CN206601348U - X ray single crystal diffraction instrument easy-weathering crystal cryo-microscope loading systems - Google Patents

X ray single crystal diffraction instrument easy-weathering crystal cryo-microscope loading systems Download PDF

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Publication number
CN206601348U
CN206601348U CN201720239861.4U CN201720239861U CN206601348U CN 206601348 U CN206601348 U CN 206601348U CN 201720239861 U CN201720239861 U CN 201720239861U CN 206601348 U CN206601348 U CN 206601348U
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China
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low temperature
crystal
single crystal
weathering
cryo
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杨培菊
沈志强
黄晓卷
任伟
胡霄雪
何荔
刘佳梅
牛建中
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Lanzhou Institute of Chemical Physics LICP of CAS
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Lanzhou Institute of Chemical Physics LICP of CAS
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Abstract

The utility model discloses a kind of X ray single crystal diffractions instrument easy-weathering crystal cryo-microscope loading system, including angular instrument and cryogenic probe, the loading system also chooses brilliant platform, micro-imaging unit and low temperature support Unit including low temperature, it is provided with directly over angular instrument and is connected with it by support and hollow low temperature of matrix immediately below cryogenic probe chooses brilliant platform, the low temperature chooses brilliant platform and passes sequentially through that coolant set by its side is imported and exported, coolant pipeline is connected with the low temperature support Unit being located at outside single crystal diffractometer;Micro-imaging unit includes industrial camera, display screen and light microscope, and display screen and light microscope are connected with industrial camera.The utility model thoroughly solves the problem of easy-weathering crystal is difficult to obtain complete diffraction data, has further expanded the function of X-ray single crystal diffractometer Cryo Equipment.

Description

X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading system
Technical field
The utility model, which is related to crystal, to be selected can realize easy-weathering crystal in low temperature with loading system, more particularly to one kind Under it is micro- select with loading system, be the expansion to X-ray single crystal diffractometer Cryo Equipment function.
Background technology
Requirement of the single crystal diffractometer to sample is very high:Single crystal samples size requires smaller, and crystal itself must be without splitting Trace, without concave surface, transparent, crystal mass directly determines that can the quality and its structure of diffraction data finally be successfully parsed. Therefore it is an extremely important link in single crystal diffractometer testing procedure that crystal, which is selected, and it is directly determined in monocrystalline test process The collection of X-ray diffraction data and the parsing of structure success.And have a class crystal easy-weathering crystal, its select and on Sample is extremely difficult.This crystalloid, which leaves mother liquor original monocrystalline is had within the limited time, becomes powder crystal.Crystal whether weathering Being taken out only from mother liquor to find, therefore can not predict in advance.Most crystal weathering are because containing in its structure cell Boiling point is than relatively low solvent molecule, and crystal, which once leaves parent solution solvents molecule, to be scattered and disappeared, and cause structural collapse.For weathering speed Slightly slow crystal can pass it through it is necessary select and cut, be sealed in 0.5 ~ 1mm thickness 1.5cm length, the glass equipped with mother liquor In capillary, then it is bonded on the glass fibre being of convenient length, and is quickly placed to the brilliant platform low-temperature test of load.But it is right The difficulty selected in the faster crystal of weathering speed is very big, but these crystal often have very high scientific research value, its Structured data is typically the information of the highly desirable acquisition of scientific research personnel, at present for these crystal because easy-weathering has led to not Into the situation of test, solution can only change solution to cultivate metastable crystal prototype again.Easy-weathering crystal is selected Problem turns into the technical problem that current monocrystalline tester urgently expects to solve.
Utility model content
The utility model is difficult to select for easy-weathering crystal causes easy-weathering crystal to be difficult to obtain complete diffraction with loading The problem of data, on the basis of existing X-ray single crystal diffractometer, devise a set of X-ray single crystal diffractometer easy-weathering crystal Cryo-microscope loading system, has further expanded the function of X-ray single crystal diffractometer Cryo Equipment.
X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading system, including angular instrument and cryogenic probe, it is special Levy and be that the loading system is also chosen directly over brilliant platform, micro-imaging unit and low temperature support Unit, the angular instrument including low temperature Brilliant platform is chosen provided with the hollow low temperature of matrix being connected with it by support and immediately below cryogenic probe, the low temperature chooses brilliant platform successively Imported and exported by coolant set by its side, coolant pipeline is connected with the low temperature support Unit outside single crystal diffractometer; The micro-imaging unit include industrial camera, display screen and light microscope, the display screen and light microscope with Industrial camera is connected.
The low temperature support Unit is low-temperature cooling fluid circulating pump or is pressurized liquid nitrogen container certainly.
The utility model has advantages below compared with prior art:
(1)Solve the problems, such as to tune and monocrystalline weathering during loading
Crystal weathering phenomenon is difficult to avoid in culture and test process.During crystal culture typically can from acetone, methanol, Solvent molecule can be sandwiched in the low boiling points such as ethanol, acetonitrile, volatile solvent, crystal growing process and obtains perfect crystal, but These solvent molecules easily lose again after mother liquor is left causes structural collapse, it is impossible to complete test.Because easy-weathering crystal is logical Often stablize relatively under low-temperature condition, the system for intending developing will utilize the principle, and single crystal samples are placed on into low temperature with mother liquor On sample stage, mother liquor is suctioned out at low temperature, and high-clear display is amplified to by video camera visualization, is cut and is selected, borrowed The cryogenic system of single crystal diffractometer is helped, loading and the test of easy-weathering crystal are completed at low temperature, easy-weathering crystal is thoroughly solved The problem of being difficult to obtain complete diffraction data.
(2)Solve the problems, such as the loading of cryogenic freezing monocrystalline
The crystal that plan development device can solve cryogenic freezing culture is selected.Due to partial crystals at normal temperatures solubility compared with Greatly, only reduction temperature can just turn out.If this crystalloid is selected at room temperature to be dissolved quickly, it is impossible to complete to survey Examination.The system for intending developing will realize whole low-temperature operation and low-temperature test, thoroughly solve the problems of dissolution of such sample.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
In figure:1- X-ray single crystal diffractometers, 2- angular instruments, 3- supports, 4- low temperature chooses brilliant platform, 5- light microscopes, 6- Industrial camera, 7- display screens, 8- cryogenic probes, 9- low temperature support Units.
Embodiment
As shown in figure 1, X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading system, including angular instrument 2 and low Temperature probe 8, the loading system is also chosen directly over brilliant platform 4, micro-imaging unit and low temperature support Unit 9, angular instrument 2 including low temperature Brilliant platform 4 is chosen provided with the hollow low temperature of matrix being connected with it by support 3 and immediately below cryogenic probe 8, the low temperature chooses brilliant platform 4 Pass sequentially through coolant import and export set by its side, coolant pipeline and the low temperature support Unit 9 outside single crystal diffractometer 1 It is connected;Micro-imaging unit includes industrial camera 6, display screen 7 and light microscope 5, and display screen 7 and light microscope 5 are equal It is connected 6 with industrial camera.
Low temperature support Unit 9 is low-temperature cooling fluid circulating pump or is pressurized liquid nitrogen container certainly.
Application method:Single crystal diffractometer glass door is opened, low temperature is chosen into brilliant platform 4 angular instrument 2 is being fixed on just by support 3 Top and immediately below cryogenic probe 8, checks and connects low temperature and choose brilliant platform 4 and low temperature support Unit 9.Open micro-imaging Display screen 7 and industrial camera 6, and focus the concave surface that low temperature is chosen into brilliant platform 4 and be amplified to display screen 7.Open single crystal diffraction The low temperature software of instrument 1 and low temperature support Unit 9 make cryogenic probe 8 and low temperature choose brilliant platform 4 to be reduced to design temperature.By easy-weathering monocrystalline Sample moves into low temperature and chooses brilliant platform 4, and fine setting light microscope focal length makes crystal clearly be amplified on display screen, then with choosing brilliant work Tool completes the washing of single crystal samples, cuts, a preferable crystal picked out, finally by the low of single crystal diffractometer at low temperature The crystal of select is rapidly arranged on and carried on brilliant platform by temperature probe.Low temperature support Unit 9 is closed, low temperature is chosen into brilliant platform 4 branch Frame moves 3 and arrives the right flank of angular instrument 2.Close single crystal diffractometer glass door, cryogenic collector crystal data.

Claims (2)

1.X- ray single crystal diffraction instrument easy-weathering crystal cryo-microscope loading systems, including angular instrument (2) and cryogenic probe (8), It is characterized in that the loading system also chooses brilliant platform (4), micro-imaging unit and low temperature support Unit (9) including low temperature, it is described to survey It is provided with directly over angle instrument (2) and chooses crystalline substance with its hollow low temperature of matrix for being connected and being located at immediately below cryogenic probe (8) by support (3) Platform (4), the low temperature chooses brilliant platform (4) and passes sequentially through coolant import and export, coolant pipeline set by its side with being located at single crystal diffraction The outside low temperature support Unit (9) of instrument (1) is connected;The micro-imaging unit include industrial camera (6), display screen (7) and Light microscope (5), display screen (7) and light microscope (5) are connected with industrial camera (6).
2. cryo-microscope loading system as claimed in claim 1, it is characterised in that the low temperature support Unit (9) is low temperature cold But liquid circulating pump or certainly supercharging liquid nitrogen container.
CN201720239861.4U 2017-03-13 2017-03-13 X ray single crystal diffraction instrument easy-weathering crystal cryo-microscope loading systems Active CN206601348U (en)

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CN201720239861.4U CN206601348U (en) 2017-03-13 2017-03-13 X ray single crystal diffraction instrument easy-weathering crystal cryo-microscope loading systems

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108572185A (en) * 2017-03-13 2018-09-25 中国科学院兰州化学物理研究所 X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading system

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108572185A (en) * 2017-03-13 2018-09-25 中国科学院兰州化学物理研究所 X-ray single crystal diffractometer easy-weathering crystal cryo-microscope loading system

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