JP2014034036A - Tablet holding frame body for infrared spectroscopic measurement and tablet molding method using the same - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a tablet holding frame body and a tablet molding method using the same, in which a process up to infrared spectroscopic measurement from tablet molding of a measurement sample is made highly efficient, and highly accurate measurement can be performed.SOLUTION: A tablet holding frame body 33 is used for making a tablet sample S by pressurizing-molding a mixed powder sample P which is filled in a disk-like hole 33a provided in a central part of the tablet holding frame body 33 by upper-lower projection parts, by inserting disk-like projection parts 31a and 32a provided in respective central parts of a lower pressing plate 31 and an upper pressing plate 32 from upper-lower parts of the hole 33a, and the tablet holding frame body 33 is composed of hard paper being a porous material.

Description

  The present invention relates to a tablet holding frame used in a tablet molding apparatus for preparing a tablet sample for infrared spectroscopic measurement, and in particular, to increase the efficiency and accuracy of the process from tablet molding to infrared spectroscopic measurement of a measurement sample. The present invention relates to the preparation of a tablet sample that enables accurate infrared spectroscopic measurement.

Conventionally, a tablet sample used for infrared spectroscopic measurement is formed by pressing a mixed powder of a powder of a sample to be measured and a powder of an infrared non-absorbing material (for example, potassium bromide (KBr)) into a disk shape. Is. As the pressure molding apparatus for molding the tablet sample, one having the configuration shown in FIG. 6 is usually used.
6A is a schematic perspective view of the pressure molding apparatus 10, and FIG. 6B is a tablet inserted between the sample setting surface 12 of the pressure molding apparatus 10 and the lower end surface of the pressure rod 15. FIG. 6C is a development view of the lower pressing plate 21, the upper pressing plate 22, and the metallic tablet holding frame body 23, which are constituent elements of the molding member 20, and FIG. 6C is a lower pressing plate 21 of the constituent elements of the tablet molding member 20. 6D is a longitudinal sectional view showing a concave portion 25 formed by combining a tablet holding frame body 23 with a circular projection 21a of FIG. 6, and FIG. 6 (D) is for tablet molding when the mixed powder sample P is filled in the concave portion 25. FIG. 6E is a longitudinal sectional view showing the positional relationship of the constituent elements of the member 20, with the disk-shaped protrusion 22 a of the upper push plate 22 in contact with the surface of the filled mixed powder sample P. Fig. 6 (F) is a longitudinal sectional view showing a tablet sample S molded by the pressure molding apparatus 10 of Fig. 6 (A). Is a perspective view showing a tablet sample S after molding held by the tablet holding frame 23. Each figure will be described in detail below.

  The pressure molding apparatus 10 of FIG. 6A includes a base 11, a sample installation surface 12, a pressure rod 13, a rotary shaft 14 that is integrally attached to the pressure rod 13, and a rotary shaft 14. And a pressure rod 15 that moves up and down in conjunction with the rotation. The tablet molding member 20 shown in FIG. 6B has a metallic lower push plate 21 having a disk-like protrusion 21a at the center and a metallic upper part having a disk-like protrusion 22a at the center. It consists of a push plate 22 and a metallic tablet holding frame 23. The tablet holding frame 23 is formed with a hole 23 a having a shape that matches the protrusion 21 a of the lower push plate 21 and the protrusion 22 a of the upper push plate 22. FIG. 6C shows a recess 25 formed by combining the protrusion 21a of the lower push plate 21 arranged on a flat surface with the hole 23a of the tablet holding frame 23. As shown in FIG. 6 (D), the lower push plate 21 and the upper push plate 22 apply pressure from the upper surface and / or the lower surface of the mixed powder sample P with the protrusions 21a and the protrusions 22a facing each other. It is a member for. FIG. 6E shows a tablet sample S formed using the lower push plate 21 and / or the upper push plate 22. FIG. 6F shows a state in which the tablet sample S is held in the hole 23a of the tablet holding frame 23 taken out from the pressure molding apparatus 10 after the pressure molding. That is, the tablet holding frame 23 is a member for holding the measurement sample in the frame before and after compression molding of the mixed powder sample P.

Hereinafter, a tablet molding method using the pressure molding apparatus 10 will be described.
After the mixed powder sample P is filled in the recess 25 shown in FIG. 6C, the protrusion 22a of the upper push plate 22 is placed on the upper surface of the mixed powder sample P, and the pressure molding apparatus 10 is kept in that state. It is inserted between the sample installation surface 12 and the lower end surface of the pressure rod 15. Next, the pressure rod 13 of the pressure molding apparatus 10 is pushed down, and the pressure rod 15 is lowered in conjunction with the pressure rod 15 to press the upper push plate 22 from above. Thereby, the protrusion 22a of the upper push plate 22 pressurizes the mixed powder sample P. By the pressurization, the tablet sample S is press-molded into the hole 23a of the tablet holding frame 23 as shown in FIG.
Then, the tablet sample S shown in FIG. 6 (F) molded by the above method is taken out from the pressure molding apparatus 10 together with the tablet holding frame 23, and spectroscopic measurement is performed by an infrared spectroscopic measuring apparatus (not shown).

However, the particle size of a sample pulverized into a powder is often not uniform. Therefore, even when the mixed powder sample P is pressed with a considerable force, the density in the tablet sample S tends to be inhomogeneous. The ideal tablet sample S needs to be homogeneous and high-density, but in actual tablet molding, the above-mentioned non-uniform particle size in the mixed powder sample P causes the tablet sample S. In many cases, a low density portion is left in the inside.
The magnitude of the density of the formed tablet sample S greatly affects the measurement result of the infrared spectroscopic measurement. For example, in the tablet sample S with a small thickness, reflected light from the upper surface and the lower surface of the tablet sample S interferes. At this time, if the density of the upper surface and the lower surface of the tablet sample S is different, the interference fringes of the interference light change greatly, and the effect is reflected in the result. On the other hand, Patent Document 1 proposes a method in which the upper surface and the lower surface are non-parallel in order to suppress interference of light from the upper surface and the lower surface of the tablet sample S.

JP-A-7-140063

  However, the method described in Patent Document 1 prevents interference between both sides of the tablet sample S, and does not solve the problem of homogenizing the density of the sample in the tablet sample S. In addition, development of a technique for improving the efficiency from the formation of the tablet sample S to the infrared spectroscopic measurement has been desired. The tablet sample S molded in the hole 23a of the metallic tablet holding frame 23 is removed from the hole 23a after infrared spectroscopic measurement, but the tablet holding frame 23 itself is made of a metal such as stainless steel. Therefore, it was necessary to clean the tablet holding frame 23 after the measurement. If the cleaning process is to be performed strictly, ultrasonic cleaning or heat treatment must be performed, which leads to extremely complicated processes. Accordingly, it has been desired to develop a disposable technology for discarding the tablet holding frame 23 together with the tablet sample S after the infrared spectroscopic measurement is completed. However, since compression molding needs to be performed at a pressure as high as possible, the metallic tablet A holding frame 23 has been used.

As described above, when tableting is performed, a technique for obtaining a tablet sample that is as uniform and dense as possible and a technique for creating a disposable tablet holding frame have been strongly desired. Conventionally, there has been no appropriate technique capable of solving the above-described problems.
The present invention has been made in view of the above-mentioned problems, and its purpose is to provide a tablet holding frame that enables high-efficiency processes from tablet molding to infrared spectroscopic measurement of a measurement sample and high-precision measurement. And providing a tablet forming method using the same.

  As a result of intensive studies by the present inventors on these conventional problems, a tablet holding frame for holding a sample before and after tablet molding is changed from a conventional metallic material to a nonmetallic material, particularly a hard paper which is a porous material. The pressure applied to the mixed powder sample during compression molding is moderately dispersed, the inner wall of the hole in the center of the tablet holding frame is deformed so as to hold a part of the tablet sample, and the density is increased. The inventors have found that a homogeneous tablet sample can be prepared, and have completed the present invention.

That is, the tablet holding frame of the present invention is disk-shaped, and the mixed powder sample filled in the hole in the center is pressed from the upper surface and / or the lower surface of the mixed powder sample by a pressure molding device. A tablet holding frame used for molding a sample and holding the tablet sample in a hole, wherein the material of the tablet holding frame is made of non-metallic, porous hard paper .
The diameter of the hole in the tablet holding frame is 3 to 13 mmφ. The tablet holding frame is deformed when it receives a force of 0.8 kN or more, and the deformed state is maintained even when the pressure during pressure molding is released.
As the hard paper, one having a density of about 1.2 mg / mm ³ or more is used.

  Even if the particle size and shape produced during the preparation of the mixed powder sample are not uniform, the mixed powder sample is pressed at once with a pressure molding device, but the thickness of the tablet sample formed thereby is thin. If it is too large, the above-described generation of interference light occurs during infrared spectroscopic measurement, and if the thickness is too thick, many non-uniform portions remain in the tablet sample. Therefore, in order to ensure the transparency of the tablet sample to the extent that infrared spectroscopic measurement is possible, the tablet sample to be molded must have an appropriate thickness. Since the inner wall portion of the hole does not deform when used, the tablet sample molder needs to adjust appropriately between the amount of the mixed powder sample to be filled in the tablet holding frame and the pressurization amount according to the amount, The adjustment work is complicated.

On the other hand, the tablet holding frame of the present invention is deformed by the pressure during pressure molding as described above, and the deformed state is maintained even when the pressure is released. It can be held in a tablet holding frame. As a result, the pressure applied to the mixed powder sample at the time of compression molding is moderately dispersed, so the tablet sampler must make fine adjustments in the amount of pressure according to the amount of the mixed powder sample filled in the tablet holding frame. It is possible to obtain a tablet sample good for infrared spectroscopic measurement.
Moreover, since the tablet holding frame of the present invention is made of a nonmetallic material, it is very inexpensive.

It is a figure which shows the structure of the member for tablet shaping | molding of a 1st Example. It is a figure which shows the structure of the member for tablet shaping | molding of a 2nd Example. It is a figure which shows the structure of the member for tablet shaping | molding of a 3rd Example. It is a figure which shows the structure of the member for tablet shaping | molding of 4th Example. It is a figure which shows the structure of the member for tablet shaping | molding of 5th Example. It is a figure which shows the structure of the conventional pressure molding apparatus and the member for tablet formation.

Hereinafter, the present invention will be described specifically by way of examples.
First Embodiment FIG. 1 is a view showing the structure of a tablet molding member 30 according to a first embodiment of the present invention. FIG. 1A is a diagram showing the components of the tablet molding member 30 in an expanded state, and FIG. 1B is a mixture before pressurization filled in the recess 35 formed in the tablet molding member 30. FIG. 1 (C) shows the tablet molding member 30 shown in FIG. 1 (B) using the pressure molding apparatus 10 shown in FIG. 6 (A). FIG. 1D is a perspective view of a tablet holding frame 33 that holds the tablet sample S. FIG.
1A includes a lower push plate 31, an upper push plate 32, and a tablet holding frame 33. The lower push plate 31 and the upper push plate 32 are each circular at the center. Plate-shaped protrusions 31a and 32a are provided. The mixed powder sample P is filled between the protrusion 31a of the lower push plate 31 and the protrusion 32a of the upper push plate 32 facing each other, and the mixed powder sample P is pressurized by the protrusions 31a and 32a. Further, it is preferable that the surfaces of the protrusions 31a and 32a are mirror-finished.
Furthermore, the area of the front end surface of these protrusions 31a and 32a can be appropriately used in a desired size. More specifically, protrusions 31a and 32a having a diameter of 3 to 13 mmφ are used.

Here, the tablet holding frame 33 is a member for holding the mixed powder sample P and the tablet sample S before and after compression molding, and the lower pressing plate 31 is provided at the center of the tablet holding frame 33. A hole 33a having a shape that matches the shape of the protrusion 31a and the protrusion 32a of the upper push plate 32 is provided. Therefore, the diameter of the hole 33a of the tablet holding frame 33 is 3 to 13 mmφ.
The material of the tablet holding frame 33 is preferably made of hard paper which is a porous material. In particular, hard paper has a density of about 1.2 mg / mm ³ or more, a tensile strength in the same direction as the molding direction of the material of about 50 MPa, and a tensile strength in a direction perpendicular to the molding direction of the material. A material having a physical property value of about 30 MPa is used. More specifically, the above-mentioned product name “Pasco” of Hokuetsu Kishu Paper Co., Ltd. or its equivalent is used.
The pressure molding apparatus 10 shown in FIG. 6A is used for pressure molding, but a pressure degree limiting mechanism that limits the degree of pressure applied to the sample by limiting the movable range of the pressure rod 13 is provided. It may be provided. For example, the pressurization degree limiting mechanism may be a mechanism that adjusts the length of the pressure rod 13 or a mechanism that limits the descending distance of the pressure rod 15. Further, unlike those mechanisms, the pressurization degree limiting mechanism is a mechanism that can adjust the relationship between the pressure generated by the pressure rod 13 and the pressure at the lower end surface of the pressure rod 15 with a simple moment amount. Good.
In this embodiment, a stopper mechanism (not shown) that limits the descending distance of the pressure rod 15 is employed. The pressure molding apparatus 10 adjusts the pressure applied to the mixed powder sample P by appropriately adjusting the stopper for limiting the descending distance of the pressure rod 15 according to the diameter of the hole 33a of the tablet holding frame 33. Can do.

Hereinafter, a tablet molding method using the tablet molding member 30 of the first embodiment of the present invention will be described. The lower push plate 31 is placed on a flat surface (for example, the sample setting surface 12 of the pressure molding apparatus 10 shown in FIG. 6A) with the protrusion 31a facing upward. The tablet holding frame 33 shown in FIG. 1 is combined with the lower push plate 31 so that the hole 33 a is fitted into the protrusion 31 a of the lower push plate 31. Thereby, a recess 35 for filling the mixed powder sample P is formed.
After filling the concave portion 35 with the mixed powder sample P, the protrusion 32a of the upper push plate 32 is applied so as to contact the upper surface of the mixed powder sample P, and the state shown in FIG. It is inserted between the sample setting surface 12 of the pressure forming device 10 and the lower end surface of the pressure rod 15.
When the pressure bar 13 of the pressure molding apparatus 10 is pushed down, the mixed powder sample P is pressurized and shaped into a tablet sample S as in the conventional tablet molding method.
Thereafter, the molded tablet sample S is attached to an infrared spectroscope (not shown) while being held by the tablet holding frame 33. When the infrared spectroscopic measurement is completed, the tablet sample S can be discarded or stored together with the tablet holding frame 33.

<Preparation of tablet sample S>
In order to perform tableting of the measurement sample, the measurement sample powder and the infrared non-absorbing material powder (that is, among infrared non-absorbing materials such as potassium bromide (KBr), potassium chloride (KCl) and cesium iodide (CSi)) A mixed powder sample P is prepared and molded. That is, the mixed powder sample P is a mixed powder sample P obtained by thoroughly mixing a sample of several μg to several tens of μg and about several tens of mg of infrared non-absorbing material and then pulverizing it into a fine powder using, for example, a mortar. The mixed powder sample P is filled in the concave portion 35 shown in FIG. 1 (B) and pressed by the pressure molding apparatus 10 shown in FIG. 6 (A), and the tablet sample is shown in FIG. 1 (C). S is formed.

When the tablet sample S is formed from the mixed powder sample P using the tablet forming member 30 as described above, a high-density tablet sample S is obtained in the hole 33a of the tablet holding frame 33, and the tablet holding frame 33 is obtained. Part of the inner wall surface 33b of the hole 33a is deformed, and the tablet sample Sa entering the recess formed thereby is obtained.
In this way, the tablet holding frame 33 that can appropriately disperse the pressure applied to the mixed powder sample P in the direction perpendicular to the pressing direction (direction perpendicular to the inner wall surface 33b) during tablet formation is used. Thus, a uniform tablet sample S can be obtained which has a higher appearance transparency than the tablet sample made of the metallic tablet holding frame 23 described above.

<Preparation of background tablet sample Sb>
In tablet sample S, in addition to the measurement sample, either one of the powders of potassium bromide (KBr) or potassium chloride (KCl), which is an infrared non-absorbing material, was included in mixed powder sample P. To obtain the spectrum of the non-infrared absorbing material from the spectrum of the tablet sample S. Therefore, after using only a non-infrared absorbing material to make a fine powder Pb using a mortar or the like and filling the fine powder Pb into the recess 35 of the tablet holding member 30 shown in FIG. A pressure is applied by the pressure forming apparatus 10 to form a background tablet sample Sb to be subtracted from the spectrum. In addition, it is preferable that the tablet sample Sb of an infrared non-absorbing material has the same density as the density of the infrared non-absorbing material in the tablet sample S.

<Example>
In this example, "Pasco (Hokuetsu Kishu Paper Co., Ltd.)" is used as the hard paper, and the tablet for background is filled with 50 mg of infrared non-absorbing material KBr in the recess 35 shown in FIG. Molded. The diameter of the hole 33a of the tablet holding frame 33 was 5 mmφ, the pressure was 0.3 kN, and the tablet sample S was prepared by pressurizing for about 2 seconds. And (a) Whether or not the tablet can be formed (b) Transparency of the tablet sample S is evaluated by appearance, and (c) Pressure [kN / mm ² ] required to dent 1 mm per unit area with respect to the tablet holding frame itself. Was measured.

<Comparative example>
For the tablet holding frame made of “Pasco” used in the examples, as comparative examples, (i) stainless steel plate (conventional product), (ii) polypropylene plate, (iii) low foam polyethylene plate, (iv) melamine urethane resin Using it as a tablet holding frame made of a plate, tableting was performed. Evaluation is performed in the same manner as in the present embodiment, and the evaluation results are described below.
In addition, about the material shown to (i)-(iv), the tablet shaping | molding was performed like the present Example except the applied pressure having been 0.5 kN.

Examples (a) Tablets could be formed.
(B) The transparency of the tablet was high.
(C) 0.87 kN / mm ²
(I) Stainless steel plate (0.5kN)
(A) A tablet was formed.
(B) The pressure applied to the mixed fine powder sample P during tablet formation cannot be properly released,
It was white or cloudy locally or entirely. Therefore, the density of the sample in the tablet was judged to be inhomogeneous.
(C) Since the stainless steel was very hard, no dent was formed.
(Ii) Polypropylene plate (0.5kN)
(A) It was possible to mold into a tablet-like solid, but the solid was cracked.
(B) The pressure applied to the fine powder sample P at the time of tablet formation was eased by compressing the wall surface of the hole in the polypropylene plate, but the tablet sample S was cracked after the pressure was released.
This was judged to be the result of the pressure exerted on the tablet sample by which the polypropylene plate returned.
(C) 1.77 kN / mm ²
(Iii) Low firing polyethylene plate (0.5kN)
(A) It was possible to mold into a tablet-like solid, but the solid was cracked.
(B) It was judged that the tablet sample was cracked for the same reason as the polypropylene plate.
(C) 0.13 kN / mm ²
(Iv) Melamine urethane resin plate (0.5kN)
(A) It could not be formed into a tablet-like solid.
(B) Unlike (ii) and (iii), the mixed powder sample P remained as it was because the flexibility of the tablet holding frame itself was too high.
(C) 0.33 kN / mm ²

Comparing the above examples with Comparative Example (i), this Example was capable of tableting at a lower pressure than Comparative Example (i). Furthermore, the transparency of the appearance of this example was high even at a lower pressure than that of Comparative Example (i). Therefore, the present Example can obtain a tablet sample with high density at a pressure lower than that of the prior art.
In Comparative Examples (ii) and (iii), a deformable material was used similarly to the tablet holding frame 33 of the present invention. However, in Comparative Examples (ii) and (iii), when the pressure at the time of tablet formation is released, the inner wall surface 33b of the hole 33a deformed by the pressurization tends to return, so that force is applied to the tablet sample S from the inner wall surface 33b. , The tablet sample S was cracked.
In contrast, in the present example, even when the pressure at the time of tablet formation was released, the inner wall surface 33b remained in a deformed state. Therefore, the tablet holding frame 33 of the present invention can produce a sample without applying extra force to the tablet sample S.
The comparative example (iv) is a porous material as in the case of the present embodiment, and is a material in which the force applied to the tablet sample S due to the return of the inner wall surface 33b of the hole 33a after the pressure release as described above is very small. However, it is considered that the mixed powder sample P did not become a solid because a sufficient pressure from the inner wall surface 33b of the hole 33a required for tablet molding could not be obtained.
On the other hand, the tablet holding frame 33 of the present invention can apply a force necessary and sufficient to form the tablet sample to the mixed powder sample P, so that the tablet can be formed.

Second Embodiment FIG. 2 is a view showing the structure of a tablet forming member 40 of the present invention. 2A is a longitudinal sectional view showing components of the tablet molding member 40, and FIG. 2B shows a tablet sample Ss molded using the tablet molding member 40 together with the tablet molding member 40. FIG. 2C is a perspective view of the tablet holding frame 33 holding the tablet sample Ss (in FIG. 2C, the transparent plate 42 is shown in order to make the tablet sample Ss easier to see). Only the outer periphery is shown with a dashed line).
The tablet molding member 40 shown in FIG. 2 (A) includes a lower push plate 31, an upper push plate 32, and a tablet holding frame 33 similar to those shown in FIG. 1 (A). Two transparent plates 41 and 42 made of an infrared non-absorbing material are used.
As shown in FIG. 2 (A), the transparent plates 41 and 42 hold the fine powder Ps made of only the sample to be measured between the transparent plates 41 and 42, and the pressure molding apparatus shown in FIG. 6 (A). 10 is inserted into a recess 35 formed by a disc-shaped protrusion 31 a of the lower push plate 31 placed on the sample setting surface 12 and a hole 33 a of the tablet holding frame 33.

Next, a method for molding a tablet sample using the tablet molding member 40 of the present invention will be described.
The fine powder Ps is sandwiched between the transparent plates 41 and 42 and inserted into the recess 35 in FIG. Thereafter, the protrusion 32 a of the upper push plate 32 is brought into contact with the upper surface of the transparent plate 42. In this state, it is inserted between the sample setting surface 12 of the pressure molding apparatus 10 shown in FIG. 6 (A) and the lower end surface of the pressure rod 15 and then pushed upward as in the case of the first embodiment. By applying pressure from the protrusion 12a of the plate 12, the powder sample Ps is formed into a tablet sample Ss as shown in FIG.
When the tablet sample Ss is formed, the inner wall surface 33b of the hole 33a of the tablet holding frame 33 shown in FIG. 2C is deformed as shown in FIG. A tablet sample Ss in which a part of the tablet is embedded in the tablet holding frame 33 is formed.
Thereafter, the molded tablet sample Ss is attached to an infrared spectroscope (not shown) while being held by the tablet holding frame 33. After the infrared spectroscopic measurement is completed, the tablet sample Ss can be discarded or stored together with the tablet holding frame 33.

Moreover, it is preferable that the degree of compression of the transparent plates 41 and 42 made of an infrared non-absorbing material is approximately the same regardless of the formation of a tablet sample and the formation of a background tablet.
By using the two transparent plates 41 and 42, it is possible to produce the tablet sample Ss even if the powder sample Ps is a minute amount.
Further, by using these transparent plates 41 and 42, it is possible to omit the step of preparing a mixed powder of the powder of the measurement sample and the powder of the infrared non-absorbing material. This makes it possible to increase the efficiency of the procedures that lead to this. Furthermore, even if the measurement sample is a poisonous or deleterious substance, as shown in FIGS. 2B and 2C, the tablet sample Ss is sandwiched between the two transparent plates 41 and 42. It is possible to move tablets easily and safely.

Third Embodiment FIG. 3 is a view showing the structure of a tablet molding member 50 of the present invention. 3 (A) is a diagram showing the components of the tablet molding member 50 in an expanded state, and FIG. 3 (B) shows a state in which the mixed powder sample P is filled in the recess 55 using the tablet molding member 50. It is a longitudinal cross-sectional view shown.

A tablet molding member 50 shown in FIG. 3A is a lower push plate 51, an upper push plate 52, a guide ring 53, and a tablet holding frame 33 used in the first embodiment. Pressurization is performed by the pressure molding apparatus 10 shown.
In FIG. 3 (A), the lower push plate 51 and the upper push plate 52 are disk-shaped convex portions 51a, 52a formed in the respective central portions and the central portions of the convex portions 51a, 52a. It has formed small disk-like protrusions 51b and 52b. Further, two handles 54 are provided on the outer peripheral portion of the lower push plate 51 so as to face each other.
FIG. 3B shows a mixed powder sample in the recess 55 formed by combining the projections 51b of the lower push plate 51 arranged on a flat surface with the holes 33a of the tablet holding frame 33 as in the first embodiment. The state filled with P is shown.

The guide ring 53 shown in FIGS. 3A and 3B is provided with a hole having a diameter capable of fitting the circular convex portions 51a and 52a from above and below. By using the guide ring 53, it is easy to press the vertical direction with the incorporation of the upper push plate 52. Furthermore, the powder of the measurement sample overflows outside the guide ring 53 in a series of operations during tablet formation. Therefore, the safety at the time of tablet formation can be ensured.
When the tablet sample S is formed, the tablet shown in the first embodiment of FIG. 1 or the second embodiment of FIG. 2 is used except that the guide ring 53 shown in FIGS. 3 (A) and 3 (B) is used. The tablet samples S and Ss can be molded in the same manner as the molding.

Fourth Embodiment FIG. 4 is a view showing the structure of the tablet forming members 60 and 65 of the present invention, and FIG. 4 (A) shows the first and second pressurizing frames 61 used in the fourth embodiment. FIG. 4B is a perspective view showing a case where the tablet holding frame 33 shown in the third embodiment is combined with the upper surface, and FIG. 4B shows a combination of components when the tablet is formed using the pressure frame 61. 4C is a perspective view showing a case where two pressure frames 61 and 62 are combined with the upper and lower surfaces of the tablet holding frame 33, and FIG. 4D is the pressure frames 61 and 62. FIG. It is a longitudinal cross-sectional view which shows the combination of each component at the time of performing tablet shaping | molding using.

The upper pressure frame 61 shown in FIG. 4 (A) and the lower pressure frame 62 shown in FIG. 4 (C) mainly apply pressure to members other than the inner wall surface 33b of the hole 33a of the tablet holding frame 33 during tablet formation. This is a component for preventing the When using the upper pressure frame 61 and the lower pressure frame 62 formed of a hard material such as metal at the time of tablet molding, the upper pressure frame 61 and the lower pressure frame 62 are not deformed. The tablet molding member 65 can concentrate the pressure applied to the mixed powder sample on the inner wall surface 33b, and the outer periphery of the tablet holding frame 33 corresponding to the contact portion between the pressure frame and the tablet holding frame 33. The part can be made difficult to deform. On the other hand, when the upper pressure frame 61 and the lower pressure frame 62 formed from a material such as a silicone resin are used at the time of tablet molding, the upper pressure frame 61 and the lower pressure frame 62 are the above inner wall surfaces 33b. The pressure from the mixed powder sample acting at an inclination relative to the tablet holding frame 33 can be moderately dispersed, and at the same time, the elastic force of the pressure frames is applied to the outer peripheral portion of the tablet holding frame 33 corresponding to the contact portion with the tablet holding frame 33 Works.
That is, by using the upper pressure frame 61 and the lower pressure frame 62, the deformation of the inner wall surface 33b at the time of tablet sample molding can be adjusted so as to be caused mainly by the pressure acting in the vertical direction.
When producing the tablet samples S and Ss, as shown in FIGS. 4B and 4D, the upper pressure frame 61 and / or the lower pressure frame 62 are arranged together with the components of the first embodiment. By doing so, the tablet sample S can be pressure-molded by the same tablet molding method as in the first embodiment shown in FIG. In addition, the lower pressing plate 51 and the upper pressing plate 52 of the third embodiment shown in FIG.

Fifth Embodiment Figure 5 is a diagram showing a configuration of a tablet molding member 70 of the present invention, FIG. 5 (A) and the reinforcing ring 71, similar tablets holding the tablet holding frame 33 shown in FIG. 1 FIG. 5B is a longitudinal cross-sectional view showing the positional relationship of each component when tableting is performed using the reinforcing ring 71. FIG.
The reinforcing ring 71 shown in FIG. 5A reinforces the inner wall surface 73b of the hole 73a of the tablet holding frame 73 when it is necessary to mold a tablet having a larger shape than usual. 5B uses the reinforcing ring 71, the tablet holding frame 73, and the lower push plate 31 and the upper push plate 32 of FIG. 1A as they are. The pressure is applied by the pressure molding apparatus 10 shown in FIG.
When preparing the tablet sample S, as shown in FIG. 5B, the mixed powder sample P is filled in the concave portion 75 formed from each component, and the same as in the first embodiment or the third embodiment. The tablet sample S is molded by the tablet molding method.

  The present invention relates to a tablet holding frame for preparing a tablet sample for analysis, and in particular, when performing infrared spectroscopic measurement, it is possible to create a homogeneous tablet sample having a high appearance transparency.

DESCRIPTION OF SYMBOLS 10 Pressure molding apparatus 11 Base 12 Sample installation surface 13 Pressure rod 14 Rotating shaft 15 Pressure rod 20, 30, 40, 50, 60, 70 Tablet molding member 21, 31, 51 Lower push plate 21a, 31a, 51b Lower push plate projections 22, 32, 52 Upper push plates 22a, 32a, 52b Upper push plate projections 33, 73 Tablet holding frame 33a, 73a Tablet holding frame holes 33b, 73b Inner wall surfaces 25, 35 , 55, 75 Recess 41, 42 Transparent plate 53 Guide ring 61, 62 Pressure frame 71 Reinforcing ring P, Ps Powder sample S, Ss Tablet sample Sb Background tablet

Claims (6)

Insert the mixed powder sample filled in the disk-shaped hole provided at the center of the tablet holding frame into the disk-shaped protrusions provided at the center of each of the lower push plate and the upper push plate from above and below the hole. A tablet holding frame used for producing a tablet sample by pressure-molding the mixed powder sample at the upper and lower protrusions,
The tablet holding frame is made of hard paper which is a porous material. In the tablet holding frame according to claim 1,
The tablet holding frame is characterized in that the hole of the tablet holding frame has a diameter of 3 to 13 mm. In the tablet holding frame according to claim 1 or 2,
The tablet holding frame is deformed when it receives a force of 0.8 kN or more, and is maintained in a deformed state even when the pressure during pressure molding is released. In the tablet holding frame according to any one of claims 1 to 3,
The tablet holding frame, wherein the hard paper has a density of about 1.2 mg / mm ³ or more. The mixed powder sample filled in the disk-shaped hole provided in the central part of the tablet holding frame made of hard paper, the disk-shaped protrusion provided in the central part of each of the lower push plate and the upper push plate in the hole A tablet molding method for creating a tablet sample by inserting from above and below and press-molding the mixed powder sample with the upper and lower protrusions,
A frame body producing step for producing the tablet holding frame body by selecting a hole diameter of the tablet holding frame body from 3 to 13 mmφ so as to align with a disk-shaped protrusion at a central portion of the lower push plate When,
A step of disposing a disk-shaped protrusion on the flat surface in the upward direction at the center of the lower push plate;
An assembling step in which the holes of the tablet holding frame are fitted into the protrusions of the lower push plate from above and combined;
Filling the mixed powder sample into the recess formed by the incorporation step;
A step of fitting a disc-shaped protrusion at the center of the upper push plate so as to contact the upper surface of the mixed powder sample filled in the recess;
A pressing step of pressing from above the upper push plate and / or from below the lower push plate,
The tablet holding frame is made of a material that deforms when it receives a force of 0.8 kN or more in the pressurizing step, and maintains the deformed state even when the pressure at the time of pressure molding is released. Tablet molding method. In the tablet molding method according to claim 5,
Instead of the mixed powder sample, the tablet is formed by inserting the transparent plate into the recess in a state where a fine powder made of a single measurement sample is sandwiched between two upper and lower transparent plates made of an infrared non-absorbing material. Method.

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