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CN110208298A - The method that active component characterizes its microstructure in separation soil microaggregate in situ - Google Patents

The method that active component characterizes its microstructure in separation soil microaggregate in situ Download PDF

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Publication number
CN110208298A
CN110208298A CN201910476008.8A CN201910476008A CN110208298A CN 110208298 A CN110208298 A CN 110208298A CN 201910476008 A CN201910476008 A CN 201910476008A CN 110208298 A CN110208298 A CN 110208298A
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soil
situ
microstructure
component
spectrogram
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CN110208298B (en
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杨建军
刘瑾
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Institute of Environment and Sustainable Development in Agriculturem of CAAS
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Institute of Environment and Sustainable Development in Agriculturem of CAAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/02Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material
    • G01N23/06Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption
    • G01N23/083Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by transmitting the radiation through the material and measuring the absorption the radiation being X-rays
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/03Investigating materials by wave or particle radiation by transmission
    • G01N2223/04Investigating materials by wave or particle radiation by transmission and measuring absorption
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/616Specific applications or type of materials earth materials

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  • Toxicology (AREA)
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  • Life Sciences & Earth Sciences (AREA)
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  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)
  • Soil Conditioners And Soil-Stabilizing Materials (AREA)

Abstract

The invention discloses the present invention to provide a kind of method for being combined using synchrotron radiation scanning transmission microscopy and mathematical statistics method and realizing its microstructure of active component and characterization in separation soil microaggregate in situ, includes the following steps: air-dried soil grind into powder;Suspension is prepared into air-dry;Using synchrotron radiation scanning transmission technology acquisition carbon, aluminium and silicon K while and iron L while X-ray near side (ns) absorbing structure spectrum and storehouse image;It is combined after the storehouse image of each element is carried out image and energy correction, then multielement principle component and cluster analysis is carried out using the polynary spectrogram of overlapping, the cluster map for representing carbon, iron and aluminium silicon difference element composition, content and structure of is obtained, realizes in separation soil agreegate in situ the organic matter fraction based on carbon, the ferriferous oxide component based on iron and the clay mineral component based on aluminium silicon and the microstructure features of these typical activity components respectively.

Description

The method that active component characterizes its microstructure in separation soil microaggregate in situ
Technical field
The present invention relates to the methods that active component in a kind of separation soil microaggregate in situ characterizes its microstructure, especially It is a kind of using in synchrotron radiation scanning transmission microscopy and mathematical statistics method combination realization separation soil microaggregate in situ The method that active component characterizes its microstructure.
Background technique
Soil nutrient test controls most important for China's agricultural Green Development with heavy metal pollution.Soil microaggregate It is the basic component units of soil, nutrient and pollutant, which enter after soil system, mainly to be handed over the active component in soil agreegate Interaction, and then influence the form of soil nutrient and pollutant, be distributed, return and become and biological effectiveness.However soil activation component Multiplicity, wherein not only soil constitution is unevenly distributed using organic matter, ferriferous oxide and clay mineral as representative, but also microstructure Difference is obvious, strongly limits the understanding to soil nutrient and pollutant distribution feature, micromorphology and biological effectiveness, in turn Effectively soil nutrient and pollutant can not effectively be managed, limit the Green Development of agricultural.Therefore, effectively to soil group It is to go deep into understanding soil agreegate and nutrient and pollutant effect machine that dimeric active component, which separates in situ and carries out Characterization for Microstructure, The premise of system.Chemical leaching test is mainly utilized currently for active component characterization in soil agreegate, such as utilizes acid-base solution Agron is extracted, extracts soil ferriferous oxide etc. using one sodium citrate of sodium dithionite, one sodium bicarbonate method, but change It learns extraction process and there is destructiveness, and the poor selectivity of extraction process to soil activation component.To overcome chemical leaching test to exist Characterize soil agreegate limitation, have researcher also report using synchrotron radiation infrared microscopy imaging technique and its with scanning The technical tie-ups such as Electronic Speculum, nanoparticle probe are specific as follows using the method for characterizing soil agreegate:
Patent 1(application number: CN201610851124.X) report a kind of utilization synchrotron radiation infrared microscopy imaging technique original position The method for studying organic carbon and mineral in soil agreegate, available organic carbon main functional group and mineral distribution characteristics.
Patent 2(application number: 201710896024.3) report it is a kind of using scanning electron microscope, synchrotron radiation infrared microscopy at As technology and nanometer secondary ion probe technique characterize organic in soil agreegate and Inorganic functional groups point on submicron-scale Cloth;The destructiveness for improving conventional soil microaggregate research method is big, complicated cumbersome, poor synchronization, visual poor, ruler in situ Spend the problems such as uncoordinated.
The in-situ study method of the above-mentioned soil agreegate reported out, but operated from characterization technique accuracy, method Property and active component structural information it is comprehensive etc. from the point of view of, lacked in above-mentioned or similar to the above report there is also some It falls into:
(1) spatial resolution of synchrotron radiation infrared microscopy imaging technique is other in the micron-scale, can not ruler in mulching soil aggregate It is very little in nanoscale solid phase active component, therefore the spatial resolution of characterization method needs to be further increased.
(2) though by combining scanning electron microscope, nanoparticle probe technique that can provide the spatial resolution of nanometer, thus more Synchrotron radiation infrared microscopy imaging technique is mended in the deficiency of spatial resolution, but scanning electron microscope and nanoparticle probe technique Electron beam and ion beam will cause sample damage, especially destruction of organic material structure, cause synchrotron radiation infrared microscopy that skill is imaged Art can not in-situ characterization soil agreegate, the structural information accuracy of acquisition leaves a question open;It is complicated for operation during being combined simultaneously, it is time-consuming Arduously.
(3) scanning electron microscope, nanoparticle probe and synchrotron radiation infrared microscopy imaging technique can not be in soil constitutions Constituent content carries out quantitatively characterizing, therefore assesses for each active component content in examination soil microaggregate.
Summary of the invention
The present invention overcomes deficiency in the prior art, provides and united using synchrotron radiation scanning transmission microscopy and mathematics The combination of meter method is realized separation soil agreegate multiple active components in situ on micron metrical scale, and is penetrated using the X of object element Line near edge structure composes the microstructure of (XANES) characterization active component typical element, is subsequent further investigation soil microaggregate Important foundation is established with nutrient/pollutant mechanism of action.
The purpose of the present invention is achieved by following technical proposals, is included the following steps:
(1) preparation of soil microaggregate: soil clay particle component is collected using sedimentation, sample is ground into after freeze-drying Powder.
(2) synchrotron radiation scanning transmission microscopy (STXM) is tested: soil clay particle component being spent ionized water and is prepared as hanging Turbid pipettes part suspension and drips on silicon nitride window, is moved into measurement chamber after dry, is passed through helium and keeps 1/6 atmospheric pressure, so Afterwards using transmission mode acquisition soil typical element carbon (C), aluminium (Al), the K ABSORPTION EDGE of silicon (Si) and iron (Fe) L ABSORPTION EDGE X The storehouse spectrogram of ray near side (ns) absorbing structure (XANES) spectrum;
(3) it separates soil agreegate activity multicomponent in situ by polygon STXM data processing and characterizes its microstructure features: will The storehouse spectrogram of soil typical element C/Fe/Al/Si carries out spectrogram correction, and the compound spectrogram of C-Fe-Al-Si is generated after overlapping, Then different clusters are obtained using multielement principal component analysis and clustering, the pattern of every kind of cluster indicates there is specific C/ The soil agreegate of Fe/Al/Si content and form, and every kind cluster in C/Fe/Al/Si element XANES spectrum can characterize it is each The component structures such as organic carbon, ferriferous oxide valence state, clay mineral or quartz in the specific soil agreegate of separation, and by each The intensity that element XANES spectrum absorbs main peak determines the main active component in the aggregate;To be realized on submicron-scale Soil activation solid phase components (soil ferriferous oxide, organic matter and clay mineral etc.) are separated in situ and characterize its microcosmic knot Structure.
The present invention separates heap of the method by each element that active component in soil microaggregate characterizes its microstructure in situ It is combined after stack image progress image and energy correction, then carries out multielement principal component using the polynary spectrogram of overlapping and gather Alanysis obtains and represents carbon, iron is formed with aluminium silicon difference element, the cluster map of content and structure of, realization separation soil in situ Organic matter fraction based on carbon, the ferriferous oxide component based on iron and the clay pit based on aluminium silicon respectively in aggregate The microstructure features of object component and these typical activity components, for understand in soil nutrient and pollutant in the micro- domain of soil with Active component (organic matter, ferriferous oxide and clay mineral) mechanism of action and its validity control are of great significance.
Detailed description of the invention
Fig. 1 is to utilize synchrotron radiation STXM characterized by techniques soil agreegate typical activity composition features (a-f), content and micro- Aromatic-C, Phenolic-C, Aliphatic-C in sight structure (g-j) g figure, Carboxyl-C expression aromatic carbon, Phenols carbon, fatty carbon and carboxyl carbon;FeCl in h figure3And FeCl2Indicate trivalent and ferrous iron;Muscovite table in i figure and j figure Show mica mineral;According to main peak height can speculate the soil micelle that cluster 6,10 represents in carbon, iron, aluminium and silicon XANES spectrum in g-j Aggressiveness is mainly organic matter;The soil microaggregate that cluster 9 represents is mainly ferric oxide;The soil that cluster 1 represents is micro- Aggregate is mainly mica mineral.
Specific embodiment
The present invention is made a more thorough explanation below with embodiment.The present invention can be presented as a variety of different forms, It should not be construed as limited to the exemplary embodiments described herein.
Separation soil in situ is realized using synchrotron radiation scanning transmission microscopy and mathematical statistics method combination in embodiment Active component and its microstructure of characterization in microaggregate;Specific steps are as follows:
(1) prepared by soil microaggregate: choosing the air-dried soil of 2 mm sieve, the clay of soil is separated and obtained using sedimentation Component is clayed into power spare after freeze-drying.
(2) STXM sample preparation: soil clay particle component and deionized water are mixed with soil suspension, then drip to nitrogen It is air-dried on SiClx window, then silicon window is moved into STXM measurement chamber, helium is passed through and keeps 1/6 atmospheric pressure;It is adopted using transmission mode Collect soil typical element carbon (C), aluminium (Al), the K ABSORPTION EDGE of silicon (Si) and iron (Fe) L ABSORPTION EDGE X-ray near side (ns) absorbing structure (XANES) the storehouse spectrogram composed, as shown in figure 1 shown in a-f.
(3) polygon STXM data processing: the storehouse of soil typical element C/Fe/Al/Si is composed using Axis2000 software The compound spectrogram of C-Fe-Al-Si is generated after figure overlapping;Utilize software Stack-Analyze 2.7 (C. Jacobsen, SUNY Stony Brook) spectrogram correction is carried out on the basis of the storehouse spectrogram of the first energy point;Recombination spectrum after finally correcting is desired to make money or profit Carry out multielement principal component analysis with PCA GUI 1.1.1 software and clustering obtain different distributions cluster figure and XANES spectrum.
(4) active component of cluster analysis result characterization soil microaggregate is utilized: every kind of above-mentioned clustering acquisition The pattern for clustering (Cluster) indicates the soil agreegate two-dimensional appearance with specific C/Fe/Al/Si content and form, utilizes The XANES spectrum of C/Fe/Al/Si element parses organic carbon in the specific soil agreegate of each separation, iron oxidation in every kind of cluster Price state, clay mineral isoreactivity component structure are determined in the aggregate by the intensity that each element XANES composes absorption main peak The relative abundance of the fixed component of activity;To be realized on micro-nano-scale to (the soil iron oxidation of soil activation solid phase components Object, organic matter and clay mineral etc.) separation in situ, and characterize it and form abundance and microstructure;As shown in figure 1 shown in g-j.
Above-mentioned example is only intended to illustrate the present invention, and in addition to this, also there are many different embodiments, and these are implemented Mode be all those skilled in the art after comprehension inventive concept it is also envisioned that therefore, will not enumerate herein.

Claims (1)

1. a kind of method that active component characterizes its microstructure in separation soil microaggregate in situ, which is characterized in that including Following steps:
(1) preparation of soil microaggregate: soil clay particle component is collected using sedimentation, sample is ground into after freeze-drying Powder;
(2) synchrotron radiation scanning transmission microscopy (STXM) is tested: soil clay particle component is spent into ionized water and is prepared as suspension, It pipettes part suspension to drip on silicon nitride window, be moved into after dry in measurement chamber, be passed through helium and keep 1/6 atmospheric pressure, it is then sharp With transmission mode acquisition soil typical element carbon (C), aluminium (Al), the K ABSORPTION EDGE of silicon (Si) and iron (Fe) L ABSORPTION EDGE X-ray The storehouse spectrogram of near side (ns) absorbing structure (XANES) spectrum;
(3) it separates soil agreegate activity multicomponent in situ by polygon STXM data processing and characterizes its microstructure features: will The storehouse spectrogram of soil typical element C/Fe/Al/Si carries out spectrogram correction, and the compound spectrogram of C-Fe-Al-Si is generated after overlapping, Then different clusters are obtained using multielement principal component analysis and clustering, the pattern of every kind of cluster indicates there is specific C/ The soil agreegate of Fe/Al/Si content and form, and every kind cluster in C/Fe/Al/Si element XANES spectrum can characterize it is each The component structures such as organic carbon, ferriferous oxide valence state, clay mineral or quartz in the specific soil agreegate of separation, and by each The intensity that element XANES spectrum absorbs main peak determines the main active component in the aggregate;To be realized on submicron-scale Soil activation solid phase components (soil ferriferous oxide, organic matter and clay mineral etc.) are separated in situ and characterize its microcosmic knot Structure.
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