JP2760104B2 - Thermogravimetric analysis of solid samples - Google Patents
Thermogravimetric analysis of solid samplesInfo
- Publication number
- JP2760104B2 JP2760104B2 JP31396989A JP31396989A JP2760104B2 JP 2760104 B2 JP2760104 B2 JP 2760104B2 JP 31396989 A JP31396989 A JP 31396989A JP 31396989 A JP31396989 A JP 31396989A JP 2760104 B2 JP2760104 B2 JP 2760104B2
- Authority
- JP
- Japan
- Prior art keywords
- weight change
- solid sample
- change curve
- weight
- sample
- 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 - Fee Related
Links
Landscapes
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Description
【発明の詳細な説明】 （イ）産業上の利用分野 この発明は固体試料の熱重量分析法に関する。さらに
詳しくは、固体試料の物性や構造解析等に好適な固体試
料の熱重量分析法に関する。The present invention relates to a thermogravimetric analysis method for a solid sample. More specifically, the present invention relates to a thermogravimetric analysis method for a solid sample which is suitable for analyzing the physical properties and structure of the solid sample.
（ロ）従来の技術 固体試料の物性や構造解析等には、熱重量法（TG）が
利用されている。このTGは、固体試料を一定速度で加熱
しながらその重量変化を連続的に測定する方法で、得ら
れる重量変化曲線から、例えば試料の熱分解反応の過
程、結晶水・脱水量の測定、沸点の決定、熱分解や、蒸
発、昇華を利用した固体混合物の分析等、種々の情報を
得ることができる。(B) Conventional technology The thermogravimetric method (TG) is used to analyze the physical properties and structure of solid samples. This TG is a method of continuously measuring the weight change of a solid sample while heating it at a constant rate.From the obtained weight change curve, for example, the process of thermal decomposition reaction of the sample, measurement of crystallization water / dehydration amount, boiling point And various kinds of information, such as the determination of a solid mixture using pyrolysis, evaporation, and sublimation, can be obtained.
上記TGにおいては、試料を加熱炉で加熱する際、該炉
内で生ずるガス対流及び浮力によって試料容器に力が作
用し、これによって得られる重量変化曲線にはベースラ
イン変動が生ずることとなる。従来このベースライン変
動の補正には、同一の空の試料容器を試料測定時と同条
件で加熱し、このとき得られる測定データをブランクデ
ータとして用いていた。In the TG described above, when a sample is heated in a heating furnace, a force acts on the sample container due to gas convection and buoyancy generated in the furnace, so that a weight change curve obtained therefrom causes a baseline variation. Conventionally, to correct this baseline variation, the same empty sample container was heated under the same conditions as when the sample was measured, and the measurement data obtained at this time was used as blank data.
（ハ）発明が解決しようとする課題 上記ベースライン変動の大きさは、試料容器及び試料
の体積及び重量に依存するものである。しかしながら、
上記方法で得られるブランクデータは、試料容器に関す
る補正だけしか考慮されないものである。(C) Problems to be Solved by the Invention The magnitude of the above-mentioned baseline fluctuation depends on the volume and weight of the sample container and the sample. However,
The blank data obtained by the above method takes into account only the correction for the sample container.
この発明はかかる状況に鑑み為されたものであり、ベ
ースライン変動が最大限補正された重量変化曲線に基づ
いて分析しうる固体試料の熱重量分析法を提供しようと
するものである。The present invention has been made in view of such circumstances, and an object of the present invention is to provide a thermogravimetric analysis method for a solid sample that can be analyzed based on a weight change curve in which a baseline variation is corrected to the maximum.
（ニ）課題を解決するための手段 かくしてこの発明によれば、固体試料を熱重量法に付
すことにより得られる重量変化曲線に基づいて該固体試
料を分析する熱重量分析法において、固体試料を一定速
度で連続的に加熱して得られる重量変化曲線の測定デー
タから、該測定後の固体試料を同一の条件下で再加熱し
て得られる重量変化曲線の測定データを減算することに
より、重量変化に関するベースライン変動を補正するこ
とを特徴とする固体試料の熱重量分析法が提供される。(D) Means for Solving the Problems According to the present invention, in a thermogravimetric analysis method for analyzing a solid sample based on a weight change curve obtained by subjecting the solid sample to a thermogravimetric method, By subtracting the measured data of the weight change curve obtained by reheating the solid sample after the measurement under the same conditions from the measured data of the weight change curve obtained by continuously heating at a constant speed, A method for thermogravimetric analysis of a solid sample is provided, wherein the method corrects for baseline variation with respect to variation.
この発明の方法は、熱重量変化後の試料を再加熱して
測定する以外は、一般のTG測定と同様に行われる。The method of the present invention is carried out in the same manner as a general TG measurement, except that the sample after the thermogravimetric change is reheated and measured.
この発明の方法において、測定対象となる固体試料
は、最初の加熱時に分解によって重量又は体積が著しく
変化するものであっても、再加熱時において目的の温度
範囲で重量変化（反応）が起こらないものであればいず
れのものであってもよい。従って例えば高分子化合物で
あっても、その化合物における脱水反応のように、最初
の加熱終了後においてはその一部だけが分解（脱水）し
ており、かつ目的の温度範囲で反応（脱水反応）が終了
するものであれば、この発明の方法に適用できるものと
なる。なお上記適用される固体試料は、最初の加熱によ
り生ずる重量変化・体積変化・構造変化等はできるだけ
小さいものが好ましい。In the method of the present invention, the solid sample to be measured does not change in weight (reaction) in the target temperature range upon reheating, even if the weight or volume of the solid sample to be measured changes remarkably due to decomposition during the first heating. Any of them may be used. Therefore, for example, even in the case of a polymer compound, only a part thereof is decomposed (dehydrated) after completion of the first heating and reacts in a target temperature range (dehydration reaction) as in the dehydration reaction of the compound. Is completed, the method can be applied to the method of the present invention. It is preferable that the solid sample to be applied has as small a weight change, a volume change, a structural change, and the like as occur as a result of the first heating.
この発明の方法において、データ測定は少なくとも２
回行われる。すなわち１回目は通常のTG測定の方法が用
いられ、２回目以降は１回目のデータ測定終了した試料
がそのまま用いられる。１回目の加熱条件と２回目以降
の加熱条件とは同一条件に設定される。In the method of the invention, the data measurement is at least 2
Is done many times. That is, a normal TG measurement method is used for the first time, and a sample after the first data measurement is used as it is for the second and subsequent times. The first heating condition and the second and subsequent heating conditions are set to the same condition.
この発明の方法の実施には、TG測定に用いられる当該
分野で公知の装置がそのまま用いられる。In carrying out the method of the present invention, an apparatus known in the art used for TG measurement is used as it is.
（ホ）作用 この発明によれば、固体試料を熱重量法に付し一定速
度で連続的に加熱して、重量変化に関する測定データを
得、次いでこの加熱後の固体試料を同一条件で再加熱し
てブランクデータを得、前記重量変化に関する測定デー
タから上記ブランクデータを減算することにより、上記
重量変化に関する測定データのベースライン変動が補正
されることとなる。(E) Function According to the present invention, the solid sample is subjected to the thermogravimetric method and is continuously heated at a constant rate to obtain measurement data relating to the change in weight. Then, the solid sample after this heating is reheated under the same conditions. Then, the blank data is obtained, and the blank data is subtracted from the measurement data regarding the weight change, whereby the baseline variation of the measurement data regarding the weight change is corrected.
以下実施例によりこの発明を詳細に説明するが、これ
によりこの発明は限定されるものではない。Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited thereto.
（ヘ）実施例 （ｉ）固体試料としてポリエステルフィルムを選択し、
この固体試料に含有される水分量をTG（TGA−50:島津製
作所製）により下記条件で測定した。(F) Example (i) A polyester film was selected as a solid sample,
The amount of water contained in this solid sample was measured by TG (TGA-50: manufactured by Shimadzu Corporation) under the following conditions.
脱水反応に伴う重量減少について得られた重量変化曲
線（減量曲線）イを第１図に示す。FIG. 1 shows a weight change curve (weight loss curve) a obtained for the weight loss accompanying the dehydration reaction.
試料量 :54.66mg 昇温速度 : 5℃/min 窒素供給量 :50ml/min 第１図に示された重量変化曲線イは、ベースラインド
リフトを含むものである。Sample amount: 54.66 mg Heating rate: 5 ° C./min Nitrogen supply amount: 50 ml / min The weight change curve A shown in FIG. 1 includes the baseline drift.
（ii）次に、上記測定後のポリエステルフィルムを室温
まで冷却した後、上記と同一条件かつ同TGにより再加熱
し、第２図に示される重量変化曲線ロを得た。(Ii) Next, after the polyester film after the above measurement was cooled to room temperature, it was reheated under the same conditions and under the same TG as above, to obtain a weight change curve B shown in FIG.
ここで得られた重量変化曲線ロは、このTGにおけるベ
ースラインドリフトそのものを表していると考えられ
る。The weight change curve B obtained here is considered to represent the baseline drift itself in this TG.
（iii）前記重量変化曲線イから上記重量変化曲線ロを
減算すると、第３図に示される重量変化曲線（減量曲
線）ハが得られる。この重量変化曲線ハはベースライン
ドリフト分が補正されたものである。(Iii) By subtracting the weight change curve B from the weight change curve A, a weight change curve (weight loss curve) C shown in FIG. 3 is obtained. This weight change curve C is obtained by correcting the baseline drift.
上記得られた重量変化曲線ハに基づけば、温度29℃か
ら100℃までの間における重量減少率は、0.0678％と得
られる。Based on the weight change curve C obtained above, the weight reduction rate between the temperature of 29 ° C. and 100 ° C. is obtained as 0.0678%.
従って、この固体試料として用いたポリエステルフィ
ルムにおける含水率は、0.068％と求められることとな
る。Therefore, the water content in the polyester film used as the solid sample is determined to be 0.068%.
（ト）発明の効果 この発明によれば、TGにおいて、ベースラインドリフ
トを最大限除去した正確な重量変化曲線を得ることがで
きる。(G) Effects of the Invention According to the present invention, it is possible to obtain an accurate weight change curve in a TG in which the baseline drift is removed to the maximum.
第１図はベースラインドリフトを含むポリエステルフィ
ルムの重量変化曲線、第２図は再加熱により得られたポ
リエステルフィルムの重量変化曲線、第３図はこの発明
の方法により得られたポリエステルフィルムの重量変化
曲線である。1 is a weight change curve of a polyester film including a baseline drift, FIG. 2 is a weight change curve of a polyester film obtained by reheating, and FIG. 3 is a weight change of a polyester film obtained by the method of the present invention. It is a curve.
Claims (1)
れる重量変化曲線に基づいて該固体試料を分析する熱重
量分析法において、 固体試料を一定速度で連続的に加熱して得られる重量変
化曲線の測定データから、該測定後の固体試料を同一の
条件下で再加熱して得られる重量変化曲線の測定データ
を減算することにより、重量変化に関するベースライン
変動を補正することを特徴とする固体試料の熱重量分析
法。1. A thermogravimetric analysis method for analyzing a solid sample based on a weight change curve obtained by subjecting the solid sample to a thermogravimetric method, wherein a weight obtained by continuously heating the solid sample at a constant rate. By subtracting the measured data of the weight change curve obtained by reheating the solid sample after the measurement under the same conditions from the measured data of the change curve, the baseline change related to the weight change is corrected. Analysis of solid samples.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31396989A JP2760104B2 (en) | 1989-11-30 | 1989-11-30 | Thermogravimetric analysis of solid samples |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31396989A JP2760104B2 (en) | 1989-11-30 | 1989-11-30 | Thermogravimetric analysis of solid samples |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03172746A JPH03172746A (en) | 1991-07-26 |
| JP2760104B2 true JP2760104B2 (en) | 1998-05-28 |
Family
ID=18047664
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31396989A Expired - Fee Related JP2760104B2 (en) | 1989-11-30 | 1989-11-30 | Thermogravimetric analysis of solid samples |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2760104B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6247246B1 (en) | 1998-05-27 | 2001-06-19 | Denver Instrument Company | Microwave moisture analyzer: apparatus and method |
| US9389194B2 (en) * | 2013-09-13 | 2016-07-12 | Netzsch-Geraetebau Gmbh | System and method for analysis in modulated thermogravimetry |
| WO2017101853A1 (en) | 2015-12-16 | 2017-06-22 | 宁波舜宇光电信息有限公司 | Lens module and capturing module integrating focusing mechanism and assembly method therefor |
-
1989
- 1989-11-30 JP JP31396989A patent/JP2760104B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03172746A (en) | 1991-07-26 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |