ocr/ORNL-0629.txt

—— ~ ORNL 629

Reéactors
Progress Report

LABORATORY LIBRARIES

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Fape K QUARTERLY s

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FOR PERIOD ENDING FEBRUARY 28, 1950
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This document has been reviewed and is determined to be -

APPROVED FOR PUBLIC RELEASE
Name/Title: Leesa Laymance, ORNLTIO
Date: December 21, 2015

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UPERATED BY
CARBIDE AND CARBON CHEMICALS DIVISION
UNIDN CAHB!DE AND CAREDN CORPORATION
PDET DFFIBE BOX P
GAK RIDBE, TENNESSEE

ORNL 629

This document congists

of 48 poges. Qapyc.?ﬁ
of 148. Beriezs &.

Contract No. ®-T7485, eng. 26

AIBCRAFT NUCLEAR PROPULSION PROJECT

ati
Gak Ridge Natioms! Laboratory
‘ 2
¥-12 Research Laboratory

A. B. ¥%einherg, Projeci Directoy

QUARTERLY PROGRESS REPORY
for Period Ending February 28, 1930

£, B, Eilis, Editovr

Diate Izauad APR E 9 T?E;U

BAE RIDGE NATIONAL LABDEATORY
eperated by

CARRBEIDE AND CARBOR CHERICALR DIVISION
nion Carbide and Carboen {orporation
Posi gffice Box P
Gak Bidge, Tennosses

INTERNAL DISTRIBUTION

1 G. T. Felbeck {(CACOC) 27 A, M. ¥Weinberg 43

2.3  T06-4 Library £8 K. Z. Morgan 44

4 706-B Library 29 J. 8. Felton 45

5 Biclogy Library 30 C. E. Winters 46~ 47

& Health Physics Library 31 d. A, Lane 48

7-8  Training School Library 3 Go . Boyd 49

.18 Central Files 33 B. ¥%. Stoughton 50

19 Y. A. Swartout 34-3% F. L. Culler 51

20 J. H. Gillette 35 Do G Bead 52

21 4. Hollaender 37 A. B, Householder 353

59 I. H. Frye, Jr, 38 F. L. Steahly 54

a3 E. J. ?s%isrph}* 39 Mb M. Mann 55

24 C. B, Center 44 A, . Snell 56

an ., ¥, Larson 41 F. £, ?ﬂnderi_,age 57

34 W. I, Lavers 42 C. B, Grabam 58
59

EXTERNAL DISTRIBUTION

60-~64  Air Force Enginesring Office, Oak Ridge

5576 Argonpe National Laboratory

77-7T8 Atomic Energy Commission, Washington

79 Battells Memorial Institute

80 Bureav of Aeronautics

81~-84  Brookhaven National Laborstory

g5 Burean of Ships

86 Chicagoe Operations Office

87-80  Genweral Electric Company, Richland

23 Hanford Operations {ffice

G293 Ydaho Operations Office

94 fowa State College

85-88 Knolls Atomic Power Laboratoery

89-101 Los Alamos |

102~ Massachusetts . Jnstitute of Techuology

103-104 National Advisory Committee for Aeromautics

1035-113 NEPA Project

114 National Advisery Committee for Asronantics, Washington

115-116 New York Opevations Office

I North American Avistion, Ine.

118 Dffice of Naval Ressarch

119 Patent Branch, Washingbon

120-134 Technical Information Branech, (ORE

135-136 University of Celifornies Badistion Laboratory

137-148 Westinghouse Elesctric Corporation

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ORNL 629

Beactors

Progress Report
Humes {K-25)

« Engberg

Lvon
Ellzs

« Gall
. M.
. Kerge
. G
I
s P
M.

Jones

Miller
Billington
Blizard
Breazeale
Frgen
Clifford
Nelson
Leverett

Central Fileg (0,93
TABLE OF CONTENTS

SUMMARY

SHIELDING

New Bulk Shield Testing Facility
Lid Tank Bulk Shielding Measurements

Water attenuation
Source powsr
Lead-water measurements
Navy H,0-Fe-Ph-shield

Instrunents
Pd Film Fast Meutron Detsctor
Neutron Energy Spectrometer
Shielding Analvsis
Shielding Materials

Uranium hydride survey
Plastics

Concretes

Portland cement-iron concrete
Fxpansivity experiments
Radiation damage tests
FEguilibrium woisture tests
Fabrication of Boral {B,0 + A1)
Plumbor™ (B, C & Pb}

Beports Issued

HEAT TRANSFER

Heat transfer theory
Experimental heat transfer
Ligmid metal pomps

Liguid metal bhandbook

METALLURGY ARD MATERIALS

Static corrosion

Lithiom handling

Lithium perification

Dynamic corrosion testing

Mechanical testing

Fffects of alloying elements and structural factors
Protective coating of high temperature materials
Circulating fuel systems

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21- 4

Reactor Core Material Studies

RADIATION DAMAGE

Accelerator experiments
Reactor experiments

Auxiliary Material Studies

High intensity gamma gource
Radiation stability of plastics
Radiation stability of metal hydrides

NUCLEAR MEASUREMENTS

THE CONCENTRATION OF LITHIUM ISOTOPES BY CHEMICAL METHODS

=

Molecular distillation of lit hium metal

; Chemical exchange methods

Ligquid-solid systems

Liquid-liquid systems

Continuous countercurrent electrolysis
Continuous countercurrent electromigration
Thermal diffusion

R R e

32

32

32
32

33

33
38
38

44
45

45
46
46
46
47
47
48
iy

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12

LIST OF FIGURES

100% H,0 Meutron Attenuation

100% H,0 Gamma Attenuation

Meutron Energy Spectrum of Mock Fission Sourcs
Neuvtron Energy Spectrum of Po-Be Source
Corrosion Capavle Assembly

Gold Lined Cup

Pneumatic Tube &pparatus

Pneumatic Tube Apparatus

Prneumatic Tube Apparatbus

Source Shield

Dissosciation Preszure of LiH

Migsociation Pressure of Zrﬁﬂhgg

3

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Heat Tramsfer. An experimental rig for heat transfer studies with lithium
at 1800°F is being fabricated from stainless steel, type 347. A canned rotor
liquid metal pump is also being constructed, using a liquid film bearing.

Metallurgy and Materials. A number of static corrosion tests have been
made in which nickel, zirconium, iron, tungstem, tantalum, molybdenum and
columbium have been exposed to liquid lithium and bismuth for four hours at
1800°F. The next series of tests will be conducted at 1800°F for 40 hours.
The first results with liquid lithium indicate best resistance in iron, mo-
lybdenum and zirconium; however, the data are still very preliminary. The
question of purity of the liquid lithium is now under study. With liquid
bismuth, zirconium was severely attacked.

Dynamic corrosion test equipment is now being constructed for measurements
under convective circulation conditions in liquid bismuth and lithium. Cor-
rosion._harps are beiné made of various stainless steels as well as V-36 and
L-605 alloys. Equipment is being designed for stress-rupture and creep tests.
Preliminary tests are underway to find container materials for liquid uranium-
bismuth and uranium-lithium alloys.

Radiation Damage. Accelerator experiments to determine radiation damage
"in various high temperature materials will shortly get underway at Berkeley
and at Purdue. Various high temperature materials will also be placed in the
Hanford reactor soon. An experiment is being designed for simultaneous
radiation damage and heat transfer tests of circulating lithium system in the
ORNL reactor,

A high-intensity gamma source has been developed for use with the ORNL
reactor, This is ahollow gold cylinder, which after irradiation for one week,
produces 10%,z/hr upon materials at its center.

Data on change in electrical properties of various irradiated plastics are
presented in this report. Preliminary measurements have been made on the radi-
ation-induced dissociation of lithium, titenium, and zirconium hydrides.

Nuclear Measurements. Preparations are underway for the neutron cross-
section measurements needed in ANP work. These will involve use of a 5 Mev
Van de Graaff accelerator and a high-speed mechanical velocity selector.

L1’ separation. The work at the Y-12 Research Laboratory on the practi-
cality of obtaining EEEEEBEFlots of highly purified Li’” by chemical methods is

discussed in this report because of the possible application of this metal as

an aircraft reactor coolant and moderator. | Separation methods under study in-
AT TS ET T e ISt~ 0T L1 metal, 1on exchange methods, countercurrent

electrolysis and electromigration. The most promising system so far is a

uae . mo

liquid-liquid exchange column using dual-temperature for continuous opération.

3

!
SHIPLDING

NEY BULK SHIELD TEBTING FACILITY

¥. B, Breazeale, J. L. ¥Heem,* B, P. Blizard

A proposall{is?} reguesting permission to build a new bulk shield testing
facility has heen transmitted to the ARO., The initial reguest was sent on
December 21, 1949, and a supplement on February 10, 1958, Formal approval has
net yet been received.

The proposal described a critical assembly made up of MIB fuel units
sperating in & pool of water which also contains the bulk shielding samples.
This low power, water cooled snd moderated {pavtiallyl}, bervilium exide re-
flected resclor serves as a fission source for seutron and gamma ray attenua-
tion measurements through bulk shielding sawmples and through mock-ups of practi-
cal shields. A maximum opersting power level of 10 kw i1s suggested.

Caleoulations by E. Greuling and M. Edlund indicate that this reactor is
inherently safe. They have investigated theoretically the result of instan-
taneously adding 2% Ak {effective} when the resctor is just critical and
operating at 10 kw, The conclusions are that it will oscillate at a mean power
level of not greater than 130 kw,

Reactor control circuits will be similar to those now under test in the
MTR Mock-Up. Expesrience gained in operation of this mock-up will be applisd
to design of the reactor for the shield testing facility.

¥f early approval for construction is received, it is expected to have the
sguipment in operation by fall {1854).

Tt is planned to investigste first a mock-up of a service shield complete,
as far as practicsble, with ducts, control parta, etc., to determine whether
or not it provides the desired attenuvation., NEPA has agreed, upon our in-
vitation, to supply this first mock-up, which presumably will resemble the
‘eurrent concept of an sircraft shield., Following this, & series of messure-
‘ments will be made on bulk ssmples to obtain dste pertinent to the snalytical
‘problsms connected with shielding., Farther work will be planned to meet pro-

blems which arise in connection with nuclear siveraft and submarine designs,

SNEFA Porzenasi,
(13 A Propoval for New Bulk Shield Testing Facility, ORNL CFad8.13.93 (Dee. 21, 1948),

{23 Supplement &5 Proposael for Bull Shield Tosfing Feeility, ORNL CF-80.2-1% (Fab. 8, 183D},

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In the measured integrsl case the measurements sample radistion at all
‘angles from the source plane, wheress for cemterline measurements we sample
only those within the angle subtended by the socurce and presume knowledge from
these data about radiastion emanasting at greater obliguity. The latter leads
to an over estimste of the contribetions at lasrge source radii, so that one
would expect higher corrected centerline determinmations relative to integrals.
This effect would be wmore evident at lerge £ than swall and move evident far
gammas than neutrons due to their longer relaxation length., Both thess effects
sre cbserved in the datae. Tt should bhe noted in sddition that this longer re-
laxation length means that more terms must be used to snorrect the centerline
messurements.,

The fission gammas would be partislly self-absorbed in the ursnium source
in sucha way as Lo concentrate the escaping radiastion about the normal. Since
the uranium iz neot s flat plste, but rather a collection of 1.l-inch diamster
slugs, a qusntitative calculastion of this collimation effect has not been made.

Summartizing, the centerline corrected neutvon water dats agree very well
‘with measured imtegrals., The gammas show higher corrected centerline measurse-
ments than integrals, which canm be expleined by either self-abseorption celli-
mation in the socurce, or by the fact that the medium is semi-infinite and not
infinite as is reguired for the corrvection, or by both of these. Within these
limitations, the different determinations of gamma and neutron attenuation are
in good agreement. The gemmas eppear to be somewhat hsrder than would be ex-
pected from previous measvrements.

Spurce Powsr. The plate of urasnium slugs which is used as a source of
neutrons and gammas for the lid tank operstes at a power determined by the im-
cident thermal flux.  Recent improvements in messurement mebhods, using better
values of the slug specific heat have indicated that the plate opesrates at
& ¢ 1 watts when the pile power is 4200 kw. This measurement should be improved
within the next month or two.

Lead-Sater Hossurements. Two ratios of lead and wster, 18% asnd 26.7% Pb
by volume, have been surveved making only centerline messurements, and indio
cations arve {1} that secondary gemmas are apparsnt s the 26.7% Pb ratio, but
not the lower one, and {2} that an even higher lead comcentration will prove
to be the eptimum for s shield using only thesse components. These preliminary
data have been used by the analvysis group to estimate weight of anm sircraft
shield,(®?

{8 Vide infre, Jhielding dnalysie,

14
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with Dr. Bichard Albert and Dr. Theodors Welton of the Westinghouse Submarine
project, and these investigators have been able to fit more recent lid tank
data with 2 "one cellision and out’™ theory., These recent lid tank dats refer
to various compositions of lead and water, and iron and water. The theory is
not believed to be applicable to shields containing ahigh percentage of nstural
boron, becauas the nstural boren is, for high nevtron energies, essentially a
scatterer, and the asbove theory reguires that the "absorption™ (including de-
gradation by hvdrogen cellision oy inelsstic secattering) constitete s major
part of the total cross section.

The mathematical method outlined im the last ORNL Quarterly report has
been further refined and applied to practicsl cesss. This method likewise
gives & sstisfactory fit to the preliminasry exparimental datas.

Calculations of airplane shield weights have been cvarried out om the
basis of H. A. Bethe's paper,’®’’ using total attesuations of e’  for usutrons
and ¢'% for gemmes, but ostherwise wsing Bethe's asssumptions. (The attenustions
used by Bethe weve higher by a factor of 10 which was due tn his assumption
of 30 ft resctor-crew-separation, whereas separation of 100 £t mow appears
fessible.}? The weight of 87 long tons for s lead-water-shield arcund a 2 ft
radivs reacior was computed in this way, in satisfsctory agreement with the
weights computed from preliminary lid tank data,

A limited amount of time was spent on cslculstions regarding the possible
£, 3387

use of hydrides in shields, az well as on comparison of wranium-horon

and wolfram-boren shields.?*%)

The following OBNL reports sere issued:

Capture Gomme Fays, B. P. Blizard, ORNL-419 {December 23, 1949},

Canadien Measurements of an Iron-Water Shield, E. P. Blizard, ORNL-438,
{Jan. 3, 1950},

Measurements on Hanferd Type Shields, E. P. Blizerd, OBNL-430 (Februsry
22, 1950},

(31} Beths, W A., Heport on the Statue of Shielding Infernation for the NEPA Project, OENL CF-48.8.148,
( Fuse 10, 18485,

{313y Brgen, ¥. E., Some Donsiderciiony Regarding the Uee of Uroniss in o Shield, ORNL CF-46.12-58,
HEPA STRE-43 (Dec. 13, 19483,

{18) Brges, ¥. Eo, snd Podger. 5., Hydrides in Shieclde, ORNL CF.-80-3-31, NEPA STRMS1 (Feb, &, 1980},
{14y Podger, $., Comparisen of Uranius, Boren and Tungsten, OBRL CF30.1.8, NEPA STRE-48 (fan. 8. 1988},
(109
12
v FlG. 3 3
4 NEUTRON ENERGY SPECTRUM
- X OF MOCK FISSION SOURGE G
10 = -
=L .
w
< 9 —
T e =
E 8H— ok
/ o
e :_/ \ e
s/ 1)
T \ -
@ 6%——,’ L I Bt
e it ¢
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- L? \\ -
x 4 1 ~=
" :
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g I *
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2 | Mo -
z |- ¥ e T
' e " ]
=~
ol g | | ==y o | T
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®

DWG. 8425

ENERGY (MEV)

-

@

N

)

5
X 10
NEUTRONS PER SECOND PER CURIE PER MEV

6l

e

UNCLASSIFIED
DWG. 8433

FIG. Y
NEUTRON ENERGY SPECTRUM

OF Po — Be SOURCE

L .

e

—F—w
NL_.

4 5% & 7 8 9 10 It [I2 13
ENERGY (MEV)

SHYELDING MATERIALSR

4. 8. Ritzes R. B, €allabery
¥. §. Huilings ¥, L. HcEinney

geactor Technoloegy pivision

Uranium Hydride Survey. Uranzum hydride (UH,} is being comsidered as a
shielding material for nuclesr powersed aivrerafe. The cheice of UH,, however,
depends upon a number of factors:

{1} Production of non-pyrophoric material in tonnage guantities.

{(2) Feasibility of compressing UH, to a density of % g/lec or UH,
to a density of 11 gfen.

{3} Production of material in such & state, in case non-pyrophoric
UH, cannot be produced,that will allow easy handling during cladding
of the material.

A survey, therefore, was initiated to determine the feasibility of produc-
ing uranium bhydride in tonnage gqusntities which would meet the above specifi-
cation. This survey has been completed and an OBNL report will soon be issued
on the suwbject., Conclusions which may be drawn from this survey are:

{1} Most lots of uranium hydride (UH,} are pyrophoric. Some have been
made which are not, With additional research and development, non-pvrophoric
uranium hydride can probablv be made. Titanium hydride was once considered
pyrophoric, but now non-pyrophoric material is made in tonpesge guantities.

{2} The denzity reguirsments can probably be met. Additional development
iz necessary however.

{3} The material can easily be clad once the pyropheric disadvantage 1is
overcome. 1he material is probably non-corrosive.

{4) No cost data are available since no large guantities bave besn made
with the desired properties.

{5} Uranium hydride dis&mciatassnmhaaﬁimgsxt%ﬁﬁﬁﬁg the UH, is in equili-
brium with hvdrogen gss at one atmosphere pressure,

{6) The radistion stability of UH, is unbnown. By enalogy, 3t is probably
as atable as titaniuvm hydride o pile radiations.

(7} UH, forms amalgaws with mercury. When mixed with molten,lead, tin or

cadmivm, thes uranium and metal alloy releasing bydrogen,

20
Plastics. Twenty sheets, 364 in. X 88} in. ¥ 1/B in. of B U and Tygon
{Tybor} bhas been fabricated for the Lid Tenk Experiwents. B,C and Tygon paint
are mixed in the ratio of 3 parts B,C to 1 pert paint by hand. This gives 80%
B.C by volame. The wixz is cast on a specially designed rolling table and
rolled to 8 uniform thickness. Thickness can be varied from 1/18 im, to 1/8
in, Cast sheets are wrapped with cheese cloth for sdditional support and are
coated with additional Tygon paint for waterproofing., Tensile streangth of
"Tybor" 1s 215 psi and age has no apparent effect on the strength. Elongation
ig about 11%. Sheets are guite flexible and can be bent around round objscts
without cracking, provided the bends are not sharp, Sheets are tempsrature
sensitive, heing more flexible at or slightly above room temperature than at
lower temperatures. The material is not brittle at tempsratures of 44-50°F,

Expervimental 4 in. ¥ 4 in. » 48 in. sgusvres of tungsten carbide and Tygon
have besn made. Hatio of W {/Tygon is I8 vo 1. W0 in the desired particle
size range is not commercially available to permit making sheets 58X in. = 46Y%
in. X 178 in., but limited peraomnel has postponed this operation. This aize
sheet can be made if the W, is screened. Tenzile strength of W C-Tygon sheets
will be determined to see whether or not a sheet 5684 in., X 66% in, » 1/8 in.
can support its own weight, The sheet will weigh approximately 150 lbs as
compared te 25 lbs for B L-Tygon sheet of eguivalent dimensiona. Other
plastics, such as polvethyvlene, polvstrene and bakelite will be used as the
binding materials instsad of Tygon. These materisls are more stable to radi~
stion than Tvgon,

Two B0, Tygon sheets, 35 dn. ¥ 5§ dn. » 3/8 in., bave besn fabricated
for the MTR Mock~Up critical experiments. These sheets were very difficunlt to

<

meke dus to the hygrossopicity of the B,0,. Ratic of B0, toTygon was 2 to 1.

oy

Tests indicate that B,0, is not as stakle to radistion as B U which apparently
%1ill preclude 1ts wase for high level irrsdistion applications, even though it
costs about 15 cents/lb cowmpared te §4.50/1b for B C.

goncretes. The concrebe work was kept to a minimum during the last
quarter, FExcept for service work no projects wers initisted.

A special MI concrete was wade for H, P, Sleeper, KAPL. The compuosition

is as follows:

f.ead Shot hd 8% Wi,
Stainless Steel Scrap 1.7
Mg O 8.2
Colemanite 8.2
Mg €1 (28° Be-Solu} 1.1
Calgon Solution . 08
&

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assumed to be reached when no loss in weight of the cement was detectable,
The cement was hested up to 300°F, and again eguilibrium was assumed when no
iose io weight wes vobiced. The temperature was then dropped to 200°F, and the
sample was allowed to come te eguilibrium, raised to 300°F, etec. The test was
continusd for 37 davs. The tests will socon be run in e newly designed apparatus
which will allow for the accumulstion of wore sccurate dats.

pabrication of Seral (8, ¢ + a1y, Boral, ss described im ORNEL-242,038) 4g
an engineering material for the sbsorption of thermal mevtrons without pre-
duction of hard gammas in a form which allows easy heat removal. Large scale
experimental vrolling was attempted at Lukens Steel Co., Usatesville, Ps. Two
large ingots 27 im, ¥ 36 im. % & in. were scheduled for rolling into sheets,
56 in, % &6% im. X 3716 im. {

was 8 failure. A second rolling is being scheduled for the latter part of

Jord =

Ine ingot was rolled inm December but the rolling
February. Precauntionary messures are beisg taken to imsure a suvecessful roll-
ing the next btime. The picture frame which cenfines the ingot has been incressed
from 1 in. to 5% in. in thinkness; the covers {cladding) hasve been increased
from ¥ in., te ¥ in. thick. Proviasion has been msde to insert a thermocouple
in the center of the ingot in order to be able to ascertain the true temperaturs
sf the core prier te rolling. A temperature of 1100°F at the cemter of the
core waterial is desired before rolling., Closer time schedules have been
warked out so that the ingots will be exposed to the westher conditions for a
minimum length of time. Tt is believed that the second rolling of these ingots
will be succesafel,

The rolled sheets, 58} in. x &84 in, * 3/16 in. will be used in the Lid
Tank Experiments. JInguiries have been received from other sites; Brookhaves,
Argonne, Hanford and KAPL have ewxpressed anm interext in acguiring large
guasntities of Boral sheets,

An estimate of the cost of fabricating a Boral sheet {58-50) is about
§15/F¢t?, Yt i1s slso estimated that a sheet of boral, 1/8 in. thick will
sttenuste thermal nentrons by a factor of 10%. In many cases, sn attenuvation
of 10% or 10% is all that is necessary. A program is being initisted therefore
to develop "Borals™ with lower B,C content. These Borals should have better
rolling characteristics, structurasl properties, thermal properties and lower
cost because of the lower B,C contents,

Thermal condugbivity specimens have been made by hot pressing B,C and Al
powder ina grapbite die st 1200°F. Preliminsry data indicates that the thermal

conductivity of Boral is 86 BTU/hr-f¢*-°F/fr. These tests will be duplicated

{15) MeEimney, ¥o L. end Rockwell, Theodera, YEI, Boral: 4 New Thermal Xeutron Shield, omnl 242,
{Aug. 31, 1849),

e

3
for other specimens. Yo the same tewmperatore range, low carbon steel iz 35 and
Al is 118. Specific heat of Boral is 0.175% BTU/°F-1b. The thermal conduc-
tivity of B0 with B,0, as a binder, Al, and mixtures of B,C and Al {amount of
Béﬁ varying from 10% - 50%} will also be determined. This work will alse be
duplicated for Plumbor (B0 and lead}.

Tensile specimens of Boral have been removed from the pile after & and 8

o~

wee ks exposures in the isotope strimger. The tensile strength of the apeci-
mens were determined after cooling for 2 days {3 mr/hr in %' s and & mr/hr in
5's un comtact).

HBesults are sheown in the following table:

SPELIMEN TENSILE STEREEMNGTEH
{ib/in" )

UGriginal Avg., H000

§ weeks Avg. 6335

8§ weeks Avg. T500

Additional samples have been placed in the X-10 pile and will be removed
after 12 months, 18 months, and 24 months sxposure. Sawmples are also being
sent to Hasford for exposures of 3 wmonths, 10 months and 20 months.

Samples of the "poor wman’s™ Horal, "Boroxal® {Ezﬁg and Al}, have also
been irradisted. These samples however, were less stable to pile radistions,
the tensile strength decreased from 2800 psi to 2050 psi after 8§ weeks ex-
posuve in the pile.

"Flumber™ (B, C & Pby. "Plumbor™ sheets (50% B O & 50% Pb) have been made,
Methods for incerporating H0% B U into Pb are being studied. Thermal and
physical properties of the Plumbors will be measured.

Reports Yssused, The following report was issued during the past guarter:
Construciion of Uheap Shields; A Surwvey by Theodore Bockwell, ¥YIY¥, OBNL 243,
{Januwary 16, 19%350;.

The material on shielding for Nucleonics is assembled and three copies

are being sent to Chivagoe for pre-declassification of shielding work.

24
HEAT TRANSFER

Regetor Techuology Divisien

Beat Tramsfer Theory (H.0. Claiberme}. Theoraticel work on hest tranafer
has consisted of a study of fluid flow and velocity distribution in conduita.
It is oma knowledge of the velocity distribution in tubss and between parallel
plates that liguid metal heat transfer theory is based. and s knowledge of
velocity distribution in channels of other shapes will aid in studying heat
trensfer in these chennels. Principal efforts have been directed toward
empirical expressions for velacity distribution in circular tubes which might
provide insight into the veloeity distributien in other channels.

Erxperisental Hest Tramnsfer (€. P. Coughlen). FEguipment for hest transfer
studies with lithium st temperatures wp to 1800°F has been designed, and work
has sterted on the fabrication of variocus cowponents. The rig will be &
figure-of-eight system, with by-passes around the test exchanger for contrsl
of the flow retes and for vapid alterstion of temperstures betwesn tests. In
sddition, & temperature conirol exchanger will be located between the test sst
up and the pump. Jts purpose will be to permit operation of the pump at a
lower temperaturs and to provide accurate centrol of the tempersture into ths
test sxchanger.

The pump and test exchanger will be connected into the system with {langes
so that they can be changed to alter the test conditions.

Stainless steel, type 347, will be used throughout, in the absence of
wmuch corrosion information with lithium., The asystem will be operated at lower
temperatures and watched closely for signs of excessive corrvosion before being
operated at 18U0°F.

Liguid Hetzl Pusps {4. RB. Frithsem,™ R. N. Lyom}. Several spprosches ars
being studied in the development of e satisfactory liguid metal pump for heat
tranafer experiments. Such a pump might also be satisfactory for the final
reactoy as well, although reguirements for the two installastions are not
gimilar. Efforts have been divected toward developing s completely encloasd
pump, thus elimineting the shaft seal problem. While slectromagnetic pumps
show lesa promise for the ANP program than for other spplicetions, s study was
made of the possibility of & pump utilizing the pressure gradient across a

liquid metal stream which is carrying & current of electricity. Preliminary

® W%, Alr Farce persennel,
results indicated that only low pressures could he realized and work on this
tvpe was shelved.

Construction of 8 canned roter for a pump is sbout half completed. The
guestion of which of twe types of bearing te use in the pump cannot be anawersd
until the completion of tests which are now in progress. Both bearings force
the shaft to turn on a laver of liguid, preventing selid-sclid contact. {One
requires liguid to be forced into the besring snd is guite similar to bearings
being developed at Allis~Chalmers. The other bearing vtilizes the viscosity
of the liguid to create sufficient pressures to keep the shaft from contact
with the bearimg., This type of bearving is also being studied at General
Electrie.

An induction pump uwsing moving magnets is under consideration. This would
be a helical pump similar to an induction electromagoetic pump being developed
at Generval Electric.

Liguid Betal Handbosk (R. N. Lyen). Editing of the bhandbook on use of
liquid metals and the compilation of a chapter on liguid metal heat transfer
has resched a point where potential publishers are being sought with the aid
of the AEC and ONE in Washington. All chapters are expected to be complete
and in the editors’ hands by March 1.

26
4 ]
Pt or L]
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NOT CLASSIFIED
DWG. 8612

\ —PLUG

o B T W LI
L AT TR

O R 7/
SRS

~—CAPSULE

e g rd s
s

SPECIMEN
| X 34 X Vg

Eﬂ\\\\i

g R T

FIG B
CORROSION CAPSULE ASSEMBLY
28
Ulobar tube furmaces. An inert gas surrounds the capavles to prevent scaling
and to minimize denger from posasible leaks. Following the reguirsd 2XPOSsULe,
the furnace is tilted to drauin the liguid metal away from the samples and up
into the hollow core of the plug, where the liguid selidifies. After removal
of the capsules from the furnsce and selidification of the contents, the plug
end of the cepsule iz sawed off snd the capsule contents removed for exsmination.
The lithive and biamuth ere analyrzed spectrographicelly for the component
elements of the semples. The lithium or bismuth is removed from the surface
of the sample, the sample is weighed and its surfsce is sxamined microscopi-
cally and by X-ray or electron diffraction.

Preliminary four-hour results from lithium tests at 18007F, which must be
rigidly checked before they can be accepted as conclusive, indicate {1} iron,
molydbenum, and zivconium suffered less weight change than the other materials
tested, (2} tungsten, tantalum, snd columbivm were not severely attacked, and
{3} cobalt and nickel underwesnt substantiel weight loss. The zirconium de~
veloped a brassy tarnish which X-vray diffraction showed to be a zirvconium
nitride filw, indicating probasble mitrogen contaminetion of the lithium.
Interpretation of these preliminary test results should take into account the
facts that procedures insuring uniformly low contamination of lithiem by oxygen
and nitrogen are not yet in osperation, and that s third component, the ivon of
the wapsules, was present in each of the svstems. Significant results, where
reguired, will be subject 2o confirmaetion in capsule liners made of the
materials undergoing tesi.

The four-hour, I1800°F tests in bhismuth, subject to the same or similar
gqualifications as the lithium tests, showed nickel and zirconium to be severely
attacked, whereas visual observation did not indicate attack of the iren,
tungsten, tantalum, molybdenum, and columbiuem,

The pext aeries of tests is being conducted at 1800°F for forty hours, and
will be followed by tests for still longer perisds of time and tests at other
temperatiyyes.

In addition to lithium and bismuth, potential coolants which are being
considered for use in later similsr sorting tests include lead, tin, magnesium,
and posaibly sodiuvm, patassiuwm, and combinstions of some of these.

Lithiss Hsndlisg., Lithium presents a serious fire hazard incase it lesks
or is spilled at high temperatures. A study to select materials for use as

insulation around vessels containing lithium indicated that the fellowing

29
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by ferl ) - Bt o A p R B o T ‘ o PR
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P 1] o0 - fierd o i e €3 I fod o] e
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gy ) seitatd oot . b = o raay o pel & o a d §a
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b = e ek 4 ; o e I L
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it [l B R S v bt - ’ . o 03 L3 et =oom W oeed b
: ’ . o L3 P = T ] o W o -
w - g s % At et tealas Yot

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on development of an experiment for the MTB. Extensive use of the MIR Mock-Up
at OHNL 313 planned.

AUXTLIARY HATERIAL RTUBIESR

¢. Sisman, Resctitor Techmology pPivision

High Iotessiiy Samma Sowrcse. In order to study the effect of gamma radi-
ation on materials, @ pneumatic tube apparatus hes been installed in the pile
for producing high intensity gemma sources by irrsdiating cylinders of gold
{Fig. 6). This equipment haa been in operation since December 19, 1949, The
gamma intensity inside the gold cylinder {3 in. long, 1 in. ID, 2 aom thick)
sfter irradiation for one week was measured to be 10% p/hr.(U

The pneumatic tube apparatus is shown in Figs. 7 snd #, and the receiving
shield is showns partislly disassembled in Fig. %. The gold cylinders arse
biown in and out of the pile by aiv preasure, operating through solensid valves.
When the gold eylinders ave discharged from the pile they fall inte one of
sight chambers in the receiving shield., These sight chambers sre arrangsd in
# circle and gearsed to an indexing handle so that s zource may be received in
any of the sight chambers and thesn rotated 180° to = position from which it
may be dropped into the source shield. When the gold is to be reinserted in
the pile the source shield is brought up under the receiving shield by means
of a 1ift truck, the gold ecvlinder is then blown from the soures shield inte
the receiving shield, and rotated 1807 to a position frowm which 1t is blown
into the pile. The large cviindrical lead plug, shown in the lower left hand
corner of Fig., ¥, normally keeps the gold cvlinders from falling out of the
receiving chember and alsc shislds the opening through which the cylinders
pass inte the source shield. When this plug is turned 30, the source falls
through an opening in the plug snd into the seurce shield. The ssveral parts
of thiz apparetus ars semled with double O rings, and air pressure is maintainsd
between the § rings to keep active air confined inside the aspparatus, from

which it is discharged inte the pile exit air line.

{ 1) Hessurements weve made with & speclaiiy designed lenizstion cohawmber aznd checksd with several Victersen
i ¥ meters, The velues obteined with the R meters st ths cenfer of the cviinder sere 0% higher than the
regding on ths isnizstisn chamber, which gives sn sverage of the enfive 3 inedh lemgih of the cylinder,
_INED CUP

FIGURE 6 GOLD
PHOTO  5R6G
NOT CLASSIFIED

PHOTO 5988
NOT CLASSIFIED

NOT CLASSIFIED

B
o
o
b
Q.

. ) . . s . . p & N P o o
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bt b ot o ) N s - g Lo )
7 ks L 2 o e . -
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& - S - o - it . s - o g e
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= D = Lo 4 3 o %
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s . - - ] S . . s [ £z w nand .
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> ., :
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s et [ . s o i d 2 o i, T Post g ]
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p P - " % iy . P o iy \ Fold P g [ P
B el A E L e EE RPN s B ] o eed & B egd G4 @
. P o i P p o k. S o~y ek
oo 2 PR I+ o om W e @y o L

PHOTO 5840

NOT CLASSIFIED

A3IHS

304N0S O! 34Nold

TABLE X

gleectrical Properties of Irradisted Plastics

YOLUBE EESISTIVITY {&kﬁﬁfﬂﬁﬁ} DIBLECTRIC SYRENGTH {(wveite /mils)

¥

HaTBERIAL

THEEBHAL ovg
' Beuwtrons ems)

BEFORR

IRRARIATIOR

AFTER

IRRADIATION

BEFORE

IRBADIATION

AFTER

IERABYIAYIOR

Methyl Methscervlate {Lucits}
Cellulose Nitrate

Celluloses Acetate

Cellulose Acstate Butyrate
Fluorothene

Ures Formaldehyde

Alkvd Resin

Polyvinyl Carbazeols

Yinylidine Chloride {(Saran}
¥inyl Chloride Acetate

Melamine Formaldehyde
Polyastyrene {eclear)

Polvstyrene {Styron 475}
Polystyrene {Styron 4110}
Poelysthylene

Phenel Formsldehyde {paper base)
Phenol Formaldehyde{ssbestos base!
Allyl Diglyeol Carbonate
Polvester Resin

Polyamide {Nylon}

8

L41 % 10%8
L34 x 1pte
L34 % 1038
26 % 308
24 % 1048
L26 x joid
(2% % Jot @
L39 ® 108
4L x 10

7 ox 108

AR G R
L00 x jotd
L0 x - 1ptd
Lo x 1ptd
L0 x. 1g e
L0 x 1018
.00 x jgt®
LBT % 1038
.65 % 108

J50 x joid

o

(]

> 1044
% iﬁii
x 1012
> 1044
> 1oid

2 % 39t

v 1$§§
> 10t
> g3
> 10is
x jptt
>.EQE$
> 3
> 1gt¢
5 1p¥4
X iﬁig
% 10%

% E@&é

x gt

X §§§3

8

B

B

v 1014

SR A
b4 Eﬁﬁﬂi

A

L]
s
Y

'v!
-
L)

3
A

60

60
740
500
1280
660
1086
850
1640
1140
1440
1220
1230
80

436
240
440
168

1300
10320
G40
490
186
80
a81¢
860
86
T

e Anlt syl v peldnogtg Janintaeln

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SUALTATAANY

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(N1 s &) seesyrpvied
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| {nngi wi rasdos lahvdebt 2 LosmdS

sdemiin Tovedetl Lelld
wisolh 1@izayiad

boe P77 wRlawyia®

vl

~
O

oy
o

PRESSURE P.S.l. GAUGE
»
o

W
o

20

10

DwG. 8995

152 °G
/9—\\
e §
\ 239 °C
/ N\
ZERO PF!ESSUREK
2.6 2.4 L 2.0 1.8
IOOO/T abs.
FIGURE i DISSOGIATION PRESSURE OF LiH

© IRRADIATED
o NON-IRRADIATED

L
PRESSURE — P.S.l, GAUGE

200

i00
20
80

70

60

50

40

30

20

10

DwG. 8596

u_—
275°C -
o N\
7 /
I P
&
7. // & \\ %
o YV
JL/ / \X \\
e
i
ZERO PRESSURE
2.6 2.4 2.2 2.0 I;8 1.6 1.4
1000/ T abs.
FIGURE 12 DISSOCIATION PRESSURE OF Z'Hn.es

W2

(O]
O

IRRADIATED
NON-IRRADIATED
materials over the nonirradiasted metearisla. Total irrsdismtion time haz been
sbhout 3 monthszs at about half wmeximusm fluwm.

It 43 tentatively planned to include wranius hydride in thess studies.

43
NUCLEAR MEABUREMENTS
4. 8. Sosill, Physics pivisien

Preparations are being made for the messursment of the variocus neutren
cross sections which can be expected toe be needed in the course of the ANP
work. The preparations sre dirvected along two lines:

{1} SBelection and preparstion of the site for the "5 MYV™ NEPA Van de
Graaff machine., Delivery of the machine is expected in September, 1850,
HBeeruiting efforts are vnder way with the object of sssembling 8 group of
physicists prepared o start the weasurements as soon as the machine atarts to
perform asufficiently well.

{2} Conatruction of a high-speed mechanical velogity sslector. This
geems attractive in visw of the recent succeas of the Argonne mschine. The
work at ORNL has to astart from scrateh; one wan has been studying the problem,

and it is hoped that s second persen can be added im June.
THE CONCENTRATION OF LITHIUM ISOTOPES BY CHEMICAL METHODS

A. Clark, Y-12 Research Laboratory

The concentration of lithium isotopes by a number of different methods has
been under investigation for the past nine months. It seems likely that high
purity "Li would be very valuable as either a coolant or a fuel-element con-
stituent for an aircraft reactor. At the Beginning of the project a survey of
the scientific literature revealed that the concentration of lithium isotopes

had been accomplished on a laboratory scale by several widely different methods.

These included the mass spectrometer, chemical exchange between a resin ion
and aqueous lithium solutions and between lithium amalgam and alcoholic lithium
solutions, electrolysis of lithium solutions in which the reduced lithium is
removed as amalgam, and electromigration in which the faster isotope migrates

more rapidly toward the cathode in a fused salt.

During the months of December, January and February, the effort has been
concentrated on molecular distillation of the metal, chemical exchange in
solid-liquid and liquid-liquid systems, continuous countercurrent electro-
migration, continuous countercurrent electrolysis, and thermal diffusion of
aqueous lithium solutions.” The end of the quarter also saw the beginning of a
new method—a dual temperature liquid-liquid chemical exchange system which
requires no reflux and a minimum of attention. This method appears highly
suitable for quantity production of 'Li if it develops satisfactorily.

Molecular Distillation of Lithium Metal. The molecular distillation
(non-equilibrium) of lithium metal should result in a concentration of ®Li in
the vapor and of ’Li in the residue. The ratio of the rates of diffusion of
Li and 'Li from the liquid metal is proportional to the inverse square root
of the mas;e;, and a theoretical separation factor (a) is calculated to be
1.08 for this process. Preliminary experiments with a single stage molecular
still have shown a separation factor = 1.018., In a typical experiment, 10.1
grams of lithium were distilled over a period of about two hours at 450°C and
15 microns pressure until onli 1 gram remained in the still pot. The resid-
ual material in the still pot assayed 92.935 & 0.015% "Li as compared with a
starting material assay of 92.500 £ 0,020%. Further experiments will be
carried out using a larger still under verious conditions of temperature and

pressure.

45

=

Chemical Exchange Methods. Chemical exchange methods for concentrating
lithium isotopes are divided irto two groups, ligquid-solid systems and liquid-
liquid systems. Although the latter are more easily adapted to continuous
ouRtercurrent operation, very few satisfactory systems are available, and

much’ of the effort has been with liquid-solid systems.:

Ligquid-Solid Systems. An attempt is being made to utilize selective
adsorption on cellulose-—a method used successfully for the separation of
different elements.. A lithium salt in an organic solvent is slowly eluted
through a column packed with activated cellulose. It is hoped that the
cellulose will exhibit a preference for one isotope so that the lithium coming]
out the bottom of the column is concentrated with respect to the isotope held |
less tightiyo To date the cellulose columns have been filled with activated
cellulose in butyl or isoamyl alcohols, and a slug of activated cellulose and
lithium salt in water added at the top of the column. Elutriation of the salt
at the bottom of the column is performed by addition of alcohol at the tOpo:
In the latest experiment the column was charged with LiOH, and over 170 hours /|
were required for the lithium to wash through a 24 inch column. No assay has |
been received for the lithium in the leading edge.- i
Another liquid-solid system is a continuous countercurrent ion exchange
resin column in which a lithium solution passes up through an ion exchange
resin which moves slowly down through the column at an almost imperceptible |
flow rate.. The experiment has recently been terminated and no assay on the |
product material has been received. In an experiment at X-10 with a "fixed" |
bed of resin, the concentrations of "Li in the leading and trailing edges were |

reported to be 93.4% and 90.0%, respectively.

In another liquid-solid system, a column of solid Li,CO; in a finely

divided state is slowly being eluted with distilled water. If there is any|

- difference in the solubility of the lithium isotopes, the more so;uble should |

| dissolve, and the less soluble should be concentrated so that when all except

: equilibrium between solid and saturated solution, and requires a long time |

a small portion of the original column is dissolved, the remaining solid shouldi
be enriched in the less soluble isotope. This is dependent on complete |
(several months) to complete the experiment.

Liquid-Liquid Systems. Isotopic exchange and enhancement is being studied
in a number of aqueous-organic liquid systems. The limited number of organic

liguids which have proved to be suitable for this method has forestalled the

development of a satisfactory systenm. Water-isoamyl alcohol solutions of LiClh

E

‘46
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have shown an inconclusive, but small concentration, and this system is still |
being investigated.” A number of less likely systems remain to be studied.

In the literature a chemical exchange and isotopic enhancement is reported
between lithium amalgam and alcoholic lithium chloride solutions.’ In order to
avoid the onerous task of refluxing at each end of the column, it has been
proposed that the dual-temperature process for hydrogen-deuterium be adapted
for lithium. In the proposed method, lithium amalgam is pumped countercurrent
to a rising column of alcoholic LiCl. By maintaining a cold column at the top
and a hot column at the bottom, the ’Li isotope is concentrated in the bottom
of the hot column and at the top of the cold while ®Li is concentrated at the
top of the hot column and in the bottom of the cold column.. In this manner a
continuous process can be operated without reflux and a minimum of difficulty.
The main obstacles remaining are large stage heights and possible low sepa-
ration factors. If these can be overcome successfully, the production of TLi
will become a reality.

Coutinuous Countercurrent Electrolysis. Since the largest factors for the
concentration of lithium isotopes have been reported for the electrolysis of

lithium solutions, some consideration and effort has been expended in the

development of a continuous method. Single stage separation factors as high
as 1.05, 1.06, and 1.07 have been reported for experiments in which lithium is
reduced at a changing mercury cathode in an aqueous lithium solution. As the
lithium amalgam is continuously removed, the concentration of 7Li remaining in
solution is increased. By combining several cells and causing the lithium to
flow counteréurrently to a stream of LiCl solution, it is hoped to concentrate
the lithium isotopes.

Continuous Countercurrent Electromigration. -The work of Brewer, Madorsky
et al datithe National Bureau of Standards during the War showed that two
isotopes of the same element might be separated by washing one back with a
countercurrent stream of electrolyte while allowing the other to migrate for-
ward to the cathode in an electromigration cell having anode and cathode con-
nected by an anti-diffusion packing. This principle has been applied to a
solution of LiOH in which an attempt has been made to separate the different
lithium sbecies which are postulated to exist. By separating the species, it
is hoped that an exchange and subsequent shift will occur so that an isotopic

concentration is effected. The work is being continued.-

47
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Thermal Diffusion.

No satisfactory component for the thermal diffusion

of a lithium liquid has been found. In lieu of this, thermal diffasion of

concentrated lithium salt solutions has been tried with no apparent success to

date.

48

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