CN104132839A - Sample-filling method used for electron spin resonance instrument - Google Patents
Sample-filling method used for electron spin resonance instrument Download PDFInfo
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- CN104132839A CN104132839A CN201310161030.6A CN201310161030A CN104132839A CN 104132839 A CN104132839 A CN 104132839A CN 201310161030 A CN201310161030 A CN 201310161030A CN 104132839 A CN104132839 A CN 104132839A
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Abstract
The invention relates to a sample-filling method used for an electron spin resonance instrument and belongs to the field of chronology. The method includes following steps: (1) filling a sample tube with a sample with a sample height being L; (2) placing the sample tube into a scaling sleeve tube, when L is less than h, enabling an inserted length of the sample tube in the scaling sleeve tube to be a+L/2, when L is not more than h, enabling an inserted length of the sample tube in the scaling sleeve tube to be a+h/2, wherein h is a height of a resonant cavity of the electron spin resonance instrument in vertical direction and a is a distance from a center of the resonant cavity to the top of a clamping part of the sample tube of the electron spin resonance instrument; (3) fixing a positioning device onto the sample tube at a position which is adjacent to the top of the scaling sleeve tube; and (4) taking the sample tube out from the scaling sleeve tube and placing the sample tube into the electron spin resonance instrument. According to the method, the sample can be located in an optimized location in the resonant 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 the regularity of distribution and formation evolution of material in the angle research Superimposed Basins from time and space, structure chronology is one of important research contents, can be used for instructing the oil-gas exploration of Superimposed Basins.The earth's crust or sedimentary basin usually form mineral or the fluid with chronology effect at tectonic activity or in forming the process developing, and the chronology feature of studying these mineral or fluid has very important meaning to inquiring into age and the phase time of formation of structure and transformation.
It is foundation that the physics with chronology meaning that mineral, fluid discharge under given conditions, the accurate test of chemical signal feature etc. are take in the research of above-mentioned structure Geochronology and solve.Electron spin resonanceapparatus is one of visual plant of realizing structure Chronologic Study, by it, excited and the electron spin signal intensity measured has reflected the concentration of unpaired electron in sample, unpaired electron in geological sample buries the radiation formation of radioelement in rear country rock by deposition, have accumulated time effect, the division and the fixed year that can be crack, tomography and dissolution stage provide foundation.
In this research field, the normal method adopting is at present, first powder or fluid sample are packed in sample hose, then sample hose is inserted in resonator cavity, unpaired electron in resonator cavity sample is under the double action of magnetic field and microwave electric field, and the microwave energy that absorbs certain frequency is realized the transition to high level by low-lying level, is absorbed micro-wave frequency and energy after being detected device and detecting, show as electron spin signal intensity, can reflect the concentration of unpaired electron in sample.
In order to obtain the test data that accuracy is higher, sample need be placed on the appropriate position of the resonator cavity of electron spin resonanceapparatus, and optimum position is generally center.Because the entry position of sample hose is positioned at the central authorities of resonator cavity in the plane, so can guarantee that sample is in the horizontal center position of resonator cavity.
Yet vertical (perpendicular to the direction of surface level) degree of depth that in the prior art, sample hose enters resonator cavity is difficult to accurate judgement conventionally.Especially in most of situation, the resonator cavity in electron spin resonanceapparatus and sample hose retained part are made by transparent materials, and this causes arriving by naked-eye observation the position of sample.Certainly, allow to the naked eye observe, be also difficult to guarantee its accuracy.
Therefore,, in the urgent need to a kind of dress quadrat method is provided, it can fast put into sample the middle position on the vertical direction of resonator cavity exactly.
Summary of the invention
In order to solve the problems of the prior art, the present invention has designed a kind of dress quadrat method for electron spin resonanceapparatus, can fast exactly sample be put into the optimum position of electron spin resonanceapparatus resonator cavity in the vertical direction, for example middle position, obtains test data accurately.
By the variant of the method according to this invention, can also make any position of sample in the vertical direction in resonator cavity, as long as know the optimum position of testing sample according to the structure of resonator cavity, just can obtain optimum measurement effect.
The present invention proposes a kind of dress quadrat method for electron spin resonanceapparatus, comprising: step 1: sample is packed in sample hose, and wherein height of specimen is L; Step 2: sample hose is put into tolerance sleeve pipe, and when L < h, making the intubating length of sample hose in tolerance sleeve pipe is a+L/2; When L >=h, making the intubating length of sample hose in tolerance sleeve pipe is a+h/2, wherein, the height of the resonator cavity in the vertical direction that h is electron spin resonanceapparatus, a is that resonator cavity center is to the distance on the sample hose retained part top of electron spin resonanceapparatus; Step 3: steady arm is fixed on sample hose in the position adjacent to tolerance cannula tip; Step 4: sample hose is taken out and put in electron spin resonanceapparatus from tolerance sleeve pipe, and fix the position of sample hose by steady arm being stuck in to the sample hose retained part top end of electron spin resonanceapparatus.
In one embodiment, tolerance sleeve pipe is that length is the tubular body of being made by transparent material of a+ (h/2), and tolerance sleeve pipe is provided with the scale indicating from the top down, is denoted as 0 topmost.
In one embodiment, at the in the vertical direction of tolerance sleeve pipe, apart from the position of a, make conspicuous mark with the top.
In one embodiment, in the situation of the L >=h of step 2, sample hose is inserted until the bottom of tolerance sleeve pipe.
In one embodiment, in the situation of the L of step 2 < h, sample hose is inserted until sample be centered close to conspicuous mark.
In one embodiment, steady arm is configured to be clamped in the flexible ring bodies that has on the outer peripheral face of sample hose.
In one embodiment, the internal diameter of tolerance sleeve pipe is than the large 1mm of the external diameter of sample hose.
Device according to the present invention requires extremely low to material, because tolerance sleeve pipe does not need to be directly placed among electron spin resonanceapparatus.And the method according to this invention, only need be by marking the intubating length that scale is adjusted sample hose on the transparent material at tolerance sleeve pipe applicable to any this type of electron spin resonanceapparatus.In conjunction with the height of specimen in sample hose and selected intubating length, the center of sample can accurately overlap with optimum position.Can suitably change the type of steady arm, be beneficial to produce simultaneously.
Above-mentioned technical characterictic can various technical feasible modes combine to produce new embodiment, as long as without prejudice to principle of the present invention.
Accompanying drawing explanation
Hereinafter by based on only for the embodiment of indefiniteness and with reference to accompanying drawing, the present invention being described in more detail.Wherein:
Fig. 1 schematically illustrates according to the dress sampling device 10 for electron spin resonanceapparatus of the present invention.Wherein Fig. 1 left side has shown resonator cavity and the sample hose retained part of conventional electron spin resonanceapparatus, and right side has shown according to the dress sampling device 10 for the instrument that resonates of the present invention.
In the drawings, identical member is indicated by identical Reference numeral.Accompanying drawing is not according to actual scale.
Embodiment
Carry out below with reference to accompanying drawings at length to introduce the present invention.
Fig. 1 schematically illustrates according to the dress sampling device 10 for electron spin resonanceapparatus of the present invention.Wherein, Fig. 1 left side shown conventional electron spin resonanceapparatus resonator cavity (under) and sample hose retained part (on), right side has shown according to the dress sampling device 10 for the instrument that resonates of the present invention.
The electron spin resonanceapparatus that the resonance instrument that Fig. 1 left side shows can for example be produced 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, only enters the part of resonator cavity for effectively measuring sample in sample hose.Resonator cavity center O is a to the distance on sample hose retained part (part that the length that is positioned at resonator cavity top is a-h/2) top.
Generally, resonator cavity in electron spin resonanceapparatus and sample hose retained part are made by transparent materials, so when sample hose is from retained part inserts, operator cannot observe the length that sample hose enters resonator cavity, thereby is not easy to determine whether in the vertical direction is positioned at suitable position to guarantee the accurate of experimental result to sample; Even so, allow to by visual inspection, be also difficult to the error of avoiding larger.Take said structure as basis, and the device 10 of the present invention design and corresponding method can guarantee that sample hose makes effective sample be in the optimum position of resonator cavity, for example center O after insertion.In the embodiment that will introduce below, for example the optimum position of sample is resonator cavity center, and object of the present invention will make sample hose insert after electron spin resonanceapparatus, the center of sample and the center superposition of resonator cavity.
The right side of Fig. 1 has shown according to device 10 of the present invention.Device 10 comprises be commonly used to hold the sample hose 2 of sample, the steady arm 3 that is used for being enclosed within the tolerance sleeve pipe 1 outside sample hose 2 and is used for fixing the position of sample hose 2 in electron spin resonanceapparatus.
Steady arm 3 for example can be sent porch for being stuck in the sample of the sample hose retained part of electron spin resonanceapparatus for can clamped-in style being connected to the flexible ring bodies that has on the outer peripheral face of sample hose 2, or adjacent to tolerance sleeve pipe 1 card in the top.By gravity and steady arm 3, can sample hose 2 is fixing with respect to electron spin resonanceapparatus or tolerance sleeve pipe 1, to confirm intubating length.
In an example, steady arm 3 can move with respect to sample hose 2 along the axial direction of sample hose 2 or be fixing with respect to sample hose 2, thereby achieves the above object.In another example, steady arm 3 can freely remove or be fixed on sample hose 2 from sample hose 2.
With reference to Fig. 1, tolerance sleeve pipe 1 is enclosed within sample hose 2 outsides.Steady arm 3 is being close to tolerance sleeve pipe 1 card at an upper portion thereof.Steady arm 3 can be fixed on the diverse location place of sample hose 2 and then be inserted into the length in tolerance sleeve pipe 1 to adjust sample hose 2.After this length determines, keep steady arm 3 fixing with respect to sample hose 2, sample hose 2 from taking out, tolerance sleeve pipe 1 is put into electron spin resonanceapparatus, steady arm 3 is stuck in the porch of the sample hose retained part of electron spin resonanceapparatus under Action of Gravity Field, and then sample hose 2 is inserted into the length of tolerance in sleeve pipe 1 and is it and was inserted into afterwards the length in electron spin resonanceapparatus.Sample hose 2 is inserted into length in electron spin resonanceapparatus more for example, in conjunction with the amount of the sample 4 in sample hose 2 height of sample (take be sign amount), can, so that the sample of any amount 4 in the vertical directions are positioned at any position of resonator cavity, be preferably in the present embodiment center and the resonator cavity center superposition of sample 4.
According to the structural property of electron spin resonanceapparatus, can judge the optimum position of sample, by device 10 according to the present invention can be easy, mode makes sample put into optimum position cheaply, accurate to guarantee measurement result.
The internal diameter of tolerance sleeve pipe 1 is designed to slightly be greater than the external diameter of sample hose 2, is preferably greater than the external diameter 1mm of sample hose 2.For example, the length of tolerance sleeve pipe 1 is a+h/2, and internal diameter is p, and wherein a+h/2 is from the resonator cavity bottom of electron spin resonanceapparatus to the distance on sample hose retained part top.For example, for the electron spin resonanceapparatus of certain model, it is the types (m > n) such as m, n that the sample hose supporting with it has diameter length, measures the reducible diameter that is greater than maximum sample pipe of internal diameter p of sleeve pipe 2, for example, be p=m+1(mm).
So, same sleeve pipe goes for the electron spin resonanceapparatus of different size, as long as the internal diameter of tolerance sleeve pipe 1 can not be less than the external diameter with the matching used maximum sized sample hose 2 of this electron spin resonanceapparatus.Improved in this way according to the applicability of device 10 of the present invention.
In another variant, the tubular body of being made by transparent material that tolerance sleeve pipe 1 is a+h/2 for length, it is provided with scale from top to bottom, and the scale at top place is made as 0.So, can differentiate the length that sample hose 2 inserts tolerance sleeve pipe 1 by scale, thereby determine that sample hose 2 inserts the length of electron spin resonanceapparatus.The intubating length of sample hose 2 is chosen as and makes to insert after the resonator cavity of electron spin resonanceapparatus when sample hose 2, and the center superposition of the resonator cavity of the free resonance instrument of the center of sample 4 and electronics, guarantees best measurement effect with this.
As shown in Figure 1, can at a distance of the position of a, make conspicuous mark 5 at the tolerance in the vertical direction of sleeve pipe 1 and 0 scale place of top.So, when the sample hose 2 of sample 4 being housed being inserted in tolerance sleeve pipe 1, as long as make the conspicuous mark of being centered close to of sample 45 places, can guarantee that sample hose 2 inserts after electron spin resonanceapparatus, the center of the center of sample 4 in resonator cavity.
According to a further aspect in the invention, also proposed a kind of dress quadrat method for electron spin resonanceapparatus, mainly comprised:
Step 1: sample 4 is packed in sample hose 2, and wherein the height of sample 4 is L;
Step 2: sample hose 2 is put into tolerance sleeve pipe 1, and when L < h, making the intubating length of sample hose 2 in tolerance sleeve pipe 1 is a+L/2; When L >=h, making the intubating length of sample hose 2 in tolerance sleeve pipe 1 is a+h/2;
Step 3: steady arm 3 is fixed on sample hose 2 in the position adjacent to tolerance sleeve pipe 1 top;
Step 4: sample hose 2 is taken out and put in electron spin resonanceapparatus from tolerance sleeve pipe 1, and fix the position of sample hose 2 by steady arm 3 being stuck in to the sample hose retained part top end of electron spin resonanceapparatus.
For the tolerance sleeve pipe 1 that is provided with from top to bottom scale (being 0) and conspicuous mark 5 topmost of being made by transparent material (its total length is a+h/2), sample hose 2 is inserted, by scale, observe, when sample hose 2 arrives intubating length to be selected, for example, when the conspicuous mark of being centered close to of sample 45 place, steady arm 3 is fixed on the outer peripheral face of sample hose 2 at the place, top adjacent to tolerance sleeve pipe 1, to carry out position mark.
In one embodiment, the height L=h of sample 4 for example, the method according to this invention is embodied as:
First, sample 4 is packed in sample hose 2, wherein the height L=h of sample 4;
Secondly, sample hose 2 is put into tolerance sleeve pipe 1, and steady arm 3 is fixed on the outer peripheral face of sample hose 2 in the position adjacent to tolerance sleeve pipe 1 top; Sample hose 2 is inserted until the bottom of tolerance sleeve pipe 1;
Finally, sample hose 2 is taken out and inserted in electron spin resonanceapparatus, and attention keeps the invariant position of steady arm 3, sample hose 2 device 3 that is positioned after the length that enters electron spin resonanceapparatus a+h/2 is held, so guaranteed that effective sample center is in the center of resonator cavity, sample in the vertical direction takes whole resonator cavity.
In another embodiment, the height L=h/2 of sample 4 for example:
First, sample 4 is packed in sample hose 2, wherein the height L=h/2 of sample 4;
Secondly, sample hose 2 is put into tolerance sleeve pipe 1, by the tolerance sleeve pipe 1 of being made by the graduated transparent material of mark, select the suitable intubating length of sample hose 2, for example intubating length is chosen as to a+h/4, make the center of sample 4 in conspicuous mark 5 places, then steady arm 3 is fixed on the outer peripheral face of sample hose 2 in the position adjacent to tolerance sleeve pipe 1 top;
Finally, sample hose 2 is taken out and inserted in electron spin resonanceapparatus, and attention keeps the invariant position of steady arm 3, sample hose 2 device 3 that is positioned after the length that enters electron spin resonanceapparatus a+h/4 is held, so guaranteed that effective sample center is in the center of resonator cavity, sample in the vertical direction medially occupies the resonator cavity of half.
Although invention has been described with reference to preferred embodiment, without departing from the scope of the invention, can carry out various improvement and can replace parts wherein with equivalent it.The present invention is not limited to disclosed specific embodiment in literary composition, but comprises all technical schemes in the scope that falls into claim.
Claims (7)
1. for a dress quadrat method for electron spin resonanceapparatus, comprising:
Step 1: sample is packed in sample hose, and wherein height of specimen is L;
Step 2: sample hose is put into tolerance sleeve pipe, and when L < h, making the intubating length of described sample hose in tolerance sleeve pipe is a+L/2; When L >=h, making the intubating length of described sample hose in tolerance sleeve pipe is a+h/2, wherein, the height of the resonator cavity in the vertical direction that h is electron spin resonanceapparatus, a is that resonator cavity center is to the distance on the sample hose retained part top of electron spin resonanceapparatus;
Step 3: steady arm is fixed on sample hose in the position adjacent to tolerance cannula tip;
Step 4: sample hose is taken out and put in electron spin resonanceapparatus from tolerance sleeve pipe, and fix the position of described sample hose by steady arm being stuck in to the sample hose retained part top end of described electron spin resonanceapparatus.
2. method according to claim 1, is characterized in that, described tolerance sleeve pipe is that length is the tubular body of being made by transparent material of a+ (h/2), and described tolerance sleeve pipe is provided with the scale indicating from the top down, is denoted as 0 topmost.
3. method according to claim 2, is characterized in that, in the vertical direction and the top of described tolerance sleeve pipe, apart from the position of a, makes conspicuous mark.
4. according to the method in claim 2 or 3, it is characterized in that, in the situation of the L >=h of step 2, described sample hose is inserted until the bottom of described tolerance sleeve pipe.
5. method according to claim 3, is characterized in that, in the situation of the L of step 2 < h, described sample hose is inserted until described sample be centered close to described conspicuous mark.
6. according to the method described in any one in the claims, it is characterized in that, described steady arm is configured to be clamped in the flexible ring bodies that has on the outer peripheral face of described sample hose.
7. according to the method described in any one in the claims, it is characterized in that, the internal diameter of described tolerance sleeve pipe is than the large 1mm of the external diameter of described sample hose.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310161030.6A CN104132839B (en) | 2013-05-03 | 2013-05-03 | Dress quadrat method for electron spin resonanceapparatus |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310161030.6A CN104132839B (en) | 2013-05-03 | 2013-05-03 | Dress quadrat method for electron spin resonanceapparatus |
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| CN104132839A true CN104132839A (en) | 2014-11-05 |
| CN104132839B CN104132839B (en) | 2016-07-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486979A (en) * | 2022-04-14 | 2022-05-13 | 国仪量子(合肥)技术有限公司 | Method for acquiring absolute spin number of unpaired electrons of sample |
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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 |
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2013
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Patent Citations (3)
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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 |
| US20110093559A1 (en) * | 2008-06-02 | 2011-04-21 | Mitsubishi Electric Corporation | Data communication system and data communication device |
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Non-Patent Citations (2)
| Title |
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| DORTHE KRISTENSEN,LEIF H. SKIBSTED: "Comparison of Three Methods Based on Electron Spin Resonance", 《J.AGRIC.FOOD CHEM.》, vol. 47, no. 8, 16 July 1999 (1999-07-16) * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114486979A (en) * | 2022-04-14 | 2022-05-13 | 国仪量子(合肥)技术有限公司 | Method for acquiring absolute spin number of unpaired electrons of sample |
| CN114486979B (en) * | 2022-04-14 | 2022-07-29 | 国仪量子(合肥)技术有限公司 | Method for acquiring absolute spin number of unpaired electrons of sample |
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| CN104132839B (en) | 2016-07-06 |
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