PHOTOCOPIES OF SCIENTIFIC ARTICLES BY TADEUSZ ADANSKI, INSTITUTE OF NUCLEAR RESEARCH, WARSAW- UNCLASSIFIED.

• Document Type: CREST
• Collection: General CIA Records
• Document Number (FOIA) /ESDN (CREST): CIA-RDP80T00246A023700140001-3
• Release Decision: RIPPUB
• Original Classification: C
• Document Page Count: 31
• Document Creation Date: December 23, 2016
• Document Release Date: August 7, 2013
• Sequence Number: 1
• Publication Date: November 1, 1963
• Content Type: REPORT

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POLSKA AKADEMIA NAUK
NSTYTUT BA DA N JADROWstCP.
PQ?ISM ACADEMY OF SCIE NOES
INSTITUTE Or NUCLEAR RESEAR::./1
PROPERTIES OF SEDIMENTS OF SPORINGLY SOLUBLE COMPOUNDS
MINED BY A VERY SLOW PRECIPIIIITION TEMNINE
%.?
Tacieust Adamoki
/
INARSAI,
Ocsobor.1962
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This report has been reproduced directly from the best
available copy
ivailable from
The Polish Government Commissioner
for Roe of Nuclear Rnergy
TRB MICE OP SCIIITIPIC,T1CHNICIL
AND MCONONICAL INFORMATION
Palace of Culture and Science
Warsaw, Poland
Drukule i rosprowadsa Oirodek Informacji Naukowej, Tech
nic sne i Ekonomicsnej Peimomocnika Rzadu do Spraw Syko-
rmystania Rnergii Jiedrovej, Naresawa,Palacjultury i Rau -
ki, 11 p., p. 1136. 101.696-73; Naklad700+7.0. urppis
RC/344/59. Zeta. Jr 4/63 Oddano do druku 1.1.1963 r.
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POLISH ACADEMY OP SCIENCES
INSTITUTE OP NUCLEAR RESEARCH
PROPERTIES OP SEDIMENTS OF SPARINGLY SOLUBLE COMPOUNDS
OBTAINED BY A VERY SLOW PRECIPITATION TECHNIQUE
0 WLASNOtCIACH ?SAWN ZWI4ZIO5W TRUDNO ROZPUSZCZALNYCH
OTRZYMYWANYCH TECHNIKA BARDZO POWOLNEGO STRACANIA
0 CBONCTBAX OCAMOB TPYMQ PACTBOMIR COELIMEHR
TIOMENECir =MCA ME& HAMMON CCUREHIA
by
Tadeusz Adamski
Abstract
A new technique of very slow precipitation
of sparingly soluble salts has been described.
With the aid of this method sediments of crys-
tallites of barium chromate have been obtained.
The different shapes of the crystallites ara
supposed to be formed due to the presence of
impurities of reagents, acting as specific
crystallization centres.
A number of characteristic features have
been observed and described, e.g. effects which
are supposed to be radiation effects provoqued
by traces of radium in chromates.
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Streszczenie
Opisano now technikt bardzo powolnego strm-
cania ?saddle soli trudno rozpuszczalnych..Spo-
sobem tym otrzymeno osady krystalitow chromianu
baru, ktorych rotne postaci przypisuje sie obec-
noci zanieczyezczeli w roztworach reagent6w two-
rzacych specyficzne oirodki krystalizacji.
Zaobserwowano I cpisano szereg charakterys-
tycznych zjawlsk, a m.in. efekty, ktore uwata
sit za uszkodzenia rsdiacyjne, a tch wysttpoks-
nie przypisuje sit dziakaniu gladSw radu obec-
nego w chromianach.
Coxeptamie
Ontcamo Homo Texxxxy ogey, mettettso-
ro ocattent ocattos Tpytmo pacTmopmmux
cote. 3rtm cnocodom notygeEo ?mum xpmc-
TMANTOB xpomaTa Oapmt. npetnotaraeTcs,
qTo pasmie sum 3TMX MIACTaAANTOB comity
Otarotapma apicyTcrimm pasmix nptmecell pe-
axTxsom, teIcTsytxxx tax cnemutimvecxxe Immo-
VIAXIMEMORHMe neHTpu.
HaOtttatici, x onmcaHu xapatTepmcmtec-
xxe swims a metty 3TBM sitopexTu, toTopue
ctitTarTcx patmansommmx nospettemmix npm-
CYTCTBIe toTopux npummumaeTcs XeMOTBNID
cxeios pawl, nptcyTcsyttero B xpomaTax.
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? Precipitation of sparingly soluble compounds is & frequent
operation in the technology of uranium. Por instance, it Is
employed with regard to sparingly soluble calcium, nrscocivv.er4
ammonium salts of polyuranyl acids, uranium dihydzwateraflAoride.
uranium trioxide and tetroxide, and complaxes of'..ranixn with
urea. Interesting is the very selective reaction o.f u.am14.1 tctre-
.
ride precipitation
UO2(1103)2 ? H202 UC. riNC
4 3
which mak...s it possible tn prepare urani4a coopoucis .t 'tar, sig"
purity for nuclear fuels. In t reaction. trt j.-an3-n totrotilP
is obtained as a light-yellow sparingly soltib.e :71dim4r.t.
though, it is amorphous, which does not premet! :Alps-11'10n Df
impuritise. Another emagple of precipitation pro7esses i rifi-
cation of the Neste 'eaters of urahium ore concentration. Tto.
waters contain traces of uranium ani lerivative rsiieactiv?- e?c-
manta, the latter being removed by coprecipitaties with azo-s.ory
sparingly soluble salts. Precipitation of sparingly wol,bl com-
pounds is a process frequently employed in cherical technology
and iS also of fundamental importance in analytics. chemistry. The
processes are usually very rapid and are as yet little knot% in
spite of numerous studies.
Pro a a list of the uses of these processes in only one taco-
nology, vis., that of lintRiMIS, it may already be seen that they
are extensively applicable.
.
The quest for means of obtaining uranium compounds of 7eri
high purity with the aid of precipitation techniques has called
attention to the fact that the parameter of time, which should be
very important, is On the whole inadequately considered in work an
precipitation. When the physics of these processes is contemolated
it should be noted that precipitation yields rather large inanti-
ties of the solid phase within a relatively short time. It is poc-
siblet for the solid phase to develop in either so ordered, crystal-
line, or a chaotic, amorphous form. For the ordered form to develop,
a amitahle period of time must be allowed. Furthermore, account
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mast be taken of the fact that the developmeat 40 the solid phase
is a process. in which suoceeeive smouats of the solid form first
and foremost on the surfaces of the first-formed solidphase.
Renee, the rate of precipitation should he adjusted according to
the area of such surfaces, if new ones are not to develop epos-
taneously. Purtkermore, ordinary coaditioas of precipitation make
it impossible for an equilibrium between the developing solid
phase and the liquid phase to become established, and also prevent
an equilibriur in the solution itself in the oase of more complica-
ted reactions. Local conditions of consentration and pR nay in eose
cases cause several solid phases to separate. even though only one
should exist under the given conditions. In earlier. Joint work
sitk 'Aeons [i] on the precipitation of neutral calcium *roseate.
this use found to be attended by separation of the sparingly so-
luble arsenates
GaAs04' Ca3(As04)2 end Ca3(As04)2 ? CatC111)2
',hes precipitation was rapid, even though the reageots were added
ic striebionetric proportions with reference to the tribasic arse-
nate. the equally kmosu but little explored processes of copreci-
piton** slight be explained siiilarly, it seems. assuming that
foretell mebstaaces, either entraised aeohaolcally or adsorbed on
earlier formed surfaces, become eovered by new lsyers of the sub-
stance precipitated and trapped firmly as impurities.
It appeared, therefore, that by widiag tho precipitant very
slowly wider vigorous stirring, asd thereby siestas the formation
of the solid phase, it should be possible to obtain purer and
better orystallised compounds, which would filter and settle well.
For the same reason the reagent should be added in a more diluted
? form in order to sloe its introduction even further and prevent
localstraagsapersaturations. fasentially. precipitation is crys-
tallizaiice and should also he assumed to involve conditions of
metastable supersaturation (Viers's theory), which promote sore
ordered deposition of the solid phase owing to some delay in its
formation.
2
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A related subject has already bees studied by P.P. von
Weimar* (2.3]. Re investigated precipitation of barium sulphate
and the ammeter of the preolpitate in relation to the degree
of the supersaturation of the solution. lbas very iighly diluted
solutions of maphates and barium malts (0.00005 - 0.00017 11)
are mired no precipitate is formed, even though the solution be-
comes supersaturated for barium sulphate. With 0.0017 it solutions
a precipitate is obtained within several seconds. When C.CC17.-
- 0.75 11 solutions are used, the precipitates are composed eccordine
to von Reims= of crystalline "sheletone'. whereas still hie:er
concentrations afford amorphous precipitates. P.B.Fisnher iniels-
tigntsd the effect of reagent concentration on the form of barium
sulphate precipitm.tes and particle site. He found Ihat with very
high dilution" of the reactants (0.0026 11) procipi:ates are ob-
tained that pass through analytical filters (the particles are
4.3 microns in size), whereas more concentrated solutions (0.0261)
yield crystallites 16 nicrons in diameter. Much h is devoted
to methods of obtaining well-filtering precipitates of barium sul-
phate (5- 10], a point important in analytical Pork. Put in
analytic ohemistry "aphasia is on the rapidity of precipitation,
which in effect, though, does not meet the requirements referred
to before. Another group of analytical research is concerned with
the technique of homogmaeous precipitation by precipitants produced
"is Situ" [11 - 22]. In this work, too, time is not a matter of
comes= end the reaction runs the full course within some scores of
Plantes at the most. Recommended analytical procedures specify only
the solution temperature ascessary for precipitation to be caused,
e.g., by urea hydrolysis, and the actual reaction undoubtedly pro-
ceeds within a time appreciably shorter than that needed to heat
the solution to the required temperature. the kinetics of precipi-
tate formation ems investigated oozy times and by various methods
(8. 23 - 30). let in these oases precipitation also took place
with the usual velocity. 3one author* recorded crystallites, their
ehapes being interpreted variously and attributed either to the
concentration or the p8 of the solutions (2, 5, 31 - 361. Much
like in the case of crystallisation process'', considerable atten-
ties is devoted in this field to crystallisation nuclei [37],
?
S
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lealiapromeip sad volt le IsCiirsil fiat Ifteiss as the klastlee
if iiimtratattia (84. 30/ 31,0 40. bs latter ease that Ohm
1001112114011120 a?10.01. sue2dOmit, soiat, their it.. haviag hoes
estimated Ia eaii if liam "tidies at 10'17 11. Closely amelated
with the problem of the presdpltatlea of sparisay soluble Son-
.d at the sans tine of the purity of the precipitates is
the phaseisenea of oopreelpitatita, espoolally important in the
porifleatien of rediesstive goatee. this is dealt by the school of
Oblepla and in sany of the publications listed in the bibliegIvelth7
(47 72).
' the nee technique presently to be gionesdbed if very slew
precipitation, whlith has been developed en the basis of the briefly
surveyed *otiose on the-foreatioa or the solid phase la preolpita-
tion:proeMea, 40100 to lend itself well for detailed studies on
the averse of these proseeses sad obeervetion of sone previously
haoen phstioaesis.
Apparatus. the apparatus reproduced in rlg.1 represeate the
lateit Melon,devaloped in the sours, of the stperlaints. the fon-
dateatat olaamit- of the apparatus is the aim. *blob sesslit of
44.4040 1410, (1). 25-40 al tetestead 'soggily SOO es long, to
tiSteiitipsst of t* is -meads! the sapillary (2) as an air
heir. Ile thiblim7r ttbs (1). 4a10-va-aszoss, is freely esspeaded
Alea-liktaziotatinue sir* lasian tufts (t). Vim the appasates is is
Olosiatien, the stiffed through the Tillery (2) bubbles up tarot,*
.eausing the liquid in the-apparatus to-oiroulato
tavaliti ? uniform rate. the Mtge is suitably sloped to prevent
sedlseetatian. The overflow (4) ?sables any mums& of. lbs solution
to ciraisi-inso th? fraction eel/actor (5), which is controlled by
a olOckwork so set as to cause the receiver vessel (6) to be
Mugged hourly. the precipitant floes from the 1-litre naplette
bottle-1M through the filter (10 and the ileitis' esp11121/7 (9)
into the reasto01). The orifice of the capillary (9) is Immersed
? little-below the surface of the solution. the nieropipetto (10)
"erre* for weteving the, flow of the reagent from the bottle (7).
aore the'AppirAtus is rut in aperation, the reactor (1) 18 .
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filled with a stook solution (se far a 5 11 solstioe of 12CrO4r
was usual) AAA the air supply is turned en. Next. the *oaks (11)
and (12) are opened to release the preeipitant fOOM the bottle .
(7), the limiting capillary (9) being so chosen as to ensure
the required flow rate at fully opened cocks. The flow rate can
be &stored with the aid of the micropipette (10)g when the cock
(11) is turned off the reagent continues to issue at the ease
rat*, but only from the micropipette (10), and the flow velocity
can be determined with the aid of a stop-watch. the reagent was
usually a 0.05 percent solution of haC12 or B(NC)2, and the
flow rate, 0.2 ml/min. An assembly of six such apparatuses is
shown in Phot. 142.25.
/n the first trials, carried out jointly with S.Rykoweti
(71), an apparatus built somewhat differently but on the same
principles was used. /n experimeots with bariun chromate used cs
a node' substance for invef?Igating the pro in point, pre-
?ation with ? diluter' olution of barium chloride was found
to yield solid. oapose f minute crystallites of the kind refer-
red to by Iron Weinarn h_ "crystalline skeletons? (Pbots.1 and 2)..
The crystallites had a stronglysdeveloped surface area owing to
numerous dendritic ramifiettiones hence, this technique wee un-
likely to 71eld solids of high purity. Basically, however, the
work showed there was justification for the view that the solid
phase can develop in this process in a more ordered manner. Owing
to the general inportance of precipitation pro in the tech-
nology of uranium and other elements: the process was investigated
more closely with the aid of the new technique outlined before.
After the precipitation technique had been Depraved, the crystal-
lites were noted to have an unusually symmetrical shape (Phots.
3 - 16), which was well reproducible (Pbots. 9 - 10), and to
settle readily. The present report describes soise of the pheno-
sena noted, an explanation of which will be given in subsequent
communications.
Barium chromate, which was used as a model substance for
studying precipitation pro proved a very suitable material
wise* it forme flat crystallites coavenisatly examined under ,
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a microscope. Barium phosphate, Ba3(204)2, yields under the
same conditions three-dimensional crystallites in the form of
four rods starting from a single point towards the vertices of
a regular tetrahedron. Barium carbonate and sulphate also yield
three-iimensional crystallites difficult to examine under an
ordinary microscope.
The structure and symmetry of all ,:rystallite!. indicates
that growth began invariably froi, a single central point. Usually
there is a distinct central body, whicn is undoubtedly the crystal-
lite nucleus (cf. Phote.11 - 16). If visible under the mi:ro-
scope, the nuclei have dimensi^ns of t'a order of 0.1 - ':0 mic-
ron, consequently also a mass of the order of 1C-12 tc 10-'5 g
and less. These dimensions approach those of thenuclei.pustulated
by other authors on the evidence of studies on the kinetics of
precipitation processes. The extraordinarily regular shape of the
cr:istallites proves that t-?e nuclei, too must be regular and sym-
metrical in shape. In some cases there-is evidence of two-stage
nucleation, with the symmetry of the largernucleus clearly dis-
cernible (cf. Phots. 15 and 16). With a view to obtaining a con-
firmation of the visual observations and tne view on the decisive
role of nuclei in the growth cf crystallites, experiments on the
following lines were made. Barium 7hr,mate was precipitated during
24-48 hours from a solution of potassium chromate according to the
technique and in the apparat-is already described. The solid was
filtered off, and precipitation was repeated. in this say a num-
ber of fractions of the precipitate were obtained, which differed
from each other distinctly in character. As a general statement we
may say that the first-formed crystallites are invariably .much
more diverse in form. The course of the phenomena observed during
repeated precipitation from the same solution ccrroborate the
surmise that crystallites form on nuclei, which consist of the
natural impurities of potassium chromate. Identification of some
of the nuclei will be dealt with further below.
Another important observation concerns the stability of the
crystallites. They are rather resistant to mechanical action, ani
kept in a solution they undergo no recrystallization. Varioua
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samples are kept in our laboratory since over four years, but no
changes can be noted. The crystallites may be safely washed with
pure water, dried, and stored. In this case too no changes can
be noted, which shows that the crystal lattice 'produced is the
most statics under the conditions described.
While the present work was in progress, another was started,
jointly with R.Przytycka, on co-precipitation of radium and barium
chromates. With the same idea on the formation of the solid phase
in mind, the technique described ia the present report was employed.
In this case barium ohromate was obtained in the form of simple
straight prisms [72]. Inside these crystals there developed two,
sometimes four symmetrically arranged spots (Phot.17), considered
first as gam bubbles, which eventually burst the crystal(cf.Phot. 18).
Hence, barium chromate crystals probably form on nuclei provided
by microcrystals of the less soluble radium chromate. In the course
of radioactive fission, radium produces the so-called radiation
lamag?, which gives rise to the observed "gas bubbles". In the
earlier stages of the process, and probably also when the amount
of radium is exceedingly minute, merely two dark dots are noted
instead of the "bubbles". Owing to their characteristic appear-
ance, this kind of barium chromate crystals are readily distin-
guished from others and identified (Phots. 19, 22, 23). They are
now the subject of detailed investigations.
In the course of work on multiple precipitation of ordinary
chemically pure potassium chromate, the removal of several frac-
tions of crystallites was invariably followed by the appearance of
the simple straight and characteristic prismatic crystals of the
"radium" type, which showed evidence of similar radiation damage.
This suggests strongly that the commercial "potassium chromate"
reagent probably contains a minute amount of radium, possibly de-
riving from the chromite ore. Por instance, industrial chromite
ore (source uncertain) has been found to contain 0.0008 percent
of uranium, consequently also a corresponding amount of radium.
In some experiments foreign ions, such as Ag4 and Wo04;-
were added. With Ag"-ions, characteristic shapes were obtainei
7
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which indicated the formation of double crystallites (Phots.20
and 21); with molybdenum, crystallites of an altogether differ-
ent shape were obtained (Phot.8). The poin %nether these
shapes are characteristic for mdlybdenum or the impurities in
its compounds will be the subject of further investigations.
To microscopy, attention MRS attracted by the fact that
crystellites similar in type are often found in clusters, even
th,a1h the microscopic slide was prepared under conditions favour-
in g uniform mixing of the crystals. The only possible interpreta-
tion of this phenomenon was that the perticular nuclei, and sub-
sequently the crystallites were formed on some basic binding si-
milar nuclei. Investigations have so far shown that this base
might he pro.fided by organi- substances (cellulose from filter
paper ,r to products of zelluloee desctruction), the fibre pro-
viding such a base tel rig invisible u.nier the microscope. In other
caee thc base is provided by amorphous substances (e.g., hydro-
xides). If th ;recipitate thus produced is not removed, the
cryetallitee continue to grow, producing eventually what is known
in analytical chemistry as "flakes" (see Phot.24).
The investigations so far made have th shown tnat:
(1) conei lerable slowing of precipitation makes it possible to
obtain crystalline solids.
(2) the decisive role is played by nu:lei, w,,i7h consist of foreign
substances,
(3) different nuclei are not invelved simultaneou.ily but in a
certair order of succeesion,
(4) the method employed in the present investigations makes it
possible tc observe the process of nucleation and precipita-
tion in stages,
(5)
the method employed enables the nuoi consequently disc, im-
purities, to be eliminated 6radually, an,.1
(6) the method enables the nuclei, donsequently ate? traces of
impurities to be iientified.
The author is very much indebte4 to Kr Lech TROJANOWSKI for
his patient aid.
6
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Ref?renc??
T.Adamski and ?Atucha. Sprawoziant Instyt.t, ??: ettn-
nicznej ( Report cf the Insti tute Inc.ranit
[2] E.P.v.ef-titarn. Gran 1?,.iv,P i?r f'.aDerstl dcncc.1 e.
:3}
P. .11^1 zern, 7,1 r Ler-e yt:r. !en Z1ele: lie
1`i14
R.B. El Lizher, Ansi 1,?5,1
S.l'cf, E.Netzmann, Ind -Eng ..:hem Anal .Ed. 4, A;
R1 syr H.Agen :n1 7:cerz... Anal .F.1 '4 ,
Mer V K,:-.)17:1,cf,ar P.R., :
[.9)
00
0,1hnsci. R.A.. Clicurke
11.6., Aa 'hem.Scand.,
inkcva 1., :num Neorg. ELim. -o3.?'.'`..7..??
10r1(.,11 .27 Burt: Af.s! .
;
( 95'. )
L. Ar.al . Chem. ? 1704 (.1'3551
3:
Jordon L., A na .;:hert , 195i, "
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?I raching ? 1. 2, 32b t.1953;
(15;
lerdor, L., Saiutsky V .L. , 1r1 lard H
tic,n Methods N - London 1959
[16)
Nightingale E. Ft,. jr. , Benck H.?.. Anal . :hem.,
117]
Burrus H.:..J .Appl .Cli es. , 11, 376 (1961)
[11:g
Cartwright 2.E.S., The Analy et 86, 688 ;961
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'6`
(19]
Dams R. Host e J., Talanta, 9. 6C4 09611
(20
ireching P.11., en., j,. 873 (1.961)
(21
Pireehing ? . H . , Anal .Chem 114 (-96'
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Norwitz 8., Anal .Ches. , fl, 31? (1.1611
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Nielsen A.R., J Sri., C, 574 ,1555
[24]
O'Rourke J.D., Johnson R.A., Anal ;Chem 27,
V
5$
(25)
Sloan C . . , Phys nuns , 934 19'05)
[261
Collins F.2., Lei neweber J.P..
oC,
a ?
[27]
Lucchesi P.3 . , j.Conoid Si.. 1' , -)56
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Hahnert H., kleber W.. Icc, 1 lo..d 1o2,
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Howard J .R. Nancollas , Pur?f.i e , Trans
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Itt, 278 1,19603
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[3o) Jaycock Parfitt G.D., ?Dette.taraday Soc., 5,2? 791
(1961)
[91] Fischer R.B., J.Chem.Xduc., /i, 484 (1947)
[2] ?lecher R.B., Anal.Chem., LI 1667 (1951)
[33] Pischer R.B.. Anal.Chsm., /i, 1544 (195))
[341 Suite E., Takiyams K., Bull.Inst.Chem.Researoh, Kyoto Univ..
88 (1956)
[35] Vancollas 0.H., Furdie W., Trane.Paraday Soc., 5,2_, 2272 (1961)
[36] Bao 0.. Longuet-R.eard J., Journ.Chim.phys.biol., 11, 434
? (1954)
Daj Powers 1.E.., e.&Ind., 1962 .627 (7.4.62)
[38] Gorbakhor S.V., Shlykov A.Y., Zhurn.Plz.nim., 21, 1777 (1956)
[393 Fischer R.B., Anal.Chia.Acte, 22, 501 (1960)
i40, Fischer R.B., knal.Chic.Acta, 22, 508 (1960)
[41] Fischer R.B., Anal.Chem., 1Z, 1127 (1960)
[421 Klein D.H., Gordon L., Walnut Th.., Talanta, 1. 334 (1958)
[45] Klein D.H., Gordon L., Walnut Th.H., Talanta, 1 177 (1960)
).1ein D.H.. Gordon L., Walnut Th.H., Talanta, 1, 187 (196c)
_45] Haber.. N., Gordon L., Fischer L.B., Anal.Chem., 22, 1901
11961)
[46] Mullin J.W., Raven F.D., Nature, 190, ?51 (1961)
47 Chlopin M.G., Isbvannyje trod, Akad.Rauk SSSR 1957
[48] Cranston :., Phil.Mag., /5, 713 (1913)
0191 KcCoy H.K., Viol Phil.Mag., j, 336 (1,)1))
tiG: Rutherfcri F., Phil.Mag., 26, 938 (1913)
[51] Hahn O., 6rbachor D., Phys.2eitschr., j, 4, 531 (1926)
,52] Icsanowitcn D.Y., J.Ghiw.Phys., LI. 1. 3 (1926)
[53] Hafesinsky K., C.r. 196 24, 1788 (1933)
154j Erbscher 0., ingew.Chem., All 1, 6 (1947)
i551 aalutsky V.L., Stites j.C.jr., Kartin A.R., AL&I.chem., 25,
1677 11953)
062 lerkulowe w.S., at al., Dok/40tad.ltauk SSW 102, 1167-9 (1955)
[57] Popov M.A? 2avodekeya Lab., 21, 1430 (1955)
[58C: cordon L., Rowley K., Anol.Chew., /1, 34 (1957)
[55] Gordon L., Ginsburg L., Anal.ch.14., 22, 38 (1957)
B-Jrk R., Kernenergie, 1, 1204 (Dit.1960)
IC
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[61] Mame R., Yernenergie, 1, 429 (1960 - V)
162] Cohen A.J., Gordon L., Talantb., 2., 195-211 (1961)
[631 Jogorov,Tu.V., Pushkarev V.V., -t al., Radiochimia,
87-96 (1961)
[641 KrawczyTiski S., Kenellakopules Atomkernenergie, 6
214 (v.1961)
[65] Mc Lane C.N., Pe:erson 3., Tr-.Uran.El.met.ts, j, 1388
(1943)
!66] Mortn R.E., Nature, 192, 72? ',25.11.1961)
?
[67] Rudnev N.A., ar,c1 Malofeeva G.i LI, 453
(11-1961)
[68] Seifert H., Cheo.Ing.Techn., ?210 (1961)
[691 stepin B.D. and Pluschev V.E., 1.h.Neorg.Khim., LI, 462
(11-1961)
[70] Weiss N.Y., Ming Gon Lai, Talanta, gb 72 (1961)
[71] Adaoski T., Rykowski S., Polio,: Acad.Se., Inst.Nucl.Res.,
Rep. 91/TV (1959)
[72] Adaoski T., Przytycka R.. Polinh Acad.Sc., Inst.Nucl.Res.,
. Rep. 266/IV (1961)
[73] Adamaki T., Mature, 222, 524 6.5.1961)
Rote: Photos Ro.4.7,8,9,11,14,1507 and 18 have been
performed by the auth'?f, in the VB-Carl Zeiss-
Jema /last Germany/ latatories by means of
thekneh indebted to 1?.1.3-aar1 Zeiss for this
kind assistance.
11
50X1 -HUM
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Phot.l. Barium chromate obtained by
conventional precipitation.
Phot.2. Barium chromate obtained by
very slow precipitation.
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Pt1OT.3. Maracteri'ltiz -t-ape cf Le
Phot .4.
Characterletic shape of the
crystal.
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Phot.5. Charaoteristio shape of the
zrystsi.
Phot.6. Tharatterlstio shape of the
cryw:al.
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Phot .7.
Characteristic shape of the
crystal.
ki,',7,.--44 A
Phot.8. characteristic shape of the
crystal.
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Pbot.9. The shapes are reproducible.
Shot.10. The shapes are reproducible.
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?
1
Phot.11. Crystallite with nucleus.
Phot.12. Crystallite with nucleus.
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?
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Phot.13. Crystallite with nucleus.
Ihot.14. Crystallite with nucleus.
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?
Phot.15. Crystallite with double nucleus.
Pbot.16. Crystallite aith double aucleue.
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1111111-11
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CIA-RDP80T00246A023700140001-3 rPrirr' r'71brIrT'7
,
Phot .17. Narita ohromate crystal with
radium nucleus. Note the "radia-
tion damage" caused probably by
radium.
Motile. Marius chromate crystal with
'radium" nucleus. Not. the "radia-
tion damage".
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Phot.19. Barium ohromate crystallites inter -
spereed with "radium" crystallites.
Phot.20. Nixed barium-silver pryttalite.
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Phot.25. Apparatuses.
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Pig. 1.
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.014
1 A I I. H 1 Mardi 2. I9E):1
? 1 )1.1 ttl It I /111111.t CCM!. ? ..p.? h 1? 141,,?f It i
onglotnerntt,. 1.?:?
modern aspeet an ii.1,1\ Is. .1,ifs wheel li?ii
lie nonvoting) of 11), t 1?41111,0 f???fiIOIII..I III
11.111,4 of abnormal .0 11.,14111.1?1 I 1?1111?11114?1/. Th.' hit ?????1
VI (Irk on t he S,rrifi 411.141.4 ele?nr1 that
illS 111.1)0?11t is not af Ills is1. lIlt t Ilitt I,,nottera411/.40 ii, ?511.1.
1.robt41,1 f?inplareii li.111,4 The nim.i.rit k
l'11\ 1?1141 It1114,INII (111..114 Of 6.1111,???( 14. gold ornitolon
own', the locality of .s hi, vit boon rt?vonit.01.
exhibit bet It 1?1111 11?11111.
(magnetite brannerue ? sante conglomerate.
ere.body densinst rui 'rat 1,?\ ? 41.: ? 41?4.10% of ILIUM, that
he mineral amanitiltio,zon Mn' ii hy itnitherinal .irlg in
The ort hist., geelogii al 1.11(,,pti,mg on the history of
attisisi.het, ha, c heen reviewed by A. 1'.
Virtofzradov` itt his Vemiulsky Memorial Leet tire. in
%shit+ ht. concludes that the prints-tat atmosphere of
methane, hydrogen and eartsm dioxide (akin to the gases
of meteorites and of tern-anal nicks of mantles origin sorb
es kiniberlitem. carbonatites arid iiiii test lasted only a
rebstively short tittle Probably it wee lost in the 1.000
million yea/1i of the Earth's history before the earlieet
known roeks came Imo being. A. A Polkanov' has lately
observed that even for these earliext Katereharvin rocks
of 3.500 ntilliort HEWN ago. Lyelhs principle of actualisti
illay not. and should not he ri?iceteit
1' It DI\ 11.4.0*
1)elisutrrietit of 0:eulogy.
l'niversity of St ..1.11dreu s
' . 11111 K.S4 1151011i
' 11.6414?4411. V. V . Nno. and., SC file 411W.",. 64 na: 11.145 113Sn* 14
1316 (14651t Ainoar Afar M. 73. I 10431 1641 tr..t .1w.o. lie .4
(IWO).
? White, Y. ii. Server Ites..,64 aur, .
aahlagton iIi 1961t
? *441tvoarv, V. i .44 koralPas.
(OniareoltaLlar4al )11041e4,14 1641)
1 Vliagradnv. ? r EllawarAnAmera R.44400:46.4 i.a44/. 4414.1 N ?*1
Noaat.nr. use
? 1`.466auir, A 1.. I ar.adot CaakArannl**** I ? *Alma aaa Morrow
10411
4,*
Tux origin of early Precambrian gold uraniutn or,
deposits ham indeed been a cent mversial issue. Hut. he 1
stated euli: d
tly in my book. I have become eonvinee
that the feature. acquired by hydrothermal processes are
doe to younger alterations. These deposits are placers
iiriginally. The hydrothermal alterations have heist
important in enriching the original placers. They may
even be at t be origin of the money- value of a given depoeit,
and consequently tarn as the roost import ant proems by
an economic geologist.
M. t ; . Ilt-ereN
Minertilogieal-t;eological Instil e.
I.?niversity of Utrecht ?
CRYSTALLOGRAPHY
Commination of Crystal Nucleation by a
Precipitation Method
Tneas are two way!, to precipitate sediments of slightly
soluble salts, namely. by simple mixing of the reagents or
by the homogeneous mothod, that is. by developing the
reagent in situ and thus precipitating the insoluble salt
homogeneouslv in the whole bulk ofthe solution. In both
eamean0 special care is taken with regent to Illicleot ion
the parameter of t 1101.
The formation of ii sediment of an insoluble salt coin-
imam two }Jame prOeemses. I be character of us hich is quite
different : a clietineal proci?ss In, oly ing t he format out of a
new compoimil of t he ions ex ee me in or introdueeil into
the sollition. and a phy sical pr 'ii." of solid phase forma-
tion. Different kinds it g.?iii?ral .1?41.11W. comprising
extreme and intermisloite aro twtrig eXttinnled. The
11?1?1?'? ????? .14 11,1 :?1111?1?11111.1 1..n,,,4t in
? ??? . lit.141? ???..k1 !al ????????? ??? /0.1 ? i? ? ?? .141?1 I It'l
?it?It??111t1114; .111 .?_????itt ?tell??? 11.? ???? did t??
1014 Milt,' /I, WI .111..1140.11s I it ,iI I 11.1.t us. Of 1??????1 is ? II I. ? ?I
,.I us! hat 11 .?1. 01 I t ,11?111110,
The mini (Jul. 11, 1111? h11,% /Mite!, 55)!!. I
ti??????li?)???11. IA to porborto Ilit? .110.111eHll 11.14 t 3??I1 ?(???
1111 44.e0+.11 4 II) (4,i11?111 R ?A??ll 111.41.11r4.11 4111111 11114,1???
ttlIon? torin t sc.ht14,11I su..h iu b.11111...
11111111 rit?l1 11 Uhl 11 II, 11/40. ?? h?????/.
-.1.t 5 44(i'
N,,44 1,111 orts hale, 1,4 gill,' I fial
(11 l'14114111/t4( on no,4,,, a? ***.o. It ;?
sitmoo eL mass of only I ' or smalli r
(21 .1 great. hitt limited. number ot cry stallite 4111.pon al**
?Naimoli. 'nu- +intim. depends t nucleus all 111111 it., .1
venire of cry stallizat ton.
(3) The different shoiron ant ohtiiin4nt tumult tititantal
44111141 shows that pea the 141)44.1th. properties of the to if.''
aro re?gwinsibh, for th...shape and hot t he properties oft he
nusiiiiin, for example. t el incentrat u. un. sorfacii tensein,
1,H. etc !Fig. It
lig. 1 4(10
(4) While introducing small quantitien of foreign ions
the basic precipitate tieing barium chromate) crystallites
of quite different shape are obtained. Hemline of the lack
of separating methods it could not be established until
now whether they were other compounds or other crystal-
line forms.
(5) A fractional precipitation performed with the aid of
the new method removes the existing nuclei. On further
precipitation the number of crystallite forms diminishes.
(6) In spite of their very delicate structure the crystal-
litea are very stable. It has been stated that sediments do
not change while in contact with the mother liquor for a
period of even four years. showing that the solid phone has
been formed under conditions enabling the building of an
ideal crystal lattice, that is, ? lattice of lowest energy.
(7) Obeervations have shown that nuclei formation
proceeds possibly on amorphous matter of indefinite
eomposition (hydroxides t. silica 7).
I thank Mr. L. Trojanowski for assistance in perforiminz
Os, experimental
T. AtiAmsini
I iepart 'mint of Chemical Technology.
Institute of Nuclear Itemearelt.
\ arsa .
Adantaki, r anal It?konskt. It.. War4a4r. Rep %I ? 91 4
(11?61t,
Aolantaki. T., Nonorf. 144 ;..14 tl n61).
? Adantaki 1 ant Pun wax. It.. N'ad InAi. II otw.... ner. No 1:444
(1541411.
4
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N. 45, NI:it-tit 9. 1940
N ikTURE
tra?
4
r
F I. I. lim.144144444 idrert on tiN4 444 pen. se of thw. ets411441. Open
Hu*. l'14,444441ty ,41 nallve 147i A eknort Mirk*, visoottitY of the 4410.14.-
,1/44141,41 UN A hatt-50e4 dries. breaking of the h)droiteo
4141) 14.4. molt 1),4TA In 001 M itldluta eitioride
10 /2
IS
dose rab? : 3.150 r We also determined the amount.
of open hydrogen bomb; in the native irradiated DNA
aceording to a method described in an earlier article'.
The viscosity of the native DNA and the hydrogen
bon( Is between the t wo strands have nearly the .an
radiosensitivity; the Le,, in about 30,000 r. After severs-
tem of the strands. however,. the 'viiicoeity drops to MI
per (4.1It after 500 r. The, doer effect curve tiepins to hAve.
two eorriponents: one with D1,. of 700 r., the other with
1),, of 1.500 r. The two components of this mires toss ho
discussed in a similar way NA Latarjet elnif ? dad when
eonsidering the inactivation of the transformirut factor in
the DNA, where the f)?-valitee of the two components
also have a ratio of 1 : 4 (1.000 and 4.000 kr.).
The breaks of the single strands are permanent in native
liNA over a longer period If the DNA is denatured only
:4 ti after irradiation id Mist r . the votectrot of the isms*
strands decreases to to per rent of the control tostend at
50 per rent. This meson that then. is a small 'after effect
of the irradiation.
If DNA in first denatured and then irradiated, the loos
of viscosity Is very small. After 1.000 r., tie change of the
viscosity was observed. The Nallle effect has hewn de-
scribed by Memoir ts/.' after irradiation of DNA with
ultra-violet light. The high sensitivity of the single
nucleotide chain in 11/1114V0 1)NA might be explained by the
fact that the target volume in the stiff double helix is
larger than the target in the eoiled single-stranded DNA.
tiAttEN
Radiologist-hes Institut der l?tiivi,raitiit.
Fo?ilairg un lirettwito.
Prac44,144. A. it. .helw IS. 10010) 11?V0ItriPf, P
set Stn4A.t A.. N44445 ?jo4433. FourtA t. Ilr.rrile.
9/4
Huller. J. A V.. /44/../ /1,4 4 211111*:011.
MAreittir..1 . Enti44,..1 .4,4411,1114 /mil 4'. /4.44r. / ? A 4/. Arad.
, II. 481 11440144
' Env. E it. M. N111111.1, N. ?. .444.1 144044,-. ./ A ter,, 'Arm .
14. 1724 4141:424
' Itattre. I `..totre. 1114. 1
? 1.40.404.1 It . I .4.144,44441?1'44 144e II. 404,1 It, I,. /441. N. 1004 Beg 11
417
'11arrutur. .f.. '1 lid/ NAM, SI F Slat Fi...a? I. 114.rn? I. 4404,444. E..
1.41144?. I. , I A .I1 I. ./ p I yood ,74.11,1? I II II 1117014,
RADIATION CHEMISTRY
Possible Radiation Damase Effects in Barium
Chromate Crystals
Bum m (411,,111101. 1.11b11111.41 the 1110110d (.1altOrtill,41
III our loltorittor:., forms crystallites the shape of IS Itteh
leponits on this kind id nucleus on whieh the crystallite
lits been finmed. Under special ermilitions. for eX111111ple.
Is fraetionid precipitation using the satin method or by
preeipitation bona dilute solutes's. reagent grade potas?
to
111,11 cob.
1005
rust. 400
rust.
sewn chromate produces ardimenta of prismatic-ehaped
barium chromate crystallites having a rhombic cress-
beet ion.
Very afire it hoe been observed that two elliptisal 'gas
bubbles* inside the prisms were formed. Crystallites of
smaller size show two 'funnels!' on the ends. instead of the
'bubbles', while others show only two or four dark point.
(Figs. I and 2). A similar feature was observed by us
earlier, while precipitating barium chromate (rota solu-
tions oonteining uranium and radium. Observations
tiercribed elsewherro-* show that crystallites are formed on
nuclei consisting of foreign substances. It is supposed
that, in the Oa*, rot-embed here, barium chromiste crystal-
lizes on isomorpholim radium ehromate nuclei, truces of
radium coming from lira and thorium always present
in chromite ores.
llie radioactive of isolate causes strong radia
lion offeets sinitiJar to those iiimeriboil, for example.
by Yoshida. and Vineywrit'. The great energy of the dismay
us also the eimcont rat ion oft he sourer.- -that is. the crystal
niieleos prisbireol Offee4.41 sufficient ly strung as to bii ii.. I,).'
microseopical obeervation. Also it has been
shown hr its (by slightly levering the tube of the mime.
seols-) that the er manioc substanee in the vicinity of the
'nubble' is of greater optical density and acts OH a 1.44g1lialf
1414141411 14.t1/4. 1/144444 01)/4/4r4-tationm tit very well to t he
feat 11054 of vacancies and interstitial formation as postii?
lutist for rnAboartivity effects in crystal lattiten. The
'funnels' already onsitioried have been observed on very
small objects 5 7? long. This fact omens to be in aceord?
onee with a ? ler eirect described for iirsttitim metal by
Rogers and Ailsins'.
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- _
11106
N A T (1 R
III WHIN. 0141.e4' II 101111I0.4 010 ks radinteiti
dlatilrato effects hake treee lIbtalle`fl. When, no further
charigrv emelt' be det.s telt In other coals, en-stolid...A of
exactly Oa. smile shape slim% eil in efforts of thin
DILITOfetleeti. aPi sueli, VAIl be asirilsat If. he different SIZAMI of
radium chromate nuclei. or to difh.root radIuM Mot opeol
preaent , 1 hat el, radium 224 - 3 64 1. 4. rrviiion-226
tb= 1620 y.) and radium 22., (le - 7 y . I. strorigeat
damage IN exported ie radium-224. Many
(Aber ofteerx alums itarolo an. in HIll 141.1.11ralinf.4, e, ii Ii t lin
imorpretation of facts pr.se?nteil here.
I. .tPAN1,41(1
1, ['WO I
Department. of Chemical l'eclinolow-.
Institute of Nuclear Research.
Warsaw.
' Adaniekl. Nolan, 1.11, 524 (1960.
? 44?Niskl, T., Nature. 117, $94 (1963i.
AddinNia. T., Nati Res. Inst. Warsaw, Rep.."', 762 4.
Adakl. T., Arid Przytyok.a. R.. Ilocznilti ('k /POI (Warm., 1111 541
(law) (In French).
Ecelokila.c.. j. PArg . See., Japan. 1.11. 41 (14011.
? 1latintrd. O. H., bile . Paea4. Sae.. SE, 7 (1961).
' Rosecii.41. aai Adimi. .1.. J. Nod. Mal.. S.
CERAMICS
A Simple Flame Fusion Apparatus
Tar need for large single eryntaiu of refractory oxides
has been ever increasing in recent years in many innilan?
ere further technological advances are being hampered by
the lack of materials of suitable punt. and perfection.
(Mn of the major Notarise of containuots ion of nutterials
prepared at lugh temperature is the coessatrier in ',ha+ th.,
nattered is heated. The flame fusiot, technique is orss
high-temperatuns crystal growth method Prim+ over-
aucare the tamtearter lirolArion iso the ranterent wirier seven
tigation acts as its own *import I rat her eweissilos.
review of the advantage*. anei
fLittne fusion furnaces is given l, Popos'us. a tia.iik
by Shubnikov and Sheftal.
This communication &writes a simple portable flame
fusion apparatus which can he constructed in most
laboratories with readily available materials.
The apparatus consists of three major components: (I )
the feed hopper and burner assembly; (2) lowering
mechanism: (3) tbe gas system. The usual feed hopper
amembly consists; of an outer and inner hopper. The
inner hopper is fitted with a tine mesh sieve which is
vibrated by a tapper mechanism for control of feed flow.
A new design of a one?botiper feed assembly has been
incorporated into a dame fusion apparatus. In this
version continuous and uninterrupted food rates are
acconiplishedt. The hop,s'r is designed such that
conniben?ially available Iiiirtii.r assemblios can he oars( ruid
interchatigesi ad!) elk-4e.
The pet-le/dal on a hi-li the rystal a growii intuit Ise
Invensl at tt, rate equal to the grewth rate of t le- crystal
In addition the rate of lia?ering mine he %iir/ablo to
coincide with slots- or rapid (.1". growth It is ver:.
important that the lowering mechanism transiec as little
vibration as porsohlo to the growing erystal. .? compact
and x?ersatili, lowering mechanism ma./ designed to elimi-
nate the difticull ion usual h encountensl. A variable-no-led
il.c. motor and it gear train system permit the growing
bold., to he Inwered in the contin range from zero to
4 in. per h. 'Flue I. airing illerflailiS/11 is equipped with
allinileporideritl NO tn rile rotation mechanism which
can rotate tint!) e. tIii'lui,,> tO MO c.p.m. by suitable
elmie., of gears and tniaiirii. The bonging for the lowering
new/Innis/1i is shrwk mounted arnf can be positioned by
1110411K 01 IS t WO-4111111.11si,mal slide rt 'at. A schematic
lutsgrann of' !fie and rotation niechanirun is
shown in Fa, I
- Cmrtiti7incl
March 9, 1963 yo, 91
HouDER FOR
. .I- REFRACTORY MATEPIA1
ENTERING ruakacr
31 "1
f
1.1
I
(2)
ROTATION
GEAR 80X 7'
0
PINION ROO
I
_1 _
- ? _
TEFLCSI ROD
Vitab Mat
?DRWRVIZE
GEAR BOX
1
11.L Lowering arallarillm
717.,
I
*%-?
CEINAINIC
CASTS%
- ?Oa suaNens IN
TOP VIEW 2 CaKtis ciF 5
0
SECTION 4-.4
Pb.! AsuieitlIng turns..
A refractory furnace muffin with tongue and groove
joints was eastfront 33 HD alundkun (Norton Refract
Worcester. Masa.) to contain the heat source. An &distort
tion of this muftis has been designed as an annealing furn-
ace to reduce the strains in growing honk* by in situ
annealing. Thin furnace consists of two rows of five
burners each Using oxy.hydrogen gas. The burners arc
positioned and the manifold east in a refractory muffle as
shown in Fig. 2.
(-A-my Approved for Release 2013/08/07 : CIA-RDP80T00246A023700140001-3