CN104122260B - In-situ visualized analysis method of organic bromine compound in soil - Google Patents
In-situ visualized analysis method of organic bromine compound in soil Download PDFInfo
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- CN104122260B CN104122260B CN201410367582.7A CN201410367582A CN104122260B CN 104122260 B CN104122260 B CN 104122260B CN 201410367582 A CN201410367582 A CN 201410367582A CN 104122260 B CN104122260 B CN 104122260B
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Abstract
The invention discloses an in-situ visualized analysis method of an organic bromine compound in soil. The in-situ visualized analysis method comprises the steps of (1) contaminating soil by an organic bromine compound, selecting water saturated microaggregate of the soil, slicing a frozen microaggregate particle to obtain a micro slicing sample and transferring the sample onto a glass slide, (2) analyzing the composition and microcell distribution of carbonic functional groups and clay minerals in the micro slicing sample of the soil to be detected by a synchrotron radiation Fourier transformation infrared micro-imaging technology, (3) analyzing the same area, detected by the synchrotron radiation Fourier transformation infrared micro-imaging technology, of the micro slicing sample by a hard X-ray micro-focusing fluorescent micro-imaging technology, and analyzing the distribution of a tracer element Br and other mineral elements in the area to be detected and the occurrence modes of other mineral elements and Br, and (4) respectively obtaining microcell distribution spectrograms of the carbonic functional groups, the clay minerals, Br and the other mineral elements in the analysis area, and analyzing the spectrograms to obtain the microcell distribution character, related influence factors and other information of the organic bromine pollutant in the soil.
Description
Technical field
The invention belongs to organic pollutant analysis chemical field, more particularly to organic bromo compound in a kind of soil
Visualized in situ analysis method.
Background technology
Organic pollution is in the interfacial migration in soil and conversion behavior and its binding site on soil media and tax
Deposit morphology related.The research of this respect is always the focus in Environmental Chemistry field.Conventional correlational study depends on
The means such as chemical extraction, mass spectral analyses.These methods inevitably disturbance and destruction are caused to soil constitution and structure it is difficult to
The true distribution situation of reflection pollutant in soil.Spatial resolution is had based on the spectroscopy technique of synchrotron radiation light source good, clever
The features such as sensitivity is high.Development with synchrotron radiation spectroscopy technique and application, make organic pollution in in-situ study surrounding medium
Binding site and occurrence patterns be possibly realized, be explore pollutant in soil environmental interface response mechanism one preferred technique.
By the use of Br as tracer element, its occurrence patterns in soil is characterized by micro- focus on light beam line, can be direct
Characterize the binding site of bromo organic pollution and its occurrence patterns in soil.Using the organic dirt of bromo in μ-XRF analysis soil
The binding site of dye thing, test limit can as little as 2mg Br/kg.Meanwhile, can be obtained using FTIR imaging technique organic in soil
The microdistribution of carbon different functional groups.Use in conjunction both technology can set up microdistribution and the soil of bromo organic pollution
Relation between the microdistribution of earth component, thus disclose the binding site of bromo organic pollution in soil visual in imagely.
Content of the invention
It is an object of the invention to provide in a kind of soil organic bromo compound visualized in situ analysis method, Ke Yiyuan
The occurrence patterns of position Visual retrieval pollutant in soil, microdistribution, the true course of reaction reflecting pollutant in soil.
For achieving the above object, the visualized in situ analysis method of organic bromo compound in the soil that the present invention provides,
Its step is as follows：
1) with organic bromo compound contaminated soil, select soil water saturation microaggregate, micro-aggregates will be freezed
Section obtains micro- section sample, and is transferred on microscope slide；
2) utilize the micro- section sample of synchrotron radiation Fourier transform infrared micro-imaging (FTIR) technical Analysis soil to be measured
In containing carbon functional group and clay mineral composition and microdistribution, select micro-cutting piece sample edge clear it is easy to the micelle of positioning gathers
Body granule；
3) application hard X ray micro- confocal fluorescence micro-imaging (μ-XRF) analysis FTIR is detected the same of micro- section sample
Region, analyzes the distribution situation of tracer element Br and other mineral elements in region to be measured, and other mineral elements and Br
Occurrence patterns；
4) obtain respectively and contain carbon functional group, clay mineral, Br and other mineral elements microdistribution in analyzed area
Spectrogram, is analyzed to spectrogram, obtains bromo organic pollution microdistribution and Correlative Influence Factors information.
In described visualization in-situ study method, the particle diameter of microaggregate is between 50-800 μm.
In described visualization in-situ study method, the thickness of micro- section sample is 2-15 μm.
In described visualization in-situ study method, microscope slide is Low-E microscope slide.
In described visualization in-situ study method, step 2) in mensure step-length be 5-30 μm.
In described visualization in-situ study method, step 3) in other mineral elements be Ca, Fe, Mn and Ti.
In described visualization in-situ study method, μ-XRF analysis region is more than and covers FTIR analyzed area, each inspection
Measuring point retention time is in the 0.5-10 second.
In described visualization in-situ study method, step 4) in be using Image-Pro Plus data processing software pair
Spectrogram is overlapped analyzing.
The visualization in-situ study method of the present invention, can in the original location, micro-meter scale, visual in image analysis in soil have
The occurrence patterns of machine bromo pollutant and the method for microdistribution, such that it is able to directly reflect bound site in soil for the pollutant
Point, it is to avoid because complicated pre-treatment causes the interference to information such as pollutant in soil binding site, microdistribution and occurrence patterns,
Response mechanism research for pollutant in soil provides direct scientific evidence.
Brief description
Fig. 1 is that the present invention utilizes two kinds of spectroscopy imaging technique in-situ study bromo organic pollutions of FTIR and μ-XRF in soil
Microdistribution schematic diagram in the micro- section sample of earth.
Fig. 2 is to be polluted using the decabromodiphenyl oxide that FTIR and μ-XRF micro-imaging technique obtains in the embodiment of the present invention 1
In soil visualization distribution and with the relation containing carbon functional group, clay mineral and other mineral elements, Br is as decabromodiphenyl oxide
Tracer element；In figure a is contaminated soil micro-cutting piece optics picture and analyzed area schematic diagram；A-D is to be shown using FTIR respectively
The contaminated soil micro-cutting piece optics picture that micro- imaging technique obtains：A is aromatic radical carbon (1613cm-1), B be carboxyl carbon (1730cm-1), C be fat-based carbon (2922cm-1), D be clay O-H (3621cm-1)；E-I is to be obtained using μ-XRF micro-imaging technique respectively
To contaminated soil micro-cutting piece analyzed area schematic diagram：E be Br, F be Ca, G be Fe, H be Ti, I be Mn.
Fig. 3 is to process, using Image-Pro Plus data processing software, the decabromodiphenyl obtaining in the embodiment of the present invention 1
Ether (darker regions) and aromatic radical carbon (light areas) visualize distribution stacking chart in contaminated soil.
Fig. 4 is can in contaminated soil using the tetrabromobisphenol A that FTIR micro-imaging technique obtains in the embodiment of the present invention 2
Depending on change distribution and with the relation containing carbon functional group, clay mineral and other mineral elements, Br as tetrabromobisphenol A spike unit
Element；In figure a is contaminated soil micro-cutting piece optics picture and analyzed area schematic diagram；A-D is using FTIR micro-imaging skill respectively
The contaminated soil micro-cutting piece optics picture that art obtains：A is aromatic radical carbon (1613cm-1), B be carboxyl carbon (1730cm-1), C be fat
Fat base carbon (2922cm-1), D be clay O-H (3621cm-1)；E-I is to obtain Polluted Soil using μ-XRF micro-imaging technique respectively
Earth micro-cutting piece analyzed area schematic diagram：E be Br, F be Ca, G be Fe, H be Ti, I be Mn.
Fig. 5 is to process, using Image-Pro Plus data processing software, the tetrabromobisphenol A obtaining in the embodiment of the present invention 2
(darker regions) and aromatic radical carbon (light areas) visualize distribution stacking chart in contaminated soil.
Specific embodiment
In the soil that the present invention provides, the visualized in situ analysis method of organic bromo compound is as follows：
1) in test sample the last week, adjust contaminated soil water content to field capacity, and keep overnight (>12 hours), carry
Select the stable microaggregate of size suitable (50-800 μm) for magnifier and optical microscope, for frozen section, make
The standby micro- section sample of 2-15 μ m thick, is placed in Low-E microscope slide, keeps in Dark Place in drying basin, standby survey；
2) analyze the composition containing carbon functional group and clay mineral in micro- section sample first with FTIR micro-imaging technique
With microdistribution information, select micro-cutting piece sample edge clear it is easy to the micro-aggregates of positioning, mensure step-length is 5-30 μ
M, resolution is 1-4cm-1, scan 32-128 time；
3) application μ-XRF analysis FTIR is detected the same area of micro- section sample, Br in analysis region to be measured, Ca, Fe,
The microdistribution information of the elements such as Mn, Ti and Br occurrence patterns in soil, exist for ensureing that two kinds of technology are imaged overlapping regions
More than 100 × 100 μm, μ-XRF analysis region is greater than and covers FTIR analyzed area, measures step-length at 1-30 μm, according to dirt
Dye thing concentration, each test point retention time is in the 0.5-10 second；
4) obtain respectively and contain carbon functional group, clay mineral, Br and other mineral elements microdistribution in analyzed area
Spectrogram, is analyzed to spectrogram using data processing software (as Image Pro Plus etc.), obtains bromo organic pollution micro-
Area's distribution and Correlative Influence Factors information.
The present invention preferred microaggregate particle diameter between 50-800 μm, with facilitate application two kinds of technical Analysis when can accurately determine
Position institute analyzed area, ensures overlapping region more than 100 × 100 μm simultaneously, carries out effective statistical analysiss and compares to facilitate.
The micro- slice thickness of the preferred soil of the present invention between 2-15 μm, with take into account two kinds of analytical technologies to spatial distribution rate and
The requirement of target detection thing concentration.
The present invention analyzes first with FTIR, then using μ-XRF analysis, is penetrated with hard X during avoiding μ-XRF analysis
The radiation damage that line causes to sample.
For verifying the feasibility of the present invention, application the inventive method analyzes two kinds of brominated flame-retardant (decabromodiphenyls respectively
Ether and tetrabromobisphenol A) binding site in brown earth.All analysis results all show, proposed by the present invention based on synchrotron radiation
Spectrum Analysis method can be realized visualized in situ and characterize binding site in soil for the pollutant, for analyzing pollutant in soil
Response mechanism provide direct evidence to support.
Embodiment 1
1) pedotheque preparation：
Decabromodiphenyl oxide (BDE-209) pollutes brown earth, and pollution concentration is 50mg Br/kg；After mixing with soil is uniform, then
Add sterilized water to field capacity, overnight after, in case section.
Select size to fit, stable microaggregate, using Microm HM525 freezing microtome, directly to microaggregate
Cut into slices, slice thickness is 2-15 μm, transfers to Low- glass slide, in case Spectrum Analysis.
2) FTIR microscopic image analysis：
As shown in figure 1, polluting brown earth micro-cutting piece using Taiwan light source (NSRRC) 14A1 light beam line direct analysis BDE-209
Sample, a length of 5-30 μm of analysis step, resolution is 1-4cm-1, scan 32-128 time；By Omnic 8.0, imaging data is carried out
Spectrum unscrambling obtains organic carbon aromatic radical (1613cm-1), carboxyl (1730cm-1), fat-based (2922cm-1) functional group and clay mineral
(the main clay mineral of brown earth is illite, and its O-H position is 3621cm-1) microdistribution figure on micro-cutting piece (Fig. 2A, B, C,
Shown in D).
3) μ-XRF microscopic image analysis：
As shown in figure 1, using BDE-209 in the surveyed the same area of SSRF (SSRF) 15U1 light beam line analysis FTIR
The microdistribution (shown in Fig. 2 E, F, G, H, I) of (Br is as tracer element) and other mineral elements (Ca, Fe, Mn, Ti etc.).
4) carry out data processing by Image-Pro Plus software and obtain BDE-209 microdistribution in brown earth being mainly subject to
Aromatic radical contains carbon functional group and controls (shown in Fig. 3).
Embodiment 2
1) pedotheque preparation：
Tetrabromobisphenol A (TBBPA) pollutes brown earth：Pollution concentration is 50mg Br/kg；After mixing with soil is uniform, add
Sterilized water to field capacity, overnight after, in case section.Soil micro-cutting piece preparation method is with example 1.
2) FTIR microscopic image analysis：
Main Analysis instrument and parameter are with example 1.Spectrum unscrambling is carried out by Omnic 8.0 to imaging data and obtains organic carbon virtue
Perfume base (1613cm-1), carboxyl (1730cm-1), fat-based (2922cm-1) functional group and clay mineral (the main clay mineral of brown earth
For illite, its O-H position is 3621cm-1) microdistribution figure (shown in Fig. 4 A, B, C, D) on micro-cutting piece.
3) μ-XRF microscopic image analysis：
By the use of in the surveyed the same area of SSRF (SSRF) 15U1 light beam line analysis FTIR, (Br is as spike unit for TBBPA
Element) and other mineral elements (Ca, Fe, Mn, Ti etc.) microdistribution (shown in Fig. 4 E, F, G, H, I).
4) carry out data processing by Image-Pro Plus software and obtain TBBPA microdistribution in brown earth being also mainly subject to
Aromatic radical contains carbon functional group and controls (shown in Fig. 5).
Claims (5)
1. in a kind of soil organic bromo compound visualized in situ analysis method, its step is as follows：
1) with organic bromo compound contaminated soil, select soil water saturation microaggregate, micro-aggregates section will be freezed
Obtain micro- section sample, and be transferred on Low-E microscope slide；
2) utilize carbon containing sense in the synchrotron radiation Fourier transform infrared micro-imaging technique analysis micro- section sample of soil to be measured
Group and clay mineral composition and microdistribution；
3) application hard X ray micro- confocal fluorescence micro-imaging technique analysis synchrotron radiation Fourier transform infrared micro-imaging technique
Detected the same area of micro- section sample, analyzed the distribution situation of tracer element Br and other mineral elements in region to be measured,
And the occurrence patterns of other mineral elements and Br；
4) obtain the microdistribution spectrogram in analyzed area containing carbon functional group, clay mineral, Br and other mineral elements respectively,
Spectrogram is analyzed, obtains bromo organic pollution microdistribution and Correlative Influence Factors information；
Wherein, other described mineral elements are Ca, Fe, Mn and Ti；
Hard X ray micro- confocal fluorescence micro-imaging technique analyzed area is more than and to cover synchrotron radiation Fourier transform infrared micro-
Imaging technique analyzed area, each test point retention time is in the 0.5-10 second.
2. in soil according to claim 1 organic bromo compound visualized in situ analysis method, wherein, micelle gather
The particle diameter of body is between 50-800 μm.
3. in soil according to claim 1 organic bromo compound visualized in situ analysis method, wherein, micro-cutting piece
The thickness of sample is 2-15 μm.
4. in soil according to claim 1 organic bromo compound visualized in situ analysis method, wherein, step 2)
In mensure step-length be 5-30 μm.
5. in soil according to claim 1 organic bromo compound visualized in situ analysis method, wherein, step 4)
In be using Image-Pro Plus data processing software spectrogram is overlapped analyze.
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| CN106680306A (en) * | 2017-01-17 | 2017-05-17 | 肖健 | Method for submicron-scale in-situ characterization of soil microaggregate |
| CN109916938B (en) * | 2019-03-08 | 2021-09-21 | 山东省农业科学院畜牧兽医研究所 | Method for measuring spatial distribution of organic pollutants adsorbed by soil organic matters |
| CN110208298B (en) * | 2019-06-03 | 2022-02-01 | 中国农业科学院农业环境与可持续发展研究所 | Method for in-situ separation of active components in soil micro-aggregates to characterize microstructure thereof |
| CN111983126A (en) * | 2020-08-31 | 2020-11-24 | 中国科学院生态环境研究中心 | Method for classifying non-target organic pollutants in soil in polluted area |
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