CN103776854B - A kind of solution sample creep experimental system - Google Patents
A kind of solution sample creep experimental system Download PDFInfo
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- CN103776854B CN103776854B CN201410038379.5A CN201410038379A CN103776854B CN 103776854 B CN103776854 B CN 103776854B CN 201410038379 A CN201410038379 A CN 201410038379A CN 103776854 B CN103776854 B CN 103776854B
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Abstract
The invention provides a kind of solution sample creep experimental system, comprising: sample vermiculator, it comprises the sample chamber that temperature-controlling chamber and that an inside is full of constant temperature circulating liquid is arranged on described temperature-controlling chamber inside; For holding the sample temporary room of solution example radioactive waste liquid side by side, it is communicated with the lower end of described sample chamber; Receive and regulate the two-dimension adjustment platform of the position of described sample temporary room according to the conditioning signal of a peripheral input; At least one is for holding the soda liquor container of cleaning fluid; And multi-ported valve door syringe pump, it comprises the syringe pump that a valve and is connected to described valve, and wherein, described valve comprises the first valve port be communicated with the upper end of described sample chamber and the 3rd valve port be communicated with described soda liquor container.The functions such as the present invention can realize solution example auto injection, automatic sample-changing, sample chamber are cleaned automatically, sample wriggling, overcome the defects such as operation inconvenience in prior art, efficiency are low, meet the application demand of automation mechanized operation.
Description
Technical field
The present invention relates to a kind of solution sample creep experimental system, belong to synchrotron radiation field.
Background technology
The Structure and Function of biomacromolecule (mainly protein) is one of current molecular biological key problem.Utilize synchrotron radiation Advance of Small-angle X-ray Scattering Technique, people can study from the sample within the scope of a few KDa to a few MDa molecular weight under solution state, and obtain its structural information.This is just for the combination of the character of research protein molecular under physiological status, conformation change and protein molecular and other substrates provides powerful.Therefore, synchrotron radiation Advance of Small-angle X-ray Scattering Technique is receiving increasing concern in recent years with the advantage of its uniqueness.
Along with the arrival of genome times afterwards comprehensively, a large amount of proteomics researches becomes focus.Conventional synchrotron radiation small angle X ray scattering needs to configure multiple variable concentrations solution for same protein sample, measures with this concentration effect reducing to interfere between particle and may exist.In addition, the impact of change on protein structure and function of the solution environmental such as damping fluid, pH, ionic strength and adjuvant is the problem that researcher is concerned about too.Due to the singularity of synchrotron radiation experiment, after optical gate is opened, experimenter closely can not manipulate sample, but, in the face of the protein example of a large amount of different solutions environment, how realizing sample operation robotization to improve conventional efficient, is the common issue that all synchrotron radiation X-ray small angle experiment centres face.
At present, there is commercial biology laboratory sample introduction equipment in the world, but for synchrotron radiation station real needs and layout, need the transformation carrying out hardware and software, be difficult to realize.And domesticly not yet have corresponding product.
Subject name is a kind of solution sample creep experimental system (patent of invention number: ZL201320203183.8; Application for a patent for invention number: patent 201310139099.9) provides one and operates experimental system of wriggling easily, but this system can not realize cleaning and auto injection function automatically, and thus the application has carried out upgrading on the basis of this patent.
Summary of the invention
For the defect existed in prior art, the object of the present invention is to provide a kind of solution sample creep experimental system automatically can cleaning auto injection, to realize solution example auto injection, the function such as automatic sample-changing, sample chamber are cleaned automatically, sample wriggling, effectively overcome the defects such as operation in prior art is inconvenient, efficiency is low, meet the application demand of synchrotron radiation station solution example automation mechanized operation.
For achieving the above object, the present invention is by the following technical solutions:
A kind of solution sample creep experimental system, this experimental system comprises:
Sample vermiculator, it comprises the sample chamber that temperature-controlling chamber and that an inside is full of constant temperature circulating liquid is arranged on described temperature-controlling chamber inside;
For holding the sample temporary room of solution example radioactive waste liquid side by side, it is communicated with the lower end of described sample chamber;
Receive and regulate the two-dimension adjustment platform of the position of described sample temporary room according to the conditioning signal of a peripheral input;
At least one is for holding the soda liquor container of cleaning fluid; And
Multi-ported valve door syringe pump, it comprises the syringe pump that a valve and is connected to described valve, wherein, described valve comprises the first valve port be communicated with the upper end of described sample chamber and the 3rd valve port be communicated with described soda liquor container, described syringe pump receives and to be drawn into by the described solution example in described sample temporary room in described sample chamber according to the control signal of a peripheral input and to make it wriggle back and forth, or sucks in sample chamber the described cleaning fluid in described soda liquor container to clean sample chamber.
Further, described sample chamber comprises the upper conduit, a kapillary and the downcomer that are communicated with successively, and the upper end of described upper conduit is communicated with described first valve port, and described downcomer is communicated with described sample temporary room.
Further, described sample temporary room is provided with the sample hole slot for holding solution example and the waste liquid hole slot for discharging waste liquid, and is full of constant temperature circulating liquid around described sample hole slot and around described waste liquid hole slot.
Preferably, described wriggling experimental system also comprises a temperature control circulating device be communicated with described sample temporary room with described temperature-controlling chamber.
Preferably, described temperature control circulating device is low temperature thermostat bath.
Further, described sample temporary room side is provided with the first entrance and the first outlet, described temperature-controlling chamber upper end is provided with the second entrance and the second outlet, wherein, the outlet of described temperature control circulating device is communicated with described first entrance, described first outlet is communicated with described second entrance, and described second outlet is communicated with the entrance of described temperature control circulating device.
Further, on the cell wall of described waste liquid hole slot side and apart from bottom land one section of At The Height of this waste liquid hole slot, be provided with a waste liquid outlet, described waste liquid outlet is connected with a peripheral waste fluid container by a connecting duct.
Aforementioned a kind of solution sample creep experimental system, described two-dimension adjustment platform comprises horizontal level adjustment module for driving described sample temporary room to move horizontally and for driving the upright position adjustment module of the vertical movement of described sample temporary room.
Further, described horizontal level adjustment module comprises the cross sliding clock and that a horizontal base, horizontal screw lead, be arranged on described horizontal base is arranged on described horizontal screw lead and is connected with described horizontal screw lead and receives the horizontal step motor of described conditioning signal;
Described upright position adjustment module comprises one and is fixedly connected on vertical base on described cross sliding clock, and the vertical slipper and that a down-feed screw, be arranged on described vertical base is arranged on described down-feed screw is connected with described down-feed screw and receives the vertical step motor of described conditioning signal.
Aforementioned a kind of solution sample creep experimental system, described valve also comprises the second valve port with air communication.
Automatically the solution sample creep experimental system can cleaning automatic sample-changing provided by the present invention has following beneficial effect relative to prior art:
(1) this device is simple to operate, and conventional efficient is high;
(2) adopt high precision multi-ported valve door syringe pump, each valve port by conduit with hold different types of soda liquor container and be communicated with, for protein solution sample of different nature, different cleaning processes can be designed;
(3) adopt two-dimension adjustment platform, by adjustment in both the horizontal and vertical directions, realize the evolution of protein solution sample;
(4) this device is provided with the waste liquid hole slot of special construction, while cleaning fluid waste liquid is discharged, can clean, effectively prevent the cross pollution of different solutions sample room to sample chamber downcomer mouth of pipe outer wall.
(5) by being connected in series with temperature control circulating device, the sample in sample chamber and sample temporary room hole slot all keeps at a constant temperature, and the SAXS achieving temperature-controllable measures;
(6) under the accurate control of peripheral computer, multi-ported valve door syringe pump and two-dimension adjustment platform cooperatively interact, and achieve automatic sample-changing, auto injection, sample chamber is cleaned automatically, dry, the functions such as sample wriggling;
(7) this device adopt correlation control unit and driver be that synchrotron radiation is special, meet synchrotron radiation station real needs and layout, become one with experiment centre miscellaneous equipment.
Accompanying drawing explanation
With reference to the accompanying drawing made as exemplary embodiments of the present invention subsequently, 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 the solution sample creep experimental system automatically can cleaning automatic sample-changing;
Fig. 2 is the structural representation of multi-ported valve door syringe pump;
Fig. 3 is the structural representation of two-dimension adjustment platform and sample temporary room;
Fig. 4 is the vertical view of sample temporary room;
Fig. 5 is the structural representation of sample vermiculator;
Fig. 6 is the control method process flow diagram of peripheral computer.
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 1-5, the invention provides a kind of solution sample creep experimental system automatically can cleaning auto injection, the SAXS for solution example measures, and the SAXS especially for protein solution sample measures.Specifically as shown in Figure 1, this experimental system mainly comprises multi-ported valve door syringe pump 1, sample vermiculator 4, loop temperature-control device 6 and the sample temporary room 3 connected successively, also comprise one for supporting sample temporary room 3 and regulating the two-dimension adjustment platform 2 of the position of sample temporary room 3, wherein, multi-ported valve door syringe pump 1 and two-dimension adjustment platform 2 control by peripheral computer 5.
Respectively each device in this experimental system is described in detail below:
As depicted in figs. 1 and 2, multi-ported valve door syringe pump 1 comprises connected syringe pump 11 and a valve 12, and valve 12 comprises multiple valve port 13-17, wherein, first valve port 13 is communicated with the upper end of sample vermiculator 4, second valve port 14 and air communication, the 3rd valve port 15,16 is communicated with 171 with the soda liquor container 151,161 holding cleaning fluid respectively by conduit with 17.In the present embodiment, control by peripheral computer 5 switching that the stepper motor (figure does not indicate) be positioned at after valve 12 can realize between each valve port 13-17, and control to be positioned at syringe pump 11 another stepper motor (figure does not indicate) below and the leading screw of syringe pump 11 (figure does not indicate) can be driven to realize high-precision solution suck and discharge.
Fig. 3 shows the structural representation of two-dimension adjustment platform 2 and sample temporary room 3.As shown in the figure, two-dimension adjustment platform 2 comprises horizontal level adjustment module and upright position adjustment module, wherein, horizontal level adjustment module comprises a horizontal base 24, horizontal screw lead 26, be arranged on horizontal base 24 cross sliding clock 28 and be arranged on horizontal screw lead 26 and is arranged on horizontal base 24 right-hand member and the horizontal step motor 22 be connected with horizontal screw lead 26; Upright position adjustment module comprises the vertical base 23, be fixedly connected on cross sliding clock 28 down-feed screw 25, be arranged on vertical base 23 vertical slipper 27 and be arranged on down-feed screw 25 and is arranged on vertical base 23 top and the vertical step motor 21 be connected with down-feed screw 25.When sample temporary room 3 needs to move horizontally, drive horizontal screw lead 24 by horizontal step motor 22, sample temporary room 3 can be driven to move horizontally; When sample temporary room 3 needs vertically to move, drive down-feed screw 25 by vertical step motor 21, sample temporary room 3 vertically movement can be driven.In the present embodiment, vertical step motor 21 and horizontal step motor 22 receive the conditioning signal that peripheral computer 5 exports, and perform an action according to this conditioning signal.
In addition, sample temporary room 3 is provided with the sample hole slot 33 of multiple accommodation sample and one for discharging the waste liquid hole slot 34 of waste liquid from its top, and its side is provided with the first outlet 31 and the first entrance 32, namely described constant temperature circulating liquid flow through sample temporary room 3 and around sample hole slot 33 and waste liquid hole slot 34, temperature control circulating device 6 is at this preferred existing low temperature thermostat bath by this first gateway 31 and 32 from temperature control circulating device 6.Wherein, on the cell wall of waste liquid hole slot 34 side and apart from bottom land one section of At The Height of hole slot 34, be provided with a waste liquid outlet 35, and the peripheral waste fluid container 36 that this waste liquid outlet 35 holds waste liquid by a connecting duct and is communicated with.
Composition graphs 3 and Fig. 4 known, sample hole slot 33 and waste liquid hole slot 34 all cylindrical, wherein, sample hole slot 33 comprises multiple hole slots such as the first sample hole slot 331 and the second sample hole slot 332, sample hole slot 33 is divided into diameter 12mm and 6mm two kinds of specifications herein, is applicable to the centrifuge tube (not shown) holding different size respectively.When the centrifuge tube filling solution example inserts in sample hole slot 33, the constant temperature circulating liquid around sample hole slot 33 can make the sample temperature in centrifuge tube remain constant.
As shown in Figure 5, for the structural representation of sample vermiculator 4, it comprises a temperature-controlling chamber 41 and being full of constant temperature circulating liquid and is arranged on sample chamber 42 in temperature-controlling chamber 41, wherein, temperature-controlling chamber 41 is preferably made of copper, this is because the heat conductivity of copper is good, temperature control Be very effective, and its top is provided with the second entrance 43 and the second outlet 44.Described constant temperature circulating liquid flows through temperature-controlling chamber 41 by this second entrance 43 and the second outlet 44, as shown in Figure 1, the outlet of temperature control circulating device 6 is communicated with the first entrance 32, first outlet 31 is communicated with the second entrance 43, second outlet 44 is communicated with the entrance of temperature control circulating device 6, thus realizes constant temperature circulating liquid temperature control circulating device 6, circulating between sample temporary room 3 and sample vermiculator 4.
In the present embodiment, the sample chamber 42 being located at temperature-controlling chamber 41 inside is made up of the upper conduit 421 be communicated with successively, kapillary 422 and downcomer 423, wherein, upper conduit 421 is communicated with the first valve port 13 of multi-ported valve door syringe pump 1, and downcomer 423 is in the sample hole slot 33 that immerses sample temporary room 3 or waste liquid hole slot 34.In addition, side seat 45 extends from the sidewall of temperature-controlling chamber 41 is outstanding, and side seat 45 is also provided with screw hole 451, thus be convenient to this sample vermiculator 4 to be fixed on by side seat on the sample stage of synchrotron radiation X-ray small angle scattering experiment centre, in like manner, also this device 4 is fixed by arranging screw hole on base 46.
Fig. 6 shows the control method process flow diagram of peripheral computer 5, and its operating process is: first, starts peripheral computer 5; Regulate the position of two-dimension adjustment platform 2, with downcomer 423 place making the first sample hole slot 331 holding solution example to be measured move to sample vermiculator 4; Sampling volume and the sample introduction speed of multi-ported valve door syringe pump 1 are set, and the first valve port 13 is set to sample introduction valve port, start sample introduction operation, so that the sample in sample hole slot 33 is sucked in kapillary 422; Then, start the sample wriggling measurement pattern of multi-ported valve door syringe pump 1, and open the beam shutter of light beam line, carry out synchrotron radiation experiment measuring; After measurement completes, regulate the position of two-dimension adjustment platform 2, to make the second empty sample hole slot 33 move to downcomer 423 place, to reclaim the solution example of discharging in downcomer 423; Subsequently, again regulate the position of two-dimension adjustment platform 2, waste liquid hole slot 34 is made to move to downcomer 423 place, and reset the sample introduction valve port of multi-ported valve door syringe pump 1, sampling volume and sample introduction speed, then sample introduction operation is started, to suck in syringe pump 11 by the cleaning fluid in soda liquor container 151,161 or 171; Finally, the nesting body sum stock layout speed of multi-ported valve door syringe pump 1 is set, and the first valve port 13 is set to stock layout valve port, start stock layout operation, so that the cleaning fluid in syringe pump 11 is injected sample vermiculator 4; After cleaning operation completes, cleaning fluid is discharged by waste liquid hole slot 34.
For understanding workflow of the present invention in more detail, lifting following examples and auto injection and automatic cleaning process be explained:
Deionized water solution is held in soda liquor container 151; The conduit be connected with the second valve port 14 is placed in air; The centrifuge tube holding testing protein solution example is inserted with in first sample hole slot 331; Second sample hole slot 332 interpolation is free centrifuge tube, gives over to and surveys protein solution recovery use.
Because downcomer 423 position of sample vermiculator 4 is fixed, two-dimension adjustment platform 2 is regulated by peripheral computer 5, to make the first sample hole slot 331 move to downcomer 423 place, and guarantee in the testing protein solution that downcomer 423 mouth of pipe immerses in the first sample hole slot 331.Sampling volume and the sample introduction speed of multi-ported valve door syringe pump 1 are set by peripheral computer 5 subsequently, and the first valve port 13 is set to sample introduction valve port, after starting sample introduction operation, testing protein solution is drawn in the kapillary 422 of sample vermiculator 4 by syringe pump 11 from the centrifuge tube of the first sample hole slot 331, the sample wriggling measurement pattern of then opening multi-ported valve door syringe pump 1 is wriggled in kapillary 422 back and forth to make testing protein solution, open beam shutter, the protein solution synchrotron radiation small angle X ray scattering carrying out antiradiation injury is measured.After measurement completes, again regulate two-dimension adjustment platform 2, downcomer 423 place is moved to make the second sample hole slot 332, by controlling multi-ported valve door syringe pump 1, the protein solution sample surveyed being discharged in the empty centrifuge tube of the second sample hole slot 332 from kapillary 422, surveying protein solution to reclaim.
Again regulate two-dimension adjustment platform 2, make waste liquid hole slot 34 move to downcomer 423 place.Then arrange sampling volume and the sample introduction speed of multi-ported valve door syringe pump 1, and the 3rd valve port 15 is set to sample introduction valve port, after starting sample introduction operation, deionized water solution is drawn in syringe pump 11 from soda liquor container 151 by syringe pump 11.The nesting body sum stock layout speed of multi-ported valve door syringe pump 1 is set, and the first valve port 13 is set to stock layout valve port, after starting stock layout operation, the deionized water solution of its inside is discharged by syringe pump 11, deionized water flows through the upper conduit 421 of sample vermiculator 4, kapillary 422, downcomer 423 flow to waste liquid hole slot 34, and be expelled in peripheral waste fluid container 36 eventually through waste liquid outlet 35.Because waste liquid outlet 35 has a segment distance apart from the bottom of waste liquid hole slot 34, when downcomer 423 stretch into waste liquid hole slot 34 inside carry out stock layout time, the deionized water residued in bottom waste liquid hole slot 34 can clean downcomer 423 mouth of pipe outer wall, effectively prevent the cross pollution of different solutions sample room.In addition, when the second valve port 14 of multi-ported valve door syringe pump 1 is set to sample introduction valve port, same to aforesaid operations, can pass into air in sample vermiculator 4, realize sample chamber functions/drying.
Should be appreciated that cleaning solution of the present invention is not limited in deionized water solution, be also not limited only to a kind of cleaning solution, for different protein solution samples, concrete cleaning process can be designed.
Above-described, be only preferred embodiment of the present invention, be not intended 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 system, is characterized in that, this experimental system comprises:
Sample vermiculator, it comprises the sample chamber that temperature-controlling chamber and that an inside is full of constant temperature circulating liquid is arranged on described temperature-controlling chamber inside;
For holding the sample temporary room of solution example radioactive waste liquid side by side, it is communicated with the lower end of described sample chamber;
Receive and regulate the two-dimension adjustment platform of the position of described sample temporary room according to the conditioning signal of a peripheral input;
At least one is for holding the soda liquor container of cleaning fluid; And
Multi-ported valve door syringe pump, it comprises the syringe pump that a valve and is connected to described valve, wherein, described valve comprises the first valve port be communicated with the upper end of described sample chamber and the 3rd valve port be communicated with described soda liquor container, described syringe pump receives and to be drawn into by the described solution example in described sample temporary room in described sample chamber according to the control signal of a peripheral input and to make it wriggle back and forth, or sucks in sample chamber the described cleaning fluid in described soda liquor container to clean sample chamber.
2. solution sample creep experimental system according to claim 1, it is characterized in that, described sample chamber comprises the upper conduit, a kapillary and the downcomer that are communicated with successively, and the upper end of described upper conduit is communicated with described first valve port, and described downcomer is communicated with described sample temporary room.
3. solution sample creep experimental system according to claim 1, it is characterized in that, described sample temporary room is provided with the sample hole slot for holding solution example and the waste liquid hole slot for discharging waste liquid, and is full of constant temperature circulating liquid around described sample hole slot and around described waste liquid hole slot.
4. solution sample creep experimental system according to claim 3, is characterized in that, described wriggling experimental system also comprises a temperature control circulating device be communicated with described sample temporary room with described temperature-controlling chamber.
5. solution sample creep experimental system according to claim 4, is characterized in that, described temperature control circulating device is low temperature thermostat bath.
6. solution sample creep experimental system according to claim 5, is characterized in that,
Described sample temporary room side is provided with the first entrance and the first outlet, described temperature-controlling chamber upper end is provided with the second entrance and the second outlet, wherein, the outlet of described temperature control circulating device is communicated with described first entrance, described first outlet is communicated with described second entrance, and described second outlet is communicated with the entrance of described temperature control circulating device.
7. solution sample creep experimental system according to claim 3, it is characterized in that, on the cell wall of described waste liquid hole slot side and apart from bottom land one section of At The Height of this waste liquid hole slot, be provided with a waste liquid outlet, described waste liquid outlet is connected with a peripheral waste fluid container by a connecting duct.
8. solution sample creep experimental system according to claim 1, it is characterized in that, described two-dimension adjustment platform comprises horizontal level adjustment module for driving described sample temporary room to move horizontally and for driving the upright position adjustment module of the vertical movement of described sample temporary room.
9. solution sample creep experimental system according to claim 8, is characterized in that,
Described horizontal level adjustment module comprises the cross sliding clock and that a horizontal base, horizontal screw lead, be arranged on described horizontal base is arranged on described horizontal screw lead and is connected with described horizontal screw lead and receives the horizontal step motor of described conditioning signal;
Described upright position adjustment module comprises one and is fixedly connected on vertical base on described cross sliding clock, and the vertical slipper and that a down-feed screw, be arranged on described vertical base is arranged on described down-feed screw is connected with described down-feed screw and receives the vertical step motor of described conditioning signal.
10. solution sample creep experimental system according to claim 1, is characterized in that, described valve also comprises the second valve port with air communication.
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| CN105154327B (en) * | 2015-09-30 | 2017-09-12 | 重庆大学 | A kind of vascular fluid artificial cell experiment instrument |
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| EP2458372B1 (en) * | 2005-08-29 | 2013-09-18 | Rigaku Corporation | Method for measuring small angle x-ray scattering |
| 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 |
| CN102998317A (en) * | 2012-11-26 | 2013-03-27 | 中国工程物理研究院核物理与化学研究所 | Continuous and automatic measuring system for two paths of radioactive liquids |
| CN103234992B (en) * | 2013-04-19 | 2015-04-08 | 中国科学院上海应用物理研究所 | Solution sample creep experimental device |
| CN203981612U (en) * | 2014-01-26 | 2014-12-03 | 中国科学院上海应用物理研究所 | A kind of solution example wriggling experimental system |
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