JP2581669B2 - Thermal analyzer - Google Patents
Thermal analyzerInfo
- Publication number
- JP2581669B2 JP2581669B2 JP60291004A JP29100485A JP2581669B2 JP 2581669 B2 JP2581669 B2 JP 2581669B2 JP 60291004 A JP60291004 A JP 60291004A JP 29100485 A JP29100485 A JP 29100485A JP 2581669 B2 JP2581669 B2 JP 2581669B2
- Authority
- JP
- Japan
- Prior art keywords
- voltage
- temperature
- sample
- thermocouple
- linear function
- 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.)
- Expired - Lifetime
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- Indication And Recording Devices For Special Purposes And Tariff Metering Devices (AREA)
- Measuring Instrument Details And Bridges, And Automatic Balancing Devices (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、検出手段の検出感度の温度依存性を出力側
にて補正する装置を具備した熱分析装置に関する。Description: TECHNICAL FIELD The present invention relates to a thermal analyzer provided with a device for correcting the temperature dependency of the detection sensitivity of a detection means on the output side.
（従来の技術） 例えば高分子物質の状態変化の解析には、試料を挿入
した試料容器と基準物質を挿入した標準容器を加熱炉内
に配設した伝熱板上に載置し、これを一定の上昇速度で
加熱し、その過程において発生する試料の吸、発熱現象
による熱エネルギーの授受を電熱板を介して行ないなが
ら、検出手段を構成する２個の熱電対から検出した示差
熱量を測定する熱流束型示差熱量測定装置が多用されて
いる。(Prior art) For example, to analyze a change in state of a polymer substance, a sample container in which a sample is inserted and a standard container in which a reference material is inserted are placed on a heat transfer plate arranged in a heating furnace, and the sample container is placed on the sample container. Heating at a constant rising rate, measuring the differential calorific value detected from the two thermocouples that constitute the detecting means, while absorbing and exchanging heat energy due to the heat generation phenomenon of the sample generated in the process. A heat flux type differential calorimeter is frequently used.
（発明が解決しようとする問題点） この種の装置において、検出手段を構成する２個の熱
電対による熱量検出感度は、熱エネルギーの授受を行な
う伝熱板の熱伝導率が温度上昇に伴なって変動するとと
もに、周囲温度に対応した輻射、対流等の熱伝達の影響
を受け、加熱温度の上昇に応じて低下する特性を示して
いる。このため、試料の吸・発熱を示すピーク波形の面
積が加熱温度の上昇に伴って減少してしまう。そこで、
加熱炉の上、下面を光沢を有する均熱ブロックにより覆
って検出手段からの熱の逃げを防止する対策が採られて
いるが、加熱炉の加熱温度を一定速度で上昇させながら
測定を行なう以上、周囲温度の変化から無関係とはなり
えず、出力ピーク波形の面積が温度に依存して変動する
という問題は依然として抱えている。(Problems to be Solved by the Invention) In this type of apparatus, the sensitivity of the calorific value detection by the two thermocouples constituting the detecting means is determined by the fact that the thermal conductivity of the heat transfer plate for transmitting and receiving thermal energy increases with the temperature rise. In addition, it shows a characteristic that it is affected by heat transfer such as radiation and convection corresponding to the ambient temperature, and is reduced as the heating temperature rises. For this reason, the area of the peak waveform indicating absorption / heating of the sample decreases with an increase in the heating temperature. Therefore,
Measures are taken to prevent the heat from escaping from the detecting means by covering the upper and lower surfaces of the heating furnace with a glossy heat equalizing block, but measurement must be performed while increasing the heating temperature of the heating furnace at a constant speed. However, there is still a problem that the area of the output peak waveform fluctuates depending on the temperature because the area cannot be irrelevant to the change in the ambient temperature.
本発明の目的とするところは、上記問題に鑑み、検出
手段の検出感度が折線開放電圧発生手段及び乗算手段と
用いて周囲温度の変動による影響を受けないように補正
を行なう改良された熱分析装置を提供することにある。SUMMARY OF THE INVENTION In view of the above problems, an object of the present invention is to provide an improved thermal analysis that performs correction so that the detection sensitivity of a detection unit is not affected by fluctuations in ambient temperature by using a broken line open voltage generation unit and a multiplication unit. It is to provide a device.
（問題点を解決するための手段） すなわち、本発明の目的とするところは、加熱温度が
変化する加熱炉と、該加熱炉に収容された基準物質と試
料との温度を検出する第１、第２の熱電対と、前記第
１、第２の熱電対からの信号の差分を検出する温度差検
出手段と、前記熱電対の一方の出力を受けて前記熱電対
の温度−出力電圧特性を補正する電圧を出力する折線関
数電圧発生手段と、前記温度差検出手段と前記折線関数
電圧発生手段との出力の積を出力する乗算手段とを備え
た点にある。(Means for Solving the Problems) That is, an object of the present invention is to provide a heating furnace in which the heating temperature changes, and a first method for detecting the temperatures of a reference substance and a sample contained in the heating furnace. A second thermocouple, temperature difference detection means for detecting a difference between signals from the first and second thermocouples, and receiving one output of the thermocouple to obtain a temperature-output voltage characteristic of the thermocouple. The present invention is characterized in that a linear function voltage generating means for outputting a voltage to be corrected and a multiplying means for outputting a product of outputs of the temperature difference detecting means and the linear function voltage generating means are provided.
（作用） 加熱炉の加熱温度の増加に伴って熱量の検出感度が低
下する検出手段からの基準物質と試料の温度差電圧を乗
算手段に入力するとともに、検出手段からの試料温度電
圧の上昇に応じて電圧増加率の変化する非線形電圧を補
正電圧として乗算手段に入力し、補正電圧を基準物質と
試料の温度差電圧に乗算することによって基準物質と試
料の温度差電圧のピーク面積の減少を補正する。(Operation) The temperature difference voltage between the reference substance and the sample from the detection means whose sensitivity decreases with the increase in the heating temperature of the heating furnace is input to the multiplication means and the sample temperature voltage from the detection means is increased. The nonlinear voltage of which the voltage increase rate changes accordingly is input to the multiplying means as a correction voltage, and the correction voltage is multiplied by the temperature difference voltage between the reference material and the sample to reduce the peak area of the temperature difference voltage between the reference material and the sample. to correct.
（実施例） 以下に本発明の詳細を図に図に示す実施例に基づいて
説明する。(Example) Hereinafter, the details of the present invention will be described based on an example shown in the drawings.
図はいずれも本発明の一実施例装置を示し、図中符号
１は試料を挿入した試料容器３と基準物質を挿入した標
準容器４を支持するとともに、試料温度及び基準物質温
度を検出して試料温度と基準物質及び試料の温度差とを
各別に出力する熱電対５、５′を配設し、銅等により構
成された伝熱板２を具備する加熱炉であって、その熱電
対５、５′の熱量検出感度は第２図（Ａ）の特性曲線ａ
で示すように加熱温度の上昇に伴って低下する特性を備
えている。なお第２図（Ａ）で実線で示す試料の吸、発
熱等における基準物質と試料の温度差電圧のピーク波形
Ｃは熱量検出感度の影響を受けてピーク面積が低下した
補正前の波形を示し点線で示すものは補正後のピーク波
形を示している。また、試料温度と基準物質との温度差
を検出する示差熱電対となる熱電対5,5′と、熱電対5,
5′で検出した示差熱信号（温度差電圧）を増幅する増
幅器６とから温度差検出手段を構成している。また７
は、試料温度を検出する熱電対５′の信号（試料温度電
圧）を増幅する増幅器であって、増幅器６は乗算手段で
ある乗算器12の端子Ｘに接続され、一方増幅器７は折線
関数電圧発生手段である折線関数電圧発生器８乃至10と
接続されている。折線関数電圧発生器８乃至10は、抵抗
R1乃至R3、R4乃至R6、R7乃至R9の各直列回路が並列接続
されるとともに、その帰還ループと出力側にそれぞれダ
イオードＤ、Ｄを接続し、非反転入力を接地し反転入力
端子を備えるオペアンプOP1、OP2、OP3が各抵抗R2、R5
及びR8に並設され、さらに両端に＋15V、−15Vの電圧を
印加された４個の直列抵抗回路から大きさの異なるバイ
アス電圧をオペアンプOP1乃至OP3の反転入力端子に分岐
し印加するように構成されている。折線関数電圧発生器
８乃至10増幅器７の出力電圧の増大に伴って、まず上記
した各直列回路を並列接続した抵抗回路に流れ、次いで
オペアンプOP1、OP2、OP3に接続したダイオードＤ、Ｄ
を順次導通させ、第２図（Ｂ）に示すように対数圧縮さ
れた折線関数電圧曲線ｂを出力し、増幅器11を介して乗
算器12の端子Ｙに入力し、その乗算電圧は端子Ｚを介し
て図示しないデータ処理装置に送出される。なお、これ
ら電圧発生器８乃至10は基準物質と試料の温度差による
熱量の検出感度特性を補正しうる傾斜特性を持つ非線形
電圧を出力するように構成されている。The figures each show an apparatus according to an embodiment of the present invention, wherein reference numeral 1 denotes a sample container 3 in which a sample is inserted and a standard container 4 in which a reference material is inserted, and the sample temperature and the reference material temperature are detected. A heating furnace is provided with thermocouples 5 and 5 'for separately outputting the sample temperature and the temperature difference between the reference material and the sample, and is provided with a heat transfer plate 2 made of copper or the like. , 5 'is shown by the characteristic curve a in FIG.
As shown by the symbol, the characteristic is reduced as the heating temperature increases. Note that the peak waveform C of the temperature difference voltage between the reference substance and the sample due to absorption and heat generation of the sample, which is indicated by a solid line in FIG. The dotted line shows the peak waveform after the correction. Further, thermocouples 5, 5 'which are differential thermocouples for detecting a temperature difference between the sample temperature and the reference material, and thermocouples 5, 5'
The temperature difference detecting means is constituted by the amplifier 6 for amplifying the differential heat signal (temperature difference voltage) detected at 5 '. 7
Is an amplifier for amplifying the signal (sample temperature voltage) of the thermocouple 5 'for detecting the sample temperature. The amplifier 6 is connected to the terminal X of the multiplier 12 as a multiplication means, while the amplifier 7 is connected to the linear function voltage. It is connected to the linear function voltage generators 8 to 10 as generating means. The linear function voltage generators 8 to 10 are resistors
Each series circuit of R 1 to R 3 , R 4 to R 6 , R 7 to R 9 is connected in parallel, diodes D and D are respectively connected to the feedback loop and the output side, and the non-inverting input is grounded. Operational amplifiers OP 1 , OP 2 , and OP 3 with inverting input terminals are connected to resistors R 2 , R 5
And they are arranged in parallel in R 8, further + 15V across branches by applying a voltage different bias voltages of four series-connected resistor circuit sizes applied to a -15V to the inverting input terminal of the operational amplifier OP 1 to OP 3 It is configured as follows. As the output voltages of the linear function voltage generators 8 to 10 increase, the current flows first through the resistor circuit in which the series circuits described above are connected in parallel, and then the diodes D connected to the operational amplifiers OP 1 , OP 2 and OP 3 , D
Are successively conducted, and a logarithmic-compressed linear function voltage curve b is output as shown in FIG. 2 (B) and input to the terminal Y of the multiplier 12 via the amplifier 11, and the multiplied voltage is applied to the terminal Z. The data is sent to a data processing device (not shown) through the data processor. Each of the voltage generators 8 to 10 is configured to output a non-linear voltage having a slope characteristic capable of correcting the detection sensitivity characteristic of the amount of heat due to the temperature difference between the reference substance and the sample.
このように構成した装置において、加熱炉１の加熱温
度を上昇させて行くと、これに応じて熱電対５、５′に
より検出された第２図（Ａ）で実線で示すピーク面積の
減少したピーク波形Ｃの示差熱温度電圧が増幅器６を介
して乗算器12の端子Ｘに入力される。一方、熱電対５′
から検出した増加する試料温度電圧を増幅器７を介して
折線関数電圧発生器８乃至10に入力する。これにより第
２図（Ｂ）の折線関数電圧曲線ｂで示すように、増幅器
７の出力電圧がV1に至る迄、抵抗R1乃至R3、R4乃至R6、
R7乃至R9の並列回路に電流が分流して線形電圧が出力さ
れ、その電圧がV1からV2の間はオペアンプOP1のダイオ
ードＤ、Ｄが導通して抵抗R2と並列回路を形成し、この
ため合成抵抗が減少し、電圧増加率の低下した電圧を出
力する。次いで電圧V2からV3の間はオペアンプOP2のダ
イオードＤ、Ｄが導通して抵抗R5と並列回路を形成し、
合成抵抗の一層の減少によりさらに電圧増加率の低下し
た電圧を出力し、最後に電圧V3からV4の間はオペアンプ
OP3のダイオードＤ、Ｄが導通して抵抗R8と並列回路を
形成し、電圧増加率の減少した電圧を出力する。折線関
数電圧発生器８乃至10の対数圧縮電圧は補正電圧として
増幅器11を介して乗算器12の端子Ｙに入力される。折線
関数電圧発生器８乃至10から出力された補正電圧は試料
温度電圧の上昇に伴って増加する電圧であるから、乗算
器12においては、示差熱温度である実線で示す振幅低下
しているピーク波形Ｃが入力される度毎に、そのピーク
波形Ｃの振幅値にこの時における補正電圧値が係数とし
て乗算され、これによりピーク波形Ｃの振幅低下は点線
で示すように増大補正され、端子Ｚを介して出力され
る。また、和若しくは差演算によって感度補正するので
はなく、補正係数の乗算によって検出感度補正するの
で、発熱反応か吸熱反応かによる演算の区別、すなわ
ち、和若しくは差演算の選択の必要がなく、補正演算に
おける１つのプロセスを省くこともできる。In the apparatus configured as described above, as the heating temperature of the heating furnace 1 was increased, the peak area indicated by the solid line in FIG. 2 (A) detected by the thermocouples 5, 5 'was correspondingly reduced. The differential thermal temperature voltage of the peak waveform C is input to the terminal X of the multiplier 12 via the amplifier 6. On the other hand, thermocouple 5 '
Are input to the linear function voltage generators 8 to 10 via the amplifier 7. Accordingly, as shown by the polygonal line function voltage curve b of FIG. 2 (B), until the output voltage of the amplifier 7 reaches V 1, resistors R 1 through R 3, R 4 to R 6,
Linear voltage is outputted by a current shunted to the parallel circuit of R 7 to R 9, a parallel circuit the voltage is from V 1 diode D between the operational amplifier OP 1 of V 2, and a resistor R 2 conducts D is Therefore, the combined resistance is reduced, and a voltage having a reduced voltage increase rate is output. Then between the voltage V 2 of V 3 forms the diode D of the operational amplifier OP 2, a resistor R 5 conducts D is a parallel circuit,
Further outputs the reduced voltage of the voltage increase rate by further reducing the combined resistance, finally between the voltage V 3 of V 4 is an operational amplifier
Diode D of OP 3, D forms a parallel circuit with the resistor R 8 conducting, and outputs the reduced voltage of the voltage increase rate. The logarithmic compression voltages of the linear function voltage generators 8 to 10 are input to the terminal Y of the multiplier 12 via the amplifier 11 as correction voltages. The correction voltage output from the linear function voltage generators 8 to 10 is a voltage that increases as the sample temperature voltage rises. Each time the waveform C is input, the amplitude value of the peak waveform C is multiplied by the correction voltage value at this time as a coefficient, whereby the decrease in the amplitude of the peak waveform C is corrected to increase as shown by the dotted line, and the terminal Z Is output via. Further, since the detection sensitivity is corrected by multiplying the correction coefficient instead of performing the sensitivity correction by the sum or difference calculation, there is no need to distinguish between the calculation based on the exothermic reaction and the endothermic reaction, that is, there is no need to select the sum or difference calculation. One process in the operation can be omitted.
なお、本実施例において検出部の検出感度補正装置を
示差走査熱量測定装置に適用した場合について説明した
が、この補正装置は示差熱分析装置にも適用可能であ
り、また折線関数電圧発生装置の個数は折線電圧の所望
の傾斜度合の精、粗に応じて適宜増減すればよい。ま
た、本実施例においては折線関数発生回路は試料温度の
上昇に伴い出力電圧の増加率が減少する回路となってい
るが、ダイオードの向きを変えることにより、途中で出
力電圧の増加率の増す回路を組むこともできる。In the present embodiment, the case where the detection sensitivity correction device of the detection unit is applied to a differential scanning calorimeter is described, but this correction device can also be applied to a differential thermal analyzer, and also a linear function voltage generator. The number may be appropriately increased or decreased according to the precision or coarseness of the desired inclination of the linear voltage. In the present embodiment, the linear function generating circuit is a circuit in which the output voltage increase rate decreases as the sample temperature rises. However, by changing the direction of the diode, the output voltage increase rate increases on the way. Circuits can also be built.
（発明の効果） 以上、説明したように本発明においては加熱温度が変
化する加熱炉と、可燃炉に収容された基準物質と試料と
の温度を検出する第１、第２の熱電対と、第1,第２の熱
電対からの信号の差分を検出する温度差検出手段と、熱
電対の一方の出力を受け、熱電対の温度−出力電圧特性
を補正する電圧を出力する折線関数電圧発生手段と、温
度差検出手段と折線関数電圧発生手段との出力の積を出
力する乗算手段とを備えるようにしたので、熱電対から
の信号に比較して極めて小さな示差熱信号を、そのレベ
ルの低下を招くことなく、温度依存性を補正することが
できる。また、和若しくは差演算によって感度補正する
のではなく、補正係数の乗算によって検出感度補正する
ので、発熱反応が吸熱反応かによる演算の区別、すなわ
ち、和若しくは差演算の選択の必要がなく、補正演算に
おける１つのプロセスを省くこともできる。(Effects of the Invention) As described above, in the present invention, the heating furnace whose heating temperature changes, the first and second thermocouples for detecting the temperatures of the reference substance and the sample housed in the combustible furnace, Temperature difference detecting means for detecting a difference between signals from the first and second thermocouples, and a linear function voltage generator for receiving one output of the thermocouple and outputting a voltage for correcting a temperature-output voltage characteristic of the thermocouple. Means, and a multiplying means for outputting the product of the outputs of the temperature difference detecting means and the linear function voltage generating means, so that a differential heat signal that is extremely small compared to the signal from the thermocouple is output at that level. The temperature dependency can be corrected without lowering. In addition, since the sensitivity is not corrected by the sum or difference calculation, but the detection sensitivity is corrected by multiplication of the correction coefficient, the calculation based on whether the exothermic reaction is an endothermic reaction, that is, there is no need to select the sum or difference calculation, and the correction is performed. One process in the operation can be omitted.
第１図は本発明の一実施例装置を示す構成図、第２図
（Ａ）は熱電対の熱量検出感度特性曲線と吸、発熱ピー
ク波形とを、同図（Ｂ）は折線関数電圧発生器の出力電
圧波形を示す図である。 １……加熱炉、５、５′……熱電対 ８、９、10……折線関数電圧発生器、 12……乗算器FIG. 1 is a block diagram showing an apparatus according to an embodiment of the present invention, FIG. 2 (A) is a diagram showing a calorimetric detection sensitivity characteristic curve of a thermocouple and absorption and heat generation peak waveforms, and FIG. FIG. 6 is a diagram showing an output voltage waveform of the container. 1 ... heating furnace, 5 5 '... thermocouple 8, 9, 10 ... linear function voltage generator, 12 ... multiplier
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｇ０６Ｇ 7/28 Ｇ０１Ｒ 15/10 Ｇ (56)参考文献 特開 昭58−21150（ＪＰ，Ａ) 特開 昭56−74717（ＪＰ，Ａ) 特開 昭57−91426（ＪＰ，Ａ) 特開 昭60−129630（ＪＰ，Ａ) 実開 昭57−199812（ＪＰ，Ｕ) 実開 昭59−155651（ＪＰ，Ｕ) 実開 昭56−25934（ＪＰ，Ｕ) 特公 昭60−4404（ＪＰ，Ｂ２) 特公 昭37−4298（ＪＰ，Ｂ１)──────────────────────────────────────────────────の Continuation of the front page (51) Int.Cl. 6 Identification code Agency reference number FI Technical indication location G06G 7/28 G01R 15/10 G (56) References JP-A-58-21150 (JP, A) JP-A-56-74717 (JP, A) JP-A-57-91426 (JP, A) JP-A-60-129630 (JP, A) Japanese Utility Model Application No. Sho 57-199812 (JP, U) Japanese Utility Model Application No. Sho 59-155551 (JP, U) JP-A 56-25934 (JP, U) JP-B 60-4404 (JP, B2) JP-B 37-4298 (JP, B1)
Claims (1)
収容された基準物質と試料との温度を検出する第１、第
２の熱電対と、前記第１、第２の熱電対からの信号の差
分を検出する温度差検出手段と、前記熱電対の一方の出
力を受けて前記熱電対の温度−出力電圧特性を補正する
電圧を出力する折線関数電圧発生手段と、前記温度差検
出手段と前記折線関数電圧発生手段との出力の積を出力
する乗算手段とからなる熱分析装置。1. A heating furnace whose heating temperature changes, first and second thermocouples for detecting the temperature of a reference substance and a sample housed in the heating furnace, and the first and second thermocouples A temperature difference detecting means for detecting a difference between signals from the thermocouple; a linear function voltage generating means for receiving one output of the thermocouple and outputting a voltage for correcting a temperature-output voltage characteristic of the thermocouple; A thermal analyzer, comprising: a detecting means and a multiplying means for outputting a product of outputs of the linear function voltage generating means.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60291004A JP2581669B2 (en) | 1985-12-23 | 1985-12-23 | Thermal analyzer |
| CN 86108245 CN1012845B (en) | 1985-12-23 | 1986-12-22 | Thermal analysing arrangements |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60291004A JP2581669B2 (en) | 1985-12-23 | 1985-12-23 | Thermal analyzer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62167454A JPS62167454A (en) | 1987-07-23 |
| JP2581669B2 true JP2581669B2 (en) | 1997-02-12 |
Family
ID=17763212
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60291004A Expired - Lifetime JP2581669B2 (en) | 1985-12-23 | 1985-12-23 | Thermal analyzer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2581669B2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5674717A (en) * | 1979-11-21 | 1981-06-20 | Shimadzu Corp | Temperature controller of thermal analysis apparatus |
-
1985
- 1985-12-23 JP JP60291004A patent/JP2581669B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62167454A (en) | 1987-07-23 |
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