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ANP PROJECT QUARTERLY PROGRESS REPORT
15 e ANALYTICAL STUDIES OF REACTOR MATERIALS
C. D. Susano
Analytical Chemistry Division
C. R. Baldock
Stable Isotope Research and Production Division
An empirical volumetric method for
the determination of zirconium in
reactor fuels has been developed. The
method is based on the measurement of
the basicity produced by the reaction
between zirconium hydroxide and excess
p o t a s s i u m f 1 u o r i d e . An i n d i r e c t
volumetric method for the determination
of zirconium, which depends oc
precipitating zirconium as the slightly
soluble benzoate or m-nitrobenzoate
and subsequently determining the
organic acid by titration, proved
unsatisfactory because of the variable
composition of the precipitate. Attempts
to determine zirconiuni by
titrating zirconium m-nitrobenzoate in
nonaqueous media with perchloric acid
were not successful. The use of
mandelic acid as a precipitant for
zirconium in the presence of a large
excess of uranium was shown to be
superior to phenyl ar sonic acid,
m-nitrobenzoic acid, and cinnamic
acid.
The stability of the chromium
comp 1 ex with diphenyl c arb az i d e was
increased by development of the complex
in 0.2 N perchloric acid. The separation
of traces of aluminum in reactor
fuels by means of anionic-exchange
resins was studied; preliminary results
indicate that this technique is feasible.
A billiography of recent literature
on bromine trifluoride as a
reagent for the determinationof oxygen
in metallic oxides has been started.
An improved apparatus for the deterniination
of trace amounts of water in
solids was designed and fabricated for
measuring the electrical conductivity
of anhydrous hydrogen fluoride to
determine its water concentration.
190
J. M. Warde
Metallurgy Division
In addition to the chemical analy-
ses, various compounds of interest
were examined by spectrographic or
petrographic techniques . The useful -
ness of the spectrograph has been
enhanced by the construction of a
source that is good for temperatures
approaching 2850°C. The petrographic
studies have led to the classification
of many complex compounds that are not
found in the literature.
‘[he work of the ANP Analytical
Laboratory service group consisted
chiefly of analyses of beryllium- and
zj rconium-bearing fluoride mixtures.
A review of the methods used and a
summary of the services performed are
included.
CHEMICAL ANALYSIS OF REACTOR FUELS
J. C. White J. E. Lee, Jr.
C. M. Boyd W. J. Ross
C. K. Talbott
Analytic a1 Chemistry Division
The research and developmental work
on methods for the analysis of reactor
fuels and their components has been
of a diversified nature during this
quarter. The pr iniary interest has
been in the development of a volumetric
method for the determination of zir-
conium. Other problems that have been
studied include: the colorimetric
determination of chromium; the de-
termination of oxygen in metallic
oxides; the separation and determina-
tion of traces of aluminum in reactor
fuels; the determination of water in
components of reactor fuels; the
design of apparatus that w i l l permit
the measurement of the conductivity
of liquid hydrofluoric acid so that