CN106442473A - Detection method of element content in compound fertilizer - Google Patents
Detection method of element content in compound fertilizer Download PDFInfo
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- CN106442473A CN106442473A CN201610791896.9A CN201610791896A CN106442473A CN 106442473 A CN106442473 A CN 106442473A CN 201610791896 A CN201610791896 A CN 201610791896A CN 106442473 A CN106442473 A CN 106442473A
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- measured
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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
- G01N21/71—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited
- G01N21/73—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light thermally excited using plasma burners or torches
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
Abstract
The invention discloses a detection method of the element content in a compound fertilizer. The method comprises the following steps that 1, a nitrite acid solution is adopted for dissolving the compound fertilizer to obtain a to-be-detected solution containing to-be-detected elements; 2, an inductive coupling plasma emission spectrometer is adopted for detecting the to-be-detected solution obtained in the step 1 to obtain the content of the to-be-detected elements, wherein the to-be-detected elements at least include one or more of S, Zn, Mg, Fe, Mn and Al. The nitrite acid is adopted for dissolving the compound fertilizer, dissolution is convenient and complete, the inductive coupling plasma emission spectrometer is adopted for determining the to-be-detected elements, the consumption of chemical reagents is small, environmental pollution is reduced, operation can be performed at normal temperature, operation is safe and easy, meanwhile, various elements in the compound fertilizer are analyzed, determination is rapid, the accuracy is high, and the precision is good.
Description
Technical field
The present invention relates to detection of content of element technical field is and in particular to adopt inductive coupling plasma emission spectrograph
The method measuring constituent content in complex fertilizer.
Background technology
The development that raising with living standards of the people and agricultural commodity produce, high yield, high-quality, high benefit are agriculture lifes
Produce the comprehensive assessment target with technology.Realize this target, in addition to breeding, high-quality chemical fertilizer and to apply fertilizers scientifically be important hand
Section, accelerated development presented in compound fertilizer industry is imperative.
Wherein, complex fertilizer is because containing various plants nutrient, proportion balance, it is convenient to apply, and saves and stores, transports, applying expense
With, the good advantage of effect of increasing production, it has also become the leading products in international Fertilizer Market, be also Chinese Growth of Chemical Fertilizer Industry must
So.
Therefore, the detection of element in complex fertilizer is monitored to promotion agricultural development, environmental protection important in inhibiting.Survey
During fixed, typically adopt water soluble method to dissolve complex fertilizer, wherein partial salts compound is difficult to be directly dissolved in water, lead to examine
Survey result inaccurate.On the other hand, measure the content of sulphur, magnesium elements using chemical analysis method, it is more to be related to chemical reagent, dirty
Dye environment, operating process is tediously long numerous and diverse.Sulfur content is measured using calcination method, needs high temperature, operational hazards；Measured using chemistry titration
Magnesium elements, operating error is big.Content using iron, manganese, Zn-ef ficiency in atomic absorption spectroscopy determination fertilizer.Atomic absorption
AAS can only survey an element every time, time-consuming longer.
Content of the invention
In view of this, the application provides a kind of detection method of constituent content in complex fertilizer.This detection method reduces ring
Border is polluted, and dissolving is convenient, simple to operate, measures quick, accurately.
In order to solve above-mentioned technical problem, the technical scheme that the present invention provides is a kind of inspection of constituent content in complex fertilizer
Survey method is it is characterised in that comprise the steps：
1) solution to be measured containing element to be measured is obtained using salpeter solution dissolving complex fertilizer；
2) adopting inductive coupling plasma emission spectrograph to described step 1) the dilution solution to be measured that obtains examines
Survey, obtain described constituent content to be measured.
Described element to be measured, is at least included one or more in S, Zn, Mg, Fe, Mn, Al.
Preferably, described step 2) it is specially：Criterion working curve；Dilute solution to be measured, using inductive etc.
Ionomer emission spectrum instrument measures element emitted luminescence intensity to be measured in the solution to be measured after dilution；After must being diluted according to measurement result
Solution to be measured in element to be measured concentration；Calculate the mass fraction of constituent content to be measured according to the concentration of element to be measured.
Preferably, the mass fraction of described constituent content to be measured is calculated as follows：
In formula：
X is the mass percent of element to be measured in complex fertilizer, and numerical value is represented with %；C is the concentration of described element to be measured,
Unit is mg/L；V is the volume of the solution to be measured after described dilution, and unit is mL；M is complex fertilizer quality, and unit is g.
Preferably, described element to be measured, including one or more in S, Zn, Mg.
Preferably, described element to be measured, presented in compound state in complex fertilizer.
Preferably, described working curve of setting up is specially：With standard reserving solution, make respectively in multiple proportion concentration
Standard liquid, using the intensity of inductive coupling plasma emission spectrograph bioassay standard solution liquid, according to concentration strengths relation
Draw out working curve.
Preferably, described complex fertilizer phosphoric acid one ammonium and/or Diammonium phosphate (DAP).
Preferably, in described salpeter solution, nitric acid and the volume ratio of water are (1～2):(1～2).
Preferably, in described salpeter solution, nitric acid and the volume ratio of water are (1～1.5):(1～1.5).
Preferably, in described salpeter solution, nitric acid and the volume ratio of water are 1:1
Preferably, described concentration of standard solution is respectively 0.00mg/L, 50.00mg/L, 100.00mg/L, 150.00mg/
L、200.00mg/L.
Preferably, described inductive coupling plasma emission spectrograph testing conditions exciting power is 1.0～1.2Kw.
Preferably, described inductive coupling plasma emission spectrograph testing conditions exciting power is 1.05～1.15Kw.
Preferably, described inductive coupling plasma emission spectrograph testing conditions exciting power is 1.1Kw.
Preferably, described inductive coupling plasma emission spectrograph testing conditions pump speed is 1.0～1.4r/min.
Preferably, described inductive coupling plasma emission spectrograph testing conditions pump speed is 1.1～1.3r/min.
Preferably, described inductive coupling plasma emission spectrograph testing conditions pump speed is 1.2r/min.
Preferably, described inductive coupling plasma emission spectrograph testing conditions cooling gas flow is 15～25LPM.
Preferably, described inductive coupling plasma emission spectrograph testing conditions cooling gas flow is 17～21LPM.
Preferably, described inductive coupling plasma emission spectrograph testing conditions cooling gas flow is 19LPM.
Preferably, described inductive coupling plasma emission spectrograph testing conditions cooling gas is argon gas.
Preferably, described inductive coupling plasma emission spectrograph testing conditions nebulizer pressure is 30～40PSI.
Preferably, described inductive coupling plasma emission spectrograph testing conditions nebulizer pressure is 33～38PSI.
Preferably, described inductive coupling plasma emission spectrograph testing conditions nebulizer pressure is 35PSI.
Preferably, described inductive coupling plasma emission spectrograph testing conditions emission lines wavelength is S：180.731nm、
Zn：206.200nm、Mg：285.213nm、Fe：238.204nm、Mn：293.306nm、Al：396.152nm.Preferably, described
Inductive coupling plasma emission spectrograph testing conditions secondary air amount is 0LPM.
Compared with prior art, its detailed description is as follows for the application：The present invention adopts nitric acid to dissolve complex fertilizer, dissolving side
Just, completely；Element to be measured is measured using inductive coupling plasma emission spectrograph, atom transits to high level institute by low-lying level
The energy needing, is to produce high-frequency electrical magnetic energy by RF generator, is coupled to by the quarter bend of cooling gas air-flow by coil, thus producing
Raw plasma.The light intensity of the characteristic spectral line that measurement standard solution is launched, then measure the characteristic spectral line intensity of concentration to be measured, from
And determining the concentration of solution to be measured, chemical reagent using few, reduces environmental pollution, normal-temperature operation, safe operation, simple, simultaneously
Multiple element in analysis complex fertilizer, mensure is quick, the degree of accuracy is high, precision is good.
Specific embodiment
In order that those skilled in the art more fully understands technical scheme, with reference to specific embodiment pair
The present invention is described in further detail.
The invention discloses in a kind of complex fertilizer constituent content detection method, those skilled in the art can use for reference this
Civilian content, is suitably modified technological parameter and realizes.Specifically, all similar replacements and change are to art technology
It is it will be apparent that they are considered as including in the present invention for personnel.The method of the present invention and application have been passed through preferably
Embodiment is described, and related personnel substantially can be to side as herein described in without departing from present invention, spirit and scope
Method and application are modified or suitably change and combine, and to realize and to apply the technology of the present invention.
In order to realize foregoing invention purpose, the present invention provides technical scheme below：
In a kind of complex fertilizer, the detection method of constituent content is it is characterised in that comprise the steps：
1) solution to be measured containing element to be measured is obtained using salpeter solution dissolving complex fertilizer；
2) adopting inductive coupling plasma emission spectrograph to described step 1) solution to be measured that obtains detects, obtains
Obtain described constituent content to be measured.
Described element to be measured, including one or more in S, Zn, Mg, Fe, Mn, Al.
Described step 2) it is specially：With standard reserving solution, make respectively concentration be respectively 0.00mg/L, 50.00mg/L,
The standard liquid of 100.00mg/L, 150.00mg/L, 200.00mg/L, is measured using inductive coupling plasma emission spectrograph
The intensity of standard liquid liquid, draws out working curve according to concentration strengths relation；Dilute solution to be measured, using inductive etc. from
Daughter emission spectrometer measures element emitted luminescence intensity to be measured in the solution to be measured after dilution；After must being diluted according to measurement result
The concentration of element to be measured in solution to be measured；Calculate the mass fraction of constituent content to be measured according to the concentration of element to be measured.
The mass fraction of described constituent content to be measured is calculated as follows：
In formula：
X is the mass percent of element to be measured in complex fertilizer, and numerical value is represented with %；C is the concentration of described element to be measured,
Unit is mg/L；V is the volume of the solution to be measured after described dilution, and unit is mL；M is complex fertilizer quality, and unit is g.
Described complex fertilizer phosphoric acid one ammonium and/or Diammonium phosphate (DAP).In some embodiments that the present invention provides, described multiple
Complex fertilizer material phosphoric acid one ammonium；In some embodiments that the present invention provides, described complex fertilizer phosphoric acid two ammonium；Carry in the present invention
For other embodiments in, described complex fertilizer phosphoric acid one ammonium and Diammonium phosphate (DAP)；.
In described salpeter solution, nitric acid and the volume ratio of water are (1～2):(1～2), preferably 1:1.There is provided in the present invention
Some embodiments in, in described salpeter solution, the volume ratio of nitric acid and water is 2:1；Some embodiments providing in the present invention
In, in described salpeter solution, nitric acid and the volume ratio of water are 1.5:1；In some embodiments that the present invention provides, described nitric acid
In solution, nitric acid and the volume ratio of water are 1:1；In some embodiments that the present invention provides, nitric acid and water in described salpeter solution
Volume ratio be 1:1.5；In other embodiments that the present invention provides, in described salpeter solution, nitric acid and the volume ratio of water are
1:2.
Described element to be measured, presented in compound state in complex fertilizer, at least includes S, Zn, Mg, Fe, Mn, Al
In one or more.
Described inductive coupling plasma emission spectrograph testing conditions exciting power is 1.0～1.2Kw, preferably 1.05
～1.15Kw, more preferably 1.1Kw.In some embodiments that the present invention provides, described exciting power is 1.0Kw；At this
In some embodiments of bright offer, described exciting power is 1.05Kw；In some embodiments that the present invention provides, described excite
Power is 1.1Kw；In some embodiments that the present invention provides, described exciting power is 1.15Kw；Another in present invention offer
In some embodiments, described exciting power is 1.2Kw.
Described inductive coupling plasma emission spectrograph testing conditions pump speed is 1.0～1.4r/min, preferably 1.1～
1.3r/min, more preferably 1.2r/min.In some embodiments that the present invention provides, described pump speed is 1.0r/min；At this
In some embodiments that invention provides, described pump speed is 1.1r/min；In some embodiments that the present invention provides, described pump speed
For 1.2r/min；In some embodiments that the present invention provides, described pump speed is 1.3r/min；The present invention provide other
In embodiment, described pump speed is 1.4r/min.
Described inductive coupling plasma emission spectrograph testing conditions cooling gas is preferably argon gas；Cooling gas flow is 15
～25LPM, preferably 17～21LPM, more preferably 19LPM.In some embodiments that the present invention provides, described cooling air-flow
Measure as 15LPM；In some embodiments that the present invention provides, described cooling gas flow is 17LPM；Some providing in the present invention
In embodiment, described cooling gas flow is 19LPM；In some embodiments that the present invention provides, described cooling gas flow is
21LPM；In other embodiments that the present invention provides, described cooling gas flow is 25LPM.
Described inductive coupling plasma emission spectrograph testing conditions nebulizer pressure is 30～40PSI, preferably 33
～38PSI, preferably 35PSI.In some embodiments that the present invention provides, described nebulizer pressure is 30PSI；In the present invention
In some embodiments providing, described nebulizer pressure is 33PSI；In some embodiments that the present invention provides, described atomization
Device pressure is 35PSI；In some embodiments that the present invention provides, described nebulizer pressure is 38PSI；There is provided in the present invention
In other embodiments, described nebulizer pressure is 40PSI.
Described inductive coupling plasma emission spectrograph testing conditions emission lines wavelength is S：180.731nm、Zn：
206.200nm、Mg：285.213nm、Fe：238.204nm、Mn：293.306nm、Al：396.152nm.Preferably, described inductance
Coupled plasma optical emission spectrometer testing conditions secondary air amount is 0LPM.
Embodiment 1～6
Determining instrument：Prodigy XP inductive coupling plasma emission spectrograph；Electronic balance.
Reagent：(1+1) nitric acid；SO4 2-, Zn, Mg, Fe, Mn, Al standard reserving solution.
Operating procedure：
Drawing curve：Use SO4 2-Standard reserving solution, makes concentration respectively and is respectively 0.00mg/L, 100.00mg/
The S standard liquid of L, 200.00mg/L, with Zn, Mg, Fe, Mn, Al standard reserving solution, makes concentration respectively and is respectively
0.00mg/L, 10mg/L, 50mg/L, using the intensity of inductive coupling plasma emission spectrograph bioassay standard solution liquid, with
Concentration of standard solution mg/L is abscissa, and corresponding intensity is ordinate drawing curve.
Method accuracy test：Electronic balance weighs the fineness ＜ 0.5mm complex fertilizer that main component is MAP, uses
(1+1) nitric acid dissolving；It is fully transferred in 250mL volumetric flask, then pipettes respective standard solution by table 1 add in volumetric flask, fixed
Hold, filter, obtain test solution.Argon gas makees cooling gas, is S in emission lines wavelength：180.731nm、Zn：206.200nm、Mg：
285.213nm、Fe：238.204nm、Mn：293.306nm、Al：396.152nm, exciting power is 1.1Kw；Pump speed is 1.2r/
Min, cooling gas flow is 19LPM, and nebulizer pressure is 35PSI, under the conditions of secondary air amount is 0LPM, using inductive etc.
Ionomer emission spectrum instrument measures constituent content to be measured, has carried out mark-on reclaims test, result of the test is shown in Table 1.
Table 1
Through the mark-on reclaims test to multiple samples, the rate of recovery, between 98～101%, is controlled and product export in satisfaction
The needs of detection, have high accuracy.
Embodiment 7
Method precision is tested：Electronic balance weighs the fineness ＜ 0.5mm complex fertilizer that main component is MAP, uses
(1+1) nitric acid dissolving；It is fully transferred in 250mL volumetric flask, constant volume obtains solution to be measured；Dilute solution to be measured, obtain sample.
Argon gas makees cooling gas, is S in emission lines wavelength：180.731nm、Zn：206.200nm、Mg：285.213nm、Fe：
238.204nm、Mn：293.306nm、Al：396.152nm, exciting power is 1.1Kw；Pump speed is 1.2r/min, cooling gas flow
For 19LPM, nebulizer pressure is 35PSII, and under the conditions of secondary air amount is 0LPM, drawing curve, using inductive etc.
Ionomer emission spectrum instrument measure 10 groups of samples in concentration of element to be measured, calculate complex fertilizer in constituent content to be measured, extreme difference with
Relative standard deviation density, result of the test is as shown in table 2.
Table 2
From 2,10 groups of result extreme differences of table, S, Mg≤0.20%；Zn, Fe, Al≤0.04%；Mn≤0.01%, relatively
Standard deviation, S, Mg ＜ 2%；Zn, Fe, Al≤5%, Matrix effects are less, and precision is preferable.
Embodiment 8
Electronic balance weighs the fineness ＜ 0.5mm complex fertilizer that main component is MAP, is respectively adopted nitric acid and water
Volume ratio is 2:1、1.5:1、1:1、1:1.5、1:2 salpeter solution dissolving complex fertilizer；It is fully transferred to 250mL volumetric flask
In, constant volume obtains solution to be measured；Dilute solution to be measured, obtain sample.Argon gas makees cooling gas, is S in emission lines wavelength：
180.731nm、Zn：206.200nm、Mg：285.213nm、Fe：238.204nm、Mn：293.306nm、Al：396.152nm, swashs
Sending out power is 1.1Kw；Pump speed is 1.2r/min, and cooling gas flow is 19LPM, and nebulizer pressure is 35PSI, and secondary air amount is
Under the conditions of 0LPM, drawing curve, concentration of element to be measured in sample is measured using inductive coupling plasma emission spectrograph,
Calculate constituent content to be measured in complex fertilizer, result of the test is as shown in table 3.
Table 3
Through contrast test, it is (1～2) using nitric acid and water volume ratio:The salpeter solution dissolving complex fertilizer of (1～2),
Measurement result is substantially better than water soluble method；It is (1～1.5) using nitric acid and water volume ratio:The salpeter solution dissolving of (1～1.5) is multiple
Complex fertilizer material, measures effect more excellent.
Embodiment 9～12
Electronic balance weighs fineness ＜ 0.5mm complex fertilizer, with the dissolving of (1+1) nitric acid；It is fully transferred to 250mL volumetric flask
In, constant volume, filters, obtains solution to be measured.Argon gas makees cooling gas, and emission lines wavelength is S：180.731nm、Zn：206.200nm、
Mg：285.213nm、Fe：238.204nm、Mn：293.306nm、Al：396.152nm, secondary air amount is that 0LPM swashs different
Send out power, pump speed, cooling gas flow, under the conditions of nebulizer pressure, drawing curve, using inductively coupled plasma transmitting
Spectrophotometer concentration of element to be measured, calculates constituent content to be measured in complex fertilizer, and result of the test is shown in Table 4.
Table 4
To sum up, inductive coupling plasma emission spectrograph testing conditions scope is：Exciting power is 1.0～1.2Kw, pump
Speed is 1.0～1.4r/min, and cooling gas flow is 15～25LPM, and nebulizer pressure is 30～40PSI.
The above is only the preferred embodiment of the present invention it is noted that above-mentioned preferred embodiment be not construed as right
The restriction of the present invention, protection scope of the present invention should be defined by claim limited range.For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, some improvements and modifications can also be made, these change
Enter and retouch also to should be regarded as protection scope of the present invention.
Claims (10)
1. in a kind of complex fertilizer the detection method of constituent content it is characterised in that comprising the steps：
1) solution to be measured containing element to be measured is obtained using salpeter solution dissolving complex fertilizer；
2) adopting inductive coupling plasma emission spectrograph to described step 1) solution to be measured that obtains detects, obtains institute
State constituent content to be measured；
Described element to be measured, including one or more in S, Zn, Mg, Fe, Mn, Al.
2. detection method according to claim 1 is it is characterised in that described step 2) it is specially：Criterion work is bent
Line；Dilute solution to be measured, element to be measured in the solution to be measured after dilution is measured using inductive coupling plasma emission spectrograph
Emitted luminescence intensity；The concentration of element to be measured in solution to be measured after must being diluted according to measurement result；Concentration according to element to be measured
Calculate the mass fraction of constituent content to be measured.
3. detection method according to claim 2 it is characterised in that the mass fraction of described constituent content to be measured as the following formula
Calculate：
In formula：
X is the mass percent of element to be measured in complex fertilizer, and numerical value is represented with %；C is the concentration of described element to be measured, unit
For mg/L；V is the volume of the solution to be measured after described dilution, and unit is mL；M is complex fertilizer quality, and unit is g.
4. detection method according to claim 1 is it is characterised in that described complex fertilizer phosphoric acid one ammonium and/or phosphoric acid
Two ammoniums.
5. detection method according to claim 1 it is characterised in that in described salpeter solution nitric acid and the volume ratio of water be
(1～2):(1～2).
6. detection method according to claim 1 is it is characterised in that described inductive coupling plasma emission spectrograph is examined
Survey condition exciting power is 1.0～1.2Kw.
7. detection method according to claim 1 is it is characterised in that described inductive coupling plasma emission spectrograph is examined
Survey condition pump speed is 1.0～1.4r/min.
8. detection method according to claim 1 is it is characterised in that described inductive coupling plasma emission spectrograph is examined
Survey condition cooling gas flow is 15～25LPM.
9. detection method according to claim 1 is it is characterised in that described inductive coupling plasma emission spectrograph is examined
Survey condition nebulizer pressure is 30～40PSI.
10. detection method according to claim 1 is it is characterised in that described inductive coupling plasma emission spectrograph
Testing conditions emission lines wavelength is S：180.731nm、Zn：206.200nm、Mg：285.213nm、Fe：238.204nm、Mn：
293.306nm、Al：396.152nm.
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