JPH06294727A - Sample holder for thermo-balance - Google Patents
Sample holder for thermo-balanceInfo
- Publication number
- JPH06294727A JPH06294727A JP10601393A JP10601393A JPH06294727A JP H06294727 A JPH06294727 A JP H06294727A JP 10601393 A JP10601393 A JP 10601393A JP 10601393 A JP10601393 A JP 10601393A JP H06294727 A JPH06294727 A JP H06294727A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- sample holder
- pin
- insertion hole
- holder
- 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.)
- Withdrawn
Links
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、例えば合成樹脂、医薬
品等の性質を知るために行われる熱重量測定（ＴＧ）に
使用される熱天秤装置に関するもので、特に水平型熱天
秤装置の試料ホルダーに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thermobalance device used for thermogravimetric measurement (TG) performed to know the properties of, for example, synthetic resins and pharmaceuticals, and particularly to a sample of a horizontal thermobalance device. Regarding the holder.
【０００２】[0002]
【従来の技術】従来、水平型熱天秤装置の試料ホルダー
としては、平底付の筒状をなすものが最も一般的であ
る。また、底部内面を逆円錐形に窪ませた試料ホルダー
も知られている（実開昭６０−６４２４６号公報）。2. Description of the Related Art Conventionally, as a sample holder for a horizontal thermobalance device, a cylindrical holder having a flat bottom is most common. A sample holder in which the inner surface of the bottom is recessed into an inverted conical shape is also known (Japanese Utility Model Laid-Open No. 60-64246).
【０００３】[0003]
【発明が解決しようとする課題】ところで、試料ホルダ
ーは、支点部から水平に延びる天秤ビームの一端部に、
測定すべき試料を収納するために設けられているもので
ある。また、最近の合成樹脂熱重量測定においては、熱
安定性を重量の微小変化として捉える高感度測定が主流
となっている。By the way, the sample holder is provided at one end portion of the balance beam extending horizontally from the fulcrum portion.
It is provided to store the sample to be measured. Further, in recent thermogravimetric measurements of synthetic resins, high-sensitivity measurement, which regards thermal stability as a minute change in weight, has become the mainstream.
【０００４】しかしながら、従来の平底付筒状容器の試
料ホルダーでは、加熱による変形や溶融に伴って試料が
試料ホルダー内で移動してその重心位置が変化してしま
うことにより、正確な測定が妨げられている。即ち、試
料ホルダー内の試料の重心が支点部から遠ざかる方向に
移動した場合、現実の試料より重い値を測定してしま
い、逆に支点部に近づく方向に移動した場合には、現実
の試料より軽い値を測定してしまうことになる。However, in the conventional sample holder of the cylindrical container with a flat bottom, the sample moves within the sample holder due to deformation and melting due to heating, and the position of the center of gravity thereof changes, which hinders accurate measurement. Has been. That is, if the center of gravity of the sample in the sample holder moves in a direction away from the fulcrum, a value that is heavier than the actual sample will be measured. You will end up measuring a light value.
【０００５】また、底部内面を逆円錐形に窪ませた試料
ホルダーの場合、当該底面の傾斜によって試料の移動を
防止することができるが、試料と窪んだ底面との間に空
間が残されるので、試料の分解ガスがこの空間に閉じ込
められて発散されずに残ってしまい、現実の試料より重
い値を測定してしまう問題がある。Further, in the case of a sample holder whose bottom inner surface is recessed in an inverted conical shape, it is possible to prevent the sample from moving due to the inclination of the bottom surface, but a space is left between the sample and the recessed bottom surface. However, there is a problem that the decomposed gas of the sample is confined in this space and remains without being diffused, so that a value heavier than the actual sample is measured.
【０００６】特に最近の高感度測定においては、０〜２
％乃至０〜４％フルスケールで測定しており、わずかな
測定誤差が測定精度に大きな影響を及ぼすので、上記の
ような理由から、信頼性の高い測定結果が得られていな
い。Particularly in recent high-sensitivity measurements, 0-2
% To 0 to 4% full scale, and a slight measurement error has a great influence on the measurement accuracy. For this reason, highly reliable measurement results have not been obtained.
【０００７】本発明は、このような従来の問題点に鑑み
てなされたもので、水平型熱天秤装置による高感度測定
において、加熱に伴う試料の移動や分解ガスの閉じ込め
による測定精度の低下を防止することを目的とする。The present invention has been made in view of the above-mentioned conventional problems, and in high-sensitivity measurement using a horizontal thermobalance device, a decrease in measurement accuracy due to movement of a sample or confinement of decomposed gas accompanying heating. The purpose is to prevent.
【０００８】[0008]
【課題を解決するための手段】このために本発明では、
図１に示されるように、差し込み孔１が形成された試料
２を差し込み支持するためのピン３が底部に立てられて
いる熱天秤用試料ホルダー４としているものである。To this end, in the present invention,
As shown in FIG. 1, a sample holder 4 for a thermobalance having a pin 3 for inserting and supporting a sample 2 in which an insertion hole 1 is formed is erected at the bottom.
【０００９】[0009]
【実施例及び作用】図１に示されるように、本実施例に
係る試料ホルダー４は、平底付の円筒形をなすホルダー
本体５の内部に、ピン３が立てられた円形の基板６が収
容されていることによって、底部にピン３が立てられた
ものとなっている。Embodiments and Functions As shown in FIG. 1, a sample holder 4 according to this embodiment accommodates a circular substrate 6 on which pins 3 are erected inside a holder body 5 having a flat bottomed cylindrical shape. As a result, the pin 3 is erected on the bottom.
【００１０】このピン３は、差し込み孔１が形成された
試料２を差し込み支持させるもので、ホルダー本体５の
底部中央に位置することが好ましい。また、試料２は、
例えば合成樹脂ペレット等で、この試料２の差し込み孔
１は例えばドリル加工等で容易に形成することができ
る。The pin 3 inserts and supports the sample 2 having the insertion hole 1 formed therein, and is preferably located at the center of the bottom of the holder body 5. Sample 2 is
For example, synthetic resin pellets or the like can be used to easily form the insertion hole 1 of the sample 2 by drilling or the like.
【００１１】上記のように底部にピン３を立て、そこに
試料２の差し込み孔１を差し込んで支持させると、分解
ガスを閉じ込めてしまう空間を残すことなく試料２を支
持できる。また、この試料２の支持によって、軟化した
試料の倒伏等による試料２の重心移動を防止することが
できる。When the pin 3 is erected on the bottom and the insertion hole 1 of the sample 2 is inserted and supported therein as described above, the sample 2 can be supported without leaving a space for trapping the decomposition gas. Further, by supporting the sample 2, it is possible to prevent the center of gravity of the sample 2 from moving due to the fall of the softened sample or the like.
【００１２】ピン３は、ホルダー本体５の底部に、例え
ば接着や融着等で直接立てて設置してもよいが、工作の
容易性から、図示されるような基板６上に立てて設置
し、この基板６ごとホルダー本体５内に収容しておくこ
とが好ましい。The pins 3 may be installed directly on the bottom of the holder body 5 by, for example, bonding or fusing, but for the sake of ease of work, the pins 3 are installed on the substrate 6 as shown in the drawing. It is preferable that the whole substrate 6 is housed in the holder body 5.
【００１３】ホルダー本体５、ピン３及び基板６の材質
としては、例えばアルミニウムや白金が使用されるが、
通常はアルミニウムである。As the material of the holder body 5, the pins 3 and the substrate 6, for example, aluminum or platinum is used.
It is usually aluminum.
【００１４】ピン３を基板６上に立てて設置するには、
図２に示されるように、別部材として用意したピン３と
基板６を、例えば接着や融着によって接合することでも
よいが、ピン３をしっかり基板６上に立てるには、図３
に示されるように、円柱状材料７を、ピン３部分と基板
６部分を残して切削することで行うことが好ましい。ま
た、図４に示されるように、基板６の一部を切り立てて
ピン３とすることもできる。To set the pin 3 upright on the substrate 6,
As shown in FIG. 2, the pins 3 and the substrate 6 prepared as separate members may be joined by, for example, adhesion or fusion, but in order to firmly stand the pins 3 on the substrate 6,
It is preferable that the cylindrical material 7 is cut by leaving the pin 3 portion and the substrate 6 portion as shown in FIG. Further, as shown in FIG. 4, a part of the substrate 6 may be cut up to form the pins 3.
【００１５】次に、上述のような本発明に係る試料ホル
ダー４及び従来の試料ホルダーを用いてＴＧ測定結果に
ついて説明する。Next, TG measurement results will be described using the sample holder 4 according to the present invention and the conventional sample holder as described above.
【００１６】使用した試料ホルダー、試料、水平型熱天
秤装置は次の通りである。The sample holder, sample, and horizontal type thermobalance apparatus used are as follows.
【００１７】（１）試料ホルダー 本発明試料ホルダー：図１及び図２に示される係る試料
ホルダー。(1) Sample Holder Sample holder of the present invention: The sample holder shown in FIGS. 1 and 2.
【００１８】従来の試料ホルダーＡ：底部内面を逆円錐
形に窪ませた試料ホルダー。Conventional sample holder A: A sample holder in which the inner surface of the bottom is depressed in an inverted conical shape.
【００１９】従来の試料ホルダーＢ：平底付円筒状の試
料ホルダー。Conventional sample holder B: A cylindrical sample holder with a flat bottom.
【００２０】（２）試料 ＡＢＳ樹脂のペレットにドリル加工で差し込み孔を形成
したもの。(2) Specimen ABS resin pellets with insert holes formed by drilling.
【００２１】（３）水平型熱天秤装置 セイコー電子工業社製水平型熱天秤装置「ＲＴＧ−２２
０型」。(3) Horizontal Thermobalance Device Horizontal thermobalance device "RTG-22" manufactured by Seiko Instruments Inc.
Type 0 ".
【００２２】上記試料について、本発明の試料ホルダー
と従来の試料ホルダーＡを用いて夫々測定を行った。測
定したＴＧ曲線を図５に示す。The above samples were measured using the sample holder of the present invention and the conventional sample holder A, respectively. The measured TG curve is shown in FIG.
【００２３】図５から明らかなように、従来の試料ホル
ダーＡを用いた場合、分解ガスが窪んだ底部に溜る結
果、本発明の試料ホルダーを用いた場合に比して質量減
少が低く、真値を示していないことが分かる。As is apparent from FIG. 5, when the conventional sample holder A is used, the decomposition gas accumulates at the bottom of the depression, and as a result, the mass reduction is lower than that in the case where the sample holder of the present invention is used. It can be seen that the value is not shown.
【００２４】また、上記試料について、従来の試料ホル
ダーＢを用いて繰り返し測定を行った。その結果、図６
及び図７に示されるようなＴＧ曲線となる場合が頻繁に
発生した。Further, the above sample was repeatedly measured using the conventional sample holder B. As a result, FIG.
Also, the TG curve as shown in FIG. 7 frequently occurred.
【００２５】図６においては試料の重心が支点部側に移
動したと見られる段差状の急激な変化が見られ、図７に
おいては試料の重心が反支点部側に移動したと見られる
段差状の急激な変化が見られる。In FIG. 6, a step-like abrupt change in which the center of gravity of the sample seems to have moved to the fulcrum side is seen, and in FIG. 7, the center of gravity of the sample seems to have moved to the anti-fulcrum part side. There is a sharp change in.
【００２６】[0026]
【発明の効果】本発明は、以上説明した通りのものであ
り、試料２の重心移動や分解ガスの閉じ込めを生じない
ため、水平型熱天秤装置による高感度測定の測定精度が
著しく向上するものである。EFFECTS OF THE INVENTION The present invention is as described above, and since the center of gravity of the sample 2 and the decomposition gas are not trapped, the measurement accuracy of high-sensitivity measurement by the horizontal thermobalance device is remarkably improved. Is.
【図１】本発明に係る試料ホルダーの一実施例を示す縦
断面図である。FIG. 1 is a vertical sectional view showing an embodiment of a sample holder according to the present invention.
【図２】ピンを基板に立てる場合の一例を示す斜視図で
ある。FIG. 2 is a perspective view showing an example of a case where pins are set up on a substrate.
【図３】ピンを基板に立てる場合の他の例を示す斜視図
である。FIG. 3 is a perspective view showing another example in which pins are set up on a substrate.
【図４】ピンを基板に立てる場合の他の例を示す斜視図
である。FIG. 4 is a perspective view showing another example in which pins are set up on a substrate.
【図５】本発明に係る試料ホルダーを用いた場合と従来
の試料ホルダーＡを用いた場合の各ＴＧ曲線を示す図で
ある。FIG. 5 is a diagram showing each TG curve when the sample holder according to the present invention is used and when the conventional sample holder A is used.
【図６】従来の試料ホルダーＢを用いて繰り返し測定を
行った時に頻繁に生じたＴＧ曲線の一例を示す図であ
る。FIG. 6 is a diagram showing an example of a TG curve that frequently occurs when repeated measurement is performed using a conventional sample holder B.
【図７】従来の試料ホルダーＢを用いて繰り返し測定を
行った時に頻繁に生じたＴＧ曲線の他の例を示す図であ
る。FIG. 7 is a diagram showing another example of a TG curve that frequently occurs when repeated measurement is performed using the conventional sample holder B.
１ 差し込み孔 ２ 試料 ３ ピン ４ 試料ホルダー ５ ホルダー本体 ６ 基板 ７ 円柱状材料 1 insertion hole 2 sample 3 pin 4 sample holder 5 holder body 6 substrate 7 columnar material
Claims (1)
支持するためのピンが底部に立てられていることを特徴
とする熱天秤用試料ホルダー。1. A sample holder for a thermobalance, wherein a pin for inserting and supporting a sample having an insertion hole is erected on the bottom.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10601393A JPH06294727A (en) | 1993-04-09 | 1993-04-09 | Sample holder for thermo-balance |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10601393A JPH06294727A (en) | 1993-04-09 | 1993-04-09 | Sample holder for thermo-balance |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06294727A true JPH06294727A (en) | 1994-10-21 |
Family
ID=14422785
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10601393A Withdrawn JPH06294727A (en) | 1993-04-09 | 1993-04-09 | Sample holder for thermo-balance |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06294727A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007285944A (en) * | 2006-04-19 | 2007-11-01 | Kureha Corp | Moisture measuring method of thermoplastic resin due to thermobalance method |
-
1993
- 1993-04-09 JP JP10601393A patent/JPH06294727A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007285944A (en) * | 2006-04-19 | 2007-11-01 | Kureha Corp | Moisture measuring method of thermoplastic resin due to thermobalance method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 20000704 |