JPH01304349A - Thermal analysis apparatus - Google Patents
Thermal analysis apparatusInfo
- Publication number
- JPH01304349A JPH01304349A JP13285888A JP13285888A JPH01304349A JP H01304349 A JPH01304349 A JP H01304349A JP 13285888 A JP13285888 A JP 13285888A JP 13285888 A JP13285888 A JP 13285888A JP H01304349 A JPH01304349 A JP H01304349A
- Authority
- JP
- Japan
- Prior art keywords
- sample
- furnace body
- sensitive plate
- temp
- vessel
- 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.)
- Granted
Links
- 238000002076 thermal analysis method Methods 0.000 title claims description 4
- 238000005452 bending Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 2
- 229910001252 Pd alloy Inorganic materials 0.000 abstract description 4
- 238000005259 measurement Methods 0.000 abstract description 4
- PXXKQOPKNFECSZ-UHFFFAOYSA-N platinum rhodium Chemical compound [Rh].[Pt] PXXKQOPKNFECSZ-UHFFFAOYSA-N 0.000 abstract description 3
- BBKFSSMUWOMYPI-UHFFFAOYSA-N gold palladium Chemical compound [Pd].[Au] BBKFSSMUWOMYPI-UHFFFAOYSA-N 0.000 abstract description 2
- 229910000629 Rh alloy Inorganic materials 0.000 abstract 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 238000003466 welding Methods 0.000 description 3
- 229910001020 Au alloy Inorganic materials 0.000 description 2
- 229910001006 Constantan Inorganic materials 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000113 differential scanning calorimetry Methods 0.000 description 2
- 238000004455 differential thermal analysis Methods 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、示差熱分析その他の熱分析を行う場合におい
て、試料および標準試料を収容してこれを加熱または冷
却する炉の、特に試料および標準試料を保持する部分の
構成に関する。DETAILED DESCRIPTION OF THE INVENTION When performing differential thermal analysis or other thermal analysis, the present invention provides a furnace for storing samples and standard samples and heating or cooling them, particularly for the parts that hold the samples and standard samples. Concerning configuration.
示差熱分析あるいは示差走査熱■分析等においては、熱
伝導の良好な例えば銀で形成した垂直な円筒状の炉の中
にコンスタンタンあるいは白金・ロノウム合金または金
・パラノウ１＼合金等で形成した円板状の感熱板を水平
に配置して、その周縁を炉の側壁における例えば中央部
に溶接等で固定し、この感熱板上に試料および標準試料
を載置する装置が用いられる。しかしコンスタンタンは
耐酸化性および耐腐食性が低い欠点があり、また後者は
熱膨張率が小さく、銀のほぼ２分の１であるから、炉温
を仮に室温から７００度まで上昇させる場合について記
すと、炉の内径か感熱板の径より約０．１５〜０．２ｍ
ｍ程度大きくなって、この感熱板に張力が加わる。従っ
て炉温の上昇に、１り感熱板に不規則な歪み、変形を生
じて試料等の位置が移動するために測定曲線のベースラ
インに曲がりを生じて、これが測定誤差となる欠点かあ
った。従って本発明は炉体と試料等を載置する感熱板と
を異種の金属等で形成した場合においても上述のような
欠点の無い装置を提供するものである。In differential thermal analysis or differential scanning thermal analysis, a circle made of constantan, a platinum-ronium alloy, or a gold-paranow 1\ alloy, etc. is placed in a vertical cylindrical furnace made of silver, which has good thermal conductivity. An apparatus is used in which a plate-shaped heat-sensitive plate is arranged horizontally, its periphery is fixed to, for example, the center of the side wall of a furnace by welding or the like, and a sample and a standard sample are placed on the heat-sensitive plate. However, constantan has the disadvantage of low oxidation resistance and corrosion resistance, and the latter has a low coefficient of thermal expansion, which is approximately half that of silver, so we will write about the case where the furnace temperature is raised from room temperature to 700 degrees Celsius. and approximately 0.15 to 0.2 m from the inner diameter of the furnace or the diameter of the heat-sensitive plate.
m, and tension is applied to this heat-sensitive plate. Therefore, as the furnace temperature rises, irregular distortions and deformations occur in the heat-sensitive plate, and the position of the sample moves, causing a bend in the baseline of the measurement curve, which may lead to measurement errors. . Therefore, the present invention provides an apparatus that does not have the above-mentioned drawbacks even when the furnace body and the heat-sensitive plate on which the sample and the like are placed are made of different metals.
本発明は感熱板における水平な試料載置部を多角形に形
成して、その各辺にそれぞれ支持翼を設けると共に各支
持翼をほぼ９０度宛て２回折り曲げることにより、ほぼ
垂直な立ち上がり部と水平な支持部とを形成して、上記
支持１１≦を筒状炉体の側壁に固着し、水平な試料載置
部の中央にそれぞれ試料と標準試料とを載置する試料支
持台を対称的に形成したものである。すなわち試料載置
部を多角形として、その各辺に連結された支持翼をほぼ
９０度宛て２回折り曲げることにより、支持翼の先端を
炉体の垂直壁に固着しである。従って感熱板と炉体との
熱膨張率の差によって、水平な試料載置部の径と炉体の
内径との差が温度変化に伴って変動すると、上記支持翼
における垂直な立」二部が容易に傾斜してその変動分を
吸収する。このため水平な試料載置部に不規則な屈曲等
を生ずるおそれがなく、試料および標準試料を炉内の一
定位置に安定に保持して、その移動によるベースライン
の曲がりを防止することができる。In the present invention, the horizontal sample mounting portion of the heat-sensitive plate is formed into a polygonal shape, supporting wings are provided on each side of the horizontal sample mounting portion, and each supporting wing is bent twice at approximately 90 degrees, thereby creating a substantially vertical rising portion. The support 11≦ is fixed to the side wall of the cylindrical furnace body, and a sample support stand on which the sample and standard sample are placed is symmetrically placed in the center of the horizontal sample placement portion. It was formed in That is, the sample mounting portion is made into a polygon, and the support blades connected to each side of the polygon are bent twice to approximately 90 degrees, so that the tips of the support blades are fixed to the vertical wall of the furnace body. Therefore, if the difference between the diameter of the horizontal sample mounting part and the inner diameter of the furnace body changes with temperature changes due to the difference in the coefficient of thermal expansion between the heat sensitive plate and the furnace body, the two vertical vertical sections of the supporting blades easily slopes and absorbs the fluctuation. Therefore, there is no risk of irregular bending in the horizontal sample mounting section, and the sample and standard sample can be stably held at a fixed position in the furnace, and the baseline can be prevented from bending due to movement. .
第１図は本発明の示差走査熱量分析装置における炉体の
縦断面および電気的構成を示した図で、銀で形成した有
底円筒状の炉体Ｉの内部に白金・ロンラム合金の感熱板
２を水平に配置して、その周辺を炉体の側壁における環
状溝に挿入して熔接等により完全に固定しである。この
感熱板２の中央部に軸対称的に形成した支持台３および
４上？こ試料容器５と標準試料容器６とを載置すると共
に上記支持台３．４の下面に金・パラジウム合金の熱電
対線７．８の一端をそれぞれ添着しである。FIG. 1 is a diagram showing the vertical cross section and electrical configuration of the furnace body in the differential scanning calorimetry analyzer of the present invention. Inside the bottomed cylindrical furnace body I made of silver, there is a heat-sensitive plate made of platinum/Lonram alloy. 2 is placed horizontally, and its periphery is inserted into an annular groove in the side wall of the furnace body and completely fixed by welding or the like. On support stands 3 and 4 formed axially symmetrically in the center of this heat-sensitive plate 2? The sample container 5 and standard sample container 6 are placed thereon, and one end of a gold-palladium alloy thermocouple wire 7.8 is attached to the lower surface of the support stand 3.4.
これらの熱電対線を示差温度検出器９に接続し、また試
料容器５を乗せた支持台３に接続した白金・ロジウム熱
電対線１０と前記熱電対線７とを試料温度の検出器１１
に接続したもので、炉体１を蓋体Ｉ２で密封すると共に
図示してないがこの炉体を電熱器の中に収容して所定の
速度で温度を徐々に上昇させることにより、各温度にお
ける試料と標準試料との間の示差温度を検出する。ずな
わちこのような装置によって示差走査熱量分析を行うこ
とができる。These thermocouple wires are connected to a differential temperature detector 9, and the platinum-rhodium thermocouple wires 10 connected to the support stand 3 on which the sample container 5 is mounted and the thermocouple wires 7 are connected to a sample temperature detector 11.
The furnace body 1 is sealed with a lid body I2, and the furnace body is housed in an electric heater (not shown) to gradually raise the temperature at a predetermined rate. Detect the differential temperature between the sample and the standard sample. Thus, differential scanning calorimetry can be carried out with such an apparatus.
第２図は」１記装置にお（プる感熱板２の平面図、第３
図はそのＡ−Ａ断面図である。すなわちこの円形感熱板
２は周縁に多数の切り込み１３ Ｉ３・・・を等間隔で
形成して、その各切り込みに挟まれる部分を直角に近い
角度で２回折り曲げることにより中央に正多角形の試料
載置部Ｉ４を形成すると共にその各辺にそれぞれ独立の
支持翼１５゜１５・・・・を形成しである。この支持翼
１５゜１５・・・・の先端を熱伝導の良好な銀製の炉体
Ｉにおける側壁のほぼ中央部に形成した環状溝に挿入し
て熔接等により強固に固着し、支持台３゜４」二に試料
または標準試料の容器５６を第１図のように載置して分
析を行う。また中央の試料載置部１４には必要に応じて
、この部分の屈曲を防止するためのリブ１６．１７等を
適当な位置に適当な形状で形成し、かつ図示してないが
支持台３の下面には金・パラジウム合金の電熱対線７お
よび白金・ロジウムの熱電対線ＩＯを接続し、支持台４
の下面には金・パラジウム合金の熱電対線８を接続する
。Figure 2 is a plan view of the heat-sensitive plate 2 that is attached to the apparatus described in 1.
The figure is a sectional view taken along line A-A. In other words, this circular heat-sensitive plate 2 has a large number of notches 13 I3... formed at equal intervals on its periphery, and the portion sandwiched between the notches is bent twice at an angle close to a right angle to form a regular polygonal sample in the center. A mounting portion I4 is formed, and independent support wings 15°, 15, . . . are formed on each side thereof. The tips of the supporting blades 15° 15... are inserted into an annular groove formed approximately at the center of the side wall of the silver furnace body I, which has good thermal conductivity, and are firmly fixed by welding or the like, and the supporting blades 3° 4. Place the sample or standard sample container 56 on the second plate as shown in FIG. 1 and perform analysis. In addition, ribs 16, 17, etc. are formed at appropriate positions and in appropriate shapes in order to prevent bending of this portion, as necessary, on the central sample mounting portion 14, and, although not shown, the support base 3 A gold/palladium alloy thermocouple wire 7 and a platinum/rhodium thermocouple wire IO are connected to the bottom surface of the support base 4.
A thermocouple wire 8 made of gold/palladium alloy is connected to the bottom surface of the thermocouple wire 8 .
上記実施例のように本発明の装置は感熱板２の周縁に多
数の切り込み１３．１３・・・を設けて、その切り込み
で挟まれる部分をほぼ直角に２回折り曲げて、周縁を炉
体Ｉの側壁に固定したものである。従って中央の試料載
置部１４は多角形を形成して、その各辺にほぼ垂直な平
面状部分が連結されて、かっこの平面状部分の両端に何
れも水平な直線状の折り曲げ部が設けられる。このため
炉材と感熱板との熱膨張率の差によって感熱板の試料載
置部が水平面内で相対的に拡大あるいは収縮すると、切
り込みＩ３に挟まれるほぼ直角に立ち上がった部分の傾
斜角が容易に変化して、上記拡大・収縮を吸収する。従
って水平な試料の載置部１４に大きな歪み力が加わって
、その部分に屈曲、変形を生ずるようなおそれがないも
ので、このため試料位置が移動し、あるいはその容器５
６が傾斜して、大きな測定誤差を生ずるような欠点が除
かれる。As in the above embodiment, the device of the present invention has a large number of notches 13, 13... provided on the periphery of the heat-sensitive plate 2, and the portion sandwiched by the notches is bent twice at approximately right angles, and the periphery is folded into the furnace body I. It is fixed to the side wall of. Therefore, the central sample holder 14 forms a polygon, with substantially perpendicular planar portions connected to each side of the polygon, and horizontal linear bent portions at both ends of the planar portion of the bracket. It will be done. Therefore, when the sample mounting part of the heat-sensitive plate relatively expands or contracts in the horizontal plane due to the difference in thermal expansion coefficient between the furnace material and the heat-sensitive plate, the inclination angle of the almost right-angled part sandwiched between the notches I3 becomes easy. to absorb the expansion and contraction mentioned above. Therefore, there is no risk that a large strain force will be applied to the horizontal sample mounting section 14, causing bending or deformation in that section, and that the sample position will move or the container 5 may be bent or deformed.
6 is tilted, resulting in large measurement errors.
第１図は本発明実施例の縦断面並びに装置の電気的構成
を示した図、第２図は第１図における感熱板の平面図、
第３図は第２図のバーＡ断面図である。
なお、図において１は炉体、２は感熱板、３４は試別支
持台、１３は切り込み、１４は試料載置部、１５は支持
翼、７８１０は熱電対線である。FIG. 1 is a diagram showing a longitudinal cross section of an embodiment of the present invention and the electrical configuration of the device, FIG. 2 is a plan view of the heat-sensitive plate in FIG. 1,
FIG. 3 is a sectional view of bar A in FIG. In the figure, 1 is a furnace body, 2 is a heat-sensitive plate, 34 is a sample support stand, 13 is a notch, 14 is a sample mounting section, 15 is a support blade, and 7810 is a thermocouple wire.
Claims (1)
方向に等間隔で形成して、上記切り込みに挟まれる各部
分をほぼ直角にそれぞれ２回あて折り曲げることにより
中央に多角形の試料載置部を設けると共にその各辺にそ
れぞれ独立の支持翼を形成して、各支持翼の先端を熱伝
導の良好な物質で形成した筒状炉体の側壁にそれぞれ固
着し、かつ前記試料載置部に試料および標準試料をそれ
ぞれ載置する試料支持台を軸対称的に形成して、上記試
料支持台にそれぞれ熱電対線を連結した熱分析装置A polygonal sample is placed in the center by forming a large number of notches at equal intervals in the radial direction on the periphery of a nearly circular heat-sensitive plate, and bending each portion between the notches twice at nearly right angles. and independent supporting wings are formed on each side of the supporting wings, the tips of each supporting wing are respectively fixed to the side wall of the cylindrical furnace body made of a material with good heat conduction, and the sample mounting part is A thermal analysis device in which a sample support stand on which a sample and a standard sample are respectively placed is formed axially symmetrically, and thermocouple wires are connected to each of the sample support stands.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13285888A JPH0656369B2 (en) | 1988-06-01 | 1988-06-01 | Thermal analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13285888A JPH0656369B2 (en) | 1988-06-01 | 1988-06-01 | Thermal analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01304349A true JPH01304349A (en) | 1989-12-07 |
| JPH0656369B2 JPH0656369B2 (en) | 1994-07-27 |
Family
ID=15091175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13285888A Expired - Fee Related JPH0656369B2 (en) | 1988-06-01 | 1988-06-01 | Thermal analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0656369B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0213841A (en) * | 1988-06-30 | 1990-01-18 | Mc Sci:Kk | Heat analyzer |
| KR100376534B1 (en) * | 1998-12-21 | 2003-06-18 | 주식회사 포스코 | Sample stand |
-
1988
- 1988-06-01 JP JP13285888A patent/JPH0656369B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0213841A (en) * | 1988-06-30 | 1990-01-18 | Mc Sci:Kk | Heat analyzer |
| KR100376534B1 (en) * | 1998-12-21 | 2003-06-18 | 주식회사 포스코 | Sample stand |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0656369B2 (en) | 1994-07-27 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |