Glass crucible tray bearing base for DSC (differential scanning calorimetry)

Abstract

The utility model discloses a glass crucible tray bearing base for DSC (differential scanning calorimetry), and belongs to the technical field of experimental equipment design. The glass crucible plate is used for placing a sample to be analyzed, the bearing base comprises a base plate and a bearing body, the bearing body is fixed on the upper surface of the base plate, a groove body for accommodating the glass crucible plate is formed in the upper surface of the bearing body, and a grabbing plate convenient for a manipulator to grab is arranged on the outer wall surface of the groove body in an outward extending manner; the grabbing disc is parallel to the base plate, and the gravity center of the groove body, the gravity center of the grabbing disc and the gravity center of the base plate are located on the same vertical line. The utility model has the advantages that the grabbing disc is additionally arranged on the groove body for bearing the base, so that the base can be conveniently grabbed and moved by a manipulator, the risk of sample scattering caused by base toppling is reduced, and the data accuracy is improved; the thickness of the grabbing disc and the weight range of the base are further increased, and the heat transfer efficiency is guaranteed.

Description

Technical Field

[0001] The utility model belongs to the technical field of experimental equipment design, and particularly relates to a glass crucible plate bearing base for DSC. Background Art

[0002] Differential Scanning Calorimetry (DSC) is a thermal analysis method used to study the thermal properties and thermal behavior of materials. DSC studies the thermal properties and thermal behavior of materials by measuring the temperature difference between a sample and a reference during heating.

[0003] For the hazard evaluation of active chemicals, DSC is often used as one of the methods for thermal stability testing. The sample needs to be run at high temperature in the DSC to check whether there is a decomposition reaction. The complex reaction mechanism of the decomposition reaction poses a challenge to determining the exact decomposition products, resulting in an unknown final pressure. In addition, the samples required by large companies vary greatly in composition, physical properties (such as vapor pressure), and reactivity. When using inappropriate DSC sample containers, such as the most common aluminum crucibles, stainless steel crucibles, etc., the container and the material itself interact, causing changes in the data and providing erroneous results. And because the material sample size is small, the contact surface between the sample and the sample container to be analyzed for DSC testing is relatively high, and good pressure resistance is required during the test. Therefore, the correct selection of the container for the sample to be analyzed is crucial to data quality.

[0004] It has been experimentally verified that the use of flame-sealed capillary glass tubes and glass ampoules as DSC sample containers to evaluate the thermal stability of reactive chemicals is an economical and feasible method. Sealed capillary glass tubes and sealed glass ampoules require a base to place them, and they also need to provide fast and efficient heat transfer between the base and the DSC sensor. When designing these bases, it is necessary to use high thermal conductivity materials to ensure good contact between all parts, polish the bottom surface as flat as possible (to reduce thermal resistance between the base and the DSC sensor), and make it as light as possible (to ensure fast thermal response).

[0005] In actual use, the base needs to be grabbed and moved to a specific placement position of the differential scanning calorimeter for experimental testing. However, because the existing base is not designed to facilitate grabbing, problems such as tipping, sample spilling, and sample shifting to an inappropriate position often occur, making the results of the automated test inaccurate.

[0006] Therefore, there is an urgent need to develop a glass crucible plate supporting base for DSC to solve the above problems. Utility Model Content

[0007] The utility model aims to meet practical needs and provide a glass crucible plate bearing base for DSC, which avoids the occurrence of tipping caused by unstable gripping of a manipulator and improves heat transfer efficiency.

[0008] In order to achieve the above-mentioned purpose of the utility model, the purpose of the utility model is to provide a glass crucible plate supporting base for DSC, the glass crucible plate is used to place samples to be analyzed, the supporting base includes a base and a receiving body, the receiving body is fixed on the upper surface of the base, the upper surface of the receiving body is provided with a trough body for accommodating the glass crucible plate, and a grabbing plate for facilitating grabbing by a robot is extended outward from the outer wall surface of the trough body, the grabbing plate is parallel to the base, and the center of gravity of the trough body and the grabbing plate is on the same vertical line as the center of gravity of the base.

[0009] In the above-mentioned solution of the glass crucible plate supporting base for DSC, the glass crucible plate is a cylindrical capillary glass tube with a diameter less than 5 mm, and the trough body is provided with a cylindrical groove for accommodating the capillary glass tube.

[0010] In the above-mentioned solution of the glass crucible plate supporting base for DSC, the height of the opening end of the cylindrical groove is greater than the height of the bottom of the cylindrical groove.

[0011] In the above-mentioned solution of the glass crucible plate supporting base for DSC, the angle between the central axis of the cylindrical groove and the horizontal plane ranges from 6° to 20°.

[0012] In the above-mentioned solution of the glass crucible tray supporting base for DSC, the glass crucible tray is a glass ampoule, and the upper surface of the trough body is provided with a spherical groove for accommodating the glass ampoule body.

[0013] In the above-mentioned solution of the glass crucible tray supporting base for DSC, a notch for placing the bottleneck of the glass ampoule is provided at the upper edge of the spherical groove.

[0014] In the above-mentioned solution of the glass crucible tray supporting base for DSC, when the glass ampoule is placed in the spherical groove and the bottleneck of the glass ampoule is stuck in the notch, the angle between the central axis of the glass ampoule and the horizontal plane ranges from 6° to 20°.

[0015] In the above-mentioned solution of the glass crucible plate supporting base for DSC, the thickness of the grabbing plate is less than or equal to 0.67 mm, and the mass of the supporting base is less than or equal to 542 mg.

[0016] In the above-mentioned solution of the glass crucible tray supporting base for DSC, the lower surface of the bottom tray contacts the DSC heat flow sensor.

[0017] In the above-mentioned solution of the glass crucible tray supporting base for DSC, the bottom plate, the receiving body, the trough body and the grabbing plate are an integrally formed structure.

[0018] The advantages and positive effects of this application are:

[0019] (1) A grabbing plate is added to the trough of the base to facilitate the robot to grab and move the base, reducing the risk of sample spillage caused by the base tipping over and improving the accuracy of the data;

[0020] (2) The thickness of the grab plate and the weight range of the base are further provided to ensure the heat transfer efficiency;

[0021] (3) For the supporting base for the capillary glass tube, the cylindrical groove in the groove body is designed to be open at one end and closed at the other end, and the groove body is set to be inclined, so that the capillary glass tube can be placed in it in an inclined state, further reducing the risk of the capillary glass tube falling during the transfer process, while improving the heat transfer efficiency.

[0022] (4) For the supporting base used for the glass ampoule, when the bottleneck is locked in the notch, the bottleneck is tilted upward, which also reduces the risk of the sample to be analyzed falling during the transfer process. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings required for use in the description of the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.

[0024] Figure 1 A schematic structural diagram of a supporting base for a capillary glass tube provided in an embodiment of the utility model is shown;

[0025] Figure 2 The structure schematic diagram of the supporting base for the glass ampoule provided in the embodiment of the utility model is shown;

[0026] Figure 3 The result diagram of the comparative test provided by the second embodiment of the utility model is shown;

[0027] Figure 4 The heat conduction of the same sample tested with five different thicknesses of the grabbing plate provided in the fourth embodiment of the utility model is shown;

[0028] Figure 5 The figure shows the fitting result of the experimental heat transfer time constant provided by the fourth embodiment of the utility model;

[0029] Figure 6 The figure shows how the proportion of tailing heat loss provided by the fourth embodiment of the present invention varies with samples of different masses.

[0030] In the figure, 1, chassis; 2, receiving body; 3, trough body; 4, grab plate; 5, notch. DETAILED DESCRIPTION

[0031] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0032] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features in the embodiments can be combined with each other.

[0033] All numerical designations, such as pH, temperature, length, flow, including ranges, are approximate. It is to be understood, although not always expressly stated, that all numerical designations are preceded by the term "about".

[0034] In the description of the invention of the present utility model, it should be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the invention of the utility model and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as a limitation on the invention of the utility model. In addition, the terms "first", "second", etc. are only used for descriptive purposes, and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, features defined as "first", "second", etc. may explicitly or implicitly include one or more of the features. In the description of the invention of the present utility model, unless otherwise specified, "multiple" means two or more.

[0035] In the description of the invention of the utility model, it should be noted that, unless otherwise clearly specified and limited, the terms "installation", "connection" and "connection" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the invention of the utility model can be understood according to specific circumstances.

[0036] See also Figures 1 to 6 ;

[0037] First embodiment

[0038] The utility model provides a glass crucible plate bearing base for DSC, the glass crucible plate is used for placing samples to be analyzed, specifically, the bearing base comprises a bottom plate 1 and a receiving body 2, the receiving body 2 is fixed on the upper surface of the bottom plate 1, the upper surface of the receiving body 2 is provided with a groove body 3 for accommodating the glass crucible plate, a grabbing plate 4 is extended outwardly from the outer wall surface of the groove body 3 for easy grasping by a robot, the grabbing plate 4 is parallel to the bottom plate 1, and the center of gravity of the groove body 3 and the grabbing plate 4 is located on the same vertical line as the center of gravity of the bottom plate 1.

[0039] In actual use, it is necessary to use a placing device to place the sample at a specific placement position of the differential scanning calorimeter. The placing device is connected to a manipulator for grabbing the sample base, but there is no position on the base for the manipulator to engage, and the grabbing is often unstable, resulting in the sample falling or not being placed stably, causing the base to tip over and the sample to spill. Based on the above considerations, a grabbing plate 4 is provided, and the center of gravity is taken into consideration during the design, which is more convenient for the operation of the manipulator; wherein, the grabbing plate 4 is arranged parallel to the base 1 and can stably contact the surface of the placement position when placed, further reducing the risk of the base tipping over.

[0040] The lower surface of the chassis 1 contacts the DSC heat flow sensor. The model of the heat flow sensor is not limited here, and is subject to the requirements of the present application.

[0041] It should be noted that the present application does not specifically limit the shape of the grabbing plate 4, and the edge of the grabbing plate 4 can be circular, elliptical, etc., which is also based on meeting actual needs.

[0042] Exemplarily, the area of ​​the plane shape formed by the edge of the grabbing plate 4 can be larger than the lower surface area of ​​the chassis 1 to facilitate the robot to perform grabbing actions. Similarly, it can also be less than or equal to meet the grabbing requirements.

[0043] Second embodiment

[0044] Based on the content of the first embodiment, further optimization is performed for the case where the glass crucible plate is a cylindrical capillary glass tube with a diameter less than 5 mm:

[0045] A cylindrical groove for accommodating the capillary glass tube is provided on the tank body 3. When injecting samples, the manipulator will generate certain vibrations during the grabbing and transportation process. Based on the particularity of the capillary glass tube, if the capillary glass tube is set horizontally, there is a risk of the capillary glass tube falling or shifting, and the sample to be analyzed is not within the base, and the differential scanning calorimeter cannot identify this situation, resulting in the measurement of empty samples or improper positions. Therefore, the height of the opening end of the cylindrical groove is set to be greater than the bottom height of the cylindrical groove, that is, the capillary glass tube is in an inclined state when placed therein.

[0046] Through experiments, by setting the groove body 3 at different angles, the correlation between the angle size and the number of drops can be clearly obtained, as shown in Table 1. Therefore, the inclination angle is further optimized, and the angle between the central axis of the cylindrical groove and the horizontal plane can range from 6° to 20°, such as 9°, 15° or 20°.

[0047] Table 1 Experimental results of the number of drops under different angle settings

[0048] Angle / ° Completely dropped The bottom no longer touches 0 4 9 3 1 5 6 0 2 9 0 0 12 0 0 15 0 0

[0049] The fact that the bottom no longer contacts the capillary glass tube indicates whether the capillary glass tube has a tendency to fall. It should be noted that the above angle range is only an example, and different settings can be made according to actual needs.

[0050] In addition, the cylindrical space for accommodating the capillary glass tube in the existing trough body 3 is open at both ends; while in the present application, there is only one open end, so that the heat generated by the sample can be transmitted to the bottom plate 1 to the greatest extent, thereby being detected by the temperature sensor, which can greatly improve the heat transfer efficiency of the sample.

[0051] The following comparative experiments were conducted:

[0052] Experimental conditions: The instrument model is DSC Q2500, T0 sealed aluminum pan is used for correction, the test sample is the same sample (6.835 mg indium metal), the test temperature range is 100-200°C, the heating rate is 10°C / min, the integration interval is 155-180°C, the inclination angle of the slot body 3 is set to 9°, and a set of comparative experiments is set. In experiment a, a cylindrical groove is set to have one end open and the other end closed. In experiment b, the existing slot body structure is used, that is, both ends of the cylindrical groove are open.

[0053] Under the above experimental design, we can get Figure 3The results shown in FIG. 1 are due to the fact that in the related structure of the present application, the sample is concentrated at the bottom of the cylindrical groove. At this time, there is only one contact point, which avoids the sample being dispersed in the capillary glass tube, thereby preventing the sample from being dispersed in the capillary glass tube and causing the sample to be tested at different positions. Figure 3 The multi-peak problem shown, as well as the problem of sample scattering from the capillary glass tube, resulting in the problem of no sample to be tested.

[0054] Third embodiment

[0055] Based on the content of the first embodiment, the glass crucible plate includes a glass ampoule, which is a small glass container for holding test samples, with a small capacity, including a bottle body and a bottleneck; it should be noted that in the present application, the bottle body is a spherical structure, and the following content is further optimized for the case where the bottle body is a sphere:

[0056] The upper surface of the groove body 3 is provided with a spherical groove for accommodating the glass ampoule body, and a notch 5 for placing the bottleneck of the glass ampoule is provided at the upper edge of the spherical groove. Exemplarily, when the glass ampoule is placed in the spherical groove and the bottleneck of the glass ampoule is stuck in the notch 5, the angle between the central axis of the glass ampoule and the horizontal plane can be in the range of 9° to 20°, such as 9°, 15° or 20°. The setting of this angle avoids the situation where the sample to be analyzed is spilled, or even the situation where an empty sample is tested.

[0057] It should be noted that the above angles are only for illustration and different settings can be made according to actual needs.

[0058] Fourth embodiment

[0059] Based on the content of the first embodiment, the thickness of the grabbing plate 4 is optimized; theoretically, the grabbing plate 4 cannot be too large or too thick, otherwise it will affect the detection of the signal by the differential scanning calorimeter, which is the reason for the excessive heat transfer inertia; and if the grabbing plate 4 is too thin, it is easy to be scratched by the robot, and the damage rate is high, which is not conducive to repeated use in practice. Therefore, it is necessary to comprehensively design the grabbing plate 4 under various conditions, and the following experiments were conducted:

[0060] Experimental conditions: The instrument model is DSC Q2500, using T0 sealed aluminum pan for correction, the test sample is the same sample (6.835 mg indium metal), the test temperature range is 100-200°C, the heating rate is 10°C / min, the integration interval is 155-180°C, and the base for glass capillaries is used for the experiments.

[0061] like Figure 4As shown, the thickness of the grab plate 4 is increased within the range of 0.45 mm to 1.40 mm. In this application, 5 groups of different thicknesses are set for experiments. As the thickness increases, the overall mass of the base also increases, resulting in an increase in the heat transfer inert material, an increase in the heat transfer buffer, and a decrease in the heat transfer rate, thus resulting in an increase in the heat transfer time constant. The experimental results are summarized in Table 2.

[0062] In addition, the exact value of the melting heat of indium is 28.71 J / g, but the slow heat transfer during the test causes severe tailing, resulting in increased heat loss, and the tested melting heat of indium continues to decrease, such as Figure 6 As shown, it is reduced to the range of 25.653 to 27.681 J / g, and the heat loss accounts for 3.6% to 10.6%.

[0063] Table 2 Experimental results of different grab plate thicknesses

[0064] Thickness / mm Total mass / mg Indium melting heat / (J / g) Time constant / s Proportion of heat loss due to tailing 0.45 454.911 27.681 4.09 3.6％ 0.70 552.112 27.139 5.06 5.5％ 0.91 636.376 26.874 6.27 6.4％ 1.13 724.548 26.288 7.41 8.4％ 1.40 829.121 25.653 9.73 10.6％

[0065] like Figure 5 As shown in the figure, taking the total mass of 454.911 mg and 829.121 mg as examples, the relationship between the base mass M and the proportion of tailing loss heat (error E) is obtained through fitting:

[0066] E = 1.25 × 10 -7 ·M 2 +2.45×10 -5 ·M-4.21×10 -5 ,

[0067] In this embodiment, if the error is to be ensured to be less than 5%, it can be calculated that the total mass of the base must be no greater than 542 mg, that is, the thickness of the robot gripping plate 4 is no greater than 0.67 mm.

[0068] It should be noted that this embodiment is described by taking the base for the capillary glass tube as an example, and the base for the glass ampoule is the same, which will not be described here.

[0069] Fifth embodiment

[0070] Based on the above embodiments, Figure 1 and Figure 2 As shown, the bottom plate 1, the receiving body 2, the groove body 3 and the grabbing plate 4 are an integrally formed structure. For example, no obvious difference can be seen between the receiving body 2 and the groove body 3 in the base for a glass ampoule, thereby improving the heat transfer efficiency of the overall device.

[0071] Sixth embodiment

[0072] Based on the above embodiments, the present application provides an application of a glass crucible tray support base for DSC in the hazard assessment of active chemicals. Other contents refer to the above embodiments and will not be described here.

[0073] Based on the above technical solution, the tipping caused by unstable grasping of the robot is avoided and the heat transfer efficiency is improved.

[0074] The above is only a preferred embodiment of the present invention. It should be pointed out that, for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be regarded as the protection scope of the present invention.

Claims

1. A glass crucible tray supporting base for DSC, wherein the glass crucible tray is used to place a sample to be analyzed, characterized in that: The bearing base comprises a chassis (1) and a receiving body (2), wherein the receiving body (2) is fixed on the upper surface of the chassis (1), and a trough body (3) for accommodating the glass crucible plate is provided on the upper surface of the receiving body (2), and a grabbing plate (4) for facilitating grabbing by a robot extends outward from the outer wall surface of the trough body (3), and the grabbing plate (4) is parallel to the chassis (1), and the center of gravity of the trough body (3) and the grabbing plate (4) is located on the same vertical line as the center of gravity of the chassis (1).

2. The glass crucible tray supporting base for DSC according to claim 1, characterized in that: The glass crucible plate is a cylindrical capillary glass tube with a diameter less than 5 mm, and the trough body (3) is provided with a cylindrical groove for accommodating the capillary glass tube.

3. The glass crucible tray supporting base for DSC according to claim 2, characterized in that: The height of the opening end of the cylindrical groove is greater than the height of the bottom of the cylindrical groove.

4. The glass crucible tray supporting base for DSC according to claim 3, characterized in that: The angle between the central axis of the cylindrical groove and the horizontal plane ranges from 6° to 20°.

5. The glass crucible tray supporting base for DSC according to claim 1, characterized in that: The glass crucible plate is a glass ampoule, and the upper surface of the trough body (3) is provided with a spherical groove for accommodating the glass ampoule body.

6. The glass crucible tray supporting base for DSC according to claim 5, characterized in that: A notch (5) for accommodating the bottleneck of the glass ampoule is provided at the upper edge of the spherical groove.

7. The glass crucible tray supporting base for DSC according to claim 6, characterized in that: When the glass ampoule is placed in the spherical groove and the bottleneck of the glass ampoule is stuck in the notch (5), the angle between the central axis of the glass ampoule and the horizontal plane is in the range of 6° to 20°.

8. The glass crucible tray supporting base for DSC according to any one of claims 1 to 7, characterized in that: The thickness of the grabbing plate (4) is less than or equal to 0.67 mm, and the mass of the bearing base is less than or equal to 542 mg.

9. The glass crucible tray supporting base for DSC according to claim 1, characterized in that: The chassis (1), the receiving body (2), the trough body (3) and the grabbing plate (4) are an integrally formed structure.

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