CN110095452A - Method that is a kind of while measuring phosphorus and potassium content in organic fertilizer - Google Patents
Method that is a kind of while measuring phosphorus and potassium content in organic fertilizer Download PDFInfo
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- CN110095452A CN110095452A CN201910485399.XA CN201910485399A CN110095452A CN 110095452 A CN110095452 A CN 110095452A CN 201910485399 A CN201910485399 A CN 201910485399A CN 110095452 A CN110095452 A CN 110095452A
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Abstract
The present invention relates to chemical analysis technology fields, and in particular to a method of phosphorus and potassium content in organic fertilizer are measured simultaneously.Method provided by the invention obtains organic fertilizer prepare liquid the following steps are included: to organic fertilizer progress digestion process；The organic fertilizer prepare liquid is subjected to inductance coupling plasma emissioning spectral analysis, the content of phosphorus and potassium in organic fertilizer is obtained according to the standard curve of phosphorus and potassium and gained emitted luminescence intensity.Compared from detection limit, Determination Limit, precision, accuracy and method etc., validity and accuracy when measuring basic, normal, high three kinds of different phosphates and potassium content organic fertilizer to the method for the present invention are assessed, the result shows that, potassium and phosphorus content in organic fertilizer are measured while method provided by the invention can be efficient, accurate, the content of potassium and phosphorus in the method measurement organic fertilizer of organic fertilizer standard (NY525-2012) can be substituted completely, so as to efficiently reduce the operating procedure of experiment, shorten experimental period, it is economical and practical.
Description
Technical field
The present invention relates to chemical analysis technology fields, and in particular to a kind of side for measuring phosphorus and potassium content in organic fertilizer simultaneously
Method.
Background technique
The conventional method of phosphorus and potassium is provided according to organic fertilizer standard (NY525-2012) in measurement organic fertilizer, is led to respectively
It crosses ultraviolet specrophotometer and flame photometer detects phosphorus and potassium therein, complex for operation step, time-consuming, effort, uneconomical reality
With.Therefore, it is necessary to establish it is a kind of quickly, efficiently, the accurate and method that measures phosphorus and potassium content in organic fertilizer simultaneously.
Summary of the invention
It is provided by the invention the purpose of the present invention is to provide a kind of method for measuring phosphorus and potassium content in organic fertilizer simultaneously
Method being capable of efficient, potassium and phosphorus in Accurate Determining organic fertilizer content.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of methods for measuring phosphorus and potassium content in organic fertilizer simultaneously, comprising the following steps:
Digestion process is carried out to organic fertilizer, obtains organic fertilizer prepare liquid；
The organic fertilizer prepare liquid is subjected to inductance coupling plasma emissioning spectral analysis, according to the standard of phosphorus and potassium song
Line and gained emitted luminescence intensity, obtain the content of phosphorus and potassium in organic fertilizer.
Preferably, digestion reagent used in the digestion process includes the concentrated sulfuric acid and hydrogenperoxide steam generator, the concentrated sulfuric acid
Density is 1.84g/cm3, the mass concentration of the hydrogenperoxide steam generator is 30%.
Preferably, the amount ratio of the organic fertilizer and dense sulfuric acid is (0.2~0.5) g:5mL.
Preferably, when carrying out the inductance coupling plasma emissioning spectral analysis, plasma rf power is
1000W。
Preferably, when carrying out the inductance coupling plasma emissioning spectral analysis, cooling air Ar, flow 0.2L/
min。
Preferably, when carrying out the inductance coupling plasma emissioning spectral analysis, auxiliary gas is Ar, flow 0L/
min。
Preferably, when carrying out the inductance coupling plasma emissioning spectral analysis, atomization gas Ar, flow 0.72L/
min。
Preferably, when carrying out the inductance coupling plasma emissioning spectral analysis, atomizing pressure 2.63bars.
Preferably, when carrying out the inductance coupling plasma emissioning spectral analysis, using peristaltic pump sample introduction, flow is
20r/min。
The present invention provides a kind of methods for measuring phosphorus and potassium content in organic fertilizer simultaneously, comprising the following steps: to organic
Fertilizer carries out digestion process, obtains organic fertilizer prepare liquid；The organic fertilizer prepare liquid is subjected to inductively coupled plasma body and emits light
Spectrum analysis obtains the content of phosphorus and potassium in organic fertilizer according to the standard curve of phosphorus and potassium and gained emitted luminescence intensity.The present invention is built
Stood using inductively coupled plasma atomic emission while the method that measures phosphorus and potassium content in organic fertilizer, and from detection limit,
Determination Limit, precision, accuracy and method compare etc., to the method for the present invention measure basic, normal, high three kinds of different phosphates and
Validity and accuracy when potassium content organic fertilizer are assessed, the results showed that, method provided by the invention can efficiently, accurately
While measurement organic fertilizer in potassium and phosphorus content, can substitute completely organic fertilizer standard (NY525-2012) method measurement have
The content of potassium and phosphorus in machine fertilizer shortens experimental period so as to efficiently reduce the operating procedure of experiment, economical and practical.
Detailed description of the invention
Fig. 1 is the standard curve of phosphorus；
Fig. 2 is the standard curve of potassium.
Specific embodiment
The present invention provides a kind of methods for measuring phosphorus and potassium content in organic fertilizer simultaneously, comprising the following steps:
Digestion process is carried out to organic fertilizer, obtains organic fertilizer prepare liquid；
The organic fertilizer prepare liquid is subjected to inductance coupling plasma emissioning spectral analysis, according to the standard of phosphorus and potassium song
Line and gained emitted luminescence intensity, obtain the content of phosphorus and potassium in organic fertilizer.
Organic fertilizer is mainly derived from plant and/or animal, is that one kind imposes on soil to provide plant nutrient as its main function
The carbonaceous material of energy.Specifically, organic fertilizer is eliminated simultaneously through biological substance, animals and plants waste, plant residue processing
Poisonous and harmful substance therein, is rich in a large amount of benefit materials, including a variety of organic acids, peptides and nitrogen abundant, phosphorus, potassium etc.
Nutrient can not only provide full nutrition for crops, and fertilizer efficiency is long, can increase and update the soil organism, promote micro-
Biological self reproducing improves the physicochemical property and bioactivity of soil, is the Main Nutrients of pollution-free food production.Potassium and phosphorus in organic fertilizer
Content it is comparatively not high, total nutrient generally requires as more than or equal to 5%, national standard analysis method, i.e. organic fertilizer standard
(NY525-2012), measuring potassium and phosphorus content in organic fertilizer is flame photometer and ultraviolet spectrophotometer method respectively, and operation is multiple
It is miscellaneous and can not realize while measure；And since organic fertilizer ground substance is complicated, and the content of potassium and phosphorus is not comparatively high, using normal
Potassium and phosphorus content in organic fertilizer are measured while rule method can not be efficient, accurate.The present invention, which establishes, utilizes inductive coupling
Plasma emission spectroscopy simultaneously measure phosphorus and potassium content in organic fertilizer method, and from detection limit, Determination Limit, precision,
Accuracy and method compare etc., when measuring basic, normal, high three kinds of different phosphates and potassium content organic fertilizer to the method for the present invention
Validity and accuracy are assessed, the results showed that, method provided by the invention measures organic fertilizer while can be efficient, accurate
Middle potassium and phosphorus content can substitute containing for potassium and phosphorus in the method measurement organic fertilizer of organic fertilizer standard (NY525-2012) completely
Amount shortens experimental period so as to efficiently reduce the operating procedure of experiment, economical and practical.
The present invention carries out digestion process to organic fertilizer, obtains organic fertilizer prepare liquid.The present invention is to the organic fertilizer without spy
Different restriction, using any organic fertilizer well known to those skilled in the art.In the present invention, disappear used in the digestion process
Change reagent and preferably include the concentrated sulfuric acid and hydrogenperoxide steam generator, the density of the concentrated sulfuric acid is preferably 1.84g/cm3, the peroxidating
The mass concentration of hydrogen solution is preferably 30%.In the present invention, the amount ratio of the organic fertilizer and the concentrated sulfuric acid be preferably (0.2~
0.5) g:5mL；The present invention does not have the dosage of the hydrogenperoxide steam generator special restriction, can guarantee that the organic fertilizer fills
Divide digestion.In the present invention, the method for the digestion process, preferably includes following steps:
It is stood after organic fertilizer, the concentrated sulfuric acid and hydrogenperoxide steam generator are mixed, obtains mixed material；
The mixed material is heated to the concentrated sulfuric acid to smolder, hydrogenperoxide steam generator is added dropwise in batches and continues to heat, until
System obtains digestive juice in colourless or faint yellow clear liquid；
It will be filtered after the digestive juice constant volume, obtain organic fertilizer prepare liquid.
The present invention is stood after preferably mixing organic fertilizer, the concentrated sulfuric acid and hydrogenperoxide steam generator, obtains mixed material.The present invention
Charging sequence and hybrid mode do not have special restriction when to the mixing of the organic fertilizer, the concentrated sulfuric acid and hydrogenperoxide steam generator,
Guarantee each component can be uniformly mixed under the premise of safety, hydrogenperoxide steam generator (mistake is such as sequentially added into organic fertilizer
The additional amount of hydrogen peroxide solution is preferred are as follows: the amount ratio of organic fertilizer and hydrogenperoxide steam generator is (0.2~0.5) g:1.5mL) and it is dense
Sulfuric acid.In the present invention, the time of the standing is preferably 10~15h；Organic fertilizer is sufficiently infiltrated during standing, is conducive to
It is sufficiently digested.In an embodiment of the present invention, specifically organic fertilizer is placed in a beaker, the concentrated sulfuric acid is added and hydrogen peroxide is molten
Liquid shakes up, and stands overnight, and obtains mixed material.
After obtaining mixed material, the mixed material is preferably heated to the concentrated sulfuric acid and smoldered by the present invention, is added dropwise in batches
Hydrogen peroxide solution simultaneously continues to heat, until system obtains digestive juice in colourless or faint yellow clear liquid.Present invention preferably employs adjustable
Electric furnace carries out the heating.In the present invention, during the hydrogenperoxide steam generator of dropwise addition in batches, peroxide is added dropwise in every batch of
The amount for changing hydrogen solution is preferably gradually successively decreased, and hydrogenperoxide steam generator is added dropwise again after preferably slightly cooling down mixed system, to guarantee to have
The sufficiently digestion of machine fertilizer.In an embodiment of the present invention, mixed material is specifically slowly heated to by the concentrated sulfuric acid using adjustable electric furnace
It smolders, removes, slightly cold rear dropwise addition hydrogenperoxide steam generator, jog beaker heats 10min；It removes, hydrogen peroxide is added dropwise again after slightly cold
Solution, jog beaker heat 10min；The step of hydrogenperoxide steam generator is added dropwise and heats is repeated, until system is in colourless or yellowish
After color clear liquid, continues to heat 10min, eliminate remaining hydrogen peroxide, obtain digestive juice；Remove, it is slightly cold after by the digestive juice
It moves into 100mL volumetric flask, adds water constant volume；Gained sample solution is filled into triangular flask with without phosphorus Filter Paper Dry, is obtained
Organic fertilizer prepare liquid is spare.During above-mentioned digestion process, the present invention does not make special limit to the slightly cold degree and mode
It is fixed, using mode well known to those skilled in the art.
After obtaining organic fertilizer prepare liquid, the organic fertilizer prepare liquid is carried out inductively coupled plasma body and emits light by the present invention
Spectrum analysis obtains the content of phosphorus and potassium in organic fertilizer according to the standard curve of phosphorus and potassium and gained emitted luminescence intensity.In the present invention
In, when carrying out the inductance coupling plasma emissioning spectral analysis, preferably surveyed under conditions of launch wavelength is 213.640nm
The emitted luminescence intensity for determining phosphorus measures the emitted luminescence intensity of potassium under conditions of launch wavelength is 766.490nm.In the present invention,
When carrying out the inductance coupling plasma emissioning spectral analysis, plasma rf power is preferably 1000W；Cooling air is preferred
For Ar, flow is preferably 0.2L/min；Assisting gas preferably to assist gas is Ar, and flow is preferably 0L/min (that is, without auxiliary gas
Under conditions of carry out inductance coupling plasma emissioning spectral analysis)；Atomization gas is preferably Ar, and flow is preferably 0.72L/min；
Atomizing pressure is preferably 2.63bars；Using peristaltic pump sample introduction, flow is preferably 20r/min.In an embodiment of the present invention, have
Body is to be purchased from JOBIN-YVON using ULTIMA inductive coupling plasma emission spectrograph.
In the present invention, the standard curve of the phosphorus and potassium specifically includes the standard curve of phosphorus and the standard curve of potassium, point
It is not using the mass concentration of phosphorus or the mass concentration of potassium as abscissa, corresponding emitted luminescence intensity is that ordinate is drawn to obtain.?
In the present invention, the method for establishing the standard curve of the phosphorus and potassium preferably includes following steps:
The mixed standard solution of series of concentrations is provided；
The mixed standard solution of the series of concentrations is subjected to inductance coupling plasma emissioning spectral analysis respectively, with hair
Penetrating luminous intensity is ordinate, and concentration is abscissa, and emitted luminescence intensity makees linear equation to concentration, respectively obtains the standard curve of phosphorus
With the standard curve of potassium.
Present invention preferably provides the mixed standard solutions of series of concentrations.In the present invention, the mixed standard solution is dense
Degree ranges preferably from 0~50.0 μ g/mL (concentration of the mixed standard solution is 0 μ g/mL, i.e., does not include phosphorus and potassium).This hair
The bright preparation method for the mixed standard solution does not have special restriction, molten using standard well known to those skilled in the art
The preparation method of liquid.In an embodiment of the present invention, the phosphorus standard substance (GSB04- of 1000mg/L is specifically pipetted respectively
1741-2004 (b)) and potassium standard substance (GSB04-1733-2004) 0mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL,
5.0mL is placed in 7 100mL volumetric flasks, 5wt% sulfuric acid solution constant volume, the concentration of phosphorus and potassium point in gained mixed standard solution
It Wei not 0.00 μ g/mL, 5.0 μ g/mL, 10.0 μ g/mL, 15.0 μ g/mL, 20.0 μ g/mL, 25.0 μ g/mL, 50.0 μ g/mL.
After obtaining the mixed standard solution of series of concentrations, the present invention is preferably by the mixed standard solution of the series of concentrations point
Not carry out inductance coupling plasma emissioning spectral analysis, using emitted luminescence intensity as ordinate, concentration is abscissa, emit light intensity
Degree makees linear equation to concentration, respectively obtains the standard curve of phosphorus and the standard curve of potassium.In the present invention, the inductive coupling
The condition of plasma emission spectrometry preferably with the inductance coupling that uses when measuring organic fertilizer prepare liquid in above-mentioned technical proposal
The consistent of plasma emission spectrometry is closed, is no longer repeated herein.In an embodiment of the present invention, the phosphorus
Standard curve and related coefficient are respectively I=290.9+564.5*C, R2=0.99944 (I is emitted luminescence intensity；C is that quality is dense
Degree, μ g/mL；R2For related coefficient)；The standard curve and related coefficient of the potassium are respectively I=2614+8011*C, R2=
0.9997 (I is emitted luminescence intensity；C is mass concentration, μ g/mL；R2For related coefficient).
In the present invention, available to have according to the emitted luminescence intensity of the standard curve of phosphorus and potassium and organic fertilizer prepare liquid
The mass concentration of phosphorus and potassium in machine fertilizer prepare liquid, and then obtain the content of phosphorus and potassium in organic fertilizer.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.It is aobvious
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Embodiment 1
The drafting of 1 standard curve
The phosphorus standard substance (GSB04-1741-2004 (b)) and potassium standard substance (GSB04- of 1000mg/L are pipetted respectively
1733-2004) 0mL, 0.5mL, 1.0mL, 1.5mL, 2.0mL, 2.5mL, 5.0mL are placed in 7 100mL volumetric flasks, 5wt%
Sulfuric acid solution constant volume, the concentration of phosphorus and potassium is respectively 0.00 μ g/mL, 5.0 μ g/mL, 10.0 μ g/ in gained mixed standard solution
mL,15.0μg/mL,20.0μg/mL,25.0μg/mL,50.0μg/mL；By the mixed standard solution carry out inductive coupling etc. from
Daughter emission spectrographic analysis, using emitted luminescence intensity as ordinate, concentration is abscissa, and emitted luminescence intensity makees linear side to concentration
Journey respectively obtains the standard curve of phosphorus and the standard curve of potassium, as shown in Fig. 1~2 and table 1；Wherein, carry out inductive coupling etc. from
Instrument needed for daughter emission spectrographic analysis is ULTIMA inductive coupling plasma emission spectrograph, is purchased from JOBIN-YVON, point
Analysis condition is specific as follows:
The emitted luminescence intensity that phosphorus is measured under conditions of launch wavelength is 213.640nm is 766.490nm in launch wavelength
Under conditions of measure potassium emitted luminescence intensity；
Plasma rf power is 1000W；
Cooling air is Ar, flow 0.2L/min；
Auxiliary gas is Ar, flow 0L/min；
Atomization gas is Ar, flow 0.72L/min；
Atomizing pressure is 2.63bars；
Using peristaltic pump sample introduction, flow 20r/min.
The standard curve of 1 phosphorus of table and the standard curve of potassium
As shown in Table 1, the standard curve of gained potassium and phosphorus, phase relation are measured using inductive coupling plasma emission spectrum method
Number R2> 0.999, linearly dependent coefficient is good, and the range of linearity is larger, can satisfy practical measurement and requires (in majority of case
Under, it will be settled to 100mL after 0.2~0.5g organic fertilizer digestion process, not needing further to dilute gained stoste can be simultaneously
The content of Accurate Determining phosphorus and potassium).
The measurement of 2 samples
2.1 prepare organic fertilizer prepare liquid
Weigh 0.2g~0.5g (be precisely placed in 100mL beaker to 0.0001g) organic fertilizer, be added the 5mL concentrated sulfuric acid (ρ=
1.84g/cm3) and 1.5mL concentration be 30wt% hydrogenperoxide steam generator, carefully shake up, stand overnight；Later in adjustable electric furnace
On be slowly heated to the concentrated sulfuric acid and smolder, remove, 15 drop 30wt% hydrogenperoxide steam generators, jog beaker, heating be added dropwise after slightly cold
10min；It removes, 5 drop 30wt% hydrogenperoxide steam generators is added dropwise after slightly cold again, repeat 30wt% hydrogenperoxide steam generator is added dropwise and simultaneously heat
The step of, until continuing to heat 10min, eliminating remaining hydrogen peroxide after system is in colourless；It removes, gained disappears after slightly cold
Change liquid to move into 100mL volumetric flask, adds water constant volume；Gained sample solution is filled into triangular flask with without phosphorus Filter Paper Dry,
It is spare to obtain organic fertilizer prepare liquid.
2.2 preparation blank prepare liquids
In addition to organic fertilizer is not added, other reagent types, dosage and operation are obtained with " 2.1 organic fertilizer digestion process " step
Blank prepare liquid is spare.
2.3 measurement
According to inductance coupling plasma emissioning spectral analysis condition in " drafting of 1 standard curve " step, have to described
Machine fertilizer prepare liquid and blank prepare liquid carry out inductance coupling plasma emissioning spectral analysis.
2.3.1 inductively coupled plasma emission spectrography measures the detection limit of potassium and phosphorus in organic fertilizer
Blank prepare liquid is measured, is measured in parallel 10 times, each measurement result is converted into according to " 2.3 measurement " step
Concentration in sample, Determination Limit be four times detection limit (by 0.2g sample, be settled to 100mL on the basis of, the detection of calculation method
Limit), it the results are shown in Table 2.Wherein, detection limit can be calculated according to the following formula:
Wherein: MDL-detection limit, %；
N-parallel determination number, n=10；
S-n times are measured in parallel the standard deviation of phosphorus or potassium content in blank prepare liquid；
xi- i-th measures the content of phosphorus or potassium in blank prepare liquid, %；
The average value of phosphorus or potassium content in-i times measurement blank prepare liquid, %；
tn-1T when-freedom degree is n-1, confidence interval is 99% is distributed (unilateral side).
2 inductively coupled plasma emission spectrography of table measures the detection limit of potassium and phosphorus in organic fertilizer
| Experiment number | K content (%) | P content (%) |
| 1 | 0.00630 | 0.01729 |
| 2 | 0.00642 | 0.01718 |
| 3 | 0.00642 | 0.01729 |
| 4 | 0.00648 | 0.01695 |
| 5 | 0.00624 | 0.01683 |
| 6 | 0.00630 | 0.01775 |
| 7 | 0.00660 | 0.01775 |
| 8 | 0.00654 | 0.01718 |
| 9 | 0.00648 | 0.01706 |
| 10 | 0.00624 | 0.01740 |
| s | 0.000127 | 0.000304 |
| Detection limit | 0.000357 | 0.000859 |
| Determination Limit | 0.001429 | 0.003435 |
As shown in Table 2, the detection limit of this method measurement potassium and Determination Limit are respectively 0.000357% and 0.001429%,
The detection limit and Determination Limit of phosphorus are respectively 0.000859% and 0.003435%, illustrate that method provided by the invention can detect
The content of potassium and phosphorus is respectively 0.001429% and 0.003435% in organic fertilizer, is fully able to meet to potassium in organic fertilizer and phosphorus
Measurement request.
2.3.2 the precision of method
6 times are carried out respectively to the organic fertilizer (being denoted as sample 1, sample 2 and sample 3 respectively) of three kinds of different phosphates and potassium content to put down
Row experiment, the results are shown in Table 3.Wherein, the precision of method indicates that calculation formula is as follows with relative standard deviation:
Wherein, RSD-relative standard deviation, %；
N-parallel determination number, n=6；
S-n times are measured in parallel the standard deviation of phosphorus or potassium content in organic fertilizer；
ci- i-th measures the content of phosphorus or potassium in organic fertilizer, %；
The average value of phosphorus or potassium content in-i times measurement organic fertilizer, %.
The precision data of 3 method of table
As shown in Table 3, the precision of potassium and phosphorus is respectively 0.93% and 1.17%, the essence of potassium and phosphorus in sample 2 in sample 1
Density is respectively 0.44% and 0.62%, and the precision of potassium and phosphorus is respectively 2.00% and 0.28% in sample 3.Three kinds of different phosphates
In the organic fertilizer of potassium content, the precision of potassium and phosphorus is measured no more than 2.00%, illustrates inductive coupling provided by the invention
The result stability of potassium and phosphorus in Coupled Plasma-Atomic Emission Spectrometric Determination organic fertilizer is preferable.
2.3.3 the accuracy of method
It is separately added into 1000mg/mL phosphorus and potassium standard solution 0.5mL, 2mL and 5mL in 5wt% sulfuric acid solution, then presses
According to " 2.1 prepare organic fertilizer prepare liquid " and " 2.3 measurement " step process and measurement, 6 parallel laboratory tests of every group of carry out, as a result such as table
Shown in 4, low concentration, middle concentration and high concentration respectively correspond phosphorus in table 4 and potassium standard solution additive amount is 0.5mL, 2mL and 5mL.
The accuracy data of 4 method of table
As shown in Table 4,98.9~101%, method is quasi- for low concentration, middle concentration and high potassium concentration and phosphorus recovery of standard addition
Exactness can reach the needs of potassium and phosphorus in detection organic fertilizer.
2.3.4 organic fertilizer standard (NY525-2012) method and inductively coupled plasma emission spectrography in the present invention
The result of phosphorus and potassium content in organic fertilizer is measured to compare
The organic fertilizer (being denoted as sample 1, sample 2 and sample 3 respectively) for taking three kinds of different phosphates and potassium content, respectively according to organic
Fertilizer standard (NY525-2012) method and the present invention in inductively coupled plasma emission spectrography measurement organic fertilizer in phosphorus and
The content of potassium, 6 parallel laboratory tests of every group of carry out.Statistical software is analyzed to the result of two kinds of different measurement methods with SPSS 19.0
T inspection is carried out, whether discriminatory analysis result has significant difference.It the results are shown in Table 5.
5 organic fertilizer standard (NY525-2012) method of table is surveyed with inductively coupled plasma emission spectrography in the present invention
Determine the result comparison data of phosphorus and potassium content in organic fertilizer
Remarks: K1And K2It respectively indicates flame photometer and inductive coupling plasma emission spectrum measures K content；P1And P2
It respectively indicates ultraviolet specrophotometer and inductive coupling plasma emission spectrum measures P content.
As shown in Table 5, compared with organic fertilizer standard (NY525-2012) method, present invention inductively coupled plasma
Emission spectrum measures the potassium and phosphorus in the organic fertilizer of three kinds of different phosphates and potassium content (including basic, normal, high content is included) simultaneously,
Phosphorus and potassium content measurement result in every group of sample there are no significant difference, illustrate inductively coupled plasma body provided by the invention
Emission spectrum measures the method for phosphorus and potassium in organic fertilizer simultaneously can substitute traditional organic fertilizer standard (NY525-2012) completely
Method.
As seen from the above embodiment, the present invention is established using inductively coupled plasma atomic emission while being measured organic
The method of phosphorus and potassium content in fertilizer, and from detection limit, Determination Limit, precision, accuracy and method comparison etc., to this
The validity and accuracy for inventing the method provided are assessed, the results showed that, method provided by the invention can be efficient, quasi-
Potassium and phosphorus content, the method that can substitute organic fertilizer standard (NY525-2012) completely measure in measurement organic fertilizer while really
The content of potassium and phosphorus in organic fertilizer shortens experimental period so as to efficiently reduce the operating procedure of experiment, economical and practical.
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 (10)
1. a kind of method for measuring phosphorus and potassium content in organic fertilizer simultaneously, which comprises the following steps:
Digestion process is carried out to organic fertilizer, obtains organic fertilizer prepare liquid；
By the organic fertilizer prepare liquid carry out inductance coupling plasma emissioning spectral analysis, according to the standard curve of phosphorus and potassium with
Gained emitted luminescence intensity obtains the content of phosphorus and potassium in organic fertilizer.
2. the method according to claim 1, wherein digestion reagent used in the digestion process include the concentrated sulfuric acid and
Hydrogenperoxide steam generator, the density of the concentrated sulfuric acid are 1.84g/cm3, the mass concentration of the hydrogenperoxide steam generator is 30%.
3. according to the method described in claim 2, it is characterized in that, the amount ratio of the organic fertilizer and the concentrated sulfuric acid be (0.2~
0.5) g:5mL.
4. the method according to claim 1, wherein carrying out the inductance coupling plasma emissioning spectral analysis
When, the emitted luminescence intensity of phosphorus is measured under conditions of launch wavelength is 213.640nm, in the item that launch wavelength is 766.490nm
The emitted luminescence intensity of potassium is measured under part.
5. according to the method described in claim 4, it is characterized in that, carrying out the inductance coupling plasma emissioning spectral analysis
When, plasma rf power is 1000W.
6. according to the method described in claim 4, it is characterized in that, carrying out the inductance coupling plasma emissioning spectral analysis
When, cooling air Ar, flow 0.2L/min.
7. according to the method described in claim 4, it is characterized in that, carrying out the inductance coupling plasma emissioning spectral analysis
When, auxiliary gas is Ar, flow 0L/min.
8. according to the method described in claim 4, it is characterized in that, carrying out the inductance coupling plasma emissioning spectral analysis
When, atomization gas Ar, flow 0.72L/min.
9. the method according to claim 4 or 8, which is characterized in that carry out the inductively coupled plasma atomic emission
When analysis, atomizing pressure 2.63bars.
10. according to the method described in claim 4, it is characterized in that, carrying out the inductively coupled plasma atomic emission point
When analysis, using peristaltic pump sample introduction, flow 20r/min.
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| CN111272741A (en) * | 2020-03-12 | 2020-06-12 | 内蒙古路易精普检测科技有限公司 | ICP (inductively coupled plasma) determination method for phosphorus pentoxide and potassium oxide in organic fertilizer |
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