CN106596607B - A kind of diffractometer of energy accurately measure albumin crystal data - Google Patents

A kind of diffractometer of energy accurately measure albumin crystal data Download PDF

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Publication number
CN106596607B
CN106596607B CN201611249140.8A CN201611249140A CN106596607B CN 106596607 B CN106596607 B CN 106596607B CN 201611249140 A CN201611249140 A CN 201611249140A CN 106596607 B CN106596607 B CN 106596607B
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induction pieces
diffractometer
sample
sensor
gasket
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CN106596607A (en
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杨利峰
汪启胜
崔莹
何建华
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Shanghai Institute of Applied Physics of CAS
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Shanghai Institute of Applied Physics of CAS
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/20Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by using diffraction of the radiation by the materials, e.g. for investigating crystal structure; by using scattering of the radiation by the materials, e.g. for investigating non-crystalline materials; by using reflection of the radiation by the materials
    • G01N23/20008Constructional details of analysers, e.g. characterised by X-ray source, detector or optical system; Accessories therefor; Preparing specimens therefor

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  • Chemical & Material Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Analysing Materials By The Use Of Radiation (AREA)

Abstract

The invention discloses a kind of diffractometers of energy accurately measure albumin crystal data, including X-ray generator, X-ray detection device and control device, the X-ray detection device includes the Angle measurement for being equipped with sample, it is characterised in that: the Angle measurement is equipped with the pressure sensitive unit for perceiving the pressure change being applied on sample to be tested.The present invention can quantitatively monitor the stability of diffractometer, exclude influence of the stability of diffractometer to sample analysis data, structure is simple, high sensitivity, and measurement data is more accurate.

Description

A kind of diffractometer of energy accurately measure albumin crystal data
Technical field
The invention belongs to X-ray diffractometer fields, more particularly, to a kind of energy accurately measure albumin crystal data Diffractometer.
Background technique
X-ray diffraction measurement is to identify the important means of large biological molecule phase structure.Usual high-precision experimental data obtains The light source, the albumin crystal sample of high quality and the diffractometer of high stability that must need high stability, if there is diffraction data Undesirable situation, it may be possible to which light is shaken, it may be possible to which albumin crystal sample property is bad, it is also possible to be sample It is shaken, the shaking of sample is it could also be possible that the shaking on ground leads to its stability of the effect of jitter of diffractometer.In order to arrange Except the unstability of diffractometer is influenced to diffraction data bring, the unstability of quantitative observation diffractometer, judgement sample are needed Situation on diffractometer, it is undesirable to attempt solution diffractometer stability bring data.And current diffractometer on the market Lack the quantitative Method and kit for for monitoring its stability in real time.
Summary of the invention
For overcome the deficiencies in the prior art, the present invention provides a kind of introduce and carries out real-time quantitative to the stability of diffractometer Monitoring, measurement data more accurately can accurately measure albumin crystal data diffractometer.
The technical solution adopted by the present invention to solve the technical problems is: a kind of energy accurately measure albumin crystal data Diffractometer, including X-ray generator, X-ray detection device and control device, the X-ray detection device includes installation There is the Angle measurement of sample, the Angle measurement is equipped with the pressure sensing list for perceiving the pressure change being applied on sample to be tested Member.The stability of sample, and then the stabilization of Quantitative Monitoring diffractometer can be quantitatively monitored by the setting of pressure sensitive unit Property, exclude the unstable of diffractometer influences to diffraction patterns bring, so that the data analysis to albumin crystal is more accurate.
Further, the pressure sensitive unit includes the attachment base that can be connected with detection device, for placing to test sample The placement portion of product, the inductive component that electric signal is converted into for incuding deformation caused by pressure change in placement portion and by deformation And the display device for converting the electrical signal to digital signal.
Further, the inductive component include induction pieces, the sensor on induction pieces, be connected with placement portion it is upper Connector and the lower connector being connected with attachment base.
Further, the induction pieces are equipped with the thinner wall section for promoting its adaptability to changes.The setting of thinner wall section is so that sense The strain property for answering part more preferably, can also generate biggish deformation when by lesser power, and sensitivity is higher, and final data is more Precisely.
Further, the sensor is resistance strain gage.
Further, the thinner wall section is located at the face position of sensor, and thinner wall section is equipped with to be set through induction pieces side wall The through-hole set.
Further, the through-hole is made of the circular opening that three horizontal cross overlap, wherein intermediate circle Perforated area is less than the circular opening area on both sides.The ingenious setting of three circular openings incudes induction pieces preferably Stress variation, pressure varies slightly after the thickness of induction pieces is reduced can pass through the present display device of sensor body well On, and the superposition of circular opening sensitivity for other shapes is more preferable, pressure slight change just passes through circular opening side The distortion of edge allow sensor more rapidly, more accurately embody deformation quantity.
Further, be equipped with the first gasket between the upper connector and induction pieces, the induction pieces and lower connector it Between be equipped with the second gasket, the cross-sectional area of first gasket and the second gasket is equal.The shape of first gasket and the second gasket Size is identical, so that the forced area of induction pieces concentrates on the first gasket and the second gasket, applies so as to preferably incude It is added in the pressure size of induction pieces two sides, and pressure size is embodied a concentrated reflection of on induction pieces, display is sent to by sensor The data of device are more accurate.
Further, the upper connector is equipped with the accommodation groove deviated in a certain range for induction pieces.Effectively avoid Induction pieces contact the inaccuracy for leading to test data with upper connector.
Further, the upper connector is equipped with the accommodating chamber for accommodating sensor.Avoid upper connector and induction Part generate in addition to the first gasket with for contact surface.
The beneficial effects of the present invention are: breaking through Traditional Thinking, increase a dimension to the analysis of diffraction image, in diffractometer Detection device on pressure sensitive unit for perceiving sample stability is set, and then quantitatively monitor the stabilization of diffractometer Property, influence of the stability of diffractometer to sample analysis data is excluded, structure is simple, high sensitivity, and measurement data is more accurate.
Detailed description of the invention
Fig. 1 is the structural schematic diagram one of pressure sensitive unit in the present invention.
Fig. 2 is the structural schematic diagram two of pressure sensitive unit in the present invention.
Fig. 3 is the structural schematic diagram three of pressure sensitive unit in the present invention.
Fig. 4 is the fit structure schematic diagram of lower connector and induction pieces.
Fig. 5 is the stress condition schematic diagram of induction pieces.
Fig. 6 is the fit structure schematic diagram of part-structure and light source of the invention.
Fig. 7 is the part-structure rough schematic of diffractometer.
Specific embodiment
In order to make those skilled in the art better understand the present invention program, below in conjunction in the embodiment of the present invention Attached drawing carries out clear, complete description to the technical solution in inventive embodiments, it is clear that described embodiment is only this A part of the embodiment of invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art Every other embodiment obtained without making creative work, should fall within the scope of the present invention.
Referring to Fig.1 shown in -7, a kind of diffractometer of energy accurately measure albumin crystal data, including X-ray are filled 4, control device and X-ray detection device 5 are set, X-ray detection device 5 includes the Angle measurement 51 for being equipped with sample, Angle measurement 51 It is equipped with pressure sensitive unit.Pressure sensitive unit successively includes the attachment base 1 being connected with X-ray detection device, for putting Set the placement portion 3 of testing protein crystal prototype, for incuding deformation caused by pressure change in placement portion 3 and converting deformation At the inductive component of electric signal and the display device for converting the electrical signal to digital signal and being displayed on the screen.
Placement portion 3 includes that needle tubing 31 is adsorbed company for the needle tubing 31 of adhesion testing protein crystal prototype, by magnetic part The upper segment body 32 connect and the lower segment body 34 being detachably connected on by knob 33 on upper connector 23.Knob 33 is equipped with interior spiral shell Line, upper connector 23 are equipped with the protrusion that be adapted to knob 33, and protrusion equipped with external screw thread, first place lower segment body 34 by when assembly Above protrusion, knob 33 passes through lower segment body 34 and is set in rotation threaded connection on the outside of protrusion.In order to mitigate whole weight, pacify It sets portion 3 to be made of aluminum material, improves whole sensitivity.Upper segment body 32 can be hollow structure, on the side of lower segment body 34 Offer the through slot 341 passed through for optical fiber.
Inductive component includes the lower connector 24 being connected with attachment base 1, the induction pieces 21 being connected with lower connector 24, setting In the sensor 22 on induction pieces 21 and the upper connector 23 being arranged in above induction pieces 21.Induction pieces 21 are in rectangular parallelepiped structure, It is fixedly connected with sensor 22 on induction pieces 21, the appearance for accommodating sensor 22 is offered on upper connector 23 cylindrical Receive chamber 232, specifically, accommodating chamber 232 is the circular groove for being provided with 23 lower surface of upper connector, the center of circle of the circular groove with The center of upper connector 23 essentially coincides.In this present embodiment, sensor 22 includes resistance strain gage and is used for resistance-strain Piece is fixedly connected on the silica gel on induction pieces 21, and the upper surface center of induction pieces 21 passes through the connected resistance strain gage of silica gel, resistance The lead of foil gauge is connected by conducting wire 221 with display device.In order to improve the adaptability to changes of sensor, induction pieces 21 and sensing The face position of device 22 is equipped with thinner wall section, specifically, the center position in induction pieces 21 opens up through-hole 211, through-hole 211 is passed through The side wall setting of induction pieces 21 is worn, and through-hole 211 is made of three circular openings on same straight line, three circular openings Juxtaposition setting, the circular opening cross-sectional area positioned at both sides it is equal and be greater than be located in the middle circular opening cross-sectional area.
The left end of 21 upper surface of induction pieces is in contact with upper connector 23 by the first gasket 251 and is connect, induction pieces The right-hand end of 21 lower surfaces is in contact with lower connector 24 by the second gasket 252 and is connect, in order to guarantee 23 He of upper connector The conduction surface that lower connector 24 is applied to the power on induction pieces 21 is equal, the cross section of the first gasket 251 and the second gasket 252 Shape, size are identical, i.e. the forced area of about 21 two sides of induction pieces is equal.In order to avoid the right-hand end of 21 upper surface of induction pieces Portion is in contact with upper connector 23, an accommodation groove 231 is formed at the lower surface edge of upper connector 23, thus even if induction pieces 21 It shifts in a certain range, also can guarantee that the right side upper surface of induction pieces 21 will not contact upper connector 23, to induction pieces 21 deformation will not have an impact, and final data measurement is more accurate.Lower connector 24 is in curved kidney-shaped structure, by passing through The mounting hole for putting on lower wall is connected on attachment base 1, for the other of X-ray detection device at the intermediate recess of lower connector 24 Component passes through.
Display device (not shown) is electrically connected by conducting wire 221 with inductive component, and display device will produce on induction pieces 21 Raw deformation is converted into electric signal by sensor, and electric signal is converted into digital signal by converter, and digital signal can lead to It crosses display screen to show, convenient for intuitively reading the pressure being applied in placement portion 3.Digital signal passes through human-computer interaction interface simultaneously Real-time display, all data storages on computers, are called convenient for later.
The working principle of the invention is: pressure sensitive unit is connected to the angle measurement of X-ray detection device by attachment base Head, due to gravity, placement portion and upper connector pass through the first gasket and generate a power horizontally to the right, lower company to induction pieces Fitting generates the power of a level to the left to induction pieces by the second gasket, and induction pieces generate certain deformation and are embodied in display dress It sets, original state resets display device, when sample to be tested is placed in placement portion, due to being applied to the first gasket and second Power on gasket changes, and induction pieces generate more deformation, and deformation is converted into electric signal and passes through wire transmission extremely by sensor Display device, display device convert electrical signals into digital signal, and experimenter can be convenient, intuitively read on inductive component Pressure change data.
When sample is placed upper placement portion, the instantaneous pressure value that is read in display device relative to original state occur compared with Big to change, when sample is removed placement portion, relative to original state larger change occurs for the instantaneous pressure value read in display device Become, when analyzing sample, the pressure value read in display device is in more stable state, under normal condition, will not produce Raw biggish fluctuation.
If transfer the data stored on computer it was found that diffraction image is bad, if it find that pressure value in addition to setting-out and It is fluctuated when sampling, is constantly in more stable state, illustrated that the stability of sample is preferable, further relate to the stabilization of diffractometer The problem of property is preferable, eliminates diffractometer;If data show that diffraction image is bad, pressure value also generates biggish wave It is dynamic, illustrate that the stability of sample is bad, it may be possible to which the de-stabilising effect of diffractometer diffraction image can exclude asking for light source etc. Topic causes diffraction image bad.So as to judge being associated between the stability of diffractometer and sample diffraction image.
Above-mentioned specific embodiment is used to illustrate the present invention, rather than limits the invention, of the invention In spirit and scope of protection of the claims, to any modifications and changes that the present invention makes, protection model of the invention is both fallen within It encloses.

Claims (8)

1. a kind of diffractometer of energy accurately measure albumin crystal data, including X-ray generator (4), X-ray detection dress (5) and control device are set, the X-ray detection device (5) includes the Angle measurement (51) for being equipped with sample, it is characterised in that: institute It states Angle measurement (51) and is equipped with the pressure sensitive unit for being used for perceiving the pressure change being applied on sample to be tested;The pressure passes Sense unit includes the attachment base (1) that can be connected with detection device, the placement portion (3) for placing sample to be tested, for incuding peace It sets deformation caused by pressure change on portion (3) and deformation is converted into the inductive component of electric signal and is used to turn electric signal Change the display device of digital signal into;The inductive component includes induction pieces (21), the sensor on induction pieces (21) (22), the upper connector (23) being connected with placement portion (3) and the lower connector (24) being connected with attachment base (1).
2. diffractometer according to claim 1, it is characterised in that: the induction pieces (21) are equipped with for promoting its strain The thinner wall section of power.
3. diffractometer according to claim 1, it is characterised in that: the sensor (22) is resistance strain gage.
4. diffractometer according to claim 2, it is characterised in that: the thinner wall section is located at the positive contraposition of sensor (22) It sets, thinner wall section is equipped with the through-hole (211) through the setting of induction pieces (21) side wall.
5. diffractometer according to claim 4, it is characterised in that: the through-hole (211) is set by three horizontal cross overlappings The circular opening composition set, wherein intermediate circular opening area is less than the circular opening area on both sides.
6. diffractometer according to claim 1, it is characterised in that: set between the upper connector (23) and induction pieces (21) Have the first gasket (251), is equipped with the second gasket (252) between the induction pieces (21) and lower connector (24), first pad The cross-sectional area of piece (251) and the second gasket (252) is equal.
7. diffractometer according to claim 6, it is characterised in that: the upper connector (23) is equipped with for induction pieces (21) The accommodation groove (231) deviated in a certain range.
8. diffractometer according to claim 6, it is characterised in that: the upper connector (23) is equipped with to be passed for accommodating The accommodating chamber (232) of sensor.
CN201611249140.8A 2016-12-29 2016-12-29 A kind of diffractometer of energy accurately measure albumin crystal data Active CN106596607B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0875678A (en) * 1994-09-01 1996-03-22 Mac Sci:Kk Quadruple shaft-type automatic diffraction apparatus
US7796726B1 (en) * 2006-02-14 2010-09-14 University Of Maryland, Baltimore County Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation
CN102435626A (en) * 2011-09-13 2012-05-02 丹东通达科技有限公司 Table type X-ray diffractometer
CN205229075U (en) * 2015-11-12 2016-05-11 中国科学院上海应用物理研究所 Response recognition device of protein crystal sample acquisition loop base

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0875678A (en) * 1994-09-01 1996-03-22 Mac Sci:Kk Quadruple shaft-type automatic diffraction apparatus
US7796726B1 (en) * 2006-02-14 2010-09-14 University Of Maryland, Baltimore County Instrument and method for X-ray diffraction, fluorescence, and crystal texture analysis without sample preparation
CN102435626A (en) * 2011-09-13 2012-05-02 丹东通达科技有限公司 Table type X-ray diffractometer
CN205229075U (en) * 2015-11-12 2016-05-11 中国科学院上海应用物理研究所 Response recognition device of protein crystal sample acquisition loop base

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