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C o n t r a c t N o . W-7k0$-eng-26

C B W C A L TECHNOLOGY D I V I S I O N P l l o t P l a n t Section

PREPM3ATSOTJ OF ENRICHING SALT 7LiF-233W4 FOR R P U E L I X G %HE MOLTEN SALT RWCTCR

Jchn M. Chandler S. E. B o l t *

MARCH 1969

“Reactor D i v i s i o n .

OAK RIBGE NATIONAL W O R A T O R Y Oak Ridge, Tennessee operated by TJBIOM CAFBIDE CORPORATION for the U. S. ATOMIC EFERGY COi?4MISSION

This r e p x i was prepared as an account of Government Hp.,nsored work. Neither the United States, nor the Commission, nor any person acting on tcluif of the Commission: A. Malies any warranty or representation, expressed Or I m p l i d , with respect tu the accuracy, completeness, or usefuiness of the information contained in t h i p report, 02‘ that the use of any information, apparatus, method, o r process disclosed in this report illay not infringe privately owned rights; or B. Assumes any llabLlItlep with respzct tu the use of. or for damage6 reSulting from the use of m y idormation, apparstua, method,UT procese disclosed in this report. AB used in the a h v e , “person acting on behalf of the Cornmiasion” includes .my e=ployee or contractor of the Commission. or employec of mch contractor, to the extent that such employee or contractor of the Comnfssior., or employee of such contractm prepnres, dieleminates, or provides acccis ta, any information pursuant to ius rrnplogment or cotztract with the Commission, or his employment uitk suck contractor.

.... . ... ...

iii

Page i Abstract

Lntroduction

Considerations

?-2*

14*

2.2

Chemistry

2.3

Fuel

Process

the

231 -"U

Description

. . . . . . . . . .

..*

One-Step T%o-Step

SaPt

Description

the

in the MSRE ....... 233 U System .......

Fuel

by Remote

Development

Low-Temperature,

Circulating

Preparation

3.2

Cold

Characteristics

High-Temperature,

1.4 . 4

Substituting

a.1

4.3

for

Nuclear

4. 2

.........................

2.1

4.1

5â&#x20AC;&#x2DC;

Means

Process Process

Production

Facility

the

. . . . .

. . . . . . . . . .

4.1.1

Cell

4.1.2

Radioactive (RHD-HOC)

TURF

Hot DraLn - Hot Off-Gas . . . . . . . . .

System

. . . . .

. . . . . . . . .

4.1.3

Cell

4.1.4

Shielding

4.1.5

Manipulators

. . . . . . .

Flowsheets

. . . . . . . .

. .

. . . . . . . .

. . . . .

. . . . . .

Process lc.2.1

High-Temperature

4.2.2

Low-Temperature

Process

Equipment

Process Process

4.3.1

Becanning

4.3.2

Reaction

4.3.3

Salt

4.3.'c-

Shipping

4.3.5

Scrubbers

4.3.6

Miscellaneo~Js

Equipment

Procedures

..................

Operating Rus with

5.1

Preoperational

5.2

Mechanical

Station Vessel

Storage

Depleted

Ventilation

and Transfer

Vessel

...............

Containers ....................

Uranium Act-ivities

Operations

9 10

J-9

........

11 11 I.3 15

22 22 27

.............

................ ............... .................

31 36 36 36 36

iv 38 42

6.1

Feed

6.2

Radiation

6.3 6.4

Oxide

6.5 6.6

Materials

e e e a e s e o e e e e e e e e e e

Levels Feed

Reduction

MaterEal of

Uranium

the

PurEfication

6.9

Container

6.1~ 6.11

Transfer

Material

Balance

i%aintenance

7.2

Redundant

7.3

Tools

7.4

Maintenance

Conclusions

Acknowledgments

the

s a 0 o o e o 0 e o e a

Salt

Eutectic

7LiF-233

Salt

Salt and

IIF4

e 8 e e * e s a G .

a S o o G I 0 o . 0

PreparatLon

Salt

c e D s . o 0 o

Product

for to

Shipment the

MSRE c

S a o a = 0 D c e e e e o e * e o

44 44 47 50 53 55 60 62 62 66

Tables

67 67 68 68

Procedures

Engineering

Spare

c e D e c e o a

o c S 0 o . D e a e e

Oxide

Eutectic

Disassembly

7-E

cf of

Feed

of UO2 e a 6 s e a 6 e e a e e B

6.7 6.8

Transfer

Oxide

Handling

Hydrofluorination Formation

the

Parts

. a

B . e a D Fittings

and Work

e a

0 0 e e 0 e . e

a 0 D e D D

71 71

John

M. Chandler

S . E. Bolt

The Molten S a l t Weackor has been r e f u e l e d wlth en (73-27mole $> e n r i c h i n g s a l t c o n c e n t r a t c , 7LiF-'33W4 Sixty-%hree kiLograme o f t h i s c o n c e n t r a t e w a s prepared ir: c e l l G of t h e Thorim-Uranium Recycle F a c i l i t y a t ORNL. lets p r e p a r a c i o n rEn a, s h i e l d e d cell was r e u i r e d because of t h e h i g h 2% content (222 ppm) of t h e e3%Je e

I n t h e shekedown run w i t h de-pletea araniwn oxide, a h i g h - t e m p e r a t u e 7 s i n g l e - s t e p process w a s used t o redllce t h e oxide 2nd t h e n convert it t o UT4 for use i n making t h e e u t e c t i c s a l t . Although this process y i e l d e d a highq u a l i s y product, s e v e r e damage t o t h e equipment w a s obs e r v e d . Therefore, it w a s d i s c a r d e d i c f a v o r of a bowtemperature, two-step process i n whick. t h e -araiiim oxide was red-xed 'eo IJ02 by Lreatrnent with kydrogeii, t h e U02 w a s converted t o LF4 by hydrofbuorination, LiF w a s added, and t h e e u t e c t i c w a s Formed by f u s h g the components. "he eu+uectic mixture, LiF-UP4 (43-27 mole w a s p u r i f i e d by treatmect with hydrogel?, which r e d w e d t h e c o r m s i o n proau c t s t o metal and subsequently allowe6 t h e i r rernoval by f i l t r s t i o n . The q u a l i t y cf t h e product w a s w e l l w i t h i n t h e requiremects e s t a b l i s h e d f o r t h e PEBE. $j)7

The f u e l concentrate, c o n x T n i n g 39.0 kg of uranium w a s packaged i n n i n e v a r i a b l e - c a p a c i t y of' uran2rz.n) s h i p p i n g c o i t a i n e r s f o r a d d i t i o n to t h e reactor f u e l d r a i n t a n k and i n 45 enrichment c i p s u l e s , each c o n t a i n i n g 96 g of uranium, f o r a d d i t i o n t c t h e bowl o f t h e fuel c i r c u l a t i n g pump. The f u e l w a s shipped i n s h i e l d e d c a r r l e r s t o t h e E R E t o acconlmodate t h e r e a c t o r enrichment schedule.

(91 k% '33U) (0.5 t o 9 lig

In July

1966, an -ad _ _ hoc _

committee w a s appointed t o s t u d y t h e

f e a s i b i l i t y of s u b s t i t u t i n g 233U f o r t h e 235U b e i n g used t o f u e l t h e Molten Salt; Reactor.

It w a s t h e recorrmecdaticn

of' t h i s committee t h a %

233U be prepared for e n r i c h i n g a charge of eurLect,ic salt c o n t a i n i n g t h e MSRE p r i o r to renova1 0:' t h e 235U from t h e system.

A s i n g l e - s t e p process, i n which t h e f u e l c o n c e n t r a t e could be

prepared d i r e c t l y from 233UC9

and LiF, i n a. s i n g l e r e a c t i o n v e s s e l

l o c a t e d i n a 'not c e l l , w a s c o m i d e r e d t o b e t h e s i m p l e s t and m o s t economical approach

E i o l o g i c a l s h i e l d i n g woxld he r e q u i r e d because

o f t h e 'nigh 232U content (222 ppm) of t h e 233U f e e d material.

The r e q u i r e d q u a n t i t y and q u a l i t y of t h e e n r i c h i n g c o n c e n t r a t e w i l l permit o p e r a t i o n of t h e MSRE a t full power f o r a t l e a s t one y e a r .

T ~ i sr e p o r t s u m a r i z e s I;he p r e l i m i n a r y phases of t h e wcrk developKent, design,and c o n s t r u c t i o n

as well as t h e a c t u a l o p e r a t i o n

of t h e process used t o p r e p a r e t h e 7LiF*'33W4

(73-27mole $1

eutectic

salt

2- CONSIDERATIONS FOR SUBSTITUTING 233U IN THE ISWE The s u b s t i t u t i o n o f 233U f o r 235LJ

frcm t h r e e s t a n d p o i n t s :

i n t h e YfRE had tc b e considered

(1) t h e n u c l e a r c h a r a c t e r i s t i c s sf t h e 233,

system, (2) t h e chexistry of t h e c i r c u l a t i n g fuel, and ( 3 ) t h e p r e p a r a t i o n and handling of a e33U salt c o n t a i n i n g 23eu

2.1 Nuclear C h a r a c t e r i s t i c s of t h e 233U System A 1 assessment2 of t h e o p e r a t i o n c;f t h e Molten

Salt Reactor w i t h

233U has i n d i c a t e d t h a t t h e following could b e l e z r n e d by s u b s t i t c t i n g

t h e new fuel charge: (1) C r i t i c a l loadings would provide a check on t h e ava-ilable

n u c l e a r d a t a cn 233U

f o r predicting c r i t i c a l conditions i n a

r e a c t o r with a neutron energy spectrum similar t o t'nat of the proposed n o a t e n s a l t breeder r e a c t o r (VEBR). (21

&leasuremeat of 234u-to-233,

atom P a t i o s over a p e r i o d cf sub-

s t a n t i a l burnup might f u r t h e r e v a l u a t e a v a i l a b l e n u c l e a r d a t a

and c a l c u l a t i o n a l nethods.

(3)

I n t e r e s t i n g d i f f e r e c c e s would b e observed i n t h e d p a q i c s of t h e r e a c t o r because of tlre smaller f r a c t i o n of delayed neutrons

3 a v a i l a b l e from 233U f i s s i o n .

S t a b l e o p e r a t i o n w i t h 233U i n

t h e E R E would t e n d t o confirm t e i t a t i v e conclusions regwcling t h e dynamics of t h e M5BR. Knowledge of t h e f i s s i o n product y i e l d s f o r 233U1 e s compared w i t h t h o s e for

"'u,

would provide a means of more p o s i t i v e l y

i d e n t i f y i n g t h e r e a c t i v i t y t r a n s i e n t s t h a t f o l l o w changes ir: power l e v e l s . Changes i n o t h e r n u c l e a r c h a r a c t e r i s t i c s , such as temperature c o e f f i c i e n t s , neukron l i f e t i m e , and control. r e d worth, would be observed

2.2 Chemistry of t h e C i r c u l a t i n g F u e l The uranium c o n c e n t r a t i o n i n t h e r e a c t c r t r i l l be reduced t o 0 . 2 mole

$; however,

s i g n i f i c a n t i n c r e a s e i n UF

t a t i o n of urar,im o r UO, i s expected. c

concentraLion or p r e c r i p ~ -

Most of the p r o p e r t i e s o f %e

f u e l charge w i l l be v e r y s i m i l a r t o t h o s e of the 235U f u e l .

new

Mo change

i s expected i n t h e c o n p a t i b i l i t y of t h e f u . e l w i t h t h e g r a p h i t e a,:id

the

H a s t e l l o y N.

F u e l P r e p a r a t i o n by Wenote Means

2.3

A s t r o n g i n c e n t i v e c x i s ts â&#x201A;Ź o r develcping an eccmomieal method f o r

r e p r o c e s s i n g irradiated f u e l f o r r e u s e i n

power r e a c t o r .

T2;e

high

232U content of t h e 233U w i l l make remote p r o c e s s i n g of' a 233U f u e l charge mandatcry.

Therefore, it i s d e s i r a b l e t o prove t h e f e a s i b i l i t y of a

simple, d i r e c t fuel r e c y c l e process without t h e n e c e s s i t y of' h i g h - l e v e l decontarnination; t h i s would emphasize t h e advantages of t h e fi?el p r e p a r a t i o n f o r molten s a l t r e a c t o r s .

The p r e p a r a t i o n of t h e e n r i c h i n g s a l t , 7 L i F * g 3 3 , 4 Prom

7LiF and '33U02 -?

by z d i r e c t high-temperature,

(73-27xole

'$>?

one-step process, wac

i n v e s t i g a t e d 4 i n t h e laborakory and Pound t o y i e l d

satisfactory prodmt =

4 Hcwever, d u r i n g t h e cold r u n i n Euilding

7930, t h e h i g h temperatures

2 e c e s s a r y for t h i s process were f'ound t o promote c o r r o s i o n of t h e eqGipment; thus, an a l t e r n a t i v e method

w a s adopted.

a low-temperatu.re, two-step process

These p r o c e s s e s a r e discussed i n d e t a i l i n S e c t . 4.2.

3 . 1 High-Temperature, One-Step Process The chemical procedures t h a t were developed f o r t h e production o f t h e fuel c o n c e n t r a t e were s i m i l a r t o t h o s e used i n t h e r o u t i n e preparat i o n oP UF4 from c x i d e s . 0;' a

(1) t h e use

Necessary m o d i f i c a t i o n s included:

v e r t i c a l l y mounted, c y l i n d r i c a l r e a c t i o n v e s s e l r a t h e r than t r a y s

o r fluidized-bed reactcrs,

(2) the addition of

LiF t o t h e i n i t i a l charge

of material, and ( 3 ) t h e o p e r a t i o n of t h e process a t temperattu-es s u f f i c i e n t t o m a i n t a i n t h e LiF i n i t s molte3 s t a t e . La-bo-ratory-scale experiments w e r e conduc6,ed by t h e Reactor Chemistry

D i v i s i o n ec g a i n k f o m a t i o n a b c x t t h e rates a t which t h e r e a c t i o n s would occur and a l s o t o e x m i n e p o s s i b l e process c o n t r o l t e c h n i q u e s .

The

r e a c t i o n s i n v e s t i g a t e d were: Sintering:

Reduction:

WyiirofEuorinatLcn:

M2-m sparge a t 930-55O"C uc* t- 4HF uF4 + 2H20

Reduction of i m p u r i t i e s :

Hydrogen sparge at 700째C bF

+ H 2 -I@

i- 2pTp

I n t h e r e d u c t i o n s t e p t h e p r o g r e s s of t h e r e a c t i o n could be follcwec? by observing t h e g e n e r a t i c ? ? of water vapor i n t h e system.

of t h e gas eff1ue:it i n c r e a s e d markedly d u r i n g t h i s p e r i o d

The temperat-Jre e

DurrEng t h e k y d r o f l u a r i n a t i o n treatment, hydrogen, along w i t h anhy-

droys E?,was admitted t o t h e r e a c t i o n v e s s e l to c o n t r o l t h e c o r r o s i o n o f the v e s s e l and a l s o t o e n s m e t h e complete r e a u c t i o n of UO

U02.

The conversion s t e p CP t h e process w a s c a r r i e d o u t a t temperatures s u f f i c i e n t l y h i g h t o keep all of t h e LiP i n s o l u t i o n .

Thus, as W4 w a s

5 produced, the liquidus temperature of the fluoride components decreased from &kg to 4gO"C,

the mel3ing point of the eutectic mixture.

21 the

equipment use$ in the development runs, $he Liquidus temperature could be measured and the

4 concentration

could be determine& by comparison

with the phase diagram. K final treatment of the melt wikh hydrogen at

qOO"â&#x201A;Ź! reduced the concentyation of nickel and iron to acceptably How levels

Upon successful comptetion of the laboratory-scale experiment, z cold run, using equipment that more closely resembled the production equipment, was conducted by the Reactor Chemistry Division. 'This rwserved to further confirm the feasibility of' the one-step process and also to train key personnel -Tor the production operations at the Thorium-Uranium Recycle Facility (TURF)

3-22 Low-Temperatce, Two-step Process As an alternative to the high-temperature method, a two-step, low-temperature process was evaluated in a labsratoaay experiment and subsequently used in the s a l t production ruis.

this process, which

is sin;ilar to that used to produce the original fuel s a l t for the E R E ,

the temperatures ere generally much lower, and the LIP is not added until the conversion of' the oxide to the fluoride has been completed by hydrofluorination.

DESCRIWIQM OF SALT PRODUCTION FACILITY

The processing equipment was installed in cell G of the

71uRp,

vhich

is located in the Melton Valley area of Oak Ridge ITational Laboratory.

This facility contains shielded c e l l s and process supporting systems to permit remote fuel reprocessing.

4-1 Description

of the TURF

The TURP, Building 7930, was constructed at Oak Ridge Rational Laboratory to help develop and demonstrate economical remote methods

for reprocessing irradiated thorium-based fuel and for refabricating the purified fertile and fissile material into fuel suitable for reuse in a power reactor.

The m e of shielding and remote fzbricaticn methods

will permit the use cf simplified processes yielding only modest decor,taminatien factors. The W has sufficient space to accomodate equipment for process-

ing and fabricating 'uwo types of fuel assemblies simultaneously. Te' facility is divided into four nator &reas:

(E) an o f f i c e area aiijacent

tc, but isolated from, areas that contairL radioactivity, ('2) an operating area with a development laboratory, chemical makeup area, and equigment rooms for service equipnent, ( 3 ) a malctenznce operating area with service areas for receiving and storing spent fuels, and

(4) a

containing seven hot cells (six shielded and one mshielded)

cell complex e

Included in the f a c i l i t y arc the services, ventilation systems,

crane and manipulator systems, viewing systems, and liquid and gaseous waste disposal systems necessary to support fuel reprocessing.

4.1.1 Cell G The 233U fuel charge fer the KWE was prepared in cell G .

interior of this cell is 20 ft wide, 16 ft longJand 33 ft 5 i g h .

The

A false

flser waE installed to elevate the process equipment so that the thmughwall naster-slave manipulators could be used and rnaximm advantage could b e taken or" the viewing capabilities of the shielding windows.

miis

decreased the effective height of the cell to 22 ft, which, in reality, was further reduced tc

14 ft of

effective headroom because of the in-

cell electremechanical manipulator system space requirements at the top of the cell.

The walls, ceiling, and floor of the cell are lined with

stainless steel. Six cell operating modules (Fig. 1) are built into t k walls of the cell; four of these are equipped with viewing windows, and two have window fo rn s that are filled with removable shielding. There are more than 100 penetrations into the cell for process services many more than are required for the salt preparatior:.

-5

The cell venti-

in. H 0 and a flow 2 of 1033 cfm of air through the c e l l ; the vessel off-gas system removes

lation system nomally maintains a pl-essure of

8 25 cfm of a i r from t h e c e l l and process v e s s e l s and r o a t e s it t o a system t h a t i s maintained a t a p r e s s u r e of -17 i n . H 0. A s m a l l e n t r y 2

p o r t permits i n t r o d u c t i o n of small t o o l s a d miscellaneous items through a glove box and an a i r l o c k .

roof of t h e c e l l c o n t a i n s a hatch with

a 10- by 6-ft opening t h e t i s s e a l e d and s h i e l d e d .

The h a t c h Frovides

access t o t h e c e l l with t h e 50-ton b u i l d i n g c r a n e .

Eight master-slave

manipulators were i n s t a l l e d i n t h e c e l l :

four C e n t r a l Research Nodel A

and f o u r C e n t r a l Research Model D u n i t s .

A Program and Remote System

Model 3000 electromechanical manipulator system i s moznted on r a i l s -Lo g i v e complete coverage of t h e c e l l .

4.1.2 Radioactive ~ o kt a i n

o ~ t ff-~a System s (RED-HOG)

The r a d i o a c t i v e hot d r a i n - - h o t o f f - g a s system i s a combination by-

product waste c o l - l e c t i o n system and v e s s e l off-gas system.

It has i n l e t

cocnections i n t h e h o t cells and a t v z r i o u s p o i n t s throughout t h e f a c i l i t y .

The network o f s t a i n l e s s s t e e l p i p i n g i s designed to han15le gas and l i c p i d i n concurreiit flow.

Liquid waste i s s e p a r a t e d from t h e off-

gas and i s c o l l e c t e d i n t a n k B-2-T i n t h e belcw-grade and s h i e l d e d waste tank p i t .

Tae gaseous stream flows through a bank o-C a b s o l u t e f i l t e r s

and then into t h e c e l l exhaust s y s t e x l o c a t e d upstream of t h e f i l t e r

units f o r t h a t system.

The l i q u i d wastes may be pumped e i t h e r i n t o t h e

Melton Valley waste system o r into c e l l G f o r recovery of v a l u a b l e materials

%wc connecti.ons from c e l l G to t h e HQG system were made f o r t h e s a l t preparetion process.

One connection was made t o t h e capsule d r i l l -

i n g stazion i~ order 'io collect t h e p a r t i c u l a t e matter r e s u l t i n g fron; the d r i l l i n g eperation. station.

The o t h e r was made t o a multipurpose manifold

With t h e HOG system pressure c o n t r o l l e d a t

-17

in.

0, t h e

2 f l o ' ~o f~ air from t h e c e l l was a d j u s t e d t o 25 cfm by a m a ~ m l l yo p e r a t e d valve.

The gaseous e f f l u e c t fl-om t h e process scrubbing system vas dis-

charged i c t o t h i s manifold s t a t i o n , t h e r e b y e n s u i n g dilution, i n t h e c a s e o f hyclrsger,, t o less t h a n t h e explosive l i m i t .

I n addition t o the

scrubber discharge, t h e manifold s t a t i o n served t h e i n - c e l l t i t r a t i o n s t a t i o n , t h e sampling s t a t i o n , t h e can-opening bcx, t h e scru-bber s y s t e n

and sink l i q u i d d r a i n s , and a l l of t h e process v e s s e l s .

Some of t h e s e

connecticns were made t o t h e manlifold s t a t i o n on t h e c e l l s i d e of t h e

manual flow r e g u l a t i n g valve, where t h e p r e s s u r e was -5 were made

-15 i n . H,?O.

i n . H 0; sene

2 %he HOG s y s t e n s i d e o f t h e valve, where t h e p r e s s u r e was The l o c a t i o n of each connectLon depenaed upon t h e p r e s s u r e

requirement for t h a t p a r t i c u l a r use e

4.1.3 Cell

Ventilation

Approximately 1033 cfrn of a i r e n t e r s c e l l

from t h e c e L l G pump

room via. a s e r i e s of filters, a f i r e danper, a back-flow preveiiter, an6 a c e l l pressure c c x t r o l valve.

It d i s c h a r g e = i n t o t h e cell from dif-

fusers t h a t are mounted on t h e c e l l c e i l i n g arid t h e n flows through roughing f i l t e r s l o c a t e d a t t h e f a l s e floor (end a l s o a t t h e c e l l floor l e v e l ) i n t o t h e c e l l v e n t i l a t i o n system macLEold i n t h e n o r t h valve

pit. duct.

The f l o w i s c o n t r c l l e d by a maRmlly loaded valve i n t h e exhaus; The exhaust 2s r o u t e d t o t h e f i l t e r p i c , where it p a s s e s thrCJugh

two sets of f i l t e r s i n s e r i e s ; from t h e r e , it passes tlirongh a 3 2 - i n . d c c t t o t h e c e n t r i f - g a l blowers and i n t o t h e 250-ft HFIR s t a c k f c r disFersPon

i n t o t h e atmosphere. a p r e s s u r e of

The c o i t r o l s or, zhe v e n t i l a t i o n system m a k i t a i r _

-5 i n . H 0 i n t h e cell under nom-a1 c o n d i t i o n s .

Pressures 2 as low as -20 i n . H 6 o r a s high as -1 i n . %E 0 car, be maintain& i n t h e 2 2 c e l l under c e r t a i n emergency c o n d i t i o n s . Only a f a i l u r e of' a l l emergency systems w o u l d a l l o w the pressure i n the cell to rise above

-4.5

i n . H20.

4.1.4

Shielding The s h i e l d i n g o f t h e TURF I s designed in scch a manner t h a t , durEng

o p e r a t i o n w i t h r a d i o a c t i v e material having an i n t e n s i t y of l C . 5 r- / h r , t h e p e n e t r a t i n g dose r a t e s i n normally occupied areas are no g r e a t e r t h a n

0.25 mrem/hr, w i t h s m a l l h o t spots no g r e a t e r t h a n 2.5 m r e m / h r .

Dose

r a t e s g r e a t e r t h a n this are p e r m i t t e d i n l i m i t e d - a c c e s s areas and â&#x201A;Źor short-term, non-routine o p e r a t i o n s .

10 To s a t i s f y t h e allowable design r a d i a t i o n l e v e l s , t h e o p e r a t i n g c e l l s have 5 - 1 / 2 - f t - t h i c k

walls of n o m a 1 c o n c r e t e up 'eo a h e i g h t of

11 ft, b1/2 f t of normal concrete f o r t h e renaining p o r t i o n s of t h e

v e r t i c a l walls, and 5 - f t - t h i c k c o n c r e t e on t h e r o o f .

This amount of

b i o l o g i c a l s h i e l d i n g w a s more t h a n adequate t o reduce exposrrre dose rates t o

< 0.1 mr/hr.

The windows a r e e s s e n t l a l l y e q u i v a l e n t , i n s h i e l d i n g t h i c k n e s s and i n t h e i r a t t e n u a t i o n of p e n e t r a t i n g r a d i a t i o n , to t h e c o n c r e t e walls i n which t h e y a r e i n s t a l l e d . blies:

Each window c o n s i s t s of two major assem-

t h e s e a l glass t h a t i s removable from i n s i d e t h e c e l l , and t h e

tank u n i t t h a t i s removable from t h e o p e r a t i n g f a c e of t h e c e l l . window i s a composite u n i t c o n s i s t i n g of

i n . of g l a s s and

hch

58 i n . ' o f

zinc bromide s o l u t i o n ; it i s w e l l s e a l e d t o mintmfze leakage of a i r around i t s p e r i p h e r y .

4 15 a

bihnipulators

A Programmed and Remote Systems Model 3900 Manipulator System i s i n s k a l l e d on a set of' rails ir_ c e l l G .

The tube h o i s c on this manip-

ulator has a v e r t i c a l t r a v e l cf l3-1/2 f t and a l i f t i n g c a p a c i t y of l~3OO lb. The t r o l l e y and b r i d g e t r a v e l , along with t h e v e r t i c a l t r a v e l of t h e t u b e hoist, provides complete n a n i p u l a t o r coverage sf t h e cell down t o the f a l s e floor.

This mit provides a l l t h e motions of t h e hurnan

a r m , p l u s wrist extension and ccnttnuous r o t a t i o n a t t h e mist and a t t h e shoulder.

A g r i p f o r c e cf 200 lb can be e x e r t e d with t h e Pingers.

The hand i s remotely removable and can be r e p l a c e d by a hook f i x t u r e o r an iKpaet wrench. One C e r t r a l Research Model

A master-slave manipulator and one

Model B master-slave manipulator a r e i n s t a l l e d a t each of t h e f o u r viewing windows i n c e l l 6 ; .

The Model A and t h e Model D manipulator have

niaximux l i f t cepabilities of 25 lb and 100 lb, r e s p e c t i v e l y . These master-zlave units were i n s t a l l e d t o o p e r a t e valves, t o make and break t u b i n g disconnects and e l e c t r i c a l and thermocouple disconnects, and t o conduct t h e hand operations required in t h e p r o c e s s . hand t o o l s were modified f o r use w L t h these manipulators.

Conventional

The PaR electromechanical manipulator was i n s 5 a l l e d r ~ cperf'crm t h e heavy-duty maintenance, to convey heavy asseribPies around t h e c e l l , t o r e a c h sone p a r t s o f t h e c e l l thak were not a c c e s s i b l e t o t h e masters l a v e manipulators, and t o provide a " t h l r d r t hand to sin-obify c e r t a i n operations.

4.2

Process Floveheets

Two p r o c e s s e s were developed f o r t h e p r e p a r e t i o c c:' tne fuel concentrate: process.

(I) a high-temperature process, and (2) a low-temperatire

The second process w e s a.dopted a f t e r conclusion of t h e c c l d

run whec it became e v i d e n t t h a t t h e o r i g i n a l process caused s e v e r e corros-ioc o f t h e r e a c t i o n v e s s e l .

4.2.1 High-Temperature Prccess The c h e x i c a l Plowsheet â&#x201A;Źor t h e one-step, high-temperature ~ m c e s s as shown ir_ block forin (Fig. 2) i n c l u d e s the Pollowing rnajcr s t e p s :

(E)

P a r k j a l r e d u c t i o n of t h e uran5.m oxiaeJ233V0 by t h e m e l

means

(2)

Furthey r e d u c t i o n t o UO by hydrogen t r e a t m e n t . 2

( 3 ) Conversion of t h e oxide t o E?4 by h y d r c f l u o r i n a t i o n and ccnc u r r e n t dissolution o f t h e 4 I n t h e rLoltear LiF t o form t.he e u t e c t i c mixture

(4)

F i n a l p u r i f i c a t i o n of t h e e u t e c t i c mixture by t r e a t m e n t w i t h h i g h - p u r i t y hydrogen.

The

7LiF

was combined with the 233U0 i n t h e i n i t i a l charge -to t h e

reaction veseel.

The r e d u c t i o n process w a s t h e n conducted a t texpera-

tures in excess o f 845Â°C (EiP m e l t i n g p o i n t ) s o t h a t t h e oxide p a r t i c l e e were suspended i n t h e n;olten f l u o r i d e .

The molten LiF served t o keep

t h e oxide p a r t i c l e s w e t , t h u s reducing t h e p o s s i b i l i t y of entrainment of p a r t i c u l a t e matter i n t h e e f f l u e n t gas stream.

During t h e h y d ~ o -

fluorination Etep, t h e progress of the r e a c t i o n was estimated by determining t h e l i q u i d u s temperature of t h e molten m a t e r i a l , and ";hen

Portid

MELT

Note:

reduction

of UQg

ANALYSIS

If results

HF STRlPPlNG

of chemical

Fig.

cmdysis

(Steep 5) d 0

Chemical

net meet

Flowsheet

spcifications,

i"or

continue

Preparation

HF-H+J

treatment

of" the

SALT

TRANSFER

(Steep 4Js

233 U Fuel

Concentrate

-for

the

b4SRE.

t h e f u r n a c e temperature c o n t r o l l e r w a s a d j u s t e d t o approximately 5 0 째 C above t h i s values Frequent t i t r a t i o n s of t h e r e a c t i o n vessel e f f l u e n t gas stream y i e l d e d v a l u a b l e i n f o r n a t i o n on t h e p r o g r e s s of t h e convers i o n of t h e oxide t o -%e f l u o r i d e s i n c e t h e u t i l i z a t i o n of

E? remained

q u i t e h i g h and n e a r l y c o n s t a n t u n t i l t h e conversion w a s completed. Chemical a n a l y s e s of f i l t e r e d samples of t h e nzeLt were made t o determine whether t h e f i n a l process by hydrogen s p a r g i n g

$he p c i f i c a t i o n cf the product

Ehould be i n i t i a t e d o r whether t h e k y d r o f l u o r f n -

a t i o n process should be continued

4.2.2 Low-Texperature Process The low-temperature process ( s e e F i g . 3 ) w a s used t o prcduce t h e

It d i f f e r s i n o n l y one rrajor r e s p e c t from t h a t used

f u e l concentrate'

i n the production of t h e o r i g i n a l 235U-bear5ng e n r i c h i n g s a l t f o r ",he

ERE.

I n t h e e a r l i e r process, t h e s t a r t i n g material w a s W4; i n t h e

low-temperature p r c c e s s , t h e s t a r t i n g inateriel i s UO

The oxide i s

d i g e s t e d a t 550째C and t h e n reduced t o UO, by t r e a t m e n t wi-ch hydrogen I i

a t temperatures ranging from 4 0 t o 550째C.

Helium i s used as a d i l u e n t

gas d u r i n g t h e reducLion s t e p until t h e major p o r t i o n of t h e exct'lermic r e a c t i o n i s conpleted.

The oxide i s t h e n conver-f;ea t o W

f l u o r i n a t i o n a t temperasures ranging f r o m ~ Q Ot o hydrogen) c o n c e n t r a t i o n s varying from

5 t o 407%.

4 by

630"~and

hjrdro-

a t MF ( i n

The f i n a l s t e p s of' t h e

process iravoive mixing arid f'using t h e f l u o r i d e salts, c o n t a m i n g with and hydrogen t o remcve r e s i d u a l oxides and c o r r o s i o n product imp u r i t i e s , acd f i l t e r i n g t h e molten s a l t d w h g i t s t r a n s f e r t o t h e s t o r a g e coritainers

The r e d u c t i o n and eonverslon p r o c e s s e s were monitored by a therrnocouple a r r a y t h a t w a s i n s e r t e d i n t o t h e powder i n t h e r e a c t i o n vessel and by measurernelzts of hydrogen u t i l i z a t i o n d u r i n g t h e r e d u c t i o n s t e p and of HF u t i l i z a t i o n d a r i n g t h e conversion s t e p .

U n f i l t e r e d and f l l -

t e r e d samples of t h e m e l t were withdrawn f o r oxide, p e t r o g r a p h i c , and

metal i m p u r i t y analyses.

....,.,. ..

, % . &

> % .;

-13e2

as uo3

3 TO 5 hr BlGESTlON AT 558°C; COOL TO 400°C.

HEAT TREAT U03P

HYDROGEN REBIBCT&ON: 810 2

START 5% 1-12 AT 4 eC AND INCREASE TO 50% Ha; T ~ ~ ~ ~ RRISES A TTO~ 490°C; ~ E TREAT AT 500-550"C AT 100% USAGE OF Hgg; COOL TO 4063°C..

START ~ 5% HF ~ IN H2 AT~ LCW@C;I ~ CREASE TO ~ 48% HF I N H2; ~ ~ ~ ~ INCREASES ~ A ~ TO I 450°C; B ~ E WHEN HF USE DECREASES BELOW 80%# INCREASE THE TEMPERATURE YO 630'C STEPWISE UNTIL HF USE ECOMES 0; COOL TO 150°C.

uog

uo2 -UF

EUTECTIC F ~ UF4 Q LiF -kJF4-

~ ~ LiF

I ADD ~ EXACT N ~ QUANTITY OF LiF; MELT UNDER 30% Hy D&GESTAT 850°C FOR 3 TO 5 hr; COOL TO 700°C.

E UTECTK PURIFICATION: MO %- HF -.MF Q H2Q MF + H q - " M Q t HF

PURGE MELT 24 TO 30 hs AT 900°C W m 20% HF IN H2; TREAT WITH M p FOR 75 TO 150 hr.

PRODUCT PURITY:

UNFILTERED SAMPLE ANALYZED FOR OXIDE CONTENT. FILTERED SAMPLE ANALYZED FOR METALLIC IMPURITIES.

P i g . 3 . Chemical Flowsheet f o r the Low-Temperature Process for Preparing the BERE Fuel Concentrate.

The temperatures e l c o u n t e r e d i n t h i s process are g e n e r a l l y 230째C lcwer ;harz t h o s e measured i n t h e s j n g l e - s t e p , h i g h - t e n p e r a t u e process The aaoption of t h i s procecs wads P e l t t o be j u s t P f i a b l e witmv.5 t k e bene-fit of a f u l l - s c a l e c o l d r u n because of t h e :

(I) success of t h e lz'boratory-scale experiment, (2) s i m i l a r i t y of t h i s process t o t h e o r i g i n a l corice:il;rate produ c t i o n process,

( 3 ) imprcvements made i n the grocess iEonitoring i r s t r u m e n t s and t e chni ques

(4) t h e time schedr;le involved. 4.3

Process E q u i p e n - t

The e q u i p e n t flcwsheet shown i n P i g .

4 is

a simplified presentation

o f t h e m L j o r corfipanents req-aired i n t h e proceEs

(I)

These components are:

t h e f u e l decanning s t a t i o n ,

(2) t h e r e a c t i o n o r oxide t r e a t m e n t v e s s e l ,

(3)

t h e s a l t storage and t r a n s f e r v e s s e l ,

(4) various

(5)

c o n t a i n e r s for s h i p p i c g t h e product,

t h e o f f - g a s scrubbers

I n addition, t h e process r e q u i r e s many o t h e r smaller p i e c e s of eqdipment, such as :

t h e oxide can p r e p a r a t i o n equipment, t h e in-cell

t i t r a t i o n assembly, t h e f u r n a c e s f o r t h e v e s s e l s , t h e enrichment capsule d r i l l i n g and weighing s t a t i o n , dlsconnect s t a t i o n s f o r e l e c t r i c a l and instrument l i n e s and process gas bines, and work t a b l e s and t o o % r a c k s .

Figures 5 and

6 show

some of' t h i s equipKent a f t e r i n s t a l l a t i o n .

A l l s e r v i c e s and r e a g e n t s c u r c e s are l o c a t e d i r a t h e p e n t h w s e

outside the c e l l .

ORNL D W G 67-11638 R 1

GAS SAMPLE ANALYSIS

FLOW

RESTRICTOR

---He

PURGES -1/2

slm

~ i g .4. Simplified ChernizaI acd Engineering o ow sheet far

Preparing 233Y Fuel Salt.

.. ....._ .

v.....

F i g . 5. Y i i n Reaction Vessel Furnace and Auxiliary Equipment fcr 233U Fuel S a l t P r e p a r a t i o n - Cell G, B u i l d i n g 793Q.

0 b

...

4.3 I Becanxirig S t a t i o n e

The decanni3g s t a t i o n (Fig.

i s a r a t h e r complicate,3 work box

t h a t i s reqLired ?or cpening t h e double-container cans, e x t r a c t i n g t h e oxide powder, f e e d i n g t h e powccr to t h e r e a c t t o r , vessel: and d i s p x i n g

To accc)mplish t h i s , t h e s t a t i o n t r e a t e d each can i n

or t h e spen5 cans.

t h e f o l l o w i n g manger : Received t h e f u l l can and f e d it i n t o a r o t a t i n g chuck. Tightened t h e c h - x k co grip t h e can while t h e grocvlng t o o l f o m e d a groove deep eno~@ t o f j x t h e Inner end o u t e r cans together.

Tkis was done twice ?or each can.

Pushed t h e can i n t o t h e OX, d i s p l a c i n g t h e prevlously o p m e d

car1

E j e c t e d ;he p r e v i c u s l y opened can and l i d . GrLpped t h e can, supported it, anC r o t a t e d it ~ h i l et h e c x t t i n g tocl c u t it oper,. Removed and r e t a i n e d t h e cv.6,-off Ild while t h e can w a s emptied of oxide b y v i b r a t i o n and kru.shing* I n s p e c t e d t h e i n s i d e of' t h e can and l i d f o r r m a i n i n g pcwder. T r a n s f e r r e d t h e powder Y r c m t h e box i n t o t h e r e a c t i o n v e s s e l by v i b r a t i o n and u s e of in-box t o o l s .

Pie decannixg s t a t i o n w a s designed f o r alpha containment. p e n e t r a t i o n s t o it were s e a l e d by O-rings and b o o t s .

AI1

Each s p e n t can

a c t e d as a. seal u n t i l it w a s d i s p l a c e d b y t h e next can. A ball valve and charging hopper s i t u a t e d on t o p of t h e box was

used t o Introduce t h e LiF t o t h e system.

4.3.2

Reaction Vessel

A l l of t h e chemical r e a c t i o n s of t h e process were conductet; i n

t h e r e a c t i o n vessel ( F i g .

7-7/16 i n . ID

and

8). The cold-run vessel was

36 i n . high, f a b r i c a t e d from

type

a r i g h t cylinder,

301;L s5alnless

ORNb DW e-67- I I674

Material: Vessel 8 P i p e 3 0 4 L SST. Liner, Diffuser 8 Dip Line:

Nickel 208

Sample Line

O f f Gas

Fig. 8. Weactisn Vessel T-P.

22 s t e e l ; it ccntaineci a free-stanciing l i n e r , 1 / E i n . t h i c k , c o n s t r u c t x d from type 201 n i c k e l , and w a s designed, on t h e b a s i s of stress r u p t u r e d a t a , f o r R e p e c i f i e d s e r v i c e 1Lfe.

The v e s s e l conteined nozzles t o

permit powder a d d f t i s n , s a l t sampling, g a s e o ~ se f f l x e n t discharge, and Wpon completion of t h e cold rmJ t h e d e s i g n of t h e

product t r a n s f e r .

v e s s e l was modified t o i n c l u d e a t r u n c a t e d c c n i c a l boxtom t o provlde b e t t e r c o n t a c t of' t h e reagent g a s e s . i n t h i s vessel. vessels

4.3.3

i E

Design information f o r t h i s v e s s e l and t h e o t h e r process

l i s t e d i n Table 1 .

S a l t Storage an6 T r a n s f e r Vessel

The t r a n s f e r v e s s e l (Fig. and

The F r o d a c t i s n runs were conducted

9) w ~ sa

riglit cylinder,

4 i n . ir, diameter

36-1/2 i n . t a l l , c o n s t r u s t e e sf type 231 nickel. ~t contained f i v e

nozTles, one cf which w a s a s p a r e .

%e f u n c t i o n of t h i s vessel wzs t o

receive a f i l t e r e d , p c r i f ' i e d b a t e h of t h e e n r i c h i n g caEt f r o m t h e rea c t i o n w s s e l and t o d i s p e n s e It t o t h e v a r i o u s product s h i p p i n g eon-

tainers.

waE

necessury for t h i s v e s s e l t o s t o r e salt f o r 24 hr o r

more C w l n g t h e ehapgeou'e of some of t h e shipping c o n t e i n e r s .

The shipping c o n t a i n e r s were arranged i n t o t h r e e a r r a y s f o r khe f i l l i n g operations.

Eater, upon completion of t h e f i l l i n g o p e r a t i o n

a.nd freezsing cf t h e salt, each a r r a y was disassembled i n t o ir-dividuel c c n t a i n e r s f o r shipmen5 t o t h e bER3. ~ 1 2 ef i r s t

a r r a y ( ~ i g10) ~ c o n s i s t e d of

4-5 enrictmext

(see F i g . E % ) , each o f which was 3/4 i n . i n d i a n e t e r and and designed t o c o c t a i n

crmiun.

capsules

6 i n . long

me capsules were connected

i n s e r i e s and arranged i n three 15-capsule decks.

An overflow p o t

c o n t a i n i n g P i q L i d l e v e l d e t e c t i o n elements and t h e m o c s u p l e s was t h e

last v e s s e l i n t h e s e r i e s .

The t u b i n g connections i n t o , and o u t of',

ezch capsule were p r e c i s e l y p o s i t i o n e d

that u n i f o m f i l l i n g ani?

sulclsequent blowback sf t h e o v e r f i l l were p o s s i b l e .

Two holes were

d r i l l e d i n each capsule t o permit t h e s a l t t o flow out when t h e capsule

23 Table 1. Equipment Design Information: MSRE 233U Fuel Salt Preparation

Item or Requirement

Reaction Vessel T-1 Outer

Reaction Vessel Inner Liner

Salt Storage Vessel T-2

Salt Addition Cana

Enrichment Capsule

Furnace Liner F-1

Furnace Liner F-2

Furnace Liner F-3

Type of material

304L SS

201 Ni

304L SS

300 ss

300

Maximum operating temp., OC

900

700

600

goo+

Maximum operating pressure, %j+at 9000~~ Free standing 20# at 700째C liner in reaction PSit3 vessel; no pressure difference developed

Open

Maximum operating vacuum, Psi@;

Design temperature, OC

900

Design pressure, psig

6# at 900"~

304 SS ELC

(Limiting condition) Calculated maximum stress, Psig

727 psi at 6 Psig

Maximum stress is that due to head of salt in liner and is negligible

3000 psi at 700" Cb

Allowable maximum stress at maximum operating temp. Overall height, in. Bottom plate thickness, in.

2560 psi at 20# gage

35-718 118

36- 112 1/4

No load carried No load carried by bottom plate by bottom plate or wall or wall

glO psi at 930째C

Variable

5/16

112

37 114 (reinforced with welded beam on diam)

Flat head thickness, in.

114

Outer diameter, in.

4- 112

2- 112

10-314

Wall thickness, in.

15./64

0.065

0.359

Inner diameter, in.

4- 1/32

2-37

10.032

Top flange OD, in.

Top flange thickness, in.

Hemispherical bottom wall thickness, in.

Hemispherical top, in.

aDesigned by MSRE. blO,OOO hr creep-rupture data; design based on service << 10,000 hr.

16 318

n, Y

2 m

P 0

E !

I z

'0 ..

v) u)

6”

P i g . EO.

PHOTO 91466

F i l l i n g Array Consisting cf

’$5 Capsul es.

O R N L DWG- 67-1 8676 R i

F i g . 11. Typical Enrichment Capsule.

i s lowered i n t o t h e MSRE pump bowl.

A cable-and-latch assembly w a s

a t t a c h e d t o each capsule for use i n t h e sampler-enriched o p e r a t i o n at the reactor.

The second a r r a y ( ~ i g .1 2 ) c o n s i s t e j of f o u r 2-i/'2-~n.-diam -3y 34-in.-long cans connected i n series f o r f i l l i n g o p e r a t i o n s . designed t o c o n t a i n pot.

7 kg

Each w a s

OS uranium and had an instrumentee overPlow

The cans were l a t e r Ciisassembled, and t h e t o p arid bottom plugs

were removed; t h e n t h e cans were f i t t e d wLth l i f t i n g b a i l s and bottcm

"stopper-tee" plugs and welghed.

They are being shipped, one a t a

t i m e , t o t h e ISRE, where t h e bottoE plug of' each can i s rexoved bef'ore t h e c m i s lowered i n t o t h e d r a i n t a n k .

I n t h i s tank, t h e s a l t xelts

and runs o u t of t h e c o n t a i n e r .

13) contained a group of s i x 2 - l / 2 - i n B - d i a K v a r i a S % e - l e n g t h c a r s (see F i g . 14) t h a t were s i m i l a r i n desrign end 'fie t h i r d a r r a y ( F i g .

arracgement t o t h o s e i n t h e second a r r a y .

One of t h e s e cans w a s used

t o s t o r e excess product rnaterial t h a t was blown back from t h e o t h e r f i v e cans a f t e r t h e y had been f i l l e d t o overflow.

The l a t t e r cans were

0.5 t o 3 kg o f u r a r i m ( 2 cans, 0.5 kg ekch; one can, 1 kg; one can, 2 kg; and one can, 3 kg).

designed t o c o n t a i n

4.3.5

Scrubbers A c a u s t i c scrubber system w a s L n s t a l l e d t o n e u t r a l i z e t h e MF

e f f l u e n t from t h e r e a c t i o n v e s s e l b e f o r e it w e s discharged to the T U i

KOG system.

The scrubbers, namely, f o u r l 3 - g a l polyethylene b o t t l e s

f i l l e d w i t h 10% KOH, were connected i n s e r i e s and f i t t e d w i t h t h e n e c e s s a r y f i l l - a n d - d r a i n connections.

The f i r s t b o t t l e i n t h e s e r i e s

w a s k e p t empty, and t h e d i p l i n e s i n t h e subsequent b o t t l e s were posi-

t i o n e d a t an e x a c t depth.

Thus t h e f i r s t b o t t l e had an adequate volume

t o r e t a i n any l i q u i d t h a t might Slow back toward t h e r e a c t i o n v e s s e l ( i n t h e event t h a t t h e p r e s s u r e d i s t r i b u t i o n i n t h e system became reversed).

Also, a vacuum b r e a k e r w a s i n s t a l l e d t o prevent t h e occur-

r e n c e of a vacuum, which could cause c o l l a p s e of t h e b o t t l e s .

28 PHOTO 984M

F i g . 12. Second F i l l i n g Array: Four Cans, Each Containing 7 kg of UranirJm.

F i g . 13. T k i r d Filling Array Containing Six Shipping Conteiners of' Miscellaneous S i z e s .

w G - 67- I I67 7

Selt eapaci t y DIMENSION 'A' Kg 3 3.59 2 14.802 IO.102

9.0 3.0 2.0

I .o 0.5

5.402 3.05%

2.I

x 0.865" \Ala I I

Tlebi ng

Fig. 14. Salt Adbition Can.

Raschig r i n g s had been i n s t a l l e d t o prevent c o l l a p s e of t h e b o t t l e s i n t h e scrubber system used i n t h e c o l d run; however, t h e s e r i n g s p r e v e r t e d u n i f o m mixing and were subsequently r e p l a c e d by

vzcu~.mb r e a k e r

4.3 6 Miscellaneous Equipment e

Oxide Can Lengthening Equipment.

The 233U0

decanning s t a t i o n

w a s designed by u s i n g can drawings and eample cans from t h e Savannah River Laboratory.

A f t e r t h e decanner w a s f a b r i c a t e d , it w a s d i s c o v e r e d

t h a t t h e a c t u a l cans were

1-3/4 i n .

s h o r t e r t h a n denoted on t h e drawings

(The measurements o f t h e a c t u a l cans had n o t been checked c l o s e l y because of t'ne high r a d i a t i o n l e v e l s of t h e o x i d e . )

Since m o d i f i c a t i o n

of t h e decanner was i m p r a c t i c a l , w e decided t o l e n g t h e n each can 1-1/2 i n . by cementing an extensicjn on it.

Three i t e m of ecpiprr,ent, as

15, were r e q u i r e d t o accomplish Lhis:

shown i n F i g .

(1) a n a c h i n i n g

f i x t u r e t o bevel t h e end of t h e can, (2) a press t o f o r c e t h e e x t e n s i z n

o n t o t h e can, and ( 3 ) a f i x t u r e t o c u r e t h e epoxy r e s i n used cernented j o i n t

the

I n - C e l l T i t r a t i o n Assembly.

The o f f - g a s t d t r a t i o n assembly

c o n s i s t e d of a t r a i n of t'nree +in.-diam

by 6 - i n . - t a l l @.ass

vessels,

a w e t t e s t meter f o r measuring gas flows, alnd t h e n e c e s s a r y t u b i n g and valves t o permit r e a g e n t s t o be added azd f l u s h e d f r o m o u t s i d e t h e c e l l . F w n a c e s and Heaters.

Three high-temperat;e>

electrical-

r e s h t a n c e - h e a t e d furnaces were i n s t a l l e d i n c e l l G f o r temperature c o n t r o l of v e s s e l s used i n t h e treatment, s t o r a g e , and t r a n s f e r of t h e

salt 8

A Zk-kw,

1 2 - i n . - c a v i t y f u r n a c e w a s used for t h e r e : x t i o n v e s s e l ;

7-1/2-kw, 4 - 7 / 8 - i n . - c a v i t y

anu a 10-kw, 4-7/8-in.-cavity assemblies.

u n i t w a s used for t h e t r a n s f e r v e s s e l ; u n i t was used f o r t h e shipping c o n t e l n e r

Locally f a b r i c a t e d clamshell heaters using tubular

r e s i s t a n c e - h e a t i n g elements provided h e a t to t h e nozzles Located on t h e t o p s of t h e vessels.

The s a l t t r a n s f e r l i n e s were h e a t e d by a t -

t a c h i n g t u b u l a r h e a t i n g elements t o t h e t u 3 i n g and t h e n appbjTing thermal. insulation.

o f f - g a s l i n e (and f i l t e r ) w a s heated with e l e c t r i c a l ,

r e s i s t a n c e - h e a t i n g t a p e t o prevent condensation of â&#x201A;ŹIF o r water v ~ p o r

i n the line.

33 Enrichrcent Capsule D r i l l i n g and Weighing F i x t u r e . - Two h o l e s were d r i l l e d i n each of' 45 e n r i c h r e n t capsules t o pemHt t h e salt 'vo f'lcw o u t whex t h e capsule i s immersed i n t h e s a l t i n t h e r e a c t o r pump bcwb. Upon disassembly of t h e capsule f i l l i n g a r r % y J each capsule w a s inser2eCL

i n t o t h e work box ( P i g .

16); here, a

bottom o u t l e t h o l e and a t o p v e c t

h o l e were d r i l l e d 4n t h e capsule, the capsule was weighed, t h e l i r t i n g b a i l wes t e s t e d for i n t e g r i t y , and the capsule was I n s e r t e d i n t c t h e shipping c a r r o - J s e l

The t r a n s p a r e n t box served as c o n t a i m e n t d u r i n g

the d r i l l i n g operation.

Off-gas from t h e capsule d r i l l i n g box passed

through a n a b s o l u t e f i l t e r and

W%E

t h e n discharged t o t h e p l a n t v e s s e l

o f f - g a s system. Disconnects. - The e l e c t r i c a l and thermocouple d i s c o n n e c t s used i n t h e cell were s t a n d a r d commercial u n i t s .

Generally, one-half of t h e

disconnect w a s rrounted r i g i d l y t o f a c i l i t a t e making and breaking operat i o n s with t h e m a s t e r - s l a v e maariprulators * S e v e r a l t y p e s of p i p e ard t u b i n g d i s c o n n e c t s were uced. t h e gas s e r v i c e line:

u t i l i z e d b a l l - c h e c k quick d i s c o n n e c t s .

I n general, Compressior

f i t t i n g s were used i n t h e salt t r a n s f e r line:: and i n t h e main o f f - g a s lines.

Conventional screwed p i p e connections were used i n a r e t s where

remote o p e r a t i o n of t h e j o i n t was n o t consldered necessary.

Loca1l.y

dceigned and f a b r i c a t e d connections w e r e u s e d i n s e v e r a l l a r g e - d i a m e t e r j o i n t s t h a t would p o s s i b l y r e q u i r e remote rmintenance. Work Tables and Tool Racks.

The p r c c e s s equipment w a s pcsitioned

i n t h e ceLl t o o b t a i n maximum advantage of t h e c a p a b i l i t i e s of t h e et@+, a v a i l a b l e m a s t e r - s l a v e maxipubators. i n g s t a n d s and mounting framework.

Extensive use was made of support-

Tool r a c k s for t h e r e q u i r e d hand

t o o l s were l o c a t e d a t t h e major work c e n t e r s .

Where p o s s i b l e , t h e void

spaces between t h e process equipment and t h e c e l l w a l l s were f i l l e d with t r a y s t o provide e x t r a work areas, space f o r temporary t o o l s t o r a g e , and

a s u r f a c e on which t o c a t c h t o o l s and s m a l l equipment L t e m s t h a t were dropped.

A l a r g e work t a b l e ( P i g .

14) w a s

i n s t a l l e d t o accommodate t h e

product s h i p p i n g c o n t a i n e r disassembly, t h e shipment p r e p a r a t i o n operat i o n s , and t h e capsule d r i l l i n g and weighing f i x t u r e .

m a 43

Fig.

17.

I n - C e l l Work ' F a b l e .

The t a b l e s , racks, and supports were f a b r i c a t e d from carbon s t e e l ; t h e t r a y s were f a b r i c a t e d from s t a i n l e s s s t e e l .

4.4

Operating Procedures

Operating procedures were developed f o r each of t h e o p e r a t i o n s r e q u i r e d f o r t h e f u e l production. w r i t t e n b e f o r e t h e cold stressed.

rilll

w a s nade. )

25 s e p a r a t e

(These procedures were

B r e v i t y and conciseness were

Complete r e v i s i o n of' most of them was necessary as a r e s u l t

of t h e experience gained i n t h e c o l 6 r w .

Review and r e v i s i o n , on a

day-to-day basis, continued throughout t h e 233U production runs ; t h e minor equipment f a i l u r e s and malfunctions t h a t occurred durring t h e s e runs l e d t o e x t e n s i v e procedural changes t o ensure continued production

of a h i g h - q u a l i t y f u e l c o n c e n t r a t e . Tables 2 l i s t s t h e r u n s h e e t s thak were prepared

'The run with d e p l e t e d uranium provided f u l l - s c a l e t e s t i n g OP t h e chemical process, o p e r a t i o n a l procedures, and sf most of t h e equipment i n t h e absence of a p e n e t r a t i n g r a d i a t i o n f i e l d .

14.6 kg

(11.6 kg of '35U) p l u s 3.4 kg of LiP were charged produce 18.7 kg of LiF*W4 (73-27 mole '$) e u t e c t i c . 5

of cranium oxide t h e system t o

I n t h i s run,

5 1 Preoperatisna.1 A c t i v i t i e s The p e r i o d from September

15, 1967, through January 159 1968, w a s

devoted t o f a c i l i t y t e s t i n g ; process equipment f a b r i c a t i o n , i n s t a l l a t i o n ,

and testing; o p e r a t o r t r a i n i n g ; p r e p a r a t i o n o f procedures and manuals; and p r e p a r a t i o n of t h e process s a f e t y review, t h e c r i t i c a l i t y review, and t h e radiochemical p l a n t s a f e t y a n a l y s i s .

5.2

Mechanical Operations

The rm with d e p l e t e d uranium began January 15, 1968, with t h e loading of

cans i n t o c e l l G from t h e s h i e l d e d c a r r i e r . 2 3 8 ~filled ~ 3-

T & l e 2* L i s t of Rimsheets PrepareE f o r 233, F u e l S a l t Prcduction

Pa-ckaging of Lip. Renoving Empty F u e l Ca.rrier Prom Building 793C Penthouse Pedes5al Preparing and Tra.nsferring &pty F u e l Carrier from Building 7930 Penthouse t o Euibding 3C19 Penthouse. Preparing and T r a n s f e r r i n g of Loaded F u e l C a r r i e r from Building 3019 Penthouse t o Building 4930 Penthouse. Checkoilt of C e l l G. P r e p a r a t i o n of KOH Scrubber System. P r e p a r a t i o n o f I n e r t 2nd Reagent G a s System.

Pressme T e s t of H e l i u m Header. P r e s s u r e T e s t o f Iz, L%nifold. 2 Pressure Test of EF I h n i f o l d ( b e f o r e any run). P r e s s u r e T e s t of T - 1 an6 T-2 Systems. b e p a r a t i o r ? _ for Operattion:

Valve m d R o t m e t e r S e t t i n g s .

Discharge OY F u e l Cans f r o m Carrier t o Cell G. Capping F u e l Cans. Decanning and Charging F u e l to T-1. Charging EiP t o Reacticn Vessel. Tyansfer of Odd-Lot LiF t o C e l l G. Eut e c t ic Format i o n

HydroYluorination Reaction Progress.

HF T i t r a t i o n ( I n l e t ) . EF T i t r a t i o n ( O a t l e t ) . Sample Procedure. S a l t T r a n s f e r f r o m Reaction Vessel T-E t o T r a n s f e r Vessel T-2.

salt T r a n s f e r from T-2 t o T-3, Run Assembly)

NO.

P (3/4-in. Capsule

S a l t T r a n s f e r from T-2 t o T-3 ( P a r t i a l F i l l i n g of T - 3 ) . Replacing S a l t Vessel Assemblies ( T - 3 ) . Capsule D r i l l i n g and Weighing. Weighing and Removal of S a l t Shipping Vessels from C e l l G . T r a n s f e r o f S a l t Shipping Vessels t o TERE.

The UO

had been processed a t t h e Y-12 P l a n t , and t h e empty i n n e r and

o u t e r cans had been o b t a i n e d from t h e Savannah River Laboratcry.

The

cans had been f i l l e d w i t h t h e oxide and s e a l e d by a magnetic f o m i n g technique t o simulate t h e product cans t h a t would l a t e r b e used i n t h e prodaction runs.

The can opening box d i d n o t perform s a t i s f a c t o r i l y ;

t h e r e f o r e , it w a s removed f'rom t h e c e l l and e x t e n s i v e l y modified.

The

alignment tolerarices were relaxed, components were strengthened, addit i o n a l equipment w a s i n s t a l l e d to a i d i n t r a n s f e r r i n g t h e powder from t h e box, ~ n d t h e viewing c a p a b i l i t i e s were i n c r e a s e d . D i f f i c - d t y w a s encountered in t r a n s f e r r i n g t h e canning box to t h e r e a c t i o n v e s s e l .

LiF from t h e de-

The a v a i l a b l e v i b r a t i o n w a s i n -

adequate, and no p r o v i s i o n had been made t o sweep or "rod1't h e powder o u t and down through t h e powder a d d i t i o n l i n e .

The v i b r a t o r s had been

l o c a t e d on t h e equipment i n slwh a way t h a t most of' t h e i r f o r c e was imparted t o t h e f i x t u r e s and mechanism i n t h e box. sone damage t o t h e equlpmect.

This r e s u l t e d i n

Because of t h i s , t h e v i b r a t o r s were used

s p a r i n g l y and with cc.,ution.

5.3

Chemical Operations

Chemical o p e r a t i o n s began on January 24,

1968, with t h e s i n t e r i n g

o p e r a t i o n , which w a s cofiducted a t 9 0 째 C w i t h a helixm flow of 1 s t d

l i t e r / m i c through t h e bed.

The s i n t e r i n g t r e a t m e n t w a s i m e d i a t e l y

f'cliowed by t h e hydrogen r e d u c t i o n s-cep z t t h e s a m e temperature.

2 - 1 i t e r / m i n i ' i o w of gas, c o n s i s t i n g i n i t i a l l y of 0.1 l i t e r o f hydrogen and

1.9 L i t e r s of

h e l i u x p e r minute, Wac a t t a i n e d i n i t i a l l y .

D - e com-

p c s i t i o n of t h i s gas w a s adzusted p e r i o d i c a l l y u n t i l a flow of pure hydrogen w a s obtained.

Then t h e flow r a t e w a s i n c r e a s e d , i n increments,

t o 10 l i t e r s / m i n , where it was maintained f o r

hr.

During t h i s treat-

ment, ;he sintered-met21 off-gas f i l t e r became plugged.

Subsequent

examinatiosl of t h e f i l t e r u n i t r e v e a l e d t h e presence of' a h a r d f i l t e r cake.

Water vapor, which is evolved during t h e r e d u c t i o n process,

c c z l d h a w ccndensed on t h e f i l c e r i n t h e event t h a t t h e f i l t e r h e a t e r

w a s improperly operated; t h i s would have p e r m i t t e d t h e f i l t e r temperature k J

t o drop below t h e dew p o i n t of' t h e e f f l u e n t .

The cc?nversicn of' t h e oxide t o t h e f l u o r i d e began J a n u a r y

27, 1968.

Anhydrous hydrogen f l u o r i d e mixed with hydrogen ( 3 2 rneq of ID' p e r l i t e r of hydrogen) wzs i n j e c t e d through a d i p l i n e t o t h e botcom cf t h e UO,

bed a t t h e r a t e of 2.2 Eiters/nGn.

This r e a c t i o n began a t

WC;"C, and

t h e temperature was p e r i o d i c a l l y decreased t o m a i n t a i n t h e m e l t a t about 50째C above t h e l i q u i d u s t e m p e r a t m e .

'Be i n - c e l l t i t r a t i o n appa-

r a t u s w a s used t o monitor t h e El' i n t h e e f f l u e n t , b u t t h e r e s u l t s were i n c o n c l u s i v e ; t h u s a n o t h e r t i t r a t i o n u n i t t h a t p e r m i t t e d p r e c i s e addit i o n of t h e e q u i l i b r a t i n g r e a g e n t s from o u t s i d e t h e ce1.l w a s Ciesigned and i n s t a l l e d .

The d a t a obtained w i t h t h e new equipment showed t h a t

t h e u t i l i z a t i o n ot' HF w&s e s s e c t i a l l y zero (which i n d i c e t e d t h a t t h e conversion o f t h e oxide w a s complete) a f t e r

295 h r of h y d r o f l u o r i n a t i o n .

An attempt to sample t h e m e l t was u n s u c c e s s f u l because of the presence

cf' a h a r d t o p layer ( o r c r u s t )

F h n o i s e vas e v i d e n t from a l i s t e n i n g

rod i n s t a l l e d t o d e t e c t bubbling from t h e d i p l i n e .

It was concluded

t h a t t h e olip l i n e had broken, by corrosi.cn o r n e l t i n g , above t h e l i q u i d This v m l d account for t h e lack o f HF u t i l i z a t i o n and t h e

interface.

slow p r o g r e s s i n tke conversion of t h e oxide. the dip

Subsequent examination of

showed a l a r g e h o l e approximately at t h e I n k e r f a c e .

A new

d i p tube, along with a s e n s i t i v e sound d e t e c t o r , w a s i n s t a l l e d , and t h e

IT3 t r e a t m e n t w a s resumed. Bubbling i n t h e melt was e a s i l y d e t e c t e d ; and, f o r the f i r s t ; time, rea,sonEble valu.es f o r t h e KF u t i l i z a t i o n were obtalned.

A f t e r 250 hr of a d d i t i o n a l KF treatment, t h e d i p l i n e be-

erne plugged at a l o c a t i o n about

1-3/4 i n .

Yrom i t s open end.

examinatioc, t h e plug m a t e r i a l appeared t o b e uranium oxide.

Upon Four su5-

sequent lLnes plugged approximately a t t h e g a s - l i q u i d i n t e r f a c e w i t h i n t h e t u b e ; i n t h e s e i n s t a n c e s , t h e plug material also appeared t o b e uranium oxide.

It was obvious, then, t h a t e x c e s s i v e m o i s t - n e w a s belr-g

introduced i n t o t h e m e l t by t h e g a s e s used i n t h e p r o c e s s .

w a s s o l v e d by i n s t a l l i n g

"'his p r s b l e a

colurnn f i l l e d with magnesixn p e r c h l o r a t e i n

t h e helium system End by i n s t a l l i n g a c a t a l y t i c recombiner, a moleculars i e v e d r y i n g c o l m (with r e g e n e r a t i v e e a p c b i l i t i e s ) , and a m o i s t u r e a n a l y z e r i n the helium system.

The e f f l u e n t gases from t h e r e a c t i o n v e s s e l were d i r e c t e d t o a c a u s t i c scrubbing system, which c o n s l s t e d sf pclyethylene b o t t l e s f i l l e d with 2Q$ KQH s o l u t i o n and RaschLg r i n g s ( t o prevent c o l l a p s e ) .

A t an

e a r l y s t a g e i n t h e process, t h e d i p l i n e s i n t h e scrubber b o t t l e s plugged, and a white p r e c i p i t a t e appeared.

Frequent sparging t o promote

mixing, f r e q u e n t recharging of t h e c a u s t i c s o l u t i o n , r i n s i n g with h o t water, and a decrease (from 2076 t o lC$)

i n KOH c o n c e n t r a t i o n permitted

use of t h e system f o r t h e r e m i n d e r of t h e cold run.

It was f e l t t h a t

t h e Raschig r i n g s were a major c o n t r i b u t o r t o t h i s problem i n t h a t t h e y promoted s t r a t i f i c a t i o n of t h e s o l u t i o n ; t h i s w a s confirmed by t h e colored i n t e r f a c e t h a t appeared i n t h e b o t t l e s when phenolphthalein indicator w a s present.

At t h e conclusion of t h e cold rung t h e scrubber

system was completely r e p l a c e d by one t h a t contarlned s p a r e l i n e s and a

vacum breaker ( t o prevent p o s s i b l e b o t t l e c o l l a p s e )

and p e r m i t t e d

r e n o t e replaeernent and f l u s h i n g of a l l l i n e s . Although it gave s a t i s f a e t o r y r e s u l t s i n t h e s m e l l - s c a l e development

runs, t h e technique of measuring t h e Eiquidus temperature of t h e n e l t and subsequently determining, from t h e b i n a r y UF4-LiF phase diagran, t h e progress of' t h e conversion r e a c t i o n d i d not prove s u c c e s s f u l i n t h i s system.

The lieat c a p a c i t i e s and thermal i n s u l a t i o n of t h e system,

along with poorly l o c a t e d thermocouples, obscured t h e i n f l e c t i o n i n t h e temperat-are decay curve of t h e melt upon cooldown.

However, t h e KF

u t i l i z a t i o n data, along with r n a t e r i a l balences for t h e system, provided s u f f i c i e n t r e a c t i o n progress information.

When t h e r e a c t i o n was judged

t o be complete, .m m f i l t e r e d sample o f t'ne m e l t w a s withdrawn and enaIjrzed, chemically and p e t r o g r a p h i c a l l y ,

f o r oxide c o n t e n t .

The p u r i f i c a t i o n c f t h e melt, by t h e r e d u c t i o n of t h e m e t a l f l u o r i d e s t o metal, w a s conducted without i n c i d e n t .

T i t r a t i o n of t h e

E? i n

t h e e f f l u e n t gas proved t o be n r e l i a b l e means of determining t h e end p o i n t of t h i s r e a c t i o n .

F i l t e r e d and ; z n f i l t e r e d samples were t a k e n a t

t h e conclusion of t h e p u r i f i c a t i o n s t e p .

The f i l t e r e d samples were

considered t o be r e p r e s e n t a t i v e o f t h e packaged product s i n c e t h e melt

was f i l t e r e d i n t h e t r a n s f e r o p e r a t i o n .

as follows:

The cold

rru?

product analyzed

Concentration (Wt $)

61.0

0.02

0.C065

Fe C.007

c.26

Al 0.1

S 9.002

The product was filtered into the intermediate storage vessel; then it was transferred t o the capsules and shipping containers by subjecting the salt to e h e l i u ~overpressure of approximately l2 to

lg p s i g and forcing it out of the vessel through z dip line.

"kits in-

volved several operations because the capsules were, fiyst, Filled and-, then, replaced in the system by the sh-ipping can container assembly for c-. ,dIing. The compression-type tubing fittings used for this operation were very difficult to open after thermal cycling and after salt hadcontacted then.

(Also, it was difficudt to make up these fittings

properly and to obtain leak-kight joints, using the master-slave manlp-

ulators.)

'The approach to a s o l u t i o n of these difficulties consicted

of: (1) modificaticn of the intermedizte transfer vessel by addition of spare nozzles, (2) yeorientation of the vessel to ixprove accessibility,

( 3 ) use of redundant fittings when necessary,

(4)

use of a high-temperature thread lubricant on a l l fittings,

(5) modification of the operating procedure to reauce the nxmker of times fittings had to be opened, and

(6)

training operators in use of the manipulators on a simzlated piping arrangement.

In s m a r y , the cold run with depleted uranium was invaluable in that it:

(I) led to a process that was more simple to operate and that was corripatible with the equipment,

42 . ... -*-

(2) pointed out design and fabrication deficiencies in the equipment

( 3 ) provided on-the-job training for the operators and supporting personnel,

(4)

tested the operational procedures, showing the need of extensive changes in them, anti

(5)

showed that comprehensive remote maintenance procedures woxld probably be mandatory to ensure successful completion of the

2 3 3 ~fuel concentrate production runs

Three production batches, using the low-temperature flowsheet, were required in order to prepare

63.4 kg of the fuel-enriching

tTate, 7LiF-233UF,tmThis concentrate contained 39 kg of u r a n i m ~

concen-

(35.6

kg of 233U)m The first run began May 9, 1968, and the third run was completed July 30, 1968. The kg enrichment capsules were filled with a portion

the first-run product; the four 7-kg shipping containers

were filled with the remainder of the first-run product, all cf' the second-run product, and a portion of' the third-run product; the miscellaneous shipping container assembly was filled with the remainder

of the third-run product.

The ten salt shipping containers and the 45

enrichment capsules were delivered to the Molten Salt Reactor as required in the reactor enrichment schedule.

6.1 Peed Materials The 233U0

M NH:4OH (in 3 had been prepared in batches by using 7 -

excess) to precipitate hyCrcus uraniam oxide from solutions that con-

M in HNO tained 10 to k j g of uranium per liter and were 1 -

and NH NO

4 3' 1964

The uraniuni in the feed solution had been purified and isolated in

and

1965 by

solvent extraction fo%lswed by ion exchange.

These treat-

ments decreased the concentrations of plutonium, thorium, fission products, and corrosion products (iron, nickel, and chromium) to acceptably

bow levels.

Table 3 shows typical analyses of the oxide feed material.

Ta,ble

R u n No.

a Compositions cf Feeds f o r Preparing IGRE Fuel Salt

RU-33- 1

RU-33-2

RU-33- 3

Impurities, ppn

I s o t o p l c Analysis o f Uraraium, at.

233,

910 35

91 47 4

P3lCU

235, 236, 238u a

7.47 0.809 9.058

.. , ... ~~

v.:.,

...

7.4:

0.948 o .e701 0-245

0.Egl

Data furnished by manufac t w e r

Lifo

gn 46 0

7.46 0 * 816 0.059 0 -232

44 (99.97$

The LiF feed

had previously been densified to 1.2

3 g/cm by hydrogen treatment at elevzted temperatures

6.2 Radiation Levels of the Oxide Feed The high radiation levels of the oxide feed material ( s e e Tabhe

result from the daughter activity of the 232U (222 ppna) in the 233ue Alpha, beta, and g a m a rac?iation is emitted in the transitions (see Fig. 18)

From the shielding standpoint, the 2 . 6 - ~ eg~a m a radiation

fron the 2G8Tl and the 2.2-Mev g a m a radiation from the 212Ei are the most important. Table

4. Radiation Levels" of Storags Cans Containing Oxide Feed MaterialD

Purificaticn (months)

Distance f r o m Source 1 ft 1m a0 f t

20 ft

1.1

13.120

250

0 120

300

0.200

0.028

a Measured with a paper shell cutie p i e . 'Each can contained 4-50 g of 233,

6.3

Oxide Feed ?.laterialHandling

233U0 had been packaged In double-walled alminum containers, 3 containing approximately 4-50g s f uranium. The cans, 2.8 in. OD by 8 in. 'Fhe

lowj

had been sealed on one end by welding, and on the other end by a

magnetic f o m i n g technique.

They had been stored in Building

3019 at

QRNl TO

prepare the 2 ' ~f u ~e l concatrate, we removed 89 cans from the

factlity and transported them, in s i x loads, to the TURF in a shielded carrier.

The carrier was positicned on a pedestal atop cell G for

unloading the cans i n t o the cell.

Nuclide pp2-

Fig;. be.

Decay Chain and Gamma A c t i v i t y in 3 0 -"33U9 Fuels. 2 2

46 NQ spread of contamination or e x c e s s i v e r a d i a t i o n exposure t o personnel occurred during t h e removal of t h e oxide cans from t h e s t o r a g e f a c i l i t y , during t h e i r t r a n s f e r t o TURF, or d u r i n g t h e i r d i s c h a r g e from t h e c a r r i e r to c e l l G . I n c e l l G, t h e cans were gaged, and any b u r s or excess w e l d m e t a l were removed by f i l i n g .

Three s e p a r a t e o p e r a t i o n s were r e q u i r e d t o

e l o n g a t e t h e cans t o the 9-L/2-ine l e n g t h r e q u i r e d f o r proper o p e r a t i o n of t h e can opening box. " t r u e " them.

F i r s t , t h e cans were machined on one end tc

A premachined end cap (with epoxy cement a p p l i e d ) was

i n s e r t e d i n t o t h e c e l l through t h e s m a l l - i t e m s e n t r y p o r t .

This cap

w a s i n s t a l l e d on t h e can i n a p r e s s i n g f i x t u r e , and t h e n t h e can (with cap) w a s placed i n a c u r i n g f i x t u r e , where f i v e cans a t a time were c - x e d m d e r l o n g i t u d i n a l p r e s s u r e for 1 h r a t a temperatxre of 110 t o 120째C.

m e can p r e p a r a t i o n equipment functioned s a t i s f a c t o r i l y , except

on one occasion i n which t h e d r i v e motor on t h e can machining f i x t u r e burned o u t .

The remaining cans for t h a t run were d r e s s e d with a f i l e ,

and t h e caps were i n s t a l l e d without i n c i d e n t .

Later, a new motor was

i n s t a l l e d remotely i n t h e f i x t u r e . The elongated cans of oxide were opened, one at a time, i n t h e decanning s t a t i m .

This w a s a time-consuming o p e r a t i o n involving t k e

zlse of equipment t k a t had been reccgnized d a r i n g t h e c o l d run t o be The decanner had a rugged chuck assembly t h a t h e l d and

mzrginal.

1-0-

t a t e d t h e cans while a c u t t i n g wheel opened them i n s i d e an a l p h a - s e a l e d box.

Most of t h e o t h e r attachments i n t h e box were o f l i t t l e velue,

and i n some i n s t a n c e s , a c t u a l l y hindered t h e o p e r a t i o n . The major p r o b l e m i n t h e decanning o p e r a t i o n can be sumarized

as follows:

(1) Alignment and c l e a r a n c e t o l e r a n c e s were tco c l o s e for h o t - c e l l operation.

(2) V i s i b i l i t y i n t h e decanning box was l i m i t e d .

( 3 ) The powder f a i l e d to flow out of t h e box e a s i l y .

(4) A

vibrator shaft seal failed, leading to loss of o x M e powder

from the box.

This caused rather extensive contaminaticn of

the cell. Modifications were made remotely during the rue1 concentra-be production to increase visibility, repaIr the seal, and to pro.vide tools inside the decanner to asslist In transferring the pow3er to the reaction vessel.

6.4 Reduction of Uranium Oxide The expanded bed of 233U0 was heated for 2 hr at 550째C in a

helium atmosphere to remove, by pyrolysis, any traces of ammonium com-

pounds or other volatiles remaining from the chemical processing. The bed was then ccoled to 4 0 0 째 C before kydrogen treatment

started.

waE

This temperature was sufficiently low to accommodate tke

temperatwe rise expected from the exothermic reaction of hydrogen with

uo3 +

- uo

-+ H2o +

72,000 cal/g-mole.

YE? concentration of hydrogen (in helium) was adjusted initially tc 5 vol $ an6 was gradually increased to 50 vo% during the Yirst 4 hr $J

of treatment.

The temperatures within the bed were monitored by En

internal probe with 12 thermocouples that were placed at 2-in. intervale along the vertical axis of the bed.

These temperatures rose in response

to an increase in hydrogen concentration and then became constsnt after

the initial excursion. The procedure of incrementally increasing the hydrogen concentration was repeated until the hydrogen:heli-mvolume ratio was 1:l; the gaseous flow rate was 2 liters/min. The location of the reaction zone and the zone movement inside the bed were clearly defined by the temperature profile.

As the

reaction progressed, the reaction zone rose, in the form of a band, up through the powder bed. Figures 19 and 20 show plots of the temperature at

16 in., respectively, from the bottom of the

24-in.-high

mznium rectuction phase of the three production runs.

6 in. and bed during the

The rise in the

8 CQ

i i E I

I [

E i

I i

temperature of t h e lower zone during t h e f i r s t 8 hr of t r e a t m e n t i s due t o t h e exothermic r e a c t i o n ( t h e reactiora vessel furnace w a s s e t t o conA f t e r t h e temperature excursion r e s u l t i n g from t h e

t r o l at hUO'C).

i n i t i a l i n c r e a s e s i n hydrogen flow had subsided (approxirnately 1 2 h r ) , t h e temperature cf t h e furnace was increased, a t t h e - a t e of 30"C/hr, u n t i l t h e bed temperat-me w e s

525

The r e d u c t i o n o p e r a t i o n w a s

k 25°C.

continued a t t h i s temperature, with

vol

4s hydrogec--50

VOL

$ helium,

u n t i l 50 t o lo05 excess over t h e s t o i c h i o m e t r i c amount o f hydrogen had

keen passed through t h e bed. Hydrogen u t i l i z a t i o n w i t h i n t h e bed w a s 100% u n t i l t h e r e a c t i o n

zone approached the top of t h e powder bed; t h e n a s l i g h t d e c r e a s e w a s Hydrogen usage was determined by a materirtl balznce of t h e

observed.

gas flowing i ~ t ot h e r e a c t i o n vessel, as measured by rotameters, t n e gas 0v.6uf10wg as measured by t h e i n - c e l l wet t e s t

6.5

MydrofEuorination

and

meter.

uo2

Upon coqLLetion of' $he oxi6e r e d u c t i o n s t e p , t h e bed was allowed t o e001 t o 400°C.

The conversion of UO

2 t o UF 4 by h y d r o f l u o r i n a t i o n , using IF gas d i l u t e d wZth hycrogen, began a t 400°C and w a s corrpleted a t 6 2 5 " ~ . F i v e t o seven days were r e q u i r e d for t h e conversion. The EF gas wzs s u p p l i e d t o t h e process by withdrawing it from t h e vapor space or a. h e a t e d 100-lb IF cylinwer. t h e m o s t e t i c a l l y c o n t r o l l e d t o provide

The c y l i n d e r h e a t e r was

vapor p r e s s u r e t o 12 t o 1 4 p s i g .

A d i f f e r e n t i a l - p r e s s u r e t r a n s m i t t e r across a c a p i l l a r y r e s t r i c t o r i n

the

HF gas supply l i n e w a s used t o monitor t h e flow. 'The gas was passed

through

maze of t i g h t l y packed n i c k e l wire i n a 2-in.-diam n i c k e l tube

t h a t w a s maintained a t

625"~t o

r e ~ o ws u l f u r from t h e stream.

It vas

t h e n x i x e d wit'n e xetel-ed amount of dry hydrogen, f i l t e r e d , and i n t r o duced t o t h e r e a c t i o n v e s s e l through a d i p tube t h a t extended t o t h e bottom of t h e UO

bed.

A t t h e beginning of' t h e h y d r o f l u o r i n a t i o n s t e p , t h e composition of

95 voE $ hydrogen--5 v o l $ KF; t h e flow r a t e of t h e mixture w a s 2 s t d l i t e r s / m i n . Over e p e r i o d of 3 t o 4 hr, t h e €IF c o n c e n t r a t i o n t h e gas w a s

w a s incrementally increase5 t o

40 v e l $

caused ;he bed t e m p e r a t m e t o r;se

as t h e exssherrric r e a c t i o n

from

i n i t i a l kours, t h e temperature w i t h i n t h e bed

450°C.

During t h e s e

W ~ E constantly

monitcred

t o determtne when t h e temperature excursion r e s u r t i n g from e s c h €E f l o w adjustment had ceased and when a n o t h e r adjustment could be made A f t e r the

vol

reached

%Ip

c o n c e n t r a t i o n of t h e h y 6 r O f l u o r i m t i n g mixture had

$ j

t h e r e e c t i c n zone tr,n,veled., i n t h e form of' a band,

up throtbgh %he bed ( i n a mnnner s i m i l a r to t h a t observed d u r i n g t h e hydrogen r e d u c t i o n ) 8,s t h e UO w a s converted %c T J F 2 4=

UQ2

-t

4I.F

The r e a . c t i o n

-+ 2Hg0 -k 144,COC cal/g-mcle

i s a c r e exothermic t h a n t h e r e d u c t i c n r e a c t i o n , b u t E t does n o t ha,ve as g r e a t a tendency t o cause t h e m a 1 excursions.

Probably, this I s t h e

r e s u l t of d i f ' f e r e i c e s between U03, U02? and UF4 w i t h r e s p e c t t o bed p e m e a b i l l t y end thermal p r o p e r t i e s

!The r e a c t i o n - zone temperatures

f o r the t h r e e production runs are p l o t t e d as a f u a c t i o n of t i m e i n F i g . PIo In runs E and 2, s e v e r e 1 f u r n a c e temperature adjustments were mtde during t h e f i r s t f i v e days of treatment in an e f f o r t t o i i i c r e e s e the bed temperature to

475-500°C (because

t o n l c k e l a t t h e h i g h e r tempera.ture).

t h e KF gas i s l e s s ~ o r r o s ! ~ v e

Ira run 3, t h e fmxnace operateC

s a t i s f a c t o r i l y and d i d not r e q u i r e adjustment.

The progress of t h e r e a c t i o n was followed by observing t h e r e a c t i o n zone t r a v e l through t h e bed and a l s o by o b t a i n i n g a material balbnce of

in t h e system.

the

P-e

ET' u t i l i z a t i o n wag e s s e n t i a l l y lOO$ fcr the

f i r s t f i v e dsys and t h e n decreased s h a r p l y as t h e r e a c t i o n zone reached t h e t o p cf t h e bed.

'Then t h e te-nperature o f t h e bed w a s i n c r e a s e d to

625"C, where i t w a s heEd f o r two days t o emure completeness of' t h e reaction.

The €IF u t i l i z a t i o n d i d n o t i c c r e e s e a t t h e h i g h e r temperature;

i n s t e a d , it continued t o decrease, s u g g e s t i n g t h a t t h e r e e e t i s n had been complete a t t h e end o f t k e f i f t h day cf h y d r o f l u o r i n a t i o n . A t o t a l of

13.5 kg of uranium, as UO,,c w a s converted t o UFIC i n

each of t h e three r u n s ; o n l y v e r y minor d i f y e r e n c e s i n t h e runs were noted.

686

660 640

620

600

RUN no. 2 - - -

580

RUN no. I

566

RUM no. 3

-P---

5 48

520

500

480 460 446

420

400

380 8

120

96 TIME

144

968

192

(hFS)

Ffg. 21. b.lax5m11~Terriperature Within Powder Bed D x i n g Hydrofluorination of UO,. L

6.6

oma at ion of t h e E u t e c t i c S a l t

The e u t e c t i c mixtwe U F , EiF

(27-73mole $I) (Pig.

22) w a s formed

by adding t h e s t o i c h o i n e t r i c q u a n t i t y of l i t h f m f l u o r F d e rjowd-er t o t h e w a n i u m t e t r a f l u o r f d e powder and f u s i n g t h e mixture

Dry EiF powder w a s a?;,ded t o t h e r e a c t i o n v e s s e l by t h e fcllowing s e r i e s of o p e r a t i o n s :

(1) It was poured -into a hopper l o c a t e d on t o p

of t h e decanning s t a t i o n ,

(2) it w a s dumped from t h e hopper i n t c the

decanner box, and ( 3 ) i6, was t r a n s f e r r e d from t h e box t o +,he vessel. by v i b r a t i o n and brushing. The temFe3-ztw-e o f t h e r e a c t i o n v e s s e l conta,ining t h e e t r a t i f i e d

LT4 end LiF powders was then increased t o 855째C i n order t o melt t h e The melt w a s d i g e s t e d a t c h i s temperai i t h i m f l u o r i d e (xp, 835째C). ture for

h r vhiLe it wads sparged with hydrogen ( a t a f l o w r a t e of C e 2

Piter/rr,in) t o reduce m y extraneous compounds t h a t might kave been introduced d w i n g ;he L i F a d d i t i o n . A sound d e t e c t o r w a s a t t a c h e d t o t h e r e a c t i o n v e s s e l d i p l i n e t o

sense t h e bubbling of t h e hydrogen sparge t h a t would occ1.x i n t h e presence of'

l i q u i d i n t h e bottom of t h e r e a c t i o n v e s s e l .

'This was

an e x c e l l e n t device for determizing when t h e rneltciow~ihad s t a r t e d .

The

i n t e r m 1 thermocouple probe confirmed t h a t , a t meltdown, a very wide rnnge 07 temperatures e x i s t e d along t h e axiz of t h e I c e l t @ A ragiE.

cooldown t o 65C"C w a s observed i n t h e lower regrion of t h e v e s s e l where liquid existed.

As; t h e sane time, temperatures as high as

859째C were

measured i n t h e upper regions of t h e vessel where Fusing of t h e compounds had 2ot y e t taken p l a c e .

A s more l i q u i d w a s formed, a g r a d u a l

s h i i ' t I n t h e temperature pro-f'ile occurred, i n d i c a t i n g a r i s i n g Liquld l e v e l i n the vessel.

The ternperatwe of t h e p o o l e v e n t u a l l y reached

850째C~ t h e s e t p o i n t of t h e furnace t e m p e r a t m e c o n t r o l l e r .

m e initial

presence of ?Ae l i q u i d and t h e r i s i n g l e v e l were also i n d i c a t e d by changes i n t h e d i p l i n e p r e s s m e as t h e back p r e s s u r e on t h i s l i n e i n c r e a s e d t o overcome t h e r i s i n g l i q u i d l e v e l . Diff'erences, with regard to cofiditions during i n i t i a l mcltdowc, were noted rn t h e rms,

I n rsv1s I and 3, t h e T J F

4 and

LiF had t c be

ORNL-LW-DWG

hi F

UF4 (mole To)

F i g - 22

LIF-UF

4 â&#x201A;Ź?lase Diagram.

47457.4

55 850°C:b e f o r e

heated, t o about

melting occurred.

I n rim 2, i n i t i a l

melting occurred a t 6 5 ~ " C , n e a r l y 200°C below t h e x e l t i n g point 07 t h e

The low-temperature i n i t i a l melting must have r e s v l t e d

Lithim fluoride.

from +,he presence O C a s i z a b l e h e e l of s a l t (mpj 4 9 0 ° C )

i n t h e r e a c t i o n v e s s e l from run E.

"seed" to p e r n i t f u s i n g of t h e W

t h a t remained

Probably, t h i s h e e l a c t e d as

4 and LiF

powders a t t h e lower tempera-

'ewes

The g-in.-deep pool of e u t e c t i c s n l t (mp, 4 9 ° C ) w a s next t r e a t e d wlth 20 v01

HF--80 v o l sf0 hydroger ( f l o v r s t e , 2.4 l i t e r s / m i n ) f o r 2k

h r a t a t e m p e r a t m e of 700°C t o remove the l a s t t r e c e s of oxide From A t t h e conclu-

t h e s a l t p r i o r t o t h e hydrogen p u r l f i e a t i o n procedure.

s i o n of t h i s treatment, an m f i l t e r e d - s ~ x p l eof' t h e salt; and analyzed f o r oxide content

cup was immersed i n

eh,"

WE?

withcirawn

(A 1/25i n -OB x 2- E/4- i n * -long n i c k e l e

s a l t t o withCi3"m a 25-g sample.)

After t h e

sample had s o l i d i f i e d : a l-in--longs e c t i o n w a s c u t from t h e c e i t e r 3 r d analyzed p e t r o g r a p h i c a l l y and chemically for i,he presence o f UO remaining p o r t i o n of the sample was submitted for analysis

The

corcplete chemical

Kydrcger- treatment of t h e s a l t w a s s t a r t e d p r i o r t o o b t a i n i n g t h e r e s - d l t s of t h e a n a l y s e s

The more r a p i d l y ~ b t t ~ i n epde t r o g r a p h i c r e s - d t s

were =sed t o determine whether h y d r o f l u o r i n a t i o n should be resumed o r whether hydrogen p u r i P i c a t i o n of t h e melt should be continued.

each

of t h e t h r e e runsg t h e UO content w a s r e p o r t e d to be l e s s t h a n t h e 2 lower limit of accuracy (200 ppm) €or t h e p e t r o g r a p h i c a p p r a i s a l ; t'n-~s,

subsequent HF t r e a t m e n t w a s unnecessary.

Chemical analyzes o f t h e sane

samples showed oxide c o n t e n t s ( i n t h e product s a l t s ) of

62, 34, and 32

ppm f o r rans P, 2? and 3 r e s p e c t i v e l y .

P u r i f i c a t i o n of t h e E u t e c t i c S a l t

6.7

The e u t e c t i c s a l t w a s p u r i f i e d by bubbling pure hydrogen gas

( 3 t o 10 ppm H,O),

at a flow r a t e of 2 s t d l i t e r s / m i n ,

through t h e

10-in.-deep m e l t . r e a c t ion, -t-

l/2 Hg

The temperature of t h e molten s a l t during t h l s

KF c M,'

is 700째C. 'The progress of the reaction was followed by titrating the effluent gas with the in-cell titration assembly. plotted in Fig. 2 3 *

These data are

"he high rates observed initially can be attributed

to the evolution of the soluble KF in the melt.

""ne first inflection

and plateau of each curve correspond to the reduction of the nickel fluoride; t h i s is folEowed by a second inflection and platex,, which represent the reduction of the iron fluoride. The end point of the purification was evident from the leveling off of the HF evolution r a t e at 0.025 meq per liter of hydrogen. The hydrogen flow rate was increased on several occasions during the process, an6 the reaction rete seemed to be almost Lndependent of the hydrogen concentration. The effect cf the hydrogen treatment on the concentration of the

corrosion products is shown in Table 5 .

The chromium concectration in

the melt was n o t affected by the hydrogen treatrrent.

Highey i n i t i p - 1

values of nickel in the thk-6 rung and of" iron in the second znd third rms, were the r e s x l t of residual lnateriab left i a r the bottom of the

reac-b-ionvessel from previous runs. Apparently, the metals had precipitated and thus hzd not been filtered eut during the transfer operetion. The levels to which the iron and nickel concentrations were lowered

by the hydrogel? reduction of the metal fluorides ere believed to be near the linit of accuracy of ?he sampling eysten; and the laboratory analyses.

The act;mb concentrations of' these impurities in the en-

richi9g concentrate, as delivered to the IfSRE, should be somewhat lower tian the values reported because an additional

24 hr

of hydrogen treat-

ment; was provided in each run after the filtered samples were withdram for analysis.

Table

to the 1LZSF.E; Table

6 gives

7 gives

the chemical analyses of the fuel shipments

the isotcpic analysis of the uranium.

During each of the three runs, the reaction vessel was exposed f o r

2C days to 40 vel

% HT--6C

vo1

$ hydrogen at temperatures ranging fron

4-00to 850째C. Approximately 5 g o f nickel (from the Kickel liner of

the reaction vessel) was lost to each melt.

mis

corresponds to z

uniform corrosion rate of slightly less than 0.001 in./yes,r - a low

r ~ t efor this type of process.

0.18

0.16

0.84

RUN

no.

I -

RUN

no.

2 --

RUM

no.

3 -----

0.86 0.04

0.02

---e ----

-----

--------_____

120

144

6.00

96 TIME

(ha)

168

192

216

Table

Type of Sample

Concentrations

Nickel (4> Run 2

Corrosian

Products

the

fitectic

Salt,

IrOll

@> Run 2

ChI-OTllil.,lXl W Run 2

wnfiltered.: Before

W2 Treatment

o.olgl

0.0038 0.430

0.0295 0.07yl

0.0066

0.0050 0.0160

0.0051

0.0750

0.0072 o.oc56 0.0040

Filtered: After

W2 Treatment

c.0115 0.0145

0.005~

01.Q065 0.0045

Table

ti Element

Analyses"

Cans B, C, D, a.nd E Chemical Spectrographic Anal-sis

of the

233, 4-7LiF

Ckremical Analysis

(27-63

mole

Capsules (45) Spectrographic Analysis

$) Fuel

Concentrate cam F, B, J, L, w, P Chemical Spectrographic Anal sis Analysis

Al. A

< 0.01

< 0.004

CC?

< 0.033

< 0.021

< 0.038

0 .ooy

< o.oce

c.0055

< 0.002

0.0045

< 0.01

0.0104

0 d-7

0.0051.

< 0.004

0.0145

< 0.09

CU Fe cd.

< 0.003

< 0.002

Li Mxl

4.83 < o.oco4

4.91 < o.coo4

< 0.004

0.0082

< 0.04

42 ppm

O2 l-b

0 -0066 52 ppm

< 0.030

EL-

< 0.002

< o.oc\lc 4.8

0.01.63

< 0.09

32 xv

< c.038

< 0.010

si S

< 20 ppm

< 0.007

< 0.004

< 0.032

< 0.002

c 0.002

< '3 .ow

< 0.008

Sn Ti V zn u aIn

64.38 wt $ unnless

given

61.8 in ppm.

63 m1.9

7 . I s o t o p l c Analysis of Uranium i n MSRE

Table

Fuel Concentrate

Capsules

(45)

Cans

91 378 7.463

91* 466 7.466

0.874

0 810

o .065

0.0585 0.196

0.218

4 300

Tot21 uranium, kg Average a t

6 583

28.ogg

233 103

T o t a l uranium, w t

6.8 Trarisfer of' t h e E u t e c t i c Salt Eight t r a n s f e r s p e r s t i s n s were necessary t o convey t h e t h r e e

13.5-kg batches o f e u t e c t i c ~ a l rnixture t from t h e reackion v e s s e l t o t h e l c t e m i e d i a t e t r a n s f e r v e s s e l and then to t h e v a r i o u s shipping cont a i n e r assemblies. p r e s s u r e cver

The t r a n z f e r s were made by applying helium gas

pool o f lraoitea salt having a temperature sf 6GO"C.

The

s a l t w a s f o r c e d out of t h e d i p l i n e and thrcugh t h e t r a n s f e r Line a d

s a l t f i l t e r t c t h e r e c e i v i n g v e s s e l , vhich was vented.

The t r a n s f e r

l i n e s were heated with t u b u l a r r e s i s t a n c e h e a t i n g elements, i n s u l a t e d t6

conserve h e a t acd avorEd c o l d s p o t s , and equipped with t h e m - o c o q l e s .

13.4 kg o f (4.7 l i t e r s o f s a l t ) Sn t h e production batches t o 4.3 kg of ua-aniLun (1.5 l i t e r s of s a l t ) t h a t was reqGired t o f i l l the 45 enrichment capsule array.

m e t r a n s f e r s ranged i n s i z e from t h e

T a - a r , i u m

"?he primary t r a n s f e r bine ( 3 / 8 - i n . - o ~ x 0.065-in. nickel tubing)

wall type 200

which connected t h e r e a c t i a n v e s s e l t o t h e b=-in.-diam

storage v e s s e l , a l s o served as t h e treatment gas supply l i n e t o t h e Uip

tube i n the reaction vessel.

During t h e processing c p e r a t i o n s , t h i s

l i n e w a s ccnnected t o t h e t r e a t a e n t gas supply l i n e i n s t e a d of t h e transfer vessel.

I n each of t h e feed b a t c h t r m s f e r s J a compression-

type f ' i t t i n g had to be broken and t h e t r a n s f e r Line had t c be zonnected to

new salt f i l t e r t h a t had p r e v i o u s l y been i n s t a l l e d i n a nozzle

a t o p t h e s5orage v e s s e l .

'&e s l r t e r e d n i c k e l f i l t e r was 3 i n , i n

diameter, and the pore s i z e

WES

20 p .

Transfers t h r o q h t h i s l i n e re-

quired an overpressure of E5 p s i g t o overcome t h e s t a t i c head (18 f t

H,O)

and the r e s t r i c t i o n t o flow o f t h e f i l t e r .

plete t h e t r a n s f e r v a r f e ? ~ r o m78 t o 140 m i n .

Time r e q d i r e d t o comI n i t i a l movement o f t h e

salt through t h e l i n e was obvious from t h e r a p i d response of t h e a t t e c h e d t h e ~ ~ ~ o ~ o t~o pthe l e ss a l t temperat-=e.

The progress of t h e t r a n s f e r

w a s followed by observing t h e r l s i c g back p r e s s u r e ec t h e h e l i m purge

t o the storage vessel dip l i n e ; t h i s indicated a r i s i n g liquid l e v e l .

The rrrsh of gas through t h e l i n e a t t h e end of t h e t r a n s f e r w a s s u d - i b l e from t h e sound d e t e c t o r .

These c o n d i t i o n s were v e r i f i e d by a s h a r p

drop i n t h e r e a c t i o n v e s s e l p r e s s u r e and a r a p i d i n c r e a s e i n gas flow through t h e s a l t t r a n s f e r l i n e . Five t r a n s f e r s were reqdired t o f i l l t h e three-pro6xct c o n t a i n e r assemblies.

They were made v i a a l/h-in.-OD

n i c k e l t r a n s f e r Pine th2-t

connected t h e assembly t o a d i p l i n e i n t h e s t o r a g e v e s s e l . f i l t e r s were not Tnvolved

ilz

Since

t h e s e t r a n s f e r s , t h e t r a r s f e r s were com-

p l e t e d i n approximately 10 m i n .

a"nermccsup1es cn t h e krransfer line and

on t h e shipping c o n t a i n e r s i n d i c a t e d t h e movement o f s a l t .

An c v e r f l s w

pot a t t h e end of t h e c o n t a i n e r s ( i n s e r i e s ) w a s equipped with Liqrrid l e v e l d e t e c t i o n probes and i n t e r n a l thermocouples t o i n d i c a t e t h e presence of s a l t .

A blowbsck of gas t h e n e n s - x e d t h a t t h e c o n t a i n e r s were

f i l l e d t o t h e proper l e v e l .

The t r a n s f e r o p e r a t i o n s were conducted a t a s a l t temperature o f 600째C.

(This temperature had been a r b i t r a r i l y s e l e c t e d , and t h e

COP-

t a i n e r s had been f a b r i c a t e d t o c o n t a i n t h e d e s i r e d q u a n t i t y of f u e l a t t h i s temperature. )

The filled c o n t a i n e r s were allowed t o cocl, and t h e

salt w a s allowed t o s o l i d i f y b e f o r e t h e disassembly o p e r a t i c n began.

62 6.9

Container Disassembly and Preparation for Shipment

The shipping container assemblies were stripped of the themocouples, overflow pots, heaters, and suppcrting harcware.

The containers

were separated from each other by cutting the interconnectiag tubing. The 45 enriching capsules were clipped and trimmed, were tested (i.e-, their lifting b a i l s were tested) with a l 5 - l b pull, were drilled

for drainfng aad venting, and were identified and weighed.

Then they

were packaged, in groups of six, in carrousel shipping containers.

The

equipment, whlch was designed to do these operations remotely, fumtioned satisfactorily. The 2-1/2-in.-diam product cans were easi%jr removed from the filling

arrays; however, removal of the top and bottcm plugs from each can was quite difficult. An inordinate amount of' force was necessary to break the bottom plug loose tram the thin salt film that had formed in the annulus between the plug and the bottom nozzle.

Several fixtures Ce-

signed for this task proved to be inedequate and had to be replaced with stcrdier units.

A liPting bail. was installed on each can?. A l s ~ , a

stopper was inserted in the bcktorn of the can to rriinimize the loss of salt dwirig handling and shipment. The cans were weighed by using a beam balance that was located in a glove box mounted cn top of the processing sell. '%he glove box became a part ef the cell containment for this operation. A long cable, with the lifting b a i l of the can attached, was sTJspended from the balance into the cell.

The gross weight of the cans ranged from

le6

to 15 kg. ALL of the shipping containers were t h e 3 stored in cell G to await

shipment tc the XSRE.

6.1~Transfer of 7LiF-233W4 Salt Product to the

MSRE

Six of the 2-%/2-in -diarn product salt containers (total uranium a

content,

33 kg) were delivered, iidividually, to

t h e MSRE In the E9-tan

fi-AB carrier. ?"ne Pu-A1 carrier wes slightly modified Per this operation.

The three-barrel magazine was removed, and a winch-and-cable

assembly w a s i n s t a l l e d on top of t h e c a r r i e r i n a. s e a l e d kousing so t h a t it S e c m e a p a r t of t h e c a r r i e r containTrect. The c a r r l e r w a s placed on t o p ot' t h e p e d e s t a l over a 6-in0-diam

p o r t t o c e l l G, and b e e m e a p a r t of t h e c e l l containment when t h e

s l i d e drawers i n botk t h e c a r r i e r and t h e p e d e s t a l were opened.

c a b l e hook w a s lowered i n t o t h e c e l l t o r e c e i v e t h e product can and t h e n r a i s e 2 t o withdraw the can from t h e c e l l i n t o t h e c a r r i e r .

The

p e d e s t a l drawer and the c e r r i e r drawer were closed, i s o l a t i n g t h e c a r r i e r arid cell from each o t h e r and from t h e a m l e n t atxosphere. manner, containment of' t h e fuel was malntained a t a.lb t i m e s .

In t h i s Tk-e c a r -

r i e r w a s t h e n rerm.,oved from t h e p e d e s t a l , s e z l e d by t h e i n s t a l l a t i o r o f t h e cover p l a t e s , and cleaned of any s u r f a c e contaEination. The f u e l c a r r i e r w a s t h e n t r a n s p o r t e d t o t h e PISRE, where it w&s p o s i t i o n e d over a t u r n t a b l e ( F i g . 24) t h a t 'was designed for charging t h e e n r i c h i n g concentrate t o t h e r e a c t o r f u e l d r a i n t a n k . Neasurements, a t t h e sm-face of t h e %-A1

c a r r i e r , of t h e r a d i a t i c n

emit5ed by one 7-kg i r a n i w f u e l ca.n are given i n T3bHe 8.

a.re produced by

(a,?) r e a x t i o m

The neutrons

on l i t h i u m and f l u o r i n e (of t h e e c t e e t i c )

by the high-energy alpha p a r t i c l e s emitted by s e v e r a l of the daughters o f t h e 23ZU The enrichment capsules were shipped t c the IGRE i n a smxller c a r r i e y t h a t was designee. t o accommodate s i x c2psules i n a c a r r o u s e l

fixture,

"he c a r r o u s e l served as a support f i x t u r e d u r i n g t r a n s p o r t

and as a h o l d e r f o r s i x bottom plug assemblies t h a t became a, p a r t of t h e sampler

e n r i c h e r system a t t h e WWE as t h e capsules were removed

â&#x201A;Ź r o m t h e c a r r i e r through a l-l/2-ine-dLam h o l e Ln t h e top. A small glove box w a s f a b r i c a t e d f o r use i n removing t h e c a r r o u s e l

assenbliee from c e l l G .

This box w a s mounted on t o p of t h e snall car-

r i e r , whichg i n t u r n , was mounted on t h e p e d e s t a l above t h e c e l l .

Then

t h e p e d e s t a l s l i d e - v a l v e drawer w a s opened, and the glove box and t h e c a r r i e r became a part of t h e cell containment.

A c a b l e from a winch

i n s i d e t h e box w a s Powered i n t o t h e cell t o r e c e i v e t h e c a r r o u s e l .

The

c a r r o w e l was withdrawn i n t o t h e c a r r i e r , t h e p e d e s t a l Crawer was closed,

ORNL-DWS 68-367

TURF CARRIER

GRAPHITE SAMPLING

--EXHAUST

Fig.

Tar&

24*

BLO'WER

Arrangement for Adding 233U Enriching Salt to Fuel Drain

Table

8. Radiation Levels, Measured at Surface of 7LiF.-*%TFk

Instr-mext Location Along Vertical *Axis of Carrier

Fuel containing

Type of Radiationa

12 in. below top of carrier

7 kg

Pu-A1 Carrier, of

of iTrenim

Radiation Level (m-em/hr) at Specified Distances frorx Cerrier Surface 0 12 in. 5 f't

ITm

'int

2'00

Center of c a r r i e r

MT Nint

o 6 75

75 0.3

c: 3 c

7.5

Gama d

18 in. zbove

bottom of

NTJ Nint = Neutron radiation (fast, thermal, and intermediate)

and then the carrier was removed from the pedestal and placed on i t s base.

The glove box was removed from the carrier, and s h i e l d plugs

were inserted in the 1/2-in.-diam and 1-1/2-in.-diam access openings in the top of the carrier. The carrier contaEned a 5-in.-dim cavity

with

4 in. of

lead shielding around it.

When the m a l l carrier housed s i x capsules, each containing 96

of' uranium in approximately 150 g of fuel concentrate, the gamma radiation level was 200 mrem/hr at the surface and decreased to 2C mrem/hr

6 ft.

The neutron radiation levels at the surface and at

6 ft were

105 mrem/hr and 10 msem/hr, respectively; -measurement made at the open

66 bettom of t h e c a r r i e r during removal from t h e p e d e s t a l i n d i c a t e d s: r a d i a t i o n l e v e l of 50,000 mremlhr The removal of t h e f u e l From c e l l G and i t s su5sequent t r a n s f e r t o t h e MSRE were c h a r a c t e r i z e d by very bow r a 2 i a t i o n exposmes t o personnel snd e s s e n t i s l l y no spread o f contamination.

In f a c t , o n l y

t h e t o p surface of t h e p e d e s t a l and a s m a l l a r e a immediately a d j a c e n t t o it had t o be deconte,minateZ.

A t o t a l of 39-72 kg o f uranium, in t h e form of uranivzq oxide powder, w a s t r a n s r e x - e d t o c e l l G o f t h e TURF. 0 :

u r a n i m , as EiP-W4,

O f thLs amcmt, 38.95 kg

w a s packaged as t h e f i n i s h e d p r o d - x t .

The can-opening o p e r a t i o n accounted f o r e l o s s o f

as = x a n i u m oxide.

245

of uranium

Most or' t h i s , 200 g, w a s l o s t throillgh t h e empty can

d i s c h a r g e chute because excessive powder had accumulated ic t h e box. l e a k i n g seal on t h e v i b r a t o r y Ecreen d r i v e s h a f t accoluited f o r

Remote r n s 6 i f i c a t i o n t o t h e decannifig s t a t i o n and changes i n o p e r a t i n g procedures elPminated t h e s e sources of EQSS a f t e r t h e fClrst batch (29

o x ~ c ~c ea n s ) had been processed. Sampling accounted f o r a loss of 1c)C g of x r a n i m .

TI.TS 15-g and

two 5 - g salt samples were r e q u i r e d i n each of t h r e e p r o e a e t i o n r u n s . I n adc?ition, s e v e r a l e x t r e samples were r e q u i r e d f o r s p e c i a l purposes.

The presence of h e e l s i n c e r t a i n v e s s e l s and t h e holdup i n t r a n s f e r l i n e s and f i l t e r s were r e s p o n s i b l e f o r t h e m a j o r i t y of t h e loss. h e e l i n the r e a c t i o n v e s s e l axounted t o

- ~ e s s e lcontained 346 replacement.

27 Q .

The

H o k w ~ ~t h : e storage

of u r a n i m as h e e l as e r e s u l t of a d i p l i n e

#The d i p l i n e

IELS

i n s t a l l e d improperly znd, as a r e s u l t ,

about b/a i n . of unrecoverable s a l t heel w a s l e f t i n t h e vessel. A sumnary of t h e uranium a c c o u n t a b i l i t y i s given i n Table

Table 9

Uranium MaterLaE Balance

Uranium receive^ as oxide

399 721

100

98.1

39,952

Finisher;prcduct, LiP-up4 Measured l o s s to h e e l s , saqles, etc

446

1.1

E s t h a t e d l o s s t o Austing, bines, f i l t e r s , e t c

322

0.8

Early i n the run with d e p l e t e d uranium, it Seczme o b v i o 7 ~ts h t some of che equi-pent

in c e l l G could not 3 e considered r e l L a b l e end

worzld have to h e r e p a i r e d o r r e p l a c e d b e f o r e t h e conclusion o f t h e

t h r e e production rms.

Many of t h e d e f i c i e n c i e s were c o r r e c t e d i n r ?

the lnterval between t h e depleted-uranium run an2 ",e it

W&E

2'3U

r-m. Since

i m p r a c t i c a l t o c o n s i d e r major equipment m o d i f i c a t f o n s a t this

t i m e beceuse of t h e f u e l d e l i v e r y schedule requirements a t t h e !GREY emphasis w a s placed on:

(1) s t o r a g e of s p a r e p a r t s i n t h e c e l l ,

(2) i n s t a l l a t i o n of redw-ciant f i t t i n g e , (3) procurement zslrt moclification of t o o i s and work tables i n c e l l G, and ( 4 ) Torrimlation of rnalntenance procedures.

7 . 1 Spare P a r t s Because of t h e d i f f i c u l t i e s involved i n o b t a i n i n g a c c e s s to %ne h o t c e l l , a generotbs supply o f replacement p a r t s w a s s t o r e d i n s i d e t h e c e l l and c a t a l o g e d for easy r e t r i e v a l .

Where a p p l i c a b l e , t h e p a r t s

were p r e f i t r l e d t o ensure c o m p a t i b i l i t y w i t h t h e system.

Threads on

the f i t t i n g s and n u t s an6 b o l t s were t r e a t e d with a l a b r i c a n t tha.'; i s s u i t a b l e for use i n high-temp%rature e n v i r o m e n t s .

7.2

Redundant F i t t i n g s

The compression-type f i t t i n g s used on t h e s a l t t r a n s f e r l i n e s and

on t h e gas supply l i n e s a t t h e v e s s e l nozzles were extremely d i f f i c u l t t o make and 'break a f t e r t h e y had been t h e r m a l l y cycled fro^ room temperah o f these t u r e t o 600-700"~.The passage o f molten salt t l a r o ~ ~ gone f i t t i n g s made the o p e r a t i o n even more d-iff'icult because t h e s a l t formed a s e a l around t h e p r o t r u s i o n of t h e tubing i n t o t h e f i t t i n g .

Since

several of t h e e e f i t t i n g s had t o be r o u t i r e l y operated i n t h e produet t r a n s f e r o p e r a t i o n s , t h e r e were s e v e r a l l i n e s i n t h e system f o r which

no a l t e r n a t e had been provided.

I n t'nese cases, redundark F i t t i n g s

vere i n s t a l l e d i n such a manner t h a t a second f L t t i n g w a s avzilable i f t h e primary f i t t i n g could not be operated.

Although complex f i t t i n g

arrangements a r e normally conducive t o leakage, enccuntered h e r e .

such problems were

On two occasions, use of t h e standby f i t t i n g vas

necessary i n o r d e r t o r e p l a c e t h e s i n t e r e d m e t a l f i l t e r i n t h e s a l t t r a n s fer l i n e

7.3

Tools and Work Tables

A l a r g e assortment of hand t o o l s , modified f o r use with t h e arianipu l s t o r s , were s t o r e d on t o o l racks i n t h e c e l l .

Usually t h e m o d i f i c a t i o n

c o n s i s t e d of welding g r i p s t o t h e t o o l t o a i d i n handling by t h e nesters l a v e manipulators.

A few special-purpose t o o l s , such as a i r - o p e r a t e d

s n i p s ( f o r c u t t i n g t h e i n t e r c o n n e c t i n g t u b i n g of t h e c a p s u l e s ) and an impact wrench ( f o r use with t h e electromechanical manipulator) a l s o s t o r e d â&#x201A;Źor l a t e r use i n t h e cell.

were

End wrenches and o t h e r fixed-

s i z e t o o l s were c o l o r coded by s i z e s for e a s e i n i d e n t i f i c a t i o n .

Work tables and t r a y s were l o c a t e d between t h e viewing windows and t'ne major p i e c e s o f equipnent.

m e y p ~ o v e dt o be i n v a l u a b l e i n t'ne

many mechanical and maintenance o p e r a t i o n s conducted i n t h e t h r e e s a l t productlon r m s because of t h e l i m i t e d reach of t h e m a s t e r - s l a v e manipu l a t o r s and a l s o because of t h e l i m i t e d riel& o f v i s i o n a v a i l a b l e through t h e windows.

A secondary, b u t very important, f u n c t i o n of t h e t r a y s

involved r e t r i e v a l of t o o l s and miscellaneous items t h a t were dropped because of wear of Eanipulator p a r t s o r because of ewkwardness on t h e

p a r t of t h e o p e r a t o r .

When an item f e l l t o t h e floor, r a t h e r t h a n

onto a t r a y , it u s u a l l y had t o be rep.'iaced si.nce r e t r i e v a l from the

f l o o r i n rrany l o c a t i o n s of t h e c e l l w a s irrpossible. The k r g e heavy-duty work tabbe (P4g.

19) designed â&#x201A;Źor t h e p r o d - x t

c o n t a i n e r and c a p s u l e a r r a y disassembly o p e r a t i o n s served 7*rePE i n t k e s e

func",icns

and w a s also used e x t e n s i v e l y as a general-purpose work bench.

7.4

Maintenance Procedures

Remote maintenence o â&#x201A;Ź t h e procecE eq-Jipmcnt was recognized, d m i n g t h e run with d e p l e t e d uranium, t o be a f o m i d ? u b l e t a s k t h a t collld not b e l e f t t o t h e o p e r a t o r ' s d i s c r e t i o n when t h e nee? a r o s e .

3 u s an

engineer was assigned, on a f u l l - t l m e b a s i s , t o develop d e t a i l e c i mhintenance proceclurcs thak vould be a p p l i c a b l e d u r i n g any conceivable F a i l u r e as well as d w i c g t h e planned maincenznce o p e r a t i c n s

A comprehensive s e t of close-up photographs was teken of tt:c

e q u i p e n t i n cell G b e f o r e t h e c e l l was sealec t o process %he r a d i o a c t i v e

material.

These were l a t e r sJ@uentec by photographs taken through t h e

Ehielding windows and t h e rr_or,ocular viewers

Altogether, mere t h a c 300

photographs were rnarje. Fif$y-fi.ve d e t a i l e d , s t e p - b y - s t e p rmintenance procedures were w r i t t e n by - s i n g t h e photographs and f i e l d sketches (more than 300) t h z t had been .used I n t h e f & h r i c a t i o n and. i n s t a l k t i o n of t h e equip-

nent.

A comapletc list of? t o o l s and m a t e r i a l s n e c e s s a r y f o r t h e job was

included i n each procedrxre

-!&ere a p p r o p r i a t e , the maintenance proce-

d u r e was r e f e r r e d t o , o r included in, an o p e r a t i n g procedure t o ensure c o n t i n u i t y of' a process o p e r a t i o n .

Although it w a s not n e c e s s a r y t o

use a l l of t h e s e procedures i n t h e f u e l production, t h e y were i n s t r u n e n t a l i n e n s u r i n g a s a f e and o r d e r l y completion of t b i s task.

CQMCLUSIOKS r

1. Reactor-grade e i l t e c t i c salt c o n c e n t r a t e , 7LiF-23JLTb (73-27 mole $), cnaa b e prepered by r e a o t e ir,eans f r o m LIF and rJ3UOr o r r33, 4 2 P'

3y t h e process d e s c r i b e d ric t'nZ~ r e p o r t .

2- Hydrogen reduction and hydrofluorination reaction rates of oxide beds can be controlled satisfactorily by adjusting hydrogen and flows to avoid excessive temperature excursions from the exothermic reactions involved.

Temperatures can be determined by placing a number

of thermocouples within the beds.

Ecpipment for a remote process of this t y p e should be designed

with a minimum number of close-tolerance fits. signed on a modular concept

It should also be de-

that components car, easily be replaced,

thus eliminating, if possible,, remote repair operations.

In general, commercial pipe, tubing, and electrical fittings

are satisfactory in this type of operation.

However, they are not

satisfactory in instances where high temperatures or exposure to molten salt are expected.

In these cases, special-purpose fittings should be

developed.

Concentrations ~f the corrosion products nickel and iron can

Se reduced to satisfactorily low levels by hydrogen treatment of molten szlt at 550째C.

Chromium was not reduced by the process described.

6. A blnary mixtme of UF4-EiF having a eutectic composition can be fused at a temperature of 650째C in the presence of a small mioauat of' liquid eutectic heel remaining in a vessel.

In t h e absence of the Eiq-

u i d heel, it is necessary to heat the materials to the melting point

of' the LiF (835째C) to achieve liquefactl ion.

7 . T c cbtain a product containing less than b ppm of oxygen and to avoid plugging of dip lines by t'ne formation of' oxides within them, it w z s necessary to install e @ata.ly-bic recombiner and a molecularsieve drying column in %he hydrogen supply system.

'The use of Einde

rype 41.4 1/16-:~-di~m sieve material in a regenerative drying co~unn

retimed the rnoistixe content of commercial-grade hydrogen to less than

3 PPm. 8.

bintenance procedures are necessary to ensure orderly corn-

pletion of a process of this nature.

They are vital when entry into a

contaminated cell is necessary and when equipment and the product must be removed from the cell.

The aukhors express $ h e i r a p p r e c i a t i o n t o %he following persons whose a s s i s t a r , c e w a s e s s e n t i a l t o t h e s u c c e s s f u l p r e p a r a t i o n of t h e enrichTng 2331J r u e 1 c o n c e n t r a t e for t h c ?ISRE:

G. I. Cathers and

J H. S h a f f e r (Reactor Chemistl-y Division) f o r process development; E. E. Nicholson and W. F. S c h a f f e r , Jr., f o r process equulpinent cleslign;

S. I k n n f o r a s s i s t a n c e i n o p e r a t i o n s arid d a t a a n a l y s i s ; J. 1. J a r v i s (cn 1oa.n t o t h e Metals and Ceramics Division f r o a t h e General Engineeri n g D i v i s i o n ) for process eqxipment i n s t a l l a t i o n and msdificacion, and

for cieveboplnent of mainteneme procedures; acd 3 . W. Anderson end

B. M e Shep'nerd (both of whom are or? l o a n t o t h e Metals and Ceramics ty Division from t h e General Engineering Division) f o r f ~ ~ c f l i cngineerfng

a.nd supportling s e r v i c e s

10. REFEF.ENCES

P o N. Haubenreizh, p r i v a t e c o r n m i c a t i o n , Beceanber 1966

J. 3. Engel, I'ERE Design and Operations Report, F a r t XI-A, ORhT-TM-2304 (September 1968) Chem. Tech. Biv. Ann. Progr. Rept., I%y

312 1968, ORNk-1~2.72,

pp. 28-33.

J. W. Anderson and J. 6.1. Chandler, S a f e t y Analysis for t h e ThoriumUranium Recycle F a c i l i t y (TURF), Building 793C, OBI%-4278 ( t o be published)

C. J . Barton e t ab.,

"Phase E q u i l i b r i a i n the A l k a l i F l u o r i d e -

Uranium T e t r a f l u o r i d e Fused S a l t Systems,"

J. h eC e r a m . S O ~ . ,

41(2), 43-69 (1958) P. N. Haiiber-retch et a l . , MSRE Design and Operations Report,

......

..?

P a r t V-A,

%:&fetyAnalysis of Operations with 233U, ORHL-TM-2211

(February

19681, p. 37.

CRNL-4 37 1

uc-80

- Reector

Technology

IMTERNAL DISY'RIBUTIOM 1, Biology L i b r a r y 2-4 Centsrel Research Library 5-6. ORNL Y-12 Technical L i b r a r y Document Reference S e c t i o n 7-41. Laboratory Records Department 42. Laboratory Records, ORNL R . C . 43. R. G. A f f e l 44. J. L. Anderson 4 5 . J . W. Anderson 46. C . F. Baes 47* S, E, B e a l l 48. M. Bender 49. E . s. Bettis 50. E , G. Bohlnan ~

51. S, E " Bobt 52. G. E. Boyd 53, R. E. Briggs 54. R . E , Brooksbank 5 5 . W. B. Burch 56. W. 9. Carr

57. G . 3 . Cathers 58-59. J, M, Chandler 60. F . L. C u l l e r , Jr. 61. S. J. D i t t o 62. W. P, Eatherly 63. 3 . 8. Engel 64. D . E . Ferguson

6 5 . E. M. 66. J . PI 67. 8. E . 68* W. R. 69. A. G .

~erria Frye, Jr.

Gehlbach Grimes Grindell 78. R. G . Gumon 71. P a x'. Saubenreich 72. 74. H. Jordan 7 3 . P. R. Kasten 74, J . W. Moger

95.

E. Lanib

76. C. E. Larson 77. M. H. Lin 78. R. â&#x201A;Ź3. Lindauer 79, A . F. Litman 80. A . E . L o t t s 81. M. Lundfn 82. PI. G. MacPherson 83. R . E . MacPhe-w o n 84. S, Mann 85. H. E . McCoy 86. J , R . McWherter 87. R. L. Moore 88. J e P . Nichols 89. E. L . Nicholson 90. A . S . Meyer

91. A . M. Perry 92-93. M. W. Rosentha1 94. Bunlap S c o t t 95. W. F. S c h a f f e r 96. J . E . S h a f f e r 97. 37. J. Skinner 98. J. W. Snider 99. B. A . Sundberg 100. R , E. Thcmna 181. W. E. Unger 182. J - E. Van Cleve, 3 r 103. A . ?Im Weinberg 104. J . E, Weir 1 0 5 . M. E . whatley 106. G . M. Watson 107. J . C . White 108. R . G. Wper 109. Gale Young

110. J. 111. P. 112. J. 113. J . Elk. E .

L. youngblood H. m e t t ( c o n s u l t a n t ) J. K a t z ( c o n s u l t a n t )

L Margrave ( c o n s u l t a n t 1 A . Mason ( c o n s u l t a n t ) 115. R . B. Richards ( c o n s u l t a n t )

EXTERNAL DISTRIXJTION

........-

116. D, E. BloomfiePd, Battelle-Northwest, Richland, Washington 117. J . A , Swartout, Union Carbide Corporation, New York 118. Laboratory and U n i v e r s i t y D i v i s i o n , AEC, OR0 119-338. Given d i s t r i b u t i o n as shown i n TID-4500 under Reactor Technology c a t e g o r y (25 c o p i e s - CFSTI)