JP2644400B2 - Method for carbon analysis of nuclear fuel oxide and platinum crucible for carbon analysis - Google Patents
Method for carbon analysis of nuclear fuel oxide and platinum crucible for carbon analysisInfo
- Publication number
- JP2644400B2 JP2644400B2 JP28875591A JP28875591A JP2644400B2 JP 2644400 B2 JP2644400 B2 JP 2644400B2 JP 28875591 A JP28875591 A JP 28875591A JP 28875591 A JP28875591 A JP 28875591A JP 2644400 B2 JP2644400 B2 JP 2644400B2
- Authority
- JP
- Japan
- Prior art keywords
- carbon
- platinum crucible
- nuclear fuel
- sample
- analysis
- 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
Links
Description
【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION
【０００１】[0001]
【産業上の利用分野】本発明は核燃料酸化物中の炭素分
析方法及び炭素分析に使用する白金ルツボに関するもの
である。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for analyzing carbon in nuclear fuel oxides and a platinum crucible used for carbon analysis.
【０００２】[0002]
【従来の技術】一般に、核燃料酸化物（ＵＯ2 ，ＰｕＯ
2 ，ＰｕＯ2 ーＵＯ2 等）にはその製造工程で炭素が不
純物として混入する可能性があり、例えば燃料ペレット
中に炭素が混入すると、高温状態でＣＯ2 、ＣＯ等のガ
スが発生して燃料ピン中の圧力を高め、燃料ピンを破損
させる要因になるため、炭素含有量は所定値以下となる
ように規制されている。そのため核燃料酸化物中の炭素
含有量を分析する必要があるが、従来、核燃料酸化物の
炭素分析は、高周波誘導用助燃剤としてタングステンの
金属片を添加し、磁製ルツボ内で高周波誘導加熱して１
２００〜１３００℃程度の高温状態にして炭素を分離
し、赤外線吸収法により行っていた。 2. Description of the Related Art Generally, nuclear fuel oxides (UO 2 , PuO)
2 , PuO 2 —UO 2 ) may have carbon as an impurity in the manufacturing process. For example, if carbon is mixed in fuel pellets, gases such as CO 2 and CO are generated at a high temperature. Since the pressure in the fuel pin is increased to cause damage to the fuel pin, the carbon content is regulated to be equal to or less than a predetermined value. Therefore, it is necessary to analyze the carbon content of the nuclear fuel oxide.However, conventionally, the carbon analysis of the nuclear fuel oxide involves adding a metal piece of tungsten as a high-frequency induction combustion aid and performing high-frequency induction heating in a porcelain crucible. 1
The carbon was separated at a high temperature of about 200 to 1300 ° C., and the separation was performed by an infrared absorption method.
【０００３】[0003]
【発明が解決しようとする課題】このように、従来の核
燃料酸化物の炭素分析は、これらの物質が高周波誘導さ
れないために高周波誘導用助燃剤としてタングステンの
金属片を添加している。そのため、核燃料酸化物と助燃
剤を良く混合する処理が必要となるため分析処理能力の
向上が困難であるとともに、分析終了後の磁製ルツボ内
には、核燃料酸化物と助燃剤として使用したタングステ
ンが溶融した形で残留してしまうために、核燃料酸化物
の回収不可能なスクラップとなってしまい、核燃料酸化
物の有効利用の妨げになっていた。また、磁製ルツボは
１２００〜１３００℃程の高温ではひびが入ってしま
い、そのため一試料毎に磁製ルツボとタングステンを使
い捨てにしており、分析単価が上がってしまうという問
題もあった。As described above, in the conventional carbon analysis of nuclear fuel oxide, since these substances are not induced by high frequency, a metal piece of tungsten is added as a combustion aid for high frequency induction. For this reason, it is necessary to perform a process of mixing the nuclear fuel oxide and the combustion aid well, so that it is difficult to improve the analysis processing capacity.In addition, after the analysis is completed, the tungsten used for the nuclear fuel oxide and the combustion aid is contained in the magnetic crucible. Because of the residual in a molten form, the nuclear fuel oxide becomes a non-recoverable scrap, which hinders the effective use of the nuclear fuel oxide. In addition, the porcelain crucible is cracked at a high temperature of about 1200 to 1300 ° C., and therefore, the porcelain crucible and tungsten are disposable for each sample, so that there is a problem that the unit price for analysis increases.
【０００４】本発明は上記課題を解決するためのもの
で、核燃料酸化物の回収を容易に行うことができ、分析
処理能力を大幅に増大するとともに、分析単価を低減化
することができる核燃料酸化物の炭素分析方法及び炭素
分析用白金ルツボを提供することを目的とする。SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems, and it is possible to easily recover nuclear fuel oxide, to greatly increase the analytical processing capacity, and to reduce the unit analysis cost. It is an object of the present invention to provide a method for carbon analysis of a product and a platinum crucible for carbon analysis.
【０００５】[0005]
【課題を解決するための手段】本発明は、核燃料酸化物
からなる試料を入れた白金ルツボを高周波誘導加熱し、
高温状態の試料から発生した炭酸ガスを赤外吸収法によ
り検出することにより、炭素含有量を求めることを特徴
とする。また、本発明は、高温状態の試料部分に酸素ガ
スを導入し、試料に接触後、発生した炭酸ガスに赤外線
を照射し、赤外線吸収量から炭素含有量を求めること、
また、白金ルツボは、１０〜２５％ロジウムを添加した
白金合金からなることを特徴とする。According to the present invention, a platinum crucible containing a sample made of nuclear fuel oxide is heated by high frequency induction heating.
The carbon content is obtained by detecting carbon dioxide gas generated from a sample in a high temperature state by an infrared absorption method. Further, the present invention is to introduce oxygen gas into the sample portion in a high temperature state, after contacting the sample, irradiate the generated carbon dioxide gas with infrared rays, and determine the carbon content from the infrared absorption amount,
Further, the platinum crucible is characterized by being made of a platinum alloy to which rhodium is added by 10 to 25%.
【０００６】[0006]
【作用】本発明は核燃料酸化物を白金ルツボに入れ、白
金ルツボを高周波誘導加熱することにより核燃料酸化物
を高温状態にして含有する炭素を分離し、これに酸素ガ
スを供給して炭素と結合させ、これに赤外線を照射して
その吸収度合いを求めることにより含有炭素の分析を行
う。本発明は、従来のように助燃剤を使用していないた
めに、分析終了後直ちに白金ルツボから核燃料酸化物を
回収でき、また助燃剤を混合する処理を省略できるため
分析処理能力を向上させ、さらに白金ルツボは半永久的
に使用できるため分析単価を大幅に低減化することが可
能となる。また、白金ルツボはロジウムを１０〜２５％
添加した白金合金製とすることにより、機械的強度を向
上させることが可能となる。According to the present invention, the nuclear fuel oxide is put into a platinum crucible, the platinum crucible is subjected to high-frequency induction heating, the nuclear fuel oxide is heated to a high temperature state, and the contained carbon is separated. Then, the carbon content is analyzed by irradiating the infrared rays to determine the degree of absorption. Since the present invention does not use a combustion aid as in the prior art, it is possible to recover nuclear fuel oxide from a platinum crucible immediately after the end of analysis, and to improve the analysis processing capacity because the processing of mixing the combustion aid can be omitted, Further, since the platinum crucible can be used semi-permanently, it is possible to greatly reduce the unit analysis cost. Platinum crucible contains 10-25% rhodium
By using the added platinum alloy, the mechanical strength can be improved.
【０００７】[0007]
【実施例】図１は本発明の炭素分析方法を説明するため
の図、図２は本発明で使用する白金ルツボの一実施例の
断面図である。図中、１は加熱容器、２は白金ルツボ、
２ａは白金ルツボ本体、２ｂは白金ルツボ架台、３は試
料、４は高周波発振器、５は高周波誘導加熱用コイル、
６はガス導入チューブ、７はガス排出用チューブ、８は
赤外光光源、９，１１はスリット、１０はモノクロメー
タ、１２は検出器である。FIG. 1 is a view for explaining a carbon analysis method of the present invention, and FIG. 2 is a sectional view of an embodiment of a platinum crucible used in the present invention. In the figure, 1 is a heating vessel, 2 is a platinum crucible,
2a is a platinum crucible body, 2b is a platinum crucible base, 3 is a sample, 4 is a high frequency oscillator, 5 is a high frequency induction heating coil,
6 is a gas introduction tube, 7 is a gas discharge tube, 8 is an infrared light source, 9 and 11 are slits, 10 is a monochromator, and 12 is a detector.
【０００８】図１において、加熱容器１は密閉状態に構
成され、核燃料酸化物の試料３を入れた白金製のルツボ
２が配置される。白金製ルツボは、図２に示すように白
金ルツボ本体２ａ、白金ルツボ架台２ｂからなり、白金
のみでは加工性は良いが機械的強度が低いので、機械的
強度に優れ、低価格で比較的入手し易いロジウム（Ｒ
ｈ）を１０〜２５％添加したものを用いて機械的強度を
出すようにしており、本実施例ではロジウムを２０％添
加した白金合金製を用い、ルツボ壁の厚み０．３ｍｍ、
ルツボ架台の外径１６φ、高さ１０ｍｍ、ルツボ本体の
入口径１７φ（外縁径２０φ）、高さ５ｍｍのものを使
用している。In FIG. 1, a heating vessel 1 is constructed in a closed state, and a platinum crucible 2 containing a nuclear fuel oxide sample 3 is arranged. As shown in FIG. 2, the platinum crucible is composed of a platinum crucible body 2a and a platinum crucible base 2b. Platinum alone has good workability but low mechanical strength. Rhodium (R
h) is added so that the mechanical strength is increased by using 10% to 25%, and in this embodiment, a platinum alloy containing 20% rhodium is used, and the thickness of the crucible wall is 0.3 mm.
A crucible base having an outer diameter of 16φ and a height of 10 mm, an inlet diameter of the crucible body of 17φ (outer edge diameter of 20φ), and a height of 5 mm are used.
【０００９】さらに、加熱容器１内には発振器４で駆動
される高周波コイル５が配置されて白金ルツボ２が高周
波誘導加熱されるようになっており、容器内へはガス導
入チューブ６より酸素が導入されるとともに、排出ガス
チューブ７より排出されるようになっている。Further, a high-frequency coil 5 driven by an oscillator 4 is arranged in the heating vessel 1 so that the platinum crucible 2 is subjected to high-frequency induction heating, and oxygen is introduced into the vessel from a gas introduction tube 6. As it is introduced, it is discharged from the exhaust gas tube 7.
【００１０】このような構成において、発振器４を発振
させて高周波コイル５より白金ルツボ２を高周波誘導加
熱することにより試料３が加熱され、１２００〜１３０
０℃程度の高温状態になると試料中に含有されている炭
素が分離する。このとき容器内に酸素を導入すると分離
した炭素と結合してＣＯ2 、ＣＯが生成され排出チュー
ブ７より排出される。そこで、赤外光の光源８より赤外
線を照射し、スリット９を通して、例えばプリズムから
なるモノクロメータ１０を通してスリット１１を通すこ
とにより所定波長の赤外光を検出する。検出波長域をあ
らかじめ炭素の吸収点に合わせておくことにより、含有
炭素量が求められる。In such a configuration, the sample 3 is heated by oscillating the oscillator 4 and inductively heating the platinum crucible 2 from the high-frequency coil 5 to heat the sample 3 from 1200 to 130.
When the temperature reaches about 0 ° C., carbon contained in the sample is separated. At this time, when oxygen is introduced into the container, it is combined with the separated carbon to produce CO 2 and CO, which are discharged from the discharge tube 7. Therefore, infrared light is irradiated from a light source 8 of infrared light, and the infrared light having a predetermined wavelength is detected by passing through a slit 9 through a slit 9, for example, a monochromator 10 composed of a prism. By adjusting the detection wavelength range in advance to the absorption point of carbon, the carbon content can be determined.
【００１１】なお、本発明は上記実施例に限定されるも
のではなく、例えば、加熱容器中で試料から分離した炭
素に対して直接赤外線を照射して炭素含有量を求めるよ
うにしてもよく、また導入するガスも酸素に限らず空気
等でもよく、また不活性ガス等のキャリアガスで外部に
排出するようにしてもよい。The present invention is not limited to the above embodiment. For example, carbon separated from a sample in a heating vessel may be directly irradiated with infrared rays to determine the carbon content. The gas to be introduced is not limited to oxygen, but may be air or the like, or may be discharged to the outside with a carrier gas such as an inert gas.
【００１２】このように、白金ルツボ自体を高周波誘導
加熱することができるので、従来のようにタングステン
金属片等の助燃剤の使用を不要にし、白金ルツボを半永
久的に使用することができ、分析終了後の試料を迅速に
回収することができる。As described above, since the platinum crucible itself can be subjected to high-frequency induction heating, it is not necessary to use an auxiliary agent such as a tungsten metal piece as in the prior art, and the platinum crucible can be used semipermanently. The sample after completion can be quickly collected.
【００１３】[0013]
【発明の効果】以上のように本発明によれば、分析試料
にタングステン金属片等の助燃剤を添加しなくても分析
が可能になるために、分析終了後の試料を迅速に回収す
ることができ、さらに回収した試料は回収粉末として再
利用できるため、核燃料酸化物の有効利用を図ることが
できる。また、同一白金ルツボで連続的に分析できるた
め、分析作業工程を簡略化することができ、分析処理能
力を大幅に改善することができ、さらに白金ルツボは半
永久的に使用可能であるために分析単価を大幅に低減化
することが可能である。As described above, according to the present invention, the analysis can be performed without adding a combustion aid such as a tungsten metal piece to the analysis sample, so that the sample after the analysis is quickly collected. Further, the recovered sample can be reused as recovered powder, so that the nuclear fuel oxide can be effectively used. In addition, the analysis can be performed continuously with the same platinum crucible, which simplifies the analysis work process, greatly improves the analysis processing capacity, and furthermore, because the platinum crucible can be used semi-permanently, The unit price can be significantly reduced.
【図１】 本発明の炭素分析方法を説明するための図で
ある。FIG. 1 is a diagram for explaining a carbon analysis method of the present invention.
【図２】 本発明で使用する白金ルツボの一実施例の断
面図である。FIG. 2 is a sectional view of one embodiment of a platinum crucible used in the present invention.
１…加熱容器、２…白金ルツボ、２ａ…白金ルツボ本
体、２ｂ…白金ルツボ架台、３…試料、４…高周波発振
器、５…高周波誘導加熱用コイル、６…ガス導入チュー
ブ、７…ガス排出用チューブ、８…赤外光光源、９，１
１…スリット、１０…モノクロメータ、１２…検出器。DESCRIPTION OF SYMBOLS 1 ... Heating container, 2 ... Platinum crucible, 2a ... Platinum crucible main body, 2b ... Platinum crucible base, 3 ... Sample, 4 ... High frequency oscillator, 5 ... High frequency induction heating coil, 6 ... Gas introduction tube, 7 ... Gas discharge Tube, 8 ... infrared light source, 9.1
1 ... slit, 10 ... monochromator, 12 ... detector.
Claims (3)
ルツボを高周波誘導加熱し、高温状態の試料から発生し
た炭酸ガスを赤外吸収法により検出することにより、炭
素含有量を求めることを特徴とする核燃料酸化物の炭素
分析方法。The present invention is characterized in that a platinum crucible containing a sample made of nuclear fuel oxide is induction-heated with high frequency, and carbon content generated from a sample in a high temperature state is detected by an infrared absorption method, thereby obtaining a carbon content. Carbon analysis method for nuclear fuel oxides.
の試料部分に酸素ガスを導入し、試料に接触後、発生し
た炭酸ガスに赤外線を照射し、赤外線吸収量から炭素含
有量を求めることを特徴とする核燃料酸化物の炭素分析
方法。2. The method according to claim 1, wherein oxygen gas is introduced into the sample portion in a high temperature state, and after contact with the sample, the generated carbon dioxide gas is irradiated with infrared rays, and the carbon content is determined from the infrared absorption amount. A method for analyzing carbon in nuclear fuel oxides.
用いる白金ルツボであって、１０〜２５％ロジウムを添
加した白金合金からなることを特徴とする白金ルツボ。3. A platinum crucible used in the method for analyzing carbon according to claim 1 or 2, wherein the platinum crucible is made of a platinum alloy added with 10 to 25% rhodium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28875591A JP2644400B2 (en) | 1991-11-05 | 1991-11-05 | Method for carbon analysis of nuclear fuel oxide and platinum crucible for carbon analysis |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28875591A JP2644400B2 (en) | 1991-11-05 | 1991-11-05 | Method for carbon analysis of nuclear fuel oxide and platinum crucible for carbon analysis |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05126733A JPH05126733A (en) | 1993-05-21 |
| JP2644400B2 true JP2644400B2 (en) | 1997-08-25 |
Family
ID=17734289
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP28875591A Expired - Lifetime JP2644400B2 (en) | 1991-11-05 | 1991-11-05 | Method for carbon analysis of nuclear fuel oxide and platinum crucible for carbon analysis |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2644400B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823749A (en) * | 2016-05-18 | 2016-08-03 | 南京信息工程大学 | Capacitor type infrared gas sensor based on MEMS and preparing method of capacitor type infrared gas sensor |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6297058B1 (en) | 1999-01-14 | 2001-10-02 | Agere Systems Optoelectronics Guardian Corp. | Process for determining impurities in refractory materials |
-
1991
- 1991-11-05 JP JP28875591A patent/JP2644400B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105823749A (en) * | 2016-05-18 | 2016-08-03 | 南京信息工程大学 | Capacitor type infrared gas sensor based on MEMS and preparing method of capacitor type infrared gas sensor |
| CN105823749B (en) * | 2016-05-18 | 2019-04-23 | 南京信息工程大学 | A kind of condenser type infrared gas sensor based on MEMS |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05126733A (en) | 1993-05-21 |
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