organic matter are handed over
The organo mineral colloidal complex mutually formed is widely present in soil and water body environment.Since soil colloid partial size is small, specific surface
Product is big, and reactivity waits by force physicochemical properties, can have stronger mobility in soil liquid long-term suspension, be Department of Soil
The main path that pollutant is migrated to water body in system.Soil colloid phosphorus, that is, the nothings such as soil phophorus and iron/aluminum oxide, clay mineral
Machine mineral gels, the organic colloids such as organic macromolecule, microorganism and Organic-inorganic composite colloid combine the one kind formed thin
Particle cluster flow.Colloid is the important carrier of the nutrients long-distance migration such as phosphorus, and colloid easily changes migration and has been found to be that soil is molten
The important channel that phosphorus element is migrated in liquid, surface water body and agricultural non-point source pollution
But the determination method about soil colloid combination phosphorus is also very deficient, currently, the analysis method of colloid phosphorus is main
There are gravity centrifugal separation and field flow partition method.Wherein, gravity concentration partition method needs low under the centrifugal force of 300 000g
Temperature centrifugation 2h, entire step and its cumbersome need to use expensive Ultracentrifuge, and consumptive materials such as centrifuge tube and its high
It is expensive, it measures 1 sample average and needs 4h, it is time-consuming and laborious.It is a kind of for macromolecular (large biological molecule and synthesis height that field flow, which separates,
Molecule), colloid, the isolated technology such as nano particle.The basic principle is that macromolecular flows through flat channel, at the same by horizontal and
The flow field of vertical direction acts on；The relatively small molecule of size, the active force by vertical direction is smaller, and flat to flat channel center
Move diffusion；And relatively large sized molecule, the active force by vertical direction is larger and is closer to wall.To in Vertical Square
To formation size gradient.And fluid, in flat channel, closer to center, flow velocity is faster, and closer to edge, flow velocity is more equal
It is even, it is slower.Therefore, the relatively small component of size is first detected by rear end detector；And the subsequent quilt of the component of larger size
Detection.To achieve the purpose that separation.Although the method effect of field flow separation is also relatively good, it also needs to use expensive
Field flow separator, price 50-100 ten thousand differs.
Therefore, the detection and analysis cost and time-consuming for how reducing soil colloid combination phosphorus are that the present invention is urgently to be resolved
Technical problem.
Summary of the invention
It is an object of the invention to solve colloid phosphorus in the prior art to be concentrated and separated existing defect, and provide a kind of utilization
The new method of the method concentration and separation colloid combination phosphorus of ultrafiltration.
Specific technical solution of the present invention is as follows:
A kind of concentration and separation method of colloid phosphorus in soil comprising following steps:
S1: weighing the soil sample of sieving in conical flask, add deionized water, extraction；
S2: extraction supernatant is centrifuged 10~12min to remove bulky grain, after taking pre- centrifugation in advance at 3000~3500g
Supernatant is filtered with 1 μm of miillpore filter, collects all filtrates after discarding primary filtrate；
S3: above-mentioned filtrate is put into the super filter tube of 3KDa, and 30~40min of ultracentrifugation under 4000g takes supernatant；Its
Middle supernatant is the true dissolved phosphorus component for removing gel component, and ultrafiltration bottom of the tube is water diffusivity colloid phosphorus concentrate.
Preferably, the soil sample is without the soil sample for grinding and crossing 8mm sieve.
Preferably, soil sample is mixed with deionized water with Tu Shui ratio 1:8 in step S1, then move in shaking table, 150
Under~160rpm extraction 16~for 24 hours.
Preferably, the amount of discarding of primary filtrate is 5mL in step S2.
Preferably, the concentration dimensions of colloid phosphorus are 3KDa-1 μm.
The invention has following technical advantage:
The concentration and separation time of colloid phosphorus is reduced to each sample by average each sample 4h of original Gravity Separation method
Product 20min, it is no longer necessary to expensive ultracentrifugation equipment.
Specific embodiment
The present invention is further elaborated and is illustrated With reference to embodiment.Each embodiment in the present invention
Technical characteristic can carry out the corresponding combination under the premise of not conflicting with each other.
In order to enable those skilled in the art to better understand specific measuring method of the invention, below with reference to specific
The present invention is further described for case study on implementation, but lifted case is not as the limitation of the invention.
Embodiment 1:
3 parts of 0-20cm soil are acquired from Zhejiang Province's Tonglu County, after taking back laboratory, soil natural is air-dried, is weighed to be measured
Not ground soil sample crosses 8mm sieve, is put into 250ml conical flask, adds deionized water, and Tu Shui ratio 1:8 is moved in shaking table,
It is extracted for 24 hours under 160rpm.Extraction supernatant is centrifuged supernatant of the 12min to remove bulky grain, after taking pre- centrifugation in advance at 3000g
Liquid is filtered with 1 μm of miillpore filter, is collected all filtrates after discarding 5mL primary filtrate, is denoted as supernatant I.By supernatant I directly into
Row ultrafiltration, supernatant I are placed in the super filter tube of 3KDa, ultracentrifugation 30min under 4000g, take supernatant (being denoted as supernatant II),
Ultrafiltration bottom of the tube is water diffusivity colloid phosphorus concentrate.
Then the total phosphorus content in above-mentioned isolated supernatant is measured using molybdenum blue colorimetric method respectively.It is total in supernatant I
Phosphorus concentration subtracts the total phosphorus concentration of supernatant II, the colloid phosphorus concentration in as supernatant I.According to supernatant I and soil sample sample
Quantity relative ratio relationship, conversion obtain the colloid phosphorus content in soil sample sample.Measurement result in the present embodiment is as shown in table 1.
Table 1 is the comparison for the colloid phosphorus content that gravity separation method and above-mentioned ultrafiltration concentration separation method measure
As shown in Table 1, the colloid phosphorus content of the colloid phosphorus content of this method measurement and traditional Gravity Separation method measurement
Value is very close, and the colloid phosphorus average value of conventional method is 7.55mg/kg, and the colloid phosphorus average value of this method measurement is
7.73mg/kg.And the error of this method measurement only has 0.06mg/kg, much smaller than the 0.30mg/kg of conventional method.Therefore, our
Method has good detection stability, can efficiently separate and fast and accurately detect the colloid phosphorus in soil.
Embodiment 2:
Tea garden soil is acquired from Region of Kaihua County county, acquires 3 parts of 0-20cm soil layer soil, after taking back laboratory, certainly by soil
It so air-dries, weighs not ground soil sample to be measured, cross 8mm sieve, be put into 250ml conical flask, add deionized water, Tu Shui ratio 1:8 is moved
Into shaking table, 16h is extracted at 150rpm.Extraction supernatant be centrifuged 10min in advance at 3500g to remove bulky grain, take it is pre- from
Supernatant after the heart is filtered with 1 μm of miillpore filter, is collected all filtrates after discarding 5mL primary filtrate, is denoted as supernatant I.By supernatant
Liquid I directly carries out ultrafiltration, and supernatant I is placed in the super filter tube of 3KDa, and ultracentrifugation 40min under 4000g takes supernatant (to be denoted as
Supernatant II), ultrafiltration bottom of the tube is water diffusivity colloid phosphorus concentrate.
Then the total phosphorus content in above-mentioned isolated supernatant is measured using molybdenum blue colorimetric method respectively.It is total in supernatant I
Phosphorus concentration subtracts the total phosphorus concentration of supernatant II, the colloid phosphorus concentration in as supernatant I.According to supernatant I and soil sample sample
Quantity relative ratio relationship, conversion obtain the colloid phosphorus content in soil sample sample.Measurement result in the present embodiment is as shown in table 2.
Table 2 is the comparison for the colloid phosphorus content that gravity separation method and above-mentioned ultrafiltration concentration separation method measure
As shown in Table 2, the colloid phosphorus content of the colloid phosphorus content of this method measurement and traditional Gravity Separation method measurement
Numerical value is very close, and the colloid phosphorus average value of conventional method is 2.46mg/kg, and the colloid phosphorus average value of this method measurement is also
2.46mg/kg.And the error of this method measurement only has 0.05mg/kg, much smaller than the 0.23mg/kg of conventional method.Therefore, our
Method has good detection stability.It can efficiently separate and fast and accurately detect the colloid phosphorus in soil.
Above-mentioned embodiment is only a preferred solution of the present invention, so it is not intended to limiting the invention.Have
The those of ordinary skill for closing technical field can also make various changes without departing from the spirit and scope of the present invention
Change and modification.Therefore all mode technical solutions obtained for taking equivalent substitution or equivalent transformation, all fall within guarantor of the invention
It protects in range.
Claims (5)
1. a kind of concentration and separation method of colloid phosphorus in soil, which comprises the steps of:
S1: weighing the soil sample of sieving in conical flask, add deionized water, extraction；
S2: extraction supernatant is centrifuged supernatant of the 10~12min to remove bulky grain, after taking pre- centrifugation in advance at 3000~3500g
Liquid is filtered with 1 μm of miillpore filter, collects all filtrates after discarding primary filtrate；
S3: above-mentioned filtrate is put into the super filter tube of 3KDa, and 30~40min of ultracentrifugation under 4000g takes supernatant；On wherein
Clear liquid is the true dissolved phosphorus component for removing gel component, and ultrafiltration bottom of the tube is water diffusivity colloid phosphorus concentrate.
2. the concentration and separation method of colloid phosphorus in soil according to claim 1, which is characterized in that the soil sample be without
Grinding and the soil sample for crossing 8mm sieve.
3. the concentration and separation method of colloid phosphorus in soil according to claim 1, which is characterized in that in step S1, soil sample with go
Ionized water with Tu Shui ratio 1:8 mixing, then move in shaking table, at 150~160rpm extract 16~for 24 hours.
4. the concentration and separation method of colloid phosphorus in soil according to claim 1, which is characterized in that in step S2, primary filtrate
The amount of discarding is 5mL.
5. the concentration and separation method of colloid phosphorus in soil according to claim 1, which is characterized in that the concentration dimensions of colloid phosphorus are
3KDa-1μm。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111214958A (en) * | 2020-01-17 | 2020-06-02 | 中山大学 | Method for extracting soil rare earth nanoparticles |
Citations (2)
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|---|---|---|---|---|
| US20100264366A1 (en) * | 2009-04-21 | 2010-10-21 | E. I. Du Pont De Nemours And Company | Process for removing phosphorus-containing colloids and their precursors from iron chloride solutions |
| CN107607484A (en) * | 2017-10-25 | 2018-01-19 | 天津市环境保护科学研究院 | The method of thimet content in quick measure soil |
-
2018
- 2018-11-27 CN CN201811428937.3A patent/CN109632448A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100264366A1 (en) * | 2009-04-21 | 2010-10-21 | E. I. Du Pont De Nemours And Company | Process for removing phosphorus-containing colloids and their precursors from iron chloride solutions |
| CN107607484A (en) * | 2017-10-25 | 2018-01-19 | 天津市环境保护科学研究院 | The method of thimet content in quick measure soil |
Non-Patent Citations (3)
| Title |
|---|
| 刘子闻: "保护性耕作及多样化轮作下稻田土壤肢体磷的赋存规律及阻控研究", 《中国优秀硕士学位论文全文数据库农业科技辑》 * |
| 刘谨: "农田土壤水分散性胶体磷的赋存形态活化机制及阻控技术研究", 《中国博士学位论文全文数据库农业科技辑》 * |
| 赵越等: "磷肥输入对稻田土壤剖面胶体磷含量的影响", 《生态学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111214958A (en) * | 2020-01-17 | 2020-06-02 | 中山大学 | Method for extracting soil rare earth nanoparticles |
| CN111214958B (en) * | 2020-01-17 | 2022-07-19 | 中山大学 | Method for extracting soil rare earth nanoparticles |
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