CN109580910A - A kind of method of colloid phosphorus and nano particle state phosphorus in synchro measure soil - Google Patents
A kind of method of colloid phosphorus and nano particle state phosphorus in synchro measure soil Download PDFInfo
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- CN109580910A CN109580910A CN201811429365.0A CN201811429365A CN109580910A CN 109580910 A CN109580910 A CN 109580910A CN 201811429365 A CN201811429365 A CN 201811429365A CN 109580910 A CN109580910 A CN 109580910A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/24—Earth materials
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N9/00—Investigating density or specific gravity of materials; Analysing materials by determining density or specific gravity
- G01N9/36—Analysing materials by measuring the density or specific gravity, e.g. determining quantity of moisture
Abstract
The invention discloses a kind of method of colloid phosphorus and nano particle state phosphorus in synchro measure soil, the extraction supernatant of pedotheque is centrifuged by this method in advance, is then filtered with 1 μm of miillpore filter.It filters and takes out two parts in gained sample as sample to be tested.First part of filtrate sample to be tested is put into the super filter tube of 3KDa, 30~40min of ultracentrifugation under 4000g, and supernatant is taken to measure total phosphorus concentration TP2；Second part of filtrate sample to be tested is first put into ultrafiltration sample in the super filter tube of 1000KDa, ultracentrifugation 20min under 3000g, and supernatant is taken to measure total phosphorus concentration TP3；Then the supernatant of acquisition is put into the super filter tube of 3KD again, ultracentrifugation 40min under 4000g, then supernatant is taken to measure total phosphorus concentration TP4.The content of colloid phosphorus and nano particle state phosphorus in soil is finally calculated according to measurement result.The present invention improves traditional Gravity Separation and field flow separation method, greatly simplifies colloid phosphorus measurement analytical procedure, shortens minute, and can efficiently separate nano particle state phosphorus.
Description
Technical field
The invention belongs to soil nutrients to monitor field, be related to a kind of colloid phosphorus in synchro measure soil in the way of ultrafiltration
With the method for nano particle state 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 phosphorus and nano particle state phosphorus are the present invention
Technical problem urgently to be resolved.
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 synchronization
The method for measuring colloid phosphorus and nano particle state phosphorus in soil.
Specific technical solution of the present invention is as follows:
A kind of method of colloid phosphorus and nano particle state phosphorus in synchro measure soil comprising following steps:
S1: the soil sample of m grams of sieving is weighed in conical flask, adds V1Ml 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；After the filtrate of collection is mixed, it is total to measure it
Phosphorus concentration TP1(mg/L)；Two parts are taken out from the filtrate of mixing simultaneously is used as sample to be tested；
S3: first part of filtrate sample to be tested being put into the super filter tube of 3KDa, 30~40min of ultracentrifugation under 4000g,
Supernatant is taken to measure total phosphorus concentration TP2(mg/L), which is the true dissolved phosphorus component for removing gel component, super filter tube bottom
Portion is water diffusivity colloid phosphorus concentrate；
S4: second part of filtrate sample to be tested is first put into ultrafiltration sample in the super filter tube of 1000KDa, is exceeded the speed limit under 3000 g
It is centrifuged 20min, supernatant is taken to measure total phosphorus concentration TP3(mg/L), which is the nanometer for removing bulky grain gel component
Grain state component solution；Then the supernatant of acquisition is put into the super filter tube of 3KD again, ultracentrifugation 40min under 4000g, then taken
Supernatant measures total phosphorus concentration TP4(mg/L), which is the true solubilised state component for removing nano particle, and ultrafiltration bottom of the tube is
Nano particle state phosphorus concentrate；
S5: the content (mg/kg) of colloid phosphorus in soil, calculation formula are calculated are as follows:
Soil colloid phosphorus content=(TP1-TP2)×V1/m
Calculate the content (mg/kg) of nano particle state phosphorus in soil, calculation formula are as follows:
Nano particle state phosphorus content=(TP in soil3-TP4)×V1/m。
In the present invention, the size for the colloid phosphorus particle for using this method separation to obtain is 3KDa-1 μm, and coincide 1nm-1 substantially
μm the colloidal solid range of definition, using 1 μm filter membrane obtain colloid size it is relatively accurate.It is separated using hyperfiltration process
The particle of the 3KDa-1000KDa of acquisition meets nano particle, and the nano particle state phosphorus of basic identical 1nm-100nm defines model
It encloses.Therefore, the particle size of said determination is really effective.
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.
Preferably, the concentration dimensions of nano particle state phosphorus are 3KDa-1000KDa.
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.This method can not only be concentrated and separated colloid phosphorus, and can divide
It is accurately measured from nano particle state phosphorus, and to its content in the soil.
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, 10g is weighed and waits for
Not ground soil sample is surveyed, 8mm sieve is crossed, is put into 250mL conical flask, deionized water 80mL, Tu Shui ratio 1:8 is added to move to shaking table
In, it is extracted for 24 hours at 160rpm.Extraction supernatant is centrifuged 12min to remove bulky grain, after taking pre- centrifugation in advance at 3000g
Supernatant is filtered with 1 μm of miillpore filter, collects all filtrates after discarding 5mL primary filtrate, filtrate volume about 75mL is collected in measurement；It will
After the filtrate of collection mixes, its total phosphorus concentration TP1 is measured；Two parts are taken out from the filtrate of mixing simultaneously is used as sample to be tested；
First part of filtrate sample to be tested is put into the super filter tube of 3KDa, ultracentrifugation 40min under 4000g takes supernatant
Measure total phosphorus concentration TP2, which is the true dissolved phosphorus component for removing gel component, and ultrafiltration bottom of the tube is water diffusivity glue
Body phosphorus concentrate；Second part of filtrate sample to be tested is first put into ultrafiltration sample in the super filter tube of 1000KDa, is exceeded the speed limit under 3000g
It is centrifuged 20min, supernatant is taken to measure total phosphorus concentration TP3, which is the nano particle state group for removing bulky grain gel component
Divide solution；Then the supernatant of acquisition is put into the super filter tube of 3KD again, ultracentrifugation 40min under 4000g, then takes supernatant
Measure total phosphorus concentration TP4, which is the true solubilised state component for removing nano particle, and ultrafiltration bottom of the tube is nano particle state
Phosphorus concentrate；Soil colloid phosphorus content (mg/kg)=(TP1-TP2) × 80mL/10g, nano particle state phosphorus content (mg/ in soil
Kg)=(TP3-TP4)×80mL/10g.The results are shown in Table 1 for colloid phosphorus yield in the present embodiment, the survey of nano particle state phosphorus
It is fixed that the results are shown in Table 2.
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.
The nano particle state phosphorus content of separation method measurement is concentrated by ultrafiltration in table 2
As shown in Table 2, the average content of the nano particle state phosphorus of this method measurement is 2.58mg/kg.Error only has
0.05mg/kg.Since there is presently no mature nano particle state phosphorus determination methods, for this purpose, this method cannot be with other methods
It is compared.But the coincide substantially nano particle state phosphorus of 1nm-100nm of the particle that the treatment process of this method obtains defines model
It encloses, therefore the nanoparticle range that theoretically this method measures is accurate, precision is higher.
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 5g not ground soil sample to be measured, cross 8mm sieve, be put into 250mL conical flask, add deionized water 40mL, Tu Shui ratio
1:8 is moved in shaking table, extracts 16h at 150rpm.Extraction supernatant is centrifuged 10min in advance at 3500g to remove bulky grain,
Supernatant after taking pre- centrifugation is filtered with 1 μm of miillpore filter, collects all filtrates after discarding 5 milliliters of primary filtrates, filter is collected in measurement
Liquid accumulates about 35mL；After the filtrate of collection is mixed, its total phosphorus concentration TP is measured1；Two parts are taken out from the filtrate of mixing simultaneously
As sample to be tested；
First part of filtrate sample to be tested is put into the super filter tube of 3KDa, ultracentrifugation 40min under 4000g takes supernatant
Measure total phosphorus concentration TP2, which is the true dissolved phosphorus component for removing gel component, and ultrafiltration bottom of the tube is water diffusivity glue
Body phosphorus concentrate；Second part of filtrate sample to be tested is first put into ultrafiltration sample in the super filter tube of 1000KDa, is exceeded the speed limit under 3000g
It is centrifuged 20min, supernatant is taken to measure total phosphorus concentration TP3, which is the nano particle state group for removing bulky grain gel component
Divide solution；Then the supernatant of acquisition is put into the super filter tube of 3KD again, ultracentrifugation 30min under 4000g, then takes supernatant
Measure total phosphorus concentration TP4, which is the true solubilised state component for removing nano particle, and ultrafiltration bottom of the tube is nano particle state
Phosphorus concentrate；Soil colloid phosphorus content (mg/kg)=(TP1-TP2) × 40mL/5g, nano particle state phosphorus content (mg/ in soil
Kg)=(TP3-TP4)×40mL/5g.Colloid phosphorus yield result is as shown in table 3 in the present embodiment, the survey of nano particle state phosphorus
It is fixed that the results are shown in Table 3.
Table 3 is the comparison for the colloid phosphorus content that gravity separation method and above-mentioned ultrafiltration concentration separation method measure
As shown in Table 3, 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, can efficiently separate and fast and accurately detect the colloid phosphorus in soil.
The nano particle state phosphorus content of separation method measurement is concentrated by ultrafiltration in table 4
As shown in Table 4, the average content of the nano particle state phosphorus of this method measurement is 0.87mg/kg.Error only has
0.06mg/kg.Since there is presently no mature nano particle state phosphorus determination methods, for this purpose, this method cannot be with other methods
It is compared.But the coincide substantially nano particle state phosphorus of 1nm-100nm of the particle that the treatment process of this method obtains defines model
It encloses, therefore the nanoparticle range that theoretically this method measures is accurate, precision is higher.
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 method of colloid phosphorus and nano particle state phosphorus in synchro measure soil, which comprises the steps of:
S1: the soil sample of m grams of sieving is weighed in conical flask, adds V1Ml 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；After the filtrate of collection is mixed, it is dense to measure its total phosphorus
Spend TP1；Two parts are taken out from the filtrate of mixing simultaneously is used as sample to be tested；
S3: first part of filtrate sample to be tested is put into the super filter tube of 3KDa, and 30~40min of ultracentrifugation under 4000g takes supernatant
Liquid measures total phosphorus concentration TP2, which is the true dissolved phosphorus component for removing gel component, and ultrafiltration bottom of the tube is water diffusivity
Colloid phosphorus concentrate；
S4: second part of filtrate sample to be tested is first put into ultrafiltration sample in the super filter tube of 1000KDa, ultracentrifugation under 3000g
20min takes supernatant to measure total phosphorus concentration TP3, which is that the nano particle state component of removal bulky grain gel component is molten
Liquid；Then the supernatant of acquisition is put into the super filter tube of 3KD again, ultracentrifugation 40min under 4000g, then supernatant is taken to measure
Total phosphorus concentration TP4, which is the true solubilised state component for removing nano particle, and ultrafiltration bottom of the tube is the concentration of nano particle state phosphorus
Liquid；
S5: the content of colloid phosphorus in soil, calculation formula are calculated are as follows:
Soil colloid phosphorus content=(TP1-TP2)×V1/m
Calculate the content of nano particle state phosphorus in soil, calculation formula are as follows: nano particle state phosphorus content=(TP in soil3-TP4)
×V1/m。
2. the method for colloid phosphorus and nano particle state phosphorus in synchro measure soil according to claim 1, which is characterized in that described
Soil sample be without grinding and cross 8mm sieve soil sample.
3. the method for colloid phosphorus and nano particle state phosphorus in synchro measure soil according to claim 1, which is characterized in that step
In S1, soil sample is mixed with deionized water with Tu Shui ratio 1:8, is then moved in shaking table, at 150~160rpm extract 16~for 24 hours.
4. the method for colloid phosphorus and nano particle state phosphorus in synchro measure soil according to claim 1, which is characterized in that step
In S2, the amount of discarding of primary filtrate is 5mL.
5. the method for colloid phosphorus and nano particle state phosphorus in synchro measure soil according to claim 1, which is characterized in that colloid
The concentration dimensions of phosphorus are 3KDa-1 μm, and the concentration dimensions of nano particle state phosphorus are 3KDa-1000 KDa.
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| CN201811429365.0A CN109580910A (en) | 2018-11-27 | 2018-11-27 | A kind of method of colloid phosphorus and nano particle state phosphorus in synchro measure soil |
| PCT/CN2019/106538 WO2020108030A1 (en) | 2018-11-27 | 2019-09-18 | Method for synchronously measuring colloidal phosphorus and nanoparticle-state phosphorus in soil |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111214958A (en) * | 2020-01-17 | 2020-06-02 | 中山大学 | Method for extracting soil rare earth nanoparticles |
| WO2020108030A1 (en) * | 2018-11-27 | 2020-06-04 | 浙江大学 | Method for synchronously measuring colloidal phosphorus and nanoparticle-state phosphorus in soil |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113514667A (en) * | 2021-07-01 | 2021-10-19 | 沈阳农业大学 | Method for detecting morphological characteristics of soil colloid |
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Application publication date: 20190405 |