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ORNL P
3252

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11:25 11.1.4 16
MICROCOPY RESOLUTION TEST CHART
NATIONAL BUREAU OF STANDARDS - 1963
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17.
TO
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THE HANDLING OF KILOGRAM QUANTITIES OF 4530 BY DIRECT AND REMOTE METHODS
....
AT THE OAK RIDGE NATIONAL LABORATORY CENTRAL DISPENSING FACILITY
-
.
CESTI PRICES
:
br.
j. R. Parrott
R. E. Brooksbank
NEW
#063.60, mw 65.91
:
1..:':
Oak Ridge National Laboratory
Oak Ridge, Tenuessee
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.
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.
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.
.
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SUMMARY
U
;
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WA
SEL
VISSZA
FI
. During the past few years, control of reactor parameters has made
possible the production of large quantities of 2530 with a desirably low
2324 content (less than 5 parts of 2320 per million parts of 233u). The
overall increase in production of 2330 in the United States led to the
establishment of a facility at ORNL to serve as a center for receiving,
purifying, and dispensing 2380 and its compounds. Extensive modifica-
tions of facilities in the original ORNL Thorex Pilot Plant (which had
later been modified for use as the Kilorod Solvent Extraction Facility)
were required to provide for the safe storage, dissolutions of solids,
and purification of materials containing 2. Installed storage systems
have capacities for 170 kg of 233v in solid foệm and 400 kg of 2330 as
uranyl nitrate solution. The original, one-cycle sulvent extraction
system, which is capable of purifying 233v at a rate of 250 g/hr, was
complemented with a glove-box solvent extraction system having a capacity
h
EN
*Research sponsored by the Atomic Energy Commission under contract with
the Union Carbide Corporation.

A
,
of 300 g per 8-hr shift. Also, the 500-gal batch dissolver was comple-
mented with a basket-type, high-efficiency leacher-dissolver that is
designed and sized to meet "ever-safe" criticality requirements. ..
This paper deals with methods anü procedures that are used to
control radiation criticality hazards; some attention is also given to
specialized equipment and to novel applications of equipment. The
facility utilizes essentially all forms of criticality control, in-
cluding mass limitation, concentration limitation, and use of neutron
poisons (fixed and soluble forms); also, in most cases, adequate shield-
ing is provided for the protection of personnel in the event of a neutron
excursion. We believe that the procedures and devices used to provide
assurance that poisons are always present will be of interest to others
in the nuclear industry; examples include the use of an ultrasonic
. method for determing the presence and distribution of borosilicate glass
rings.
.
.
.
1

-
-
-
ORAL-p-32.52
.
.
BIO
A.
....
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925 1957
.
*
**
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.
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.
.
"The Handling of Kilogram Quantities of
WU by Direct and Remote Methods at the
AL
.
*
.
..
1
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'
Oak Ridge National Laboratory Central
Dispensing Facility"*
.?.-
..
.
.:
.
by
12
-
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J. R. Parrott
R. E. Brooksbank ..
.
.
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LEGAL NOTICE
ICA
iii
*
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.
.
.
The raport www popard u nocount of Covenant pomnored worker Netther the United
that, nor the Countman, nor y porn noting a bowall at the Commons
A. Men many warranty or openentatios, proud or implied, with report to the accu-
moy, complemena, o tenen of the wormation contained in this report, or that the wo
ny mormation, Apparatua, methods of peown Milestoned in the report may not infringe
potwenty owned nog
1. Around my Mobile wala rueprot to the wood or for damage round thang from the
to ale nformation, marin, method, poow doctomd lan the report.
As mand un the whova, "person soting on hotell of the Courteetan i metodou may one
paya or contractor of the a utodel or employee al mal contractor, to the nation that
such employea or contractor a² the Commission, or employne of such contractor prejares,
Momentos,
w, may more pornt to Me ployment or contrnet
what we declan, « Mouplemust wat wel contractor.
.
!!
.
.
. .
.
.
Mais
.
.
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S
.
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Fili
TY
This paper (assigned Serial No. 15-43) 18 to be
submitted for the Winter ANS Meeting, Remote Systems
Technology Division, Chicago, Ill., October, 1967.
LET
'
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.
.
si
SIS
....
Research sponsored by the Atomic Energy Commission under contract with .
the Union Carbide Corporation.
ap
.
:
.:
They
.
.
DISTRIBUTION OF THIS DOCUMENT IS UNL MITED.'
.
THE HANDLING OF KILOGRAM QUANTITIES OF 2334 BY DIRECT AND REMOTE METHODS
AT THE OAK RIDGE NATIONAL LABORATORY CENTRAL DISPENSING FACILITY
J. R. Parrotit
R. E. Brooksbank,
Oak Ridge National Laboratory
Oak Ridge, Tennessee
ABSTRACT
onbekende
entiende en
The facility at Oak Ridge National Laboratory serves as a national
center for receiving, storing, purifying, and dispensing 2380. Kilogram
quantities (solid or solution) can be safely stored, retrieved for process-
ing, and purified to remove daughter products, chemical impurities, and
fission products. The handling techniques, both direct and remote, are
· described in detail; special processing equipment and controls for the
prevention of a nuclear excursion are also described.
motion du
.
o
inden it'* ; Pr
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bare me kontrolleride verb
t
... De
INTRODUCTION
...
EU
.....
In the program for developing economically competitive nuclear power,
use of the Th-238U breeding cycle 1.8 potentially significant; the interest
in exploiting this breeding cycle results from several factors, including
the high eta value for 2330, the abundance of thorium, and the elimination
of the need for separating uranium isotopes. However, until three years


.
.
...:
181
2
"
ago, the high 2320 content (greater than 40 ppm) of the 233y and the
radiation background resulting from the decay of <*U to high-energy
daughters dictated the use of shielded remote facilities for i abri-
cation of fuel elements.
-
V
**
:
*
*
.
The radiation problem was reduced by a factor of 10 when kilogram
quantities of u were produced under controlled reactor conditions
such that the 2340 concentration was less than 6 ppm. Although the bulk
of this material was earnarked for the Light Water Breeder Program,
approximately 150 kg was made available for experimental use. The
availability of this uranium, along with approximately 100 kg (“U
concentration: 250 ppm) that will be used in the ORNL Možten Salt Reactor
and an additional 50 kg (2920: 50 ppm) that had not been allocated,
resulted in the designation of ORNL as a central storage, purification,
· and distribution facility.
Extensive modifications to the original ORNL Thorex Pilot Plant
(which had later been modified for use as the Kilorod Solvent Extraction
Facility ) were required to provide for the safe storage, dissolution
of solids, and purification of materials containing 1sotopically pure
Pri
:
:
5.
AVE
2330.
This paper describes the storage systems, the dissolvers, and the
purification systems, with particular emphasis on operating techniques
and criticality controls.
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VIRT
STORAGE FACILITIES AND OPERATIONS
Quantities of 238U handled by the facility during the past seven
years are shown in Fig. 1. The material received through 1963 (and
shipped through 1964) includes the 32 kg separated during operation of
the Thorex Pilot Plant in the mid-1950's. The material with low 2320
content was transferred to the facility in 1965 and 1966.
Storage of Solids
The first 2384 received after establishment of the facility was in
the form of vo, canned in aluminum. Since sone of this material contained
as much as 250 parts of 2940 per million parts of 2380, it was necessary
to provide shielded storage with provisions for remote transfer into the
processing facility. The radiation level of the cans, each of which
contained 500 g of 2330, was approximately 1000 m/hr one month after
processing. This level had reached 150,000 mr/hr after storage for one
year.
Storage for solid material was provided as shown in Fig. 2 by drilling
vertical 5-in.-diam holes in the 5-ſt. shielding walls between adjacent
cells. These holes, lined with 4-in. SS pipe, were approved by the ORNL
Criticality Review Committee for storage at a maximum concentration of
1 kg of 2380 per foot of depth. The prime concern was that solution might
get into the holes, resulting in a drastic change in criticality mass
limits. Each hole is ventilated separately, thus pernitting the 1solation
of a hole with a leaky can. The latter condition can be determined
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readily from monitoring the off-gas, since 2330 emits high-activity
radon.
..
The charging of cans into the dissolver involves the use of a
shielded carrier. With the carrier in place over the storage hole, a
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into the dissolver, which is located in the upper part of the cell below
the pedestal.
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Storage of Solutions
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The solution storage facility is composed of five 240-gal tanks
located in the pipe tunnel area, which is adjacent to the cell wall and
below the operating area. This location took advantage of existing
· shielding (6 ft of concrete) on one side, earth fill on the opposite
side, and 4 ft of concrete' on top, leaving only the ends to be shielded.
The tanks, one of which is shown in Fig. 3, are 3 ft in diameter and
5 ft long, with a wall thickness of 3/16 in. Each tank is packed with
borosilicate-glass Raschig rings that are 1.50 in. OD, 1.042 in. ID,
1.75 in. long, and have a total glass volume that is equal to 31% of the
tank volume. The tanks have been approved by the ORNL Criticality Review
Committee for a 2330 concentration of 250 g per liter, with the volume
never to exceed 70% of the total available volume. Thus the storage
capacity 1s 110 kg of 233v per tank or a total of 550 kg for the five
tanks. The concentration limit was recently increased from 180 to 250
& per liter as a result of experiments performed by the ORNL Neutron
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Physics Division. Their data showed zero material buckling in a similar
tank filled with glass rings having the same packing fraction. It should
be noted that the borosilicate-glass rings have a certified composition
of 11.8 to 13.8 wt % B,0, and a 70B/+B ratio of 0.25 +0.01. The rings
are tested both chemically and mechanically prior to use.
A major consideration in using glass rings in a remote tank is the
possibility of crushing of the rings; this would lower the level of glass
,
.
.
.
.
in the tank, and could therefore result in a critical depth of solution
above the glass. The presence of rings is verified by an ultrasonic
technique that was modified for this purpose. This technique employs
an ultrasonic transducer that is lowered from the floor above into a 2-in.-
diam tube that is filled with water and sealed at the botton. The piezo-
electric crystal transmits a sonic pulse of 2.25 megacycle frequency
.
.. toward the outer tank shell and, in turn, receives the "echo." An echo
from the tank wall indicates the absence of any deflecting media, or rings,
at that position in the tank. The absence of the echo indicates an inter-
ference due to rings in the beam pafh. The transducer can be accurately
positioned and rotated to cover the entire depth and circumference of
the tank. Before the rings were added, the echo intensity was measured
at 200 locations in each tank. The volume of glass in each tank 18
measured by draining the uranium solution and filling the tank with a
known volume of water.
Chemical stability of the boron in the glass is an additional concern.
It is conceivable, although highly improbable, that under certain ideal
chemical conditions and over a period of years the boron could be leached
from the glass into the solution. The presence of boron in the glass is
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determined at intervals by withdrawing glass samples, which were in-
stalled in a perforated pipe on a stainless-steel stringer, and
submitting them for boron analysis. Since the tanks are unit-shielded
with 4 in. of lead, entrance into the area is permitted.
The array of tanks is shown in Fig. 4.
These tanks are connected
.
to a central vacuum pot that is located on the level above. Solution
transfers are performed by evacuating the pot with a steam exhauster
and opening the proper valve. Once in the vacuum pot, the solution may
be transferred to either of two solvent extraction feed adjustment tanks
or withdrawn for shipment. This vacuum pot is the only means for trans-
ferring solution into or out of the system. Valves that are kept locked
and require a key from the operating supervisor provide an additional
safety feature to prevent the transfer of an excessive amount of material
into an unsafe tank.
PROCESSING FACILITIES
..
Processing facilities in the ORNL 2380 Center consist of equipment
for dissolving uranium-bearing solids, and two different-sized solvent
extraction systems for purifying uranium solutions. This combination of
facilities provides sufficient flexibility to meet a wide range of pro-
duction requirements up to a maximum processing rate of 25' kg of 2380
per week. The facilities are described in more detaļl below.
Solids Dissolution
The original Thorex 500-gal batch dissolver was complemented by a
batch leacher (Fig. 5) that is similar to the one developed by the Power
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Reactor Fuel Processing Group at ORNL for leaching spent reactor fuels.”
The 2330 unit 18 designed to critically safe dimensions that permit
dissolution of uo, at a rate of 5 kg per day. Salient features of the
unit are the removable perforated basket, which permits leaching of fuel
from insoluble hulls or the dissolution of high-fired oxide chards with-
out fear of plugging the dissolver bottom, and the specially designed
draft tube, which will keep as much as 3 kg of fine oxide in suspension
until the dissolution 18 complete. The unit will dissolve 100 to 150 g
of vo, per liter; this solution can then be used as feed for either of the
solvent extraction systems, which will be described later.
SIN
***
.
Purification Systems
1
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The large Kilorod solvent extraction system is composed of an
extraction column. for separating 2384 from thorium, aluminum daughter
products, and fission products, and a stripping column for transferring
the 238u to the aqueous phase for concentration. Since this system has
previously been discussed in detail, emphasis here will be on criti-
cality control, which 18 of primary concern during operation of a
nongeometrically safe system at a throughput of 250 g of 4380 per hour.
The head-end vessels are large-diameter tanks in which criticality
is controlled both hy concentration (less than 10 8 of 2330 per liter of
solution) and by the use of thorium as a soluble poison. The thorium
concentration 18 maintained at a Th/U ratio of greater than 40. Transfer
of high-concentration solution into these tanks. is limited to 500 g per
batch, with a minimum agitation period of 15 min between batches, to
.
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ensure a homogenous mixture of uranium.
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The pulsed columns are 5-in. ID; this size ensures a safe geometry.
However, the organic-aqueous separators, or end sections, are 16-in. in
diameter. They are filled with borosilicate-glass Raschig rings, whose
presence 18 verified by annual x-ray inspection. The x-ray film clearly
show& the positions of the rings inside the stainless-steel containers.
All other vessels that contain uranium are also packed with rings; their
presence is verified either by this x-ray technique or by physical in-
LII
spection.
The large solvent extraction facility is capable of purifying “SU
at the rate of 25 kg per week, using nitrate solution for feed makeup.
Approximately 0.2% of the 2390 18 routinely lost, primarily to the
aqueous raffinate from the extraction colum.
The 258U product 18 concentrated to 200 g per liter for shipment.
· The only detectable contaminant in the product is thorium, which con-
stitutes approximately 1.5% of the product. Since thorium has not been
detrimental to the proposed uses to date, no attempt has been made to
reduce this concentration, although a simple anion-exchange column would
provide excellent separation.
Because of the high throughput and holdup of the existing solvent
extraction system and the increasing demand for gran quantities of "PU
for experimental purposes, a small solvent extraction system, directly
operated through gloves, was designed and constructed. The chemical
flowsheet (Fig. 6) utilizes uranium feed at a concentration of 100 g ...
per liter and an extractant of 30% tributyl phosphate in Adakane. The
pulsed columns are 3/4-in. ID with 48-in.-long active sections. The
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pulse plates are spaced 1/4-in. apart, and have 1/32-in.-diam holes to
give a 5% free area.
The system was designed to purify 2330 at a rate of 1.96 kg per day.
A 300-g batch can be completely processed, including feed makeup, column
operation, and product withdrawal, in 8 hr.
Product concentration is accomplished with a climbing-film type of
evaporator. This is an excellent apparatus for evaporating radioactive
liquids because of its small volume holdup per unit volume handled and
because of the ease of continuous operation. Such a unit, which is
capable of evaporating 300 kg/hr, has been successfully operated at the
Eurochemic, plant for more than three years. © Pepper 20 gives formulas
for the design calculations for small climbing-film evaporators. An
engineering flowsheet of the installed evaporator is shown in Fig. 7.
• This unit will concentrate solutions by a factor of 7. As in the case
of most evaporators, the overhead from the evaporator is used to steam-
strip the incoming feed. The unit operates at a steam pressure of. 22
psig and requires no controls except for the feed rate, which is con-
trolled by the density of the product. The evaporator is overdesigned
by 50% to reduce the lag between column shutdown and product withdrawal.
A photograph of the complete solvent extraction facility without
containment panels is shown in Fig. 8. The stripping column, uranium
évaporator, feed and product tanks, and pumps and pulsers are visible.
A photograph of the unit after enclosure is shown in Fig. 9.
The system will handle 233u that has a 2320 content as high as 40
ppm and has been stored as long as one year. The bottom section of the
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extraction column and the raffinate waste tanks are unit-shielded to
reduce radiation exposures to permissible levels.
PRODUCT HANDLING AND SHIPPING
The 2330 product is withdrawn into the vacuum pot shown in Fig. 4
and is then drained by gravity into a 3-liter bottle in an adjacent
glove box. The 4-in.-diam bottle is filled to 2.5 liters, giving a
maximum bottle content of 500 g of 2530.
The bottles are then placed in foam-glass shipping containers
(Fig. 10). These containers, consisting of a section of sched-80 pipe
mounted in foam glass inside a 50-gal drum, are approved by the AEC,
Bureau of Explosives, and the ORNI. Criticality Committee for commercial
shipment of up to 1 kg of 233u per container.
.
CONCLUSION
The ORNL 233u Center can receive aged 2330 in any solid form,
packaged in aluminum cans, provided that the form is compatible with
dissolution in nitric acid in stainless steel equipment. Solution can
be received in polyethylene bottles no larger than 4 in, in diameter
and 3 liters in capacity.
The current inventory of "U that is available through the AEC is
approximately 350 kg. The isotopic purity of this material varies from
91 to 98 wt%; the 2320 content varies from 3 to 250 ppm.
1.**..; consideration
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REFERENCES
b
.
1. E. D. ARNOLD, "Radiation Hazards of Recycled -SU-Thorium Fuels,"
Proceedings of the Thorium Fuel Cycle Symposium, Gatlinburg,
Tennessee, December 5-7, 1962. TID-7650.,.
-.
.
.
2. R. E. BROOKSBANK, J. P. NICHOLS, and A. L. LOTTS, "The Impact of.
Kilorod Operational Experience on the Design of Fabrication Plants
for 233U-Thorium Fuels," Proceedings of the Thorium Fuel Cycle
Symposium, Gatlinburg, Tennessee, May 3-6, 1966.
i
!
.
3.
C. C. HAWS, J. L. MATHERNE, F. W. MILES, and J. E. VAN CLEVE,
"Summary of the Kilorod Project - A Semi-Remote 10 kg/day Demon-
stration of 233002-Th02 Fuel Element Fabrication by the ORNL
Sol-Gel Vibratory Compaction Method," ORNL-3681, Oak Ridge National
Laboratory (1965).
4. 'J. T. THOMAS, Neutron Physics Division, Oak Ridge National Laboratory,
Personal Communication (June 29, 1967).
5. K. K. KLINDT, Inspection Engineering Department, Oak Ridge National
Laboratory, Personal Communication (1965).'..
6. M. E. WHATLEY et al., "'Unit Operations Monthly Progress Report,
17. January, 1964," ORNL-TM-798, Oak Ridge National Laboratory (1964).
7. A. M. ROM, "Design of a Critically Safe 4380. Batch Dissolver for
Building 3019," ORNL-4029, Oak Ridge National Laboratory (1966)...
223.
J. KLITGAARD, "Design of a Small Solvent Extraction Facility to
Purify 2330 Solutions," ORNL-CF-64-11-8, Oak Ridge National Labora-
tory (1964).
1.
9. J. KLITGAARD, L. GEENS, et al., "Experiments Carried out on the
Eurochemic Testing Station Climbing Film Evaporator," Eurochemic-TR-
160 (1964).
10. D. PEPPER, "The Design and Performance of Small Climbing Film
Evaporators," AERE CE/R 1779 (1965).
.
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Fig. 1. 233 U Receipts and Shipments, Bldg 3019 Dispensing Focility
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END

DATE FILMED
10 / 26 /67
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