Chemical Processing Department Monthly Report: April 1964 Page: 38 of 53
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-1 W-82089
cell. Both calibrations were accurate to plus or minus 1.0 per cent.
Analysis for NH3 in H-,drazine
An analysis was developed for ammonia in 35 per cent hydrazine solu-
tions. Hydrazine was first oxidized by bromination in an acid system.
The residual ammonia was then determined by oxidation with hypobromite
formed on making the sample basic. Standard recoveries were 100 plus
or minus 2 per cent.
Atomic Absorption
The Jarrell-Ash absorption photometer was used during the month to
determine detection limits for iron, gallium, and aluminum. The
instrument has been used as both an absorption unit and as an
emission unit. With a stoichiometric mixture of 02 and H2 as fuel, the
instrument sometimes performs better as an emission unit than it does
for absorption, i.e., a detection limit of 3 ug/ml versus .025 ug/ml
for gallium. The "OH" lines may be the reason for interference with
gallium. No work has been done as yet using the oxygen-acetylene
flame, which will probably be a superior flame for aluminum as well
as gallium.
5. Plutonium Chemistry Laboratory
a. Electrorefining Plutonium Metal
The formation of unconsolidated plutonium metal product continues to
be the major difficulty. Chlorine was substituted for hydrogen
chloride as a sparge gas with little or no improvement.
Changing the approach to this problem from improvement of consoli-
dation to prevention of finely divided product formation has produced
fruitful results. Experiments were conducted at a temperature below
the melting point of plutonium metal so that the cathode product
would be trapped at the cathode. This produced a large black mass
at the cathode within 3 - 5 minutes. This seemed to add further
emphasis to previous observations that the phenomenon is a cathodic
process.
The one cathode variable that can be readily studied is current
density. Reducing this from the usual 3-5 amps/cm2 as used in
electrowinning to about 0.4 amps/cm2 produced no unconsolidated
product and an anode efficiency of 90 per cent.
b. Ion Exchange Resin Stability
Preliminary ignition tests on Dowex 50Wx8 cation resin have shown
no appreciable hazard. Sample treatments included (1) loading with
americium, (2) washing with 7 M HN03, (3) contacting for 90 hours
with 7 M HNO, (4) contacting with DBBP-CCl4 or (5) as-received.
No explosion or reaction other than charring occurred up to
temperatures of 2000 to 2150 C. Removal of surface moisture started
N~ eplsin r eatin thr ha carin ocure u t
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Hanford Atomic Products Operation. Chemical Processing Department. Chemical Processing Department Monthly Report: April 1964, report, May 22, 1964; Richland, Washington. (https://digital.library.unt.edu/ark:/67531/metadc1310867/m1/38/: accessed April 16, 2024), University of North Texas Libraries, UNT Digital Library, https://digital.library.unt.edu; crediting UNT Libraries Government Documents Department.