Sample container and thermal analysis device

Abstract

To provide a sample container and thermal analysis device, which enable stable observation of a measurement sample during thermal analysis.SOLUTION: A sample container 2 for use with a thermal analysis device 1 designed to measure thermal behavior associated with temperature changes of a measurement sample S due to heating or cooling and to observe the measurement sample is provided, the sample container comprising a cylindrical main body 21 with a bottom and an open top, a transparent or translucent holding plate 22 accommodated inside the main body and designed to hold down a measurement sample mounted on a bottom surface of the main body from above, and a lid 24 with a hole 24h for observing the measurement sample, the lid being accommodated inside the main body and mounted on a top surface of the holding plate.SELECTED DRAWING: Figure 2

Description

Technical Field

[0001] The present invention relates to a sample container used in a thermal analysis apparatus for measuring a physical change including thermogravimetry or calorimetry of a measurement sample accompanying a temperature change by heating a (measurement) sample, and a thermal analysis apparatus using the same.

Background Art

[0002] Conventionally, as a method for evaluating the temperature characteristics of a sample, a method called thermal analysis has been performed, in which the sample is heated and the physical change of the sample accompanying the temperature change is measured. Thermal analysis is defined in JIS K 0129:2005 "General Rules for Thermal Analysis", and all methods for measuring the physical properties of a measurement object (sample) when the temperature of the measurement object (sample) is program-controlled are regarded as thermal analysis. Commonly used thermal analysis includes (1) differential thermal analysis (DTA) for detecting temperature (temperature difference), (2) differential scanning calorimetry (DSC) for detecting heat flow difference, (3) thermogravimetry (TG) for detecting mass (weight change), (4) thermomechanical analysis (TMA) for detecting mechanical properties, and (5) dynamic viscoelasticity measurement (DMA). In addition, there is also a thermogravimetry / differential thermal simultaneous measurement apparatus (TG / DTA or TG / DSC) that simultaneously measures thermogravimetry and differential heat.

[0003] In recent years, there has been a desire to observe the state of a sample during thermal analysis. A thermal analysis apparatus is known in which an opening is provided in a heating furnace for heating the sample, and the sample can be observed through this opening (see, for example, Patent Documents 1 and 2). In such an observation, a sample container in the form of an open-top bottomed cylinder with an open upper part as described in Patent Document 2 is used.

[0004] By the way, in film-like samples such as polymer films and papers, thermal deformation such as shrinkage and warping may occur during heating. However, in conventional open-type sample containers, this thermal deformation cannot be reduced, while in sealed-type sample containers, there is a problem that the sample cannot be observed. In addition, in a thermal analysis apparatus for observing a sample container in the prior art, when thermal deformation occurs during heating or cooling, changes in the inclination of the sample surface cause changes in the specular reflection and angle of the reflected light, which may inhibit the observation of the color and structure of the sample, or the position of the sample being observed may move, resulting in a change in the analyzed region of the sample. Therefore, a technique has been reported (Patent Document 3) in which a transparent or translucent pressing plate is placed on the upper surface of the sample, and the sample is sandwiched between the bottom surface of the sample container and the pressing plate to suppress deformation of the sample.

Prior Art Documents

Patent Documents

[0005]

Patent Document 1

Patent Document 2

Patent Document 3

Summary of the Invention

Problems to be Solved by the Invention

[0006] However, since the pressing plate described in Patent Document 3 presses the sample against the bottom surface of the sample container by its own weight, the pressing of the sample may be insufficient, or it may be difficult to uniformly press the entire surface of the sample. In addition, when the thermal deformation of the sample is severe, the pressing plate may bend under the deformation force of the sample, or the sample may shrink, making it difficult to observe the sample.

[0007] Therefore, the present invention has been made to solve the above problems, and an object thereof is to provide a sample container and a thermal analysis apparatus capable of stably observing a measurement sample during thermal analysis.

Means for Solving the Problems

[0008] In order to achieve the above object, a sample container of a thermal analyzer is a sample container used in a thermal analyzer that measures the thermal behavior accompanying temperature changes caused by heating or cooling of a measurement sample and observes the measurement sample, and has a bottomed cylindrical main body with an open top, a pressing plate that is transparent or translucent and is housed inside the main body and presses the measurement sample placed on the bottom surface of the main body from above, and a lid portion that is housed inside the main body, placed on the upper surface of the pressing plate, and has a hole for observing the measurement sample.

[0009] According to this sample container of the thermal analyzer, since the lid portion is placed on the measurement sample in addition to the pressing plate, the pressing of the measurement sample is sufficient, the entire surface of the measurement sample can be uniformly pressed, deformation of the measurement sample and the pressing plate can be suppressed, and the measurement sample can be stably observed during thermal analysis.

[0010] In the sample container of the thermal analyzer of the present invention, further, pressing means for pressing the lid portion toward the pressing plate may be provided. According to this sample container of the thermal analyzer, since the lid portion is pressed by the pressing means, the pressing plate presses the measurement sample via the lid portion, the pressing of the measurement sample becomes even more sufficient, the entire surface of the measurement sample can be uniformly pressed, and deformation of the measurement sample and the pressing plate can be further suppressed.

[0011] In the sample container of the thermal analyzer of the present invention, the lid portion forms a flange that vertically rises upward from its outer peripheral edge, the pressing means is the opening edge portion of the main body portion and the flange, and at least a part of the opening edge portion and the flange may be bendable downward together. According to this sample container of the thermal analyzer, the lid portion can be easily pressed by bending the opening edge portion and the flange.

[0012] In the sample container of the thermal analyzer of the present invention, the sample container has the measurement sample between the bottom surface of the main body portion and the pressing plate, and the pressing means may be composed of a bent portion in which at least a part of the opening edge portion and the flange are bent downward together. According to the sample container of this thermal analyzer, the lid can be easily pressed by the opening edge and the bent portion where the flange is bent.

[0013] In the sample container of the thermal analyzer of the present invention, when the equivalent circle diameter of the lid is C1 and the equivalent circle diameter of the hole is C2, 0.4 ≦ C2 / C1 ≦ 0.9 may be satisfied.

[0014] In the sample container of the thermal analyzer of the present invention, the thickness of the lid may be equal to or greater than the thickness of the side wall of the main body portion.

[0015] The thermal analyzer of the present invention includes the sample container of the thermal analyzer, a heating furnace that surrounds the sample container and has an observation opening, and imaging means that can observe the measurement sample through the observation opening, and is characterized by measuring the thermal behavior accompanying the temperature change of the measurement sample in the heating furnace.

[0016] The thermal analyzer of the present invention may be a differential thermal analyzer, a differential scanning calorimeter, or a thermogravimetric analyzer.

[0017] The thermal analyzer of the present invention further includes image processing means for generating predetermined color information from the image data of the measurement sample acquired by the imaging means, and the color information and the thermal behavior may be superimposed and displayed with respect to temperature.

Advantages of the Invention

[0018] According to the present invention, a sample container and a thermal analyzer capable of stably observing a measurement sample during thermal analysis can be obtained.

Brief Description of the Drawings

[0019]

Figure 1

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Figure 10

Mode for Carrying Out the Invention

[0020] Hereinafter, embodiments of the present invention will be described with reference to the drawings. FIG. 1 is a cross-sectional view showing the configuration of a thermal analyzer according to an embodiment of the present invention. The thermal analyzer 1 is a differential scanning calorimeter (DSC), and has the same configuration as a conventional differential scanning calorimeter except that a window 11W through which the inside can be observed is provided in the lid 11 of the heating furnace 10, so an overview will be described.

[0021] The thermal analyzer 1 includes a measurement sample container 2 for storing a measurement sample S, a reference material container 3 for storing a reference material R, a heating furnace 10, a thermal resistor 4 connected between the measurement sample container 2 and the reference material container 3 and the heating furnace 10 to form a heat flow path therebetween, a measurement sample side thermocouple 7, a reference material side thermocouple 8, a light source 31 such as an LED serving as illumination means for irradiating at least the measurement sample S with visible light, a CCD camera 32 serving as imaging means for imaging at least the measurement sample S, and a personal computer 50. A coil-shaped heater 12 is wound around the outer periphery of the heating furnace 10 to heat the heating furnace 10. The outside of the heater 12 is covered with a cover (not shown). The CCD camera 32 is, for example, an area scan type, but may also be a line scan type or the like, or other solid-state imaging devices such as a CMOS camera may be used.

[0022] The personal computer 50 includes a CPU (Central Processing Unit) 51, a storage unit 52 such as a hard disk, a display unit 53 such as a liquid crystal monitor, and a keyboard, a mouse, etc. (not shown).

[0023] The heating furnace 10 is formed in a cylindrical shape, and the cross-section along the axial direction is in an H shape. And a substantially double-disk-shaped heat plate 5 is placed above an annular protrusion protruding radially inward from the center in the axial direction. Furthermore, the measurement sample container 2 and the reference substance container 3 are placed on the upper surface of the heat plate 5 via two heat resistors 4, respectively, and the measurement sample container 2 and the reference substance container 3 are housed in the internal space surrounded by the heating furnace 10.

[0024] The measurement sample S is accommodated in the measurement sample container 2, and a pressing plate 22 and a lid portion 24 (Fig. 2) are placed on the upper surface of the measurement sample S. Here, the pressing plate 22 is transparent or translucent and is made of a material that transmits visible light at a predetermined light transmittance. As the transparent (translucent) material, quartz glass, sapphire glass, or YAG (yttrium aluminum garnet) ceramics, Tempax, Neoceram (registered trademark), Vycor, Pyrex (registered trademark) can be preferably used. On the other hand, for the reference substance container 3 holding the reference substance R, in order to ensure that the measurement sample S and the reference substance R are heated under the same conditions in the heating furnace 10, it is desirable to place the same pressing plate as the measurement sample container on the reference substance R. Note that it is not necessary to place a pressing plate on the reference substance R.

[0025] The thermocouple 7 on the measurement sample side and the thermocouple 8 on the reference material side penetrate the heat resistor 4 and the heat plate 5, and the tips thereof are connected to the lower surfaces of the measurement sample container 2 and the reference material container 3 by brazing or the like. On the other hand, the other ends of the thermocouple 7 on the measurement sample side and the thermocouple 8 on the reference material side are drawn out below the heating furnace 10 and connected to an amplifier 14 forming a signal processing circuit. In this way, the thermocouple 7 on the measurement sample side and the thermocouple 8 on the reference material side form a so-called differential thermocouple, and can detect the temperature difference between the measurement sample S and the reference material R. This temperature difference is recorded as a heat flow difference signal. On the other hand, the temperature of the measurement sample is recorded from the thermocouple 7 on the measurement sample side.

[0026] Furthermore, the temperature of the heating furnace 10 is input to the CPU 51 via various control circuits, and the CPU 51 controls the energization of the heater 12 to control the heating furnace 10 to be heated or cooled at a constant speed.

[0027] Also, a lid 11 is detachably placed on the upper end opening of the heating furnace 10, blocking the inside of the heating furnace 10 from the outside air. Furthermore, a window 11W made of quartz glass is provided at a portion of the lid 11 that overlaps the measurement sample container 2 in the axial direction of the heating furnace 10, and a CCD camera 32 is arranged above the window 11W. Also, a light source 31 for illuminating the measurement sample S in the heating furnace 10 through the window 11W is arranged above the window 11W and on a line different from the axis of the CCD camera 32. Incident light (visible light) 31L is irradiated from the light source 31 to the measurement sample S, and the CCD camera 32 acquires the luminance and intensity of the reflected light 32L from the measurement sample S.

[0028] Filters 31F and 32F are respectively arranged between the window 11W and the light source 31, and between the window 11W and the CCD camera 32, irradiating only light of a specific component to the window 11W and allowing only the reflected light of the specific component to be received by the CCD camera 32. However, the filters 31F and 32F are not essential. Also, in the case of coaxial epi-illumination (half mirror type), the optical axes of the light source 31 of the irradiation light and the camera 32 coincide.

[0029] Next, the measurement sample container 2 according to the first embodiment of the present invention will be described by taking the measurement sample container 2 as an example. FIG. 2 is a perspective view showing the configuration of the measurement sample container 2, and FIG. 3 is a cross-sectional view along the axial direction L of the measurement sample container 2. The measurement sample container 2 includes a main body portion 21 having a bottomed cylindrical shape with an open upper portion, a pressing plate 22, and a lid portion 24. The pressing plate 22 and the lid portion 24 have a substantially disk shape with the same diameter as the inner diameter of the main body portion 21 or a smaller diameter than the inner diameter. The pressing plate 22 is transparent or translucent as described above, and presses the measurement sample S placed on the bottom surface of the main body portion 21 from above. The main body portion 21 and the lid portion 24 are made of, for example, aluminum (alloy).

[0030] The lid portion 24 is placed on the upper surface of the pressing plate 22, and one hole 24h for observing the measurement sample is opened at the center. Further, the outer peripheral edge 24e of the lid portion 24 rises vertically upward to form a flange. The number of the holes 24h is not limited, and the position of the holes 24h is not limited to the center.

[0031] Here, as shown in FIG. 4, with the measurement sample S disposed between the bottom surface of the main body portion 21 and the pressing plate 22, at least a part (in this example, the entire circumference) of the opening edge portion 21e of the main body portion 21 and the outer peripheral edge (flange) 24e of the lid portion 24 are bent downward together, thereby forming a bent portion 26. By forming the bent portion 26, the lid portion 24 is pressed downward (toward the pressing plate 22), so that the bent portion 26 corresponds to the "pressing means" in the claims. In order to enable bending, the opening edge portion (side wall in this example) 21e of the main body portion 21 and the peripheral edge (flange) 24e of the lid portion 24 need to be substantially parallel, and it is necessary that the lid portion 24 forms a flange.

[0032] FIG. 5 shows the process of bending the sample container 2. First, the measurement sample S, the pressing plate 22, and the lid portion 24 are accommodated in the main body portion 21 in this order (FIG. 5(a)). Then, from above the lid portion 24, the groove portion 500v of the bending jig 500 is pressed against the opening edge portion 21e and the outer peripheral edge (flange) 24e (FIG. 5(b)). Here, the opening edge portion 21e protrudes upward (toward the bending jig 500 side) from the outer peripheral edge (flange) 24e, and the opening edge portion 21e is bent downward by the groove portion 500v. Also, by pressing the groove portion 500v, the lid portion 24 is pressed downward. Note that the groove portion 500v is an annular concave portion capable of accommodating the opening edge portion 21e.

[0033] Furthermore, the groove portion 500v of the bending jig 500 is pressed against the opening edge portion 21e and the outer peripheral edge (flange) 24e (FIG. 5(c)). As a result, the outer peripheral edge (flange) 24e is also bent downward. The groove portion 500v of the bending jig 500 is further deeply pressed against the opening edge portion 21e and the outer peripheral edge (flange) 24e (FIG. 5(d)). As a result, while the opening edge portion 21e encloses the outer peripheral edge (flange) 24e, both the opening edge portion 21e and the outer peripheral edge (flange) 24e of the lid portion 24 are bent, and the bent portion 26 is formed.

[0034] As described above, since the lid portion 24 is placed on the measurement sample S in addition to the pressing plate 22, the pressing of the measurement sample S becomes sufficient, the entire surface of the measurement sample S can be uniformly pressed, deformation of the measurement sample S and the pressing plate 22 can be suppressed, and the measurement sample can be stably observed during thermal analysis. Furthermore, if the lid portion 24 is pressed by the pressing means, the pressing plate 22 presses the measurement sample S via the lid portion 24, the pressing of the measurement sample S becomes even more sufficient, the entire surface of the measurement sample S can be uniformly pressed, and deformation of the measurement sample S and the pressing plate 22 can be further suppressed.

[0035] Note that if the opening end 21e and the peripheral edge (flange) 24 are bent portions, winding or the like used for can manufacturing or the like may be employed. Also, although it is preferable that the entire circumference of the opening end 21e and the peripheral edge (flange) 24e is bent, if the pressing of the measurement sample S is sufficient, a part of the peripheral edge (for example, four locations at equal intervals in the circumferential direction) may be used.

[0036] When the equivalent diameter of the circle of the lid portion 24 is C1 and the equivalent diameter of the circle of the hole 24h is C2, it is preferable to satisfy 0.4 ≤ C2 / C1 ≤ 0.9. If (C2 / C1) is less than 0.4, the hole 24h may be too small, making it difficult to observe the measurement sample S inside the lid portion 24. If (C2 / C1) exceeds 0.9, the hole 24h becomes too large, the width of the peripheral edge 24e portion of the lid portion 24 becomes small, the rigidity decreases, the lid portion 24 may bend in the pressed state, and the pressing of the measurement sample S may become insufficient.

[0037] It is preferable that the thickness of the lid portion 24 is equal to or greater than the thickness of the side wall of the main body portion 21. If the thickness of the lid portion 24 is less than the thickness of the side wall of the main body portion 21, the rigidity of the lid portion 24 may decrease, the lid portion 24 may bend in the pressed state, and the pressing of the measurement sample S may become insufficient.

[0038] Next, referring to FIGS. 6 and 7, the sample container 2B according to the second embodiment of the present invention will be described. FIG. 6 is a cross-sectional view along the axial direction L of the sample container 2B according to the second embodiment of the present invention, and FIG. 7 is a cross-sectional view of the state where the sample container 2B is assembled. The measurement sample container 2B includes a bottomed cylindrical main body portion 21B with an open upper portion of the cylinder, a pressing plate 22, and a lid portion 24B. The pressing plate 22 and the lid portion 24B have the same diameter as the inner diameter of the main body portion 21B or a substantially disk shape with a smaller diameter than the inner diameter. Since the pressing plate 22 is the same as that of the sample container 2 according to the first embodiment, the description thereof will be omitted.

[0039] A female screw 21f is formed on the inner surface side of the side wall of the main body portion 21B. The lid portion 24B is placed on the upper surface of the pressing plate 22, and one hole 24h2 for observing the measurement sample is opened at the center. Further, the outer peripheral edge 24e2 of the lid portion 24B rises vertically upward to form a side wall, and a male screw 24m for screwing with the female screw 21f is formed on the outer surface side of this side wall.

[0040] Then, as shown in FIG. 7, with the measurement sample S placed between the bottom surface of the main body portion 21B and the pressing plate 22, by screwing the male screw 24m of the lid portion 24B onto the female screw 21f of the main body portion 21B, the lid portion 24B is pressed downward (toward the pressing plate 22). Therefore, the female screw 21f and the male screw 24m correspond to the "pressing means" in the claims. Also in the second embodiment, the lid portion 24B and the pressing plate 22 press the measurement sample S, ensuring sufficient holding of the measurement sample S, enabling uniform pressing of the entire surface of the measurement sample S, suppressing deformation of the measurement sample S and the pressing plate 22, and allowing stable observation of the measurement sample during thermal analysis.

[0041] Next, referring to FIGS. 8 and 9, the sample container 2C according to the third embodiment of the present invention will be described. FIG. 8 is a cross-sectional view along the axial direction L of the sample container 2C according to the third embodiment of the present invention, and FIG. 9 is a view showing the shrinkage of the lid portion 24C as seen from above. The measurement sample container 2C includes a main body portion 21C having a bottomed cylindrical shape with an open upper portion of the cylinder, a pressing plate 22, and a lid portion 24C. The pressing plate 22 has a substantially disk shape with the same diameter as the inner diameter of the main body portion 21 or a smaller diameter than the inner diameter. Since the pressing plate 22 is the same as that of the sample container 2 according to the first embodiment, the description thereof is omitted.

[0042] The lid portion 24C has a ring shape, is placed on the upper surface of the pressing plate 22, and has one hole 24h3 for observing the measurement sample opened at the center.

[0043] As shown in FIG. 9, the lid portion 24C is a C-shaped snap ring, and in the open state, the outer diameter of the lid portion 24C is larger than the inner diameter 21i of the main body portion 21C. Then, with the measurement sample S placed between the bottom surface of the main body portion 21C and the pressing plate 22, insert the tip of a pair of tweezers or the like through the gripping holes 24s at both ends of the lid portion 24C to reduce the distance between the gripping holes 24s, and accommodate the lid portion 24C while pressing it against the main body portion 21C (FIG. 9(a)). After removing the tweezers and releasing the contraction of the lid portion 24C, the lid portion 24C expands in diameter inside the main body portion 21C and is fixed within the main body portion 21C, and the lid portion 24C is pressed downward (toward the pressing plate 22) (FIG. 9(b)). Therefore, the periphery of the lid portion 24C corresponds to the "pressing means" in the claims. Also in the third embodiment, the lid portion 24C and the pressing plate 22 press the measurement sample S, ensuring sufficient holding of the measurement sample S, enabling uniform pressing of the entire surface of the measurement sample S, suppressing deformation of the measurement sample S and the pressing plate 22, and allowing stable observation of the measurement sample during thermal analysis.

[0044] Next, according to the flowchart of FIG. 10, the operation of the sample container and the thermal analysis apparatus using the same will be described. First, visible light is irradiated onto the measurement sample S by the light source 31, and initial image data of the measurement sample S is acquired by the CPU 51 of the personal computer 50 using the CCD camera 32 (step S10).

[0045] Next, the image data is displayed on the display unit 53 of the personal computer 50, and the user sets the position information of the analysis region in the image of the measurement sample S on the display unit 53 using a mouse, keyboard (not shown), etc. (step S12). Note that this position information may be a single point or a region having an area tracing the outer edge. Also, when specifying a single point, a circle with a predetermined radius or area centered thereon may be regarded as a virtual region.

[0046] While heating or cooling the measurement sample S by the heater 12 or a cooling means (not shown), a heat flow difference signal (DSC signal) is acquired at each time (step S14). The process of step S14 is the same as the process performed by a conventional differential scanning calorimetry (DSC) meter, where the measurement sample S itself is heated or cooled, and its differential scanning calorimetry (DSC) is measured. Note that in the present invention, the DSC signal is acquired with respect to either the variable of time or temperature. In a general differential scanning calorimeter, the heating or cooling rate is constant, and time and temperature are correlated.

[0047] The CCD camera 32 acquires image data of the measurement sample S at each time and outputs the image data to the CPU 51. (Step 16) When acquiring the image data in step S16, it is preferable to use the same variable as the variable (time in this embodiment) for acquiring the heat flow difference signal (DSC signal) in step S14, but different variables may also be used.

[0048] Next, the CPU 51 acquires the image data of the position information part of the measurement sample S set in step S12 from the image data for each time in step S16. (Step S18) This image data is stored in the storage unit 52. When the measurement sample S is an area having an area, a value obtained by averaging the luminance or intensity of each pixel in the image data within the area is adopted.

[0049] The image data of the measurement sample S acquired in step S18 and the heat flow difference signal (DSC signal) of the measurement sample S acquired in step S14 are superimposed and displayed on the display unit 53. (Step 20) Next, the user determines whether measurement is required to end. If it is required (YES), the measurement ends. If it is not (NO), the process returns to step S14. (Step S22). The determination of whether measurement needs to end in step S24 may, for example, regard the maximum temperature or the minimum temperature for heating or cooling the measurement sample S in advance as the end temperature and consider the measurement to be ended, and there is no particular limitation.

[0050] In the above embodiment, visible light from a light source is irradiated, but electromagnetic waves other than visible light such as X-rays, infrared rays, and ultraviolet rays may be irradiated, and the reflected light may be detected by a detector other than a CCD camera such as an X-ray detector.

[0051] In addition, when acquiring an image of the measurement sample S, it may be acquired as a color change. As the color, in addition to the luminance of a specific wavelength, information obtained by quantifying the color may also be used. Examples of such quantified information include Lab (L*a*b*) values in the CIE (International Commission on Illumination) 1976 color space; RGB values representing colors by combinations of Red, Green, and Blue, which are referred to as the "three primary colors of light"; CMYK values representing colors by combinations of three colors, Cyan, Magenta, and Yellow, which are called the "three primary colors of color", and Black; etc., but are not limited thereto. For example, XYZ values in the CIE 1931 color space, L*u*v* values in the CIE 1976 color space, CIECAM02, etc. may also be mentioned.

[0052] The present invention is not limited to the above-described embodiments, and it goes without saying that the present invention extends to various modifications and equivalents included in the spirit and scope of the present invention. For example, the shapes of the sample container, the main body, the pressing plate, the lid, etc. are not limited to the above-described examples. For example, the sample container is not limited to a cylinder, and may be a rectangular tube or an elliptical tube. In addition, the thermal analyzer of the present invention, in addition to the above-described thermogravimetric / differential thermal measurement (TG / DTA) apparatus defined in JIS K 0129:2005 "General Rules for Thermal Analysis", measures the physical properties of a sample when the temperature of the measurement target (sample) is program-controlled, and can be applied to a thermal analyzer equipped with differential scanning calorimetry (DSC) for detecting a heat flow difference, but can also be applied to a differential thermal analyzer (DTA) meter and a thermogravimetric measurement (TG) meter.

Explanation of Signs

[0053] 1 Thermal analyzer 2, 2B, 2C (Measurement) sample container 10 Heating furnace 11W Observation opening (window) 21, 21B, 21C Main body 21e Opening edge 22 Pressing plate 24, 24B, 24C Lid 24h, 24h2, 24h3 Hole 24e Outer peripheral edge (flange) 26 Bending part 31 Light source 32 Imaging means (CCD camera) 51 CPU (Control unit) 53 Display unit S (Measurement) sample

Claims

1. A sample container for a thermal analyzer that measures the thermal behavior accompanying temperature changes due to heating or cooling of a measurement sample and observes the measurement sample, comprising: a main body portion having a bottomed cylindrical shape with an open top; a pressing plate that is transparent or translucent and is housed inside the main body portion and presses the measurement sample placed on the bottom surface of the main body portion from above; a lid portion that is housed inside the main body portion, placed on the upper surface of the pressing plate, and has a hole for observing the measurement sample; A sample container for a thermal analyzer, characterized by comprising the above.

2. The sample container for a thermal analyzer according to claim 1, further comprising pressing means for pressing the lid portion toward the pressing plate.

3. The lid portion forms a flange that rises vertically upward from its outer peripheral edge; The pressing means is the opening edge portion of the main body portion and the flange, The sample container for a thermal analyzer according to claim 1 or 2, characterized in that at least a part of the opening edge portion and the flange can be bent downward together.

4. The sample container has the measurement sample between the bottom surface of the main body portion and the pressing plate, The pressing means is a bent portion formed by bending at least a part of the opening edge portion and the flange downward together. The sample container for a thermal analyzer according to claim 3.

5. When the equivalent circle diameter of the lid portion is C1 and the equivalent circle diameter of the hole is C2, The sample container for a thermal analyzer according to claim 1 or 2, characterized by satisfying 0.4 ≤ C2 / C1 ≤ 0.

9.

6. The sample container for a thermal analyzer according to claim 1 or 2, characterized in that the thickness of the lid portion is equal to or greater than the thickness of the side wall of the main body portion.

7. A sample container for a thermal analyzer according to claim 1 or 2, a heating furnace that surrounds the sample container and has an observation opening, and imaging means that can observe the measurement sample through the observation opening, Comprising: A thermal analyzer characterized by measuring the thermal behavior accompanying temperature changes of the measurement sample in the heating furnace.

8. The thermal analyzer according to claim 7, characterized in that the thermal analyzer is a differential thermal analyzer, a differential scanning calorimeter, or a thermogravimetric analyzer.

9. The thermal analyzer further comprises image processing means for generating predetermined color information from the image data of the measurement sample acquired by the imaging means, The thermal analyzer according to claim 7, characterized in that the color information and the thermal behavior are superimposed and displayed with respect to temperature.

Images