CA1250378A - Method of removing carbon-14 from particulate, ion exchange resin - Google Patents
Method of removing carbon-14 from particulate, ion exchange resinInfo
- Publication number
- CA1250378A CA1250378A CA000472962A CA472962A CA1250378A CA 1250378 A CA1250378 A CA 1250378A CA 000472962 A CA000472962 A CA 000472962A CA 472962 A CA472962 A CA 472962A CA 1250378 A CA1250378 A CA 1250378A
- Authority
- CA
- Canada
- Prior art keywords
- carbon
- exchange resin
- barium
- ion exchange
- particulate
- 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
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/60—Cleaning or rinsing ion-exchange beds
-
- 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
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/40—Capture or disposal of greenhouse gases of CO2
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treating Waste Gases (AREA)
Abstract
TITLE
A METHOD OF REMOVING CARBON-14 FROM PARTICULATE, TON EXCHANGE
RESIN
INVENTORS
L.P. Buckley, B.L. Woods and W.J. Ward ABSTRACT
Carbon-14 is removed from particulate ion exchange resin by contacting, preferably at 70°C, a bed of the resin with a stream of air, enriched with carbon dioxide, while the particulate ion exchange resin is in contact with water to displace the carbon-14 as gaseous carbon dioxide, and then scrubbing the gaseous carbon dioxide with soluble salts of calcium or barium, e.g. calcium hydroxide and barium hydroxide, to form, as a stable, carbon-14 containing compound, either calcium carbonate or barium carbonate.
The gaseous carbon dioxide may be contacted with an aqueous solution of sodium and barium chloride to form the stable, carbon-14 containing compound which may be immobilized in cement.
A METHOD OF REMOVING CARBON-14 FROM PARTICULATE, TON EXCHANGE
RESIN
INVENTORS
L.P. Buckley, B.L. Woods and W.J. Ward ABSTRACT
Carbon-14 is removed from particulate ion exchange resin by contacting, preferably at 70°C, a bed of the resin with a stream of air, enriched with carbon dioxide, while the particulate ion exchange resin is in contact with water to displace the carbon-14 as gaseous carbon dioxide, and then scrubbing the gaseous carbon dioxide with soluble salts of calcium or barium, e.g. calcium hydroxide and barium hydroxide, to form, as a stable, carbon-14 containing compound, either calcium carbonate or barium carbonate.
The gaseous carbon dioxide may be contacted with an aqueous solution of sodium and barium chloride to form the stable, carbon-14 containing compound which may be immobilized in cement.
Description
~iO37~3 This invention relates to a method of removing carbon-14 from particulate, ion exchange resin.
Ion-exchange resins are used in heavy water moderated, natural uranium, nuclear reactors chiefly to purify the heavy water coolant and moderator systems~
These resins, stored on-site, contain about 80% of the gross ~y radioactivity produced per year in these reactors excepting the activity within the nuclear fuel bundles.
While contaminated resins make up only 3% of the total unprocessed reactor waste volume generated each year by these reactors, processing of most of the other wastcs increases this to 12%. Since these resins are contaminated with high concentrations of the long lived isotopes Cs-137 and C-14, an efficient method for their permanent disposal will be required. If the volume of these resins, produced at the rate of about 130 m3 per year, cannot be reduced, they can be expected to take up approximately 20% of the space in a reactor waste respository.
The present invention is concerned with the segregation of Carbon-14 which is present on the ion-exchange resin primarily as carbonate. Some of it is produced by neutron activation of the moderator at the rate of 440 Ci/GW(e)-year in a 540 MW~e) heavy water moderated, natural uranium, nuclear reactor. Oxidation of the carbon to CO2 by oxygen radicals formed from ~V378 radiolytie decomposition of the heavy water is the postulated mechanism. The carbon-14 is then removed from the moderator during passage of the moderator through a sidestream purification system con-taining cation-anion ion-exehange resin.
As already stated, this ion-exchange resin eontains signifieant quantities of earbon-14 (1.7 to 7.2 TB2/m ). The long half-life of this isotope (5,730 years) makes it diffieult to eonsider disposal of the ion-exchange resin eontaining this isotope in a low-level repository where the significant isotopes will be Cs-137 and Sr-90 (30-year half-life). It would be advantageous to remove the C-14 from the resin to permit volume reduction of the resin and to dispose of the C-14 in a repository as a ehemieally stable solid.
Aeeording to the present invention there is provided a method of removing earbon-14 from particulate, ion exehange resin, eomprising contacting the particulate, ion exchange resin with a stream of air, enriched with earbon dioxide, while the partieulate ion exchange resin is in eontaet with water to displaee carbon-14 from the partieulate, ion exehange resin as gaseous carbon dioxide, and then contacting the gaseous carbon dioxide thus formed with at least one absorbent substance selected from the group consisting of water soluble salts of calcium and barium to form as a chemically stable, carbon-14 containing compound, a carbonate of calcium if calcium is present in the absorbant substance, and barium if barium is present in the absorbent substance.
In some embodiments of the present invention the absorbent is at least one substance selected from the group consisting of calcium hydroxide and barium hydroxide.
In other embodiments of the present invention the absorbent substance is an aqueous solution of sodium hydroxide and barium chloride.
Preferably the ion exchange resin is contacted with the air, enriched with carbon dioxide, at about 70C.
The chemically stable, carbon-14 containing compound is preferably immobilized in cement.
In the accompanying drawings, Figure 1 is a diagrammatic view of an apparatus used to verify the present invention, and Figure 2 is a graph showing the amount of C-14 released plotted against time,for scrubber solutions produced in the apparatus shown in Figure 1 and immobilized in various substances.
Referring now to Figure 1, there is shown a
Ion-exchange resins are used in heavy water moderated, natural uranium, nuclear reactors chiefly to purify the heavy water coolant and moderator systems~
These resins, stored on-site, contain about 80% of the gross ~y radioactivity produced per year in these reactors excepting the activity within the nuclear fuel bundles.
While contaminated resins make up only 3% of the total unprocessed reactor waste volume generated each year by these reactors, processing of most of the other wastcs increases this to 12%. Since these resins are contaminated with high concentrations of the long lived isotopes Cs-137 and C-14, an efficient method for their permanent disposal will be required. If the volume of these resins, produced at the rate of about 130 m3 per year, cannot be reduced, they can be expected to take up approximately 20% of the space in a reactor waste respository.
The present invention is concerned with the segregation of Carbon-14 which is present on the ion-exchange resin primarily as carbonate. Some of it is produced by neutron activation of the moderator at the rate of 440 Ci/GW(e)-year in a 540 MW~e) heavy water moderated, natural uranium, nuclear reactor. Oxidation of the carbon to CO2 by oxygen radicals formed from ~V378 radiolytie decomposition of the heavy water is the postulated mechanism. The carbon-14 is then removed from the moderator during passage of the moderator through a sidestream purification system con-taining cation-anion ion-exehange resin.
As already stated, this ion-exchange resin eontains signifieant quantities of earbon-14 (1.7 to 7.2 TB2/m ). The long half-life of this isotope (5,730 years) makes it diffieult to eonsider disposal of the ion-exchange resin eontaining this isotope in a low-level repository where the significant isotopes will be Cs-137 and Sr-90 (30-year half-life). It would be advantageous to remove the C-14 from the resin to permit volume reduction of the resin and to dispose of the C-14 in a repository as a ehemieally stable solid.
Aeeording to the present invention there is provided a method of removing earbon-14 from particulate, ion exehange resin, eomprising contacting the particulate, ion exchange resin with a stream of air, enriched with earbon dioxide, while the partieulate ion exchange resin is in eontaet with water to displaee carbon-14 from the partieulate, ion exehange resin as gaseous carbon dioxide, and then contacting the gaseous carbon dioxide thus formed with at least one absorbent substance selected from the group consisting of water soluble salts of calcium and barium to form as a chemically stable, carbon-14 containing compound, a carbonate of calcium if calcium is present in the absorbant substance, and barium if barium is present in the absorbent substance.
In some embodiments of the present invention the absorbent is at least one substance selected from the group consisting of calcium hydroxide and barium hydroxide.
In other embodiments of the present invention the absorbent substance is an aqueous solution of sodium hydroxide and barium chloride.
Preferably the ion exchange resin is contacted with the air, enriched with carbon dioxide, at about 70C.
The chemically stable, carbon-14 containing compound is preferably immobilized in cement.
In the accompanying drawings, Figure 1 is a diagrammatic view of an apparatus used to verify the present invention, and Figure 2 is a graph showing the amount of C-14 released plotted against time,for scrubber solutions produced in the apparatus shown in Figure 1 and immobilized in various substances.
Referring now to Figure 1, there is shown a
2.5 cm. internal diameter stainless steel column 1, having a stainless steel screen 2, has an air inlet 4 connected to a pipe 6 and an air outlet 8 connected to a pipe 10, an electrical heating coil 12 is disposed around the column 1.
The pipe 6 has two branches 14 and 16. The branch 14 is for connection to an air supply (not shown~ via a flow meter 18 and valve 20. The branch 16 is for connection to a gaseous CO2 supply (not shown) via a flow meter 22 and a valve 24.
The pipe 10 is connected to three off-gas scrubbers 26 to 28 arranged in series flow. An outlet 30 from scrubber 28 is for connection to a vacuum pump (not shown) which delivers any air therefrom to an exhaust fume hood (not shown).
Organic mixed-bed ion-exchange resins are commonly used in heavy water moderated, natural uranium, nuclear reactors: Amberlite IRN-150 (trademark) is used in the moderator system and Amberlite IRN-154 (trademark) is used in the primary heat transport system from the heavy water moderated, natural uranium, nuclear reactor generating station of Pickering, Ontario, Canada. Both of these amberlite resins are obtainable from Rohm & Haas Co., Philadelphia, PA, USA. The major contaminants on the resins are C-14 and Cs-137, respectively. As well as being present in high concentrations, the Cs-137 and especially the C-14 are, as already stated, long-lived species and must be contained for long periods of time.
~2~ 3'~
In experiments to confirm the present invention, Amberlite IRN-150 resin, traced with C-14 was used.
The column 1 was filled with a bed 32 of 45 g of dewatered, C-14 traced, Amberlite IRN-150 resin in particulate form. The resin 32 was supported on the stainless steel screen 2. The pipe 14 was connected to an air source (not shown)~ the pipe 16 was connected to a gaseous CO2 source (not shown) and the outlet was connected to a vacuum pump (not shown). The scrubbers 26 to 28 were filled with 200 mL of 2 kmol/m3 NaOH and 0.4 kmol/m BaC12.
In operation, a stream of air enriched with C2 was drawn by vacuum along the pipe 6 and through the bed 32 of C-14 traced, Amberlite IRN-150 designated 32 with the bed 32 heated to 25C or 75C by the heater 12.
The following Table 1 gives the results of different experiments.
~ZS;~78 THE EFFECT OF CARBON DIOXIDE TO DISPLACE
C-14 FROM ION-EXCI~NGE RESIN
Experiment Time of C2 in Velocity Temperature C-14 Removal Number Exposure Contacting of Gas of Resin Red Efficiency to Gas Gas Stream Stream h mL/s C %
1 2 O 2.5 25 0.05 2 2 10 2.5 25 21.8
The pipe 6 has two branches 14 and 16. The branch 14 is for connection to an air supply (not shown~ via a flow meter 18 and valve 20. The branch 16 is for connection to a gaseous CO2 supply (not shown) via a flow meter 22 and a valve 24.
The pipe 10 is connected to three off-gas scrubbers 26 to 28 arranged in series flow. An outlet 30 from scrubber 28 is for connection to a vacuum pump (not shown) which delivers any air therefrom to an exhaust fume hood (not shown).
Organic mixed-bed ion-exchange resins are commonly used in heavy water moderated, natural uranium, nuclear reactors: Amberlite IRN-150 (trademark) is used in the moderator system and Amberlite IRN-154 (trademark) is used in the primary heat transport system from the heavy water moderated, natural uranium, nuclear reactor generating station of Pickering, Ontario, Canada. Both of these amberlite resins are obtainable from Rohm & Haas Co., Philadelphia, PA, USA. The major contaminants on the resins are C-14 and Cs-137, respectively. As well as being present in high concentrations, the Cs-137 and especially the C-14 are, as already stated, long-lived species and must be contained for long periods of time.
~2~ 3'~
In experiments to confirm the present invention, Amberlite IRN-150 resin, traced with C-14 was used.
The column 1 was filled with a bed 32 of 45 g of dewatered, C-14 traced, Amberlite IRN-150 resin in particulate form. The resin 32 was supported on the stainless steel screen 2. The pipe 14 was connected to an air source (not shown)~ the pipe 16 was connected to a gaseous CO2 source (not shown) and the outlet was connected to a vacuum pump (not shown). The scrubbers 26 to 28 were filled with 200 mL of 2 kmol/m3 NaOH and 0.4 kmol/m BaC12.
In operation, a stream of air enriched with C2 was drawn by vacuum along the pipe 6 and through the bed 32 of C-14 traced, Amberlite IRN-150 designated 32 with the bed 32 heated to 25C or 75C by the heater 12.
The following Table 1 gives the results of different experiments.
~ZS;~78 THE EFFECT OF CARBON DIOXIDE TO DISPLACE
C-14 FROM ION-EXCI~NGE RESIN
Experiment Time of C2 in Velocity Temperature C-14 Removal Number Exposure Contacting of Gas of Resin Red Efficiency to Gas Gas Stream Stream h mL/s C %
1 2 O 2.5 25 0.05 2 2 10 2.5 25 21.8
3 4 10 2.5 25 25.8
4 2 50 2.5 25 26.5 2 100 2.5 25 11.0 6 2 10 12,5 25 54.4 7 2 10 25.0 25 7.8 8 2 O 2.5 70 0.06 9 2 10 2.5 70 101.2 l 10 ~.~ 70 62.6 It will be seen from the results in Table 1 that about 22% of the C-14 initially present on the resin was liberated by passing air, with 10 vol % CO2, over the resin at 2.5 mL/s for 2 hours at 25 C. The release of C-14 was not affected by increasing the time of exposure of the resin to the air stream, or the volume fraction of CO2 in the air stream. However, at increased temperatures, release of C-14 was enhanced such that at about 70C, 100% of the C-14 was liberated in 2 hours. It was found that if resins )3~8 are dried by passing air over the resins for 2 hours at about 70C, no C-14 is released when CO2 is contacted with the resins, suggesting that the presence of H2O is important in the mechanism for release of C-14. The mechanism for release of C-14 can probably be explained on the basis of the hydration, exchange and dehydration reactions described in "Advanced Inorganic Chemistry", 3rd Edition, F.A. Cotton and G. Wilkinson, Interscience Publishers, Toronto, 1972, p. 297, and given below.
C2 + H20 _ H2C03 (1) (RzNR3)2 CO3 + H2C3 ~ ~ (RZNR3)2co3+H2 C3 (2) H2 CO3 ~ ~ 14co2 + H2O (3) The simple step of con-tacting C-14 contaminated resins with air and CO2, preferably at about 70C, accord-ing to the present invention, can be used to recover C-14 from the resins before the resins are incinerated or vitrified. Ash from incinerated resin may be immobilized in cement, polyester, bitumen, glass and glass-ceramic compositions.
The C-14-contaminated scrubber solutions must be immobilized and disposed of. Barium carbonate waste slurries result if C-14-contaminated NaOH scrubbing solutions are treated with soluble salts of barium or if Ba(OH)2 solid sorbents are used to trap C-14. To evaluate 3 f ~
possible materials for disposal of these scrubber solutions, slurries of 50 wt% barium carbonate traced with 6 GBq/L of C-14 were immobilized in cement, polyester and bitumen.
The cement, polyester and bitumen products were leached to measure C-14 releases. Details of the products and leaching experiment are given in the following Table 2 and in Figure 2.
IMMOBILIZATION MATRIX .
Speclmen Description Portland l'olyester Resin Oxidized Type III Ashland WEP-661-P Bitumen, Type Cement SP-170 .
Matrix Material, wt% 60.0 50.0 60.0 Dry Amberlite IRN-150, wt~ 10.0 12 5 40.0 Water Content, wt% 30.0 37.5 <0.5 Sample Weight, g 81.6 43.4 51.2 Sample Volume, mL 41.4 36.6 37.7 Surface Area Exposed to Leachant, cm2 67.4 61.6 62 3 Initial Cs-14 Activity, MBq, in Specimen 96 9 64.0 233.0 Volume of Leachant, mL 250 260 260 l Ci = 37 GBq.
~378 In Figure 2 leaching time (LT) in days is plotted against cumulative fraction leached (CFL) in centi-meters, from immobilized barium carbonate slurry, and ~ designates a 12 weight % slurry immobilized in poly~ster, q designates a 10 weight % slurry immobilized in bitumen, and o designates a 10 weight % slurry immobilized in cement.
As illustrated in Figure ~ releases of C-14, 10 cm in 120 days, were lowest for the cement products.
Releases from the bitumen and polyester products were 2 and 20 times higher at 120 days after leaching started.
Since Ba(OH)2 in C-14 off-gas scrubbers will not be completely converted to BaCO3, the effects of incorporating Ba(OH)2 in cement were examined. A slurry, 50 wt~ water using a solid phase of 30 wt% BaCO3 and 70 wt% Ba(OH)2 traced with 6 GBq/L of C-14, was immobilized in cement and leached to measure C-14 releases. After 30 days of leachings, the C-14 releases were the same as those illustrated in Fig. 2 for the BaCO3 products.
Unsuccessful attempts were made to incorporate BaCO3 into boro-silicate glass. Even at low loadings of BaCO3, 5 wt~, the BaCO3 formed a separate phase on the top of the glass.
C2 + H20 _ H2C03 (1) (RzNR3)2 CO3 + H2C3 ~ ~ (RZNR3)2co3+H2 C3 (2) H2 CO3 ~ ~ 14co2 + H2O (3) The simple step of con-tacting C-14 contaminated resins with air and CO2, preferably at about 70C, accord-ing to the present invention, can be used to recover C-14 from the resins before the resins are incinerated or vitrified. Ash from incinerated resin may be immobilized in cement, polyester, bitumen, glass and glass-ceramic compositions.
The C-14-contaminated scrubber solutions must be immobilized and disposed of. Barium carbonate waste slurries result if C-14-contaminated NaOH scrubbing solutions are treated with soluble salts of barium or if Ba(OH)2 solid sorbents are used to trap C-14. To evaluate 3 f ~
possible materials for disposal of these scrubber solutions, slurries of 50 wt% barium carbonate traced with 6 GBq/L of C-14 were immobilized in cement, polyester and bitumen.
The cement, polyester and bitumen products were leached to measure C-14 releases. Details of the products and leaching experiment are given in the following Table 2 and in Figure 2.
IMMOBILIZATION MATRIX .
Speclmen Description Portland l'olyester Resin Oxidized Type III Ashland WEP-661-P Bitumen, Type Cement SP-170 .
Matrix Material, wt% 60.0 50.0 60.0 Dry Amberlite IRN-150, wt~ 10.0 12 5 40.0 Water Content, wt% 30.0 37.5 <0.5 Sample Weight, g 81.6 43.4 51.2 Sample Volume, mL 41.4 36.6 37.7 Surface Area Exposed to Leachant, cm2 67.4 61.6 62 3 Initial Cs-14 Activity, MBq, in Specimen 96 9 64.0 233.0 Volume of Leachant, mL 250 260 260 l Ci = 37 GBq.
~378 In Figure 2 leaching time (LT) in days is plotted against cumulative fraction leached (CFL) in centi-meters, from immobilized barium carbonate slurry, and ~ designates a 12 weight % slurry immobilized in poly~ster, q designates a 10 weight % slurry immobilized in bitumen, and o designates a 10 weight % slurry immobilized in cement.
As illustrated in Figure ~ releases of C-14, 10 cm in 120 days, were lowest for the cement products.
Releases from the bitumen and polyester products were 2 and 20 times higher at 120 days after leaching started.
Since Ba(OH)2 in C-14 off-gas scrubbers will not be completely converted to BaCO3, the effects of incorporating Ba(OH)2 in cement were examined. A slurry, 50 wt~ water using a solid phase of 30 wt% BaCO3 and 70 wt% Ba(OH)2 traced with 6 GBq/L of C-14, was immobilized in cement and leached to measure C-14 releases. After 30 days of leachings, the C-14 releases were the same as those illustrated in Fig. 2 for the BaCO3 products.
Unsuccessful attempts were made to incorporate BaCO3 into boro-silicate glass. Even at low loadings of BaCO3, 5 wt~, the BaCO3 formed a separate phase on the top of the glass.
Claims (5)
1. A method of removing carbon-14 from particulate, ion exchange resin, comprising: contacting the particulate ion exchange resin with air, enriched with carbon dioxide, while the particulate ion exchange resin is in contact with water to displace carbon-14 from the particulate, ion exchange resin as gaseous carbon dioxide, and then contacting the gaseous carbon dioxide thus formed with at least one absorbent substance selected from the group consisting of water soluble salts of calcium and barium to form as a chemically stable, carbon-14 containing compound, a carbonate of calcium if calcium is present in the absorbant substance, and barium if barium is present in the absorbant substance.
2. A method according to claim 1, wherein the absorbent is at least one substance selected from the group consisting of calcium hydroxide and barium hydroxide.
3. A method according to claim 1, wherein the absorbent substance is an aqueous solution of sodium hydroxide and barium chloride.
4. A method according to claim 1, wherein the ion exchange resin is contacted with the air, enriched with carbon dioxide, at about 70°C.
5. A method according to claim 1, wherein the chemically stable, carbon-14 containing compound is immobilized in cement.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000472962A CA1250378A (en) | 1985-01-28 | 1985-01-28 | Method of removing carbon-14 from particulate, ion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000472962A CA1250378A (en) | 1985-01-28 | 1985-01-28 | Method of removing carbon-14 from particulate, ion exchange resin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1250378A true CA1250378A (en) | 1989-02-21 |
Family
ID=4129689
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000472962A Expired CA1250378A (en) | 1985-01-28 | 1985-01-28 | Method of removing carbon-14 from particulate, ion exchange resin |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1250378A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10163536B2 (en) | 2014-11-19 | 2018-12-25 | Framatome Gmbh | Method and apparatus for recovery of radioactive nuclides from spent resin materials |
-
1985
- 1985-01-28 CA CA000472962A patent/CA1250378A/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10163536B2 (en) | 2014-11-19 | 2018-12-25 | Framatome Gmbh | Method and apparatus for recovery of radioactive nuclides from spent resin materials |
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Effective date: 20060221 |