CN106841253B - A kind of compound diffractometer of energy accurately measure albumin crystal data - Google Patents

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

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Publication number
CN106841253B
CN106841253B CN201611249150.1A CN201611249150A CN106841253B CN 106841253 B CN106841253 B CN 106841253B CN 201611249150 A CN201611249150 A CN 201611249150A CN 106841253 B CN106841253 B CN 106841253B
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compound
diffractometer
sample
induction pieces
gasket
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CN106841253A (en
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杨利峰
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
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/05Investigating materials by wave or particle radiation by diffraction, scatter or reflection
    • G01N2223/056Investigating materials by wave or particle radiation by diffraction, scatter or reflection diffraction
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/10Different kinds of radiation or particles
    • G01N2223/101Different kinds of radiation or particles electromagnetic radiation
    • G01N2223/1016X-ray
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2223/00Investigating materials by wave or particle radiation
    • G01N2223/60Specific applications or type of materials
    • G01N2223/612Specific applications or type of materials biological material

Abstract

The invention discloses a kind of compound diffractometers of energy accurately measure albumin crystal data, 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 not only judge the presence or absence of sample to be tested, and 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 compound 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 Compound 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 It must need the light source, the albumin crystal sample of high quality and the diffractometer of high stability of high stability.Since experimental implementation is made mistakes, It will appear albumin crystal sample not when on Angle measurement also by generation the case where step progress diffraction analysis, waste time energy, Testing efficiency is low, it is therefore desirable to which one carries out a pre- judgement to whether sample to be tested is in target position before testing.
When being tested, if there is the undesirable situation of diffraction data, it may be possible to which light is shaken, it may be possible to Albumin crystal sample property is bad, it is also possible to be that sample is shaken, the shaking of sample it could also be possible that ground shaking Lead to its stability of the effect of jitter of diffractometer.It influences, needs to diffraction data bring in order to exclude the unstability of diffractometer Want the unstability of quantitative observation diffractometer, situation of the judgement sample on diffractometer, to attempt to solve diffractometer stability band The data come are undesirable.And diffractometer on the market lacks the quantitative Method and kit for for monitoring its stability in real time at present.
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 compound diffractometer.
The technical solution adopted by the present invention to solve the technical problems is: a kind of energy accurately measure albumin crystal data Compound diffractometer, including X-ray generator, X-ray detection device, control device and data processing equipment, the X penetrate Line detection device includes the Angle measurement for being equipped with sample, and the Angle measurement is equipped with the optoelectronic induction list for incuding sample to be tested Member and the pressure sensitive unit for perceiving the pressure change being applied on sample to be tested.The number that optoelectronic induction unit will measure According to optical signal is converted into, then convert optical signals into electric signal by photoelectric cell, with reach judge sample to be tested whether position In target position, i.e., it whether there is the purpose of sample to be tested on angular instrument;It can be quantitatively by the setting of pressure sensitive unit The stability of sample, and then the stability of Quantitative Monitoring diffractometer are monitored, the unstable of diffractometer is excluded and is brought to diffraction patterns Influence so that more accurate to the analysis of the data of albumin crystal.
Further, the pressure sensitive unit include the attachment base that can be connected with X-ray detection device, for place to The placement portion of sample, the induction that electric signal is converted into for incuding deformation caused by pressure change in placement portion and by deformation Component and 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 placement portion is equipped with the through slot being adapted to optoelectronic induction unit.
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 X-ray detection device on pressure sensitive unit for perceiving sample stability is set, and then not only may determine that test sample The presence or absence of product can also quantitatively monitor the stability of diffractometer, exclude shadow of the stability to sample analysis data of diffractometer It rings, 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 compound diffractometer of energy accurately measure albumin crystal data, including X-ray Generating device 4, control device, X-ray detection device 5 and data processing equipment, X-ray detection device 5 include being equipped with sample Angle measurement 51, Angle measurement 51 be equipped with optoelectronic induction unit and pressure sensitive unit.Pressure sensitive unit successively includes penetrating with X The attachment base 1 that line detection device is connected, the placement portion 3 for placing testing protein crystal prototype, for incuding placement portion 3 Deformation is simultaneously converted into the inductive component of electric signal and is used to convert the electrical signal to digital letter by deformation caused by pressure change Number and the display device that is 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.
Optoelectronic induction unit includes light source, optical path and photoelectric cell, and upper segment body 32 can be hollow structure, and center has For the through-hole that light passes through, the through slot 341 passed through for photoelectric cell etc. is offered on the side of lower segment body 34.Optoelectronic induction unit Can be by whether being judged across sample to be tested to light source, and measurement result is converted into optical signal, then by photo elements Part converts optical signals into electric signal, conducts to control device and the data processing equipment being electrically connected with control device, so as to intuitive Judge whether sample to be tested is in suitable position.Optoelectronic induction unit and pressure sensitive unit can be electric with control device respectively Even, after optoelectronic induction unit senses the presence of sample to be tested, control device sends signal, starting to pressure sensitive unit Pressure sensitive unit works.
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: whether optoelectronic induction unit is located at X-ray detection device to sample to be tested first The suitable position of Angle measurement judges, and after obtaining result existing for sample to be tested, pressure sensitive unit is passed through attachment base It is connected to the Angle measurement of X-ray detection device, due to gravity, placement portion and upper connector pass through the first gasket to induction pieces A power horizontally to the right is generated, lower connector generates the power of a level to the left, induction pieces to induction pieces by the second gasket It generates certain deformation and is embodied in display device, original state resets display device, sample to be tested is placed in placement portion When, since the power being applied on the first gasket and the second gasket changes, induction pieces generate more deformation, and sensor is by deformation Electric signal is converted by wire transmission to display device, display device converts electrical signals into digital signal, and experimenter can be with Conveniently, the pressure change data on inductive component are intuitively read.
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 compound diffractometer of energy accurately measure albumin crystal data, including X-ray generator (4), X-ray Detection device (5), control device and data processing equipment, the X-ray detection device (5) includes the Angle measurement for being equipped with sample (51), it is characterised in that: (51) are equipped with for incuding the optoelectronic induction unit of sample to be tested and for perceiving on the Angle measurement It is applied to the pressure sensitive unit of the pressure change on sample to be tested;The pressure sensitive unit includes that can fill with X-ray detection Set connected attachment base (1), the placement portion (3) for placing sample to be tested, for incuding pressure change institute on placement portion (3) Deformation is simultaneously converted into the inductive component of electric signal and is used to convert the electrical signal to the display dress of digital signal by the deformation of generation It sets;The inductive component includes induction pieces (21), the sensor (22) being set on induction pieces (21), is connected with placement portion (3) Upper connector (23) and the lower connector (24) being connected with attachment base (1).
2. compound diffractometer according to claim 1, it is characterised in that: the induction pieces (21) are equipped with for being promoted The thinner wall section of its adaptability to changes.
3. compound diffractometer according to claim 1, it is characterised in that: the sensor (22) is resistance strain gage.
4. compound diffractometer according to claim 2, it is characterised in that: the thinner wall section is being located at sensor (22) just To position, thinner wall section is equipped with the through-hole (211) through the setting of induction pieces (21) side wall.
5. compound diffractometer according to claim 4, it is characterised in that: the through-hole (211) is by three horizontal cross The circular opening composition overlapped, wherein intermediate circular opening area is less than the circular opening area on both sides.
6. compound diffractometer according to claim 4, it is characterised in that: the upper connector (23) and the induction pieces (21) the first gasket (251) are equipped between, the second gasket is equipped between the induction pieces (21) and the lower connector (24) (252), the cross-sectional area of first gasket (251) and the second gasket (252) is equal.
7. compound diffractometer according to claim 6, it is characterised in that: the upper connector (23) is equipped with for induction The accommodation groove (231) that part (21) deviates in a certain range.
8. compound diffractometer according to claim 1, it is characterised in that: the placement portion (3) is equipped with and light inductance The through slot (341) for answering unit to be adapted to.
CN201611249150.1A 2016-12-29 2016-12-29 A kind of compound diffractometer of energy accurately measure albumin crystal data Active CN106841253B (en)

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Citations (5)

* 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
CN101490537A (en) * 2006-05-09 2009-07-22 马自达公司 Automated analyzer using light diffraction
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 (5)

* 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
CN101490537A (en) * 2006-05-09 2009-07-22 马自达公司 Automated analyzer using light diffraction
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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