JPH05302902A - Analyzing method for vanadium pentoxide in vanadium trioxide - Google Patents
Analyzing method for vanadium pentoxide in vanadium trioxideInfo
- Publication number
- JPH05302902A JPH05302902A JP10723192A JP10723192A JPH05302902A JP H05302902 A JPH05302902 A JP H05302902A JP 10723192 A JP10723192 A JP 10723192A JP 10723192 A JP10723192 A JP 10723192A JP H05302902 A JPH05302902 A JP H05302902A
- Authority
- JP
- Japan
- Prior art keywords
- vanadium
- vanadium pentoxide
- trioxide
- pentoxide
- differential thermal
- 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.)
- Pending
Links
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 title claims abstract description 72
- QUEDYRXQWSDKKG-UHFFFAOYSA-M [O-2].[O-2].[V+5].[OH-] Chemical compound [O-2].[O-2].[V+5].[OH-] QUEDYRXQWSDKKG-UHFFFAOYSA-M 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 16
- 230000008018 melting Effects 0.000 claims abstract description 16
- 238000004455 differential thermal analysis Methods 0.000 claims abstract description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 13
- 238000011088 calibration curve Methods 0.000 claims abstract description 6
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical class [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 abstract description 10
- 229910001935 vanadium oxide Inorganic materials 0.000 abstract description 10
- 238000000634 powder X-ray diffraction Methods 0.000 abstract description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021542 Vanadium(IV) oxide Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000012916 structural analysis Methods 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 1
- GRUMUEUJTSXQOI-UHFFFAOYSA-N vanadium dioxide Chemical compound O=[V]=O GRUMUEUJTSXQOI-UHFFFAOYSA-N 0.000 description 1
- IBYSTTGVDIFUAY-UHFFFAOYSA-N vanadium monoxide Chemical compound [V]=O IBYSTTGVDIFUAY-UHFFFAOYSA-N 0.000 description 1
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、三酸化バナジウム中の
五酸化バナジウムの分析方法に関する。The present invention relates to a method for analyzing vanadium pentoxide in vanadium trioxide.
【０００２】[0002]
【従来の技術】従来、ノーヒューズブレーカーの心臓部
である限流素子の原料として、三酸化バナジウムを主成
分としたＰＴＣ（positive temperature coefficient）
セラミックスが用いられている。上記三酸化バナジウム
を製造するには、水素雰囲気中にて焼成を行う必要があ
る。従って、この焼成を行う際、三酸化バナジウム中に
五酸化バナジウムが不純物として含まれると水が生成さ
れる。この水は焼成時の熱により水蒸気となって急膨張
するので、焼成時に小爆発が起こるおそれがある。2. Description of the Related Art Conventionally, PTC (positive temperature coefficient) containing vanadium trioxide as a main component has been used as a raw material for a current limiting element which is the heart of a no-fuse breaker.
Ceramics are used. In order to manufacture the above vanadium trioxide, it is necessary to perform firing in a hydrogen atmosphere. Therefore, when vanadium trioxide is included as an impurity in vanadium trioxide, water is generated during the firing. Since this water becomes steam due to heat during firing and expands rapidly, a small explosion may occur during firing.
【０００３】このようなことから、限流素子を製造する
にあたって、五酸化バナジウムを含まない三酸化バナジ
ウム原料を安定して購入する必要があり、また三酸化バ
ナジウム中の五酸化バナジウムを正確に定量する必要が
ある。From the above, it is necessary to stably purchase a vanadium trioxide raw material containing no vanadium pentoxide in manufacturing a current limiting element, and to accurately determine vanadium pentoxide in vanadium trioxide. There is a need to.
【０００４】[0004]
【発明が解決しようとする課題】一般に、三酸化バナジ
ウム中の不純物であるバナジウムの酸化物としては、一
酸化バナジウム、二酸化バナジウム、五酸化バナジウム
の４種類が挙げられる。現在、上記各酸化バナジウムの
構造解析分析として粉末Ｘ線回析方法が一般に行われて
いる。しかし、不純物レベルの精密な分析は主成分であ
る三酸化バナジウムに妨害され、精密な分析を行うこと
は困難である。Generally, as vanadium oxides which are impurities in vanadium trioxide, there are four kinds of vanadium monoxide, vanadium dioxide and vanadium pentoxide. Currently, a powder X-ray diffraction method is generally used as a structural analysis analysis of each vanadium oxide. However, precise analysis of the impurity level is hindered by vanadium trioxide, which is the main component, and it is difficult to perform precise analysis.
【０００５】また、上記粉末Ｘ線回折方法にて用いられ
る粉末Ｘ線回析装置は特殊な機器であり、汎用性がな
い。Further, the powder X-ray diffraction apparatus used in the above-mentioned powder X-ray diffraction method is a special device and is not versatile.
【０００６】本発明は上記背景の下になされたものであ
り、精度が高く、かつ安価で汎用的な装置を用いた三酸
化バナジウム中の五酸化バナジウムの分析方法を提供す
ることを目的とする。The present invention has been made in view of the above background, and an object thereof is to provide a method for analyzing vanadium pentoxide in vanadium trioxide using a highly accurate and inexpensive general-purpose device. .
【０００７】[0007]
【課題を解決するための手段及び作用】本発明者らは、
バナジウム酸化物において、唯一五酸化バナジウムの融
点のみが６９０℃と低く、他のバナジウム酸化物の融点
は五酸化バナジウムの融点の３倍近く、1950〜1970℃に
達していることに着目し、鋭意検討を重ねて本発明を完
成した。Means and Actions for Solving the Problems The present inventors have
Focusing on vanadium oxide, the melting point of vanadium pentoxide is as low as 690 ° C, and the melting points of other vanadium oxides are almost 3 times the melting point of vanadium pentoxide, reaching 1950 to 1970 ° C. The present invention has been completed through intensive studies.
【０００８】即ち、本発明は三酸化バナジウム中の五酸
化バナジウムの分析方法において、前記分析方法として
示差熱分析を用いるとともに、示差熱分析時における融
解時の吸熱ピーク面積と、予め作成した五酸化バナジウ
ム含有量と前記ピーク面積との検量線とにより五酸化バ
ナジウムの含有量を決定することを特徴とする。That is, according to the present invention, in the method for analyzing vanadium pentoxide in vanadium trioxide, the differential thermal analysis is used as the analytical method, and the endothermic peak area at the time of melting in the differential thermal analysis and the pentoxide prepared in advance are used. It is characterized in that the content of vanadium pentoxide is determined from the calibration curve of the vanadium content and the peak area.
【０００９】上記のように示差熱分析にを用いて分析を
行うことにより、従来の粉末Ｘ線回折法等に比べて高精
度に三酸化バナジウム中の五酸化バナジウムの定量を行
うことができる。By performing the analysis using the differential thermal analysis as described above, it is possible to quantify vanadium pentoxide in vanadium trioxide with higher accuracy than in the conventional powder X-ray diffraction method and the like.
【００１０】[0010]
【実施例】以下、本発明を実施例によって説明する。EXAMPLES The present invention will be described below with reference to examples.
【００１１】一般的に知られている酸化バナジウムの物
性を表１に示す。この表により、各酸化バナジウムにお
いて、唯一五酸化バナジウムの融点のみが690℃と低
く、他の酸化バナジウムの融点は五酸化バナジウムの融
点の３倍近く、1950〜1970℃に達していることがわか
る。Table 1 shows the generally known physical properties of vanadium oxide. According to this table, in each vanadium oxide, only the melting point of vanadium pentoxide is as low as 690 ° C, and the melting points of other vanadium oxides are almost 3 times the melting point of vanadium pentoxide, reaching 1950 to 1970 ° C. Recognize.
【００１２】[0012]
【表１】 [Table 1]
【００１３】このことから、示差熱分析により五酸化バ
ナジウムの分別定量分析を試みた。以下にその詳細を示
す。From this, the differential quantitative analysis of vanadium pentoxide was attempted. The details are shown below.
【００１４】まず、純度99％の三酸化バナジウムと五酸
化バナジウムとを種々の比率で混合して標準粉体を作成
した。First, standard powder was prepared by mixing vanadium trioxide and vanadium pentoxide having a purity of 99% at various ratios.
【００１５】この標準粉体を用いて示差熱分析を窒素ガ
ス雰囲気中、昇温温度を毎分20℃としてい、融解時の吸
熱ピーク面積と含有量の関係をプロットした。Using this standard powder, a differential thermal analysis was carried out in a nitrogen gas atmosphere at a temperature rise temperature of 20 ° C. per minute, and the relationship between the endothermic peak area during melting and the content was plotted.
【００１６】尚、上記示差熱分析において使用するセル
としては白金、アルミナ等があるが、白金セルを用いた
場合は酸化バナジウムの溶解体が白金と化合して化合物
を生成するおそれがあるので、アルミナセルを使用す
る。The cells used in the above-mentioned differential thermal analysis include platinum, alumina and the like. However, when a platinum cell is used, a solution of vanadium oxide may combine with platinum to form a compound. Use an alumina cell.
【００１７】また、数％程度の五酸化バナジウムを分析
するためには、試料量として２００ｍｇ前後が必要とな
る。Further, in order to analyze vanadium pentoxide of several%, a sample amount of about 200 mg is required.
【００１８】更に、一般的な示差熱分析の昇温速度は毎
分１０〜20℃であるが、数％程度の五酸化バナジウムを
定量するためには毎分20℃が妥当である。この際、加熱
雰囲気は窒素またはアルゴンガスなどの不活性なガスと
し、毎分100ml程度を流すものとした。Further, the rate of temperature rise in general differential thermal analysis is 10 to 20 ° C. per minute, but 20 ° C. per minute is appropriate for quantifying vanadium pentoxide of several%. At this time, the heating atmosphere was an inert gas such as nitrogen or argon gas, and about 100 ml / min was allowed to flow.
【００１９】上記示差熱実験の測定結果を図２に、また
Ｖ2Ｏ5含有量と融解時の吸熱ピーク面積との相関を表す
グラフを図１に示す。FIG. 2 shows the measurement results of the above-mentioned differential thermal experiment, and FIG. 1 shows a graph showing the correlation between the V 2 O 5 content and the endothermic peak area upon melting.
【００２０】図２において、Ａ線は温度とＴｇとの相関
を、またＢ線は温度とＤＴＡとの相関を示す。In FIG. 2, line A shows the correlation between temperature and Tg, and line B shows the correlation between temperature and DTA.
【００２１】また、図１においてＶ2Ｏ5の検量線（ｙ＝
−1.1×10-2ｘ−1.69）の相関係数は0.9951となり、良
好な結果が得られていることがわかる。Further, in FIG. 1, a calibration curve of V 2 O 5 (y =
The correlation coefficient of −1.1 × 10 −2 x−1.69) is 0.9951, which shows that good results are obtained.
【００２２】従って、三酸化バナジウム中の五酸化バナ
ジウムの分析において、上記検量線を用いて示差熱分析
を行うことにより、高精度に五酸化バナジウムの定量を
行うことができることがわかる。Therefore, it is understood that in the analysis of vanadium pentoxide in vanadium trioxide, the differential thermal analysis using the above calibration curve enables highly accurate determination of vanadium pentoxide.
【００２３】[0023]
【発明の効果】本発明においては上記のように三酸化バ
ナジウム中の不純物の分析を行っているので、以下のよ
うな効果が得られる。In the present invention, since the impurities in vanadium trioxide are analyzed as described above, the following effects can be obtained.
【００２４】１．三酸化バナジウム中の五酸化バナジウ
ムの分析が可能である。1. It is possible to analyze vanadium pentoxide in vanadium trioxide.
【００２５】汎用性の高い示差熱分析により、迅速かつ
簡単に三酸化バナジウム中の五酸化バナジウムの定量が
可能である。A highly versatile differential thermal analysis enables rapid and simple determination of vanadium pentoxide in vanadium trioxide.
【００２６】２．三酸化バナジウムの品質管理ができ
る。2. You can control the quality of vanadium trioxide.
【００２７】従来は三酸化バナジウムと五酸化バナジウ
ムとの分別定量が困難であったが、本分析方法によりこ
の分析が可能となり、三酸化バナジウムの十分な品質管
理が実現される。Conventionally, it was difficult to separate and quantify vanadium trioxide and vanadium pentoxide, but this analysis method enables this analysis and realizes sufficient quality control of vanadium trioxide.
【００２８】３．安定した製造が可能となる。3. Stable manufacturing becomes possible.
【００２９】従来は限流素子の製造工程において、焼成
を行う際に三酸化バナジウム中の五酸化バナジウムによ
る小爆発が懸念されたが、本分析方法の適用により、十
分な品質の原料の購入が可能となり、限流素子を安定し
て製造することが可能となる。Conventionally, in the manufacturing process of a current limiting element, there was a concern that a small explosion due to vanadium pentoxide in vanadium trioxide would occur when firing, but by applying this analysis method, it is possible to purchase raw materials of sufficient quality. It becomes possible, and it becomes possible to manufacture a current limiting element stably.
【図１】Ｖ2Ｏ5含有量と融解時の吸熱ピーク面積との相
関を表すグラフFIG. 1 is a graph showing the correlation between the V 2 O 5 content and the endothermic peak area upon melting.
【図２】示差熱実験の測定結果を表すグラフFIG. 2 is a graph showing measurement results of a differential thermal experiment.
Claims (1)
の分析方法において、前記分析方法として示差熱分析を
用いるとともに、示差熱分析時における融解時の吸熱ピ
ーク面積と、予め作成した五酸化バナジウム含有量と前
記ピーク面積との検量線とにより五酸化バナジウムの含
有量を決定することを特徴とする三酸化バナジウム中の
五酸化バナジウムの分析方法。1. A method for analyzing vanadium pentoxide in vanadium trioxide, wherein a differential thermal analysis is used as the analytical method, and an endothermic peak area upon melting in the differential thermal analysis and a vanadium pentoxide content prepared in advance. A method for analyzing vanadium pentoxide in vanadium trioxide, characterized in that the content of vanadium pentoxide is determined by a calibration curve of the above and the peak area.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10723192A JPH05302902A (en) | 1992-04-27 | 1992-04-27 | Analyzing method for vanadium pentoxide in vanadium trioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10723192A JPH05302902A (en) | 1992-04-27 | 1992-04-27 | Analyzing method for vanadium pentoxide in vanadium trioxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05302902A true JPH05302902A (en) | 1993-11-16 |
Family
ID=14453819
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10723192A Pending JPH05302902A (en) | 1992-04-27 | 1992-04-27 | Analyzing method for vanadium pentoxide in vanadium trioxide |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05302902A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019066233A (en) * | 2017-09-29 | 2019-04-25 | 本田技研工業株式会社 | Method for measuring residual amount of resin material in metal porous body |
| KR102654032B1 (en) * | 2023-10-17 | 2024-04-03 | 케이원에코텍 주식회사 | Two way strainer |
-
1992
- 1992-04-27 JP JP10723192A patent/JPH05302902A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019066233A (en) * | 2017-09-29 | 2019-04-25 | 本田技研工業株式会社 | Method for measuring residual amount of resin material in metal porous body |
| KR102654032B1 (en) * | 2023-10-17 | 2024-04-03 | 케이원에코텍 주식회사 | Two way strainer |
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