SCIENTIFIC ABSTRACT NISELSON, L. A. - NISELSON, L. A.

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December 31, 1967
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SCIENTIFIC ABSTRACT
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69217 SXnthesir of Tantalum- and I'liobium lodiden br S/07,-,/-(0/005/02/003/04r* Interaction of 'TaCl 5 and NtCl5 With Al 216 and SIIJ4 B004/B016 eo" H. 1. Kalin" A-TJI SjBHI'I*TEDs gaptember V4 1950 Card 3/3 -- SIBILIWE, L.A.g SWAKOV. G.T. %rat4was SiC14 ~P"30 UG14 -"C'3 , and SIC24 - pcl~, ftr.narc.kbla. 5 so-P1139-1145 vi 160. (KULA 138 7) L *$kMkly 1"141%At tgyftlWkb K*t&UGT IN. VOLWICLUAS. (3111con ciaorlde) (ftoopharvA chlorlde) (rbowyboryl ablortdo) 07 '07/0'o'r S / 6/60/C05/C o,,10431YX B004/B060 AUTIIORS:~ Hisel'tron, L4' A., Chern;aypv, Y. fi. TITLEs 311 Bi and Sil Al I Syt;,.Gmv 4 2 6 PERIODICAL: Zhurnal n4organicheskoy khimilt 1960, Vol. 5P 1#00 it 1564-1566 TSXTs In view of the fact that volatile iodides are used to Produce high- ~Puriiy elements, the authors examined the phase equilibria in the Sil - Bil 4nd Sil - Al I systems. The phase equilibrium betueen 4 3 4 2 6 crystals and liquid vas determined by a method deszribe4 in Ref. 1, and the boifing point according to Refo 2 a'. 760 torre Result's are given in Tables 1,2 and in'Figai 1#2. Card 114. and Sil Sil.4 BI5 4 2,6 S/078 60 005/OOT/u,;" 0 0 BM4% Vc f IV. 21 Card 2/4 -,t 511 DI &nd 511 Al 16 C, S/071 '60/005/007/055/043/YJ 4 3 4 %OY B00411060 Nutoctics appear in both systems. A linear dependence was found between the logarithm of the solar SIX 4 fraction and the reciprocal value of absolute temperature. The thermal effects calculated Cron the tangent of this straight line lie near the melting hoate of SIX 4 and Al 216* The systems, therefore, follow the Schrdder equation. The Raoult law holde for both systess, Thiswas confirced by zeasuring the pressure of' saturated vapor of pure SIX 40 Table 3 gives the boiling points of Al .16 between 148 and 054.5 torr, and of SIX 4 between 105*5 and 880.0 torr, determined by means of a Sventoslavskty ebulltonster. The authors point to the pos- sibility of calculating the phase equilibriun between liquid and vapor from the data relative to the phase equilibrium crystal - liquid, and vice versa, on the basis of the act1vttj coefficients, provided the system does not deviate too tuch from an Ideal one. There are 2 ficures, 5 t&ble-, and 2 referencese I Soviet, I US, and I German. SUBMITTED# March 12, 1959 Card 3/4 Sil al and ail Al I -/O7Y6O/C,05/007/0 5 5/04,,/Xr 4 - 3 4 - 2 6 Systen't ? B004 '060 Legend to ]rig* It Phase equilibria in the 3114 - Bi13 syfltOm Logtnd to.Fig. 2t Phase equilibria In the 511 4 ' Al216 Oystom To both Irigs.1 I points determined experinqntally 2~ calculated by Ranult's equation Card 4/4 NISILISON, rkA, faftemston betwoes ftCI% and MY and betweas UAIS "d mi 34 SkrooraorgAftine 5 ao*7tl631# it 160. (KM 1387) (Inablas chloride) MmIlium chloride) (fhlopboophoryl chloride) S/078/60/C-05/009/016/040/XX ?017/BO56 AUTHORS: Ivanov - Em4n, S. N. ani Nisellson, L. A~ A TITLE: Amphoteric Properties of Ytterbiu and Liteclum Hydroxides PERIODICAL: Zhurnal noorganich*skoy khicii, 1960, To! 5, No. 9, pp. 1921 - 1923 TEXT: The alkali salts of the hexahydrozo compounds of ytterblux and lutsoium were synthotized. Ytterbium and luteclum oxides with a purity of 99.95% were used as starting caterials. The azphot*r1c hydroxides were treated w4.th a concentrated sodluz hydroxide solution for 48 hours in an autoclave at 180 - 2000C,. The isolated compounds have the following composition. X*31W~ V D(OH )61 an 4 P43tLu(OH)6 Card 112 Amphoteric Properties of S/070 /60/005/009/0 1 81040AX Ytterbium and Lutecium Hydroxides 3010058 The hydroxQcompounds of ytterbium and lutecium decompose in mater to form sodium hydroxide and the correspon4inC hy4rox1des- Through heat treatment of the hydrozo compounds of yttorblum ani lutecium at 320-- 3500C, these compounds lose two water molec-iles. Sodium met&- ytterblste WaThO2 and sodium =*ta-lutectato WaLuO 2 are proluced by heating equivalent mixtures of the correspondirg lanthanide ox1des with Na2CO3 at 91360C. There are 2 figures, I tabled ati 6 reforonc#s: 2 Soviet, 3 G*rzan, and 1 Cze-.hoslovaklan. SUBMITTED: June 19 1959 Card 212 A WOO AUTHORS- Ivanov-Emin, B. N.. Nisellson, L. A., Larionova, L. Te TlTLEs Study of the Behavior of Some Fluoro Callates"llf Alkali Ketals In Aqueous Solutions PLRIODICALs Zhurnal neorganicheekoy kh1oll, 1960, Vol~ 5, No. 9. pp. 1993-1995 TEXTs The fluoro gallates of potassium, rubidium and cesiuz were stulieit in aqueous phase by means of electrical conductivity measurements. The molecular electrical conductivities found for the compounds [(;aF 3' 5H2010 K2 (GaF 5'H20]. Rb (aar4.2H.0) and Cs(GaF 4 ' 21120) aro given In Fig. i and Table 1. The determination was cade at 20 0C. It-follows from the studios of the conductivity of fluoro gallates of potissium rubilium and cesium that the complex anion decomposes in aqueous solution according to the reaction schemes K,[GaF 5 *H201-4 2 KF + Gar 3 + H20 and Ca (G FA F4' 2H201^ CsF 1* GaF34H20, S/OT8j6O/OO5/009,/07R/040./XY Card 112 855~9 Study of the Behaviour of Some Fluoro 3/078J60/005/009/028/040/XX Gallatea of Alkali Metals in Aqueous Solutions B017/BO58 respectively. When diluting the gallium fluoride solutions, hydration and dissociation of the hydrated gallium fluoride molecule+sets-in according to the reaction schemet(GaF 3' 3H201 + H20-1 [GaF 2*4H2O'l + F . The Us- sociation rises slowly with increasing dilution and the molecular conductivity attains tile valence of a two-ion electrolyte only at a dilution of V:000 - 10001/mole. Tile authors mention I. V. Tananayev and N. V. Bausova. There are I figure, 2 tables, nnd 5 references$ 4 Soviet and I British. SUBMITTEDi June 6, 1953 Card 217 S/07" f601OO51O;)?,1r)2 ")/'XX BOI 77BO58 AUTHORSt Ivanov-Emin. B. N., Nisellson, L. A., Grekes, Ta._ ------------- TITLEs Study of the Solubility of Indium Hydroxm4in Solium Hydroxide Solutior,s V PERIODICALt Zhurnal neolganicheekoy khiaii, 1960, Vol, 5, No. 9, pp. 1996-1998 TEXTs The solubility of Iftdium hydroxide In sodium hydroxide solutions with concentrations of from I to 17 mol/l was studied at 250C. Indium hydroxide was prepared according to the method by N. A. Teasnayev (Ref.6) and subsequently converted into the crystalline state according to the method by Fricke and Seitz (Ref. 7). The analysis results of cryntalline indium hydroxide. dried at 1200C, corresponded to formula In(OH) 3. The solubility of indium, hydroxide in solutions of uo4iun hydroxide at 250C is given in Table 1, and Fig. 1 0hop.graphicalLy the dependence of the sol4bility of indium hydroxide at 2 on the :oncentration of sodium Card V2 Study of the Solubility of rn4lum Hy4roxid* S/OTS/60/005/009/029/040/XX in Sodium flydrozido Solutions B017/8050 hydroxide. The maximum solubtlity of In(OH) 5 in sodium hy4roxide solutions (11.33 mol '11ROH/1) amounts to 11.0 C/l, The (solid phase consists of indium hydroxide at a soda lye concentration of up to 11 .0 g1l, ani of a h1drate of sodium hexahydroxo indate at a soda lye concentration above 11.0 g/1. The solubility of wiorphous and crystalline Indium hydroxide In the same. The authors mentio% E. A. Oatroumov, N. V. Aksellru4, V. B. Spivakovskiy, E. X, Deyohman, 7, P. Chslyy and S. P. Rozheriko. D. Okhodnitski and Ta. ChIshniar participated In the study, There are I f4ure. I l9, and 6 relerentfas 5 Soviet, I French, and I German, SUBMITTEDt June 6, 1959 Card 212 B010064 AUTHORS: Ivanov-Smin, B. K., Hisiollsonp L. A.$ I a, A. T. TITLE: Study of the Solubility of Scanlium Hydroxide 10; in Sodium Hydroxide Solutions PERIODICAL: Zhurnal neorganichoskoy khimil, 1960, Vol. 5, Ko. 12, pp. 2841-2042 TEXT: The solubility of scandium, hydroxid 10 in god ign hydroxide solutions containing I - 19 moles of NaOR/l was studied at 25 C. itaximum solubility of So(OR), In an 11.7-mole solution of sodium hydroxide to 5.n g11. The existence of peaks on the solubility curve indicate@ the formation of sodium hydroxo scandiato. The solid phase up to the peak to crystalline V/ scandium hydroxide, and the solid ph& b; nd the peak Is a hydrate of sodium hexahydroxo scandiats Ma 3 13 :7OR 61 ,2H20. N. A. Tananayev to mentionod. There are I figure, I table, and 9 references; 4 Soviet, 2 British, 2 German, an4 I Czechoslovakian. S/079/60/005/012/015/016 SUBVITTED: December An. 1959 Card 1/1 SMO/W/033AOSA05/013 AW31AOOI AUMORS - Mlsel'son,_L.A.,-Sokolova, T. T'- 11 An Investigation of the Kinetics of Interaction Between the Higher Oxides of Tantalum, Klobimm, VZtantum and Zirconium &-t4 Eliosphorus Pentachlor I 1", 0 do V MIODT-CALLC ZF=rnal prikladnoy kthimll, 1960, V01.", No. 8, PP- 1755-1765 TMt The kinetics of chlorination of higher oxides of tantalum, nioblum, titanium and zirconium with liquid phoxitorus pentschlorldiO'I&s studied. The inves- tigation was based on the assumptions 1) that chlorination In the condensated phase causes only a slight change in the concentration of the chlorinating agent; 2) that the experimental arrangement of the Investlgatlon is easy, 3) that chlori~atlcn products are obtained which can be used for Thai separation and purification of x1rconium, tantaluin and n1oblum by the rectification method. The- results obtained In the expertments, presqnted in the form of a relation between the logarithm of oxide chlorination rate and the Inverse absolute temperature of chlorination, obey in all cases the linear law. This proves that In the tempera- ture lr~Urval studied (150-3000C) the chlorination processes take place in the kinetic region, I.e., the rate of the process Is determined by the rate of the Card 1/2 31109016011033140081W5A 13 A003/AOOI An Investigation or the Kinetics of Interaction Between the Higher Oxides of Tantalum, Nioblum, Titanium and Zirconium and Fhoephorus Pentachloride chemical interaction. Based on the tangents of the Inclination angles of the curves obtained the activation energies of the process were calculated. The values obtained vary within the narrow limits of 25-33 kcal/wole and change little at the transition from one oxide to the other. For zircontwu dioxide the activation energy In 11.0 kcal/mole, but the reproducibliltr of the results Is low. The chlorination rate of oxides in relation to the weight unit (in X/g'mln) depends mainly on the temperature of their preliminary calcination. The principal cause of the change In the oxide chlorination rate In this case is the change of their specific surface. The character of the modification or the ocides attdied has only a slight effect on the chlorinatIon rate. "Ihe chlorination rate of -r-MbA~ (calcinated at 8000C) differs from that of (X,-%O by only 1.5 times, whereas for the same monoolinic modification of z1rConIu= d?oxide, but calcinated at 600 and 8000C the chlorination rates differ by a factor of 5.6. There are 6 figures, I table &:A IS referencess 12 Soviet, 2 American, 2 French, I Englisti and I German. SUBKr=o December 21, 1959 Card 2/2 S/076J60/0 54/007/016/042/1Z B0041BOtO AUTHOR: ffivolls-Qn~ 1- A TITLI?.- Classification of 39paration Tochniquos PERIODICAL: Zhurnal ficichtskoy khtmii, 1960, Vol. 54, No. 7, pp. 1460-1469 TXXT: This paper is an attemptio classify complex separation techniques according to the different dynamics of material flow of the components to be separated. The concept@ of "dynamically reversible" and "dynamically Irreversible" elementary processes are Introduced. The naterial flow of three column processes in discussed in more detail, i.e., 1) counterflow; 2) tonal flowl and 3) chromatographic process*@. The#* three processes are typos of limiting cases. Kultistago column processes say consist of combi- nations of the@* typos. Transitions from one type to anotber are possible. A classification scheme to suggested: Card 1/3 Classification of Separation Techniques Simple (*Iexontar Mynamic reversible Processesl 0 0 93 V-4 r4 0 40 V4 ~4 $4 V4 d a 0 40 Is 4P .4 k v4 4a 411 01144 40 x coluan jZoaal pro-c-e-s-e-s-91 J6010341007JO1610421XX 5/076_ B004/8068 on techniqueall mynamic irreverstuie Drocessesi 0 -V4 $4 10 $4 40 "4 0 0 40 Coaplex cascade procests Ermatographio Counterflow processed Card 2/3 Classification of Separation Techniques S/076/60/034/007/016/042/XX BOWPO~9 On the basis of this classification, now processes can be developeA which have not been used by now. Comparison on the basis of some cammon parameter in suggested for determining the efficiency Et E w G/W 9(dg/dv). 0 to the quantity of the main component; IT is the parameter chosenj dN/dt is tt's variation of the second component with tim** Thor* are 4 figures and 4 references: 7 Soviet, 3 US, I British, 2 German. ani I Swiss. ASSOCIATION: Nookovokly institut tgvetnykh m*tallov i zolota im. V. I. Kalinina, (Moscow institute of Nonferrous Metals and Cold imeni M. I Kalinin) SUBMITTED:- September 15t 1958 Card 3/3 Lf%~ V A Crystotle-liquid in birAr7 isystw.-a fon-c-I ZrG" ~-jqj" j, -4' q,rcl , snci and :ACI Z:.,L~-. nccrZ. khLt. 6 no.I:IV. al. 3 (IM A It,92) Wmanltrz cl.lo-t-I-A (Wnium cuorten) rale cid -.1-Allbrim) 2- T 1B 2 018 AUTHORS: linellson, L. A-t 14truaQvicht I. T. TITLE: Phase eqLui1ibr-1'& it, the systema. SLCI - Bel an& SiRr' BEr 4 5 4 PERIODICAL; Zhurnal neorganicheakoy khimil, v. 6, no. 5, 1961. T4e-7491 TEXT; The phase oQuilibria in the syste mp SiCl 4 - V C 13ani SiPr 4 - ?Br3 WOM at-adied. The starting materialsi were purified by continuous boiling vith copper filings and outsequent rectification. The s,,ratems were thermal-17 ana- lyzed by the heating curves recc-ded by Kurnakc--rls pyrometer. The celtine- poirA diagrams of the systems atudiel are of the eutectic type. The heat rf' solution of Sicl 4 in BC1 5 was fcund to to the heat rill' solution of SiBr 4 In BBr 3 was 2.9 kcal/mole. A chezi-~&l reaetilor, te%veer, the components in the systeme SiCl, - BC1 and StBr - BBr was net observed. 4 5 4 5 The vapor pressure of the saturated BBr vapora may be expreersed by the, 3 S(LU&tion Cart 1/2 S/07SJ61/006/003/022/022 B121/B208 AUTHORS: Vakso S. A., Seryakov, 0. V.9 51sollson, L. A., Sidorina, L. S. TITLE: Liquld-vapor equilibrium In systems formed from the tetra- chlorides of titaniump silicon, and carbon PERIODICAL: Zhurnstl neorganicheskoy khtall, v. 6, no- 3, 1961, T56-753 TEXT: The equilibrium between liquid and vapor (at 760 m ffe) In the systems TICI 4 - Sicl 40 TIM 4 - Ccl 4# and CC14 - 5'C'4 was studied rofraotometrioally at 20 0C. The tetrachlorides had been purified by distillation, and the titanium and silicon chlorides also chemically. Data on the liquid-vapor equilibrium In the systems TIM 4 - SICI 4 t TICI 4 -CC1 40 and CC14 - S'Cl4 at 760 = Ve are summarized In a table. The refractive index In the systems TICI 4 - CM 4 and TICI 4 - SICI4 was found to be a linear function of the composition. In the system Card 1/1 Liquid-vapor equilibrium... SIOTO1611006100310221022 8121/1208 TiCl 4 -sici 4# a negative deviation from Raoult's law was found on the side of the lower-boiling component. The systea TICI 4 - eel4 to nearly Ideal, while the Wotan eel 4 -SIM 4 distinatly dIffors from the Ideal *tat* with respect to the course of the Interface between liquid and vapor. Thor* are 4 figures, I table, and 3 Woroncos: I Soviet-bloc and 2 non-Sovist-bloo. SUBMITTED: August 2, 1960 Card 2/3 Liquid-vapor equilibrium... Card 3/3 T=m MI. - MCf. AC-emw =74 14 4;~' S7.2 too too 10.1 $7.9 97AS 100 6,78 59.7 is 10:22 767 79 W.9 87:44 N 09 7:15 83:1 61.9 8S.0 98:0 &.7 #6,4 63.8 W 2 017,t4 SA 113.1 66.1 73:15 go in 9.3 (02.4 69.1 66.4 114:78 9.25 ttz'( 78.0 40.5 91-8 125t4 88.9 30.4 83 2 1 :4 130 105.2 . 17.0 06:5 136.1 Ito.$ 8.7 46 4 9.1 jz3.4 S.S 33:2 Be t29.0 250 (s$ 6:6 132,3 0:81 6:0 9.4 i34.4 0.37 3A 8.0 MS.$ 136 4 o.19 1 0 1.54 0 9.3 - . too 97.91 0.9 77.7 0.5 32.4 31-0 23.0 Ij to 3J0 0 -%-r4 w S/078/61/006/005/02,1/022 5121/3200 WIMS OC14 - S(Ctd gtnd to the Tables $r I "Stem; 2 content, rnle%; a in liquid ph&-pe; b) In vapor phSs~; 3) relative fugacity- 100 - 2 (01) (W .01 14 '1 12 5 Is's 97.n 5:2 W .0 193 : M.S VIS.03 53 1 $7.0 79.0 IN 92.0 5:3 t W.0 72.1 1.48 85-2 SA 'z 54.0 06's WO MS S.0 67.2 30.7 50-5 ill$ s0'$ 4.9 087 27.6 41.0 f.82 3g,Z Sj 71:2 19.3 3D.0 9-79 12ol 4.6 12A 13-2 20-2 "a 0 - 14.4 5.6 it 5 1.01 7$'s 0 0 ITANOY-OfIN# R&H.; 91,51Z!AM - RtBCVIK. ra, I.c LARICKYA, L.Ye. ,L, ~~tktj, _ Complex compounds of Callimm Wides vith o-phammthrollne. Zhur. neargAhis. 6 no.5tll4Z-1146 It. 116le (MM 14-4) (aillium compound&) (Phananthrolins) UBMISM, L.A. Density or ZrClk and RM4 in th* vapor and liquid state,. Mar. tworgAhus 6 n*.5vl24Z-;IZW W 1161* (MM 14: 4) (timonlum efdorlde) (Nafniun chloride) I:VANIY4-EMIYE, NI MWS04, L.A.; IVOLGINAI- AL,-k, Solubility of' yttrium hydroxide in sodium hydroxide solutions. . Zhur.nocrg.khL-4., 6 no,6r1483-148-4, is 061. (JaRk 14M) (Yttrium oxide) (Sodjux hydroxide) HISEWSONj, L.A.; SDMMVA, T.D. U &"par phaim *qiuUbrim in rystms farwd by TJCJ I and rOCL3* ZhUr. neorg. khin. 6 no.7tI645-1651, Af 5 W.U* (MM 14t7) (systme (chomistrr)) S/080/61/034/011/001/020 D201ID301 AUTHORS: Ivanov-Emin, B.N-t Hisellsono L.A., and Petrusevich, 'ITLEs The synthesis and purification of boron broolde and iodide PERIODICAL: Zhurnal prikladnoy khimiio v. 34, no@ 11, 1961, 2378 - 2384 TEXT3 The authors carried out experiments for prepanng boron bro- mide and iodide directly from the elements. As starting materials pure bromine and iodine and samples of amorphous boron containing 87 - 99.5 % B were used. The halogenatione were periormed in ver- tical quartz reactorep 3 - 5 cm in diameter. Boron was bricketed with a sugar solution in methanol and the hologenation process was carried out in a stream of argon at 640 - 10500C for 3 - 6 hours. During halogenation fractions of the halodee were analyzed for free Br. and 1. contents. For comparison purposes, one bromation reac- tion was pcrforned In the reactor lying almost horizontally. All ex- Card 1/3 3/080/61/034/011/101/020 The synthesis and purification D201/D301 perimental details are given in full. The yields were markedly hi- gher in vertical reactors than in the horizontal ones. the optimum temperature being 850 - 9000C for both halogenation renctions; the bromination yield was 94.5 - 99.5 % B Br 3* The iodination process was quite similar to that of bromination, but with lower yields (63.5 - 50 %). Purification of the crude halides, as well as of technical B Cl was carried out by distillation In a rectifying column of a platle-sieve type# with 25 real plates. The rectifica- tion of technical B01 and that of the crude BBr3 faas easily car- distillation BC13 was practically free ried outt after the f from 3101 and C0012, present in the Initial productp and BBr3 was practiaLlty free from 5IBr4 and other volatile components; a pure colorless product was obtained by a second distillation in presence of copper filings. Furif:~catlon of the crude iodide was not so easy owing to the high iodide content in the product. This was overco=e by converting the fr e I to SnI # with metallic tin. The authors were able$ by this m:thoi, to obtain from 3.2 kg of the lodination productp containing about 25 % of Sn14t 0 .4 % S114 and some other impurities, 2.05 kg of practically pure B130 after one frnctional Card 213 The synthesis and purification ... distillation. There are 3 figures and 4 6 Soviet-bloc and 5 non-Soviet-bloc. The language publications read as follows: E. Stoff, J.Am. Chem. Soc., 62# 12579 1940; Banus, J. Am. Chem-Soc., 71, 3225, 1949. SUBMITTED: December 12, 1960 S/080/61/034/011/'COI/020 D201/D301 tables and 11 references: references to the English- Gamble, P. Gilmont, J. W. Schumb, E. Gamble, r. Curd 315 S/828/62/000/000/015/OL7 E071/EI35 AUTHOR; Nise 1-1 fi~n-- L. -~-- TITLZi Separation and purification of halogenides of zirconium and hafnium, nlobium and tantalum by methods based on differences in. the volatility SOURCES Razdeleniye blizkikh po, svoystvaw redkikh retalLov. .%Iezhvuz. konfer. po a-zetodam razdel. blizkikh po svoyst. red. metallov. Moscow, 12-1,etaLlurgizuat, 1902, 166-16j. TEXT: The possibiLities of separation of the above elements by rectification are discussed and supported by experimeittal data obtained on a laboratory apparatus. The ColLowing processes were examined: separation and purification of.tantalum and niobium by rectification of products of interaction of their pentachlorides with phosphorus oxychloride; rectification of pert&chlorides br tantalum and niobium; separation of zircconlum and hafnium by rectification of products of interaction of their tetrachlorides with phosphorus oxychloride; separation of t1rconium and hafnium by extractive rectification of their tetrachlorides !-Abstractor's notes this process is discussed but no experimental ~;ork is Card 1/2 Separation .and purification of ... 5/62d/62/000/000/oli/017 E071/EI33 reported, separation of zirconium and hafnium by rectiVication of their tetrachlorides under pressure. The latter process is of particular interest for industrial application but it presents difficult problems. These could be solved by designing special apparatus applying reliable temperaturg monitoring, salts as heat carriers, voltage stabilization and automation of the process with a view to continuous operation. There are 3 figures and 4 tables. Card 2/2 S/826/62/000/0GO/016/017 EO? I/E; 13 5 AUTHURSs Zelikman, A.N., Kreyn, O.Ye., Nisellson, L. Gorovitse j%.N*$ and Ivanovaq, . . TITLEs Separation of tungsten and molybdenum by utilising the difference in volatility of th*lr chlorides and oxychlorides 5OURCE; Razdeleniye blizkikh po avoystvan redkikh netAllov. Pozhvuz. konfer. po inatodam-razdel. bLizkikh po evoyst. red. metallov. Moscow, Motallurgizdat, 14)U2, IOU-197. TEXT: A method of separating tungsten from molybdenum, based on evaporation of Moo2C12 on heating of odlybdenum trichloride with sodium chloride to a temperature of 6oo-700 *C. was studied. With contents of 0.01 to 0.16 and 1.u35% W in the starting molybdenum tritxide the purified product contained less than (6 to 9) x 10- and 1,5 x 10-31, jj respectLvely. It was established that it is possible to separate tungsten and molybdenum by rectification of their higher chlorides. WC16 nd MOCI (rectification column data: diameter 30 mm, h:ight (jog mm, 15 sieve plate&, with 45 holes of I om diameter). Card 1/2 SeparAtion of tungsten and molybdenum... S/d2d/62/000/000/016/017 E071A135 From tungsten sexquichlorido containing about molybdenum pentachloride containing about 5~9 chlorides containing below 0.01#,# or admixture tungsten respectively with yields of the main 70-dO% were obtainad. There are 6 figure* and 7 tables, 51., YoC.15. and from WC16, purified of molybdenum or fraotions of Card 2/2 33279 SATO 62/007/002/006/019 3119 silo AUTSORS, 11sollson, L. A., Toytovich, B. A. TITLEe The SiCl 4 - POCI 3 'Bel5 system PERIODICALt Zhurnal neorganicheskoy khtsil, v. 7, no- 2. 1962, 360 - 363 TEXTs The equilibria between crystalline and liquid phases and be'..ween liquid and vapor phases of the systems POCI 3 - Bel5 and SICI 4 - POCI3 - Bel ) were studied. The methods are described by the first author In Zh. neorg. khi iij 5.- 1139 (1960)1 1. 2150 (19501 and 1. A. Shcheka et al., 1, 964 (1;56 . This study is of interest for obtaining purest SI. ResulC~o Bel 3 and POCI 3 form in solid state the compound BCl 3' POCI 3which dissociates almost completely on melting (melting point 83.80C). (The equation of A. B. Slodseyevekty and 0. A. Yesin can be used for calculating the dissociation constant immediately above the melting point.) The heat of solution of Bel 3* Pocl3in SIC14 to 4.6 kcal/sole. Then dissolved in Sicl 4' the compound is totally dissociated (in Bel 5 and POCI The Card 1/2 33279 5/070/62/007/002/006/019 The 501 4 'FOCI 3 ' BCl3 system 3119/allo eiaultaneaus presence of suall BCl5 and POCI, quantities in S'C14 has no influeace on their relative volatility as to SICI 4* Ther* are 4 f1gures, 2 tables, and 9 rtferencess. 7 Soviet and 2 non-Soviet. The reference to the English-language publication read@ as followst A. B. Burg, M. R. Pose. J. Amer. the=. Soc., 65, 1637 (1943). ASSOCIATIONs Gosularstwennyy Institut redkikh metallov (State Institute of Rar~ Ifetals) SUBMITTEN Decesber 24, 1960 Card 2/2 ITAIM-MINO B.N.; RSELIS~M--,,~,L-LIARIONOVkj T.,.Ta, Frapert1w of saluUaw of alkall mwt&X gaUatese Zhur.noorg.rhf-- 7 m.3022-V6 W 962. (MM 15:3) (GaUlc bonxide) 34M68 S/OT8/62/007/003/015/019 31101sise AWHOito 111sel 'son, Le A. TITLEs Constitution diagrams of binary eyetess formed by zirconium and hafnium halides PERIODICALs Zburnal neorgenloheskoy khIm11# v- 7# no. 5t 1962, 693 - 694 TEM's The ;rystal - liquid phase equilibrium was Investigated In binary systems of zirconium and hafnium totrachloridto, setrabrosides, and tatratodides. The halides were produced from Zr (0.05% Hf), Rf (0.$,A Zr), Cl, Brq, and 1. The binary systems ZrC1 4'fffC1 40 ZrAr4-Mr 4' Zr'4-gf'4 xhibit unlimited solubility In the liquid and solid states. Their con- : titution diagrams show an almost straight-line course for the liquidus curve with the solidus almost beside It* This to because the Zr and ur atonto radii are almost equal# the tetrshalide crystal lattices are identical, and their melting points are very close. The systems Zrl Zral and Zr3r -ZrC1 constitute a continuous sari** of solid solu- 4-. . 4' . 4 4 tions with a minimum. Zrr Zrol has a lower miniaus (v 58 a*14 of ZrCl., 4- 4 Card 1/2 S/OTO/62/007/003/015/019 Constitution disgra" of binarys** B110/313a ^J3680C) due to the groater diff*rence between the &taste radli of I and CI than between Br and G1, There are 2 figureep I tablet and 3 r*ferencess 2 Uviet and I non-Soviet* SUMUTUD t 06tab*r 4, 1960 Card 2/2 3/07BJ62/007/005/004/014 B101/Btlo AUTHORSs Nisollson, L. A., Teslitskaya, V. V., Shvedov&, T. A. TITLL's Synthe3is of zirconiua(IV) iodide and hafnium(IV) io*dide by halogen oxchange FERIODICALt Zhurnal neorganicheskoy khinii, V- 7, no. 5, 1962, 971 - 974 TEXTa The following reactions are discussed for preparing pure Zr(Hf)l 4S (A) ZrCl4 + 4N&1.- Zrl 4 -+*4NaCl. The initial mixture was molten In an 'Ovacsiated ampoule (650-70000), and the ampoule heated on one side (initially 4000C, finally 650-7000C) to effoot sublization of the substance/ into the colder part. The sublimate contained 65.50' by weight of Zrl 4 and 14.5A by weight of ZrCl 4' Complete separation of the chloride from the iodide was not attained. (B) ZrCl + SiI Zrl + Sicl, (at 250-3200C) 4 4 4 4 also yielded only 7a% substitution of chlorine by iodine. (C) 3Zr(Hf)cl4 Card 1/3 S/076/62/00T/005/004/014 Synthesis of zirooniup(ly) iodide ... BIOI/BttO + 2AI 216 c=! 3 Zr (111f) 144 2A1 2CI6(at 300-3650c) produced. a 100;~ yiol& of ZrI 4' or UfT 4' reapeetively, containing 0.1-0-051)'"1. The reaction, with &1 2 Yielded OnIr 80-85~ substitution., (D) ZrCI + 4HI ZrI + OCI- Because of the bigh vapor pressure of the resulting IICI, work. was carried out &t atmcepheric pressure, and the 111. in Ar its carrier gran won condwotod over Zrf:l4 heated to 3700C. 01.5-82,'; substitution wan attainedL. M sinoe ZrI and ZrCl form no stable compounds with each other and. have different 4 4- volatilities, their separution was attempted by distillation. A zixture of 29.,t,' by- weight of ZrC14 and 70.6~ by weight of ZrI 4 vas healed to 400-4200C, finallY to 50C-520 0G. The a=poula was cut into zones,, and the cori,i!ennates of the individual zoneet were analyzed. Fraction I cormiated of Z.-Cl'4with only 0.11~3 ZrI 41 fraction Y consisted of' 95A ZrI 41 and. the lirtilletion recidue of iW4 11-free ZrI 4' wh ile the initial aixtuxe, containal 0.1'f Al. Besides thiff separation, the impurity-was also removed. F Card 2A ITAXOT4baNO B.P.; KIPL'SMj L.L.; GVOZDLYLO N.I. S*UUUty of CialUum bldroKIdle in softm by&oxLde &M potascLcm hydroxide solutions at 254C, 2mr,raorgekhimt. 7 no.WI50-1153 V4r 162o (MM 150) (GalUm hydroxide) (Alkalles) (SolubLILty) 8/0816210OT/0210OZ/022 AUTROIM 11*91(sont L, L,j SokoLovat T. Dt TITM Or4hobaric; densities and critical parameters of x1rooniss (IT) WA harnium (IT) halides: 'nRIODICAL: Shurnal neorganichookor khimiij, Y. Tt no. 12t 196Z, 2653-2660 TRXT.- From the orthobaria densities doteriined In high-purity Er and R60- totraiodides, totrabromides and tetrachlorides, the critical value& or these compounds were calculated. The vapor and liquid donsitioa were determined In a range from about 360 to 690% OC'in a transparent oven 0 containing a nitrite-nitrate bath for temperatures below 500 G or a nickel block for higher temperatures. The sample enclosed in asealed ampoule or a pyonouster was placed Inthe bathor block. The values: found for ZrCl4 and,HfCl4 wore somewhat higher and had a flatter "ximus thtn, those published *arlior.(Zb. noorgan. khlaii, 6s 1242 (1961))# The critical temperature was derived fro* the maximum of the orthobaric density,* The, critical density was found according to the Cailletet-Mathiam lawl for C's." 1/2 S/080/62/035/005/002/015 D204/D307 AUTHORS: Ninol-Ison, L. A_,, Petrusevich, I. V., Sha=.-ay, F. I. and Fedorov, T. F. TITLE: Preparation of elemental boron by reduction of itcl halides with ~4drogen PLRIODICAL: Zhurnal prikladnoy khimii, v. 35, 1962, 984-969 TEXT&: The present work was carried out to supplement existing da- ta on the preparation of elemental L. Purified BCIV BBr,, B 13 and Ii .2 were used under anhydrous condit:.ons. The rear-tor consisted of a q,uartz tube enclosing a pair of Mo electrodes connected by a Tit wire 100 x a x 0.10 mm, on which -he B was de ooited Temperatures were varied from 600 to 140000 and the molar M 3 Wk) ratios, (n), were made lt3-25. The interactions took place over 1.7 - d hours. The rate of B deposition increased rapidly with temperature and tended to be higher for lower n. ?or BBr 3 /H2 mixtures the Card 112 5/080/62/035/005/002/015 ?.ra~aration of elemental D204/D307 y1elds of B increased linearly from -3% at 800 OC to -50';4 at 13000C, ~elperature the rate of B almost independently of n. For a given . . deposition increased in the order BOI /,BBr