CN103940836A - Liquid X ray scattering sample cell - Google Patents
Liquid X ray scattering sample cell Download PDFInfo
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- CN103940836A CN103940836A CN201310023004.7A CN201310023004A CN103940836A CN 103940836 A CN103940836 A CN 103940836A CN 201310023004 A CN201310023004 A CN 201310023004A CN 103940836 A CN103940836 A CN 103940836A
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Abstract
The invention relates to a liquid X ray scattering sample cell. The liquid X ray scattering sample cell comprises a cell body provided with a cavity and a sample cell which is arranged inside the cell body and is open at the top. The cell body is internally provided with a separating plate, and a water inlet pipe and a water outlet pipe are respectively arranged at the two sides of the separating plate; and a mounting shaft is arranged on the side wall of the cell body, and the mounting shaft is connected with a diffractometer side angle head. The liquid X ray scattering sample cell can be applied to a synchrotron radiation X ray multicircle diffractometer experimental facility and also can meet the requirement of a portable temperature control liquid sample cell of a diffractometer in a laboratory, so that the problems that a liquid sample cannot be filled, the temperature is controlled and the liquid sample is convenient to carry when structural information of liquid is measured by adopting an X ray reflection method are solved; and the application range of a powder diffractometer in the research field of solution structures is expanded, and a necessary experiment foundation is laid for carrying out solution X ray scattering new method study.
Description
Technical field
The present invention relates to the scattering experiment technical field of liquid structure, relate in particular to liquid X ray scattering sample cell.
Background technology
The unordered architectural feature of long-range because liquid has shortrange order.Therefore, its structure measurement not only will be by means of modern diffraction experiment technology but also will be in conjunction with microcomputer data processing.By experiment, directly on the basis of acquisition structural information, by theoretical model, calculating the forest spatial structure parameters such as bond distance, coordination number, bond angle that provide first and second coordination shell.Solution structure parameter and radial distribution function are not only development crystal model and the radial distribution function model two requisite bases of large class solution theory, and are that polywater salt system balances each other and is situated between the important foundation of research, solution macroscopic thermodynamics character of surely balancing each other.Synchrotron radiation light source brightness is large, stability is high, high directivity, collimation are good, is that liquid-scattering is tested optimal light source, and the brightness that just overcomes laboratory diffractometer is low, poor stability, the shortcoming such as directivity is low, and diversity is strong, time-consuming.Synchrotron radiation EXAFS general Study is compared with the partial structurtes of thick atom ordinal number system, and the one-piece construction of SR scattering method research is subject to atomic number restriction less.For the biological and vital life water of medical science with learn over the ground significant natural water as seawater and salt lake, the lucky and EXAFS mutual supplement with each other's advantages of scattering method.Certainly, the exploitation of synchrotron radiation new method, is the key point of liquid structure research.
At present, the X ray scattering method of liquid structure is the important experimental technique that directly obtains structural information, not only can measure the structural informations such as bond distance, coordination number, bond angle and steric configuration of the first coordination shell, and can obtain the structural information beyond the first coordination shell.The develop rapidly of the seventies computer technology and scattering experiment technology and application, just make the scattering experiment research of liquid structure become a reality.Up to now, θ-2 θ type the angular instruments (vertical or horizontal) due to no matter, or the sample cell of many circle diffractometers configuration can only meet solid state powder sample surfaces diffraction, and cannot realize, has the liquid of mobility in the scatterometry of different specific temperature conditions.Although and θ-θ type diffractometer can carry out Free Surface scattering experiment, liquid evaporation changes solution concentration and even causes crystallization, or reacts with air.
The sample cell that X-ray diffractometer is subsidiary, can only meet the diffraction experiment of solid sample.Imitate the liquid sample pool of this sample cell processing, although can cover the film that some X ray are transparent, can contain fluid sample, but the scattering strength that cannot obtain the most frequently used reflection method for measuring due to its shape, size, size especially thickness does not belong to maximum scattering intensity, correct absorption correction can not be carried out, accurately radial distribution function cannot be obtained.If adopt not too conventional transmission beam method, absorption correction does not generally have problems, and is only applicable to the sample of the special low absorption coefficient of minority, but is not suitable for the sample of most higher absorption coefficients.The fluid sample of transmission beam method and film absorb very large to X ray, the scattering strength of detector measurement will meet statistical counting error 1%, and the data acquisition time needing is longer, and the time of even measuring a fluid sample needs one week.Height is absorbed to sample, and transmission beam method does not collect scattering strength.
Adopt in addition cylindrical geometry to learn and measure liquid structure, only have source of parallel light could obtain good scattering data.And common diffractometer light source strictly belongs to divergent light source in fact, the liquid-scattering of measurement is generally difficult to obtain accurately radial distribution function.
Single angle holding from the scattering experiment sample of liquid, also has the method that adopts kapillary contain fluid abroad, be only confined to not to be subject to solubleness affect with normal temperature under the fluid sample measured.
Because existing all X-ray diffractometers be not both equipped with the sample cell of liquid measure, corresponding liquid measure program and data processing software are not installed yet.Therefore the present invention is on the basis of powdery diffractometry, the exploitation to existing diffractometer function.
Summary of the invention
Technical matters to be solved by this invention be to provide a kind ofly facilitate that liquid sample holds, temperature control and the liquid X ray scattering sample cell that carries.
For addressing the above problem, liquid X ray scattering sample cell of the present invention, is characterized in that: it comprises and is provided with the pond body of cavity and is located at the open-topped sample cell in the body of described pond; In the body of described pond, be provided with dividing plate, the both sides of this dividing plate are respectively equipped with water inlet pipe, rising pipe; Described pond body sidewall is provided with installation shaft, and this installation shaft is connected with diffractometer side angle head.
In described water inlet pipe and described rising pipe, be equipped with temperature probe, this temperature probe is connected with miniature electronic temperature-controlling system.
The volume of described sample cell is 15 ~ 25 mL, and its top covers Mylar film or the beryllium window that X ray transmissivity is 60 ~ 90%.
The thickness of described Mylar film is 4 ~ 8 μ m.
The thickness of described beryllium window is 0.05 ~ 0.15mm.
The present invention compared with prior art has the following advantages:
1,, because the present invention is provided with Mylar film or beryllium window at sample cell top, therefore, the θ-θ type diffractometer for sample cell horizontal positioned, can effectively prevent the evaporation of liquid and reacting of may occurring with air, is especially applicable to supersaturated solution.
2,, owing to being provided with the temperature probe being connected with miniature electronic temperature-controlling system in the present invention, therefore, can conveniently realize the thermostatic control of fluid sample.
3, the kapillary sample cell method of successively reporting with at present external Synchrotron Radiation and cylinder liquid gunite, the flat samples pond transmission beam method that is only applicable to normal temperature and pressure measurement are compared, the present invention has advantages of that Pool body design shape, size dimension and diffractometer geometry are identical, therefore, can obtain maximum scattering strength, thereby effectively shorten Measuring Time.Meanwhile, easily carry out absorption correction and the polarization recovery of fluid sample, can obtain to more accurate radial distribution function under fixed temperature.
4, because its top in the present invention covers Mylar film or beryllium window, the desirable arbitrary orientation of sample cell window and angular turn, liquid all can not flow out.Therefore, both can be used for synchrotron radiation X-ray and justified different angular instrument (the vertical or horizontal) experimental provisions of diffractometer more, and can meet the Portable temperature-controlling liquid sample pool of the different angular instruments of laboratory diffractometer (vertical or horizontal), thereby when having solved X ray reflection method and measuring liquid structure information, liquid sample cannot hold, temperature control and the problem such as be convenient for carrying.Expand powder diffractometer in the range of application of solution structure research field simultaneously, carry out the research of solution X ray scattering new method and established necessary experiment basis.
5, the present invention is simple in structure, with low cost, belongs to the exploitation to laboratory two circles and synchronous conventional many circle diffractometer functions, is not only applicable to low absorption fluid sample, and the sample of applicable high absorption coefficient; As electrolyte aqueous solution, nonelectrolyte aqueous solution, non-aqueous electrolytic solution etc., comprising amino acid solution and protein aqueous solution etc.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is structural representation of the present invention.
Fig. 2 is side view of the present invention.
Fig. 3 is vertical view of the present invention.
In figure: the body 2-sample cell 3-dividing plate 4-water inlet pipe 5-rising pipe 6-installation shaft of 1-pond.
Embodiment
As shown in Figure 1, liquid X ray scattering sample cell, it comprises and is provided with the pond body 1 of cavity and is located at the open-topped sample cell 2 in pond body 1.In pond body 1, be provided with dividing plate 3, the both sides of this dividing plate 3 are respectively equipped with water inlet pipe 4, rising pipe 5; Body 1 sidewall in pond is provided with installation shaft 6, and this installation shaft 6 is connected with diffractometer side angle head.
Wherein: in water inlet pipe 4 and rising pipe 5, be equipped with temperature probe, this temperature probe is connected with miniature electronic temperature-controlling system.
The volume of sample cell 2 is 15 ~ 25 mL, and its top covers Mylar film or the beryllium window that X ray transmissivity is 60 ~ 90%.
The thickness of Mylar film is 4 ~ 8 μ m.The thickness of beryllium window is 0.05 ~ 0.15mm.
Claims (5)
1. liquid X ray scattering sample cell, is characterized in that: it comprises and is provided with the pond body (1) of cavity and is located at the open-topped sample cell (2) in described pond body (1); In described pond body (1), be provided with dividing plate (3), the both sides of this dividing plate (3) are respectively equipped with water inlet pipe (4), rising pipe (5); Described pond body (1) sidewall is provided with installation shaft (6), and this installation shaft (6) is connected with diffractometer side angle head.
2. liquid X ray scattering sample cell as claimed in claim 1, is characterized in that: in described water inlet pipe (4) and described rising pipe (5), be equipped with temperature probe, this temperature probe is connected with miniature electronic temperature-controlling system.
3. liquid X ray scattering sample cell as claimed in claim 1, is characterized in that: the volume of described sample cell (2) is 15 ~ 25 mL, and its top covers Mylar film or the beryllium window that X ray transmissivity is 60 ~ 90%.
4. liquid X ray scattering sample cell as claimed in claim 3, is characterized in that: the thickness of described Mylar film is 4 ~ 8 μ m.
5. liquid X ray scattering sample cell as claimed in claim 3, is characterized in that: the thickness of described beryllium window is 0.05 ~ 0.15mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310023004.7A CN103940836A (en) | 2013-01-22 | 2013-01-22 | Liquid X ray scattering sample cell |
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| CN201310023004.7A CN103940836A (en) | 2013-01-22 | 2013-01-22 | Liquid X ray scattering sample cell |
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| CN103940836A true CN103940836A (en) | 2014-07-23 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124531A (en) * | 2016-06-29 | 2016-11-16 | 浙江泰克松德能源科技有限公司 | The shuttle detected for X and gamma-ray spectroscopy instrument |
| CN107034262A (en) * | 2017-04-10 | 2017-08-11 | 中国科学院上海应用物理研究所 | A kind of X ray genetic marker probes based on synchronous light source and preparation method thereof and application |
| CN107357329A (en) * | 2017-07-14 | 2017-11-17 | 河北工业大学 | A kind of temperature regulating device for liquid-scattering measurement |
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2013
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106124531A (en) * | 2016-06-29 | 2016-11-16 | 浙江泰克松德能源科技有限公司 | The shuttle detected for X and gamma-ray spectroscopy instrument |
| CN107034262A (en) * | 2017-04-10 | 2017-08-11 | 中国科学院上海应用物理研究所 | A kind of X ray genetic marker probes based on synchronous light source and preparation method thereof and application |
| CN107034262B (en) * | 2017-04-10 | 2020-01-03 | 中国科学院上海应用物理研究所 | X-ray genetic marker probe based on synchronous light source and preparation method and application thereof |
| CN107357329A (en) * | 2017-07-14 | 2017-11-17 | 河北工业大学 | A kind of temperature regulating device for liquid-scattering measurement |
| CN107357329B (en) * | 2017-07-14 | 2022-07-26 | 河北工业大学 | Temperature control device for liquid scattering measurement |
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