WO2009157435A1 - Dispositif de concentration de tritium multi-étages et procédé de concentration de tritium - Google Patents

Dispositif de concentration de tritium multi-étages et procédé de concentration de tritium Download PDF

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Publication number
WO2009157435A1
WO2009157435A1 PCT/JP2009/061393 JP2009061393W WO2009157435A1 WO 2009157435 A1 WO2009157435 A1 WO 2009157435A1 JP 2009061393 W JP2009061393 W JP 2009061393W WO 2009157435 A1 WO2009157435 A1 WO 2009157435A1
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tritium
water
electrolysis
chamber
anode
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PCT/JP2009/061393
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English (en)
Japanese (ja)
Inventor
正明 斎藤
洋 今泉
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地方独立行政法人 東京都立産業技術研究センター
国立大学法人新潟大学
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Publication of WO2009157435A1 publication Critical patent/WO2009157435A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D59/00—Separation of different isotopes of the same chemical element
    • B01D59/38—Separation by electrochemical methods
    • B01D59/40—Separation by electrochemical methods by electrolysis
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B5/00—Water
    • C01B5/02—Heavy water; Preparation by chemical reaction of hydrogen isotopes or their compounds, e.g. 4ND3 + 7O2 ---> 4NO2 + 6D2O, 2D2 + O2 ---> 2D2O
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4005—Concentrating samples by transferring a selected component through a membrane
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/18—Water
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4005—Concentrating samples by transferring a selected component through a membrane
    • G01N2001/4011—Concentrating samples by transferring a selected component through a membrane being a ion-exchange membrane
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N2001/4038—Concentrating samples electric methods, e.g. electromigration, electrophoresis, ionisation

Definitions

  • the present invention relates to a multi-stage tritium concentrating device and a tritium concentrating method for concentrating sample water containing tritium.
  • sample water can be circulated between the cathode chamber and the anode chamber, and the concentration of deuterium is increased by electrolyzing the sample water into hydrogen and oxygen. I am letting.
  • sample water can be circulated between the cathode chamber and the anode chamber, and the concentration of deuterium is increased by electrolyzing the sample water into hydrogen and oxygen. I am letting.
  • Patent Document 3 hydrogen isotopes produced as a result of electrolyzing sample water are diffused and separated, and the hydrogen isotopes are concentrated by recombination with oxygen.
  • the amount required for preparing a concentrated solution (concentrated water) so as to fall within the desired tritium concentration range and measuring the concentration is generally not large, and is 10 ml in the international standard.
  • the operation could not be stopped unless about 50 ml of final concentrated water was produced due to various spatial constraints.
  • the measurement required 10 ml was taken from there, and the remaining 4/5 concentrated water had to be wasted and was not efficient.
  • the apparatus described in Patent Document 3 requires a gas hydrogen isotope separation action by an electrolytic cell or a multistage exchange tower, a recombination battery, and the like, and the structure tends to be complicated.
  • the present invention has been made in view of such problems, and a multi-stage tritium concentrator and a tritium concentrator capable of efficiently increasing the tritium concentration in the sample water to a desired concentration rate with a simple structure. It aims to provide a method.
  • a multistage tritium concentrator of the present invention is provided in each of an anode chamber and a cathode chamber, an ion exchange membrane provided in the vicinity of the anode chamber and the cathode chamber, and an anode chamber and a cathode chamber.
  • a tritium concentrator for increasing the tritium concentration in the sample water by electrolysis wherein a plurality of electrolysis cells are connected in series, The cathode chamber of the electrolysis cell and the anode chamber of the latter electrolysis cell are connected by a connecting pipe.
  • the tritium concentration method of the present invention is a tritium concentration method in which the tritium concentration in the sample water is concentrated by electrolysis using the multistage tritium concentration apparatus, and the sample water is placed in the anode chamber of the first stage electrolysis cell.
  • the first stage electrolysis cell is electrolyzed with electricity after being put in, and the stored water enriched with tritium leached into the cathode chamber of the first stage electrolysis cell by the progress of electrolysis is passed through the connecting pipe.
  • the tritium concentration method of the present invention comprises an anode chamber and a cathode chamber, an ion exchange membrane provided in the vicinity of the anode chamber and the cathode chamber, and an anode and a cathode provided in each of the anode chamber and the cathode chamber.
  • a tritium concentration method for concentrating tritium concentration in sample water by electrolysis using a tritium concentrating device configured to include an electrolytic cell having power supplied to the electrolytic cell after the sample water is placed in the anode chamber of the electrolytic cell
  • the amount of sample water remaining in the anode chamber or the amount of stored water leached in the cathode chamber is stored by storing the condensed water in which tritium is leached into the cathode chamber of the electrolysis cell as the electrolysis progresses.
  • the stored water is recirculated to the anode chamber, and the electrolytic cell is supplied again to store the stored water in which tritium is further concentrated in the cathode chamber. And by repeating the refluxing a reservoir of stored water, concentrating the tritium reservoir water.
  • the sample water supplied to the anode chamber is electrolyzed by supplying power to the electrolysis cell, and hydrogen ions generated at the anode by the electrolysis use the accompanying water. At the same time, it passes through the ion exchange membrane and leaches from the anode chamber toward the cathode chamber. At that time, decomposition of H 2 O contained in the sample water occurs preferentially with respect to decomposition of HOD and HOT (D: deuterium, T: tritium), so that the concentration of tritium in the stored water accumulated in the cathode chamber increases. To do.
  • the stored water is further introduced into the anode chamber of the same or another electrolysis cell, and the desired concentration is repeated by repeating the electrolysis of the stored water, the storage of the stored water in the cathode chamber, and the introduction of the stored water into the anode chamber.
  • the tritium in the sample water can be concentrated efficiently at a high rate. Further, such concentration of sample water can be realized by a simple configuration such as a multi-stage configuration of an electrolytic cell or a combination of an electrolytic cell and a circulating mechanism of stored water.
  • the tritium concentration in the sample water can be efficiently increased to a desired concentration rate with a simple structure.
  • FIG. 1 is a front view showing a multistage tritium concentrator according to a preferred embodiment of the present invention.
  • FIG. 2 is an exploded perspective view of the electrolytic cell in FIG. 1. It is a front view which shows the tritium concentration apparatus concerning the modification of this invention.
  • FIG. 1 is a front view showing a multistage tritium concentrating device 1 according to the first embodiment of the present invention
  • FIG. 2 is an exploded perspective view of the electrolytic cell 3a of FIG.
  • the multistage tritium concentrating device 1 is a device for concentrating the tritium concentration of sample water to be inspected containing tritium, and a plurality of electrolytic cells 3a to 3d are connected in series between the sample water container 2a and the storage water container 2b. It has the structure connected to.
  • the electrolytic cell 3 a has a circular membrane ion exchange membrane 7 in the center, and a disk-shaped anode 8 having a smaller diameter than the ion exchange membrane 7 on both sides of the ion exchange membrane 7 and A cathode 9 is disposed oppositely.
  • the ion exchange membrane 7 is composed of a solid polymer electrolyte (SPE: Solid Polymer Electrolyte) membrane having high proton conductivity.
  • SPE Solid Polymer Electrolyte
  • the anode 8 is made of DSA (Dimensionary Stable Anode), and the cathode 9 is made of various metals such as stainless steel, which are each processed into a fiber shape and then compressed into a disk shape.
  • the electrolytic cell 3a includes the inner circumferential surface of the comb packing 10, the anode block 14 partitioned by the metal block 12 and the ion exchange membrane 7, the inner circumferential surface of the comb packing 11, and the metal block 13. And the cathode chamber 15 partitioned by the ion exchange membrane 7 are formed (FIG. 1). Accordingly, the ion exchange membrane 7 is provided close to the anode chamber 14 and the cathode chamber 15, so that the anode chamber 14 and the cathode chamber 15 are separated from each other by the ion exchange membrane 7. Furthermore, the anode 8 and the cathode 9 are in close contact with the ion exchange membrane 7 in the anode chamber 14 and the cathode chamber 15, respectively.
  • Two through holes 16a and 17a are formed in the metal block 12 so as to penetrate between the inner surface 12a and the outer surface 12b on the anode 8 side, and the metal block 13 has an inner surface 13a and an outer surface 13b on the cathode 9 side.
  • Two through holes 16b and 17b are formed so as to penetrate there between.
  • Each of the through holes 16a and 17a is connected to the ends of the tubes 6a and 5a on the outer surface 12b, so that the sample water flows between the sample water container 2a and the anode chamber 14 and is generated in the anode 8. Gas can be discharged.
  • each of the through holes 16b and 17b is connected to the ends of the tubes 6b and 5b on the outer surface 13b, whereby the sample water flows between the subsequent electrolytic cell 3b and the cathode chamber 15, and the cathode 9 The generated gas can be discharged.
  • lead wires 18 and 19 for supplying power to the anode 8 and the cathode 9 are connected to the metal blocks 12 and 13, respectively.
  • a charge is supplied from the power source to the anode 8 through the lead wire 18 and the metal block 12, and a charge is supplied from the power source to the cathode 9 through the lead wire 19 and the metal block 13.
  • electrical connection is achieved between the metal block 12 and the anode 8 or between the metal block 13 and the cathode 9 by contact when the electrolytic cell 3a is assembled.
  • the metal blocks 12 and 13 do not necessarily need to be a metal, and may be comprised with the insulator which has sufficient mechanical strength.
  • the lead wires 18 and 19 extending from the power source may be directly connected to the anode 8 and the cathode 9.
  • the electrolytic cell 3a is composed of the circular ion exchange membrane 7, the anode 8, the cathode 9, the rubber packings 10 and 11, and the metal blocks 12 and 13, the shape of these members is limited to a circle. Instead, any shape such as a rectangle including a square can be selected.
  • the electrolysis cells 3b to 3d have the same structure as the electrolysis cell 3a.
  • the electrolytic cells 3a to 3d have tubes (connecting tubes) 5b, 5c, 5c, 5c, so that the through hole 17b of the cathode chamber 15 of the preceding electrolytic cell is connected to the through hole 17a of the anode chamber 14 of the subsequent electrolytic cell. They are sequentially connected by 5d.
  • the tubes 5b, 5c and 5d are made of an insulating material such as resin in order to obtain insulation between the electrolytic cells 3a to 3d.
  • the cathode chamber 15 of the last stage electrolysis cell 3d is connected to the storage water container 2b through the tube 5e.
  • DC power supplies 20a to 20d are individually connected to the anode 8 and the cathode 9 of the electrolysis cells 3a to 3d, respectively.
  • the DC power sources 20a to 20d are electrically connected to water level sensors 21 for detecting the water levels in the tubes 6a of the electrolysis cells 3a to 3d, respectively, and the sample water in the anode chambers 14 of the electrolysis cells 3a to 3d is respectively connected. It operates so as to turn on / off the power supply to the electrolysis cells 3a to 3d in accordance with the change in the water level.
  • sample water containing tritium is put into the sample water container 2a, so that sample water is put into the anode chamber 14 of the electrolytic cell 3a. Thereafter, while the water level of the sample water in the sample water container 2a exceeds the position of the water level sensor 21, electric charge is supplied from the DC power source 20a to the anode 8 and the cathode 9 of the electrolytic cell 3a, and the sample water in the electrolytic cell 3a is supplied.
  • electrolysis Specifically, hydrogen ions are generated at the same time as oxygen gas is generated in the vicinity of the anode 8, and hydrogen ions with accompanying water are leached from the anode chamber 14 toward the cathode chamber 15 through the ion exchange membrane 7. At the same time, hydrogen gas is generated in the vicinity of the cathode 9. As a result of such electrolysis, the accompanying water enriched with tritium is gradually stored in the cathode chamber 15 as stored water.
  • the stored water stored in the cathode chamber 15 of the electrolytic cell 3a in this way is introduced into the anode chamber 14 of the electrolytic cell 3b through the tube 5b. Further, when the water level in the sample water container 2a is lowered with the movement of the accompanying water and comes below the position of the water level sensor 21, the power supply from the DC power source 20a is automatically turned off, and the sample water in the electrolysis cell 3a is turned off. Electrolysis stops. On the other hand, when the level of the stored water introduced into the anode chamber 14 of the electrolysis cell 3b rises to the position of the water level sensor 21, electric charge is supplied from the DC power source 20b to the anode 8 and the cathode 9 of the electrolysis cell 3b, and the electrolysis cell 3b. Electrolysis is performed in the stored water. Thereby, the accompanying water gradually leaches out into the cathode chamber 15 of the electrolytic cell 3b.
  • sample water containing tritium was placed in the sample water container 2a and electrolysis was performed for about 80 minutes, and the tritium concentration in the anode chamber 14 was made uniform by the stirring action of oxygen gas bubbles generated in the anode chamber 14. . And 60g sample water was extract
  • the water vapor lost by the decomposition gas during this electrolysis was condensed and refluxed by a cooling pipe cooled to 0 to 1 ° C.
  • the water vapor loss amount was estimated to be 0.01 g with respect to the decomposition amount of 1 g of water.
  • each sample water was distilled and purified, and their tritium concentration [Bq / kg ⁇ 2 ⁇ ] was measured by the tritium analysis method standardized by the Ministry of Education, Culture, Sports, Science and Technology. It was. That is, the sample water A was 73 ⁇ 1, the sample water E was 74 ⁇ 1, and the sample waters B, C, and D were 95 ⁇ 2, 96 ⁇ 2, 96 ⁇ 2, respectively.
  • the sample water supplied to the anode chamber 14 of the electrolytic cell 3a is electrolyzed when the electrolytic cell 3a is supplied with power and is electrolyzed.
  • Hydrogen ions generated at the anode 8 pass through the ion exchange membrane 7 with accompanying water and are leached from the anode chamber 14 toward the cathode chamber 15.
  • decomposition of H 2 O contained in the sample water occurs preferentially with respect to decomposition of HOD and HOT (D: deuterium, T: tritium), so that the concentration of tritium in the stored water accumulated in the cathode chamber 15 is To rise.
  • this stored water is further introduced into the anode chamber 14 of the subsequent electrolysis cells 3b to 3d in order, and electrolysis of the stored water, storage of the stored water in the cathode chamber 15, and introduction of the stored water into the subsequent anode chamber 14 are performed.
  • the tritium in the sample water can be efficiently concentrated at a desired concentration rate. Further, such concentration of the sample water can be realized by a simple configuration such as a multi-stage configuration of the electrolytic cell.
  • sample water having a constant concentration ratio is generated by one leaching of the accompanying water from the anode chamber 14 to the cathode chamber 15 in the electrolysis cells 3a to 3d
  • the water retention state of the ion exchange membrane 7 can be maintained by stopping the electrolysis when the water level of the sample water remaining in the anode chambers 14 of the electrolysis cells 3a to 3d falls below the position of the water level sensor 21. .
  • FIG. 3 is a front view showing a tritium concentrator 101 according to the second embodiment of the present invention.
  • the tritium concentrator 101 is composed of a sample water container 102a, a storage water container 102b, an electrolysis cell 3, and a pump (circulation mechanism) 104.
  • the configuration of the electrolysis cell 3 is the same as the electrolysis cell 3a in the first embodiment.
  • the sample water container 102a is connected to the anode chamber 14 of the electrolytic cell 3 by two tubes 5a and 6a, and the storage water container 102b is connected to the cathode chamber 15 of the electrolytic cell 3 by two tubes 5b and 6b.
  • a DC power supply 20 is connected to the lead wires 18 and 19 of the electrolytic cell 3, and charges are supplied from the DC power supply 20 to the anode 8 and the cathode 9.
  • a water level sensor 121 provided in the middle of the tube 5a is electrically connected to the DC power source 20, and power is supplied from the DC power source 20 according to changes in the water level of the sample water in the anode chamber 14 and the sample water container 102a. It is set to be turned on / off.
  • a water absorption pipe 104a and a drain pipe 104b are attached to the pump 104, the water absorption pipe 104a is branched and connected to the tube 5b, and the drain pipe 104b is branched and connected to the tube 5a.
  • This pump 104 sends the accompanying water collected in the reservoir container 102b connected to the cathode chamber 15 to the tube 5a connected to the anode chamber 14, thereby the accompanying water generated in the cathode chamber 15 of the electrolysis cell 3 after the concentration treatment.
  • a water level sensor 122 provided in the middle of the tube 5b is electrically connected to the pump 104, and the pump 104 is started or stopped according to a change in the water level of the accompanying water accumulated in the cathode chamber 15 and the storage water container 102b. It is set to be.
  • sample water containing tritium is put into the sample water container 102a to introduce the sample water into the anode chamber 14 of the electrolytic cell 3.
  • the level of the sample water in the sample water container 102a exceeds the position of the water level sensor 121, electric charge is supplied from the DC power source 20 to the anode 8 and the cathode 9, and electrolysis occurs in the sample water.
  • the accompanying water enriched with tritium is leached into the cathode chamber 15 and stored in the storage water container 102b.
  • the power supply from the DC power source 20 is automatically turned off, and the electrolysis cell 3 Electrolysis of the sample water at is stopped.
  • the pump 104 is automatically activated by detecting the power supply OFF of the DC power supply 20, and the accompanying water stored in the storage water container 102 b is introduced into the anode chamber 14.
  • the pump 104 is automatically stopped and the circulation of the accompanying water is stopped.
  • the power supply from the DC power source 20 is turned on again, and electrolysis of the sample water in the electrolysis cell 3 is started again. Thereby, the accompanying water is leached into the cathode chamber 15 and stored in the storage water container 102b. Thereafter, power supply to the electrolysis cell 3, storage of associated water, and circulation are repeated until the water levels detected by the water level sensors 121 and 122 are both lower than the positions of both sensors.
  • the tritium in the sample water can be efficiently concentrated at a desired concentration rate by setting the sample water amount and the concentrated water amount to constant values.
  • concentration of sample water can be realized by a simple configuration of a combination of a single electrolysis cell and a circulation mechanism.
  • the measurement results when the sample water is concentrated by the tritium concentration method using the tritium concentration apparatus 101 are shown in comparison with the conventional apparatus.
  • 600 g of sample water containing tritium was put in the sample water container 102a, and the concentration process was repeatedly performed by automatic operation of the DC power source 20 and the pump 104.
  • the amount of sample water generated on the cathode chamber 15 side by the tritium concentrator 101 was 27 ⁇ 1 g, and the concentration ratio was 10.3 ⁇ 0.2 times.
  • the apparatus described in Japanese Patent No. 3748304 is used, the amount of sample water generated in the entire apparatus is 54 ⁇ 1 g, and the concentration ratio is 7.0 ⁇ 0.2 times. Met.
  • the DC power supply may be less than the number of electrolytic cells, and at least one DC power supply may be connected in parallel to a plurality of electrode cells. In this way, the number of power supplies for supplying power to each electrolytic cell can be reduced.
  • the pump 104 is set to be activated when the water level of the sample water accumulated in the cathode chamber 15 and the reservoir container 102b exceeds a certain level. It may be set to start when the water level of the sample water accumulated in the sample water container 102a falls below a certain level.
  • the DC power source 20 is set to be turned on / off according to the water level of the sample water in the anode chamber 14 and the sample water container 102a, but the sample water collected in the cathode chamber 15 and the reservoir water container 102b. It may be controlled to turn on / off according to the water level.
  • a solid polymer electrolyte membrane as the ion exchange membrane. Since such a solid polymer electrolyte membrane is a material having excellent stability, hydrogen ions generated at the anode can be stably moved.
  • the present invention uses a multi-stage tritium concentrating apparatus and a tritium concentrating method for concentrating sample water containing tritium, and efficiently increases the tritium concentration in the sample water to a desired concentration rate with a simple structure. .
  • SYMBOLS 1 Multistage-type tritium concentrator, 3, 3a-3d ... Electrolytic cell, 5b, 5c, 5d ... Tube (connection pipe), 7 ... Ion exchange membrane, 8 ... Anode, 9 ... Cathode, 14 ... Anode chamber, 15 ... Cathode chamber, 20, 20a to 20d: DC power supply.

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Abstract

La concentration de tritium dans une eau d'échantillonnage est augmentée de façon efficace à un taux de concentration souhaité par une structure simple. Un dispositif de concentration de tritium multi-étage (1) pour augmenter électrolytiquement la concentration de tritium dans de l'eau d'échantillonnage est configuré pour inclure des cellules d'électrolyse (3a à 3d) comprenant chacune une chambre anodique (14), une chambre cathodique (15), une membrane échangeuse d'ions (7) disposée près de la chambre anodique (14) et de la chambre cathodique (15), et une anode (8) et une cathode (9) qui sont disposées respectivement dans la chambre anodique (14) et la chambre cathodique (15). Les cellules d'électrolyse multiples (3a à 3d) sont couplées en série, et la chambre cathodique (15) d'une cellule d'électrolyse d'étage précédent et la chambre anodique (14) d'une cellule d'électrolyse d'étage ultérieur sont reliées par un tube (5b, 5c, 5d).
PCT/JP2009/061393 2008-06-26 2009-06-23 Dispositif de concentration de tritium multi-étages et procédé de concentration de tritium WO2009157435A1 (fr)

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JP2008-167551 2008-06-26
JP2008167551A JP2010006637A (ja) 2008-06-26 2008-06-26 多段式トリチウム濃縮装置、及びトリチウム濃縮方法

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WO2012007504A1 (fr) * 2010-07-14 2012-01-19 Qiagen Gmbh Nouveau dispositif pour le traitement des liquides
WO2014153647A1 (fr) 2013-03-29 2014-10-02 Atomic Energy Of Canada Limited Séparation électrochimique à faible énergie d'isotopes
WO2015014716A1 (fr) * 2013-07-31 2015-02-05 Industrie De Nora S.P.A. Procédé d'enrichissement électrolytique de l'eau lourde
CN106990427A (zh) * 2017-03-21 2017-07-28 榆林学院 用于检测地下水中低水平氚含量的电解装置及检测方法
US10094749B2 (en) 2010-07-14 2018-10-09 Qiagen Gmbh Storage, collection or isolation device
CN109444944A (zh) * 2018-12-21 2019-03-08 清华大学 水中氚的快速自动分析方法及装置
CN113430550A (zh) * 2021-02-24 2021-09-24 中国地质科学院水文地质环境地质研究所 一种采用不锈钢毛细管排气的电解池
CN115180670A (zh) * 2022-06-07 2022-10-14 中国地质大学（武汉） 地下水氚样多级蒸发浓缩装置及前处理方法

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KR101918087B1 (ko) 2014-08-18 2018-11-13 드 노라 페르멜렉 가부시키가이샤 트리튬수를 포함하는 원료수의 처리 방법
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Cited By (16)

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