CN110333209A - A kind of detection method of soil available Se - Google Patents
A kind of detection method of soil available Se Download PDFInfo
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- CN110333209A CN110333209A CN201910623479.7A CN201910623479A CN110333209A CN 110333209 A CN110333209 A CN 110333209A CN 201910623479 A CN201910623479 A CN 201910623479A CN 110333209 A CN110333209 A CN 110333209A
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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
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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
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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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
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
- G01N21/6404—Atomic fluorescence
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Abstract
The present invention provides a kind of detection methods of soil available Se, and soil is successively air-dried, crushed and is sieved, obtained pedotheque is extracted with potassium dihydrogen phosphate, leaching liquor is centrifuged, obtains supernatant；It is detected after supernatant resolution using Hydrides AFS spectrometer, obtains the content of effective selenium in soil.The present invention extracts effective selenium in soil using potassium dihydrogen phosphate, the concentration of potassium dihydrogen phosphate is 0.45~0.8mol/L, pH value is 7~10, extraction time is 30~120min, optimize the optimum condition that soil available Se extracts by Star point design-response phase method are as follows: biphosphate potassium concn is 0.5mol/L, pH value is 10, extraction time is 72min, effective selenium recovery rate highest, the selenium extracted and the selenium correlation in plant are good, the Se content in supernatant is directly tested using Hydride Generation Atomic Fluorescence Spectrometry, applied widely, analysis cost is low.
Description
Technical field
The present invention relates to technical field of analysis and detection, in particular to a kind of detection method of soil available Se.
Background technique
Selenium is the essential trace elements of the human body, is of great significance to the health of the mankind, and selenium-rich soil is in plant
One of main source of selenium.Existing form has water-soluble state, exchangeable species, mineral reference state, organically combine state to selenium in the soil
And residual form, the summation of various Se forms are known as total selenium, total selenium is able to reflect the reserves of selenium.Wherein can directly it be absorbed by crops
What is utilized is known as biologically effective selenium, including selenite radical ion, selenic acid radical ion and part organic selenium small molecule.A large amount of research
Report, crop selenium content do not have significant correlation with the total selenium of soil, and significant with effective selenium correlation.About soil available Se
Extraction, commonly use the chemical method of continuous extraction or single extraction, extractant has water, CaCl2、NaHCO3、K2SO4It is slow with phosphate
Fliud flushing etc. generally uses NaHCO though not building consensus to the extraction of different types of soil available Se3Solution extraction, HCO3 -
Mainly making iron and the aluminum water solution in conjunction with selenium and releases selenium, the selenium amount of water-disintegrable height, extraction is also higher, therefore extract
Selenium amount may not necessarily react crop to the uptake of Selenium in Soil well.Commonly there are also forms point for the test method of soil available Se
The Se content of analysis method, i.e. survey different shape calculates summation, the content of as effective selenium again.This method is only applicable to test selenium-rich
Effective Se content in pedotheque, the total selenium of non-selenium-rich area soil is in 0.40mg/kg hereinafter, effectively selenium is generally in 0.08mg/
Kg needs to carry out carrying out by solid phase solvent extraction instrument hereinafter, measuring effective selenium in soil using morphological analysis rich
Collection, technical difficulty are larger.
Summary of the invention
In view of this, it is an object of that present invention to provide a kind of detection methods of soil available Se.Method provided by the invention
The reciprocation of many factors is comprehensively considered, it is determined that the optimum extraction condition of soil available Se, and extraction process
Simply, the selenium extracted and the selenium correlation in plant are good, and detection method provided by the invention is applied widely, to non-selenium-rich
Soil is also suitable.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
A kind of detection method of soil available Se, comprising the following steps:
(1) soil is successively air-dried, crushed and is sieved, obtain pedotheque；
(2) pedotheque is extracted with potassium dihydrogen phosphate, obtains leaching liquor；The potassium dihydrogen phosphate
Concentration is 0.45~0.8mol/L, and pH value is 7~10, and extraction time is 30~120min；
(3) leaching liquor is centrifuged, obtains supernatant；
(4) Hydrides AFS spectral detection will be carried out after supernatant resolution, and will obtain containing for effective selenium in soil
Amount.
Preferably, the mesh number of the sieving is 60~100 mesh.
Preferably, the concentration of the potassium dihydrogen phosphate is 0.50mol/L.
Preferably, the ratio of the volume of the potassium dihydrogen phosphate and the quality of the pedotheque is 10~40mL:
1g。
Preferably, the ratio of the volume of the potassium dihydrogen phosphate and the quality of the pedotheque is 27mL:1g.
Preferably, the time of the extraction is 72min.
Preferably, the temperature of the extraction is 25~30 DEG C.
Preferably, the digestion solution used of clearing up is nitric acid and hydrogen peroxide.
Preferably, the volume ratio of the nitric acid and hydrogen peroxide is 7:1.
The present invention provides a kind of detection methods of soil available Se, and soil is successively air-dried, crushed and is sieved, will
It obtains pedotheque to be extracted with potassium dihydrogen phosphate, leaching liquor is centrifuged, obtain supernatant；Supernatant is cleared up laggard
Row Hydrides AFS spectral detection obtains the content of effective selenium in soil.Method of the invention is molten using potassium dihydrogen phosphate
Liquid extracts effective selenium in soil, and wherein the concentration of potassium dihydrogen phosphate is 0.45~0.8mol/L, and pH value is 7~10,
Extraction time be 30~120min, the concentration, pH value and extraction time be comprehensive considering various effects reciprocation after
It arrives, the selenium extracted and the selenium correlation in plant are good, and extraction process is simple；And the present invention uses hydride-
Atomic fluorescence spectrometry directly detects the Se content in supernatant, and applied widely, analysis cost is low.
Detailed description of the invention
Fig. 1 is the response surface of Y=f (A, D) in embodiment 1, and wherein Y is selenium extracted amount, and A is leaching liquor concentration, and D is liquid sample
Than；
Fig. 2 is the response surface of Y=f (A, C) in embodiment 1, and wherein Y is selenium extracted amount, and A is leaching liquor concentration, and C is extraction
Time；
Fig. 3 is the response surface of Y=f (A, B) in embodiment 1, and wherein Y is selenium extracted amount, and A is leaching liquor concentration, and B is extraction
Liquid pH value；
Fig. 4 is the response surface of Y=f (C, D) in embodiment 1, and wherein Y is selenium extracted amount, and C is extraction time, and D is liquid sample
Than；
Fig. 5 is the response surface of Y=f (B, D) in embodiment 1, and wherein Y is selenium extracted amount, and B is leaching liquor pH value, and D is liquid sample
Than；
Fig. 6 is the response surface of Y=f (B, C) in embodiment 1, and wherein Y is selenium extracted amount, and B is leaching liquor pH value, and C is extraction
Time.
Specific embodiment
The present invention provides a kind of detection methods of soil available Se, comprising the following steps:
(1) soil is successively air-dried, crushed and is sieved, obtain pedotheque；
(2) pedotheque is extracted with potassium dihydrogen phosphate, obtains leaching liquor；The potassium dihydrogen phosphate
Concentration is 0.45~0.8mol/L, and pH value is 7~10, and extraction time is 30~120min；
(3) leaching liquor is centrifuged, obtains supernatant；
(4) Hydrides AFS spectral detection will be carried out after supernatant resolution, and will obtain containing for effective selenium in soil
Amount.
Soil is successively air-dried, crushed and is sieved by the present invention, obtains pedotheque.The present invention does not have the soil
Particular/special requirement, selenium-rich soil or non-selenium-rich soil, in the art, total Se content of non-selenium-rich soil generally exist
0.40mg/kg is hereinafter, its effective Se content is generally 0.08mg/kg or less.The present invention is not special to the air-dried method
It is required that natural air drying；In the present invention, the crushing is preferably hammered into shape using plastic hammer broken；The mesh number of the sieving is preferred
For 60~100 mesh, more preferably 80 mesh, soil fineness is affected below 60 mesh to extraction effect of the invention, 60-100
Mesh difference is little, thus the present invention controls soil fineness in 60~100 mesh.
After obtaining pedotheque, the present invention extracts pedotheque with potassium dihydrogen phosphate, obtains leaching liquor.?
In the present invention, the concentration of the potassium dihydrogen phosphate is 0.45~0.8mol/L, preferably 0.5~0.8mol/L, further
Preferably 0.5~0.6mol/L, most preferably 0.5mol/L, the pH value of the potassium dihydrogen phosphate are 7~10, preferably 8
~10, further preferably 9~10, most preferably 10；The matter of the volume of the potassium dihydrogen phosphate and the pedotheque
The ratio of amount is preferably 10~40mL:1g, more preferably 27mL:1g.
In the present invention, the extraction carries out under oscillating condition, and the time of the extraction is 30~120min, more preferably
For 45~100min, further preferably 60~90min, most preferably 72min；The temperature of the extraction is preferably 25~30
DEG C, more preferably 30 DEG C.
In the present invention, the optimal conditions of the extraction are as follows: the concentration of potassium dihydrogen phosphate is 0.5mol/L, di(2-ethylhexyl)phosphate
The pH value of hydrogen potassium solution is 10, and the ratio of the quality of the volume and pedotheque of potassium dihydrogen phosphate is 27mL:1g, when extraction
Between be 72min.Potassium dihydrogen phosphate concentration of the invention, pH value, the quality of the volume of potassium dihydrogen phosphate and soil
Condition than (i.e. liquid sample ratio) and extraction time be obtain after the reciprocation for comprehensively considering four factors (utilize response surface
Analytic approach obtains) it is compared with traditional single_factor method, the extracting condition extracting effect that the present invention limits is more preferable, extracts
Selenium and the selenium correlation in plant are more preferable.
In leaching process, H2PO4 -It is acted on by anion exchange and replaces out by the selenium for being adsorbed on solid phase of soil surface,
The replaced selenium of exchange is relatively easy to release under the conditions of general soil, thus the selenium that the present invention extracts is more representative of soil
The validity of earth selenium, it is more preferable with the selenium correlation in plant.
After the completion of extraction, the leaching liquor is centrifuged by the present invention, obtains supernatant.In the present invention, turn of the centrifugation
Speed is preferably 3000r/min, and the time is preferably 15min；The supernatant obtained after centrifugation can effective selenium extracting solution.
After obtaining supernatant, the present invention carries out Hydrides AFS spectral detection after clearing up the supernatant, obtains
The content of effective selenium in soil.In the present invention, the resolution is preferably nitric acid and hydrogen peroxide with digestion solution；The nitric acid is preferred
The concentrated nitric acid for being 65~68% for mass fraction；The mass fraction of the hydrogen peroxide is preferably 30%；The nitric acid and hydrogen peroxide
Volume ratio be preferably 7:1.The present invention does not have particular/special requirement to the detailed process of the resolution, ripe using those skilled in the art
The method known carries out, can be with reference to the side in " measurement of GB5009.93-2017 national food safety standard selenium in food "
Method carries out, specifically includes the following steps:
It takes the supernatant 5mL in micro-wave diminishing pot, HNO is added37mL, H2O21mL is cleared up (by all forms
Selenium be converted into hexavalent selenium), after Specimen eliminating, remove counteracting tank, be heated on electric hot plate closely dry, be added after cooling
5mL 6mol/L hydrochloric acid, continuing to be heated to solution becomes Clear colourless and (converts tetravalence for hexavalent selenium with white cigarette appearance
Selenium), it is cooling, it is transferred in 10mL volumetric flask, the potassium ferricyanide (screening agent) solution 1mL is added, with 5% hydrochloric acid solution constant volume
Then 10mL measures Se content using Hydride Generation Atomic Fluorescence Spectrometry.
The present invention does not have particular/special requirement, reference to the testing conditions of the Hydride Generation Atomic Fluorescence Spectrometry
Condition in " measurement of GB5009.93-2017 national food safety standard selenium in food " is configured, and is being embodied
Testing conditions can be adjusted according to apparatus status in the process, and those skilled in the art are rule of thumb adjusted, this hair
It is not specifically limited in bright.
Scheme provided by the invention is described in detail below with reference to embodiment, but they cannot be interpreted as pair
The restriction of the scope of the present invention.
Embodiment 1
The present embodiment uses response surface experimental verification extraction conditions of the present invention, and steps are as follows:
1, response surface experimental design factor and level
Center combination design is carried out using response surface center of surface combination experiment software design scheme.Empirical factor and corresponding
It is horizontal such as table 1.
1 response surface empirical factor of table and water-glass
Experimental procedure: soil pretreatment: soil natural is air-dried, beats broken, 60 meshes excessively with plastics；By the soil after sieving
It is vibrated on constant temperature oscillator in earth and potassium dihydrogen phosphate merging centrifuge tube, to having extracted processing in the centrifuge tube
Solution carries out centrifugal treating, leaves and takes supernatant after centrifugal treating, takes supernatant 5mL in micro-wave diminishing pot, and HNO is added37mL,
H2O21mL is cleared up, and after Specimen eliminating, removes counteracting tank, is heated to closely doing on electric hot plate, 5mL is added after cooling
6mol/L hydrochloric acid, continues to be heated to solution to become Clear colourless and occur with white cigarette, cooling, is transferred in 10mL volumetric flask,
Potassium ferricyanide solution 1mL is added to be measured with 5% hydrochloric acid solution constant volume by Hydride Generation Atomic Fluorescence Spectrometry, determines that selenium mentions
Taken amount.
2, the results are shown in Table 2 for the effective selenium extraction of center combination response surface experimental design.
The effective selenium of 2 response phase method experimental design of table extracts result
Response surface analysis between 2.1 different factors
As shown in figs. 1 to 6, response surface is steeper for reciprocation in model between each factor, shows that the interaction between two factors is made
With more significant, Open Side Down for the paraboloid of 3 curved surfaces of AC, AD, CD, shows leaching liquor concentration, extraction time and liquid-to-solid ratio tool
There is maximum point, AB, BC and BD curved surface are upward, show that maximum value has not been reached yet in leaching liquor pH.
The variance analysis of 2.2 response-surface models
It is designed using Box-Behnken Design (BBD) to data in table 2 with Design-expert 8.05b software
Response surface analysis is carried out, model is obtained by multiple regression Fitting Analysis and carries out variance analysis, obtains effective selenium in soil
Optimize mathematical regression equation are as follows:
R=0.49+0.033A+0.056B+0.028C+0.050D-0.005AB+0.012AC-0.005 AD-0.029 BC-
0.021BD+0.017CD-0.019A2+0.007 B2-0.027C2-0.027D2。
In formula: R is soil available Se extracted amount (mg/kg), and A is leaching liquor concentration (mol/L), and B is leaching liquor pH value, C
It is liquid-to-solid ratio (mL/g) for extraction time (min), D.
F inspection and variance analysis are carried out to model, the results are shown in Table 3.
The variance analysis of 3 response surface regression equation of table
It is obtained by equation Monomial coefficient in table 3, influences the sequence that soil available Se extracts yield factor are as follows: leaching liquor pH
Value > liquid-to-solid ratio > leaching liquor concentration > extraction time.As variance interpretation of result is shown in table: the F value 7.09 of regression equation, Prob > F
The value of item illustrates that the model is extremely significant less than 0.01, and wherein A, B, D influence entire experiment extremely significant, and C is influenced less than 0.05
Significantly.
By response surface analysis and forecast of regression model, the optimum extraction condition of soil available Se is obtained are as follows: leaching liquor is dense
Degree 0.52mol/L, pH value 9.94, extraction time 72.21min, liquid-to-solid ratio 27.44 are ultimately determined in conjunction with practical operation: extraction
Liquid concentration 0.5mol/L, pH value 10, extraction time 72min, liquid-to-solid ratio 27:1, effective selenium extraction amount actual value are 0.56mg/kg,
Desired value is 0.53mg/kg, and error amount is only 0.03mg/kg, illustrates that the model can predict mentioning for soil available Se well
Taken amount.
Embodiment 2
Rate of recovery test:
Three samples are acquired from the double river fort the Yang Jia vegetable garden soils of Enshi City, three trouble sand dam rice soil, red temple Xihe River dam rice soil
Product are successively labeled as sample 1, sample 2 and sample 3.
Sample 1, sample 2 and sample 3 each 1.0g, spiked levels 0.2mg/kg, 0.4mg/kg, 0.6mg/kg are taken, accurately
The potassium dihydrogen phosphate 27mL of 0.5mol/L is added, 72min is vibrated on constant temperature oscillator, then carries out centrifugal treating, from
Supernatant 5mL is left and taken in micro-wave diminishing pot after heart processing, and HNO is added37mL, H2O21mL is cleared up, and Specimen eliminating finishes
Afterwards, counteracting tank is removed, closely dry, addition 5mL 6mol/L hydrochloric acid after cooling is heated on electric hot plate, continues to be heated to solution change
Occur for Clear colourless and with white cigarette, it is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added, with 5% salt
Acid solution constant volume, is measured by Hydride Generation Atomic Fluorescence Spectrometry, determines selenium extracted amount, and calculate the rate of recovery and standard deviation
Value.
Acquired results are as shown in table 4, and the background values in table 4 refers to effective Se content of sample itself.
4 method determination of recovery rates result of table
Concentration is added between 0.01~0.1mg/kg, relative standard deviation < 20% that accuracy requirement allows adds dense
When degree>0.10mg/kg, relative standard deviation<15% of permission.Above different types of 3 pedotheque rate of recovery are 75.89
Between~89.42%, RSD% illustrates that measurement result of the invention is accurate between 1.17~7.15%.
Embodiment 3
Pedotheque 0.4005g is weighed in centrifuge tube, the accurate KH that 0.8mol/L is added2PO4Leaching liquor (pH value 7)
10mL, vibrates 30min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, takes supernatant 5mL in micro-
In wave counteracting tank, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, on electric hot plate
It is heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continue to be heated to solution to become Clear colourless and occur with white cigarette,
It is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-atom
Fluorescence spectrum method for measuring, effective Se content are 0.454mg/kg.
Embodiment 4
Pedotheque 0.4001g is weighed in centrifuge tube, the accurate KH that 0.8mol/L is added2PO4Leaching liquor (pH value 10)
10mL, vibrates 75min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, takes supernatant 5mL in micro-
In wave counteracting tank, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, on electric hot plate
It is heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continue to be heated to solution to become Clear colourless and occur with white cigarette,
It is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-atom
Fluorescence spectrum method for measuring, effective Se content are 0.552mg/kg.
Embodiment 5
Pedotheque 0.4006g is weighed in centrifuge tube, the accurate KH that 0.45mol/L is added2PO4(pH value is leaching liquor
10) 10mL, vibrates 30min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, takes supernatant 5mL
In micro-wave diminishing pot, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, in electric heating
It is heated to closely dry on plate, 5mL 6mol/L hydrochloric acid is added after cooling, continue to be heated to solution to become Clear colourless and with white cigarette
Occur, it is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydrogenation
Object-AFS DETERMINATION, effective Se content are 0.534mg/kg.
Embodiment 6
Pedotheque 0.2509g is weighed in centrifuge tube, the accurate KH that 0.8mol/L is added2PO4Leaching liquor (pH value 7)
10mL, vibrates 75min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, takes supernatant 5mL in micro-
In wave counteracting tank, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, on electric hot plate
It is heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continue to be heated to solution to become Clear colourless and occur with white cigarette,
It is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-atom
Fluorescence spectrum method for measuring, effective Se content are 0.535mg/kg.
Embodiment 7
Pedotheque 1.0001g is weighed in centrifuge tube, the accurate KH that 0.45mol/L is added2PO4Leaching liquor (pH value 7)
10mL, vibrates 30min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, takes supernatant 5mL in micro-
In wave counteracting tank, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, on electric hot plate
It is heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continue to be heated to solution to become Clear colourless and occur with white cigarette,
It is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-atom
Fluorescence spectrum method for measuring, effective Se content are 0.359mg/kg.
Embodiment 8
Pedotheque 1.000g is weighed in centrifuge tube, the accurate KH that 0.45mol/L is added2PO4Leaching liquor (pH value 7)
10mL, vibrates 120min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, take supernatant 5mL in
In micro-wave diminishing pot, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, in electric hot plate
On be heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continues to be heated to solution to become Clear colourless and go out with white cigarette
It is existing, it is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-
AFS DETERMINATION, effective Se content are 0.383mg/kg.
Embodiment 9
Pedotheque 0.2504g is weighed in centrifuge tube, the accurate KH that 0.45mol/L is added2PO4Leaching liquor (pH value 7)
10mL, vibrates 30min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, takes supernatant 5mL in micro-
In wave counteracting tank, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, on electric hot plate
It is heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continue to be heated to solution to become Clear colourless and occur with white cigarette,
It is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-atom
Fluorescence spectrum method for measuring, effective Se content are 0.457mg/kg.
Embodiment 10
Pedotheque 0.2506g is weighed in centrifuge tube, the accurate KH that 0.45mol/L is added2PO4Leaching liquor (pH value 7)
10mL, vibrates 120min at constant temperature oscillator 1500r/min, 30 DEG C, and 3000r/min is centrifuged 15min, take supernatant 5mL in
In micro-wave diminishing pot, HNO is added37mL, H2O21mL is cleared up, and after Specimen eliminating, counteracting tank is removed, in electric hot plate
On be heated to closely dry, 5mL 6mol/L hydrochloric acid is added after cooling, continues to be heated to solution to become Clear colourless and go out with white cigarette
It is existing, it is cooling, it is transferred in 10mL volumetric flask, potassium ferricyanide solution 1mL is added with 5% hydrochloric acid solution constant volume and passes through hydride-
AFS DETERMINATION, effective Se content are 0.550mg/kg.
Easy to operate according to above embodiments it is found that method and step provided by the invention is simple, gained extraction conditions are comprehensive
Consider the reciprocation of many factors, the selenium correlation in the selenium and plant extracted is good, and test result is accurate.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of detection method of soil available Se, which comprises the following steps:
(1) soil is successively air-dried, crushed and is sieved, obtain pedotheque；
(2) pedotheque is extracted with potassium dihydrogen phosphate, obtains leaching liquor；The concentration of the potassium dihydrogen phosphate
For 0.45~0.8mol/L, pH value is 7~10, and extraction time is 30~120min；
(3) leaching liquor is centrifuged, obtains supernatant；
(4) Hydrides AFS spectral detection will be carried out after supernatant resolution, obtains the content of effective selenium in soil.
2. detection method according to claim 1, which is characterized in that the mesh number of the sieving is 60~100 mesh.
3. detection method according to claim 1, which is characterized in that the concentration of the potassium dihydrogen phosphate is
0.5mol/L。
4. detection method according to claim 1 or 3, which is characterized in that the volume of the potassium dihydrogen phosphate and institute
The ratio for stating the quality of pedotheque is 10~40mL:1g.
5. detection method according to claim 1 or 3, which is characterized in that the volume of the potassium dihydrogen phosphate and institute
The ratio for stating the quality of pedotheque is 27mL:1g.
6. detection method according to claim 1, which is characterized in that the time of the extraction is 72min.
7. detection method according to claim 1 or 6, which is characterized in that the temperature of the extraction is 25~30 DEG C.
8. detection method according to claim 1, which is characterized in that the digestion solution used of clearing up is nitric acid and dioxygen
Water.
9. detection method according to claim 8, which is characterized in that the volume ratio of the nitric acid and hydrogen peroxide is 7:1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910623479.7A CN110333209A (en) | 2019-07-11 | 2019-07-11 | A kind of detection method of soil available Se |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910623479.7A CN110333209A (en) | 2019-07-11 | 2019-07-11 | A kind of detection method of soil available Se |
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