CN108181300A - The assay method of available phosphorus content in a kind of pedotheque - Google Patents
The assay method of available phosphorus content in a kind of pedotheque Download PDFInfo
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- CN108181300A CN108181300A CN201810047775.2A CN201810047775A CN108181300A CN 108181300 A CN108181300 A CN 108181300A CN 201810047775 A CN201810047775 A CN 201810047775A CN 108181300 A CN108181300 A CN 108181300A
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- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
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Abstract
The invention discloses a kind of assay methods of available phosphorus content in pedotheque.The assay method includes the following steps：Phosphorus standard solution is prepared, adds in NaHCO thereto respectively3Then solution adds in the pH value of HCl solution regulation system, treats CO2It after emptying, is detected after constant volume using inductive coupling plasma emission spectrograph, obtains radiation intensity；With a concentration of abscissa of phosphorus in phosphorus standard solution, make working curve by ordinate of radiation intensity；NaHCO is added in into pedotheque3Solution is extracted, and obtains filtered fluid；It draws filtered fluid and adds in HCl solution and adjust pH value, treat CO2It after emptying, is detected after constant volume using inductive coupling plasma emission spectrograph, obtains radiation intensity, the concentration of P elements in filtered fluid is obtained according to working curve, according to formula (A) up to the concentration of available phosphorus in pedotheque.The method of the present invention quick and precisely, with the development of science and technology the method for ICP OES methods measure soil available phosphorus, is the development trend that available phosphorus measures, has real and theory double meaning.
Description
Technical field
The present invention relates to a kind of assay methods of available phosphorus content, and in particular to available phosphorus content in a kind of pedotheque
Assay method.
Background technology
Nutrient necessary to phosphorus is crops normal growth, available phosphorus are the phosphorus components being easily absorbed by plants in soil,
Effective phosphorus yield has direct indicative function to the ability of soil supply phosphorus, to guidance fertilising, improves soil phosphorus content and protection
Environment important in inhibiting.In recent years, because it is continuous a large amount of using fertilizer caused by agricultural land soil phosphorus accumulation, soil can be caused effective
Phosphorus to water body loss cause surface water eutrophication and underground water pollution the problems such as, serious threat Environmental Health.Soil has
The Accurate Determining of effect phosphorus can make the ability that we understand soil supply phosphorus, apply fertilizer to scientific guidance, improve soil, improve crop
Quality and economic benefit are of great significance, and simultaneously for soil environment quality is improved, environmental protection reduces the loss of available phosphorus
There is directive significance.
Soil available phosphorus is the Phosphorus Fractions In Soils that can be absorbed in vegetation period by root system of plant, including whole water solubilitys
Phosphorus, weakly stable state phosphorus, exchangeability phosphorus and ease of solubility solid phosphate.The assay method of soil available phosphorus most the recognized standard at present
Method is that sodium bicarbonate extraction-molybdenum-antimony anti-spectrophotometric method, the method is applicable in most of soil, and usability is wider, but colour developing pair
Available phosphorus measurement result is affected, and colorimetric method is complicated for operation, and detection efficiency is low.
With the development of science and technology the measuring technology of soil available phosphorus has more developing direction, such as flow injection point
The development and application of the instrument and equipments such as analyzer, ion chromatograph is that soil is surveyed using advanced instrument and equipment analysis soil nutrient
Try the new trend of development.
Invention content
The object of the present invention is to provide a kind of assay method of available phosphorus content in pedotheque, specially sodium bicarbonate soaks
It carries, the method that hydrochloric acid adjusts acidity-inductive coupling plasma emission spectrograph (ICP-OES), which can improve
Working efficiency reduces analysis time；Relate generally to the quick measure of available phosphorus content in calcareous, alkalescent soil.
The assay method of available phosphorus content, includes the following steps in pedotheque provided by the present invention：
(1) the phosphorus standard solution of at least three kinds of various concentrations is prepared, adds in NaHCO into the phosphorus standard solution respectively3Water
Then solution adds in the pH value of HCl solution regulation system, treats CO2After emptying, sent out after constant volume using inductively coupled plasma
It penetrates spectrometer (ICP) to be detected, obtains radiation intensity；With a concentration of abscissa of phosphorus in the phosphorus standard solution, with radiation
Intensity is ordinate, makes working curve；
(2) NaHCO is added in into pedotheque3Aqueous solution is extracted, filtered to obtain filtered fluid；
(3) it draws the filtered fluid and adds in the HCl solution and adjust pH value, treat CO2After emptying, institute is used after constant volume
It states inductive coupling plasma emission spectrograph to be detected, obtains spectral intensity, according to the working curve, obtain the mistake
The concentration of P elements, is denoted as ρ in filtrate0, unit mg/mL；
The concentration of available phosphorus in pedotheque is obtained according to formula (A), is denoted as ω, unit mg/kg,
In formula, ρ2Represent the concentration of P elements in the blank solution obtained according to standard curve, unit mg/mL；
The blank solution refers to the filtered fluid obtained when not adding in the pedotheque in step (2)；
V represents the volume of the filtered fluid, unit mL；
M represents the quality of pedotheque, unit g；
D, which represents to divide, takes multiple, i.e. NaHCO described in digestion agent in step (2)3The volume of aqueous solution takes the ratio of volume with dividing
Value, described point takes the volume that volume refers to filtered fluid described in step (3), and the D can be 5：2.
In above-mentioned assay method, the phosphorus standard solution can be the aqueous solution of potassium dihydrogen phosphate；
The volumetric concentration of the phosphorus standard solution can be 0~20 μ g/mL.
In above-mentioned assay method, the NaHCO3The pH value of aqueous solution is 8.5, is regulated and controled by sodium hydrate aqueous solution, such as
Mass percent is used to be regulated and controled for 10% sodium hydrate aqueous solution；
The NaHCO3The concentration of aqueous solution can be 0.5mol/L.
In above-mentioned assay method, the HCl solution is 1 by volume ratio：1 water and hydrochloric acid is prepared to obtain.
In above-mentioned assay method, in step (2), the pedotheque and the NaHCO3The proportioning of aqueous solution is：1g：
20mL。
In above-mentioned assay method, in step (2), the pedotheque is the sample after 1.0~2.0mm screenings.
In above-mentioned assay method, in step (2), the leach step is carried out on the oscillator,
25~35min is vibrated under conditions of rotating speed is 180~200r/min, is then filtered with without phosphorus filter paper, uses beaker
Filtered fluid is spare described in access.
In above-mentioned assay method, in step (1), the HCl solution and the NaHCO3The volume ratio of aqueous solution can be
1：5~8, such as 1：6.7.
In above-mentioned assay method, when adding in the HCl solution, need carefully slowly to add, side edged shakes, and prevents
CO2Solution is made to spray bottleneck.
In above-mentioned assay method, before the inductive coupling plasma emission spectrograph (ICP) is detected, root is needed
According to instrument performance, the optimization of the measuring conditions such as argon flow amount, observed altitude, radio-frequency signal generator power, the time of integration is carried out；Measure phosphorus
When wavelength be 213.618nm.
Sodium bicarbonate provided by the invention extracts, hydrochloric acid adjusts acidity-inductive coupling plasma emission spectrograph (ICP-
OES) the method for the soil available phosphorus content measured, compared with existing method-sodium bicarbonate extraction-molybdenum-antimony anti-spectrophotometric method,
There was no significant difference for the result of measure, and assay method provided by the invention measures the rate of recovery of available phosphorus up to 92~106%,
And reproducibility is ideal.And existing method (sodium bicarbonate extraction-molybdenum-antimony anti-spectrophotometric method) testing procedure is more, colorimetric
Method is complicated for operation and the used time is more, and process color is affected to available phosphorus measurement result, and detection efficiency is low；And the present invention carries
The method of confession, quick and precisely, with the development of science and technology the method that ICP-OES methods measure soil available phosphorus, is that available phosphorus measures
Development trend, method provided by the invention can improve working efficiency, reduce analysis time, have reality and theoretical dual meaning
Justice.
Description of the drawings
Fig. 1 is the standard curve that assay method of the present invention (ICP-OES) obtains.
Fig. 2 is the standard curve that conventional method (sodium bicarbonate extraction-molybdenum-antimony anti-spectrophotometric method) obtains.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Reagent used in following embodiments is as follows：
Sodium hydroxide solution：ω (NaOH)=10%, it is soluble in water to weigh 10g sodium hydroxides, is diluted with water to 100ml.
Sodium bicarbonate solution：c(NaHCO3)=0.5mol/L weighs 42.0g sodium bicarbonates and is dissolved in about 800ml water, adds
Water is diluted to about 990ml, is adjusted to pH=8.5 and (is measured with pH meter) with sodium hydroxide solution (above-mentioned solution), water is added to be settled to
1L。
Hydrochloric acid solution：The hydrochloric acid solution of the hydrochloric acid composition of (1+1) HCl, the water of 1 part of volume and 1 part of volume.
Phosphorus standard solution：ρ (P)=100mg/L weighs 0.4394g potassium dihydrogen phosphates and is dissolved in about 200ml water, adds in 5ml
Then sulfuric acid is moved in 1000ml volumetric flasks, add water constant volume mixing.
Phosphorus standard solution：ρ (P)=5.00mg/L.The above-mentioned phosphorus standard solution of 5.00ml is measured in 100ml volumetric flasks,
Scale is diluted to above-mentioned sodium bicarbonate solution.
The measure of embodiment 1, soil available phosphorus content
First, the processing of sample
1st, the extraction of sample
Weigh soil sample 2.50g.It is placed in dry 150ml triangular flasks, NaHCO is added in into pedotheque3Solution 50mL,
It is placed on oscillator, rotating speed is 180~200r/min, vibrates 30min, is filtered immediately with without phosphorus filter paper, is filtered with beaker access
Liquid is spare.
2nd, the acidification of filtered fluid
Filtered fluid 20.0mL is in 50mL volumetric flasks for absorption, addition 3.0mL HCl solutions, adjusting filtrate pH (it is careful to add slowly,
Side edged shakes, the CO prevented2Solution is made to spray bottleneck).
3rd, upper ICP is measured
Wait CO2After fully releasing, scale is settled to deionized water, upper ICP is measured, and obtains radiation intensity.
Before measure, according to instrument performance, the surveys such as argon flow amount, observed altitude, radio-frequency signal generator power, the time of integration are carried out
Condition optimizing is measured, wavelength when measuring phosphorus is 213.618nm.
2nd, the drafting of standard working curve
The phosphorus standard solution 0 of absorption 50ug/mL, 0.20,0.50,1.00,5.00,10.00,20.00mL are in 50mL respectively
In volumetric flask, add c (NaHCO3The NaHCO of)=0.5mol/L, pH=8.53Solution 20.0mL adds the HCl solution of 3.0mL (1+1)
Adjusting pH value of solution, (careful to add slowly, side edged shakes, the CO prevented2Solution is made to spray bottleneck), wait CO2After fully releasing, spend
Ionized water constant volume, it is respectively 0ug/mL, 0.2ug/mL, 0.5ug/mL, 1.0ug/mL, 5.0ug/mL, 10.0ug/ to be configured to concentration
The standard series of mL and 20.0ug/mL, direct ICP are measured；Normal concentration numerical value (radiation intensity) corresponding with its is depicted as
Standard working curve.
3rd, result calculates
The mass fraction ω of available phosphorus, numerical value are represented with mg/kg in pedotheque,
In formula：
ρ0- from the developing solution (filtered fluid in i.e. one) that standard working curve acquires phosphorus concentration, unit mg/mL；
ρ2- from the blank solution that standard working curve acquires phosphorus concentration, unit mg/mL；
Blank solution refers to being not added with the filtered fluid obtained during pedotheque.
V-leaching liquor volume, unit mL；
M-sample quality, unit g；
D-point take multiple, sample extraction reagent (NaHCO3Solution) volume and filtered fluid volume ratio (in the present embodiment
Filtered fluid 20mL, NaHCO are drawn in step (2)3Digestion agent volume is 50mL, so D is 5:2).
The comparing result of embodiment 2, the method for the present invention and conventional method standard curve
The step of being drawn according to 1 standard curve of embodiment makes standard curve, be made phosphorus concentration (ug/mL) for 0,0.2,
0.5th, 1,5,10,20 standard series, corresponding radiation intensity is 11.4,23.7,52.5,102.5,491.4,957.5,
2074.4 (Int (s/s), draw standard curve it is as shown in Figure 1.
(sodium bicarbonate extraction-molybdenum-antimony anti-spectrophotometric method) makes standard curve according to conventional methods, and phosphorus concentration is made
(ug/mL) standard series for being 0,0.05,0.1,0.3,0.5,0.8 and 1, corresponding light absorption value is 0.002,0.039,0.79,
0.223rd, 0.376,0.578 and 0.682, the standard curve of drafting is as shown in Figure 2.
As depicted in figs. 1 and 2, the standard linear regression equation of the method for the present invention：Y=102.39x-6.3145, the equation
R be equal to 0.999, the curve of the method for the present invention and conventional method is ideal curve, illustrates that the method for the present invention curve has very
High accuracy.
Embodiment 3, different regions pedotheque different measuring methods contrast and experiment
By the pedotheque of different regions respectively with conventional method (sodium bicarbonate extraction-molybdenum-antimony anti-spectrophotometric method) and this
The assay method (ICP-OES) provided is invented, sample detection step such as embodiment 1 is operated, and is measured in pedotheque effectively
Phosphorus content, as a result as shown in 1 data of table.
The result that result and the conventional method that the measuring method of the present invention measures it can be seen from the data in table 1 measure without
Significant difference.
Available phosphorus in the method for the conventional method of table 1 and the present invention detection different regions soil
Note：(p<0.5).
Embodiment 4, the method for the present invention reproducibility
4 kinds of standard substances are chosen, identical 5 parts of samples is weighed, does parallel test, sample detection step such as embodiment 1 carries out
Operation, obtained data are shown in Table 2, and as can be seen from Table 2,4 kinds of standard substances, 5 parallel samples of each standard substance are surveyed
For fixed average value substantially close to intermediate value, and all in the range of indicated value allowable error, standard deviation is relatively low, therefore the invented party
Method has very high reproducibility and stability, suitable for promoting.
2 soil available Standard Reference Materials for Determination of table
Embodiment 5：Available phosphorus determination of recovery rates in pedotheque
6 parts of pedotheques are chosen, each soil sample weighs 2 parts of Duplicate Samples, wherein 1 part adds in standard solution and is measured, surveys
Determine step such as embodiment 1, so as to obtain the rate of recovery of available phosphorus, rate of recovery data are shown in Table 3, from table 3 it can be seen that using this hair
The rate of recovery for the available phosphorus that bright method measures shows to survey using the method (ICP-OES) of patented invention of the present invention more than 92%
Determine available phosphorus in soil and comply fully with requirement.
3 effective phosphorous recovery catalog data of table
Claims (9)
1. the assay method of available phosphorus content, includes the following steps in a kind of pedotheque：
(1) the phosphorus standard solution of at least three kinds of various concentrations is prepared, adds in NaHCO into the phosphorus standard solution respectively3Aqueous solution,
Then the pH value of HCl solution regulation system is added in, treats CO2After emptying, light is emitted using inductively coupled plasma after constant volume
Spectrometer is detected, and obtains radiation intensity；With a concentration of abscissa of phosphorus in the phosphorus standard solution, sat using radiation intensity to be vertical
Mark makes working curve；
(2) NaHCO is added in into pedotheque3Aqueous solution is extracted, filtered to obtain filtered fluid；
(3) it draws the filtered fluid and adds in the HCl solution and adjust pH value, treat CO2After emptying, the electricity is used after constant volume
Sense coupled plasma optical emission spectrometer is detected, and is obtained radiation intensity, according to the working curve, is obtained the filtered fluid
The concentration of middle P elements, is denoted as ρ0, unit mg/mL；
The concentration of available phosphorus in pedotheque is obtained according to formula (A), is denoted as ω, unit mg/kg,
In formula, ρ2Represent the concentration of P elements in the blank solution obtained according to standard curve, unit mg/mL；
The blank solution refers to the filtered fluid obtained when not adding in the pedotheque in step (2)；
V represents the volume of the filtered fluid, unit mL；
M represents the quality of pedotheque, unit g；
D, which represents to divide, takes multiple, i.e. NaHCO described in step (2)3The volume of aqueous solution takes the ratio of volume with dividing, and described point takes body
Product refers to the volume of filtered fluid described in step (3).
2. assay method according to claim 1, it is characterised in that：The phosphorus standard solution is water-soluble for potassium dihydrogen phosphate
Liquid；
The volumetric concentration of the phosphorus standard solution is 0~20 μ g/mL.
3. assay method according to claim 1 or 2, it is characterised in that：The NaHCO3The pH value of aqueous solution is 8.5, by
Sodium hydrate aqueous solution regulates and controls；
The NaHCO3A concentration of 0.5mol/L of aqueous solution.
4. assay method according to any one of claim 1-3, it is characterised in that：The HCl solution is by volume ratio
1：1 water and hydrochloric acid is prepared to obtain.
5. according to the assay method described in any one of claim 1-4, it is characterised in that：In step (2), the pedotheque
With the NaHCO3The proportioning of aqueous solution is：1g：20mL.
6. assay method according to any one of claims 1-5, it is characterised in that：In step (2), the pedotheque
For the sample after 1.0~2.0mm screenings.
7. according to the assay method described in any one of claim 1-6, it is characterised in that：In step (2), on the oscillator into
The row leach step,
25~35min is vibrated under conditions of rotating speed is 180~200r/min.
8. according to the assay method described in any one of claim 1-7, it is characterised in that：In step (1), the HCl solution
With the NaHCO3The volume ratio of aqueous solution is 1：5~8.
9. application of the inductive coupling plasma emission spectrograph in pedotheque in the measure of available phosphorus content.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109358039A (en) * | 2018-12-19 | 2019-02-19 | 青海省核工业地质局核地质研究所（（青海省核工业地质局检测试验中心）） | The measuring method of available phosphorus in a kind of soil |
| CN112577950A (en) * | 2020-12-14 | 2021-03-30 | 中信建设有限责任公司 | Method for determining available phosphorus in soil |
| CN113189017A (en) * | 2021-03-12 | 2021-07-30 | 北京农业信息技术研究中心 | Method and device for detecting content of available nitrogen, phosphorus and potassium in soil |
| CN114428062A (en) * | 2022-01-26 | 2022-05-03 | 辽宁省德明环境检测有限公司 | Method for detecting microbial phosphorus in wetland vegetation soil |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109358039A (en) * | 2018-12-19 | 2019-02-19 | 青海省核工业地质局核地质研究所（（青海省核工业地质局检测试验中心）） | The measuring method of available phosphorus in a kind of soil |
| CN109358039B (en) * | 2018-12-19 | 2021-08-24 | 青海省核工业地质局核地质研究所（（青海省核工业地质局检测试验中心）） | Method for determining available phosphorus in soil |
| CN112577950A (en) * | 2020-12-14 | 2021-03-30 | 中信建设有限责任公司 | Method for determining available phosphorus in soil |
| CN113189017A (en) * | 2021-03-12 | 2021-07-30 | 北京农业信息技术研究中心 | Method and device for detecting content of available nitrogen, phosphorus and potassium in soil |
| CN114428062A (en) * | 2022-01-26 | 2022-05-03 | 辽宁省德明环境检测有限公司 | Method for detecting microbial phosphorus in wetland vegetation soil |
| CN114428062B (en) * | 2022-01-26 | 2024-07-02 | 辽宁省德明环境检测有限公司 | Wetland vegetation soil microbial phosphorus detection method |
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Application publication date: 20180619 |