CN108680563A - A kind of solid organic fertilizer element silicon detection method and application - Google Patents
A kind of solid organic fertilizer element silicon detection method and application Download PDFInfo
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- CN108680563A CN108680563A CN201810467378.0A CN201810467378A CN108680563A CN 108680563 A CN108680563 A CN 108680563A CN 201810467378 A CN201810467378 A CN 201810467378A CN 108680563 A CN108680563 A CN 108680563A
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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
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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
- G01N1/38—Diluting, dispersing or mixing samples
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/3103—Atomic absorption analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
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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
- G01N2001/2866—Grinding or homogeneising
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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
- G01N1/38—Diluting, dispersing or mixing samples
- G01N2001/386—Other diluting or mixing processes
Abstract
A kind of solid organic fertilizer element silicon detection method of present invention offer and application, solid organic fertilizer are sampled, samples taken after drying, grinding, obtains the first pretreatment sample to be tested successively；Take the first pretreatment sample to be tested that hydrofluoric acid dissolution acidification is added, obtain sample acidifying solution, high temperature deionized water is added to dilute the sample acidifying solution, so that the be dissolved in the sample acidifying solution first pretreatment sample to be tested is adequately ionized, obtains the second pretreatment sample to be tested；Sample is detected using inductively-coupled plasma spectrometer, icp ms or absorption flame photometry instrument；The beneficial effects of the present invention are clearing up, step is simple, and the detection of element silicon can be completed in the short time；It avoids generating a large amount of acid mists in operation, reduces pollution；Compensate for the blank that element silicon in the prior art quickly adheres to detection.
Description
Technical field
The invention belongs to fertilizer detection fields, and in particular to a kind of solid organic fertilizer element silicon detection method and application.
Background technology
For organic fertilizer because its nutrient is comprehensive, fertilizer efficiency is lasting, has good improvement result to soil, universal by people in recent years
Pay attention to and extensive use, element silicon play important work as one of the trace element needed for plant growth, to the growth of plant
With, therefore the element silicon detection in organic fertilizer is particularly significant, and in current organic chemical fertilizer detection method, no matter it is fortunately tradition
National Standard Method or novel ICP detection methods all not to element silicon fast and effectively detection method.
Invention content
To overcome above-mentioned technological deficiency, a kind of solid organic fertilizer element silicon detection method of present invention offer and application.
Specific technical solution is as follows：
A kind of solid organic fertilizer element silicon detection method, the difference is that, the solid organic fertilizer Element detection side
Method includes the following steps：
A：Solid organic fertilizer is sampled, after drying, grinding, it is to be measured to obtain the first pretreatment successively for samples taken
Sample；
B：It takes the first pretreatment sample to be tested described in step A that hydrofluoric acid dissolution acidification is added, obtains sample acidifying solution, be added
75 DEG C~100 DEG C deionized waters dilute the sample acidifying solution, make be dissolved in the sample acidifying solution described first pre-
Processing sample to be tested is adequately ionized, and obtains the second pretreatment sample to be tested；
C:The second pretreatment sample to be tested described in step B is taken, extension rate is arranged according to the concentration for being actually subjected to detection elements,
It is carried out using inductively coupled plasma spectrometry or icp ms or absorption flame photometry instrument
Detection；
The step B is plastics with the C instruments directly contacted in operation with sample and hydrofluoric acid, the step
Grinding is using iron in A.
In above-mentioned technical proposal, the drying temperature of samples taken is 70 DEG C~100 DEG C in the step A, drying time 7
Hour~12 hours.
In above-mentioned technical proposal, samples taken is by grinding in step A, if particle diameter is more than 4mm, by pellet through sieves,
It is 2-4mm to make its diameter.
In above-mentioned technical proposal, the mass concentration of hydrofluoric acid is 49% in step B, the addition volume of hydrofluoric acid and takes the
The mass figures ratio of one pretreatment sample to be tested is (2.5~25) ml:75 DEG C~100 DEG C deionized waters are added by the acid in 1g
After changing liquid dilution, the second pretreatment sample to be tested volume and the volume ratio of the acidifying solution are (100~15):1.
In above-mentioned technical proposal, the second pretreatment sample to be tested passes through inductively coupled plasma spectrometry in the step C
Or after inductivity coupled plasma mass spectrometry or absorption flame photometry detection, with standard concentration curve by comparing, i.e.,
Solid organic fertilizer silicon content can be obtained.
The application of above-mentioned solid organic fertilizer element silicon detection method, the difference is that, the solid organic fertilizer element
The mass percent of its organic matter of the solid organic fertilizer sample of detection method test is 1%~5%.
The beneficial effects of the present invention are the beneficial effects of the present invention are (1) resolution step it is simple, single treatment sample
Afterwards, the detection of element silicon can be completed in the short time；(2) it avoids generating a large amount of acid mists in operation, reduces laboratory pollution；(3) more
The blank that element silicon in the prior art quickly detects is mended.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to specific embodiment to this
Invention is described in further detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and do not have to
It is of the invention in limiting.
Hydrofluoric acid is added after the silicon-containing material separation in sample a large amount of high temperature deionized waters and promotes it quickly and almost complete
Full ionization, upper machine testing, wherein inductively-coupled plasma spectrometer after so that detected element is fully converted into ionic state
(ICP-OES) it is according to each atom under the excitation of heat, the Elements Atom to be measured in excitation state is launched when returning to ground state
Characteristic electromagnetic radiation, it is qualitative and fixed to be carried out to the element by the judgement of wavelength and intensity to this characteristic spectral line
Amount analysis；Absorption flame photometry instrument (AA) be when the light of wavelength appropriate is by steam containing ground state atom,
Ground state atom can absorb the light of certain wavelength and be excited to excitation state from ground state, to generate absorption spectrum；Inductance coupling
Close plasma mass spectrograph (ICP-MS) according to mass/charge than it is different separate successively, finally examined by ion detector
It surveys, the signal of generation is detected after amplification by signal measuring system.
The volume of liquid volume and the acidifying solution after 75 DEG C~100 DEG C deionized waters dilute the acidifying solution is added
Than for (100~15):1, it is because organic matter is mostly weak electrolyte, there is invertibity, high temperature to accelerate sample ionization for ionization
Speed selects this ratio to be diluted, it is ensured that after promoting ionization using high temperature, its ionic condition is still kept steady after cooling
It is fixed, reversible reaction will not occur, and then influence the accuracy of test.
In operating process, whole process avoids contacting with glass apparatus, can be to avoid introducing silicon impurities.
To verify the accuracy of test method of the present invention, select organic fertilizer known to four kinds of silicon contents as test specimens
This.
Embodiment one：
The Chinese medicine residue organic fertilizer that quality of organic matter percentage is 3%, silicon content 25.1330ppm
1, Chinese medicine residue organic fertilizer is dried：
Sample 10-25g is taken, is placed in 90 DEG C of baking ovens 9-10 hours, evaporates all moisture, another its is completely dried.
2, it grinds and claims sample：
(1) after sample is completely dried, ground manually using iron mortar, make particle in 2-4mm sizes.
(2) the sample 1g ground is weighed using a ten thousandth balance.
3, the preparation of ionic liquid
(1) 1g samples are poured onto in 100ml plastic conical bottles, add the HF solution of 25ml, shake up.
(2) (100 DEG C) deionized water will be boiled, 500ml plastics volumetric flasks are added, shakes up simultaneously constant volume 2 hours.
4, it detects
The sample that 10ml has dissolved is drawn using liquid-transfering gun, will be started using ICP-OES preheating ignitings, setting dilution times
Number is 1, carries out machine testing, is detected using 5110 models of Agilent ICP-OES, the content for obtaining silicon through 1 minute.
Embodiment two：
The Chinese medicine residue organic fertilizer element silicon that quality of organic matter percentage is 1% detects, and silicon content is
24.8867ppm：
1, Chinese medicine residue organic fertilizer is dried：
Sample 10-25g is taken, is placed in 80 DEG C of baking ovens 9-12 hours, evaporates all moisture, another its is completely dried.
2, it grinds and claims sample：
(1) after sample is completely dried, ground manually using iron mortar, make particle in 2-4mm sizes.
(2) the sample 1g ground is weighed using a ten thousandth balance.
3, the preparation of ionic liquid
(1) 1g samples are poured onto 50ml plastic conical bottles, the HF solution of 5ml.(2), by 80 DEG C of deionized water, it is added
250ml plastics volumetric flasks shake up simultaneously constant volume 2 hours.
4, it detects
The sample that 10ml has dissolved is drawn using liquid-transfering gun, will be started using AA preheating ignitings, setting extension rate is
1, machine testing is carried out, is detected using 5110 models of Agilent ICP-OES, silicon content was obtained through 1 minute.
Embodiment three：
The cow dung organic fertilizer organic fertilizer Element detection that quality of organic matter percentage is 4%, silicon content are
22.4225ppm：
Concrete operation step is as follows：
1, cow dung organic fertilizer is dried：
Sample 10-25g is taken, is placed in 90 DEG C of baking ovens 8-9 hours, evaporates all moisture, another its is completely dried.
2, it grinds and claims sample：
(1) after sample is completely dried, ground manually using iron mortar, make particle in 2-4mm sizes.
(2) the sample 1g ground is weighed using a ten thousandth balance.
3, the preparation of ionic liquid
(1) 1g samples are poured onto in 50ml plastic conical bottles, add the HF solution of 15ml, shake up.
(2) by 75 DEG C of deionized water, 1L plastics volumetric flasks are added, shake up simultaneously constant volume 2 hours.4, it detects
The sample that 10ml has dissolved is drawn using liquid-transfering gun, will be started using ICP-MS preheating ignitings, setting dilution times
Number is 1, carries out machine testing, is detected using 5110 models of Agilent ICP-OES, full constituent content was obtained through 1 minute.
Example IV：
The cow dung organic fertilizer Element detection that quality of organic matter percentage is 2%, silicon content 22.1758ppm.
Concrete operation step is as follows：
1, cow dung organic fertilizer is dried：
Sample 10-25g is taken, is placed in 90 DEG C of baking ovens 7~8 hours, evaporates all moisture, another its is completely dried.
2, it grinds and claims sample：
(1) after sample is completely dried, ground manually using iron mortar, make particle in 2-4mm sizes.
(2) the sample 1g ground is weighed using a ten thousandth balance.
3, the preparation of ionic liquid
(1) 1g samples are poured onto in 100ml plastic conical bottles, add the HF solution of 20ml, shake up.
(2) by 90 DEG C of deionized water, 500ml plastics volumetric flasks are added, shake up simultaneously constant volume 2 hours.
4, it detects
The sample that 10ml has dissolved is drawn using liquid-transfering gun, will be started using ICP-OES preheating ignitings, setting dilution times
Number is 1, carries out machine testing, is detected using 5110 models of Agilent ICP-OES, silicon content was obtained through 1 minute.
1 embodiment test result testing result of table
Test result of the present invention is consistent with the silicon content in organic chemical fertilizer it can be seen from upper table test result, fills
It defends oneself and the accuracy of this test method is illustrated, in addition digestion procedure of the present invention is simple, and detection is quick, avoids laboratory from generating a large amount of
Acid mist reduces laboratory pollution.
Claims (6)
1. a kind of solid organic fertilizer element silicon detection method, which is characterized in that the solid organic fertilizer method for detecting element includes
Following steps：
A：Solid organic fertilizer is sampled, samples taken after drying, grinding, obtains the first pretreatment and wait for test sample successively
Product；
B：It takes the first pretreatment sample to be tested described in step A that hydrofluoric acid dissolution acidification is added, obtains sample acidifying solution, be added 75 DEG C
~ 100 DEG C of deionized waters dilute the sample acidifying solution, make to be dissolved in first pretreatment in the sample acidifying solution and wait for
Sample is adequately ionized, and obtains the second pretreatment sample to be tested；
C:The second pretreatment sample to be tested described in step B is taken, extension rate is arranged according to the concentration for being actually subjected to detection elements, is utilized
Inductively coupled plasma spectrometry or inductivity coupled plasma mass spectrometry or absorption flame photometry are detected；
The instrument that the step B and C is directly contacted with sample and hydrofluoric acid in operation is plastic material, the step
A iron or aluminium oxide mortar are ground.
2. a kind of solid organic fertilizer element silicon detection method according to claim 1, which is characterized in that institute in the step A
It is 70 DEG C ~ 100 DEG C to take the drying temperature of sample, and drying time is 7 hours ~ 12 hours.
3. a kind of solid organic fertilizer element silicon detection method according to claim 1, which is characterized in that sampled in step A
For product by pellet through sieves after grinding, it is 2-4mm to make its diameter.
4. a kind of solid organic fertilizer element silicon detection method according to claim 1, which is characterized in that hydrofluoric acid in step B
Mass fraction be 49%, the addition volume of hydrofluoric acid is with the mass figures ratio of the first pretreatment sample to be tested is taken（2.5~
25）ml:75 DEG C ~ 100 DEG C deionized waters are added by after acidifying solution dilution in 1g, and described second pre-processes sample to be tested volume
Volume ratio with the acidifying solution is（100~15）:1.
5. a kind of solid organic fertilizer element silicon detection method according to claim 1, which is characterized in that in the step C
Two pretreatment samples to be tested are by inductively coupled plasma spectrometry or inductivity coupled plasma mass spectrometry or atomic absorption spectrophotometry
After photometric analyzer detection, with standard concentration curve by comparing, you can obtain solid organic fertilizer silicon content.
6. a kind of claim 1 ~ 5 application of solid organic fertilizer element silicon detection method, which is characterized in that the solid has
The mass percent of its organic matter of the solid organic fertilizer sample of machine fertilizer method for detecting element test is 1% ~ 5%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110133052A (en) * | 2019-06-14 | 2019-08-16 | 湖北科艾乐检测科技有限公司 | A kind of soil fertility detection method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110133052A (en) * | 2019-06-14 | 2019-08-16 | 湖北科艾乐检测科技有限公司 | A kind of soil fertility detection method |
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