JPH03214100A - Managing method of nuclear fuel reprocessing process - Google Patents

Managing method of nuclear fuel reprocessing process

Info

Publication number
JPH03214100A
JPH03214100A JP2010265A JP1026590A JPH03214100A JP H03214100 A JPH03214100 A JP H03214100A JP 2010265 A JP2010265 A JP 2010265A JP 1026590 A JP1026590 A JP 1026590A JP H03214100 A JPH03214100 A JP H03214100A
Authority
JP
Japan
Prior art keywords
concentration
nuclear fuel
solution
fillers
column
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.)
Granted
Application number
JP2010265A
Other languages
Japanese (ja)
Other versions
JP2508335B2 (en
Inventor
Masami Matsui
松居　正己
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shimadzu Corp
Original Assignee
Shimadzu Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Shimadzu Corp filed Critical Shimadzu Corp
Priority to JP1026590A priority Critical patent/JP2508335B2/en
Publication of JPH03214100A publication Critical patent/JPH03214100A/en
Application granted granted Critical
Publication of JP2508335B2 publication Critical patent/JP2508335B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E30/00—Energy generation of nuclear origin
    • Y02E30/30—Nuclear fission reactors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies

Landscapes

  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)

Abstract

PURPOSE:To detect a change in the minute concentration of tributyl phosphate surely and quickly by analyzing a nuclear fuel reprocessing liquid by gas chromatography and by detecting the concentration of butyl alcohol. CONSTITUTION:Fillers 2 are produced by preparing a solution wherein polyethylene glycol to be a coating agent is dissolved in methanol, for instance, so that a concentration (e.g. about 1%) being suitable for producing the fillers be obtained, by adding porous polymer beads of about 80 to 100 meshes to be stationary-phase carriers to the solution thus prepared, by driving the solution in the environment of about 100 deg.C subsequently, by filling it up in a glass column thereafter and by subjecting it to an aging process with a temperature raised from about 200 deg.C to about 300 deg.C in 24 hours. These fillers 2 are filled up in an analyzing column 1. One end of the column 1 is connected to a carrier gas source 5 through a sample vaporizing device 3, while the other end is connected to a detector 5.

Description

【発明の詳細な説明】 （産業上の利用分野） 本発明は、核燃料処理工程で使用されるリン酸トリブチ
ルの品位を管理するのに適した分析技術に開する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention is directed to an analytical technique suitable for controlling the quality of tributyl phosphate used in nuclear fuel processing steps.

（従来技術） 使用済み核燃料からウランやプルトニュームを抽出する
核燃料再処理作業には、使用済み核燃料を硝酸により溶
解する工程と、３０バーセシトのリン酸トリブチルのｎ
−トチカン溶液により前記溶解液からウランやプルトニ
ュームを抽出する工程とを備えたとニーレックス法が用
いられでいる。(Prior art) Nuclear fuel reprocessing work to extract uranium and plutonium from spent nuclear fuel involves the process of dissolving the spent nuclear fuel with nitric acid and the process of dissolving the spent nuclear fuel with nitric acid, and the process of dissolving the spent nuclear fuel with nitric acid.
- extracting uranium and plutonium from the solution using a totican solution.

この抽出工程は硝Ｍを含む溶液の下で行なわれるため、
リン酸トリブチルが加水分解によりリン酸ジブチル（Ｄ
ＢＰ）、リン酸モノブチル（ＭＢρ）、及びリン酸に変
化しでしまい、ウランやプルトニュームの抽出効率が低
下するという問題がある。Since this extraction step is carried out under a solution containing nitrate M,
Tributyl phosphate is hydrolyzed to dibutyl phosphate (D
BP), monobutyl phosphate (MBρ), and phosphoric acid, resulting in a problem that the extraction efficiency of uranium and plutonium decreases.

（発明が解決しようとする問題点） このため、核燃料再処理作業では、リン酸トリブチルの
濃度か抽出効率を左右することになり、リン酸トリブチ
ルの濃度測定が極めて重要な問題となる。(Problems to be Solved by the Invention) Therefore, in nuclear fuel reprocessing work, the concentration of tributyl phosphate determines the extraction efficiency, and measurement of the concentration of tributyl phosphate becomes an extremely important problem.

このような問題を解決するため、赤外線吸光法や等速電
気泳動法により濃度管理を行なうことも考えられるが、
これらの手法では感度や精度が低いため、核燃料処理で
求められるような僅かの濃度変化を検出するに必要な場
合には十分な分析精度を得ることができず、リン酸トリ
ブチルの品位管理に使用することができないという問題
がある。In order to solve this problem, concentration control using infrared absorption method or isotachophoresis method may be considered.
Due to the low sensitivity and accuracy of these methods, they cannot provide sufficient analytical accuracy when necessary to detect small concentration changes such as those required in nuclear fuel processing, and are used for quality control of tributyl phosphate. The problem is that it cannot be done.

本発明はこのような問題に鑑みてなされたちのであって
、その目的とするところは、リン酸トリブチルの僅かな
濃度変化をガスクロマトグラフィにより検出することか
できる新規な分析方法を提案することにある。The present invention was made in view of these problems, and its purpose is to propose a new analytical method that can detect slight changes in the concentration of tributyl phosphate using gas chromatography. .

（課題を解決するための手段） このような問題を解決するために本発明においては、リ
ン酸トリブチルか加水分解するときに１しるｎ−ブチル
アルコールをガスクロマトグラフにより検出するように
した。(Means for Solving the Problems) In order to solve such problems, in the present invention, when tributyl phosphate is hydrolyzed, n-butyl alcohol is detected using a gas chromatograph.

（作用） カスクロマトグラフは、ｎ−ブチルアルコールを極めて
高い感度で検出するため、ｎ−ブチルアルコールと等比
間係にあるリン酸の濃度、したかってリン酸トリブチル
の濃度を知ることか可能となる。(Function) Because the cass chromatograph detects n-butyl alcohol with extremely high sensitivity, it is possible to know the concentration of phosphoric acid, which is in a geometric relationship with n-butyl alcohol, and therefore the concentration of tributyl phosphate. .

（実施例） そこで、以下に本発明の詳細を実施例に基づいて説明す
る。(Example) Therefore, the details of the present invention will be explained below based on an example.

第１図は本発明に使用する装置の一例を示すものて、図
中符号１は、分析カラムで、ポーラスポリマービーズを
固相担体とし、これの表面にシリコン系高分子ポリマー
、またはポリエチレングリコールをコーティングしてな
る充填剤２．２．２・・・・を封入して構成されたｎ−
ブチルアルコールを分離するのに適したものが選択され
でおり、端には試料気化製雪３が、また他端には検出器
、例えばＦＩＤ４を接続しで構成されている。Fig. 1 shows an example of the apparatus used in the present invention, and reference numeral 1 in the figure is an analytical column, which uses porous polymer beads as a solid phase carrier and coated with a silicon-based polymer or polyethylene glycol on the surface. An n- compound formed by enclosing a coating filler 2.2.2...
A device suitable for separating butyl alcohol has been selected, and is configured with a sample vaporizer 3 connected to one end and a detector such as an FID 4 connected to the other end.

なあ、図中符号５は、キャリアガス源を示す。Incidentally, the reference numeral 5 in the figure indicates a carrier gas source.

上述の充填剤の一例について説明する。An example of the above-mentioned filler will be explained.

メタノールにコーティング剤となるポリエチレングリコ
ール（商品名ＰＥＧ−２０Ｍ）を、充填剤を造るのに適
した濃度、例えば濃度１パーセントとなるように溶解し
てなる溶液を用意し、これに固定相担体となる８０乃至
１００メツシユのポーラスポリマービーズを加え、溶液
を排除して３０分室温で放言し、次いで１００℃の環境
下で間乾燥したのち、ガラスカラムに充填し、これを温
度約２００℃からほぼ２４時間掛けて温度３００℃まで
昇温させてエージングして構成されでいる。Prepare a solution by dissolving polyethylene glycol (trade name: PEG-20M), which will serve as a coating agent, in methanol to a concentration suitable for making a packing material, for example, 1%, and add a stationary phase carrier and a solution to this solution. 80 to 100 meshes of porous polymer beads were added, the solution was removed, and the solution was left to stand at room temperature for 30 minutes. After drying for a while in an environment of 100°C, it was packed into a glass column and heated from a temperature of about 200°C to about 100°C. It is constructed by aging by raising the temperature to 300°C over 24 hours.

このエージング処理により、コーティング剤塗布工程で
圧しるポーラスポリマーど−ズの露出面の０．００１Ｌ
Ｊｍ程度以下の細孔だけを選択的に除去することができ
た。Through this aging treatment, 0.001L of the exposed surface of the porous polymer which is pressed in the coating agent application process is
It was possible to selectively remove only pores of about Jm or less.

このように構成した装置に、濃度５０パーセントの硝酸
２０ミリリツトルと、ｎ−ドデカンに濃度３０パーセン
トとなるように純粋なリン酸トリブチルを溶解したもの
５０ミリリツトルとを混合してなるサンプルを温度３０
℃に維持しながら、これの上澄み液を単位時間毎に採取
したものを試料に用いて分析を行なった。A sample prepared by mixing 20 milliliters of nitric acid with a concentration of 50 percent and 50 milliliters of pure tributyl phosphate dissolved in n-dodecane to a concentration of 30 percent was heated in the apparatus constructed in this manner at a temperature of 30 percent.
While maintaining the temperature at °C, the supernatant liquid was collected at every unit time and used as a sample for analysis.

この結果、第２図に示したように時間の経過とともに （１）リン酸トリブチルリン酸十Ｈ２０十硝酸　→リン
酸ジブチル ■リン酸ジプチル＋Ｈ２０＋硝酸　→ リン酸モノブチル （３）リン酸モノブチル＋Ｈ２０＋硝酸　→リン酸＋ｎ
−ブチルアルコール なる加水分解反応により発生するＰＰＭオーダのｎ−ブ
チルアルコールを、強酸の存在下において試料注入から
８分後に検出することができた。As a result, as shown in Figure 2, over time, (1) tributyl phosphate deca H20 deca nitric acid → dibutyl phosphate ■ diptyl phosphate + H20 + nitric acid → monobutyl phosphate (3) monobutyl phosphate + H20 + nitric acid → Phosphoric acid + n
-Butyl alcohol, n-butyl alcohol on the PPM order generated by the hydrolysis reaction, could be detected 8 minutes after sample injection in the presence of a strong acid.

なあ、この実施例においては硝酸の濃度を５０パーセン
トと核燃料再処理液よりも高くして実験時間の短縮を図
るとともに、核燃料物質の入手が極めて困難なため、核
燃料物質を含まないものをサンプルに用いているが、硝
酸濃度を通常の再処理工程におけるものと同一の濃度に
するとともに、核燃料物質が含まれでいでもｎ−ブチル
アルコールＭＰＰＭオーダで検出できることは明らかで
ある。In this example, the concentration of nitric acid was 50% higher than that of the nuclear fuel reprocessing liquid to shorten the experiment time, and since it was extremely difficult to obtain nuclear fuel material, we used a sample that did not contain nuclear fuel material. However, it is clear that the nitric acid concentration is the same as that in a normal reprocessing process, and n-butyl alcohol can be detected on the order of MPPM even though it does not contain nuclear fuel material.

なあ、この実施例においては充填剤としてポーラスポリ
マービーズにエチレングリコールをコーティングしたも
のを使用しでいるが、メタノールにコーティング剤とな
るシリコン系高分子ポリマー（商品名○Ｖ−１７）を、
充填剤を造るのに適した濃度、例えば濃度１パーセント
となるように溶解してなる溶液を用意し、これに固定相
担体となる８０乃至１００メ・ンシュのポーラスポリマ
ーど一ズを加え、水流アスどレータで２分間排気し、こ
の減圧下で２０分間放画し、次いで１００℃の環境下で
間乾煉したのち、温度約２００°Ｃからほぼ２４時間掛
けて温度３００℃まで昇温させてエージングしたものを
用いても同様の作用を奏する。Incidentally, in this example, porous polymer beads coated with ethylene glycol were used as the filler, but a silicone-based polymer (trade name ○V-17) as a coating agent was added to methanol.
Prepare a solution at a concentration suitable for making a filler, for example, 1%, add a porous polymer of 80 to 100 mesh to serve as a stationary phase carrier, and add it to the solution with a water stream. The mixture was evacuated for 2 minutes using an asturator, left to cool for 20 minutes under this reduced pressure, and then dry-melted in an environment of 100°C, and then heated from about 200°C to 300°C over approximately 24 hours. The same effect can be obtained even if the aged material is used.

（発明の効果） 以上、説明したように本発明においでは核燃料再処理液
をガスクロマトグラフィにより分析して、ブチルアルコ
ールの濃度泡検出するようにしたので、リン酸トリブチ
ルのＰＰＭオーグの濃度変化を確実、かつ迅速に検出す
ることかでき、核燃料再処理溶液の品位を高い精度で管
理して核燃料再処理工程を高い効率で運用することか可
能となる。(Effects of the Invention) As explained above, in the present invention, the nuclear fuel reprocessing liquid is analyzed by gas chromatography to detect the concentration bubbles of butyl alcohol, so changes in the concentration of PPM og of tributyl phosphate are reliably detected. , and can be detected quickly, making it possible to manage the quality of the nuclear fuel reprocessing solution with high precision and operate the nuclear fuel reprocessing process with high efficiency.

【図面の簡単な説明】[Brief explanation of drawings]

第１図は本発明に使用するガスウロマトグラフの一例を
示す構成図、第２図はサンプルの分析結果を示す線図で
ある。FIG. 1 is a block diagram showing an example of a gas uromatograph used in the present invention, and FIG. 2 is a diagram showing the analysis results of a sample.

Claims (1)

【特許請求の範囲】[Claims] 核燃料再処理液をガスクロマトグラフィにより分析して
、ブチルアルコールの濃度を検出することを特徴とする
核燃料再料理工程管理方法。A nuclear fuel re-cooking process management method characterized by analyzing nuclear fuel reprocessing liquid by gas chromatography to detect the concentration of butyl alcohol.
JP1026590A 1990-01-18 1990-01-18 Nuclear fuel reprocessing process management method Expired - Lifetime JP2508335B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1026590A JP2508335B2 (en) 1990-01-18 1990-01-18 Nuclear fuel reprocessing process management method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1026590A JP2508335B2 (en) 1990-01-18 1990-01-18 Nuclear fuel reprocessing process management method

Publications (2)

Publication Number Publication Date
JPH03214100A true JPH03214100A (en) 1991-09-19
JP2508335B2 JP2508335B2 (en) 1996-06-19

Family

ID=11745485

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1026590A Expired - Lifetime JP2508335B2 (en) 1990-01-18 1990-01-18 Nuclear fuel reprocessing process management method

Country Status (1)

Country Link
JP (1) JP2508335B2 (en)

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01285899A (en) * 1988-05-12 1989-11-16 Nippon Atom Ind Group Co Ltd Quantity measuring method of deteriorating constituent in deterioration solvent
JPH01304353A (en) * 1988-06-01 1989-12-07 Sumitomo Chem Co Ltd Method of measuring degree of deterioration of extractant

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01285899A (en) * 1988-05-12 1989-11-16 Nippon Atom Ind Group Co Ltd Quantity measuring method of deteriorating constituent in deterioration solvent
JPH01304353A (en) * 1988-06-01 1989-12-07 Sumitomo Chem Co Ltd Method of measuring degree of deterioration of extractant

Also Published As

Publication number Publication date
JP2508335B2 (en) 1996-06-19

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