CN106596536B - Soil Nitrogen stage division under a kind of natural particle size - Google Patents
Soil Nitrogen stage division under a kind of natural particle size Download PDFInfo
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- CN106596536B CN106596536B CN201611160091.0A CN201611160091A CN106596536B CN 106596536 B CN106596536 B CN 106596536B CN 201611160091 A CN201611160091 A CN 201611160091A CN 106596536 B CN106596536 B CN 106596536B
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- nitrogen
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- acidolysis
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 265
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 132
- 239000002689 soil Substances 0.000 title claims abstract description 59
- 239000002245 particle Substances 0.000 title claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000000605 extraction Methods 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005342 ion exchange Methods 0.000 claims abstract description 24
- 239000000243 solution Substances 0.000 claims abstract description 23
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000000126 substance Substances 0.000 claims abstract description 13
- 102000012286 Chitinases Human genes 0.000 claims abstract description 12
- 108010022172 Chitinases Proteins 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000001103 potassium chloride Substances 0.000 claims abstract description 8
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 7
- 239000008351 acetate buffer Substances 0.000 claims abstract description 7
- YBCVMFKXIKNREZ-UHFFFAOYSA-N acoh acetic acid Chemical compound CC(O)=O.CC(O)=O YBCVMFKXIKNREZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229910002551 Fe-Mn Inorganic materials 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000006228 supernatant Substances 0.000 claims description 24
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 17
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- 125000001477 organic nitrogen group Chemical group 0.000 claims description 15
- 229910002651 NO3 Inorganic materials 0.000 claims description 14
- 238000002798 spectrophotometry method Methods 0.000 claims description 13
- MMDJDBSEMBIJBB-UHFFFAOYSA-N [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] Chemical compound [O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[NH6+3] MMDJDBSEMBIJBB-UHFFFAOYSA-N 0.000 claims description 12
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 238000004737 colorimetric analysis Methods 0.000 claims description 10
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 6
- 238000005259 measurement Methods 0.000 claims description 6
- 150000001413 amino acids Chemical class 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 150000002337 glycosamines Chemical class 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 239000012528 membrane Substances 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000000706 filtrate Substances 0.000 claims 1
- FEMOMIGRRWSMCU-UHFFFAOYSA-N ninhydrin Chemical compound C1=CC=C2C(=O)C(O)(O)C(=O)C2=C1 FEMOMIGRRWSMCU-UHFFFAOYSA-N 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 description 10
- 238000004172 nitrogen cycle Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- JVMRPSJZNHXORP-UHFFFAOYSA-N ON=O.ON=O.ON=O.N Chemical compound ON=O.ON=O.ON=O.N JVMRPSJZNHXORP-UHFFFAOYSA-N 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000003864 humus Substances 0.000 description 1
- 150000002469 indenes Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000013139 quantization Methods 0.000 description 1
- 239000007974 sodium acetate buffer Substances 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
Classifications
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
Abstract
The invention discloses Soil Nitrogen stage divisions under a kind of natural particle size, and the specific steps are 1) free state nitrogen FN in pedotheque is extracted using deionized water；2) pedotheque intermediate ion exchange state nitrogen IEN is extracted using potassium chloride (KCl) again；3) carbonate combine state nitrogen CN and Fe-Mn oxide nitrogen IMON in pedotheque is extracted using Acetate-acetate buffer solution and sodium hydroxide NaOH respectively again；4) the acidolysis state nitrogen HN in pedotheque is extracted using hydrochloric acid HCl again；5) residual nitrogen RN finally is measured with alkaline chitinase resolution-ultraviolet spectrophotometer method.This method refines the classification of nitrogen in soil under natural particle size, be classified it is more scientific and comprehensive, by the selection and sequence of extraction of different chemical extraction agent ensure that classification it is accurate with it is reliable.
Description
Technical field
The present invention relates to Soil Nitrogen classifications, more particularly to a kind of classification side specifically for Soil Nitrogen under natural particle size
Method belongs to Soil Nitrogen classification technique field.
Background technique
Nitrogen is both the driven factor of plant growth indispensable element and pollution of area source and greenhouse effects.Rich in rich in soil
Rich nitrogen substance, be lithosphere, hydrosphere, in atmospheric thermodynamics and biosphere nitrogen important source/remittance.The life of different shape nitrogen in soil
Having differences property of change behavior, is formed and distribution using the occurrence patterns of nitrogen in suitable technique study soil, is accurate understanding
Nitrogen biochemistry circulation and its important prerequisite of Impacts on ecology and environment in the ball ecosystem.
Nitrogen includes organic nitrogen and inorganic nitrogen two parts in soil, wherein based on organic nitrogen.The occurrence patterns master of organic nitrogen
It is divided into Organic residues and humus, the Nomenclature Composition and Structure of Complexes is extremely complex, divides more difficult.Inorganic nitrogen occurrence patterns mainly wrap
Include ammonium nitrogen, nitrate nitrogen, nitrite nitrogen etc..
Traditional measuring method of Soil Nitrogen is research total nitrogen, organic nitrogen and inorganic nitrogen after air-drying and grinding by soil at present, this
Kind method is although simple and convenient, but cannot accurately provide the information of soil nitrogen cycle.Soil particle has special heterogeneity, greatly
Small and structure composition has differences, and bulky grain is difficult to be crushed in Environmental variations, escapes nitrogen and participates in circulation, soil
In really participate in circulation be soluble nitrogen and graininess nitrogen.Traditional measuring method of Soil Nitrogen, which is difficult to distinguish, really to be changed to participation
The nitrogen form of circulation, can not effect of the accurate description Soil Nitrogen occurrence patterns in ground behavior, limit terrestrial ecosystem
The research of middle nitrogen cycle.
Summary of the invention
For existing Soil Nitrogen stage division above shortcomings, it is an object of the invention to propose it is a kind of specifically for
Soil Nitrogen stage division under natural particle size.This method refines the classification of nitrogen in soil under natural particle size, and classification is more
Science and comprehensively, by the selection and sequence of extraction of different chemical extraction agent ensure that classification it is accurate with it is reliable.
The technical scheme of the present invention is realized as follows:
Soil Nitrogen stage division under a kind of natural particle size, it is characterised in that: this method first acquires fresh soil sample sample, so
It is extracted step by step with chemical extraction agent afterwards, i.e., using different chemical reagent to the occurrence patterns of nitrogen in pedotheque under natural particle size
It extracts, the specific steps are as follows:
1) free state nitrogen FN in pedotheque, including free state total nitrogen FTN, soluble total nitrogen are extracted using deionized water
DTN, free state ammonia nitrogen F-NH4 +, free state nitrate nitrogen F-NO3 -, free state particle nitrogen FPN and soluble organic nitrogen DON；
2) pedotheque intermediate ion exchange state nitrogen is extracted using potassium chloride (KCl) again in the pedotheque after step 1) extraction
IEN, including ion-exchange state total nitrogen IETN, ion-exchange state ammonia nitrogen IE-NH4 +, ion-exchange state nitrate nitrogen IE-NO3 -, ion hand over
Change state organic nitrogen IEON；
3) distinguished again using Acetate-acetate buffer solution and sodium hydroxide NaOH in the pedotheque after step 2 extraction
Extract carbonate combine state nitrogen CN and Fe-Mn oxide nitrogen IMON in pedotheque；
4) the acidolysis state nitrogen HN in pedotheque is extracted using hydrochloric acid HCl again in the pedotheque after step 3) extraction,
Including acidolysis total nitrogen HTN, acidolysis ammonium nitrogen AN, acidolysis amino-acid nitrogen AAN, acidolysis amino sugar state nitrogen ASN and acidolysis unknown state
Nitrogen UAN；
5) residual with alkaline chitinase resolution-ultraviolet spectrophotometer method measurement in the pedotheque after step 4) extraction
Stay state nitrogen RN.
Compared with prior art, the invention has the following beneficial effects:
1, the present invention is directed to availability, activity and the nitrogen cycle participation of natural particle size Soil Nitrogen, by Soil Nitrogen preservation shape
State is divided into free state nitrogen, ion-exchange state nitrogen, carbonate combine state nitrogen, Fe-Mn oxide nitrogen, acidolysis state nitrogen and residual nitrogen,
The differentiation and extraction that SOIL ORGANIC NITROGEN and inorganic N forms under natural particle size can be combined help to study and assess comprehensively
Nitrogen form migration, conversion characteristic and its validity in global chemical recycle, to announcement Soil Nitrogen occurrence patterns to terrestrial ecosystem nitrogen
The contribution of element circulation is of great significance.
2, stage division proposed by the present invention be on the basis of referring to traditional measuring method, using separation and Extraction step by step and
Spectrophotometry is finely divided quantization to Soil Nitrogen occurrence patterns, selection and sequence of extraction by different chemical extraction reagents,
Not only the science and accuracy of classification ensure that, but also can be further work of the research Soil Nitrogen occurrence patterns in global chemical recycle
With and prevention and control pollution of area source and greenhouse effects etc. important theoretical foundation and technological means is provided.
3, compared to traditional Nitrogen Determination method, the present invention segments ammonia nitrogen, nitrate nitrogen and organic nitrogen, to natural particle size
The classification of lower Soil Nitrogen is refined, and can be understood under actual environmental conditions, the nitrogen of any combining form is easier to release
It puts, and can further speculate participation and contribution rate of the nitrogen in geochemistry nitrogen cycle in soil.
4, classification process technology path proposed by the present invention is to realize and design soil nitrogen automation point under natural particle size
Grade provides a kind of possibility, has extensive market development prospect and economic benefit.
Detailed description of the invention
Soil Nitrogen is classified process Technology Roadmap under Fig. 1-natural particle size of the present invention.
Specific embodiment
Soil Nitrogen stage division under natural particle size of the present invention first acquires fresh soil sample sample, then uses chemical extraction agent
It extracts, i.e., is extracted using occurrence patterns of the different chemical reagent to nitrogen in pedotheque under natural particle size, specifically step by step
Steps are as follows:
1) free state nitrogen FN in pedotheque, including free state total nitrogen FTN, soluble total nitrogen are extracted using deionized water
DTN, free state ammonia nitrogen F-NH4 +, free state nitrate nitrogen F-NO3 -, free state particle nitrogen FPN and soluble organic nitrogen DON；
2) pedotheque intermediate ion exchange state nitrogen is extracted using potassium chloride (KCl) again in the pedotheque after step 1) extraction
IEN, including ion-exchange state total nitrogen IETN ion-exchange state ammonia nitrogen IE-NH4 +, ion-exchange state nitrate nitrogen IE-NO3 -, ion exchange
State organic nitrogen IEON；
3) Acetate-acetate buffer solution (pH=5) and sodium hydroxide are used again in the pedotheque after step 2 extraction
NaOH extracts carbonate combine state nitrogen CN and Fe-Mn oxide nitrogen IMON in pedotheque respectively；
4) the acidolysis state nitrogen HN in pedotheque is extracted using hydrochloric acid HCl again in the pedotheque after step 3) extraction,
Including acidolysis total nitrogen HTN, acidolysis ammonium nitrogen AN, acidolysis amino-acid nitrogen AAN, acidolysis amino sugar state nitrogen ASN and acidolysis unknown state
Nitrogen UAN；
5) residual with alkaline chitinase resolution-ultraviolet spectrophotometer method measurement in the pedotheque after step 4) extraction
Stay state nitrogen RN.
Invention is further described in detail with reference to the accompanying drawings and detailed description.
Soil Nitrogen classification concrete operations are as follows under natural particle size of the present invention, Technology Roadmap referring also to shown in FIG. 1:
(1) fresh soil sample 6.0-8.0g is weighed, is placed in 100ml centrifuge tube, 50ml deionized water is added, vibrates 2h
(300r, 20-25 DEG C) is centrifuged 8min(3500 rmin), form supernatant A.Aspirate supernatant A 5-10ml is using alkaline mistake
Potassium sulfate oxidation-determined by ultraviolet spectrophotometry free state total nitrogen (FTN)；Remaining supernatant A is filtered with the filter membrane of 0.45um, shape
At liquor B.It draws liquor B 5-10ml and soluble total nitrogen (DTN) is measured using reagent colorimetric method；Draw liquor B 5-
10ml measures free state ammonia nitrogen (F-NH using reagent colorimetric method4 +)；It draws liquor B 5-10ml and uses uv-spectrophotometric
Method measures free state nitrate nitrogen (F-NO3 -)；Free state particle nitrogen (FPN) and soluble organic nitrogen (DON) are then acquired using minusing,
That is FPN=FTN-DTN, DON=DTN-(F-NH4 ++ F-NO3 -);
(2) 50ml 2mol L is added to the soil residue after above-mentioned steps (1) centrifugation-1Potassium chloride (KCl) solution, oscillation
3h(300r, 20-25 DEG C), it is centrifuged 8min(3500 rmin), form supernatant B.Aspirate supernatant B 10-15ml uses alkali
Property peroxide potassium sulfate-ultraviolet spectrophotometry measurement ion-exchange state total nitrogen (IETN)；Aspirate supernatant B 10-15ml is used
Reagent colorimetric method measures ion-exchange state ammonia nitrogen (IE-NH4 +)；Aspirate supernatant B 10-15ml uses uv-spectrophotometric
Method measures ion-exchange state nitrate nitrogen (IE-NO3 -)；Ion-exchange state organic nitrogen (IEON) is then acquired using minusing, i.e. and IEON=
IETN-(IE-NH4 ++ IE-NO3 -)；
(3) after the soil residue after extracting KCl is cleaned twice with saturation NaCl solution, 50ml 0.5mol L is added-1Vinegar
Sour sodium-acetate buffer solution (pH=5), vibrate 6h(300r, 20-25 DEG C), be centrifuged 8min(3500 rmin), formed supernatant C,
With 0.5mol L-1NaOH adjusts supernatant C to pH=6.5, is then settled to 100ml, draws 20-30ml constant volume liquid and use with alkalinity
Peroxide potassium sulfate-ultraviolet spectrophotometry measures carbonate combine state nitrogen (CN)；
(4) it after the soil residue after Acetate-acetate buffer solution extracts is cleaned twice with saturation NaCl solution, is added
50ml 0.1mol L-1NaOH, vibrate 17h(300r, 20-25 DEG C), be centrifuged 10min(3500 rmin), formed supernatant D.
Aspirate supernatant D 10-15ml measures Fe-Mn oxide nitrogen using alkaline chitinase oxidation-ultraviolet spectrophotometer method
(IMON)；
(5) after cleaning the soil residue after step (4) extraction twice with saturation NaCl solution, 25ml 6mol L is added-1
Hydrochloric acid solution vibrate 3h(300r, 20-25 DEG C) after, be transferred in 50ml high temperature resistant colorimetric cylinder, in 120 DEG C of pressure cookers sealing acid
12-24h is solved, is transferred to after being cooled to room temperature in 100ml centrifuge tube, 10min(3500 rmin is centrifuged) obtain supernatant E, supernatant
Liquid E is poured into beaker, with 1mol L-1NaOH is adjusted to pH=6.5, and after being settled to 100ml, and filtering forms prepare liquid E.It draws
Prepare liquid E 10-15ml is using alkaline chitinase oxidation-ultraviolet spectrophotometer method measurement acidolysis total nitrogen (HTN)；Draw to
Liquid E 10-15ml is surveyed using reagent colorimetric method measurement acidolysis ammonium nitrogen (AN)；It draws prepare liquid E 10-15ml and uses indenes three
Ketone colorimetric method for determining acidolysis amino-acid nitrogen (AAN)；It draws prepare liquid E 10-15ml and acidolysis is measured using Elson-Morgen method
Amino sugar state nitrogen (ASN)；Acidolysis unknown state nitrogen (UAN) is then acquired using minusing, it may be assumed that UAN=HTN- (AN+AAN+ASN)；
(6) after cleaning the soil residue after acidolysis twice with saturation NaCl solution, 4% alkaline chitinase of 25ml is added
Solution, vibrates 3h(300r, and 20-25 DEG C), it is transferred to disappear in 50ml high temperature resistant colorimetric cylinder and boils 1h(120 DEG C) and, it is settled to after cooling
50ml uses determined by ultraviolet spectrophotometry residual nitrogen (RN) after filtering.
The present invention is to utilize different chemical extraction agents according to the difference between Soil Nitrogen occurrence patterns structure composite degree and activity
Between Soil Nitrogen occurrence patterns multiplicity and activity stepwise dissociation and extraction, thus reach separation Soil Nitrogen occurrence patterns mesh
's.Thus the present invention has strict requirements to the selection of chemical extraction agent and sequence.Firstly, chemical extraction agent cannot influence soil
The interstructural multiplicity of the original nitrogen occurrence patterns of earth and activity can not excite original interstructural conversion of nitrogen occurrence patterns；Its
Secondary, extraction sequence must convert step by step according to weak digestion agent to strong digestion agent, i.e. chemical extraction ability gradually increases, and otherwise having can
It can cause high activity in soil, the loss of low multiplicity Soil Nitrogen occurrence patterns and low-activity, high multiplicity Soil Nitrogen preservation shape
The increase of state causes Soil Nitrogen occurrence patterns to be classified deviation, influences Soil Nitrogen grading effect.
Finally, it should be noted that examples detailed above of the invention is only example to illustrate the invention, and it is not
It is the restriction to embodiments of the present invention.It is right although applicant describes the invention in detail referring to preferred embodiment
For those of ordinary skill in the art, can also make on the basis of the above description other it is various forms of variation and
It changes.Here all embodiments can not be exhaustive.All belong to that technical solution of the present invention amplifies out aobvious and
The variation or variation being clear to are still in the scope of protection of the present invention.
Claims (1)
1. Soil Nitrogen stage division under a kind of natural particle size, it is characterised in that: this method first acquires fresh soil sample sample, then
Extracted step by step with chemical extraction agent, i.e., using different chemical reagent to the occurrence patterns of nitrogen in pedotheque under natural particle size into
Row extracts, the specific steps are as follows:
1) free state nitrogen FN in pedotheque, including free state total nitrogen FTN, soluble total nitrogen DTN, trip are extracted using deionized water
Amorph ammonia nitrogen F-NH4 +, free state nitrate nitrogen F-NO3 -, free state particle nitrogen FPN and soluble organic nitrogen DON；
2) pedotheque intermediate ion exchange state nitrogen IEN is extracted using potassium chloride (KCl) again in the pedotheque after step 1) extraction,
Including ion-exchange state total nitrogen IETN, ion-exchange state ammonia nitrogen IE-NH4 +, ion-exchange state nitrate nitrogen IE-NO3 -, ion-exchange state
Organic nitrogen IEON；
3) it is extracted respectively using Acetate-acetate buffer solution and sodium hydroxide NaOH again in the pedotheque after step 2 extraction
Carbonate combine state nitrogen CN and Fe-Mn oxide nitrogen IMON in pedotheque；
4) the acidolysis state nitrogen HN in pedotheque is extracted using hydrochloric acid HCl again in the pedotheque after step 3) extraction, including
Acidolysis total nitrogen HTN, acidolysis ammonium nitrogen AN, acidolysis amino-acid nitrogen AAN, acidolysis amino sugar state nitrogen ASN and acidolysis unknown state nitrogen
UAN；
5) residual is measured with alkaline chitinase resolution-ultraviolet spectrophotometer method in the pedotheque after step 4) extraction
Nitrogen RN；
Each step specifically,
(1) fresh soil sample 6.0-8.0g is weighed as pedotheque, is placed in 100ml centrifuge tube, and 50ml deionized water is added,
2h is vibrated at 300r, 20-25 DEG C, 8min is then centrifuged at 3500 r/min, forms supernatant A；Aspirate supernatant A 5-
10ml, using alkaline chitinase oxidation-determined by ultraviolet spectrophotometry free state total nitrogen FTN；Remaining supernatant A 0.45um
Filter membrane filter, formed liquor B；Three parts of liquor B, every part of 5-10ml are drawn respectively, and a copy of it uses reagent colorimetric method
Measure soluble total nitrogen DTN；Another measures free state ammonia nitrogen F-NH using reagent colorimetric method4 +；Third part is using ultraviolet
Spectrophotometry measures free state nitrate nitrogen F-NO3 -；Free state particle nitrogen FPN and soluble organic nitrogen DON are then asked using minusing
, i.e. FPN=FTN-DTN, DON=DTN-(F-NH4 ++ F-NO3 -)；
(2) 50ml 2mol L is added to the soil residue after above-mentioned steps (1) centrifugation-1Potassium chloride (KCl) solution, 300r,
3h is vibrated at 20-25 DEG C, 8min is then centrifuged at 3500 r/min, forms supernatant B；Tri- parts of Aspirate supernatant B respectively,
Every part of 10-15ml, a copy of it use alkaline chitinase oxidation-determined by ultraviolet spectrophotometry ion-exchange state total nitrogen
IETN；Another measures ion-exchange state ammonia nitrogen IE-NH using reagent colorimetric method4 +；Third part uses uv-spectrophotometric
Method measures ion-exchange state nitrate nitrogen IE-NO3 -；Ion-exchange state organic nitrogen IEON is then acquired using minusing, i.e. IEON=IETN-
(IE-NH4 ++ IE-NO3 -)；
(3) after cleaning the soil residue after step (2) KCl extraction twice with saturation NaCl solution, 50ml 0.5mol L is added-1And the Acetate-acetate buffer solution of pH=5,6h is vibrated at 300r, 20-25 DEG C, is then centrifuged 8min at 3500 r/min,
Supernatant C is formed, with 0.5mol L-1NaOH is settled to 100ml after adjusting supernatant C to pH=6.5, draws 20-30ml constant volume
Liquid alkaline chitinase oxidation-determined by ultraviolet spectrophotometry carbonate combine state nitrogen CN；
(4) after the soil residue after the extraction of step (3) Acetate-acetate buffer solution is cleaned twice with saturation NaCl solution, add
Enter 50ml 0.1mol L-1NaOH vibrates 17h at 300r, 20-25 DEG C, and 10min, shape are then centrifuged at 3500 r/min
At supernatant D；Aspirate supernatant D 10-15ml measures ferrimanganic oxygen using alkaline chitinase oxidation-ultraviolet spectrophotometer method
Change state nitrogen IMON；
(5) after cleaning the soil residue after step (4) extraction twice with saturation NaCl solution, 25ml 6mol L is added-1Salt
Acid solution is transferred in 50ml high temperature resistant colorimetric cylinder after vibrating 3h at 300r, 20-25 DEG C, in 120 DEG C of pressure cooker sealing acid
12-24h is solved, is transferred in 100ml centrifuge tube after cooling, is centrifuged 10min at 3500 r/min, obtains supernatant E；Supernatant E
It pours into beaker, with 1mol L-1NaOH is adjusted to pH=6.5, and after being settled to 100ml, and filtering forms prepare liquid E；It draws to be measured
Tetra- parts of liquid E, every part of 10-15ml, a copy of it is total using alkaline chitinase oxidation-ultraviolet spectrophotometer method measurement acidolysis
Nitrogen HTN；Second part measures acidolysis ammonium nitrogen AN using reagent colorimetric method；Third part measures acidolysis using ninhydrin colorimetry
Amino-acid nitrogen AAN；4th part measures acidolysis amino sugar state nitrogen ASN using Elson-Morgen method；Acidolysis unknown state nitrogen UAN is then
It is acquired using minusing, it may be assumed that UAN=HTN- (AN+AAN+ASN)；
(6) after cleaning the soil residue after step (5) acidolysis twice with saturation NaCl solution, the alkaline over cure of 25ml 4% is added
Sour potassium solution vibrates 3h at 300r, 20-25 DEG C, is then transferred to disappear in 50ml high temperature resistant colorimetric cylinder in 120 DEG C and boils 1h, cold
But to 50ml is settled to after room temperature, filtrate after the filtering of constant volume liquid is used into determined by ultraviolet spectrophotometry residual nitrogen RN.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611160091.0A CN106596536B (en) | 2016-12-15 | 2016-12-15 | Soil Nitrogen stage division under a kind of natural particle size |
Applications Claiming Priority (1)
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| CN111380730B (en) * | 2020-03-23 | 2020-11-20 | 西安科技大学 | Method for gradually leaching trace elements of stone coal and analyzing occurrence state |
| CN112082965A (en) * | 2020-09-18 | 2020-12-15 | 武汉工程大学 | Method for determining occurrence state of residual ammonium salt in weathered crust elution-deposited rare earth ore |
| CN113406031A (en) * | 2021-06-16 | 2021-09-17 | 南京工业大学 | Quantitative calculation method for nitrogen migration and conversion in pipeline sediment-water system |
| CN113406027B (en) * | 2021-06-16 | 2022-06-14 | 南京工业大学 | Quantitative calculation method for phosphorus migration and conversion in pipeline sediment-water system |
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