JPH06201621A - Thermal analyzer - Google Patents
Thermal analyzerInfo
- Publication number
- JPH06201621A JPH06201621A JP36001992A JP36001992A JPH06201621A JP H06201621 A JPH06201621 A JP H06201621A JP 36001992 A JP36001992 A JP 36001992A JP 36001992 A JP36001992 A JP 36001992A JP H06201621 A JPH06201621 A JP H06201621A
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- Prior art keywords
- sample
- amount
- correction
- data
- temperature
- 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.)
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- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
(57)【要約】
【目的】 簡単な操作で正確な補正を行なえるようにす
る。
【構成】 熱膨張量が既知の試料を熱機械分析装置で測
定し、そのときの測定値Ｌo(Ｔ）が求められる。その試
料の理論上の伸びをＬst(Ｔ）とすると、Ｌst(Ｔ）から
Ｌo(Ｔ）が引かれることによって補正値（Ｌsys(Ｔ）＋
Ｌb）が求められ、その値が各温度ごとの補正データと
して全膨張測定補正データ記憶手段１０に記憶される。
熱膨張量が未知の試料を測定したとき、その測定データ
Ｌo(Ｔ）に対し、データ補正手段１２によって、全膨張
測定補正データ記憶手段１０に記憶されている補正デー
タ（Ｌsys(Ｔ）＋Ｌb）の各温度ごとの補正値が加えら
れ、その試料の真の熱膨張量Ｌst(Ｔ）が求められる。
(57) [Summary] [Purpose] To make accurate corrections with simple operations. [Configuration] A sample having a known thermal expansion amount is measured by a thermomechanical analyzer, and a measured value Lo (T) at that time is obtained. If the theoretical elongation of the sample is Lst (T), the correction value (Lsys (T) +
Lb) is obtained, and the value is stored in the total expansion measurement correction data storage means 10 as correction data for each temperature.
When a sample whose thermal expansion amount is unknown is measured, correction data (Lsys (T) + Lb) stored in the total expansion measurement correction data storage unit 10 by the data correction unit 12 for the measurement data Lo (T). The correction value for each temperature is added to obtain the true thermal expansion amount Lst (T) of the sample.
Description
【０００１】[0001]
【産業上の利用分野】本発明は熱機械分析装置、示差熱
分析装置又は示差走査熱量計などの熱分析装置に関し、
特にそのデータ処理装置に特徴を有する熱分析装置に関
するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a thermal analysis device such as a thermomechanical analysis device, a differential thermal analysis device or a differential scanning calorimeter,
In particular, the present invention relates to a thermal analysis device characterized by its data processing device.
【０００２】[0002]
【従来の技術】熱分析装置のうち、熱機械分析装置は、
試料を加熱したときの試料の伸びを温度の関数として測
定するものである。熱機械分析装置における全膨張測定
を模式的に表したものが図１であり、支持管２の底面に
試料４をおき、試料４の上面に検出棒６の先端を接触さ
せ、試料４の温度を変化させて検出棒６により試料４の
膨張量を測定する。温度を上昇させると、試料４の膨張
量Ｌ（伸び）が図２に示されるように変化したとする
と、膨張量は（Ｌ2−Ｌ1）／（Ｔ2−Ｔ1）として求めら
れる。しかし、温度が上昇するにつれて支持管２や検出
棒６を含む測定系も伸びるため、測定データには誤差が
生じる。すなわち、測定系の温度を上昇させると、試料
４とともに検出棒６も支持管２も伸びる。支持管２と検
出棒６の材質が同じである場合には検出棒６の部分では
誤差が発生しないが、試料４の長さ部分ｘについては試
料４の伸びと支持管２の伸びの差が誤差としてデータに
含まれることになる。その誤差を補正する方法として、
温度の測定範囲をＴ1〜Ｔ2とすれば、その間の温度Ｔ0
における測定系の膨張量を、膨張量が既知の試料を測定
することによって求め、Ｔ1とＴ2の間で求められた膨張
量をＴ0での測定系の補正値により補正している。2. Description of the Related Art Of the thermal analyzers, the thermomechanical analyzer is
It measures the elongation of a sample when it is heated as a function of temperature. FIG. 1 schematically shows the total expansion measurement in the thermomechanical analyzer. The sample 4 is placed on the bottom surface of the support tube 2, the tip of the detection rod 6 is brought into contact with the top surface of the sample 4, and the temperature of the sample 4 is measured. And the amount of expansion of the sample 4 is measured by the detection rod 6. Assuming that the expansion amount L (elongation) of the sample 4 changes as shown in FIG. 2 when the temperature is increased, the expansion amount is calculated as (L 2 −L 1 ) / (T 2 −T 1 ). However, as the temperature rises, the measurement system including the support tube 2 and the detection rod 6 also expands, so that an error occurs in the measurement data. That is, when the temperature of the measurement system is raised, both the detection rod 6 and the support tube 2 extend along with the sample 4. When the material of the support tube 2 and the detection rod 6 is the same, no error occurs in the portion of the detection rod 6, but for the length x of the sample 4, there is a difference between the extension of the sample 4 and the extension of the support tube 2. It will be included in the data as an error. As a method of correcting the error,
Assuming that the temperature measurement range is T 1 to T 2 , the temperature T 0 between them is T 0.
The amount of expansion of the measurement system in ( 1) is obtained by measuring a sample with a known expansion amount, and the amount of expansion obtained between T 1 and T 2 is corrected by the correction value of the measurement system at T 0 .
【０００３】示差熱分析装置（ＤＴＡ）では、試料と基
準物質を炉内で同じ条件で加熱し、両者の温度差を測定
する。このときに試料に起こる結晶化や融解などの現象
を基準物質との温度差からピークとして検出し、その面
積から吸熱量や発熱量を求める。例えば図３に示される
ようにそのデータ曲線のピークの面積Ｓを求め、それに
比例定数Ｋをかけて熱量ΔＨを求める。In a differential thermal analyzer (DTA), a sample and a reference substance are heated in a furnace under the same conditions, and the temperature difference between them is measured. Phenomena such as crystallization and melting that occur in the sample at this time are detected as a peak from the temperature difference from the reference substance, and the amount of heat absorption and the amount of heat generation are obtained from the area. For example, as shown in FIG. 3, the area S of the peak of the data curve is obtained, and the proportional constant K is multiplied to obtain the heat quantity ΔH.
【０００４】示差走査熱量計（ＤＳＣ）の場合は、試料
と基準物質が同一温度で上昇するようにそれぞれに加熱
用の電流を流し、その通電量から試料の発熱量や吸熱量
を求める。この場合もデータ曲線としては図３のような
ピークが得られる。データ曲線のピーク面積Ｓを熱量に
変換する比例定数Ｋは温度の関数であり、従来は温度に
関する二次式の形で表わし、ピークの頂点を補正点Ｔ0
として選び、そのＴ0における比例定数Ｋを面積Ｓにか
けている。Ｋの温度に対する各項の係数を求めるため
に、融解熱の知られている高純度金属を試料として測定
し、その結果から係数を求めている。In the case of a differential scanning calorimeter (DSC), a heating current is applied to each of the samples so that the sample and the reference substance rise at the same temperature, and the heat generation amount and the heat absorption amount of the sample are determined from the energization amount. Also in this case, the peak as shown in FIG. 3 is obtained as the data curve. The proportional constant K for converting the peak area S of the data curve into the amount of heat is a function of temperature, and is conventionally expressed in the form of a quadratic equation relating to temperature, and the apex of the peak is corrected to T 0
And the area S is multiplied by the proportional constant K at T 0 . In order to obtain the coefficient of each term with respect to the temperature of K, a high-purity metal whose heat of fusion is known is measured as a sample, and the coefficient is calculated from the result.
【０００５】[0005]
【発明が解決しようとする課題】熱機械分析において、
図２に示されるように測定温度範囲Ｔ1〜Ｔ2の間の１点
Ｔ0のみで補正を行なうとすれば、得られた解析結果の
定量性が乏しくなる。示差熱分析装置や示差走査熱量計
で図３のようにピークトップの温度で補正を行なう場合
には、ピークの形状によっては補正点が面積の重心と異
なる場合が生じる。そのときには誤差が生じる。本発明
はこのような熱分析装置のデータ処理を行なう際に、簡
単な操作で正確な補正を行なえるデータ処理装置を備え
た熱分析装置を提供することを目的とするものである。In thermomechanical analysis,
As shown in FIG. 2, if the correction is performed only at one point T 0 between the measurement temperature ranges T 1 and T 2 , the quantification of the obtained analysis result becomes poor. When correction is performed at the peak top temperature as shown in FIG. 3 with a differential thermal analyzer or a differential scanning calorimeter, the correction point may be different from the center of gravity of the area depending on the shape of the peak. At that time, an error occurs. It is an object of the present invention to provide a thermal analysis device equipped with a data processing device capable of performing accurate correction with a simple operation when performing data processing of such a thermal analysis device.
【０００６】[0006]
【課題を解決するための手段】図４に本発明を熱機械分
析装置に適用した場合のデータ処理装置を示す。１０は
熱膨張量が既知の試料を測定したときの既知量と実測値
との差から求められた各温度における補正値を記憶する
全膨張測定補正データ記憶手段であり、１２は熱膨張量
未知の試料を測定したときの各温度の測定データを全膨
張測定補正データ記憶手段１０に記憶された補正値によ
り補正するデータ補正手段である。FIG. 4 shows a data processing device when the present invention is applied to a thermomechanical analysis device. Reference numeral 10 is a total expansion measurement correction data storage means for storing a correction value at each temperature obtained from a difference between a known amount and a measured value when a sample having a known thermal expansion amount is measured, and 12 is an unknown thermal expansion amount. This is a data correction means for correcting the measurement data of each temperature when the sample is measured with the correction value stored in the total expansion measurement correction data storage means 10.
【０００７】図５に本発明を示差熱分析装置又は示差走
査熱量計に適用した場合のデータ処理装置を示す。１４
は吸熱量又は発熱量が既知の試料を測定したときの既知
量と実測値との熱量の差から求められたデータ曲線の補
正係数を記憶する補正係数記憶手段であり、１６は吸熱
量又は発熱量が未知の試料を測定したときのデータ曲線
を補正係数記憶手段１４に記憶された補正係数を用いて
各温度ごとに補正するデータ曲線補正手段、１８はその
補正されたデータ曲線のピーク面積から吸熱量又は発熱
量を算出する面積算出手段である。FIG. 5 shows a data processing device when the present invention is applied to a differential thermal analyzer or a differential scanning calorimeter. 14
Is a correction coefficient storage means for storing the correction coefficient of the data curve obtained from the difference between the heat quantity of the known amount and the measured value when the sample of which the heat absorption or heat generation is known is measured, and 16 is the heat absorption or heat generation. Data curve correction means for correcting a data curve when an amount of an unknown sample is measured for each temperature using the correction coefficient stored in the correction coefficient storage means 14, and 18 is a peak area of the corrected data curve. It is an area calculation means for calculating the amount of heat absorption or the amount of heat generation.
【０００８】[0008]
【作用】熱機械分析を示す図１において、温度Ｔにおけ
る試料の熱膨張測定値をＬo(Ｔ）、真の熱膨張値をＬst
(Ｔ）、支持管２の熱膨張をＬsys(Ｔ）とし、測定系の
温度分布によるバックグラウンドをＬｂとすれば、全膨
張測定では次の関係式（１）から（３）が成立する。 Ｌo(Ｔ）＝Ｌst(Ｔ）−（Ｌsys(Ｔ）＋Ｌb） （１） Ｌsys(Ｔ）＋Ｌｂ＝Ｌst(Ｔ）−Ｌo(Ｔ） （２） Ｌst(Ｔ）＝Ｌo(Ｔ）＋（Ｌsys(Ｔ）＋Ｌb） （３） この（３）式の関係を模式的に示したのが図６である。In FIG. 1 showing the thermomechanical analysis, the measured thermal expansion value of the sample at the temperature T is Lo (T) and the true thermal expansion value is Lst.
(T), if the thermal expansion of the support tube 2 is Lsys (T) and the background due to the temperature distribution of the measurement system is Lb, the following relational expressions (1) to (3) are established in the total expansion measurement. Lo (T) = Lst (T)-(Lsys (T) + Lb) (1) Lsys (T) + Lb = Lst (T) -Lo (T) (2) Lst (T) = Lo (T) + (Lsys (T) + Lb) (3) FIG. 6 schematically shows the relationship of the equation (3).
【０００９】熱機械分析に適用した本発明は、熱膨張量
が既知の試料を用いて求めた測定系の伸び（Ｌsys(Ｔ）
＋Ｌb）を補正データとして記憶しておき、試料を測定
したときにその測定データＬo(Ｔ）の各温度に対し記憶
されている補正データを加えることによって、図７に示
されるように各温度における真の熱膨張Ｌst(Ｔ）を求
めるものである。熱機械分析に適用した本発明で、補正
データの記憶の動作を図８に、試料の測定の動作を図９
に示す。図８に示されるように、補正係数（熱膨張量）
が文献値などで分かっている試料を熱機械分析装置で測
定し、そのときの測定値Ｌo(Ｔ）を求められる。その試
料の理論上の伸びをＬst(Ｔ）とすると、Ｌst(Ｔ）から
Ｌo(Ｔ）が引かれることによって補正値（Ｌsys(Ｔ）＋
Ｌb）が求められる。その値が各温度ごとの補正データ
として全膨張測定補正データ記憶手段１０に記憶され
る。The present invention applied to thermomechanical analysis is based on the elongation (Lsys (T) of the measuring system obtained by using a sample whose thermal expansion amount is known.
+ Lb) is stored as correction data, and when the sample is measured, the stored correction data is added to each temperature of the measurement data Lo (T), so that at each temperature as shown in FIG. The true thermal expansion Lst (T) is obtained. In the present invention applied to thermomechanical analysis, the operation of storing correction data is shown in FIG. 8 and the operation of measuring a sample is shown in FIG.
Shown in. As shown in FIG. 8, the correction coefficient (thermal expansion amount)
Is measured by a thermomechanical analyzer, and the measured value Lo (T) at that time can be obtained. If the theoretical elongation of the sample is Lst (T), the correction value (Lsys (T) +
Lb) is required. The value is stored in the total expansion measurement correction data storage means 10 as correction data for each temperature.
【００１０】熱膨張量が未知の試料を測定するときは、
図９に示されるように、その測定データＬo(Ｔ）に対
し、データ補正手段１２によって、全膨張測定補正デー
タ記憶手段１０に記憶されている補正データ（Ｌsys
(Ｔ）＋Ｌb）の各温度ごとの補正値が加えられ、その試
料の真の熱膨張量Ｌst(Ｔ）が求められる。示差熱分析
装置又は示差走査熱量計においては、例えば図１０
（Ａ）のようなデータ曲線が得られたとする。ベースラ
インが傾いている場合は従来からも行なわれているよう
にベースライン補正が行なわれることにより、（Ｂ）の
ようにベースラインが水平になるように補正される。し
かし、ベースライン補正はピーク面積の補正ではない。
そこで、本発明によりこのデータ曲線の各温度における
各データが補正されることによって、（Ｃ）に示される
ようにピーク面積が補正される。When measuring a sample whose thermal expansion amount is unknown,
As shown in FIG. 9, for the measured data Lo (T), the correction data (Lsys stored in the total expansion measurement correction data storage unit 10 by the data correction unit 12 is used.
A correction value of (T) + Lb) for each temperature is added to obtain the true thermal expansion amount Lst (T) of the sample. In the differential thermal analyzer or the differential scanning calorimeter, for example, FIG.
It is assumed that the data curve as shown in (A) is obtained. When the baseline is tilted, the baseline correction is performed as is conventionally done, so that the baseline is corrected to be horizontal as shown in (B). However, the baseline correction is not a peak area correction.
Therefore, the peak area is corrected as shown in (C) by correcting each data at each temperature of this data curve according to the present invention.
【００１１】一般的に、示差熱分析装置及び示差走査熱
量計の出力信号は、 −ａＲ（Ｃｓ−Ｃｒ） （４） として表わされる。ここで、ａは昇温速度、Ｒは熱伝達
係数、Ｃｓは試料の熱容量、Ｃｒは基準物質の熱容量で
ある。本発明ではこの熱伝達係数Ｒを温度Ｔの二次関数
で近似し、 Ｒ＝αＴ2＋βＴ＋γ （５） と表わす。その各項の係数α，β，γを補正データとす
る。図１１に示されるように、吸熱量又は発熱量が既知
の試料として例えば高純度金属を用いてその融解熱を測
定し、そのデータ曲線から補正係数α，β，γが求めら
れ、補正データとして補正係数記憶手段１４に記憶され
る。Generally, the output signals of the differential thermal analyzer and the differential scanning calorimeter are expressed as -aR (Cs-Cr) (4). Here, a is the temperature rising rate, R is the heat transfer coefficient, Cs is the heat capacity of the sample, and Cr is the heat capacity of the reference substance. In the present invention, this heat transfer coefficient R is approximated by a quadratic function of the temperature T and expressed as R = αT 2 + βT + γ (5). The coefficients α, β and γ of each term are used as correction data. As shown in FIG. 11, the heat of fusion is measured using, for example, a high-purity metal as a sample of which the amount of heat absorption or the amount of heat generation is known, and the correction coefficients α, β, γ are obtained from the data curve, and the correction data are obtained. It is stored in the correction coefficient storage means 14.
【００１２】次に、吸熱量や発熱量が未知の試料を測定
するときは、図１２に示されるように、得られたデータ
曲線についてデータ曲線補正手段１６で補正データを用
いて各温度でのデータの補正が行なわれ、補正後のデー
タ曲線がＣＲＴ上などに表示される。その補正されたデ
ータ曲線のピーク面積が面積算出手段１８で算出され
る。そのピーク面積は吸熱量や発熱量に対応した値とな
る。Next, when measuring a sample of which the amount of heat absorption or the amount of heat generation is unknown, as shown in FIG. 12, the obtained data curve is corrected by the data curve correction means 16 at each temperature using the correction data. The data is corrected, and the corrected data curve is displayed on the CRT or the like. The area calculating means 18 calculates the peak area of the corrected data curve. The peak area has a value corresponding to the amount of heat absorption and the amount of heat generation.
【００１３】[0013]
【実施例】図１３は熱機械分析装置、示差熱分析装置又
は示差走査熱量計などの熱分析装置のデータ処理装置を
概略的に表わしたものである。ＣＰＵ２０のバス２２に
は、測定装置からの温度データをデジタル信号に変換し
て取り込むＡ／Ｄコンバータ２４、測定装置の膨張量や
試料と基準物質との温度差、又は試料側と基準側への通
電量の差などをデータとして取り込み、デジタル信号に
変換するＡ／Ｄコンバータ２６、取り込まれた温度やデ
ータを記憶するハードディスク装置２８、ＣＰＵ２０の
処理プログラムなどを記憶しているＲＯＭなどのメモリ
装置３０、分析結果などを表示するＣＲＴ３２、及び操
作や条件を入力するキーボード３４などが接続されてい
る。ＣＰＵ２０は測定に必要な処理を制御するととも
に、得られたデータの計算などの処理を行なう。EXAMPLE FIG. 13 schematically shows a data processing device of a thermal analysis device such as a thermomechanical analysis device, a differential thermal analysis device or a differential scanning calorimeter. The bus 22 of the CPU 20 converts the temperature data from the measuring device into a digital signal and takes in the A / D converter 24, the expansion amount of the measuring device, the temperature difference between the sample and the reference substance, or the sample side and the reference side. An A / D converter 26 that takes in a difference in the amount of energization as data and converts it into a digital signal, a hard disk device 28 that stores the taken temperature and data, a memory device 30 such as a ROM that stores processing programs of the CPU 20, and the like. A CRT 32 for displaying analysis results and the like, and a keyboard 34 for inputting operations and conditions are connected. The CPU 20 controls the processing required for measurement and also performs processing such as calculation of the obtained data.
【００１４】ＣＰＵ２０からの制御に従って所定の温度
プログラムに従って加温し又は降温する。Ａ／Ｄコンバ
ータ２４，２６からはそれぞれ温度と測定データが時間
データとともにハードディスク装置２８に格納されてい
く。格納されたデータはＣＰＵ２０によって補正量が加
算されたり、補正係数がかけられたりして、各温度ごと
に補正されたデータがＣＲＴ３２上に表示される。ＣＲ
Ｔ３２上に表示されたデータがＣＰＵ２０によって解析
され、膨張量が算出されたり、面積計算から発熱量や吸
熱量が計算されてＣＲＴ３２上に表示される。Under the control of the CPU 20, the temperature is raised or lowered according to a predetermined temperature program. From the A / D converters 24 and 26, temperature and measurement data are respectively stored in the hard disk device 28 together with time data. A correction amount is added to the stored data by the CPU 20, and a correction coefficient is applied to the stored data, so that the data corrected for each temperature is displayed on the CRT 32. CR
The data displayed on T32 is analyzed by the CPU 20, the expansion amount is calculated, and the heat generation amount and the heat absorption amount are calculated from the area calculation and displayed on the CRT 32.
【００１５】[0015]
【発明の効果】本発明による熱分析装置では、熱機械分
析装置の全膨張測定において、測定系の伸びが補正デー
タとして記憶されており、正確に試料の伸びを補正する
ことができる。また測定系の伸びを示す補正データは測
定された温度域にわたって連続的であるため、補正点を
何点も設定するわずらわしさがない。本発明を示差熱分
析装置又は示差走査熱量計に適用すれば、データ曲線自
身に補正係数をかけてより正確なデータ曲線を得ること
ができるため、従来のように補正を行なうピークトップ
の温度と面積の重心がずれて正しく補正ができなくなる
というような問題はなく、常に正しい熱量を求めること
ができるようになり、熱量解析に対する定量性が増す。In the thermal analyzer according to the present invention, the elongation of the measurement system is stored as correction data in the total expansion measurement of the thermomechanical analyzer, and the elongation of the sample can be accurately corrected. Further, since the correction data indicating the elongation of the measurement system is continuous over the measured temperature range, there is no need to set any correction points. If the present invention is applied to a differential thermal analyzer or a differential scanning calorimeter, a more accurate data curve can be obtained by multiplying the data curve itself by a correction coefficient, and therefore, the temperature at the peak top to be corrected as in the conventional case There is no problem that the center of gravity of the area shifts and correct correction cannot be performed, and the correct calorific value can always be obtained, and the quantitativeness for calorific value analysis increases.
【図１】熱機械分析装置の測定部分を概略的に示す正面
図である。FIG. 1 is a front view schematically showing a measurement part of a thermomechanical analyzer.
【図２】従来の熱機械分析における補正方法を示す図で
ある。FIG. 2 is a diagram showing a correction method in a conventional thermomechanical analysis.
【図３】従来の示差熱分析におけるピーク面積の補正方
法を示す図である。FIG. 3 is a diagram showing a method of correcting a peak area in a conventional differential thermal analysis.
【図４】本発明の熱機械分析装置のデータ処理装置を示
すブロック図である。FIG. 4 is a block diagram showing a data processing device of the thermomechanical analyzer of the present invention.
【図５】本発明の示差熱分析装置又は示差走査熱量計に
おけるデータ処理装置を示すブロック図である。FIG. 5 is a block diagram showing a data processing device in the differential thermal analyzer or the differential scanning calorimeter of the present invention.
【図６】本発明を熱機械分析に適用した場合の真の値と
測定値の関係を示す図である。FIG. 6 is a diagram showing a relationship between a true value and a measured value when the present invention is applied to thermomechanical analysis.
【図７】本発明の熱機械分析における補正方法を示す図
である。FIG. 7 is a diagram showing a correction method in thermomechanical analysis of the present invention.
【図８】本発明の熱機械分析における補正データ作成の
フローチャート図である。FIG. 8 is a flow chart of correction data creation in thermomechanical analysis of the present invention.
【図９】本発明の熱機械分析での試料測定時の補正方法
を示すフローチャート図である。FIG. 9 is a flow chart diagram showing a correction method at the time of sample measurement in thermomechanical analysis of the present invention.
【図１０】本発明を示差熱分析装置又は示差走査熱量計
に適用する場合の補正を示す図である。FIG. 10 is a diagram showing correction when the present invention is applied to a differential thermal analyzer or a differential scanning calorimeter.
【図１１】本発明の示差熱分析装置又は示差走査熱量計
における補正データの作成方法を示すフローチャート図
である。FIG. 11 is a flowchart showing a method of creating correction data in the differential thermal analyzer or the differential scanning calorimeter of the present invention.
【図１２】本発明の示差熱分析装置又は示差走査熱量計
における補正方法を示すフローチャート図である。FIG. 12 is a flow chart showing a correction method in the differential thermal analyzer or the differential scanning calorimeter of the present invention.
【図１３】一実施例のデータ処理装置を示すブロック図
である。FIG. 13 is a block diagram showing a data processing device of an embodiment.
２ 支持管 ４ 試料 ６ 検出棒 １０ 全膨張測定補正データ記憶手段 １２ データ補正手段 １４ 補正係数記憶手段 １６ データ曲線補正手段 １８ 面積算出手段 ２０ ＣＰＵ ２８ ハードディスク装置 ３０ メモリ装置 2 Support tube 4 Sample 6 Detection rod 10 Total expansion measurement correction data storage means 12 Data correction means 14 Correction coefficient storage means 16 Data curve correction means 18 Area calculation means 20 CPU 28 Hard disk device 30 Memory device
Claims (2)
に検出棒の先端を接触させ、試料の温度を変化させて検
出棒により試料の膨張量を測定する熱機械分析装置にお
いて、そのデータ処理装置に、熱膨張量が既知の試料を
測定したときの既知量と実測値との差から求められた各
温度における補正値を記憶する全膨張測定補正データ記
憶手段と、熱膨張量未知の試料を測定したときの各温度
の測定データを前記補正値により補正するデータ補正手
段と、を備えたことを特徴とする熱分析装置。1. A thermomechanical analyzer in which a sample is placed on the bottom surface of a support tube, the tip of a detection rod is brought into contact with the upper surface of the sample, and the temperature of the sample is changed to measure the expansion amount of the sample with the detection rod. In the data processing device, a total expansion measurement correction data storage means for storing a correction value at each temperature obtained from a difference between a known amount and a measured value when a sample having a known thermal expansion amount is measured; And a data correction unit that corrects the measurement data at each temperature when the sample is measured with the correction value.
または発熱量の差に基づいてデータ曲線を得、そのピー
ク面積から吸熱量又は発熱量を求める示差熱分析装置又
は示差走査熱量計において、そのデータ処理装置に、吸
熱量又は発熱量が既知の試料を測定したときの既知量と
実測値との熱量の差から求められたデータ曲線の補正係
数を記憶する補正係数記憶手段と、吸熱量又は発熱量が
未知の試料を測定したときのデータ曲線を前記記憶手段
の補正係数を用いて各温度ごとに補正するデータ曲線補
正手段と、その補正されたデータ曲線のピーク面積から
吸熱量又は発熱量を算出する面積算出手段と、を備えた
ことを特徴とする熱分析装置。2. A differential thermal analyzer or a differential scanning calorimeter, in which a sample and a reference substance are heated, a data curve is obtained based on the difference in the amount of heat absorption or the amount of heat generation between them, and the amount of heat absorption or heat generation is determined from the peak area. In the data processing device, a correction coefficient storage means for storing the correction coefficient of the data curve obtained from the difference in heat quantity between the known amount and the measured value when the sample of which the amount of heat absorption or the amount of heat generation is known is measured, Endothermic amount from the data curve correction means for correcting the data curve at the time of measuring the sample of which the endothermic amount or the calorific value is unknown using the correction coefficient of the storage means, and the peak area of the corrected data curve Alternatively, an area calculating unit that calculates a calorific value is provided, and the thermal analysis device.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP36001992A JP3178133B2 (en) | 1992-12-30 | 1992-12-30 | Thermal analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP36001992A JP3178133B2 (en) | 1992-12-30 | 1992-12-30 | Thermal analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06201621A true JPH06201621A (en) | 1994-07-22 |
| JP3178133B2 JP3178133B2 (en) | 2001-06-18 |
Family
ID=18467480
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP36001992A Expired - Fee Related JP3178133B2 (en) | 1992-12-30 | 1992-12-30 | Thermal analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3178133B2 (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08240547A (en) * | 1995-03-03 | 1996-09-17 | Rigaku Corp | Method for measuring sample length and thermal expansion in thermomechanical analyzer |
| JP2011209047A (en) * | 2010-03-29 | 2011-10-20 | Yamatake Corp | System and method for creating heat value calculation formula, and system and method for measuring heat value |
| JP2016095196A (en) * | 2014-11-13 | 2016-05-26 | サムソン エレクトロ−メカニックス カンパニーリミテッド． | Thermal expansion coefficient measurement method and thermomechanical analysis apparatus |
| JP2017021016A (en) * | 2015-07-03 | 2017-01-26 | ネッチ ゲレーテバウ ゲーエムベーハー | Method and apparatus for thermomechanical analysis of samples |
| CN110443006A (en) * | 2019-08-29 | 2019-11-12 | 江西理工大学 | A method for calculating the volume ratio of two-phase transition of metallic materials by measuring the area |
| CN118883301A (en) * | 2024-08-28 | 2024-11-01 | 上海大学 | A method for characterizing non-isothermal creep of thin film samples using a dynamic mechanical analyzer |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102069624B1 (en) * | 2013-05-24 | 2020-01-23 | 삼성전기주식회사 | Method for measuring coefficient of thermal expansion and Thermal Mechanical Analyzer |
-
1992
- 1992-12-30 JP JP36001992A patent/JP3178133B2/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08240547A (en) * | 1995-03-03 | 1996-09-17 | Rigaku Corp | Method for measuring sample length and thermal expansion in thermomechanical analyzer |
| JP2011209047A (en) * | 2010-03-29 | 2011-10-20 | Yamatake Corp | System and method for creating heat value calculation formula, and system and method for measuring heat value |
| JP2016095196A (en) * | 2014-11-13 | 2016-05-26 | サムソン エレクトロ−メカニックス カンパニーリミテッド． | Thermal expansion coefficient measurement method and thermomechanical analysis apparatus |
| JP2017021016A (en) * | 2015-07-03 | 2017-01-26 | ネッチ ゲレーテバウ ゲーエムベーハー | Method and apparatus for thermomechanical analysis of samples |
| CN110443006A (en) * | 2019-08-29 | 2019-11-12 | 江西理工大学 | A method for calculating the volume ratio of two-phase transition of metallic materials by measuring the area |
| CN110443006B (en) * | 2019-08-29 | 2022-11-29 | 江西理工大学 | Method for calculating two-phase transformation volume ratio of metal material by measuring area |
| CN118883301A (en) * | 2024-08-28 | 2024-11-01 | 上海大学 | A method for characterizing non-isothermal creep of thin film samples using a dynamic mechanical analyzer |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3178133B2 (en) | 2001-06-18 |
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