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1 OF 1
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1944
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1.:25 14 46
MICROCOPY RESOLUTION TEST CHART
NATIONAL BUREAU OF STANDARDS - 1963
arsin D-194.4
CONF: 660305-4 137
PREPARATION OF MEGACURIE QUANTITIES OF CESIUM-137 SATIS
AND SOURCE COMPOUNDS AT OAK RIDGE NATIONAL LABORATORY***
MEC - OFFICIAL

R. E. Lewis and C. L. Ottinger
.:FED 2
.
Isotopes Development Center
Oak Ridge National Laboratory
Oak Ridge, Tennessee
.
RELEASED FOR ANNOUNCEMENT
IN NUCLEAR SCIENCE ABSTRACTS
.:::
ABSTRACT
:
.........
Processes used at the Fission Products Development Laboratory,
Oak Ridge National Laboratory, for recovery, purification, and !
... conversion of megacurie quantities of 1970s to salts and source.
compounds are reviewed with special emphasis on the conversion
of cesium alum to cesium carbonate by the cesium tetraoxalate
process. Subsequent conversion of cesium carbonate to source
compounds is discussed.
.
::.
.
..
INTRODUCTION
.... ..
Fission-product 137cs has been recovered and purified at Oak Ridge National
. . Laboratory since 1940 to provide gamma-ray sources IOI Teletherapy, raus
48 to provide gamma-ray sources for teletherapy, radiography, .
and irradiation units. The first large source was a teletherapy unit fabricated
•:*:; in 1954 which contained 1540 curies of 197Cs in the form of compacted Csci encap- ..
sulated in stainless steel. Within a few years, 10%Cs teletherapy sources were
... ;widely accepted by medical facilities and there was a demand for sources contain-
ing 1000 to 3000 curies. The number of teletherapy sources prepared annually at
ORNL has increased to about 25; in addition ORNL also sells considerable quanti-
ties of 137Cs to private firms who fabricate teletherapy and radiography sources.
ini
::
.
.
.
.
In the past three years, the increased supply of purified 137Cs and reduction in
price (presently $0.125/curie in quantities >200,000 curies) has made 137Cs more
attractive for industrial-scale irradiators.1,2 Two large sources recently pre-
pared that are of special significance are a 200,000-curie 137CsCl source, in .
rectangular wafers (Fig. 1), for the Radiation Laboratory,
Brookhaven National Laboratory, and a 176,000-curie source for Saint-Gobain
Techniques Nouvelles, Seine, France. Inquiries from a number of irradiation
facilities have indicated current interest in sources of 100,000 to 300,000, curies
of 237Cs and long-range plans for even larger quantities in the range of 0:4 to
1.0 megacurie of 137Cs. Cesium-137 and its daughter, 137Ba, decay by beta and
gamma emission to yield 4.8 watts thermal power per 1000 curies, which makes it
potentially useful as a heat source.
.
.
.............
..
.
..
....
...
. *Research sponsored by the U. S. Atomic Energy Commission vnder contract
with the Union Carbide Corporation.
LEGAL NOTICE
:::... ..
This roport mo prepared us in account of Government sponsored work. Neither the United
States, nor the Commission, nor any person aoting on behall of the Commission:
A. Makes may warranty or representation, expressed or implied, with respect to the noor-
racy, completeness, or undtalsen of the information contained in this report, or that the who
I of any information, apparatus, mathod, or procesi dielowed la the report may not lattage
privately owned restes or
B. Asnim any labuuang with respect to the une of, or for damage results from the
un of any information, apparte, method, or procul dulowed in this report.
As wood in the above, "por og nothing on behalf of the Commission" motud may a.
ploys or contractor of the Comminaton, or employw of soh contractor, to the entent that
such employu or contrnotor of the Commission, or amployu at nok contrmotor preporu,
dienominatas, or provides noomse to, may taformation purminnt to wo employment or contrast
with the Commission, or Me employment with such contrmotor,
ORNL - AEC - OFFICIAL
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Fig. 1. 70,000 Curies of 1370s as Square Wafers (Radiation Source). .
ORNI - AEC - OFFICIAL
Prior to 1961, fission products were first recovered from waste solutions gen-
erated by pilot plant processing of irradiated uranium at ORNL and from liquid
waste shipped to ORNL.? In order to meet the growing demand for 137Cs, a tech-
nique was developed for selective sorption of 13Cs on an inorganic ion
(Decalso) from the supernatant of neutralized fission-product wastes. Shipment.
of crude 15%Cs concentrated from waste tanks located at Hanford was begun in
1961. Purification of the crude 137Cs and conversion to compounds useful as
radiation or heat sources are accomplished at ORNL in the Fission Products
Development Laboratory (FPDL) at a rate of 1.0 megacurie/year.
ONNI - AEC - OFFICIAL
DISCUSSION
... Recovery of Cesium-137 From Fission-Product Wastes by Decalso Process
.
In recovery of 137Cs by the Decalso process, 3,4 neutralized Hanford Purex Super-
mi natant 103A, with a sodium ion concentration of 5 to 7 M, is passed through a
radiation-shielded tank containing 400 gal of 20-30 mesh Decalso at 25° C until
.. the cesium begins to break through or when -50,000 curies of 157Cs has been: :
sorbed. The beds are then covered with water and the casks (Fig. 2) are sea).ed.
The casks are loaded, two to a modified gondola car (Fig. 3), and shipped from
Hanford to ORNL. "At ORNL, more than 97% of the 137Cs is eluted from the Decalso
::.. beds at FPDL with 1000-1200 gal of 5 M NH4NO3 at 80°C at a f.low rate of 4 gal/min.
The eluant is stored in underground tanks, which have storage capacity for as
Cs. The ion-exchange beds are rinsed and returned
to Hanford, in the ammonium form, to be reloaded with cesium. The original",
Decalso beds placed in the shipping casks in 1961 are still being used after.
twelve loading and elution cycles and have shown no loss of selectivity for:
: sorbing cesium. .
i
i
: The. 137Cs processing rate in the FPDL is dependent primarily on the shipping
schedule for the feed. Four shipping casks are presently in use. Each 400-gal
Decalso bed will transport 50,000. curies; and with a chipping cycle of eight weeks
per four STT's, the 137Cs processing rate is about one megacurie of 137Cs per
year. In the period from April 1961 to January 1965, over 2.5 megacuries of
1970s has been processed at ORNL.
..
..
.
Purification of Cesium-137 by Alum Process
....
....
...
The alum process5-12 is based on the isomorphous cocrystallization of small amounts
of cesium with large amounts of ammonium alum. The concentration of ammonium alum
in solution also decreases the cesium alum solubility, resulting in high 187Cs
recovery. After collecting the cesium in the ammonium alum beds, the more soluble
ved by a heating and cooling cycle to effect fractional crystalli-
zation of the alums. After three to five such cycles, and removal of the aqueous.
phase each time, the more insoluble cesium alum is obtained in a relatively pure
of other alums and other fission products. Cesium losses recycled
from subsequent processing steps are also collected by the alum process for re-
processing. This multiple use of the alum process makes it the key process in the i
FPDL 1,37Cs integrated process (Fig. 4).
...
The 5.M NH4NO3 eluant resulting from the elution of the 1970s from the Decalso
beds is diluted to 2.5 M NH4NO3 and the 2,500-curie, batch of 137Cs is then trans-
ferred to a vessel containing an ammonium alur bed. Cesium-137 is then collected
ORNL - AEC - OFFICIAL .
1
.
..
.
.
.
.
.
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Fig. 3. Gondola Cars for Transporting Shipping Casks (STT)
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OINE - AEC - OFFICIAL

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11!510 - DIV-INUO
ORNL-OWO 3-10!
H2O RINSE.

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5M NHA NO3
ELUTION OF
0.05 MEGACURIE
CS FROM DECALSO
FEED STORAGE
0.2 MEGACURIE 137CS
IN NH, NO, SOLUTION
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RINSE MgO STORAGE
BATCH FEED MAKEUP
0.0025 MEGACURIE 137CS
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FRACTIONAL CRYSTALLIZATION
' TO REMOVE NHAT, RD*
FILTRATE WICK
SCAVENGE ON
NH. * ALUM
FILTRATE
TO WASTE
17CS NHALUM RECYCLE
(~2% HICS)
i
37CS ALUM
137CS OXALATE DISSOLVED IN H20.
BATCH CRYSTALLIZATION
OF 18°C OXALATE
0.05 MEGACURIE ..
137CS ALUM ACCUMULATION
0.2 MEGACURIE
OXALIC
ACID
CRYSTALLIZATION OF
137CS OXALATE
1 005M NHL
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FILTRATE RECYCLE
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CALCINATION OF
137CS OXALATE TO
137CS CARBONATE
H20, 002. TO HOT OFF-GAS
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Cscos.
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TO HOT OFF-GAS
Te
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HC-
137CS CONVERSION TO
. 137CS CHLORIDE
EVAPORATION TO DRYNESS
137CS CONVERSION TO
137CS -GLASS
MELTED AT 1200°C
-.-.-i
........
-
.
.
,
UL
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137. CI TO
SOURCE FABRICATION
15168-GLASS
TO SOVACE FABRICATION ..::
:
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Fig. 4. FPDL 137Cs Processing Flow Diagram. ::
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. on the ammonium alum beds by a heating and cooling procedure. The solution
1. remaining from this crystallization is transferred to a second vessel also con-
taining ammonium aium, and the same process repeated two times to effect recov- .
ery of >98% of the 137Cs. Subsequent batches of 2,500 curies of 137Cs are
transferred to the alum crystallizers and the process is repeated..
When ~50,000 curies of 137Cs has been collected on the alum beds (about one ·
week's operation at FPDL), water is added to the mixed alums and the more soluble
!' : ammonium and fission-product rubidium alums, as well as traces of fission prod - ..
.. ucts, are removed by several fractional crystallizations. The more insoluble
cesium alum is then transferred to an accumulation vessel. The alum cocrystal-
.lization and fractional crystallization process is repeated until ~200,000 curies
of 137Cs has been accumulated. It is then converted to cesium tetráoxalate by
à subsequent process (Fig. 4).
.......
.
.
".....
.
.
Conversion of Cesium-137 Alum to Source Compounds by Cesium Tetraoxalate Process
. .
.
.
Various processes have been used at FPDL to convert cesium alum to other cesium
compounds. In one of the early ORNL procedures, ammonium hydroxide was added
to the alum to form aluminium hydroxide, ammonium sulfate, and cesium sulfate.
After the insoluble aluminum hydroxide had been filtered off, the cesium sulfate
solution was heated with HNO3 to oxidize the residual NH4*. Hydrochloric acid
was added to remove the HNO3 and the Cs2S04 solution was passed through a . .
: hydroxide-form anion-exchange column to remove the sulfate ion. The resulting :
cesium hydroxide was neutralized with HCl and evaporated to prepare Csci crystals.
. .
..
.
.
,,.
il
is
.
.
In a later process, 8 cesium alum was converted to cesium chloroplatinate which
was recovered and then converted by an aqueous solution of hydrazine hydrate to
platinum metal, cesium chloride, and ammonium chloride. The platinum metal was
.. removed by filtration, nitric acid was added, and the solution was heated to
3. oxidize the ammonium ion. Hydrochloric acid was then added and the solution heated
: : to remove the excess HNO3; the cesium chloride was evaporated to recover the CsCl.
Because of the necessity of handling relatively large quantities of HCl and HNO3
.. and the time required for evaporating the acids and recovering the platinum,
this method has been replaced by the cesium tetraoxalate process.18
.
..
The advantages of the tetraoxalate process are the easy separation of the cesium
from aluminum, simple calcination of the tetraoxalate to cesium carbonate, and
the ready conversion of the carbonate to usable end-products. The process is
amenable to large-scale processing of fission cesium and the soluble fraction
of cesium is recycled to the preceding alum process to effect high recoveries
of product.
:
.
.:
Cesium tetraoxalate, CsHa(C204)2:2H20, can be crystallized from simple salt solu-
tions such as those occurring in solvent extraction raffinates or from the
:cesium alum procesis. The solubility of cesium tetraoxalate in water and 1.0 M
oxalic acid solution at various temperatures is shown in Table 1. Laboratory
studies show that cesium is crystallized as cesium tetraoxalate from cesium
alum oxalic acid solution, witir little coprecipitation of Al(III) at cesium
concentrations of <20 g cesium per liter (Table 2). It was found that the addi-
tion of small amounts of NHa* ion increased the yield of cesium tetraoxalate and
decreased the percentage of the aluminum that coprecipitated (Table 3).
ORNL - AEC - OFFICIAL
.
....
.
.....
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.
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:...
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.
irijisso - DIV-INIO
Water
Table 1. . Effect of Temperature on Solubility of Cesium
Tetraoxalate in Water and in 1.0 M Oxalic Acid Solution
Temperature, : CsHg(C204)2•2H20 solubility, g/liter
1.0 M Oxalic acid
2.65
8.8
4.60
13.0
: 5.00
11.7
40.0
67.5
61.6
117.0
83.2
22.6
30.8
AGRO
Table 2. Effect of Cesium Alum Concentration on Cocrystallization
of Aluminum Oxalate with Cesium Tetraoxalate ..
(Temperature 14°C; 1 hr stirring) :
Initial cesium Cesium. Al carried, 4 Initial oxalic
concentration, crystallized, of initial Al acid concentration,
g/liter
:: in solution
M :
10
<1.0
1.0
1.0:
1.1.
15
20
2.1
i
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WOO90 g
5.2
22.0
.1.2
.
35.0
72.0
83.0
1.25
1.5
1.8
2.9
:00
.
.
Table 3. Effect of Ammonium Ion on Crystallization of Cesium
Tetraoxalate from Cesium Alum and Oxalic Acid Solution
(Temperature 14°C; 1 hr stirring;
1.25 M oxalic acid; cooling rate 1°C/min)
Cesium
Cesium Al carried, %
concentration, concentration, crystallized, of initial 'AL
g/liter
in solution
NH+.
..
....
20
0.0
0.05
0.0
0.05
2.5
0.1
5.2
0.2
ORNL - AEC - OFFICIAL :
- -
.
-
.....
.
•
i "
i
.
In the 137Cs. processing ac FPDI, the cesium alum is converted to cesium tetra-
.. oxalate after 200,000 curies of pure cesium alum has been accumulated by
crystallization in a 400-liter volume of 1.2 to 1.25 M oxalic acid, 0.05
.. and 15 to 25 g of cesium per liter. The first crystallization is not necessary
i for purification but is very useful in the transfer of 157Cs from the cesium
alum crystallizers and aids in getting representative samples of the solution
for radiochemical analysis. The cesium tetraoxalate is dissolve
transferred in 50,000-curie butches to a 100-liter vessel.
ORNE - AEC - OFFICIAL
..
-
:
The second crystallization is made in the 100-liter vessel from 1.1 to 1.C M
oxalic acid. The solution is cooled to 25°C at a rate of 1°C/min. The cooling
rate is halted at 25°C for 15 min and then cooled to 14-16°C at a rate of 0.5°C/min.
.: Yields of cesium tetraoxalate are 70% on the first crystallization and 929 a the.
.:: second crystallization. The increased yield on the second crystallization is due
primarily to the lower concentration of aluminum ions.
.
:.
The soluble cesium in the supernatant fraction is recycled to the alum system
... · for recovery as cesium alum. The integrated cesium process used at FPDL is :.
shown in Fig. 4,
Preparation of Cesium Carbonate from Cesium Tetraoxalate
.
Cesium carbonate is easily prepared by heating cesium tetraoxalate to a suffi- .
ciently high temperature to volatilize excess oxalic acid and water and decompose
the oxalate. to carbonate and carbon monoxide. The calcination is endothermic
..and there is no danger of uncontrolled burning.
In laboratory studies of the calcination, cesium tetraoxalate was heated for :
different times and temperatures in a shallow nickel tray in a muffle furnace
with an air stream passing through. The resulting compounds were assayed for
drogen ion, oxalate, and carbonate. From these studies,
the reactions in different temperature ranges were determined to be:
CsH (C204)2.2H20 105-120°C> CsH (C204)2 + 2H2O
..
..
.
.
CsH3(C204)2 -120-200°C > CsHC204 + H2C204
2CSHC204 200-300°C-> Cs2C204 + H2C204
Cs2C204 300-450°C, Mixture of Cs2003,
Cs20, co, and co2
Cs2003 - 3450°C-> Cs20 + CO2
..
.::.
When cesium tetraoxalate is heated to 100°C, the crystals melt. Continued heat-
ing at 120°C sublimes the excess oxalic acid, leaving cesium acid oxalate, CsHC204.
The conversion of CsHC204 to Cs2003 is complete after 2 hr at 300°C. This pro-
cedure is used to convert fission-product cesium tetraoxalate to cesium carbonate.
The cesium compounds prepared from cesium tetraoxalate are low in Al2O3 and Fezos
since oxalic acid complexes both aluminum and ferric iron and keeps these ions in
solution. Trace amounts of iron and aluminum (~0.mg/g cesium tetraoxalate)
that do cocrystallize with the cesium tetraoxalate are converted to the insoluble
oxides at 300°C and are removed by filtration of the dissolved cesium carbonate
· ORNL - AEC - OFFICIAL
10
solution prior to making other cesium compounds. Carbon, which also forms from
the calcination of ammonium tetraoxalate, is also removed by the filtration. .
The resulting cesium carbonate solution contains no detectable alkaline earth,
trivalent metal ions, or armonium ions.
.
..
Preparation of Cesium Source Compounds from Cesium Carbonate
...
Cesium carbonate is used to prepare a variety of source compounds. Cesium chlo.
ride is the primary form for radiation sources, but other salts or compounds can
be prepared for heat sources or special application.
IL
Dry powdered 137Csci is prepared in 50,000-curie batches by reacting the filtered
Csacos solution with a slight excess of hydrochloric acid. 12-14 The 137Csci
solution is again filtered, and the filtrate is evaporated in tantalum equipment
to yield the dry salt. The powder is baked with constant stirring at 300°C for
4 hr to remove the last traces of HCl; it is then stored in lots of 10,000 curies
in stainless steel cans in water-cooled storage wells. The cesium chloride has
an activity concentration of 125 curies 137Cs per gram CsCl, as measured by
calorimetric methods;16,17 this varies slightly due to differences in the 18708
isotopic concentration. : :
The cesium chloride is pressed 18 into a variety of sizes and shapes such as right :
cylinders, square wafers (Fig. 1), or segments of a ring, and then hermetically
.. sealed in Type 316 LC stainless steel capsules by fusion welding techniques. 18,2
-- Long-term compatibility studies I have shown fission-product cesium chloride is
compatible with Type 316 stainless steel capsules.
.
Cesium sulfate is prepared by adding a stoichiometric amount of dilute sulfuric
acid to the cesium carbonate solution and evaporating to near dryness. An equal
volume of ethyl alcohol is added to the concentrate to decrease the solubility
of the cesium sulfate, and the crystals are filtered from the solution and dried.
This procedure is better than the procedure of evaporating acid cesium sulfate
solutions to dryness because the cesium sulfate prepared from cesium carbonate
does not contain CSHSO4, which is highly corrosive. ..
Several types of cesium glasses23,24 containing 40-45% cesium have been prepared
from cesium carbonate. About 100,000 curies of 157Cs gla
but experience has shown that fabrication of cesium glass as small rods or
special shapes is very difficult. Cesium glass in the form of right cylinders
for use as a heat source25 was prepared (Fig. 5).
.
NL - AEC - OFFICIAL
ORNI MAEC - OFFICIAL
ORNL - AEC - OFFICIAL:::...

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Fig. 5. 28,000 Curies of 137Cs Borosilicate Glass for Use as Heat Source.
..
..12
..
.
REFERENCES
1. Food irradiation, Section III, Isotopes and Radiation Technology 3(1): 0
30-48 (1965).
ORNI - AEC - OFFICIAL
I
.
2. Process radiation development, Section IV, Isotopes and Radiation Technology
3(1): 49-66 (1965).
3. R. E. Lewis, T. A. Butler, and E. Lamb, Recovery of 137Cs from fission-product
wastes and transport by an aluminosilicate ion exchanger, USAEC Rpt. ORNI
3765, Oak Ridge National Laboratory (May 1965).
R. E. Lewis, T. A. Butler, and E. Lamb, An aluminosilicate ion exchanger fo
recovery and transport of 157Cs from fission-product wastes, Nucl. Sci. Eng.
(in press).
1
.
:: 5. S. J. Rimshaw, Recovery of cesium values with anmonium alum, U. S. Patent
1 2,925,323 (February 1960).
6. S. J. Rimshaw, Decontamination of fission product wastes, with separation of
kilocurie quantities of cesium, strontium, rare earth, and ruthenium, USAEC
Rpt. TID-7517, p. 303 (1956).
7. A. F. Rupp, Large-scale production of radioisotopes, Proc. Intern. Conf.
Peaceful Uses At. Energy, 1956, Geneva 14: 68-84, UN, New York. ...
::
Peaceful
1.8. E. Lamb, H. E. Seagren,' and E. E. Beauchamp, Fission-product pilot plant and
other developments in the radioisotopes program at the Oak Ridge National
Laboratory, Proc. 2nd UN Intern. Conf. Peaceful Uses At. Energy, 1958, Geneva
20:. 38-44, UN, New York.
9. A. F. Rupp, Fission product processing, USAEC Rpt. IDO-14363, pp. 777-99
:: (April 1956).
10. A. F. Rupp, Progress in Nuclear Energy Series III, Process Chemistry, vol. I,
Pergamon Press, 1956, pp. 345-55.
T.' A. Butler, E. Lamb, and A. F. Rupp, New processing techniques for radioiso-
topes at Oak Ridge National Laboratory, Radioisotopes in the Physical Sciences
and Industry, vol. II, p. 407, International Atomic Energy f.gency, Vienna, 1962.
12. C. L. Ottinger, Isotope production and development, Isotopes and Radiation
Technology. 1: 35-43 (1963).
13. R. E. Lewis, . Method for conversion of cesium alum to radiation source mate-
... rial, U. S. Patent 3, 124,538 (March 10, 1964) and Canadian Patent 710,349
(May 25, 1965). :
N
.
14. R. E. Lewis, Development and use of a process for crystallization of cesium
tetraoxalate: An intermediate for preparing 137Cs source compounds, USAEC
... Rpt. ORNL-3667, Oak Ridge National Laboratory (1964).
7.
VIDL140 - 534-100
a
..
i
.
'.
.15., J. H. Gillette - Ingrid B. Lane, comp., Review of radioisotopes, USAEC Rpt.
.. .ORNL-3802, Oak Ridge National Laboratory (May 1965).
.
OFFICIAL
.
16.
J. C. Posey, T. A. Butler, and P. S. Baker, Hot-cell calorimetry for routine
determination of thernal power generated by kilocurie sources, Proc. loth
Conf. on Hot Laboratory and Equipment, pp. 263-8 (1962).
J. C. Posey, Calorimetry in measuring radioactivity, Isotopes and Radiation
Technology 1(1): 92-6 (1963).
ii.,
•
J. A. Jones, Fabrication of 1970s sources, USAEC Rpt. OF
National Laboratory (September 1964).
1
.
19. , E. E. Pierce, Remote welding of stainless steel capsules, USAEC Rpt. ORNL-
2280, Oak Ridge National Laboratory (March 22, 1957).
20. B. F. Early, private communication, Oak Ridge National Laboratory (December
1965).
w
r.
21. K. W. Haff, Examination of a nine-year-old 137CsCl source capsule, USAEC .
Rpt. ORNL-TM-584, Oak Ridge National Laboratory (August 5, 1953).
22. B. F. Warner, Fabrication de sources 1870s, d'un kilocurie, Energie Nucleaire
1: 161-71 (1957).
mo
C. Quinby, Method of preparing radioactive cesium sources., U. S. Patent
3, 114,716 (December 17, 1963).
24. R. E. Lewis, Source development, Isotopes and Radiation Technology 1(1): '.
84-8 (1963).
25.
C. L. Ottinger, E. E. Pierce, and R. W. Schaich,. Preparation of a cesium
(137Cs) borosilicate glass power source, USAEC Rpt. ORNL-3669, Oak Ridge
National Laboratory (April 1965).
Sien
.:.
ODNI Dericia.
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