CN104132839B - Dress quadrat method for electron spin resonanceapparatus - Google Patents
Dress quadrat method for electron spin resonanceapparatus Download PDFInfo
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- CN104132839B CN104132839B CN201310161030.6A CN201310161030A CN104132839B CN 104132839 B CN104132839 B CN 104132839B CN 201310161030 A CN201310161030 A CN 201310161030A CN 104132839 B CN104132839 B CN 104132839B
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Abstract
The present invention relates to a kind of dress quadrat method for electron spin resonanceapparatus, belong to chronology field.Including: step 1: loaded by sample in sample cell, wherein height of specimen is L；Step 2: sample cell is put in tolerance sleeve pipe, as L < h so that sample cell intubating length in tolerance sleeve pipe is a+L/2；As L >=h so that sample cell intubating length in tolerance sleeve pipe is a+h/2, and wherein, h is the height of the resonator cavity in the vertical direction of electron spin resonanceapparatus, and a is the resonator cavity center distance to the sample cell retained part top of electron spin resonanceapparatus；Step 3: localizer is fixed on sample cell in the position adjacent to tolerance cannula tip；Step 4: sample cell is removed and placed in electron spin resonanceapparatus from tolerance sleeve pipe.The method according to the invention can make sample be in optimum position in resonator cavity.
Description
Technical field
The present invention relates to a kind of dress quadrat method for electron spin resonanceapparatus, belong to chronology field.
Background technology
For from the regularity of distribution of material in the angle research Superimposed Basins in time and space with for mineralizing evolution, structural foliation is one of important research contents, it is possible to be used for instructing the oil-gas exploration of Superimposed Basins.The earth's crust or sedimentary basin frequently form the mineral with chronology effect or fluid in the process of tectonic activity or mineralizing evolution, and there are very important meaning in the age and phase time of inquiring into structure formation and transformation by the chronology feature studying these mineral or fluid.
The accurate tests with the physics of chronology meaning, chemical signal feature that the research of above-mentioned structural foliation problem and solution discharge under given conditions with mineral, fluid etc. are for foundation.Electron spin resonanceapparatus is one of visual plant realizing structural foliation research, the electron spin signals intensity excited by it and measure reflects the concentration of unpaired electron in sample, unpaired electron in geological sample is buried the radiation of radioelement in rear country rock by deposition and is formed, there is accumulated time effect, can for the division of crack, tomography and dissolution stage and determine year provide foundation.
In this research field, at present frequently with method be, first powder or fluid sample are loaded in sample cell, then sample cell is inserted in resonator cavity, unpaired electron in resonator cavity sample is under the dual function of magnetic field and microwave electric field, and the microwave energy absorbing certain frequency realizes by the transition of low-lying level to high level, by the frequency of absorption microwave and energy be detected by the detector rear, show as electron spin signals intensity, the concentration of unpaired electron in sample can be reflected.
The test data higher in order to obtain accuracy, sample need to be placed on the appropriate position of the resonator cavity of electron spin resonanceapparatus, and optimum position is generally center.Owing to the entry position of sample cell is positioned at the central authorities of resonator cavity in the plane, it is possible to ensure that sample is in the horizontal center position place of resonator cavity.
But in the prior art, sample cell enters vertical (being perpendicular to the direction of horizontal plane) degree of depth of resonator cavity and is generally difficult to accurate judgement.Particularly in major part situation, resonator cavity and sample cell retained part in electron spin resonanceapparatus are made by transparent materials, and this causes passing through the naked-eye observation position to sample.Certainly, namely allow to the naked eye be observed, it is also difficult to ensure its accuracy.
Therefore, in the urgent need to providing a kind of dress quadrat method, sample fast can be put into the middle position on the vertical direction of resonator cavity by exactly.
Summary of the invention
In order to solve the problems of the prior art, the present invention devises a kind of dress quadrat method for electron spin resonanceapparatus, fast exactly sample can be put into the optimum position of electron spin resonanceapparatus resonator cavity in the vertical direction, for instance middle position, obtain and test data accurately.
By the variant of the method according to the invention, it is also possible to make sample in the vertical direction be in any position in resonator cavity, as long as know the optimum position of testing sample according to the structure of resonator cavity, it becomes possible to obtain optimum measurement effect.
The present invention proposes a kind of dress quadrat method for electron spin resonanceapparatus, including: step 1: loaded by sample in sample cell, wherein height of specimen is L；Step 2: sample cell is put in tolerance sleeve pipe, as L < h so that sample cell intubating length in tolerance sleeve pipe is a+L/2；As L >=h so that sample cell intubating length in tolerance sleeve pipe is a+h/2, and wherein, h is the height of the resonator cavity in the vertical direction of electron spin resonanceapparatus, and a is the resonator cavity center distance to the sample cell retained part top of electron spin resonanceapparatus；Step 3: localizer is fixed on sample cell in the position adjacent to tolerance cannula tip；Step 4: sample cell is removed and placed in electron spin resonanceapparatus from tolerance sleeve pipe, and fixes the position of sample cell by localizer being stuck in the sample cell retained part top end of electron spin resonanceapparatus.
In one embodiment, the tubular body being made of clear material of tolerance sleeve pipe to be length be a+ (h/2), tolerance sleeve pipe is provided with the scale indicated from the top down, is topmost denoted as 0.
In one embodiment, conspicuous labelling is made in the position of the in the vertical direction of tolerance sleeve pipe with distance a topmost.
In one embodiment, when the L >=h of step 2, sample cell is inserted until measuring the bottom of sleeve pipe.
In one embodiment, when the L < h of step 2, sample cell is inserted until sample is centrally located at conspicuous mark.
In one embodiment, localizer is configured to be clamped in and has elastic ring bodies on the outer peripheral face of sample cell.
In one embodiment, the internal diameter 1mm bigger than the external diameter of sample cell of sleeve pipe is measured.
Tolerance sleeve pipe according to assembly of the invention, material required extremely low, because need not be placed directly among electron spin resonanceapparatus.And the method according to the invention is applicable to this type of electron spin resonanceapparatus any, only the intubating length of sample cell need to be adjusted by marking scale on the transparent material of tolerance sleeve pipe.In conjunction with the height of specimen in sample cell and selected intubating length, the center of sample accurately can overlap with optimum position.Can suitably change the type of localizer simultaneously, be beneficial to produce.
Above-mentioned technical characteristic various technically feasible modes can be combined to produce new embodiment, without departing from principles of the invention.
Accompanying drawing explanation
Hereinafter by based on being only the embodiment of indefiniteness and with reference to accompanying drawing, the present invention being described in more detail.Wherein:
Fig. 1 schematically illustrates the dress sampling device 10 for electron spin resonanceapparatus according to the present invention.Wherein showing resonator cavity and the sample cell retained part of conventional electron spin resonanceapparatus on the left of Fig. 1, right side shows the dress sampling device 10 for the instrument that resonates according to the present invention.
In the drawings, identical component is indicated by identical accompanying drawing labelling.Accompanying drawing is not drawn according to actual ratio.
Detailed description of the invention
Come below with reference to accompanying drawings to introduce the present invention in detail.
Fig. 1 schematically illustrates the dress sampling device 10 for electron spin resonanceapparatus according to the present invention.Wherein, show on the left of Fig. 1 conventional electron spin resonanceapparatus resonator cavity (under) and sample cell retained part (on), right side shows the dress sampling device 10 for the instrument that resonates according to the present invention.
The electron spin resonanceapparatus that the resonance instrument of display on the left of Fig. 1 can such as produce for Brooker company.In the schematic structure shown in Fig. 1, the height of the resonator cavity in the vertical direction of resonance instrument is h, and the part only entering resonator cavity in sample cell is effective measuring samples.Resonator cavity center O is a to the distance on sample cell retained part (being positioned at the part that the length above resonator cavity is a-h/2) top.
Under normal circumstances, resonator cavity and sample cell retained part in electron spin resonanceapparatus are made by transparent materials, so after sample cell inserts from retained part, operator cannot observe sample cell and enter the length of resonator cavity, thus being not easy to determine whether in the vertical direction is positioned at suitable position to ensure the accurate of experimental result to sample；Even so, namely allow to pass through perusal, it is also difficult to avoid bigger error.Based on said structure, device 10 and the corresponding method of present invention design can ensure that sample cell makes effective sample be in the optimum position of resonator cavity after such insertion, for instance center O.In the embodiment will introduced below, for instance the optimum position of sample is resonator cavity center, then namely the purpose of the present invention to make sample cell insert after electron spin resonanceapparatus, the center of sample and the center superposition of resonator cavity.
The right side of Fig. 1 shows according to assembly of the invention 10.Sample cell 2 that device 10 includes being commonly used to holding sample in electron spin resonanceapparatus, localizer 3 for the tolerance sleeve pipe 1 being enclosed within outside sample cell 2 and the position being used for fixing sample cell 2.
Localizer 3 such as can for can be connected to the elastic ring bodies that has on the outer peripheral face of sample cell 2 by clamped-in style, and the sample for being stuck in the sample cell retained part of electron spin resonanceapparatus delivers porch, or adjacent to tolerance sleeve pipe 1 end caught thereon.By gravity and localizer 3, it is possible to sample cell 2 is fixed relative to electron spin resonanceapparatus or tolerance sleeve pipe 1, to confirm intubating length.
In one example, localizer 3 can move relative to sample cell 2 along the axial direction of sample cell 2 or fix relative to sample cell 2, thus reaching above-mentioned purpose.In another example, localizer 3 can freely remove from sample cell 2 or be fixed on sample cell 2.
With reference to Fig. 1, it is outside that tolerance sleeve pipe 1 is enclosed within sample cell 2.Localizer 3 abutted to tolerance sleeve pipe 1 portion caught thereon.Localizer 3 can be fixed on the various location of sample cell 2 and then to adjust the length that sample cell 2 is inserted in tolerance sleeve pipe 1.After this length determines, it is held in position device 3 to fix relative to sample cell 2, electron spin resonanceapparatus is put into after being taken out from tolerance sleeve pipe 1 by sample cell 2, localizer 3 is stuck in the porch of the sample cell retained part of electron spin resonanceapparatus under gravity, and then the length that sample cell 2 is inserted in tolerance sleeve pipe 1 is its length being inserted in electron spin resonanceapparatus later.Sample cell 2 is inserted into the amount (such as with the height of sample for mark amount) in conjunction with the sample 4 in sample cell 2 of the length in electron spin resonanceapparatus, center and the resonator cavity center superposition of sample 4 so that sample 4 in the vertical direction of any amount is positioned at any position of resonator cavity, can be preferably in the present embodiment.
Structural property according to electron spin resonanceapparatus may determine that the optimum position of sample, by mode easy, low cost sample being made to put into optimum position according to assembly of the invention 10, to ensure that measurement result is accurate.
The internal diameter of tolerance sleeve pipe 1 is designed as the external diameter being slightly larger than sample cell 2, it is preferable that more than the external diameter 1mm of sample cell 2.Such as, the length of tolerance sleeve pipe 1 is a+h/2, and internal diameter is p, and wherein a+h/2 is the distance from the resonator cavity bottom of electron spin resonanceapparatus to sample cell retained part top.Such as the electron spin resonanceapparatus of certain model, the sample cell supporting with it has diameter length to be the types (m > n) such as m, n, then the internal diameter p measuring sleeve pipe 2 can be approximately more than the diameter of maximum sample pipe, for instance for p=m+1(mm).
So, same sleeve pipe goes for various sizes of electron spin resonanceapparatus, as long as the internal diameter of tolerance sleeve pipe 1 will not less than the external diameter of maximum sized sample cell 2 matching used with this electron spin resonanceapparatus.Improve the suitability according to assembly of the invention 10 in this way.
In another variant, tolerance sleeve pipe 1 is the tubular body being made of clear material that length is a+h/2, and it is from top to bottom provided with scale, and the scale at top place is set to 0.So, it is possible to differentiate sample cell 2 by scale and insert the length of tolerance sleeve pipe 1, so that it is determined that sample cell 2 inserts the length of electron spin resonanceapparatus.The intubating length of sample cell 2 is chosen so as to after sample cell 2 inserts the resonator cavity of electron spin resonanceapparatus, the center superposition of the resonator cavity of the center of sample 4 and the free resonance instrument of electronics, ensures the measurement effect of the best with this.
As shown in Figure 1, it is possible to make conspicuous labelling 5 with 0 scale place of top at a distance of the position of a at the in the vertical direction of tolerance sleeve pipe 1.So when the sample cell 2 equipped with sample 4 is inserted in tolerance sleeve pipe 1, as long as making sample 4 be centrally located at conspicuous labelling 5 place, then, after can ensure that sample cell 2 inserts electron spin resonanceapparatus, the center of sample 4 is in the center of resonator cavity.
According to a further aspect in the invention, it is also proposed that a kind of dress quadrat method for electron spin resonanceapparatus, specifically include that
Step 1: loaded by sample 4 in sample cell 2, wherein the height of sample 4 is L；
Step 2: sample cell 2 is put in tolerance sleeve pipe 1, as L < h so that the sample cell 2 intubating length in tolerance sleeve pipe 1 is a+L/2；As L >=h so that the sample cell 2 intubating length in tolerance sleeve pipe 1 is a+h/2；
Step 3: localizer 3 is fixed on sample cell 2 in the position adjacent to tolerance sleeve pipe 1 top；
Step 4: sample cell 2 is removed and placed in electron spin resonanceapparatus from tolerance sleeve pipe 1, and fixes the position of sample cell 2 by localizer 3 being stuck in the sample cell retained part top end of electron spin resonanceapparatus.
For be made of clear material be provided with scale (topmost be 0) and the tolerance sleeve pipe 1 of conspicuous labelling 5 from top to bottom for (its total length is a+h/2), sample cell 2 is inserted, observed by scale, when sample cell 2 arrives intubating length to be selected, such as when sample 4 is centrally located at conspicuous labelling 5 place, localizer 3 is fixed on the outer peripheral face of sample cell 2 at the top place adjacent to tolerance sleeve pipe 1, to carry out position mark.
In one embodiment, for instance the height L=h of sample 4, then the method according to the invention is embodied as:
First, sample 4 is loaded in sample cell 2, wherein the height L=h of sample 4；
Secondly, sample cell 2 is put in tolerance sleeve pipe 1, and localizer 3 is fixed on the outer peripheral face of sample cell 2 in the position adjacent to tolerance sleeve pipe 1 top；Sample cell 2 is inserted until measuring the bottom of sleeve pipe 1；
Finally, being taken out by sample cell 2 inserts in electron spin resonanceapparatus, and note the invariant position being held in position device 3, sample cell 2 is positioned device 3 after the length entering electron spin resonanceapparatus a+h/2 and holds, so ensure that effective sample center is in the center of resonator cavity, sample in the vertical direction takes whole resonator cavity.
In another embodiment, for instance the height L=h/2 of sample 4:
First, sample 4 is loaded in sample cell 2, wherein the height L=h/2 of sample 4；
Secondly, sample cell 2 is put in tolerance sleeve pipe 1, by being suitably inserting length by what mark that the tolerance sleeve pipe 1 that graduated transparent material makes selects sample cell 2, such as intubating length is chosen as a+h/4, namely the center making sample 4 is in conspicuous labelling 5 place, is then fixed on the outer peripheral face of sample cell 2 in the position adjacent to tolerance sleeve pipe 1 top by localizer 3；
Finally, being taken out by sample cell 2 inserts in electron spin resonanceapparatus, and note the invariant position being held in position device 3, sample cell 2 is positioned device 3 after the length entering electron spin resonanceapparatus a+h/4 and holds, so ensure that effective sample center is in the center of resonator cavity, sample in the vertical direction medially occupies the resonator cavity of half.
Although by reference to preferred embodiment, invention has been described, but without departing from the scope of the invention, it is possible to it is carried out various improvement and parts therein can be replaced with equivalent.The invention is not limited in the specific embodiment disclosed in literary composition, but include all technical schemes falling in scope of the claims.
Claims (5)
1. for a dress quadrat method for electron spin resonanceapparatus, including:
Step 1: loaded by sample in sample cell, wherein height of specimen is L；
Step 2: sample cell is put in tolerance sleeve pipe, as L < h so that described sample cell intubating length in tolerance sleeve pipe is a+L/2；As L >=h so that described sample cell intubating length in tolerance sleeve pipe is a+h/2, and wherein, h is the height of the resonator cavity in the vertical direction of electron spin resonanceapparatus, and a is the resonator cavity center distance to the sample cell retained part top of electron spin resonanceapparatus；
Step 3: localizer is fixed on sample cell in the position adjacent to tolerance cannula tip；
Step 4: sample cell is removed and placed in electron spin resonanceapparatus from tolerance sleeve pipe, and fixes the position of described sample cell by localizer being stuck in the sample cell retained part top end of described electron spin resonanceapparatus.
2. method according to claim 1, it is characterised in that described tolerance sleeve pipe is length is the tubular body being made of clear material of a+ (h/2), and described tolerance sleeve pipe is provided with the scale indicated from the top down, is topmost denoted as 0.
3. method according to claim 2, it is characterised in that make conspicuous labelling with the position of distance a topmost at the in the vertical direction of described tolerance sleeve pipe.
4. the method according to any one of Claim 1-3, it is characterised in that described localizer is configured to be clamped in has elastic ring bodies on the outer peripheral face of described sample cell.
5. the method according to any one of Claim 1-3, it is characterised in that the internal diameter 1mm bigger than the external diameter of described sample cell of described tolerance sleeve pipe.
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| CN201310161030.6A CN104132839B (en) | 2013-05-03 | 2013-05-03 | Dress quadrat method for electron spin resonanceapparatus |
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| CN201310161030.6A CN104132839B (en) | 2013-05-03 | 2013-05-03 | Dress quadrat method for electron spin resonanceapparatus |
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| CN104132839B true CN104132839B (en) | 2016-07-06 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102297875A (en) * | 2010-06-23 | 2011-12-28 | 中国科学院生态环境研究中心 | Method for measuring hydroxyl free radical in plant body |
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| JP2001139395A (en) * | 1999-11-09 | 2001-05-22 | Sumitomo Metal Ind Ltd | Silicon single crystal, epitaxial wafer, method of measuring amount of nitrogen in silicon single crystal, sample tube unit used in esr method and method of measuring esr spectra |
| KR101398346B1 (en) * | 2008-06-02 | 2014-05-22 | 미쓰비시덴키 가부시키가이샤 | Data communication system and data communication device |
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| CN102297875A (en) * | 2010-06-23 | 2011-12-28 | 中国科学院生态环境研究中心 | Method for measuring hydroxyl free radical in plant body |
Non-Patent Citations (2)
| Title |
|---|
| Comparison of Three Methods Based on Electron Spin Resonance;Dorthe Kristensen,Leif H. Skibsted;《J.Agric.Food Chem.》;19990716;第47卷(第8期);3099-3104 * |
| 标准曲线法测定煤中自由基含量;郑榕萍等;《波谱学杂志》;20110630;第28卷(第2期);259-264 * |
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