used in earlier work in this Jaboratory.1l/ Its medium was a cellophane

dialysis membrane previously found to have a pore size of 12 to 40 A,

One thickness of cellophane at a pressure of 400 psig (under nitrogen)
gave a flow rate of 3.5 to 4.0 mli/hr. After the whole supernatant aliquot, had passed the filter, a garma counting aliquot of the effluent

was taken.

Upon disassembly of the ultrefilter, the membrane was counted

to determine the gamma activity in the collcidal fraction.

The solid fraction separeted by centrifugation was transferred

quantitatively to a weighed fritted glass filter using anhydrous methanol
and after drying the filter was weighed again. Then the solid on the

filter was dissoived with 6N-HCl and washed through.

After several

washings, the combined filtrates were transferred to a 100-n1l volumetric
flask and made un to volume. An eliquot of this dissolved solid frace
tion was taken from this solution for gamma counting.
Thus, for each sample five gemma counts were taken, (1) original

slurry, (2) supernatant, (3) ultrafiltrate, (4) colloidal fraction, and

(5) solid fraction, This procedure allowed the calculation of an activity
balance for the two separation steps. The last. three counts gave the
breakdown of the gamma activity into fonic, colloidal, and solid fractions,
These samples were also used to follow the gamma decay of the fractions
for all the shots. For the fractions of the samples from Shots 1 and 2

lead absorption date were taken; for the fractions of the samples from
Shots 2,3, and 4 ganma analyzer data were taken. Finally, portions of

the fracticns of samples from Shots 2,3, and 4 were returned to USNRDL
for quantitative analysis of their mejor and minor constituents,

3.2.2

Resulis

The results of these studies are siven in the following sections.

302e2.1

Gamma Activily Distribution Among Physical State Fractions
In general, gooc activity balances were obtained for the sera-

ration steps.

The sum of the total gcmma counts of the liquid (super-

natant) and the solic fractions was 94 to 103 per cent of the total

gemma count for all samples, except one, as determined by the assay of
the original sample. Similarly, recoveries in the ultrefiltration step
(sun of collcidal and ultrafiltered fractions) ran about &6 to 96 per
cent of the total liquid activity.

Totals were normalized to 100 per cent

by taking account of the known sources of loss. In the solid~liquid
separation the main source of loss was in the transfer of the solid to
the frit and in the residue left on the frit after the acid wash. In
the ultrafiltration separation the main source of loss was in adsorption
on the metal surfaces of the ultrafilter below the membrane. Separate
experimente showed that the extent ofthese losses was sufficient to

account for an occasional low recovery. Tables 3.5 and 3.6 summarize
the gamma activity fractionation results together with pH values and
percentage of solids by weight. Table 3.5 gives the results for the
individual samples while Table 3,6 gives ranves of values for all semples
analyzed in each shot, and grouns these results by type of shot. Sone
pertinent observations based on Table 3.€ are:

34

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