LT4725B - Sorbent for iodine and method for the preparation thereof - Google Patents
Sorbent for iodine and method for the preparation thereof Download PDFInfo
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- LT4725B LT4725B LT2000013A LT2000013A LT4725B LT 4725 B LT4725 B LT 4725B LT 2000013 A LT2000013 A LT 2000013A LT 2000013 A LT2000013 A LT 2000013A LT 4725 B LT4725 B LT 4725B
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- iodine
- sorbent
- activated carbon
- pdmdaaj
- solution
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 36
- 239000011630 iodine Substances 0.000 title claims abstract description 36
- 239000002594 sorbent Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229940107816 ammonium iodide Drugs 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 14
- XZXYQEHISUMZAT-UHFFFAOYSA-N 2-[(2-hydroxy-5-methylphenyl)methyl]-4-methylphenol Chemical compound CC1=CC=C(O)C(CC=2C(=CC=C(C)C=2)O)=C1 XZXYQEHISUMZAT-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000002657 fibrous material Substances 0.000 claims 1
- 239000008187 granular material Substances 0.000 claims 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- 239000006096 absorbing agent Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000002250 absorbent Substances 0.000 abstract 3
- 230000002745 absorbent Effects 0.000 abstract 3
- 229910052799 carbon Inorganic materials 0.000 abstract 3
- -1 diallyl ammonium iodide Chemical compound 0.000 abstract 2
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 description 20
- 239000000370 acceptor Substances 0.000 description 8
- 238000001179 sorption measurement Methods 0.000 description 6
- 238000010335 hydrothermal treatment Methods 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- LPSCRKGVODJZIB-UHFFFAOYSA-N [I].[C] Chemical class [I].[C] LPSCRKGVODJZIB-UHFFFAOYSA-N 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000010299 hexamethylene tetramine Nutrition 0.000 description 1
- 239000004312 hexamethylene tetramine Substances 0.000 description 1
- 229910001511 metal iodide Inorganic materials 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
Description
Išradimas priklauso chemijos inžinerijos sričiai ir gali būti panaudotas specialiose jodo surišimo ir nukenksminimo technologijose. Tame tarpe šalinant jį iš dujų ar oro išlakų srauto absorberiuose.The invention relates to the field of chemical engineering and can be used in special iodine-binding and decontamination technologies. This includes removing it from the gas or air stream in the absorbers.
Žinoma, kad jodo surišimui išlakose naudojamos aktyvintos anglys [žr. kn.: Filterung von Abluft aus Kemtechnischen Anlagen und Isotopenlaboratorien/ vonActivated charcoal is known to bind iodine in emissions [cf. kn .: Filtering from Abluft aus Kemtechnischen Anlagen und Isotopenlaboratorien / von
J.G.Wilhelm. Schriftenreihe Reaktorsicherheit und Strahlenschutz.-BMU, 1998, 376 s.; Ta300HHCTKa h κοΗτροπΒ ra3OBbix BBidpocoB A3C/ H.E.HaxyTHH, /TB.Oukhh, H.M.CMnpHOBa h /ip..- M.: SHepro- aioMinaai, 1983.-24 c.]. Jodo sorbcijai padidinti aktyvintos anglys yra impregnuojamos įvairiomis vandenyje tirpiomis organinėmis ir neorganinėmis medžiagomis: heksametilentetraminu [žr. TS: TY 6-16-3028-87], trietilendiaminu [žr. kn.: Ta3oomiCTKa h KOHTporib ra30Bbix BbiopocoB A3C/ H.E.HaxyniH, JĮ.B.Oukhh, H.M.CMnpHOBa n ap..- M.: 3HeproaTOMii3^aT, 1983.-24 c.], metalų jodidais [žr. kn. H.Deubner, K.Gerlach. Parametrische Untersuchungen zur Abscheidung von Methljodid an einer KJimpemierten Aktivkohle KfK 3746, Forschungscentrum Karlsruhe, 1984 ir TS: TYJ. G. Wilhelm. Schriftenreihe Reaktorsicherheit und Strahlenschutz.-BMU, 1998, 376 s .; Ta300HHCTKa h κοΗτροπΒ ra3OBbix BBidpocoB A3C / H.E.HaxyTHH, /TB.Oukhh, H.M.CMnpHOBa h /ip..- M.: SHeproaioMinaai, 1983- 24 c.]. Activated carbon is impregnated with a variety of water-soluble organic and inorganic materials, hexamethylenetetramine, to increase the sorption of iodine. TS: TY 6-16-3028-87], triethylenediamine [cf. kn .: Ta3oomiCTKa h KOHTporib ra30Bbix BbiopocoB A3C / H.E.HaxyniH, J.B.Oukhh, H.M.CMnpHOBa n ap ..- M.: 3HeproaTOMii3 ^ aT, 1983.-24c.], metal iodides [see. kn. H.Deubner, K.Gerlach. Parametrische Untersuchungen zur Abscheidung von Methljodid an einer KJimpemierten Aktivkohle KfK 3746, Forschungscentrum Karlsruhe, 1984 and TS: TY
6-16-3028-87], sidabro nitratu.6-16-3028-87], silver nitrate.
Jų trūkumas tas, kad heksametilentetraminas ir trietilendiaminas yra toksiški ir degūs junginiai [žr. kn.: npeųenbHO aonycTHMbie KOHueHTpamm XHMHHecKHX BeiųecTB b OKpy/Kaiomeii cpene/ Γ.Ε. EecnaMHTHiiKOBa, K).A. ΚροτοΒ.-Jl: Χημηλ, 1985]. Į tai būtina atsižvelgti jodo absorberių eksploatavimo metu, ypač jų įkrovimo metu.Their disadvantage is that hexamethylenetetramine and triethylenediamine are toxic and flammable compounds [cf. kn .: npeøenbHO aonycTHMbie KOHueHTpamm XHMHHecKHX BeiųecTB b OKpy / Kaiomeii cpene / Γ.Ε. EecnaMHTHiiKOBa, K) .A. ΚροτοΒ.-Jl: Χημηλ, 1985]. This must be taken into account during operation of the iodine absorbers, especially during charging.
Dažniausiai naudojami netoksiški metalų jodidai. Žinomas mažai tirpus, bet intensyviai sorbuojantis jodą nedegus ir netoksiškas polimeras polidimetildialilamonio jodidas (PDMDAAJ) [žr. Lietuvos pat. Nr. 4497, TPK C08F 126/02,1999]. 20 °C temperatūros vandenyje PDMDAAJ ištirpsta 0,5 g/l, 95 °C - 65 g/l. Taigi ir PDMDAAJ tirpumas vandenyje esant aukštesnei temperatūrai gerokai padidėja.Non-toxic metal iodides are commonly used. Poly (dimethyldiallyl) ammonium iodide (PDMDAAJ), a low-soluble but high-sorption iodine non-flammable and non-toxic polymer, is known. Lithuanian Pat. No. 4497, TPK C08F 126 / 02,1999]. In 20 ° C water, PDMDAAJ dissolves in 0.5 g / l, 95 ° C - 65 g / l. Thus, the solubility of PDMDAAJ in water at elevated temperatures is also significantly increased.
Esminis visų aukščiau paminėtų jodo sorbentų trūkumas - mažas atsparumas hidroterminiams poveikiams dėl naudojamų jodo akceptorių tirpumo vandenyje. Su išlakomis į absorberį patekus garams ar kitaip padidėjus išlakų drėgmei ir temperatūrai jodo akceptoriai gali migruoti ir kondensaciniu vandeniu būti išplauti iš aktyvintų anglių.A major disadvantage of all of the above iodine sorbents is the low resistance to hydrothermal effects due to the water solubility of the iodine acceptors used. When vapors get into the absorber or other humidity and temperature rise, the iodine acceptors can migrate and be washed off with activated water from the condensing water.
Artimiausias pateiktam išradimui yra praktikoje naudojamos kalio jodidu (KI) impregnuotos aktyvintos anglys [žr. TS: ΊΎ 6-16-3028-87 ir kn.: Filterung von Abluft aus Kemtechnischen Anlagen und Isotopenlaboratorien/ von J.GAVilhelm. Schriftenreihe Reaktorsicherheit und Strahlenschutz.-BMU, 1998, 376 s]. Kalio jodido kiekis sorbente sudaro 1-2% .Closest to the present invention are potassium iodide (KI) impregnated activated carbon for use in practice. TS: ΊΎ 6-16-3028-87 et al .: Filterung von Abluft aus Kemtechnischen Anlagen und Isotopenlaboratorien / von J.Gavilhelm. Schriftenreihe Reaktorsicherheit und Strahlenschutz.-BMU, 1998, 376 s]. Potassium iodide content in sorbent is 1-2%.
Šio išradimo tikslas - gauti jodo sorbentą, kuris yra atsparesnis hidroterminiam poveikiui, t.y. daugkartinių apdorojimų karštu (85-95 °C temperatūros) vandeniu metu jodo akceptorius neišplaunamas. Tokiu jodo akceptoriumi yra imobilizuotas aktyvintoje anglyje polidimetildialilamonio jodidas.It is an object of the present invention to provide an iodine sorbent which is more resistant to hydrothermal effects, i. multiple treatments with hot (85-95 ° C) water do not wash the iodine acceptor. Such an iodine acceptor is immobilized on activated carbon polydimethyldiallyl ammonium iodide.
Šis tikslas pasiekiamas impregnavus aktyvintas anglis vandeniniu 1 - 4 % PDMDAAJ tirpalu ir išdžiovinus. Tokiu būdu gautas granuliuotų impregnuotų aktyvintų anglių jodo sorbentas turi nuo 1 iki 4 % jodo akceptoriaus, pluoštinis impregnuotų aktyvintų anglių jodo sorbentas - 5 % PDMDAAJ.This objective is achieved by impregnating the activated carbon with an aqueous solution of 1-4% PDMDAAJ and drying. The thus obtained granular impregnated activated carbon iodine sorbent has from 1 to 4% iodine acceptor and the fibrous impregnated activated carbon iodine sorbent contains 5% PDMDAAJ.
1-oje lentelėje pateikiami duomenys apie įvairius jodo sorbentus, 2-oje lentelėje - duomenys pagal kuriuos palygintas jodo sorbentų, gautų pagal prototipą ir pagal siūlomą būdą, hidroterminis atsparumas. Kaip matyti iš 1 lentelėje pateiktų duomenų, jodo akceptoriai padidina jodo surišimą impregnuotomis aktyvintomis anglimis. Impregnuotų aktyvintų anglių jodo sorbcinė galia priklauso nuo naudojamų aktyvintų anglių impregnavimui, akceptoriaus ir jo kiekio sorbente. Imobilizavus aktyvintose anglyse tokį pat PDMDAAJ kiekį kaip naudoto prototipe kalio jodido (1 lentelė, Nr. 2, 3), jos sorbcinės savybės pagerėja. Impregnuotų PDMDAAJ aktyvintų anglių sorbcinė galia didėja didėjant PDMDAAJ kiekiui sorbente (1 lentelė, Nr. 3-5). Tačiau impregnuoti aktyvintas anglis didesnės koncentracijos PDMDAAJ tirpalais negalime dėl riboto polimero tirpumo vandenyje) [žr. Lietuvos pat. Nr. 4497, TPK C08F,1999j. Pluoštinių aktyvintų anglių jodo sorbcinė galia dėl didesnio jų aktyvaus paviršiaus yra didesnė už granuliuotų. Jas apdorojus PDMDAAJ tirpalu (1 lentelė, Nr. 7) gaunamas didesnės sorbcinės galios jodo sorbentas.Table 1 provides data on various iodine sorbents, and Table 2 compares the hydrothermal resistance of iodine sorbents obtained by the prototype and the proposed process. As can be seen from the data in Table 1, iodine acceptors increase iodine binding by impregnated activated carbon. The sorption power of the impregnated activated carbon iodine depends on the activated carbon used for impregnation, the acceptor and its content in the sorbent. Immobilization of activated carbon on the same amount of PDMDAAJ as the prototype used potassium iodide (Table 1, Nos. 2, 3) improves its sorption properties. The sorption power of impregnated PDMDAAJ-activated carbons increases with increasing PDMDAAJ content in the sorbent (Table 1, # 3-5). However, we cannot impregnate activated carbon with higher concentrations of PDMDAAJ solutions due to the limited water solubility of the polymer). Lithuanian Pat. No. 4497, TPK C08F, 1999j. The fibrous activated carbon has a higher iodine sorption capacity due to its higher active surface area than granular. They are treated with PDMDAAJ solution (Table 1, # 7) to obtain a higher sorption power iodine sorbent.
Atsparūs hidroterminiam apdorojimui jodo sorbentai gaunami tik pagal siūlomą būdą (2 lentelė). Dešimties hidroterminio apdorojimo ciklų metu iš jodo sorbento pagal prototipą pašalinami 94% jame buvusio kalio jodido, kai tokių pat apdorojimų metu iš impregnuotų pagal siūlomą būdą pavyzdžių pavyksta išplauti tik nedidelę dalį nesurišto polimerinio jodo akceptoriaus.Resistant to hydrothermal treatment, iodine sorbents are obtained only according to the proposed process (Table 2). During ten hydrothermal treatment cycles, 94% of the potassium iodide present in the iodine sorbent is removed from the prototype, while only a small fraction of unbound polymeric iodine acceptor is leached from the impregnated samples in the same process.
Jodo sorbentų hidroterminio atsparumo nustatymas atliekamas 20 g sorbento, pagaminto pagal 1 - 4 pavyzdį, užpilant lOOg 90-95 °C distiliuoto vandens ir išlaikant 10 min. Nudekantavus vandenį operacija kartojama iki 10 kartų.The determination of the hydrothermal resistance of iodine sorbents is carried out by adding 20 g of sorbent prepared according to Examples 1-4 to 100 g of 90-95 ° C distilled water and holding for 10 minutes. After trapping water, the operation is repeated up to 10 times.
Išradimas iliustruojamas pateiktais pavyzdžiais:The invention is illustrated by the following examples:
pavyzdysexample
Paruošia lOOOg 1%-tinio PDMDAAJ tirpalą, 990 ml vandens ištirpinant lOg PDMDAAJ. Į paruoštą tirpalą prideda 500g granuliuotų aktyvintų anglių (TU 6-162727-84). Po 20 min tirpalą nusiurbia. Drėgnų granulių priesvoris 100%. Jas paskleidžia plonu sluoksniu ir išdžiovina konvekcinėje džiovykloje, esant 90 - 105 °C temperatūrai. Gaunamas jodo sorbentas, turintis 1% PDMDAAJ. Statinėmis sąlygomis iš oro jis suriša 22mg L·/ lg sorbento (1 lentelė, Nr 3). Po 10 hidroterminio apdorojimo ciklų lieka 0,75% PDMDAAJ nuo sorbento masės (2 lentelė).Prepare lOOOg 1% PDMDAAJ by dissolving 990 mL of water in 10O PDMDAAJ. Add 500g of granular activated carbon (TU 6-162727-84) to the prepared solution. After 20 min, remove the solution. Weight of wet pellets 100%. They are spread in a thin layer and dried in a convection dryer at 90 - 105 ° C. An iodine sorbent containing 1% PDMDAAJ is obtained. Under static conditions, it binds 22mg L · / lg of sorbent from air (Table 1, No 3). After 10 cycles of hydrothermal treatment, 0.75% PDMDAAJ remains on the sorbent mass (Table 2).
pavyzdysexample
Impregnavimą atlieka pagal 1 pavyzdį, tik vietoj 1%-tinio PDMDAAJ tirpalo naudoja 2%-tinį PDMDAAJ tirpalą. Gaunamas jodo sorbentas turintis 2%The impregnation is carried out according to Example 1, but uses only 2% PDMDAAJ solution instead of 1% PDMDAAJ solution. Obtained 2% iodine sorbent
PDADMAJ. Statinėmis sąlygomis iš oro jis suriša 33mg I2/ lg sorbento, dinaminėmis - 90mg I2/ lg sorbento (1 lentelė, Nr 4).PDADMAJ. Under static conditions in air it binds 33 mg I 2 / lg resin, dynamic - 90mg 2 / lg resin (Table 1, No. 4).
pavyzdysexample
Impregnavimą atlieka pagal 1 pavyzdį, tik vietoj 1%-tinio PDMDAAJ tirpalo naudoja 4%-tinį PDMDAAJ tirpalas. Gaunama? jodo sorbentas turintis 4% PDADMAJ. Statinėmis sąlygomis iš oro jis suriša 41mg I2/ lg sorbento (1 lentelė, Nr 5). Po 10 hidroterminio apdorojimo ciklų lieka 2,94% PDMDAAJ nuo sorbento masės (2 lentelė).The impregnation is performed according to Example 1, only 4% PDMDAAJ solution is used instead of 1% PDMDAAJ solution. Incoming? iodine sorbent containing 4% PDADMAJ. Under static conditions, it binds 41mg I 2 / lg of sorbent from air (Table 1, No. 5). After 10 cycles of hydrothermal treatment, 2.94% PDMDAAJ remains on the sorbent mass (Table 2).
pavyzdys lOOOg 1%-tinio PDMDAAJ tirpalo paruošia pagal 1 pavyzdį. Į paruoštą tirpalą įmerkia 150g pluoštinių aktyvintų anglių. Po 20 min tirpalą nusiurbia. Drėgnų pluoštinių anglių priesvoris 500%. Drėgnas pluoštines anglis išdžiovina konvekcinėje džiovykloje, esant 90 - 105 °C temperatūrai. Gaunamas jodo sorbentas, turintis 5% PDMDAAJ. Statinėmis sąlygomis iš oro jis suriša 154mg I2/ lg sorbento, dinaminėmis - 450mg I2/ lg sorbento (1 lentelė, Nr 4).Example 10000g of 1% PDMDAAJ solution is prepared according to Example 1. Immerse 150 g of activated carbon in the prepared solution. After 20 min, remove the solution. Weight of wet fibrous coal 500%. The wet fibrous charcoal is dried in a convection dryer at 90 to 105 ° C. An iodine sorbent containing 5% PDMDAAJ is obtained. Under static conditions in air, and bound 154mg 2 / lg resin, dynamic - 450 mg I 2 / lg resin (Table 1, No. 4).
pavyzdysexample
Paruošia lOOOg 1%-tinio kalio jodido tirpalo, ištirpinant lOg KI (GOST 4232-74) 990 ml vandens. Į jį suberia 500g granuliuotų aktyvintų anglių. Po 20 min tirpalas nusiurbia. Drėgnų granulių priesvoris 100%. Jas paskleidžia plonu sluoksniu ir išdžiovina konvekcinėje džiovykloje, esant 90 - 105 °C temperatūrai. Gaunamas jodo sorbentas, turintis 1% KI. Statinėmis sąlygomis iš oro jis suriša 21mg I2/ lg sorbento (1 lentelė, Nr 2). Po 10 hidroterminio apdorojimo ciklų lieka 0,06% kalio jodido nuo sorbento masės (2 lentelė).Prepare lOOOg 1% potassium iodide solution by dissolving lOg KI (GOST 4232-74) in 990 mL water. 500g of granulated activated carbon is added to it. After 20 min, the solution is suctioned off. Weight of wet pellets 100%. They are spread in a thin layer and dried in a convection dryer at 90 - 105 ° C. Obtained iodine sorbent with 1% CI. Under static conditions, it binds 21mg I 2 / lg of sorbent from air (Table 1, No 2). After 10 cycles of hydrothermal treatment, 0.06% by weight of potassium iodide remains on the sorbent (Table 2).
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Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| LT2000013A LT4725B (en) | 2000-02-23 | 2000-02-23 | Sorbent for iodine and method for the preparation thereof |
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| LT2000013A LT4725B (en) | 2000-02-23 | 2000-02-23 | Sorbent for iodine and method for the preparation thereof |
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| LT2000013A LT2000013A (en) | 2000-08-25 |
| LT4725B true LT4725B (en) | 2000-11-27 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| LT4497B (en) | 1998-08-06 | 1999-05-25 | Kauno technologijos universitetas | Polytetra-ammonium salt, method for preparation and use thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| LT4497B (en) | 1998-08-06 | 1999-05-25 | Kauno technologijos universitetas | Polytetra-ammonium salt, method for preparation and use thereof |
Non-Patent Citations (4)
| Title |
|---|
| G. E. BESPAMJATNIKOBS, JU. A. KROTOV: "Predelno dopystimje koncentracii chimičeskich veščectv" |
| H. DEUBNER, K. GERLACH: "Parametrische Untersuchungen zur Abscheidung von Methjodid" |
| I. E. NACHUTIN ET AL.: "Gazoočistka i kontpol gazovijch vijbrosov AES", pages: 24 |
| VON J. G. WIHELM: "Filterung von Abluft aus Kerntechnischen Anlagen", pages: 376 |
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| LT2000013A (en) | 2000-08-25 |
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