X-ray single crystal diffraction sample tube device and method of use

Abstract

This invention provides an X-ray single-crystal diffraction sample sealing device and its usage method. The X-ray single-crystal diffraction sample sealing device includes a base, a sampling tube, and a sealing valve. The base has a chamber extending through its bottom. The sampling tube is airtightly connected to the top wall of the chamber, and its bottom end communicates with the top end of the chamber. The sealing valve is threaded into the chamber and has an internal channel connecting the top and bottom ends of the chamber. A sealing element is provided between the top surface of the sealing valve and the top wall of the chamber, and the sealing element cooperates with the sealing valve to seal the bottom end of the sampling tube. Compared with the prior art, this invention can achieve sealed transfer of air-sensitive samples and has the advantages of simple operation and reusability.

Description

Technical Field

[0001] This invention relates to the field of X-ray single crystal diffraction technology, and in particular to an X-ray single crystal diffraction sample sealing device and its usage method. Background Technology

[0002] Single-crystal X-ray diffraction (SXRD) utilizes the principle that periodically arranged points within a crystal diffract X-rays of a specific wavelength. Diffraction images of the crystal are collected and subjected to a series of data restoration and correction processes to obtain a set of diffraction data. Then, specialized crystal structure analysis software is used to derive the atomic coordinates of the compound, thereby obtaining information such as the compound's molecular spatial structure, bond lengths, bond angles, and the spatial arrangement and packing of molecules. In sciences closely related to synthetic chemistry, including coordination chemistry, organometallic chemistry, organic chemistry, inorganic materials chemistry, and bioinorganic chemistry, especially in research related to crystal engineering and supramolecular chemistry, X-ray single-crystal structure analysis has become an indispensable research tool.

[0003] Single crystal testing requires two steps: sample selection and transfer. Samples sensitive to oxygen, water, and temperature, or those prone to losing solvent molecules and efflorescence that prevents separation from the mother liquor, are typically transferred using a sealed tube method. This involves first using a pipette to remove the selected single crystal sample, then transferring it into a conical capillary glass tube. Depending on the crystal size, the crystal will be positioned at different locations. The capillary tube is then cut off at both ends and sintered to seal it. This method has drawbacks such as complex operation, non-reusable glass tubes, and difficulty in accurately positioning the sample, leading to misalignment. Summary of the Invention

[0004] The purpose of this invention is to address the shortcomings of the prior art by providing an X-ray single-crystal diffraction sample sealing device and its usage method, which enables the sealed transfer of air-sensitive samples and allows for reuse.

[0005] To achieve the above objectives, the present invention adopts the following technical solution:

[0006] In a first aspect, the present invention provides an X-ray single-crystal diffraction sample sealing device, comprising:

[0007] A base having a cavity extending through its bottom;

[0008] A sampling tube is airtightly connected to the top wall of the chamber, and the bottom end of the sampling tube is connected to the top end of the chamber.

[0009] A sealing valve is threaded into the chamber. The sealing valve has an internal channel connecting the top and bottom of the chamber. A sealing element is provided between the top of the sealing valve and the top wall of the chamber. The sealing element can cooperate with the sealing valve to seal the bottom of the sampling tube.

[0010] Preferably, the sampling tube includes an outer tube and an inner tube, the inner tube is disposed inside the outer tube and communicates with the top of the chamber, the inner diameter of the outer tube is larger than the size of the single crystal sample, the inner diameter of the inner tube is smaller than the minimum size of the single crystal sample, and the height of the inner tube is lower than the height of the outer tube.

[0011] Preferably, the top wall of the chamber has a countersunk hole and a through hole, the through hole connecting the chamber and the countersunk hole, and the outer tube and the inner tube are respectively inserted into the countersunk hole and the through hole.

[0012] Preferably, the sealing element is a sealing ring, which is disposed around the periphery of the sampling tube.

[0013] Preferably, the top end face of the sealing valve also has a plug corresponding to the bottom end of the sampling tube.

[0014] Preferably, the diameter of the top of the sealing valve is smaller than the diameter of the top of the chamber, and an air gap is formed between the circumferential sidewall of the top of the sealing valve and the circumferential sidewall of the top of the chamber, and the internal channel communicates with the top of the chamber through the air gap.

[0015] Preferably, the base is made of ferromagnetic material and the base is cone-shaped.

[0016] Preferably, it further includes a sealing cover placed on the base, the bottom of the base having a flange disposed opposite to the bottom surface of the sealing cover, and a sealing ring disposed between the bottom surface of the sealing cover and the flange.

[0017] Preferably, the shape of the internal cavity of the sealing cover matches the base and the sampling tube.

[0018] In a second aspect, the present invention also provides a method for using the X-ray single-crystal diffraction sample sealing device described in the first aspect above, characterized by comprising the following steps:

[0019] Place the culture dish on the microscope stage, add an appropriate amount of solvent for growing single crystals into the culture dish, take a small amount of mother liquor and single crystal sample and place them in the culture dish, and select a suitable single crystal sample under the microscope.

[0020] Rotate the sealing valve downwards so that the bottom end of the sampling tube is connected to the top end of the chamber. Insert a pipette from the bottom end of the chamber and aspirate some mother liquor under a microscope to test the sealing performance of the connections between the components.

[0021] The top of the sampling tube is aligned with a suitable single crystal sample, and a negative pressure is created in the chamber by a pipette. The single crystal sample is drawn in and stuck in the sampling tube under atmospheric pressure. The mother liquor can be drawn into the sampling tube, the chamber, and the pipette head.

[0022] Seal the top of the sampling tube;

[0023] Remove the pipette and rotate the sealing valve upwards to seal the bottom of the sampling tube;

[0024] The sealing device was transferred to the die carrier for testing.

[0025] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0026] In use, this invention first generates negative pressure inside the base using a pipette or similar tool, then draws air-sensitive samples through the sampling tube. After sample aspiration, both ends of the sampling tube are sealed. The air-sensitive sample and sealing device are then transferred together to the crystal stage for single-crystal testing. Because both ends of the sampling tube are sealed during transfer, and mother liquor remains inside the tube after sample aspiration, the sample is completely isolated from air and remains in the mother liquor environment, thus maximizing the preservation of the sample's original state. Furthermore, after single-crystal testing, the invention allows for the removal of the sealing material at the top of the sampling tube and the opening of the bottom of the tube via a sealing valve, removing the sample and mother liquor for subsequent sample transfers. Therefore, this invention enables sealed transfer of air-sensitive samples and offers advantages such as ease of operation and reusability. Attached Figure Description

[0027] To more clearly illustrate the specific embodiments of the present invention, the accompanying drawings used in the specific embodiments will be briefly described below. It should be noted that in all the drawings, the elements or parts are not necessarily drawn to actual scale.

[0028] Figure 1 This is a schematic diagram of the overall structure of the X-ray single-crystal diffraction sample sealing device described in an embodiment of the present invention;

[0029] Figure 2 This is a schematic diagram of the overall structure of the X-ray single crystal diffraction sample sealing device in an embodiment of the present invention when the sealing cover is not installed;

[0030] Figure 3 This is a cross-sectional view of the overall structure of the X-ray single-crystal diffraction sample sealing device described in this embodiment of the invention;

[0031] Figure 4 for Figure 3A magnified view of a section at point A in the middle;

[0032] Figure 5 This is a cross-sectional view of the overall structure of the base of the X-ray single-crystal diffraction sample sealing device described in this embodiment of the invention;

[0033] Figure 6 This is a cross-sectional view of the overall structure of the sealing valve of the X-ray single crystal diffraction sample sealing device described in this embodiment of the invention;

[0034] Figure 7 This is a schematic diagram of the overall structure of the sealing valve of the X-ray single crystal diffraction sample sealing device described in this embodiment of the invention;

[0035] Figure 8 This is a schematic diagram illustrating the use of the X-ray single-crystal diffraction sample sealing device in an embodiment of the present invention.

[0036] In the picture:

[0037] 1. Base; 11. Chamber; 12. Countersunk hole; 13. Through hole; 14. Flange; 2. Sampling tube; 21. Outer tube; 22. Inner tube; 3. Sealing valve; 31. Internal channel; 311. First channel; 312. Second channel; 32. Plug; 33. Slotted groove; 4. Seal; 5. Sealing cover; 6. Sealing ring. Detailed Implementation

[0038] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this invention. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention.

[0039] In the description of this invention, it should be noted that the terms "upper," "lower," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the system or component referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. Furthermore, the terms "first," "second," etc., used to define components are merely for the convenience of distinguishing the aforementioned components. Unless otherwise stated, these terms have no special meaning and should not be construed as indicating or implying relative importance.

[0040] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; and they can refer to the internal connection of two components. Those skilled in the art can understand the specific meaning of the above terms in this invention based on the specific circumstances.

[0041] Single-crystal testing requires two steps: sample selection and transfer. Samples sensitive to oxygen, water, and temperature, or those prone to losing solvent molecules and efflorescence that prevents separation from the mother liquor, are typically transferred using a sealed tube method. This involves first using a pipette to remove the selected single-crystal sample, then transferring it into a conical capillary glass tube. Depending on the crystal size, the crystal will be positioned at different locations. The capillary tube is then cut off at both ends and sintered to seal it. This method has drawbacks such as complex operation, non-reusable glass tubes, and difficulty in accurately positioning the sample, leading to misalignment. Therefore, this invention provides an X-ray single-crystal diffraction sample sealing device and method, which enables sealed transfer of air-sensitive samples and allows for reusability.

[0042] Exemplary embodiments of the invention will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided to enable a more thorough understanding of the invention and to fully convey the scope of the invention to those skilled in the art.

[0043] like Figures 1-8 As shown, this embodiment of the invention provides an X-ray single-crystal diffraction sample sealing device, comprising:

[0044] Base 1, base 1 having a cavity 11 extending through its bottom;

[0045] Sampling tube 2 is airtightly connected to the top wall of chamber 11. The bottom end of sampling tube 2 is connected to the top end of chamber 11. Sampling tube 2 is used to absorb single crystal samples.

[0046] The sealing valve 3 is threaded into the chamber 11. The sealing valve 3 has an internal channel 31 that connects the top and bottom of the chamber 11. There is a sealing element 4 between the top of the sealing valve 3 and the top wall of the chamber 11. The sealing element 4 can cooperate with the sealing valve 3 to seal the bottom of the sampling tube 2.

[0047] In this embodiment of the invention, a negative pressure is first generated inside the base 1 using a pipette or similar device, and the air-sensitive sample is then drawn through the sampling tube 2. After sample drawing, the top of the sampling tube 2 is sealed with polyisobutylene or paraffin, and the bottom of the sampling tube 2 is sealed with a sealing valve 3. The air-sensitive sample and the sealing device are then transferred together to the crystal stage for single-crystal testing. Because both ends of the sampling tube 2 are sealed during the transfer process, and the mother liquor remains inside the sampling tube 2 after sample drawing, the sample is completely isolated from air and remains in the mother liquor environment during the transfer process, which maximizes the protection of the original state of the sample. Furthermore, after the single-crystal test is completed, the sealing material at the top of the sampling tube 2 can be removed, and the bottom of the sampling tube 2 can be opened through the sealing valve 3 to remove the sample and mother liquor from the sampling tube 2 for subsequent sample transfer. Therefore, this invention enables the sealed transfer of air-sensitive samples and has advantages such as ease of operation and reusability.

[0048] Furthermore, such as Figure 4 As shown, the sampling tube 2 includes an outer tube 21 and an inner tube 22. The inner tube 22 is disposed inside the outer tube 21 and communicates with the top of the chamber 11. The inner diameter of the outer tube 21 is larger than the size of the single crystal sample, and the inner diameter of the inner tube 22 is smaller than the minimum size of the single crystal sample. The height of the inner tube 22 is lower than the height of the outer tube 21. The outer tube 21 and the inner tube 22 can be thin tubes made of materials with high X-ray transmittance, such as polyimide or quartz.

[0049] like Figure 3 and Figure 5 As shown, the top wall of chamber 11 has a countersunk hole 12 and a through hole 13 coaxially arranged. The through hole 13 connects chamber 11 and countersunk hole 12. The outer tube 21 and the inner tube 22 are respectively inserted into the countersunk hole 12 and the through hole 13. The outer tube 21 is sealed to the side wall of the countersunk hole 12 by means of adhesive bonding or interference fit, and the inner tube 22 is sealed to the side wall of the through hole 13 by means of adhesive bonding or interference fit.

[0050] Preferably, the wall thickness of the outer tube 21 and the inner tube 22 is 0.01mm-0.02mm. This allows the outer tube 21 and the inner tube 22 to have good mechanical properties while having a certain X-ray transmittance, thereby ensuring the normal use of the outer tube 21 and the inner tube 22.

[0051] It should be noted that the height difference between the outer tube 21 and the inner tube 22 in this embodiment depends on the size and shape of the single crystal sample. Preferably, the height difference between the outer tube 21 and the inner tube 22 is 0.5mm-3mm.

[0052] In this embodiment, when the sampling tube 2 absorbs the single crystal sample, the inner diameter of the inner tube 22 is smaller than the minimum size of the single crystal sample. The single crystal sample will be blocked at the top of the inner tube 22, allowing for precise positioning of the sample. Therefore, in this embodiment, the position of the single crystal sample within the sampling tube 2 is constant each time it is absorbed, which is beneficial for positioning and alignment of the single crystal sample in subsequent tests.

[0053] It should be noted that the sampling tube 2 of the present invention is not limited to the sampling tube 2 of the above-described structure. In some other embodiments, other types of sampling tubes 2, such as tapered tubes, can also be used.

[0054] Furthermore, the sealing element 4 is a sealing ring, which is arranged around the periphery of the sampling tube 2. In this embodiment, when it is necessary to seal the bottom end of the sampling tube 2, the sealing valve 3 can be rotated upwards, and the sealing ring is pressed against the top wall of the chamber 11 by the top surface of the sealing valve 3. The top surface of the sealing valve 3 and the sealing ring cooperate to seal the top end of the sampling tube 2.

[0055] Preferably, the top end face of the sealing valve 3 also has a plug 32 corresponding to the bottom end of the sampling tube 2. In this embodiment, by providing a plug 32 on the top end face of the sealing valve 3, the plug 32 can block the bottom end of the sampling tube 2 when the sealing valve 3 and the sealing element 4 cooperate to seal the bottom end of the sampling tube 2, thereby further improving the sealing effect on the bottom end of the sampling tube 2.

[0056] It should be noted that other types of seals 4 may be used in some other embodiments, and the present invention does not limit this. For example, in some other embodiments, other types of seals 4, such as gaskets, may be used.

[0057] Specifically, such as Figure 3 As shown, the diameter of the top of the sealing valve 3 is smaller than the diameter of the top of the chamber 11. An air gap is formed between the circumferential sidewall of the top of the sealing valve 3 and the circumferential sidewall of the top of the chamber 11. The internal channel 31 includes an intersecting first channel 311 and a second channel 312. The first channel 311 is arranged axially along the sealing valve 3 and communicates with the bottom of the chamber 11. The second channel 312 is arranged radially along the sealing valve 3 and communicates with the air gap. The first channel 311 and the second channel 312 communicate with the top of the chamber 11 through the air gap. The sealing valve 3 also has a slot 33 for screwing the sealing valve 3.

[0058] Preferably, the base 1 is made of ferromagnetic material and its bottom dimensions match the dimensions of the crystal carrier. The base 1 is generally conical in shape, and its bottom surface also has steps whose size and shape match the top surface of the crystal carrier. With the above configuration, the base 1 of this embodiment can be directly adsorbed onto the crystal carrier by magnetic force during use, making installation convenient. Its bottom dimensions match the dimensions of the crystal carrier, and its bottom surface has steps whose size and shape match the top surface of the crystal carrier, enabling rapid alignment and improving the quality of test data. On the other hand, its overall conical shape can avoid interference with X-rays (incident light) and diffraction signals (outgoing light) during single crystal testing.

[0059] Furthermore, it also includes a sealing cover 5 mounted on the base 1. The bottom of the base 1 has a flange 14 opposite to the bottom surface of the sealing cover 5, and a sealing ring 6 is provided between the bottom surface of the sealing cover 5 and the flange 14. It is understood that the sealing cover 5 can be made of materials with good thermal conductivity such as copper or aluminum, and can be connected to the base 1 by means of threaded connection, snap-fit ​​connection, etc.

[0060] In this embodiment, by setting a sealing cover 5, when it is necessary to transfer the single crystal sample for a long time or over a long distance, the sealing cover 5 can be placed on the base 1 to seal the sampling tube 2, thereby providing further protection for the single crystal sample.

[0061] Preferably, the shape of the internal cavity of the sealing cover 5 matches the shape of the base 1 and the sampling tube 2. This can minimize the internal space of the sealing cover 5 and prevent the mother liquor in the sampling tube 2 from evaporating during the transfer process.

[0062] Example 2

[0063] This invention provides a method for using the X-ray single-crystal diffraction sample sealing device as described in Embodiment 1, comprising the following steps:

[0064] Step 1: Place the culture dish on the microscope stage and control the temperature of the stage using an inert gas temperature control system. Add an appropriate amount of solvent for growing single crystals to the culture dish. Take a small amount of mother liquor and single crystal sample and place them in the culture dish. Select a suitable single crystal sample under the microscope.

[0065] Step 2: Rotate the sealing valve 3 downwards to connect the bottom end of the sampling tube 2 with the top end of the chamber 11. Insert the pipette from the bottom end of the chamber 11 and take some of the mother liquor under the microscope to test the sealing performance of the connections between the components.

[0066] Step 3: Align the top of sampling tube 2 with the appropriate single crystal sample and create negative pressure in chamber 11 using a pipette. The single crystal sample is drawn in and stuck in sampling tube 2 under atmospheric pressure. The mother liquor can be drawn into sampling tube 2, chamber 11 and pipette head.

[0067] Step 4: Seal the top of sampling tube 2 with polyisobutylene or paraffin;

[0068] Step 5: Remove the pipette, rotate the sealing valve 3 upwards to seal the bottom of the sampling tube 2. When it is necessary to transfer single crystal samples for a long time or over a long distance, place the sealing cover 5 on the base 1.

[0069] Step 6: Transfer the sealing device to the die carrier for testing. If the base 1 is covered with a sealing cover 5, the sealing cover 5 must be removed first before quickly transferring the sealing device to the die carrier.

[0070] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.

Claims

1. A sample sealing device for X-ray single-crystal diffraction, characterized in that, include: A base (1) having a cavity (11) extending through its bottom; Sampling tube (2), the sampling tube (2) is airtightly connected to the top wall of the chamber (11), and the bottom end of the sampling tube (2) is connected to the top end of the chamber (11); A sealing valve (3) is threaded into the chamber (11). The sealing valve (3) has an internal channel (31) that connects the top end of the chamber (11) and the bottom end of the chamber (11). A sealing element (4) is provided between the top end of the sealing valve (3) and the top wall of the chamber (11). The sealing element (4) can cooperate with the sealing valve (3) to seal the bottom end of the sampling tube (2). The diameter of the top end of the sealing valve (3) is smaller than the diameter of the top end of the chamber (11). An air gap is formed between the circumferential sidewall of the top end of the sealing valve (3) and the circumferential sidewall of the top end of the chamber (11). The internal channel (31) communicates with the top end of the chamber (11) through the air gap. A sealing cover (5) is provided on the base (1). The bottom of the base (1) has a flange (14) that is opposite to the bottom surface of the sealing cover (5). A sealing ring (6) is provided between the bottom surface of the sealing cover (5) and the flange (14). The shape of the internal cavity of the sealing cover (5) matches that of the base (1) and the sampling tube (2).

2. The X-ray single-crystal diffraction sample sealing device as described in claim 1, characterized in that, The sampling tube (2) includes an outer tube (21) and an inner tube (22). The inner tube (22) is disposed inside the outer tube (21) and communicates with the top of the chamber (11). The inner diameter of the outer tube (21) is larger than the size of the single crystal sample, and the inner diameter of the inner tube (22) is smaller than the minimum size of the single crystal sample. The height of the inner tube (22) is lower than the height of the outer tube (21).

3. The X-ray single-crystal diffraction sample sealing device as described in claim 2, characterized in that, The top wall of the chamber (11) has a countersunk hole (12) and a through hole (13). The through hole (13) connects the chamber (11) and the countersunk hole (12). The outer tube (21) and the inner tube (22) are respectively inserted into the countersunk hole (12) and the through hole (13).

4. The X-ray single-crystal diffraction sample sealing device as described in claim 1, characterized in that, The sealing element (4) is a sealing ring, which is arranged around the sampling tube (2).

5. The X-ray single-crystal diffraction sample sealing device as described in claim 4, characterized in that, The sealing valve (3) also has a plug (32) on its top end face corresponding to the bottom end of the sampling tube (2).

6. The X-ray single-crystal diffraction sample sealing device as described in claim 1, characterized in that, The base (1) is made of ferromagnetic material and the base (1) is cone-shaped.

7. A method of using the X-ray single-crystal diffraction sample sealing device as described in any one of claims 1-6, characterized in that, Includes the following steps: Place the culture dish on the microscope stage, add an appropriate amount of solvent for growing single crystals into the culture dish, take a small amount of mother liquor and single crystal sample and place them in the culture dish, and select a suitable single crystal sample under the microscope. Rotate the sealing valve (3) downwards so that the bottom end of the sampling tube (2) is connected to the top end of the chamber (11). Insert a pipette from the bottom end of the chamber (11) and aspirate some mother liquor under a microscope to test the sealing performance of the connections between the components. The top of the sampling tube (2) is aligned with a suitable single crystal sample and a negative pressure is formed in the chamber (11) by a pipette. The single crystal sample is drawn in and stuck in the sampling tube (2) under atmospheric pressure. The mother liquor can be drawn into the sampling tube (2), the chamber (11) and the pipette head. The top of the sampling tube (2) is sealed; Remove the pipette and rotate the sealing valve (3) upward to seal the bottom end of the sampling tube (2); The sealing device was transferred to the die carrier for testing.

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