JP2008096330A - Capillary rotation apparatus, x-ray diffraction apparatus using the same, and raman spectrometry analyzer - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a capillary rotation apparatus capable of readily reducing the deflections of capillaries. <P>SOLUTION: The capillary rotation apparatus 10 is provided with a first guide member 11, a second guide member 12, a third guide member 13, and a rotation support mechanism 14, sequentially arranged starting from the side of a tip part of a capillary C to the side of its rear end part. The rotation support mechanism operates, in such a way as to support the rear-end part of the capillary and rotate the capillary in the axial direction. Recessed grooves of the first and third guide members are arranged on the same surface side of the capillary, and a recessed groove of the second guide member is arranged on the opposite surface side. When the capillary is rotated in the axial direction, at least by the rotation support mechanism, the clearance between the recessed grooves of the first and second guide members is set substantially at the same clearance as that of the outer diameter of the capillary, and the recessed groove of the third guide member is positioned, in such a way that the capillary is pressed against the side of the recessed groove of the second guide member by the recessed groove of the third guide member. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a capillary rotation device used as a container for containing a substance when the substance is analyzed (for example, analyzing a crystal form of a compound) by an X-ray diffractometer or a Raman spectroscopic analyzer, and the like. More particularly, the present invention relates to a capillary rotation device that can easily suppress rotational shake of the capillary that causes a reduction in analysis accuracy, and an X-ray diffraction device and Raman spectroscopy analysis device using the capillary rotation device.

  Generally, a compound such as a pharmaceutical has a plurality of crystal forms (crystal polymorphs). And depending on each crystal form, its stability and the like may be different, and particularly in the case of a pharmaceutical, its therapeutic effectiveness may be different. Therefore, when evaluating a newly developed compound, the compound is crystallized under various conditions, and the stability of each crystal form generated thereby is analyzed using an analyzer such as an X-ray diffractometer or Raman spectrometer. Is used, and a useful crystal form and crystallization conditions for obtaining this crystal form are selected and determined.

  Here, when analyzing the crystal form of a compound using an analyzer such as the X-ray diffractometer, an elongated container made of glass (outer diameter 0.1) is used as a container for containing the compound. About 1.5 mmφ) is widely used. Hereinafter, an X-ray diffractometer will be described as an example of an analysis apparatus using a capillary, and its configuration will be specifically described.

  FIG. 1 is a front view schematically showing a schematic configuration of an X-ray diffraction apparatus to which the capillary is attached. As shown in FIG. 1, an X-ray diffraction apparatus 100 includes an X-ray tube 20 that emits X-rays, an optical element 30 that collimates the X-rays emitted from the X-ray tube 20, and a capillary C And an X-ray detector 40 for detecting diffracted X-rays diffracted by the compound contained in With such a configuration, the X-ray emitted from the X-ray tube 20 and collimated by the optical element 30 is contained in the inside of the capillary C through the tip side wall (about 5 to 20 mm in length). Will diffract strongly in a specific direction depending on the crystal form of the compound. Then, by rotating the X-ray detector 40 in the direction of the arrow in FIG. 1 and sequentially measuring the intensity of the diffracted X-rays, the rotation angle (2θ) of the X-ray detector 40 and the direction corresponding to each rotation angle. Thus, a relationship (diffraction pattern) with the intensity of the diffracted X-rays in the graph is obtained. Based on the diffraction pattern, the peak position of the diffracted X-ray is detected, and the crystal form of the compound accommodated in the capillary C is evaluated based on the detected peak position.

  Here, the capillary C attached to the X-ray diffractometer 100 can be rotated around the axial direction by the capillary rotator so that the peak positions of the diffracted X-rays can be detected in all directions of the crystals of the accommodated compound. Has been.

  FIG. 2 is a side view schematically showing a schematic configuration of a conventional capillary rotating device. As shown in FIG. 2, a conventional capillary rotating apparatus 10A includes a goniometer head (sometimes referred to as a goniometer head) 101 for attaching a capillary C and adjusting its position and direction, and a goniometer head 101 on a rotating shaft. A rotation motor 102 that rotates the capillary C together with the gonio head 101 in the axial direction by being attached is provided.

  The capillary C is attached to the gonio head 101 by fixing the rear end portion thereof to a metal pin P using wax, clay or the like, and screwing the pin P to the gonio head 101. The gonio head 101 includes, for example, a triaxial translation mechanism orthogonal to each other and a biaxial tilt mechanism (swivel mechanism) orthogonal to each other. With these mechanisms, the position of the attached capillary C and the like The direction can be adjusted.

  Here, if the rotation center of the capillary C (the rotation center MC of the rotation motor 102) and the axis CC of the capillary C do not coincide with each other, when the capillary C is rotated by the capillary rotation device 10A, the rotation angle is set. Correspondingly, rotational shake in which the position and direction of the capillary C fluctuate occurs. As described above, since the capillary C is fixed to the metal pin P using wax, clay, or the like, even if the axis of the pin P and the rotation center MC of the rotary motor 102 are made to coincide with each other with high accuracy. Even if it is possible, it is difficult to make the axial center CC of the capillary C coincide with the rotation center (rotation center of the capillary C) MC of the rotary motor 102 with high accuracy.

  If excessive rotational vibration occurs in the capillary C, there is a problem that the analysis accuracy of the crystal form of the compound is lowered. That is, if excessive rotational shaking occurs in the capillary C, the compound contained in the capillary C is not properly irradiated with X-rays, so that the peak position of the diffracted X-rays cannot be accurately detected, or all the orientations of the compound are detected. The peak position of the diffracted X-ray cannot be detected, or the diffracted X-ray cannot be obtained depending on the degree of rotational shake. Therefore, in the conventional capillary rotating apparatus 10A, after the capillary C is attached to the gonio head 101, the position and direction of the capillary C are adjusted using the parallel movement mechanism and the tilt mechanism of the gonio head 101, and the rotation center of the capillary C and the capillary The work of matching the C axis CC as much as possible is performed.

  However, the adjustment work described above is extremely troublesome to manually adjust the amount of movement of the parallel movement mechanism included in the gonio head 101 and the amount of tilt of the tilt mechanism while magnifying the vicinity of the attachment location of the capillary C using a microscope. Therefore, it is a factor that hinders the improvement of the efficiency of the crystal form evaluation test using the X-ray diffractometer. In addition, since the adjustment accuracy depends on the experience and skill of the operator, it is a factor that hinders the improvement in reproducibility of the crystal form evaluation test.

  The problems of the prior art described above are not limited to the exemplified X-ray diffractometers, and are not limited to the case of analyzing the crystal form of a compound. A capillary containing a substance is rotated around an axial direction. This is a problem common to various types of analysis devices that need to be performed.

  The present invention has been made to solve the problems of the prior art, and can easily suppress the rotational shake of the capillary, and as a result, when applied to an analysis apparatus for analyzing a substance contained in the capillary. It is an object of the present invention to provide a capillary rotating device capable of obtaining a highly accurate analysis result, and an X-ray diffractometer and a Raman spectroscopic analyzer using the capillary rotating device.

  In order to solve the above-mentioned problems, the present invention provides a first guide member, a second guide member, a third guide member, and a rotation support mechanism which are arranged in order from the front end side to the rear end side of the capillary. The rotation support mechanism supports the rear end portion of the capillary and operates to rotate the capillary in the axial direction, and the first guide member, the second guide member, and the third guide Each of the members includes a groove for guiding the capillary, and the groove of the first guide member and the groove of the third guide member are disposed on the same side of the capillary, The groove of the second guide member is disposed on the side surface of the capillary facing the side surface of the capillary where the groove of the first guide member and the third guide member is disposed, and at least the rotation support mechanism Yo When the capillary is rotated about the axial direction, the separation distance along the facing direction of the concave groove of the first guide member and the concave groove of the second guide member is set to be substantially equal to the outer diameter of the capillary. In addition, the concave groove of the third guide member is positioned so that the capillary is pressed against the concave groove side of the second guide member by the concave groove. Is.

  The capillary rotating device according to the present invention includes a first guide member, a second guide member, and a third guide member that are sequentially arranged from the front end side to the rear end side of the capillary. The first guide member, the second guide member, and the third guide member are each provided with a groove for guiding the capillary, and the groove of the first guide member and the groove of the third guide member are the capillary. The concave groove of the second guide member is disposed on the side surface of the capillary opposite to the side surface of the capillary where the concave grooves of the first guide member and the third guide member are disposed. The Further, when the capillary is rotated around the axial direction, the separation distance along the facing direction of the concave groove of the first guide member and the concave groove of the second guide member is set to be substantially equal to the outer diameter of the capillary, The concave groove of the third guide member is positioned so that the capillary is pressed toward the concave groove side of the second guide member by the concave groove. As a result, the portion on the rear end side of the second guide member of the capillary is deformed in a concave shape toward the concave groove side of the second guide member, and the portion on the tip side of the second guide member of the capillary is based on the lever principle. However, as a result of trying to move to the concave groove side of the first guide member using the concave groove of the second guide member as a fulcrum, the predetermined part of the capillary is always pressed against the concave groove of the first guide member.

  The capillary rotating device according to the present invention includes a rotation support mechanism that supports the rear end portion of the capillary and operates to rotate the capillary around the axial direction. When the capillary is rotated in the axial direction by this rotation support mechanism, as described above, the capillary rotates in a state where a predetermined portion is always pressed against the concave groove of the first guide member according to the principle of the lever. Become. For this reason, even if the rotation center of the rotation support mechanism does not coincide with the axial center of the capillary at the rear end of the capillary or the axial center of the predetermined portion of the capillary pressed against the concave groove of the first guide member, The center of rotation of the predetermined part of the capillary pressed against the concave groove of the guide member always coincides with the axis of the predetermined part of the capillary, and the center of rotation of the part closer to the tip than the first guide member of the capillary is also the center of the capillary. This substantially coincides with the axial center of the tip side portion.

  As described above, according to the capillary rotating device according to the present invention, the rotational shake of the capillary (the rotational shake of the portion on the tip side of the first guide member) can be easily performed without requiring labor-consuming adjustment work. It is possible to suppress. Therefore, if the capillary rotating apparatus according to the present invention is applied to an analysis apparatus (for example, an X-ray diffractometer) for analyzing a substance, X-rays are irradiated to a portion on the tip side of the first guide member of the capillary. It is possible to obtain a highly accurate analysis result.

  Preferably, the third guide member and the rotation support mechanism are configured to be movable along a facing direction of the concave groove of the first guide member and the concave groove of the second guide member.

  According to such a preferable configuration, by adjusting the movement amount of the third guide member and the rotation support mechanism, the deformation amount of the capillary in the portion on the rear end side from the second guide member, and hence the first guide member of the capillary The advantage that the pressing force against the concave groove can be adjusted is obtained. Further, when attaching the capillary, the concave groove of the third guide member is separated from the concave groove of the second guide member by a distance equal to or larger than the outer diameter of the capillary, and the concave groove of the first guide member and the second guide member are separated. Since the third guide member can be moved to the second guide member side after the capillary is inserted and attached to the concave groove, there is also an advantage that the capillary mounting operation is further simplified. It is done.

  As a specific configuration of the rotation support mechanism constituting the capillary rotation device according to the present invention, for example, a pulley into which the rear end portion of the capillary is fitted, a rotation motor, and the rotational power of the rotation motor are transmitted to the pulley. It is possible to employ | adopt the structure provided with the power transmission mechanism for doing.

  Preferably, the capillary rotating device is applied to an X-ray diffractometer, and the first guide member is a region where X-rays are irradiated to the substance accommodated in the capillary and diffracted X-rays diffracted by the substance are An opening is disposed on the emission side, has a width smaller than the outer diameter of the capillary, and extends along the axial direction of the capillary.

  According to such a preferable configuration, since the width of the diffracted X-ray detected by the X-ray detector of the X-ray diffractometer is limited by the opening having a width smaller than the outer diameter of the capillary, the peak of the diffracted X-ray It is possible to increase the position detection resolution. In addition, since the capillary part itself that emits X-rays and emits diffracted X-rays is pressed against the first guide member, X-rays are radiated to the part closer to the tip side than the first guide member of the capillary and diffracted. Compared with the case of detecting X-rays, it is possible to further suppress the influence of rotational shake on the analysis accuracy.

  In order to solve the above problems, the present invention is also provided as an X-ray diffractometer provided with the capillary rotator or a Raman spectroscopic analyzer characterized by including the capillary rotator. The

  According to the capillary rotating apparatus according to the present invention, it is possible to easily suppress the rotational shake of the capillary, and to obtain a highly accurate analysis result by applying it to an analyzing apparatus that analyzes the substance accommodated in the capillary. Is possible.

  Hereinafter, the case where the capillary rotating apparatus according to the present invention is applied to an X-ray analyzer will be described as an example with reference to the accompanying drawings.

  FIG. 3 is a side view schematically showing a schematic configuration of the capillary rotating device according to the embodiment of the present invention. As shown in FIG. 3, the capillary rotating device 10 according to the present embodiment includes a first guide member 11, a second guide member 12, which are arranged in order from the front end side to the rear end side of the capillary C, A third guide member 13 and a rotation support mechanism 14 are provided. In the present invention, a portion where the first guide member is disposed or a portion closer to the tip than the first guide member is set as an X-ray irradiation region (a region where the substance contained in the capillary C is irradiated with X-rays). However, with respect to the first guide member 11 according to the present embodiment, the portion closer to the tip than the first guide member 11 is an X-ray irradiation region.

  The first guide member 11, the second guide member 12, and the third guide member 13 are each provided with a concave groove for guiding the capillary C. Hereinafter, the configuration of such a concave groove will be specifically described. FIG. 4 is a diagram showing a specific configuration of the first guide member 11, the second guide member 12, and the third guide member 13 according to the present embodiment. FIG. 4 (a) is a side view, and FIG. ) Is a view seen from the direction of the arrow A shown in FIG. 4A, and FIG. 4C is a view seen from the direction of the arrow B shown in FIG. As shown in FIG. 4, the first guide member 11, the second guide member 12, and the third guide member 13 according to the present embodiment have an axis M (FIG. 4A) and an axis N (FIG. 4B). And a concave groove G defined by a truncated cone-shaped wall surface. The smaller diameter of the truncated cone is about 0.03 to 0.2 mm larger than the outer diameter D (see FIG. 3) of the capillary C, and the larger diameter is 0.5 to 0.5 mm larger than the outer diameter D of the capillary C. It is set to be about 2 mm larger. By providing such a concave groove G, when the capillary C is rotated in the axial direction as will be described later, the capillary C is formed in the concave groove G included in the first guide member 11 to the third guide member 13. It will be guided in a stable contact state. More specifically, the wall surface of the concave groove G prevents the capillary C from moving not only in a direction parallel to the paper surface of FIG. Further, when the third guide member 13 is moved as will be described later, even if the angle formed between the moving direction and the axis of the capillary C is not exactly a right angle, the third guide member 13 is formed by the concave groove G of the third guide member 13. Even after the capillary C is pressed and deformed, the concave groove G of the third guide member 13 can be brought into firm contact with the capillary C.

  In addition, the wall surface shape of the ditch | groove G which the 1st guide member 11, the 2nd guide member 12, and the 3rd guide member 13 comprise is not restricted to the form shown in FIG. 4, For example, as shown in FIG. As long as a stable contact state can be obtained even when the capillary C rotates, such as a polygonal frustum shape, various forms can be employed. Moreover, since the 1st guide member 11, the 2nd guide member 12, and the 3rd guide member 13 contact the capillary C which rotates so that it may mention later, the material (giving no excessive contact resistance with respect to the capillary C ( For example, it is preferable to use resin.

  Moreover, when applied to an X-ray diffractometer like the capillary rotating device 10 according to the present embodiment, a form as shown in FIG. 6 can be used as the first guide member. 6A and 6B are diagrams illustrating a specific configuration of the first guide member according to another embodiment, in which FIG. 6A is a side view and FIG. 6B is an arrow F in FIG. 6A. FIG. 6C shows a view seen from the direction, and FIG. 6C shows a view seen from the direction of the arrow G in FIG. The first guide member 11A shown in FIG. 6 is disposed in the X-ray irradiation region of the capillary C and on the side where the diffracted X-rays diffracted by the substance are emitted. That is, in this embodiment, X-rays are irradiated from the direction of the arrow F, pass through the capillary C, and diffracted X-rays are emitted in the direction of the arrow F. An opening having a width smaller than the outer diameter D of the capillary C and extending along the axial direction of the capillary C is provided.

  More specifically, the first guide member 11 </ b> A includes a pair of columnar (for example, columnar) members 111 disposed on the surface side in contact with the capillary C, and a surface in contact with the capillary C of the columnar member 111. And a plate-like member 112 provided on the opposite side and provided with an opening window 112a. The lengths of the columnar member 111 and the opening window 112a are set substantially equal to the length of the X-ray irradiation region at the tip of the capillary C. The width of the gap between the pair of columnar members 111 is set smaller than the outer diameter D of the capillary C. That is, the gap between the pair of columnar members 111 corresponds to the opening described above, and a concave groove (in this case, a through groove) for guiding the capillary C is formed by the opening and the pair of columnar members 111. become. In addition, Preferably, the material of the member which divides the said opening part is formed using a material with a high X-ray absorption. In the case of the first guide member 11 </ b> A shown in FIG. 6, the columnar member 111 that partitions the opening is formed using a material having high X-ray absorption (such as tantalum, lead, or brass).

  By adopting the first guide member 11A shown in FIG. 6, the width of the diffracted X-ray detected by the X-ray detector of the X-ray diffractometer is limited by the opening having a width smaller than the outer diameter D of the capillary C. Therefore, it is possible to increase the detection resolution of the peak position of the diffracted X-ray. As will be described later, the side wall of the capillary C is pressed against the first guide member. However, by adopting the first guide member 11A shown in FIG. One guide member 11A is pressed. For this reason, as shown in FIG. 3, compared to the case of detecting the diffracted X-rays by irradiating the X-ray to the tip side of the capillary C from the first guide member 11, the influence of the rotational shake on the analysis accuracy is reduced. Further suppression is possible. Furthermore, since the columnar member 111 is formed using a material having a high X-ray absorption, it is possible to effectively suppress detection of diffracted X-rays transmitted through the columnar member 111 by the X-ray detector. It is.

  As shown in FIG. 3, the concave groove G of the first guide member 11 and the concave groove G of the third guide member 13 are arranged on the same side of the capillary C (upper surface in the example shown in FIG. 3). The concave groove G of the second guide member 12 is formed on the side surface side of the capillary C facing the side surface side of the capillary C in which the concave grooves G of the first guide member 11 and the third guide member 13 are arranged (example shown in FIG. 3). In FIG. In the present embodiment, as a preferable configuration, the third guide member 13 is configured so that the concave groove G of the first guide member 11 and the concave groove G of the second guide member 12 face each other (the direction of the arrow Y in FIG. 3). And corresponds to one radial direction of the capillary C which is not bent). Specifically, the third guide member 13 is placed on a uniaxial stage (not shown) that is driven by a stepping motor. By driving the uniaxial stage, the third guide member 13 is moved in the direction of the arrow Y by a set distance. It can be moved. Further, in the present embodiment, the second guide member 12 can be similarly moved in the direction of the arrow Y by the uniaxial stage.

  The rotation support mechanism 14 supports the rear end of the capillary C and operates to rotate the capillary C around the axial direction. 7A and 7B are diagrams showing a specific configuration of the rotation support mechanism 14 according to the present embodiment, in which FIG. 7A is a side sectional view, and FIG. 7B is an arrow shown in FIG. 7A. The figure seen from the direction of E is represented. As shown in FIG. 7, the rotation support mechanism 14 according to the present embodiment includes a pulley 141 into which the rear end portion of the capillary C is fitted, a rotation motor 142, and a pulley 141 for transmitting the rotational power of the rotation motor 142 to the pulley 141. And a power transmission mechanism 143. With such a rotation support mechanism 14, the capillary C rotates at a rotation speed of about 60 to 600 rpm around the axial direction.

  More specifically, the power transmission mechanism 143 according to the present embodiment includes an O-ring 143a fitted in a concave groove 141a formed on the outer periphery of the pulley 141, and a rubber roller attached to the rotary shaft of the rotary motor 142. 143b and a driven roller 143c made of rubber or other material. In such a configuration, when the rubber roller 143b and the O-ring 143a come into contact with each other, the rotational power of the rotary motor 142 is transmitted to the pulley 141 via the rubber roller 143b and the O-ring 143a. At this time, the pulley 141 can be easily and stably rotated by bringing the driven roller 143c into contact with the O-ring 143a together with the rubber roller 143b. As the pulley 141 rotates, the capillary C fitted into the pulley 141 rotates in the circumferential direction (around the axial direction).

  In the present embodiment, as a preferred configuration, the rotation support mechanism 14 is along the facing direction (the direction of the arrow Y in FIG. 3) between the groove G of the first guide member 11 and the groove G of the second guide member 12. It is configured to be movable. Specifically, the rotation motor 142, the rubber roller 143b, and the driven roller 143c constituting the rotation support mechanism 14 are placed on a uniaxial stage (not shown) driven by a stepping motor, and by driving the uniaxial stage, , It can be moved in the direction of the arrow Y by the set distance. Further, the pulley 141 and the O-ring 143a constituting the rotation support mechanism 14 naturally move as the capillary C is pressed and deformed by the concave groove G of the third guide member 13 as will be described later. .

  In the present embodiment, the power transmission mechanism 143 includes a rubber roller 143b for transmitting rotational power to the O-ring 143a and thus the pulley 141, and a driven roller 143c for easily and stably rotating the pulley 141. The configuration provided is described. However, the present invention is not limited to this, and it is also possible to employ a configuration in which only the rubber roller 143b is brought into contact with the O-ring 143a without including the driven roller 143c. Further, in order to stabilize the rotation of the pulley 141, it is also possible to form a concave groove corresponding to the dimension of the O-ring 143a at a portion where the O-ring 143a of the rubber roller 143b contacts.

  Further, the power transmission mechanism according to the present invention is not limited to the configuration shown in FIG. 7, and for example, a power transmission mechanism 143A as shown in FIG. 8 can be adopted. The power transmission mechanism 143A shown in FIG. 8 includes a pulley 143d attached to the rotation shaft of the rotary motor 142 and a rubber belt 143e having an endless track that is stretched between the pulley 141 and the pulley 143d. In such a configuration, the rotational power of the rotary motor 142 is transmitted to the pulley 141 via the pulley 143d and the rubber belt 143e, whereby the capillary C fitted into the pulley 141 rotates in the circumferential direction (around the axial direction). Become. In addition, the power transmission mechanism according to the present invention can employ various configurations as long as the rotational power of the rotary motor 142 can be transmitted to the pulley 141.

  Hereinafter, the initial setting operation of the capillary rotating apparatus 10 having the above-described configuration will be described with reference to FIG. 9 as appropriate. FIG. 9 is an explanatory diagram for explaining an initial setting operation of the capillary rotating device according to the present embodiment. As an initial setting of the capillary rotating device 10, first, a substance to be analyzed is accommodated in the capillary C, and the rear end portion of the capillary C is fitted into the pulley 141. Next, as shown in FIG. 9A, the capillary C is placed so that the side wall near the rear end of the X-ray irradiation region at the front end of the capillary C is in a position where it contacts the groove G of the first guide member 11. After positioning, the uniaxial stage (not shown) is driven to move the second guide member 12 in the direction of the arrow Y1. At this time, the distance in the facing direction (the direction of the arrow Y1) between the concave groove G of the first guide member 11 and the concave groove G of the second guide member 12 is substantially equal to the outer diameter of the capillary C (the capillary C In consideration of the tolerance of the outer diameter, it is preferably set slightly wider than the nominal outer diameter.

  Next, a uniaxial stage (not shown) is driven to move the third guide member 13 in the direction of the arrow Y2. At this time, as shown in FIG. 9B, the third guide member 13 is moved until the capillary C is pressed against the groove G side of the second guide member 12 by the groove G of the third guide member 13. Move. More specifically, as shown in FIG. 9B, the separation distance L2 along the direction of the arrow Y2 between the concave groove G of the third guide member 13 and the concave groove G of the second guide member 12 is: The third guide member 13 is moved downward until it becomes smaller than the separation distance L1 along the facing direction of the concave groove G of the first guide member 11 and the concave groove G of the second guide member 12. Furthermore, you may move below rather than the position from which the separation distance L2 becomes zero. With this operation, the capillary C is pressed toward the concave groove G of the second guide member 12 by the concave groove G of the third guide member 13, and the rear end portion side of the second guide member 12 is located on the second guide member 12. It will deform | transform into a concave shape toward the ditch | groove G side. Then, on the principle of the lever, the portion of the capillary C closer to the tip than the second guide member 12 moves to the concave groove G side of the first guide member 11 with the concave groove G of the second guide member 12 as a fulcrum (FIG. 9). As a result of trying to move in the direction of the arrow Y1 shown in (a), a predetermined part of the capillary C (a side wall near the rear end of the X-ray irradiation region) was always pressed against the concave groove G of the first guide member 11. It becomes a state.

  Finally, the uniaxial stage (not shown) is driven to move the rotation motor 142, the rubber roller 143b, and the driven roller 143c in the direction of the arrow Y3, and as shown in FIG. 9C, the rubber roller 143b and the driven roller 143c. Is stopped at a position where the surface contacts the O-ring 143 a fitted in the pulley 141, the initial setting of the capillary rotating device 10 is completed.

  In the present embodiment, the configuration in which the rotation motor 142, the rubber roller 143b, and the driven roller 143c are moved until the surfaces of the rubber roller 143b and the driven roller 143c come into contact with the O-ring 143a has been described, but the present invention is not limited to this. Instead, a configuration is adopted in which the positions of the rotation motor 142, the rubber roller 143b, and the driven roller 143c are fixed, and the third guide member 13 is moved until the O-ring 143a contacts the surfaces of the rubber roller 143b and the driven roller 143c. Is also possible.

  As described above, after the initial setting operation of the capillary rotating device 10 is completed, the analysis operation by the X-ray diffractometer is executed. At this time, the rotation motor 142 is driven to rotate the capillary C in the axial direction. As described above, the capillary C has a predetermined portion (side wall near the rear end of the X-ray irradiation region) according to the principle of the insulator. It rotates in the state always pressed against the concave groove G of the first guide member 11. For this reason, a predetermined center of the capillary C pressed against the rotational center of the rear end of the capillary C (the rotational center PC of the pulley 141) and the axial center of the rear end of the capillary C or the concave groove G of the first guide member 11 is assumed. Even if the axial center CC of the part does not match, the rotation center CC ′ of the predetermined part of the capillary C pressed against the concave groove G of the first guide member 11 is always the axial center CC of the predetermined part of the capillary C. Will match. The center of rotation of the portion (X-ray irradiation region) on the tip side of the first guide member of the capillary C also substantially coincides with the axis of the portion on the tip side of the capillary C. In this way, according to the capillary rotating device 10 according to the present embodiment, the rotational shake of the capillary C (on the tip side of the first guide member 11) can be achieved without requiring an adjustment work which is troublesome as compared with the prior art. It is possible to easily suppress the rotational shake of the part.

Table 1 shows the results of investigating a range of initial setting values that are preferable for suppressing rotational shake for capillaries C having various outer diameters D (see FIG. 3). More specifically, Table 1 shows a preferable amount of movement of the third guide member 13 expressed by the radius of curvature R of the approximate circle. More specifically, the arc in the case where the axial center of the capillary C located between the second guide member 12 and the third guide member 13 after completion of the initial setting is approximated to be an arc in a side view. The preferred range of the radius of curvature R is shown. It means that the smaller the curvature radius R, the larger the deformation amount of the capillary C and the larger the movement amount of the third guide member 13 (the greater the pressing force of the third guide member 13). Table 1 also shows a preferable range of the separation distance L (see FIG. 3) along the axial direction of the capillary C between the first guide member 11 and the second guide member 12.

  In order to suppress the rotational shake of the capillary C as much as possible, it is preferable to increase the pressing force by increasing the amount of movement of the third guide member 13, but the capillary C is more difficult to deform as the outer diameter D of the capillary C increases. Become. And if an excessive pressing force is applied and deformed, the capillary C may be damaged. Therefore, as shown in Table 1, as the outer diameter D of the capillary C increases, the preferable range of the radius of curvature R shifts to a larger value. Further, in order to simplify the initial setting, when the movement amount of the third guide member 13 is set to be constant regardless of the size of the outer diameter D of the capillary C (the curvature radius R is set to be constant), the outer diameter D is set. The larger the capillary C, the larger the pressing force that the third guide member 13 should apply. Along with this, the pressing force applied to the first guide member 11 also increases. However, the first guide member 11 is increased by increasing the separation distance L between the first guide member 11 and the second guide member 12 according to the principle of the lever. Therefore, the pressing force applied to the second guide member 12 is also reduced. Therefore, as shown in Table 1, as the outer diameter D of the capillary C increases, the capillary C is less likely to be damaged due to being excessively pressed against the first guide member 11 and the second guide member 12. The preferable range of the separation distance L is shifted to a large value.

  By performing the initial setting as described above, it is possible to prevent the capillary C from being damaged, and it is possible to effectively suppress rotational shake (rotational shake at a position closer to the distal end than the first guide member 11). It was.

  More specifically, after initial setting is performed on the capillaries C of various outer diameters D under the conditions shown in Table 1, the rotation motor 142 is driven to rotate the capillaries C around the axial direction, and the rotation blurring occurs. Evaluated. Here, the rotational shake is observed by magnifying a portion included in the X-ray irradiation region of the capillary C (specifically, a portion spaced about 10 mm closer to the distal end side than the first guide member 11) with a microscope, Evaluation was made as the amount of change in position of the capillary C in the radial direction. As a result, under any condition, it was possible to suppress rotational shake to ± 20 μm or less. In particular, with respect to the conditions of the outer diameter D = 0.5 mmφ, L = 10 mm, and R = 1000 mm, the rotational shake could be suppressed to about ± 9 μm. On the other hand, in the configuration in which the first guide member 11, the second guide member 12, and the third guide member 13 are not provided, the rotation motor 142 is driven to rotate the capillary C around the axial direction, and the rotational shake is similarly evaluated. As a result, the rotational shake became extremely large at ± 500 μm.

  As described above, when the capillary rotating device 10 according to the present embodiment is used, it is possible to effectively suppress the rotational shake of the capillary C, and thus it is possible to improve the analysis accuracy of the X-ray diffractometer.

FIG. 1 is a front view schematically showing a schematic configuration of an X-ray diffraction apparatus using a capillary. FIG. 2 is a side view schematically showing a schematic configuration of a conventional capillary rotating device. FIG. 3 is a side view schematically showing a schematic configuration of the capillary rotating device according to the embodiment of the present invention. FIG. 4 is a diagram illustrating a specific configuration of the first to third guide members illustrated in FIG. 3. FIG. 5 is a diagram illustrating another configuration example of the first to third guide members illustrated in FIG. 3. FIG. 6 is a diagram illustrating another configuration example of the first guide member illustrated in FIG. 3. FIG. 7 is a diagram showing a specific configuration of the rotation support mechanism shown in FIG. FIG. 8 is a diagram illustrating another configuration example of the rotation support mechanism illustrated in FIG. 3. FIG. 9 is an explanatory diagram for explaining an initial setting operation of the capillary rotating device according to the present embodiment.

Explanation of symbols

DESCRIPTION OF SYMBOLS 10 ... Capillary rotation apparatus 11 ... 1st guide member 12 ... 1st guide member 13 ... 3rd guide member C ... Capillary

Claims (6)

A first guide member, a second guide member, a third guide member, and a rotation support mechanism that are arranged in order from the front end side to the rear end side of the capillary;
The rotation support mechanism supports the rear end of the capillary and operates to rotate the capillary around the axial direction;
The first guide member, the second guide member, and the third guide member each have a concave groove for guiding the capillary,
The concave groove of the first guide member and the concave groove of the third guide member are disposed on the same side surface side of the capillary, while the concave groove of the second guide member includes the first guide member and the first guide member. 3 disposed on the side surface of the capillary facing the side surface of the capillary where the concave groove of the guide member is disposed,
When the capillary is rotated about the axial direction by at least the rotation support mechanism, the separation distance along the facing direction of the concave groove of the first guide member and the concave groove of the second guide member is the outer diameter of the capillary. And the concave groove of the third guide member is positioned so that the capillary is pressed against the concave groove side of the second guide member by the concave groove. Rotating device.   The said 3rd guide member and the said rotation support mechanism are comprised so that a movement is possible along the opposing direction of the ditch | groove of the said 1st guide member, and the ditch | groove of the said 2nd guide member. 2. The capillary rotation device according to 1.   The rotation support mechanism includes a pulley into which a rear end portion of the capillary is fitted, a rotation motor, and a power transmission mechanism for transmitting the rotation power of the rotation motor to the pulley. Or the capillary rotating apparatus of 2. The capillary rotating device is applied to an X-ray diffractometer,
The first guide member is disposed in a region where a substance contained in the capillary is irradiated with X-rays and on a side where a diffracted X-ray diffracted by the substance is emitted, and is smaller than an outer diameter of the capillary 3. The capillary rotating device according to claim 1, further comprising an opening having a width and extending along an axial direction of the capillary.   An X-ray diffractometer comprising the capillary rotating device according to claim 1.   A Raman spectroscopic analyzer comprising the capillary rotating device according to claim 1.

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