JPS59173730A - Method for forming tablet of trace solid sample - Google Patents
Method for forming tablet of trace solid sampleInfo
- Publication number
- JPS59173730A JPS59173730A JP58048548A JP4854883A JPS59173730A JP S59173730 A JPS59173730 A JP S59173730A JP 58048548 A JP58048548 A JP 58048548A JP 4854883 A JP4854883 A JP 4854883A JP S59173730 A JPS59173730 A JP S59173730A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- holder
- holes
- metal
- tablet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000007787 solid Substances 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims description 17
- 229910052751 metal Inorganic materials 0.000 claims abstract description 17
- 239000002184 metal Substances 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 6
- 239000003513 alkali Substances 0.000 claims description 4
- 150000004820 halides Chemical class 0.000 claims description 4
- 238000000862 absorption spectrum Methods 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 abstract description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 5
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 2
- 239000010935 stainless steel Substances 0.000 abstract description 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 12
- 238000005259 measurement Methods 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
Description
【発明の詳細な説明】
（発明の技術分野）
本発明は、赤外吸収スペクトル測定のために微量或いは
極微量の固体試料の錠剤を成形する方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Technical Field of the Invention) The present invention relates to a method for forming tablets of minute or extremely small amounts of solid samples for infrared absorption spectroscopy.
（発明の技術的背景）
近年、赤外吸収スペクトルの測定は、装置の進歩ともめ
いまり物質の同定や構造研究に欠くことのできない手段
として生体成分等の微量成分の研究にも用いられるよう
になってきている。(Technical Background of the Invention) In recent years, due to advances in equipment, infrared absorption spectra measurement has come to be used as an indispensable means for identification of substances and structural research, and for research on trace components such as biological components. It has become to.
このような微量の固体試料の赤外吸収スペクトル測定用
錠剤を成形する方法としては、従来から次のようないく
つかの方法が開発されていた。As methods for forming tablets for measuring infrared absorption spectra of such small amounts of solid samples, the following several methods have been developed in the past.
Ｕ）集中法
臭化カリウム（ＫＢｒ）等の錠剤に細孔をあけ、ここに
微量試料をつめて加圧成形する。U) Concentration method A small hole is made in a tablet of potassium bromide (KBr), etc., and a small amount of sample is filled in the hole and pressure molded.
Ｑ） アルミニウム円板法
長方形の窓をもつアルミニウムの円板を用い、この窓に
試料とＫＢｒとの混合物をつめて加圧成形する。Q) Aluminum disk method: An aluminum disk with a rectangular window is used, and the sample and KBr mixture is filled in the window and pressure-formed.
（３）ろ紙円板法
中央に孔を打抜いたろ紙の孔部に、試料とＫＢｒとの混
合物音ろ紙と同じ厚さにつめ、ろ紙ごと加圧する。(3) Filter paper disc method A mixture of the sample and KBr is packed into the hole of a filter paper with a hole punched in the center to the same thickness as the filter paper, and the filter paper is pressurized.
（４） ミクロ錠剤法
第１図に示すように、中央に２〜５ｍｍ径の円孔があけ
られた厚さ２〜３第３調程金属円板１の円孔に、試料と
ＫＢｒとの混合物２全つめ、これ全円孔にちょうどはす
る大きさの凸部を有する２枚の凸形円板３．４によシ上
下がらはさんで加圧成形する。(4) Micro-tablet method As shown in Figure 1, the sample and KBr are inserted into the circular hole of the 2-3rd diameter metal disk 1 with a thickness of 2 to 3 mm and a circular hole with a diameter of 2 to 5 mm in the center. The entire mixture 2 is pressure-molded by sandwiching it between two convex disks 3.4, which have convex portions just large enough to fit into the circular holes, from top to bottom.
（背景技術の問題点）
しかしながらこれらの方法においては、いずれも以下に
示すような欠点がめった。(Problems with Background Art) However, all of these methods often have the following drawbacks.
すなわち（１）の集中法においては、錠剤に細孔をあけ
る必要があるばかりでなく測定後の試料の回収が離しい
という欠点があり、Ｃ２）のアルミラム円板法において
は、アルミニウムがＫＢｒ粉末に比べて圧縮されにくい
ため透剤な錠剤を作ることが困難であるばかりでなく、
アルミニウムとの境界面で試料錠剤がはがされやすいと
いう欠点があった。That is, in the concentration method (1), there is a disadvantage that not only it is necessary to make pores in the tablet, but also it is difficult to collect the sample after measurement. Not only is it difficult to make drug-permeable tablets because it is difficult to compress compared to
There was a drawback that the sample tablet was easily peeled off at the interface with aluminum.
また（３）のろ紙円板法においては、試料混合物の量が
多いと錠剤にひびが入ジやすく、菫た試料の一部はどう
しても、φ紙にしみ込んで完全回収および連続使用が困
難であるという欠点があった。In addition, in the filter paper disc method (3), if the amount of sample mixture is large, the tablets tend to crack, and some of the mixed sample inevitably soaks into the φ paper, making complete recovery and continuous use difficult. There was a drawback.
さらに（４）のミクロ錠剤法においては、凸形円板６．
４をはがす過程で錠剤が破損しゃすいばかりでなく、全
面が平滑な錠剤を得ることが離しいという欠点があった
。Furthermore, in the micro-tablet method (4), a convex disk 6.
There was a drawback that not only the tablets were easily damaged in the process of peeling off No. 4, but also that it was difficult to obtain tablets with smooth surfaces.
（発明の目的）
本発明はこれらの従来方法の欠点を解消するためになさ
れたもので、固体微量試料の表面平滑で透明な錠剤を簡
単に成形することのできる方法を提供することを目的と
する。(Objective of the Invention) The present invention was made in order to eliminate the drawbacks of these conventional methods, and an object of the present invention is to provide a method that can easily form transparent tablets with a smooth surface from a small amount of solid sample. do.
（発明の概要）
本発明は、中心に直径が１〜１０■の全てほぼ同じ形状
および大きさの開孔を有する複数枚の薄い金属円板全積
重して成るホルダーの前記開孔に、固体試料とハロゲン
化アルカリ粉末との混合物を充填し、これを前記ホルダ
ーの上下側からそれぞれ２枚の金属平面板ではさんで加
圧することを特徴とする固体微量試料の錠剤成形方法で
ある。(Summary of the Invention) The present invention provides a holder comprising a plurality of stacked thin metal discs each having a hole in the center having a diameter of 1 to 10 cm and all having approximately the same shape and size. This is a tablet forming method for a small amount of a solid sample, which is characterized by filling a mixture of a solid sample and an alkali halide powder, and pressing the mixture between two flat metal plates from the upper and lower sides of the holder.
（発明の実施例〕
以下本発明の実施例について図面を参照しながら説明す
る。(Embodiments of the invention) Examples of the invention will be described below with reference to the drawings.
実施例においては、第２図に示すように、１ず金属製の
下側平面板５の上に、中心に開孔６を有し後述する錠剤
成形器の内径よりわずかに小さい直径を持つ複数枚の金
属製円板７を、開孔６の中心をそろえて積み重ね、ホル
ダー８を形成する。In the embodiment, as shown in FIG. 2, first, a plurality of holes having an opening 6 in the center and having a diameter slightly smaller than the inner diameter of a tablet molding machine, which will be described later, are placed on the lower plane plate 5 made of metal. A holder 8 is formed by stacking two metal discs 7 with the centers of the apertures 6 aligned.
ここで中心に開孔６を有する円板７を構成する材料、！
：してｕ、ステンレススチール、ニッケル、アルミニウ
ム、銅などの赤外線全透過させない金属を用いるのが望
”ｉＬ、＜、１枚の板厚は強度の点で１０〜５００μの
範囲にすることが好ましい。Here, the material constituting the disk 7 with the aperture 6 in the center!
:It is preferable to use a metal that does not transmit all infrared rays, such as stainless steel, nickel, aluminum, or copper. .
また開孔６は、円、だ円、矩形等いがなる形状のもので
もよいが、得られる錠剤の強度の点から直径が１〜１０
ｗｎの範囲にあることが望ましい。The opening 6 may have a circular, oval, or rectangular shape, but from the viewpoint of the strength of the resulting tablet, the diameter should be 1 to 10 mm.
It is desirable that it be in the range of wn.
さらに複数枚の金属製円板７は全てほぼ同じ形状および
大きさの開孔６ｔ−有するように構成する。Further, the plurality of metal disks 7 are all configured to have openings 6t of approximately the same shape and size.
次いでこうして構成されたホルダー８の開孔６に、固体
試料とＫＢｒのようなハロゲン化アルカリ粉末との混合
物９をつめた後、ボルダ−８の上に金属製の上側平面板
１０ｔ−載せて押える。この状態で通常の錠剤成形器１
１の所定の位置にセットし、矢印の方向に真空引きしな
から押棒１２により加圧して成形する。加圧の大き′さ
は開孔６の大きさすなわち成形すべき錠剤の大きさによ
り適当に加減することが望ましい。尚、図中１６はパツ
キンを示す。Next, a mixture 9 of a solid sample and an alkali halide powder such as KBr is filled into the opening 6 of the holder 8 constructed in this manner, and then the upper flat metal plate 10t is placed on the boulder 8 and held down. . In this state, a normal tablet press 1
1, and then evacuated in the direction of the arrow and then pressurized with the push rod 12 to form the mold. It is desirable to adjust the amount of pressure appropriately depending on the size of the opening 6, that is, the size of the tablet to be molded. In addition, 16 in the figure shows a packing.
このように構成された実施例によれば、通常の錠剤成形
器を用いて表面平滑で透明な固体微量試料の錠剤を成形
することができる。According to the embodiment configured in this way, a tablet of a small amount of a solid sample with a smooth surface and a transparent surface can be molded using an ordinary tablet molding machine.
また測定後の試料回収が容易であるばがｐでなく、金属
製円板７の厚さや積重枚数或いは開孔１６の直径を試料
の量に応じて選ぶことによって、最も特性の良好な錠剤
を成形することができる。さらに実施例により得られる
錠剤は周りの金属製円板７に対する固着力が大きいので
、界面から剥れ落ちたりすることがない。In addition, by selecting the thickness of the metal disc 7, the number of stacked metal discs, or the diameter of the opening 16 according to the amount of the sample, instead of selecting the one that facilitates sample collection after measurement, tablets with the best properties can be obtained. can be molded. Furthermore, since the tablets obtained in the examples have a strong adhesion force to the surrounding metal disk 7, they do not peel off from the interface.
（発明の効果〕
以上の記載から明らかなように、本発明によれば、微量
の固体試料を用い特性の良好な錠剤を特別な成形器を用
いることなく簡単に成形することができる。(Effects of the Invention) As is clear from the above description, according to the present invention, tablets with good properties can be easily molded using a small amount of solid sample without using a special molding machine.
第１図は従来のミクロ錠剤法を説明するための断面図、
第２図は本発明の一実施例を説明するための断面図であ
る。
５−・・・−・・・・・・・・−・・・・・・・下側平
面板６・・−・・・・・−・・・・・・・・・・−・開
孔７・・・・・・・・・・−・・・・・・・・・・金属
製円板８・・・・・・・・・・・・・・−・・・・・・
ホルタ−９・・・・・・・・・・・・・・・・・・・・
・固体試料とハロゲン化アルカリ粉末との混合物
１０・・・・・・−・・−・−・・・・・・・上側平面
板１１・・・・・・・・・・・・・−・・・・・・・錠
剤成形器第１図
第２図
１４３−Figure 1 is a cross-sectional view for explaining the conventional micro-tablet method;
FIG. 2 is a sectional view for explaining one embodiment of the present invention. 5--・・・--------------------------------- 7・・・・・・・・・・・・・・・・・・・・・・・・Metal disc 8・・・・・・・・・・・・・・・・・・・・・・・・
Holter 9・・・・・・・・・・・・・・・・・・
・Mixture of solid sample and alkali halide powder 10 ・・・・・・・−・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・・ Upper flat plate 11 ・・・・・・・・・・・・...Tablet press Figure 1 Figure 2 143-
Claims (1)
大きさの開孔を有する複数枚の薄い金属円板全積重して
なるホルダーの前記開孔に、赤外吸収スペクトルを測定
すべき固体試料とハロゲン化アルカリ粉末との混合物を
充填し、これを前記ホルダーの上側および下側からそれ
ぞれ２枚の金属平面板ではさんで加圧することを特徴と
する固定微量試料の錠剤成形方法。1. Measure the infrared absorption spectrum at the aperture of a holder consisting of a stack of multiple thin metal disks, all of which have an aperture in the center with a diameter of 1 to 10 cm, all having approximately the same shape and size. 1. A method for forming a tablet for a fixed small sample, which comprises filling a mixture of a solid sample and an alkali halide powder, and pressing the holder between two flat metal plates from above and below, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58048548A JPS59173730A (en) | 1983-03-23 | 1983-03-23 | Method for forming tablet of trace solid sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58048548A JPS59173730A (en) | 1983-03-23 | 1983-03-23 | Method for forming tablet of trace solid sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS59173730A true JPS59173730A (en) | 1984-10-01 |
Family
ID=12806422
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58048548A Pending JPS59173730A (en) | 1983-03-23 | 1983-03-23 | Method for forming tablet of trace solid sample |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59173730A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5353112A (en) * | 1990-01-25 | 1994-10-04 | Gersan Establishment | Optical inspection method and apparatus |
| JPH07140063A (en) * | 1993-11-12 | 1995-06-02 | Kuromato Sci Kk | Method and device for molding tablet sample for infrared spectrophotometry |
| JP2014034036A (en) * | 2012-08-07 | 2014-02-24 | Jasco Corp | Tablet holding frame body for infrared spectroscopic measurement and tablet molding method using the same |
| CN105372201A (en) * | 2015-10-30 | 2016-03-02 | 连云港市产品质量监督检验中心 | Sample wafer making device with microscopic infrared biological material |
-
1983
- 1983-03-23 JP JP58048548A patent/JPS59173730A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5353112A (en) * | 1990-01-25 | 1994-10-04 | Gersan Establishment | Optical inspection method and apparatus |
| JPH07140063A (en) * | 1993-11-12 | 1995-06-02 | Kuromato Sci Kk | Method and device for molding tablet sample for infrared spectrophotometry |
| JP2014034036A (en) * | 2012-08-07 | 2014-02-24 | Jasco Corp | Tablet holding frame body for infrared spectroscopic measurement and tablet molding method using the same |
| CN105372201A (en) * | 2015-10-30 | 2016-03-02 | 连云港市产品质量监督检验中心 | Sample wafer making device with microscopic infrared biological material |
| CN105372201B (en) * | 2015-10-30 | 2018-03-16 | 连云港市产品质量监督检验中心 | A kind of infrared microscopy biomaterial sample preparation sheet devices |
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