CN103234992B - Solution sample creep experimental device - Google Patents
Solution sample creep experimental device Download PDFInfo
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- CN103234992B CN103234992B CN201310139099.9A CN201310139099A CN103234992B CN 103234992 B CN103234992 B CN 103234992B CN 201310139099 A CN201310139099 A CN 201310139099A CN 103234992 B CN103234992 B CN 103234992B
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Abstract
The invention provides a solution sample creep experimental device which comprises a temperature control room, a sample room, a container and an injection pump, wherein the temperature control room is fixedly arranged through a base and is fully filled with constant temperature circulation fluid; the sample room is arranged in the temperature control room and consists of an upper duct, a capillary tube and a lower duct, which are sequentially connected; the container is connected with the lower end of the lower duct and is used for containing a solution sample; the injection pump is connected with the upper end of the upper duct; the solution sample is sucked into the capillary tube from the container under the action of the injection pump and creeps back and forth; and light-transmitting orifices are symmetrically formed in the side wall of the temperature control room on the height corresponding to the capillary tube. The solution sample creep experimental device is simple and convenient to operate, high in efficiency and good in sealing performance; the quartz glass capillary tube at a light-transmitting window is low in background scattering and small in absorption amount; the sample creep is realized, and the damage of X rays on the protein solution sample is avoided; and the experimental device is combined with a temperature control device, so that the small angle X-ray scattering (SAXS) measurement for temperature control can be performed.
Description
Technical field
The present invention relates to synchrotron radiation small angle X ray scattering field, be specifically related to a kind of solution sample creep experimental device.
Background technology
Synchrotron radiation small angle X ray scattering utilizes synchrotron radiation light as probe to study a kind of technology and the means of material submicroscopic structure and morphological feature, is widely used in the ambits such as Condensed Matter Physics, material science, biomacromolecule.Wherein, along with the construction and development of Synchrotron Radiation and the generation of various modeling method and perfect, Advance of Small-angle X-ray Scattering Technique (SAXS) has become a kind of important instrument in structure biology gradually, compared with other experimental techniques, the great advantage of SAXS is the structure and the conformation change that may be used for studying biomacromolecule in solution, the assembling of such as protein, the dynamic process such as folding.
In the SAXS of protein solution measures, solution example chamber device is one of critical component.Solution example for weak scattering signal is measured, and requires: 1) optical transmission window backscatter in sample chamber is low below sample chamber device demand fulfillment, absorbs few; 2) prevent X-ray bundle to the radiation damage of protein; 3) experimentally require to realize the control to sample temperature.But the sample chamber device that current most of synchrotron radiation experiment line station adopts is liquid sample pool.This sample cell is made up of copper, stainless steel or organic glass, and central authorities have aperture, and two ends use the polymeric membrane sealings such as Kapton film as X-ray transparent window.Sample cell top has sample holes, flows into for solution example.Often survey a sample, all needed Kapton film to tear, cleaning sample cell.But there is following a few point defect in this sample chamber device: all again will make sample cell before 1) often measuring a sample, operation inconvenience, efficiency is low; 2) if Kapton film does not cement, easily sample leakage is caused; 3) high-throughout synchrotron radiation light easily causes radiation damage to static protein solution; 4) be not easy to carry out temperature controlled measurement.
Summary of the invention
Object of the present invention is just to provide a kind of solution sample creep experimental device, thus overcomes operation inconvenience in prior art, and efficiency is low, and solution example is easily revealed, the easy radiation damage of protein example, and is not easy to carry out temperature controlled defect.
For achieving the above object, the present invention is by the following technical solutions:
There is provided a kind of solution sample creep experimental device, described device comprises: by a hard-wired temperature-controlling chamber of base, be full of constant temperature circulating liquid in described temperature-controlling chamber; Be located at the sample chamber of described temperature-controlling chamber inside, described sample chamber is made up of the upper conduit connected successively, kapillary and downcomer; The container for holding solution example be connected with the lower end of described downcomer; And the syringe pump to be connected with the upper end of described upper conduit; Wherein, solution example is drawn into described kapillary from described container under the effect of described syringe pump also wriggles back and forth, and sidewall symmetry on the height corresponding to described kapillary of described temperature-controlling chamber is having printing opacity mouth.
Described temperature-controlling chamber is connected with a loop temperature-control device.
Described loop temperature-control device is low temperature thermostat bath.
The top of described temperature-controlling chamber is provided with entrance and exit, and described constant temperature circulating liquid flows into described temperature-controlling chamber by described entrance from described low temperature thermostat bath, and flows out to described low temperature thermostat bath by described outlet from described temperature-controlling chamber.
The upper and lower end of described kapillary is connected with described upper and lower conduit respectively by heat-shrink tube.
Described kapillary is quartz glass capillary.
The wall thickness of described quartz glass capillary is 0.010-0.015mm.
The wall thickness of described quartz glass capillary is preferably 0.01mm.The backscatter of quartz glass capillary to light beam of this thickness is low, absorbs few.
Described device also comprises side seat, and described side seat extends from the sidewall of described temperature-controlling chamber is outstanding respectively.For described sample chamber device is fixed on synchrotron radiation line station.
Described temperature-controlling chamber is made of copper, because the heat conductivity of copper is good, and temperature control Be very effective.
Solution sample creep experimental device provided by the present invention has following beneficial effect relative to existing technologies:
(1) this device is convenient to experimental implementation, improves conventional efficient;
(2) this device good seal performance, avoids solution example to reveal;
(3) adopt the backscatter of quartz glass capillary to light beam low, absorb few.
(4) by being connected with syringe pump, the sample that can realize in experimentation is wriggled, and avoids test process to occur protein example radiation damage.
(5) by loop temperature-control device, sample chamber is kept at a constant temperature, achieve temperature controlled SAXS and measure.
Accompanying drawing explanation
With reference to subsequently as the accompanying drawing shown in exemplary embodiments of the present invention, this explanation will be easier to understand, but should not be construed as limitation of the scope of the invention.
Fig. 1 is the structural representation of solution sample creep experimental device in accordance with a preferred embodiment of the present invention;
Fig. 2 is device shown in Fig. 1 removing the structural representation after container, loop temperature-control device and the syringe pump holding solution example;
Fig. 3 is the side view of structure shown in Fig. 2.
Embodiment
For making to understand technological means of the present invention and feature further in depth, careful cooperation accompanying drawing gives citing again and illustrates in rear further:
As Figure 1-3, the invention provides a kind of solution sample creep experimental device of preferred embodiment, the SAXS for solution example measures, and the SAXS especially for protein solution sample measures.Specifically as shown in Figure 1-2, this solution sample creep experimental device mainly comprises: base 1, temperature-controlling chamber 2, sample chamber 3, container 4, syringe pump 5, side seat 6 and loop temperature-control device 7.Wherein, temperature-controlling chamber 2 is located at the top of base 1, and its upper wall is respectively equipped with entrance 22 and outlet 23, is connected, thus passes in temperature-controlling chamber 2 by constant temperature circulating liquid with loop temperature-control device 7; The inside of described temperature-controlling chamber 2 is located in sample chamber 3, be made up of the upper conduit 31 connected successively, kapillary 32 and downcomer 33, the upper and lower end of kapillary 32 is connected with upper conduit 31 and downcomer 33 respectively by heat-shrink tube 34 further, and then plays the effect of sealing linking; Container 4 is connected with the bottom of downcomer 33, for holding testing protein solution example; Syringe pump 5 is connected by the top of conduit with upper conduit 31; Side seat 6 extends from the sidewall of temperature-controlling chamber 2 is outstanding, and side seat is also provided with screw hole 61, thus is convenient to this device to be fixed on the sample stage at online station by side seat, in like manner, base 1 also can arrange screw hole, for fixing this device.According to the conventional design of this area, base 1 and side seat 6 are rotational symmetry design, to strengthen the stability of this device.
As shown in Figure 3, on the left and right sidewall of described temperature-controlling chamber 2 correspond to kapillary 32 height also respectively symmetry have printing opacity mouth 21, protein solution sample is drawn into described kapillary 32 from container 4 under the effect of syringe pump 5, reach the At The Height corresponding with printing opacity mouth 21, and wriggle back and forth up and down under the effect of syringe pump 5, now light beam is just in time irradiated to the protein solution sample in quartz glass capillary 32 by printing opacity mouth 21.The wall thickness of the quartz glass capillary 32 adopted in the present embodiment is 0.01mm, and this kapillary is few to beam absorption, and backscatter is low.The sample peristaltic velocity that the present embodiment adopts is 10 μ L/s.Because in measuring process, protein solution sample continues wriggling back and forth always, thus effectively ensure that the infringement of X ray to protein example is reduced to minimum value.
Should be appreciated that in the present invention, the peristaltic velocity of solution example is not limited in 10 μ L/s, preferably measurement effect radiation damage as far as possible being reduced can be realized.The constant temperature circulating liquid adopted in the present invention is also not limited in water, for different requirement of experiment, can also be alcohol or glycerine.Device of the present invention not only can be used for detecting protein solution sample, is equally applicable to other solution examples.In the present invention, the temperature general control of temperature-controlling chamber is between-40 ~ 100 DEG C, and according to the difference of solution example to be measured, loop temperature-control device can carry out different set, accurately controls the temperature of sample chamber.
Above-described, be only preferred embodiment of the present invention, and be not used to limit scope of the present invention, the above embodiment of the present invention can also make a variety of changes.Namely every claims according to the present patent application and description are done simple, equivalence change and modify, and all fall into the claims of patent of the present invention.The not detailed description of the present invention be routine techniques content.
Claims (10)
1. a solution sample creep experimental device, is characterized in that, described device comprises:
By a base (1) hard-wired temperature-controlling chamber (2), described temperature-controlling chamber is full of constant temperature circulating liquid in (2);
Be located at the sample chamber (3) that described temperature-controlling chamber (2) is inner, described sample chamber (3) are made up of the upper conduit connected successively (31), kapillary (32) and downcomer (33);
The container (4) for holding solution example be connected with the lower end of described downcomer (33); And
The syringe pump (5) be connected with the upper end of described upper conduit (31);
Wherein, solution example is drawn into described kapillary (32) from described container (4) under the effect of described syringe pump (5) also wriggles back and forth, and sidewall symmetry on the height corresponding to described kapillary (32) of described temperature-controlling chamber (2) is having printing opacity mouth (21).
2. solution sample creep experimental device according to claim 1, is characterized in that, described temperature-controlling chamber (2) is connected with a loop temperature-control device (7).
3. solution sample creep experimental device according to claim 2, is characterized in that, described loop temperature-control device (7) is low temperature thermostat bath.
4. solution sample creep experimental device according to claim 3, it is characterized in that, the top of described temperature-controlling chamber (2) is provided with entrance (22) and outlet (23), described constant temperature circulating liquid flows into described temperature-controlling chamber (2) by described entrance (22) from described low temperature thermostat bath, and flows out to described low temperature thermostat bath by described outlet (23) from described temperature-controlling chamber (2).
5. solution sample creep experimental device according to claim 1, is characterized in that, the upper and lower end of described kapillary (32) is connected respectively by heat-shrink tube (34) and described upper and lower conduit (31,33).
6. solution sample creep experimental device according to claim 1, is characterized in that, described kapillary (32) is quartz glass capillary.
7. solution sample creep experimental device according to claim 6, is characterized in that, the wall thickness of described quartz glass capillary is 0.010-0.015mm.
8. solution sample creep experimental device according to claim 7, is characterized in that, the wall thickness of described quartz glass capillary is 0.010mm.
9. solution sample creep experimental device according to claim 1, is characterized in that, described device also comprises side seat (6), and described side seat extends from the sidewall of described temperature-controlling chamber (2) is outstanding respectively.
10. solution sample creep experimental device according to claim 1, is characterized in that, described temperature-controlling chamber (2) is made of copper.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201310139099.9A CN103234992B (en) | 2013-04-19 | 2013-04-19 | Solution sample creep experimental device |
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| CN201310139099.9A CN103234992B (en) | 2013-04-19 | 2013-04-19 | Solution sample creep experimental device |
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| CN103234992A CN103234992A (en) | 2013-08-07 |
| CN103234992B true CN103234992B (en) | 2015-04-08 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103776854B (en) * | 2014-01-26 | 2015-12-23 | 中国科学院上海应用物理研究所 | A kind of solution sample creep experimental system |
| CN109374908B (en) * | 2018-11-23 | 2024-01-26 | 中国科学院上海高等研究院 | Vacuum automatic sample device and vacuum sample chamber suitable for high-throughput screening of solution |
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| EP1925932A1 (en) * | 2005-08-29 | 2008-05-28 | Rigaku Corporation | Vertical/horizontal small-angle x-ray scattering device and measuring method for small-angle x-ray scattering |
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| CN201575979U (en) * | 2009-10-22 | 2010-09-08 | 中国科学院高能物理研究所 | Liquid sample cell and liquid sample device |
| CN203275321U (en) * | 2013-04-19 | 2013-11-06 | 中国科学院上海应用物理研究所 | Wriggle test device for solution sample |
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| EP1925932A1 (en) * | 2005-08-29 | 2008-05-28 | Rigaku Corporation | Vertical/horizontal small-angle x-ray scattering device and measuring method for small-angle x-ray scattering |
| CN201397294Y (en) * | 2009-05-13 | 2010-02-03 | 上海棱光技术有限公司 | Capillary microscale fluorescent sample testing rack |
| CN201575979U (en) * | 2009-10-22 | 2010-09-08 | 中国科学院高能物理研究所 | Liquid sample cell and liquid sample device |
| CN203275321U (en) * | 2013-04-19 | 2013-11-06 | 中国科学院上海应用物理研究所 | Wriggle test device for solution sample |
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