SAMPLE HOLDER FOR PERFORMING X-RAY ANALYSIS ON A CRYSTALLINE SAMPLE, AND SAMPLE HOLDER HANDLING SYSTEM

Abstract

A sample holder (3) for performing X-ray analysis on a crystalline sample (11) comprises a mounting support with a first end that can be attached to a goniometer head, whereby the crystalline sample (11) can be attached to the mounting support at a distance to the first end. The sample holder (3) further comprises a holder base at the first end of the mounting support with means for mounting the holder base to the goniometer head, whereby the holder base is configured to fit into a well (2) of a well plate (1). The holder base comprises a ferromagnetic material for mounting the holder base to a magnetic base element at or within the goniometer head. The mounting support comprises a tube preferably made of glass into which the crystalline sample (11) can be inserted. The sample holder (3) can also comprise a base disk (14) that provides for a lid for a well (2) of the well plate (1) after insertion of the sample holder (3) into the well (2). The holder base can also comprise a holder ring (7) that is arranged at the first end of the mounting support and that surrounds the mounting support in a circumferential manner The base disk (14) can be removably attachable to the holder ring (7). A crystalline sponge is attached to the mounting support.

Claims

1. A sample holder (3) for performing X-ray analysis on a crystalline sample (11), whereby the sample holder (3) comprises a mounting support with a first end that can be attached to a goniometer head, whereby the crystalline sample (11) can be attached to the mounting support at a distance to the first end, characterized in that the sample holder (3) comprises a holder base at the first end of the mounting support with means for mounting the holder base to the goniometer head, and whereby the holder base is configured to fit into a well (2) of a well plate (1).

2. The sample holder (3) of claim 1, wherein the holder base comprises a ferromagnetic material for mounting the holder base to a magnetic base element at or within the goniometer head.

3. The sample holder (3) of claim 1, wherein the mounting support comprises a tube into which the crystalline sample (11) can be inserted.

4. The sample holder (3) of claim 3, wherein the tube is a glass tube (6).

5. The sample holder (3) of claim 1, wherein the sample holder (3) comprises a base disk (14) that provides for a lid for a well (2) of the well plate (1) after insertion of the sample holder (3) into the well (2).

6. The sample holder (3) of claim 1, wherein the holder base comprises a holder ring (7) that is arranged at the first end of the mounting support and that surrounds the mounting support in a circumferential manner.

7. The sample holder (3) of claim 5 and claim 6, wherein the base disk (14) is removably attachable to the holder ring (7).

8. The sample holder (3) of claim 1, wherein a crystalline sponge is attached to the mounting support.

9. The sample holder (3) of claim 3 and claim 8, wherein the crystalline sponge is arranged inside of the tube.

10. The sample holder (3) of claim 1, wherein the sample holder (3) comprises a protective container (17) that encases the mounting support and a crystalline sample (11) that can be attached to the mounting support at a distance to the first end.

11. A sample holder handling system for performing X-ray analysis on crystalline samples (11) with a goniometer with a goniometer head, with at least one sample holder (3) and with a well plate (1), wherein the sample holder (3) is configured according to one of the preceding claims and fits into a well (2) of the well plate (1).

12. The sample holder handling system of claim 11, wherein the sample holder (3) comprises a base disk (14) with a diameter that matches the diameter of the well (2) of the well plate (1).

13. The sample holder handling system of claim 12, wherein the base disk (14) comprises fastening means for engagement of the base disk (14) with an automated sample holder operating system.

14. The sample holder handling system of claim 12, wherein an insert ring (14) is arranged at the bottom (10) of a well (2) of the well plate (1) that supports the base disk (14) of a sample holder (3) that is inserted into the well (2) of the well plate (1).

15. The sample holder handling system of claim 11, wherein the holder base comprises a holder ring (7) and wherein the outer diameter and the lateral surface of the holder ring (7) is adapted to match the diameter and the inner surface of a well (2) of the well plate (1) at the top of the well (2).

16. The sample holder handling system of claim 15, wherein the holder ring (7) comprises fastening means for engagement of the holder ring (7) with an automated sample holder operating system.

17. The sample holder handling system of claim 15, wherein an insert ring (14) is arranged at the bottom (10) of a well (2) of the well plate (1) that supports the holder ring (7) of a sample holder (3) that is inserted into the well (2) of the well plate (1).

18. The sample holder handling system of claim 11, wherein the sample holder (3) comprises a protective container (17) and wherein the outer diameter, the lateral surface and the height of the protective container (17) is adapted to match the diameter, the inner surface and the height of a well (2) of the well plate (1).

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0030] The present invention will be more fully understood, and further features will become apparent, when reference is made to the following detailed description and the accompanying drawings. The drawings are merely representative and are not intended to limit the scope of the claims. In fact, those of ordinary skill in the art may appreciate upon reading the following specification and viewing the present drawings that various modifications and variations can be made thereto without deviating from the innovative concepts of the invention. Like parts depicted in the drawings are referred to by the same reference numerals.

[0031] FIG. 1 illustrates a three-dimensional sketch of a standardized well plate with 96 wells that are arranged in a regular pattern, whereby in some wells a sample holder according to the invention is inserted into the corresponding well,

[0032] FIG. 2 illustrates an exploded and schematic view of a sample holder with a holder ring that is configured to be placed inside of a customized well of the well plate,

[0033] FIG. 3 illustrates a schematic view of the sample holder with a well of FIG. 2, whereby the sample holder with the holder ring is placed inside of the well,

[0034] FIG. 4 illustrates an exploded and schematic view of another embodiment of the sample holder with a holder ring that is configured to be placed inside of a standardized well of the well plate,

[0035] FIG. 5 illustrates a schematic view of the sample holder with a well of FIG. 4, whereby the sample holder with the holder ring is placed inside of the well,

[0036] FIG. 6 illustrates an exploded and schematic view of another embodiment of the sample holder with a base disk and a pin-like mounting support that is configured to be placed inside of a standardized well of the well plate,

[0037] FIG. 7 illustrates a schematic view of the sample holder with a well of FIG. 6, whereby the sample holder with the base disk is placed inside of the well,

[0038] FIG. 8 illustrates an exploded and schematic view of another embodiment of the sample holder with a base disk, a pin-like mounting support and a surrounding tube that is configured to be placed inside of a standardized well of the well plate,

[0039] FIG. 9 illustrates a schematic view of the sample holder with a well of FIG. 8, whereby the sample holder with the pin-like mounting support and the surrounding tube is placed inside of the well.

DETAILED DESCRIPTION OF THE INVENTION

[0040] A well plate 1 with 96 wells 2 is shown in FIG. 1. The wells 2 are arranged in a regular and matrix-like pattern on the well plate 1. The arrangement of the wells 2 corresponds with standards for such well plates 1 that can be used with many different machines and handling systems.

[0041] In some of the wells 2, namely in five of the wells 2 at positions A1 to A5 of the well plate 1 shown in FIG. 1, a sample holder 3 according to the invention is placed inside of the well 2. Different embodiments of sample holders will be further described and are shown in FIGS. 2 to 9. A bottom side 4 of each of the sample holders 3 is flush with the upper surface 5 of the well plate 1. In FIG. 1, only the bottom side 4 of each of the sample holders 3 can be seen.

[0042] In general, the well plate 1 should preferably confirm to the dimensions given by the American National Standards Institute (ANSI) for compatibility with pipetting robots or other automation devices. The current standard dimensions descriptions include ANSI/SLAS 1-2004 (Footprint Dimensions), ANSI/SLAS 3-2004 (Bottom Outside Flange Dimensions), ANSI/SLAS 4-2004 (Well Positions) and possibly ANSI/SLAS 2-2004 (Height Dimensions), possibly ANSI/SLAS 6-2012 (Well Bottom Elevation). The standard dimensions of well plates 1 are length of 127.76 mm and width of 85.48 mm. The well plate 1 should further be adjusted to applicable future standardizations for well plates 1.

[0043] A first embodiment of a sample holder 3 according to the invention is shown in FIGS. 2 and 3. In these Figures as well as in further similar Figures, a cross-section through the well plate 1 from the left edge of the well plate 1 is shown. However, only the first well 2 is indicated, while half of the second well 2 is only simulated with a dashed line. The sample holder 3 comprises a glass tube 6 wherein the glass tube 6 can be similar to a capillary that is commonly used in X-ray structure elucidation today, e.g. a model produced by Hilgenberg (Malsfeld, Germany) with a wall thickness of 0.01 mm, a funnel like opening on one side and a closed off end on the other (Article no. 4007630). The glass tube 6 has a thin wall thickness on the bottom to enable direct measurements of samples inside the glass tube in an X-ray diffractometer. Furthermore, the length of the glass tube 6 is configured to fit into the height of the well plate 1, which is for instance 14 mm, 22 mm or 44 mm and, at the same time, is configured to fit into the goniometer set up, i.e. on top of a goniometer head that is not shown in the Figures. The dimension range that is compatible with the currently commercially available goniometer heads allows a total length of the glass tube 6 of approx. 22 mm to 32 mm. By using the sample holder 3 with other goniometer heads and/or goniometer set ups, the dimensions of the glass tube 6 could be extended, e.g. from 10 mm to 50 mm, 100 mm, or even 250 mm.

[0044] The glass tube 6 of the sample holder 3 is surrounded by a holder ring 7. The holder ring 7 further comprises features that make it suitable to be directly attached to a goniometer in an X-ray diffractometer as mentioned above. These features can comprise a metal ring 8 which magnetically can be held by a goniometer head with a magnet inside of or on top of the goniometer head. The dimensions of the holder ring 7 are preferably compatible with the currently used base magnetic attachments to goniometer heads, e.g. the commercially available magnetic base support “Magnetic Base Support Z with Strong Magnet” from Rigaku (Art. Nr. 1013161) that can be used with a goniometer head from Rigaku (Art. Nr. 1013156). Other features for an attachment to the goniometer head could include a screw thread, a certain diameter in combination with a material that is pressure-insensitive for interlocking with or clamping on the goniometer head.

[0045] The dimensions of the holder ring 7 could also be different, which would then just require some changes on the goniometer head to be able to attach them. These changes can comprise a small adapter to the current design.

[0046] Preferably, the shape of the holder ring 7 is round, i.e. a circular shape. However, the holder ring 7 also can be of any other shape, e.g. with a square footprint. The shape of the holder ring 7 preferably fits into the well 2 of the well plate 1 and does not sink too far into the well 2 but is held back at the top, i.e. in close proximity to the opening of the well 2 at the surface 5 of the well plate 1. As can be seen in FIGS. 2 and 3, the well 2 of the well plate 1 is customized for reception of the sample holder 3 by adding an opening 9 into a bottom 10 of each of the wells 2, thus enabling the glass tube 6 to reach through the opening 9 into the body of the well plate 1.

[0047] The holder ring 7 can be permanently attached to the glass tube 6 to ensure best stability. The holder ring 7 can also be removably attached to the glass tube 6 in order to allow for recycling by replacing the glass tube 6. However, it is regarded as a basic requirement that the holder ring 7 does not detach from the glass tube 6 during a measurement.

[0048] Preferably, the holder ring 7 has a circular cross-section and a conical outer shape. The holder ring 7 is made from a polymer that can be glued to the glass tube 6. Preferably, a metal ring 8 is attached to the polymer base of the holder ring 7 as the feature for attachment to the goniometer head. However, a direct attachment of the feature for attachment to the goniometer head to the glass tube 6 is also possible. In one embodiment, a metal ring 8 can be attached directly to the glass tube 6.

[0049] The crystalline sample 11 is placed inside of the glass tube 6. The crystalline sample 11 can be a single crystal to be used for X-ray diffraction measurements. The crystalline sample 11 can also be composed of a crystalline sponge that is soaked with a crystalline solution comprising crystal molecules.

[0050] In FIGS. 4 and 5 the combination of another embodiment of the sample holder 3 with a standardized well plate 1 is shown. An insert ring 12 is inserted into the well 2 and placed on the bottom 10 of the well 2. An upper side 13 of the insert ring 12 provides for a stop that supports the holder ring 7 of the sample holder 3. The length of the insert ring 12 is configured to fully encompass the glass tube 6 that serves as a mounting support for the crystalline sample 11 inside of the glass tube 6.

[0051] A base disk 14 is attached to the holder ring 7 and provides for a closure of the glass tube 6, thus protecting the content of the glass tube 6, i.e. the crystalline sample 11 inside of the glass tube 6. The dimensions and the shape of the sample holder 3 with the base disk 14 can be configured to be fully placed inside of the well 2, a back side of the base disk 14 being flush with the surface 5 of the well plate 1. However, it is also possible and can be advantageous to have the base disk 14 outside of the well 2 which may allow for easy handling of the sample holder 3 with automated sample holder operating and handling systems.

[0052] Preferably, the base disk 14 closes the glass tube 6 tightly and guarantees the retention of any material such as organic solvents in the glass tube 6. The feature for attachment of the glass tube 6 to the goniometer head such as a magnetic material, i.e. the metal ring 8 can also sit on top of said base disk 14. The base disk 14 can also comprise a thread or a screw-in mechanism to guarantee a tight closing. The base disk 14 can also comprise a septum or a similar device that enables the transfer of material through the base disk 14 by puncturing it temporarily.

[0053] The sample holder 3 might be equipped with a feature for unique identification, such as a bar code, a two-dimensional bar code, QR code an RFID chip, or another characteristic of such kind, which can be captured and read by a machine.

[0054] In FIGS. 6 and 7 the sample holder 3 comprises a pin-like pole 15 instead of the glass tube 6 of the previous embodiment that serves as the mounting support for the crystalline sample 11 that is attached to a free end 16 of the pin-like pole 15. The pin-like pole 15 is mounted onto the base disk 14. A protective container 17 that surrounds and encompasses the pole 15 is removably attached to the base disk 14. The dimensions and the shape of the protective container 17 are configured to be fully placed inside of the well 2 of the well plate 1.

[0055] In FIGS. 8 and 9 yet another embodiment of the invention is shown. The sample holder 3 comprises both, a pin-like pole 15 and a glass tube 6 that surrounds and encompasses the pin-like pole 15 with the crystalline sample 11 attached to the free end 16 of the pin-like pole 15. The pin-like pole 15 and the glass tube 6 are attached to the base disk 14 that also comprises a metal ring 8 embedded into the base disk 14.

EXAMPLE

[0056] Hereinafter, the present invention is described in more detail and specifically with reference to the example, which however is not intended to limit the present invention.

[0057] For the proof of concept, a prototype of a sample holder 3 with a glass tube 6 was produced. It comprised a glass tube 6 made from borosilica glass with a diameter of 0.3 mm and a wall thickness of 0.01 mm. Such a glass tube 6 is commercially available e.g. as a capillary with a length of several centimeters. The glass tube 6 was melted shut with a flame at a distance of approx. 22 mm measured from an open end of the glass tube 6.

[0058] The glass tube 6 was glued into a holder ring 7 that comprised of a short plastic pipe with a length of approx. 9 mm, an outer diameter of 4 mm and an inner diameter of 3 mm. A previously closed end of the glass tube 6 is hidden within the holder ring 7, while the open end of the glass tube 6 pointed out. On top of the holder ring 7, i.e. on the side of the holder ring 7 where the open end 18 of the glass tube was not pointing out, a small metal ring 8 was glued. The metal ring 8 was a shim normally used as a distance plate for screws with an inner diameter of 3.2 mm and an outer diameter of 7 mm.

[0059] For a test during an application, a crystalline sponge, prepared as stated in a publication (M. Hoshino, A. Khutia, H. -Z. Xing, Y. Inokuma, M. Fujita, IUCrJ, 2016, 3, 139-151), was loaded into the glass tube 6 under a microscope. The sample holder 3 with the loaded glass tube 6 was then magnetically attached to the magnetic goniometer head. The diffraction pattern of the crystalline sample 11 within the crystalline sponge was successfully recorded at a temperature of 200 K and the structure could successfully be solved using standard protocols.

[0060] A well plate 1 with a customized design was created according to the following requirements. It comprised the base dimensions of well plates as defined by ANSI. The height was 34 mm. The wells 2 themselves were round had a diameter of approx. 9 mm. The wells 2 submerged into the well plate 1 for about 9 mm in a cylinder like shape. At the bottom 10 of the wells 2, there was a cutout in the middle with a diameter of approx. 2 mm.

[0061] When a sample holder 3 with a glass tube 6 as described above was placed in the prototype of the customized well plate 1, the tip of the glass tube 6 could fit through the cutout hole in the middle of the well 2. The sample holder 3 rested with the holder ring 7 on the bottom 10 of the well 2 of the customized well plate 1.

[0062] It was demonstrated that a magnet could be used to take the sample holder 3 out of the well plate 1 or to insert the sample holder 3 into the well 2 for storing and transporting the sample holder 3 before, between and after measurements.