ORNL-1771 - Oak Ridge National Laboratory

zirconium or aluminum complex, or lake, is also
being investigated. In this method, the solution of
fluoride is titrated with a colored zirconium com-
plex, and the change in absorbance of the solution
is plotted as a function of the concentration of
zirconium in the complex. Zirconium alizarin
sulfonate and zirconium eriochrome cyanine both
react rapidly with fluoride ion and will receive
further study. Preliminary results indicute that the
reactions of these compounds with the fluoride ion
are reproducible. A simple titration cell is being
designed.
Oil Contamination in ARE Helium
G. Goldberg
Analytical Chemistry Division
The contamination of the helium for the ARE with
oil from valves and fittings was checked befare the
gas at the site was used. The method used for
these tests was to pass the gas through dual
scrubbing towers contain in g petroleum ether and
then to evaporate the ether to dryness and weigh
the residue. In the initial test on a tank car of
helium, 360 pg/ft3 was found. A tower containing
70 in., of charcoal was placed in the gas line, but
it had little effect in eliminating the oil. Further
tests on the same tank car showed that bleeding the
I ine before samples were taken markedly lowered
the contamination level. For example, in three
successive samples of 15.5 ft3 of gas eech, the
contamination decreased from 100 to 10 pg/ft3.
These tests indicate that bleeding the line with
50 to 100 ft3 of gas before the equipment is coupled
into the system will effectively remove oil from
fittings and valves.
PETROGRAPHIC INVESTIGATIONS OF
FLUORIDE FUEL
G. D. White, Metallurgy Division
T. N. McVay, Consultant
Petrographic studies of UF, in alkali-metal fluo-
ride systems have shown that two phases exist in
the KF-UF, system. One is red and is near
3KF*UF,, and the other is blue and is near KF-UF,.
Only one binary phase is present in the NaF-UF,
system, and it is probably 3NaF.2UF3. Lithium
fluoride has not been found to combine with UF,
in either the binary system LiF-UF,, in the ternary
154
systems LiF-KF-UF, or LiF-NaF-UF,, ar in the
quarternary system Li F-NaF-KF-UF,. Cesium
fluoride was found to form a complex with UF,,
with a composition near ~CSF-UF,. Some work was
done on the systems LiF-ZnF, and NaF-CsF, and
no binary Compounds were found,
Part of a loop in which NaF-ZrF,-UF, (50-46-4
mole %) had been circulated was received from
Rattelle Memorial Institute, Samples tuken from the
wall contained about 50% ZrO,, and the balance
was an NaF-ZrF, (53-47 mole 76) coinpound. In
addition, several loops containing NaF and ZrF,
with reduced UF, have been examined, and no
appreciable oxidation of the UF, could be found.
SUMMARY OF SERVICE ANALYSES
J. C. White W. F. Vaughan
C. R. Williams
Analytical Chemistry Division
Most of the samples received during the past
quarter were from NaZrF,- and NaF-KF-Li F-base
materials. Other types of samples that were
analyzed included silver fluoride, chromium fluo-
rides, iron fluorides, beryllium, sodium, and
rubidium metals, Inconel, end alkali-metal car-
bonates. A revised procedure was established to
determine UF, and lJF, in NaF-KF-LiF-base fuels.
Also, the method of White, Ross, and Rowon” was
adapted successfully to the determination of oxygen
and metallic impurities in rubidium metal.
A total of 1,165 samples, involving 10,702 de-
terminations, was analyzed. A breakdown of the
work is given in Table 10.1.
15J. C. White, W. J. Ross, and R. Rowan, Jr., Anal.
Cbem. 26, 210 (1954).
TABLE 10.1. SUMMARY OF SERVICE
ANALYSESREPORTED
Number of Number of
Samples Determinations
Reactor Chemistry 679 6,694
Fuel Production 38 395
Experimental Engineering 379 3,406
Miseel Ioneou s
69
...__
207
1,165 10,702