3/4

K /PS449
DE84 011589
Date of I ssue: May 1983
UFg CYLINDER HOMOGENIZATION STUDY - EXPERIMENTAL RESULT
WITH A 10- TON CYLINDER
S. H. Par k
Syst ems and Equi pment Technol ogy
Pr ocess Suppor t Di vi si on
Uni on Car bi de Cor por at i on, Nucl ear Di vi si on
Oak Ri dge Gaseous Di f f usi on Pl ant
1
Oak Ri , dge, Tennessee
DI SCLAI MER
This report was prepared as an account of work sponsored by an agency of the United States
Government. Neither the United States Government nor any agency thereof, nor any of their
employees, makes any warranty, express or implied, or assumes any legal liability or responsi- '
bility for the accuracy, completeness, or usefulness of any information, apparatus, product, or
process disclosed, or represents that its use would not infringe privately owned rights. Refer-
ence herein to any specific commercial product, process, or service by trade name, trademark,'
manufacturer, or otherwise does not necessarily constitute or imply its endorsement, recom-
mendation, or favoring by the United States Government or any agency thereof. The views
and opinions of authors expressed herein do not necessarily state or reflect those of the
United States Government or any agency thereof. />
BSTOBOTOf Of TWS DflCWiWT IS Wl l WT! 0
5/ 6
TABLE OF CONTENTS
ABSTRACT -
7
I NTRODUCTI ON 9
I NSTRUMENTATI ON AND PROCEDURE .' 10
Gener al .'" ... .1 10
Q
Experi mental .Desi gn 12
T est. 16
RESULTS
1 6
o
it ,
CONCLUSION. . 27
ACKNOWLEDGEMENT ' 29
DI STRI BUTI ON
31
7/ 8
ABSTRACT
The UFg cyl i nder homogeni zat i on pr ocess has been i nvest i gat ed
exper i ment al l y wi t h a 10- t on cyl i nder . A speci al l y modi f i ed cyl i nder
equi pped wi t h sampl i ng pr obes and t emper at ur e sensor s was f i l l ed wi t h
essent i al l y equal amount s of t hr ee di f f er ent assay mat er i al s. The
cyl i nder was t hen heat ed i n an aut ocl ave wi t h sat ur at ed st eam f or
13 hour s. Sampl es wer e dr awn f r om each of f our sampl i ng por t s f or
11 hour s. Temper at ur e measur ement s i ndi cat ed t hat sol i d UFg exi st ed i n
t he cyl i nder f or 5 hour s, and t he assay mi xi ng pat t er n dur i ng t hi s
per i od was f ai r l y l ocal i zed. Lar ge scal e mi xi ng of t he di f f er ent assay
mat er i al s f ol l owed af t er t he compl et e mel t down of t he sol i d UFg due co
a l ar ge t emper at ur e gr adi ent i n t he l i qui d. The t emper at ur e gr adi ent
decr eased t o l ess t han 1F/ f t af t er 11 hour s of heat i ng; hencef or t h, t he
mi xi ng mot i on by l i qui d convect i on pr act i cal l y ceased. The t est r esul t s
i ndi cat ed t hat t he var i ance of assay sampl es, at any gi ven t i me, wer e
never smal l er t han t he var i ance of t he spect r omet er measur ement s dur i ng
t he ent i r e t est per i od and, hence, i t can be concl uded t hat t he cyl i nder
never achi eved absol ut e homogenei t y. The def i ni t i on or r equi r ement s f or
homogenei t y of a UFg i s beyond t he scope of t hi s r epor t ; however , si nce
t he anal ysi s f or assay of a cyl i nder i s consi der ed t o be accur at e t o
0. 1%, t hi s woul d seem t o be a mi ni mum r equi r ement . The assays at t he
f our por t s wer e wi t hi n 0. 1%of . each ot her af t er 8. 5 hour s of heat i ng and
wi t hi n 0. 05% af t er 11 hour s of heat i ng. Two l i qui d sampl es wer e t aken
at t he end of t he t est t hrough t he val ve. The aver age assay val ue of
t hese was 2. 1743%
2 3
U whi ch was 0. 02%of f f romt he t heor et i cal l y cal cu-
l at ed val ue. * @>
o
9
I NTRODUCTI ON
I n t he dai l y oper at i on of t ne ur ani um t ol l enr i chment pr ocess,
sampl i ng of a cyl i nder t o det er mi ne i t s assay i s an i mpor t ant t ask.
Thi s pr ocess i s al so t i me consumi ng si nce i t i nvol ves heat i ng t he
cyl i nder f or a suf f i ci ent amount of t i me t o ensur e t hat t he cont ent s ar e
i n a homogeneous st at e i n t er ms of assay. I n t he U. S. enr i chment pr o-
cess, t he heat i ng of t he cyl i nder i s conduct ed i n an aut ocl ave wi t h
sat ur at ed st eam. The pr ocedur e adopt ed at t he Oak' Ri dge Gaseous
Di f f usi on Pl ant ( ORGDP) i s t o pl ace a cyl i nder i n an aut ocl ave i n t he
af t er noon and heat i t over ni ght , f ol l owed by sampl i ng t he next ' mor ni ng.
The assay val ue det er mi ned by t he sampl e t hen, r epr esent s t he assay of
t he cyl i nder . Thi s heat i ng
1
t i me, 18 hour s or l onger , may or may not
be suf f i ci ent t o ensur e assay homogenei t y i n t he cyl i nder . Al l i ndi ca-
t i ons woul d evi dence t hat i t i s a suf f i ci ent amount of t i me f or a
cyl i nder t o r each assay homogenei t y; however , t her e exi st ed st r ong needs
f or i nf or mat i on on t he mi ni mum t i me r equi r ement s f or a gi ven si ze of
cyl i nder t o r each assay homogenei t y under aut ocl ave oper at i ng condi t i ons
and how t he var i at i on of oper at i ng condi t i ons mi ght af f ect t he t i me of
heat i ng. Thi s i nf or mat i on i s needed t o det er mi ne t he f easi bi l i t y of
pr epar i ng a cyl i nder f or sampl i ng wi t hi n an 8 hour shi f t and al so i n
hel pi ng t o est abl i sh an i nt er nat i onal st andar d f or t he cyl i nder sampl i ng
pr ocedur e. Ther e have been sever al at t empt s i n t he past t o answer t hese
quest i ons. One r ecent st udy conduct ed by R. F. Smi t h* at t he Paducah
Gaseous Di f f usi on Pl ant ( PGDP) showed t hat a 14- t on cyl i nder r eached
assay homogenei t y i n 12 hour s. The st udy was conduct ed wi t h ni ne cyl i n-
der s whi ch wer e spi ked wi t h di f f er ent assay mat er i al of known amount s.
The cyl i nder s wer e t hen heat ed and sampl ed at var i ous t i me i nt er val s.
One maj or dr awback of t hi s met hod was t he sampl i ng t echni que whi ch
i nvol ved st oppi ng t he heat i ng pr ocess and r ot at i ng t he cyl i nder . Thi s
i nt er r upt ed t he mel t i ng and convect i ve, mi xi ng mot i on of UFg i nsi de t he
cyl i nder and cr eat ed addi t i onal l ar ge scal e mi xi ng by t ur ni ng t he
cyl i nder . The pr esent st udy was desi gned t o i nvest i gat e t he assay homo-
genei t y pr ocess wi t h mi ni mumdi st ur bances of
1
t he mi xi ng pr ocess- i n or der
t o obt ai n unbi ased dat a. The t wo obj ect i ves of t he st udy ar e:
1. Det er mi ne t he mi ni mum t i me f or a 10- t on cyl i nder t o r each
assay homogenei t y.
!: 2. Det er mi ne a cor r el at i on bet ween t emper at ur e and assay
i, var i at i ons i n t he l i qui d UF
6
dur i ng t he heat i ng per i od.
i, ' -
f. The f i r st obj ect i ve coul d be r eadi l y achi eved by assay sampl i ng of
t he cyl i nder . Thi s, however , woul d not pr ovi de i nf or mat i on on t he
ef f ect of changes i n cyl i nder si ze and aut ocl ave oper at i ng condi t i ons on
t he mi ni mumt i me r equi r ement t o obt ai n homogenei t y. I t was deci ded t hat
t hi s i nf or mat i on coul d best be obt ai ned by devel opi ng a numer i cal moci el
Smi t h, R. F. , St eamBat h Cycl e Requi r ed f or I sot opi c Homogenei t y of c
14- Ton UF
6
Cyl i nder ( U) , KY- 556, Uni on Car bi de Cor p. , Nucl ear Di v. ,
Paducah Gaseous Di f f usi on Pl ant , J une 17, 1968. UNCLASSI FI ED. ' j
,"' <
l
' * ' \ i- . ""'. ' '" ' " ' ' " >
:
.
' " \ o - ' " - . . ' ' ' '
K
\
10
of t her mal convect i on cur r ent s i n t he cyl i nder . The model woul d be
const r uct ed t o mat ch known t emper at ur e gr adi ent s i n t he cyl i nder whi ch
coul d be cor r el at ed t o assay gr adi ent s. I n or der t o meet t hi s obj ec-
t i ve, i t was essent i al t o obt ai n t he var i at i on wi t h space and t i me of
t he t emper at ur e and assay of t he UFg i n t he cyl i nder .
I t was par amount t hat t hese par amet er s be obt ai ned wi t h mi ni mum
i nt er f er ence of t he heat i ng and mi xi ng mot i ons whi ch r equi r ed subst an-
t i al changes t o t he sampl i ng t echni ques t hat had been empl oyed i n t he
past . , Thi s was accompl i shed by pr ovi di ng f our sampl i ng l i nes whi ch
penet r at ed t he aut ocl ave and t he cyl i nder so t hat - Sampl es coul d be t aken
at any t i me wi t hout openi ng t he aut ocl ave or r ot at i ng t he cyl i nder . The
space var i at i on of t emper at ur e/ assay was obt ai ned f r omt he posi t i oni ng
of t he pr obes i n t he cyl i nder / and t he t i me var i at i on was acqui r ed by
sampl i ng at var i ous t i mes dur i ng t he heat i ng per i od.
< I NSTRUMENTATI ON AND PROCEDURE ' '
GENERAL
As st at ed above, one of t he r equi r ement s t o accompl i sh t he obj ec-
t i ves of t he exper i ment was t o obt ai n dat a wi t h mi ni mumdi st ur bance t o
t he UF
6
cont ent s. Thi s r equi r ed t wo basi c changes i n t he met hod of "
aut ocl ave oper at i on:
1. The t est ' cyl i nder , once pl aced i n t he aut ocl ave, woul d not
be r ot at ed or t i l t ed. V,, The heat i ng pr ocess woul d not be
st opped dur i ng t he t est .
n
2. The t emper at ur e and assay woul d be moni t or ed cont i nuousl y
,J t hr oughout t he heat i ng ( peri od. .
u
The exper i ment was conduct ed, wi t h a 10- t on cyl i nder . The cyl i nder
was modi f i ed t o accept t hr ee t emper at ur e/ assay pr obes and one pr essur e
t ap. The pr obes, descr i bed i n det ai l i n r epor t K/ PS- 452*, consi st
h
of
1- i nch di amet er st eel pi pes, 4 f eet i n l engt h, whi ch cont ai n f i ve t em-
per at ur e sensor s and one assay sampl e por t ; one pr obe cont ai ns t wo
sampl i ng por t s. The posi t i on of t hese pr obes, shown i n Fi gur e 1, i ndi -
cat es t he r el at i ve posi t i on of t he \ sampl e por t s. The cyl i nder cont ai ned
15 t emper at ur e sensor s, f our sampl i ng por t s, and one (pressure t r ans-
ducer . Wi t h thi s' -i i nst r ument at i on, i t was possi bl e t o moni t or
t emper at ur e/ pr essur e cont i nuousl y and dr aw sampl es wi t hout i nt er f er i ng
wi t h t he heat i ng process- ; The over al l scheme of t he t est was t o heat
t he cyl i nder wi t h t hr ee di f f er ent assay mat er i al s of known amount s and
sampl e unt i l t he assay of t he sampl es r eached t he cal cul at ed val ue of t he
mi xt ur e. Unf or t unat el y, t he assay of t he sampl es coul d not be det er -
; mi ned i nst ant aneousl y, so i t was necessar y t o t ake sampl es over a suf -
- - i l
;_, '2
'- *Br anam, D. A. , UFg Homogeni zat i on St udy Sampl e Pr obes, ( U) ,
K/ PS- 452, Uni on Car bi de Cor p. , Nuci ear
;
i ui v. , TO be i ssued at oak Ri dge
Gaseous Di f f usi on Pl ant . UNCLASSI FI ED. tt
S1 S2
P1
S3
w

T2()
)>
T3()AB
AD
T4()
DWC. NO. K/ G- S3
|U)
LAA
L/2.
T 5Q ^C
L/6
S1,S2, S3 -TEMPERATURE/ASSAY
O - TEMPERATURE SENSORS
A - ASSAY SAMPLE PORT
PI, P2 - PRESSURE TAP
Figure 1
SCHEMATIC DIAGRAM OF THE TEST CYLINDER
12
f i ci ent t i me span t o ensur e t hat t he cyl i nder r eached t he homogenous
st at e.
EXPERI MENTAL DESI GN
The cyl i nder was l oaded wi t h t hr ee di f f er ent assay mat er i al s of
al most equal amount s, as shown i n Tabl e 1.
Tabl e 1. Summary of t he Feed Mat er i al s
J>
Material
No. i p
Assay
wt %
235
o
2.6098
Amount
l bs
1
Assay
wt %
235
o
2.6098 6,752
2 2.1759 6,750
3 1.7394 6,767
Each assay mat er i al ' was f ed i nt o t he cyl i nder f ol l owed by a mi ni mum
of 3 days of cool i ng t o sol i di f y t he mat er i al . Thi s was t o mi ni mi ze
mi xi ng dur i ng t he f eedi ng pr ocess and t o cr eat e t he desi r ed st r at i f i ca-
t i on of assays. The choi ce of t hr ee assay mat er i al s was made t o reduce
t he t i me of each f i l l and
i
mi ni mi ze t he amount of mel t i ng and mi xi ng wi t h
t he pr evi ous f i l l . The 2. 6098 wt per cent 235
a ma
t
e
r i al was f ed f i r st ,
f ol l owed "by 2. 1759 and 1. 7394 wt per cent ^Sy mat er i al , r espect i vel y.
Wi t h t hi s f eedi ng, t he, . t heoret i cal assay of t he mi xt ur e was 2. 17471 wt
per cent 235
u%
O
!|
'>
The i deal si t uat i on woul d be t o moni t or t he t emper at ur es and sampl e
f or assay cont i nuousl y, but i t was physi cal l y i mpossi bl e t o manage at
t hi s t i me. ._
J
The t emper at ur es wer e moni t or ed every 10 mi nut es whi l e
sampl es wer e dr awn every hour . The l onger sampl i ng t i me span was di c-
t at ed by t he sampl i ng sequence adopt ed f or t hi s exper i ment . The
sampl i ng syst em, shown i n Fi gur e 2, consi st ed of a pr obe wi t h a sampl e
por t , copper t ubi ng, and val ves t o t r ansf er t he"sampl e t o t he sampl e
t ube, and auxi l i ar y syst ems f or dumpi ng UFg and cl eani ng t he l i nes.
Ther e wer e f our i dent i cal syst ems i n t he exper i ment . Al l t he l i nes wer e
heat ed wi th- , heat utape t o pr event sol i di f i cat i on of UF
g
. The maj or
sampl i ng oper at i ons i ncl uded f l ushi ng l i nes wi t h l i qui d UFg t o t he dump
t ank bef or e t r appi ng sampl es. The' , trapped mat er i al was t hen t r ansf er r ed
i nt o t he sampl e t ube. The amount of UFg t aken i n each t ube was approxi =^
mat el y 10 gr ams , / )
Fi gur e 3 and Fi gur e 4 pi ct ur e t he t est cyl i nder wi t h i t s i nst r umen-
t at i ons and sampl i ng panel .
TO 1423
EVACUATION
SS SYSTEM
0
NITROGEN
PCV
/pzz=zs
N
2
/
DWG. NC
AUTOCLAVE
. K/G-S2-236R1
/
h
\
h
\
10 TON
FEED
CYLINDER rv
V
k
v
El
?
N.
1
f
S
2
XS
3
-M
A
D
- VACUUM | 1
GAGE I
SIGHT Qj
GLASS
1
[TT1 SAMPLE PORT
FEP TEFLON SAMPLE TUBE
'
*2
DUMP TANK
- Figure 2
SCHEMATIC DIAGRAM OF THESAMPLING SYSTEM o
xff
PHOTO NO. K/PH-BZ-41Z2
Figure 3
TESTCYUNDER IN AUTOCLAVE NUMBER 1 WITH INSTRUMENTATIONS
PHOTO NO. K/PHt2-442f
(u) <
Figure 4
SAMPLING SYSTEM PANEL
16
TEST
The t est was conduct ed at t he K- 1423, Tol l Enr i chment Faci l i t y, i n
a speci al l y modi f i ed aut ocl ave. The sampl e l i nes and t her mocoupl e wi r es
wer e i nst al l ed t hr ough f l anges. The sampl i ng syst em assembl y was
i nst al l ed on t he f l oor l evel so t hat l i qui d f l ow woul d be enhanced by
t he combi nat i on of pr essur e di f f er ent i al bet ween t he cyl i nder and t he
dump t ank and t he gravi t y f or ce. Besi des t he 15 t her mocoupl es i nsi de
t he cyl i nder / t her e wer e 17 t her mocoupl es on t he ext er nal sur f ace of t he
cyl i nder and t he aut ocl ave wal l t o moni t or t hei r t emper at ur e var i at i on
dur i ng t he heat i ng per i od. The t est was conduct ed on December 13, 19S2.
Bef or e cl osi ng of t he aut ocl ave, t he t est cyl i nder was spi ked wi t h
473 gr ams of Cr 02F2 and 58 gr ams of MoFg by Anal yt i cal Chemi st r y
Depar t ment per sonnel f or i nvest i gat i on of chemi cal di st r i but i on bet ween
t he phases These chemi cal s of known amount wer e t o be used as sol ubl e
t r aces.
The aut ocl ave t emper at ur e set t i ng was at 220F.
RESULTS
Si nce t her e wer e t hree di f f er ent assay mat eri al si i n t he cyl i nder /
t he posi t i on of each r el at i ve t o t he t emper at ur e sensor
(
and/ par -
t i cul ar l y t o t he sampl i ng por t s at var i ous ' t i mes, was i mpor t ant i n
i nt er pr et i ng t he t est r esul t s. Fi gur e 5 shows t he schemat i c of t he
r el at i ve posi t i ons of t hese mat er i al s i n sol i d and l i qui d phases , at t he
t r i pl e poi nt . I f t he mat er i al s wer e not mi xeddur i ng t he f eedi ng
per i od/ sampl e por t s A, C, and D woul d be i n t he ' 2. 6098 wt per cent
235
U r egi me and por t B woul d be i n t he 2. 1759 wt per cent , . j
235
U r egi me
when t he "UFg mel t s. Al l t he t emper at ur e sensor s r ecor ded t he
sol i d/ l i qui d UFg t emper at ur es except T1, l ocat ed 1/ 2 i nches f r om t he
i nt er nal sur f ace of t he cyl i nder, , whi ch measur ed t he UFg vapor t emp-
er at ur e. The pr obe S3, whi ch was l ocat ed i n t he mi ddl e of t he
cyl i nder , mi ght r epr esent most cl osel y a t wo- di mensi onal r epr esent at i on
of t he phenomena occur r i ng i n t he cyl i nder . The t emper at ur e pr of i l e of
t hi s pr obe, pl ot t ed i n^cFi gure 6, r eveal s some i nt er est i ng f act s about
t he behavi or of UFg dur i ng t he heat i ng per i od. The f i r st not i ceabl e
f act was t he compl et e mel t down t i me appr oxi mat el y <5 hour s af t er st eam
was admi t t ed t o t he aut ocl ave. The t emper at ur e gr adi ent bet ween t he
sensor s dur i ng t he sol i d- l i qui d phase per i od^r emai ned l ar ge and
decr eased r api dl y af t er compl et e mel t i ng^of t he sol i d. The cr oss- over
of t emper at ur e pr of i l es bet ween sensor s T4 and T5 af t er 3 1/ 2 hour s of
heat i ng r esul t ed f r om t he sol i d UFg movement t owar d t he bot t omof t he
cyl i nder . A r api d l i qui d mi xi ng per i od f ol l owed t he compl et e mel t down
of t he sol i d' because of t he l arge t emper at ur e gr adi ent s and sl owed as
t he t emper at ur es appr oached uni f or mi t y.
The t emper at ur es of t he l i qui d appr oached a uni f or mval ue appr oxi -
mat el y 9 hour s af t er heat i ng began and t he t emper at ur e gr adi ent bet ween
sensor s was l ess t han 1F/ f t . Thi s i ndi cat ed t hat t her mal mi xi ng of t he
f l ui d had ceased f or al l pr act i cal pur poses.
17
L.M.H. _ ASSAY LEVEL OF FEED MATERIAL
O - TEMPERATURE SENSOR POSITION
A - ASSAY SAMPLE PORT
DWG. NO. K/G-83-110S
^TJ
M
H
SOLID AT
147.3F
T2 O
TI O'AB
T2 0 A D
T5 Q AA.C
M
H
'VJJ
it
LIQUID AT
147.3F
A>
<; >-
, " ' 'Figure 5
v ;
RELATIVE POSITIONSOF FEED MATERIAL AT DIFFERENT PHASE
: . u - ' . - ' , ;, ft, .
, , - . ( # . to.
DWG. NO. K/G-B3-1B07
00
4 5
TIME OF HEATING, hr
Figure 6
TEMPERATURE PROFILE OF PROBE S3
-^
19
Fi gur e 7 shows t he t emper at ur e pr of i l es of S1 and S3 i n or der t o
exami ne hor i zont al as wel l as ver t i cal var i at i ons of t he t emper at ur e i n
t he cyl i nder . The t emper at ur e pr of i l e of t he pr obe S1 agr eed wel l wi t h
t hat of S3 even t hough S1 was l ocat ed at t he end of t he cyl i nder . The
onl y measur abl e di f f er ences occur r ed i n t he l i qui d/ sol i d r egi me. The
cyl i nder sur f ace measur ement s showed t hat t he aver age t emper at ur e of t he
end pl at es wer e r el at i vel y l ower t han t he si de wal l dur i ng t hi s per i od.
Thi s i s r ef l ect ed i n Fi gur e 7 wher e a l ower sol i d UFg t emper at ur e was
measur ed at S1 t han S3. >Over al l , i t mi ght be concl uded t hat t he t hr ee-
di mensi on ef f act on t he t emper at ur e pr of i l e dur i ng t he heat i ng per i od
was mi ni mi zed.
^
The r el at i ve shape and posi t i on of sol i d at t he pl anes S1 and S3 i s
shown i n Fi gur e 8 as n f unct i on of t i me. The one- di . Ti ensi onal r epr esen-
t at i on can be pi ct ur ed i n t wo di mensi ons as di sks wi t h no t hi ckness at
pl anes S1 and S3. The di sks mai nt ai n a const ant di amet er f or 1 hour and
20 mi nut es unt i l t he sol i d st ar t s t o mel t and t he di amet er begi ns t o
di mi ni sh at pl ane S3. The mel t i ng at pl ane S1 begi ns 10 mi nut es l at er ,
but occur s at a sl ower r at e as i ndi cat ed by t he l ar ger di amet er di sk S1
compar ed t o S3. The sl ower mel t i ng r at e at S1 i s caused by t he l ower
t emper at ur e and heat i nput at t he end of t he cyl i nder whi ch i s a <con-
sequence of t he l ocat i on of t he st eaml i nes t hat ext end al ong t he l engt h
of t he cyl i nder . The uneven mel t i ng f ashi ons a cont our ed dumbbel l shaped
sol i d i n t he cyl i nder whi ch i s hel d i n posi t i on by t he convex ends unt i l
t he cent er at pl ane S3 br eaks^af t er 3 1/ 2 hour s. The di scont i nui t y of
t hese cur ves bet ween 3 1/ 2 hour s and 4 1/ 2 hour s of heat i ng coul d be
expl ai ned due t o t he f act t hat t he sol i d pi ece r emai ned bet ween t he t em-
per at ur e sensor s of T4 and T5.
t
.
I t was concl uded pr i or t o t he t est t hat sampl es shoul d be obt ai ned
i n t he ear l y t i me per i od of heat i ng t o pr ovi de i nf or mat i on on t he mi xi ng
mot i on, wi t h l ar ge t emper at ur e gr adi ent s. Consequent l y, i t was pl anned
t o obt ai n sampl es af t er t he compl et e mel t down of sol i d whi ch was
assumed' >t o be 2 t o 3 hour s af t er
-
t he st eam was admi t t ed t o t he
aut ocl ave. However , i t was f ound t hat t he t i me r equi r ed f or mel t i ng was
much ' l onger- t han expect ed. Ther ef or e, i t was det er mi ned dur i ng t he t est
t o i ni t i at e >sampl i ng at 2 1/ 2 hour s af t er t he st eamwas appl i ed, even
t hough sol i d UFg st i l l exi st ed i nt he syst em. Because of t he exi st i ng
sol i d phase, onl y t wo sampl es coul d be obt ai ned f r om t he f our sampl e
por t s i n t he f i r st sampl i ng per i od. The next sampl e per i od yi el ded f our
sampl es, as di d t he f ol l owi ng ni ne sampl e per i ods. I n al l , 42 sampl es
wer e anal yzed by mass spect r omet r y accor di ng t o an exper i ment al desi gn*
whi ch assur ed a f ai r compar i son of t he f our por t s wi t hi n each t i me
per i od. Ther e wer e 3 t o 6 det er mi nat i ons per each sampl e whi ch r esul t ed
i n an aver age of 4. 57 det er mi nat i ons per sampl e. The st at i st i cal
r esul t s of t he sampl e, as anal yzed by K. L. McCor mi ck*, ar e l i st ed i n
*K. L. McCor mi ck, Uni on Car bi de Cor p. , Nucl ear Di v. , Oak Ri dge
Gaseous Di f f usi on Pl ant , l et t er t o S. H. Par k, Mar ch 7, 1983.
UNCLASSI FI ED. *" ' " '
- c
""~" "*"" ' '
OWG. NO. K/G-83-1506
(U)
2 3 4 5
TIME OF HEATING, hr
Figure 7
TEMPERATURE PROFILES OF PROBES S1 AND S3
to
o
21
DWG. NO. K/ G- 83- 2010
(U)
2 3
TIME OF HEATING, hr
Figure 8
SOLID UF
6
SIZE AND POSITION DURING THE HEATING PERIOD
22
11
Tabl e 2. The r esul t s ar e al so pl ot t ed i n Fi gur e 9, and can be cat e-
gor i zed i nt o t hr ee di f f er ent r egi mes of mi xi ng. The f i r st r egi me
cover ed t he f i r st 5 hour s of heat i ng when t he cyl i nder cont ai ned bot h
sol i d and l i qui d UFg. I n t hi s r egi me, t he assays of each sampl e por t s
wer e di ct at ed by t he movement of sol i d UF
6
, and l i qui d mi xi ng. The
second r egi me of mi xi ng occur r ed f r om 5 t o 9 hour s af t er heat was
appl i ed when l ar ge scal e mi xi ng mot i ons exi st ed i n t he l i qui d UFg. The
l ast' ' -regi me pr evai l ed af t er 9 hour s and was char act er i zed by ver y l i t t l e
mi xi ng mot i on. Thi s l ast r egi me coi nci ded wi t h t he per i od when t he t em-
per at ur e gr adi ent t hr oughout t he cyl i nder was smal l .
//
The mi xi ng pr ocess of t he sol i d/ l i qui d r egi me, whi ch l ast ed f or
5 , hours, was t he most di f f i cul t pr ocess t o under st and. The assay
r esul t s f rom t he i ni t i al sampl es i ndi cat ed t hat mi xi ng had al r eady
occur r ed because t hey di f f er ed f rom t he assays of any of t he f eed
mat er i al s. However , t he assay at C was st i l l t he hi ghest , whi ch i ndi -
cat ed t hat most of each mat er i al f ed i nt o t he cyl i nder r emai ned i n i t s
r el at i ve posi t i on. The decr easi ng assays of A, B, and C i n t he next 3
t o 4 hour s coul d be expl ai ned by a chunk of sol i d UFg, whi ch consi st ed
of l ow and medi um assay mat er i al , sl owl y si nki ng t o t he bot t omof t he
cyl i nder , and mi xi ng wi t h t he hi gher assay mat er i al s t hat exi st ed i n
t hat l ocat i on. The l ower assay exi st i ng at A compared t o C dur i ng t hi s
per i od, coul d have r esul t ed f r omexcessi ve mi xi ng when t he mat er i al s wer e
f ed i nt o t he cyl i nder s and mor e mel t i ng and mi xi ng occur r ed at t he end
t han t he mi ddl e of t he cyl i nder because of t he cl ose pr oxi mi t y t o t he
f eed val ve. The mi xi ng i n t he 4 hour s f ol l owi ng compl et i on of sol i d
mel t down was pr oduced sol ey by t he convect i ve mot i on of t he ' l i qui d UFg
whi ch devel oped f r om t he t emper at ur e gr adi ent . Thi s l arge scal e or
r api d mi xi ng was enhanced by compar at i vel y l arge densi t y di f f er ences i n
t he l i qui d. As t he t emper at ur e gr adi ent decr eased wi t h t i me, t he degr ee
of mi xi ng mot i on subsi ded i n di r ect pr opor t i on. The t hr ee di f f er ent
mi xi ng r egi mes ar e depi ct ed agai n i n Fi gur e 10 by t he maxi mumdi f f er ence
i n assay bet ween sampl es at each sampl e t i me whi ch i s nor mal i zed t o t he
mean val ue and pl ot t ed as a f unct i on of t i me. The pl ot shows t hr ee di f -
f er ent pat t er ns; i ncr easi ng di f f er ences f ol l owed by f ast decr easi ng
val ues bef or e r eachi ng an al most f l at pat t er n of smal l di f f er ences i n
sampl e assays. The i ncr easi ng por t i on of r egi me coi nci ded wi t h t he
sol i d/ l i qui d r egi me wher e l ocal i zed mel t i ng and mi xi ng of UFg cr eat ed
l ar ge assay di f f er ences bet ween^por t s. The peak of t hi s regi me coi n-
ci ded wi t h t he compl et e mel t down t i me of t he sol i d UFg. The f ast
decr easi ng r egi me i n t he next 4 hour s cor r esponds t o t he l i qui d mi xi ng
r egi me whi ch was f ol l owed by a regi me of great l y r educed mi xi ng. The
ext er nal var i ance of assays bet ween por t s was never smal l er, t han t he
i nt er nal var i ance dur i ng t he t est and absol ut e homogenei t y of t he con-
. t ent s was never achi eved. Obt ai ni ng compl et e homogenei t y i n a cyl i nder
woul d r equi r e an i nf i ni t e t i me and i s not f easi bl e, but a degr ee of
homdgeni zat i on i s needed. The cur r ent met hods' f or det er mi ni ng t he assay
of cyl i nder s i s not consi der ed t o be mor e accur at e t han 0. 1%. I f t hi s
amount of var i at i on i n cyl i nder assay i s consi der ed t o be adequat e f or
homogeni zat i on, t hen i t was achi eved i n t he t est af t er 8. 5 hour s and a
var i at i on of l ess t han 0. 05%was achi eved af t er 11 hour s of heat i ng.
23
Tabl e 2. Summar y St at i st i cs of t he Exper i ment al Dat a
Hour s
2. 5
3. 5
4. 5
5. 5
6. 5
7. 5
8. 5
9, 5
St andar d
Por t Aver age Devi at i on
B 2. 2063 0. 000075
C 2. 2612 0. 000072
A 2. 1735 0. 000111
B
-,
2. 1918 v 0. 000132
C 2. 2706 0. 000284
D 2. 1831 0. 000164
A 2. 1988
0
0. 000161
B 2. 1374 0. 000080
C 2. 2246 0. 000017
D 2. 1829 0. 000167
A 2. 0871 0. 000079
B 2. 0936 0. 000043
c ' 2. 1999 0. 000081
D 2. 2121
rj
0. 000176
A 2. 1784 0. 000106
B 2. 1776 0. 000104
C 2. 1717 0. 000075
D" 2. 1817 0. 000076
A 2. 1799 , 0. 000039 "
B 2. 1757 0. 000076
C 2. 1698 0. 000102
D 2. 1766 0. 000147
A 2. 1765 0. 000055
B 2. 1754 0. 000102
C 2. 1749 0. 0 00025
D 2. 1744
rfV> , ,
0. 0 00063
A 2. 1758 * 0. 000077
B 't 2. 1755 0. 000121
C 2. 1748 0. 0 00022
D.
m
'
: v
. 2. 1754 ' 0. 000173
24
Tabl e 2. Summar y St at i st i cs of t he Exper i ment al Dat a ( cont i nued)
Hour s
10. 5
11. 5
12. 5
Por t
A
B
C
D
A
B
C
D
A '
B
C
D
Aver age
2. 1759
2. 1757
2. 1746
2. 1758
2. 1756
2. 1754
2. 1748
2. 1750
2. 1756
2. 1755
2. 1749
2. 1757
1
St andar d
Devi at i on
0. , 000177
0. , 000156
0. 000167
0. 000104
0. , 000119
0. , 000090
0. , 000162
0. , 000094
0. , 000083
0. , 000105
0. , 000133
0. , 000089
3
in
CO
CM
7 8 9
TIME OF HEATING, hr
-
~
DWG.
( U)
^
\ D
2.30
C .
c \
\ B \
S^ ^ T a =jp
2.20
A. B
D
vv
\ * -JJK""^
A. B
D
vv
A. B
vv
-
--
v
A
NJC
/ -
2.10
r
*
z
>*
2,00 I ' I I I 1
i " i i
1 1
NO. K/G-83-1509
10 11
Figure 9
VARIATION OF ASSAYS DURING THE HEATING PROCESS
- 2.182
2.180
A 2.178
2.176
2.174 $
- 2.172
- 2.170
- 2.168
12 13
to
ui
26
DWG. NO. K/G-83-1368
(" 1
2.5
\ -
*.10-2<
<
...
M
E
A
N

V
A
L
U
E

\ ll
P
S
P
R
E
A
D

A
S
S
A
Y

.-
\
s
.
u.
O
i /
O
1-
<
tt
t
10
'
B
0
D "
10-4 I 1 1
1 1 1
4.5 6.5 8.5
TIME, hrs.
10.5 12.5
Figure 10 \^
VARIATION OF ASSAY DEVIATION IN THE CYLINDER WITH TIME
27
The measur ed cyl i nder pr essur e was pl ot t ed i n Fi gur e 11 wi -th cal cu-
l at ed pr essur es based on l i qui d and vapor- t emper at ur es. The measur ed
val ues wer e hi gher t hr oughout t he exper i ment whi ch i ndi cat es t he
exi st ence of t he l i ght gases i n t he syst em.
CONCLUSI ON
Thi s r epor t cont ai ns t he exper i ment al r esul t s of t he st udy wi t h a
10- t on' cyl i nder . The compl et e mel t down t i me of t he UFg i n t he cyl i nder
wi t h 220F aut ocl ave cont r ol t emper at ur e was about 5 hour s. The l argest^- ; ,
t emper at ur e gradi ent exi st ed af t he end. of compl et e mel t down of sol i d
UF
6
and t he t emper at ur e gr adi ent decr eased t o l ess t han 1F/ f t i n ^
9 hour s of heat i ng t i me. The assay mi xi ng pr ocess was st r ongl y
dependent on t he t enper at ur e gr adi ent i n t he cyl i nder . Dur i ng t he f i r st
" 5 hour s of heat i ng, t he mi xi ng pr ocess was f ai rl y l ocal i zed wi t h t he ,
exi st ence of sol i d UFg i n t he l i qui d. " I n t he next 4 hour s, however , t he
mi xi ng pr ocess became most act i ve as a r esul t of t he convect i ve mot i on
i n t he l i qui d whi ch was i nduced by l arge t emper at ur e gr adi ent s i n t he
l i qui d UFg. The t emper at ur e gr adi ent decr eased t o l ess t han 1F/ f t <,
af t er 9 hour s of heat i ng. The mai n mechani smof any f ur t her mi xi ng f r om
t hi s poi nt was pr obabl y di f f usi on whi ch i s about t wo or der s of magni t ude
smal l er t han achi eved f r om t he convect i ve mot i on of l i qui d UFg. " The
i) spr ead of>'i-
/;
assay val ues bet ween por t s was reduced t o 0. 1% af t er
8 1/ 2 hour s of heat i ng and, , to 0. 05%af t er 11 hour s. The accur acy of t he
Jl assay val ues det er mi ned was _+ 0. 055%. Hence, i t was assumed t hat t he ->"
:
'J>J UFg r eached i t s assay homogenei t y at 11 hour s of heat i ng even t hough t he
ext er nal var i ance was never smal l er t han t he i nt ernal var i ance dur i ng
t he ent i r e t est per i od. The r el at i onshi p bet ween t he assay and t he t em-
per at ur e of UFg obt ai ned dur i ng t hi s exper i ment wi l l be used as a basi s
i n const r uct i ng a numer i cal model wi t h whi ch t he ef f ect of t he
var i at i ons of physi cal and oper at i onal condi t i ons on t he' mi ni mum t i me ,.,
scal e of homogenei t y can be i nvest i gat ed.
t
10 -
DWG. NO. K/O-83-IB04
<U|
MEASURED
BY SATURATED LIQUID TEMPERATURE
= 8 = 8 = 8 = =
=8
BY SATURATED VAPOR TEMPERATURE
MEASURED
n CALCULATED BY VAPOR TEMPERATURE
O CALCULATED BY LIQUID TEMPERATURE
5 6
TIMEOFHEATING.hr .
10
Figure 1 i -
COMPARISON OF CYLINDER PRESSURES - MEASURED AND CALCULATED VALUES
11
CD
29/ 30
ACKNOWLEDGMENT
>
'
The aut hor wi shes t o acknowl edge t he many who cont r i but ed t o t he
successf ul compl et i on of t hi s t est . Speci al r ecogni t i on shoul d be gi ven
t o J . O. Dodson and t he ent i r e Tol l Enr i chment per sonnel wher e t he t est
was
1
per f or med. The exper i ence of t he Anal yt i cal Chemi st r y per sonnel ,
who handl ed t he UFg sampl es, was cr uci al t o t he success of t he pr oj ect
as wel l as t he saf et y aspect . The aut hor woul d al so l i ke t o expr ess hi s
gr at i t ude t o D. L. Gr ay and J . L. Pat t on who par t i ci pat ed i n t he
sampl i ng
r
as wel l as J . H. Vance f or hi s cont i nuous i nvol vement i n t he
pr oj ect .
31
DI STRI BUTI ON
Admi ni st r at i ve Of f i ces
Thomas, W. F.
Separ at i on Syst ems Di vi si on
Ri epe, R. C.
Capaci t y Expansi on Pr ogr am
Dykst r a, J .
Gambl e/ J . F.
St er nber g, E. o.
Comput i ng Technol ogy Di vi si on
Bear d, B.
Ki r kpat r i ck, J . R.
Engi neer i ng Di vi si on
Kel l ogg, D. R.
Par sons, J . A.
Tr ot t er , T. C.
Heal t h, Saf et y and Envi r onment al
Af f ai r s Di vi si on
Gol l i her , W. R.
Oper at i ons Anal ysi s and
Pl anni ng Di vi si on
Br adbur y, J . T.
Davi s, W.
Younki n, J . M.
Y- 12 Pl ant
Whi t ehead, H. D. ,,
Goodyear At omi c Cor por at i on
Li nvi l l e, W. E.
Manni ng, R. E.
Ment ges, C. A.
, , Neel y, R. S.
Sandman, R. R.
Wol t z, F. E.
Paducah Pl ant
Br ei der t , E. C.
Bur net t , W. A.
Li l l e, C. D.
Lovel and, C. w.
Smi t h, R. F.
Wal t er , C. W. ^
Zer by, C D. ^\
Oper at i ons Di vi si on
Dodson, J . 0.
For bes, R. J .
Legeay, A. J . / Pet er son, C. H.
Shoemaker , J . E. , J r .
Pr ocess Suppor t Di vi si on
Bar ber , E. J .
Bor ough, G. B.
Br anam, D. A. "
Br ady, J i . P.
Dpnnel l y, R. G. / Pashl ey, J . H.
' Eby, *R." S. ^
Gambi l l , E. F.
Gr ay, D. L.
f
,
Grametbauer, G. L.
Hedge, W. D.
Howard, 0. H.
McCormick, K. L .
Merri man, J . R.
Park, S. H. (5)
Q$ Pi erce,
1
G. V.
Smi th, L. A.
Tayl or, M . J .
Vance, J . M.