THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org
THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org
THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org
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Notes<br />
7.<br />
8.<br />
9.<br />
10.<br />
11.<br />
12.<br />
13.<br />
(a)<br />
(b)<br />
(c)<br />
(d)<br />
(e)<br />
(f)<br />
(!3)<br />
(h)<br />
(i)<br />
(j)<br />
(k)<br />
(1)<br />
Allow the solution from (5) to drain down to the top of the<br />
chromatographic column maintaining a flow rate of approximately<br />
0.5 ml/min. Add 40 ml 8 ~ HN03 and allow to drain through the<br />
column at the same rate.<br />
Transfer the eluted solution to a 100-ml separating funnel and wash<br />
with 10 ml conditioned CC14, repeat the wash with two further<br />
portions of 10-ml CC14.<br />
Transfer the washed solution to the 50-ml beaker and evaporate to<br />
dryness in a fume cupboard. Note (m).<br />
Redissolve the residue in 1 ml 6 M HC1 while the beaker is still<br />
—<br />
warm.<br />
Duplicate reagent blanks are prepared using the procedure and re-<br />
agents above, but omitting the Pu.<br />
Prepare the electrodes for sparking by pipetting 0.1 ml of the solution<br />
from (10) on to the tops of a pair of waterproofed graphite electrodes,<br />
dividing the aliquot equally between the two electrodes, and dry under<br />
an infrared lamp. Prepare duplicate pairs of electrodes for each<br />
standard sample and reagent blank solution. Note (n).<br />
Remove the adsorbed Pu from the column by eluting with O.32 y<br />
HN03 (Note (o)) and then wash the column with water to remove the<br />
HN03. Note (p).<br />
Prepared from gaseous HC1 and deionized water,<br />
HN03 AR redistilled from silica apparatus. Diluted with deionized<br />
water.<br />
Prepared from HF AR and deionized water.<br />
CC14 AR conditioned before use by shaking with an equal volume of<br />
8 ~ HN03 .<br />
Commercial TBP purified by steam distillation and alkaline washing<br />
(see Appendix).<br />
Low density KelF modding powder, less than 100 mesh (see<br />
Appendix).<br />
0.1% Apiezon ~ in CC14.<br />
Each sample should be done in duplicate.<br />
A vigorous reaction occurs if addition of concentrated HN03 is made<br />
to hot residue.<br />
H the residue is allowed to go to dryness it will be difficult to re-<br />
dissolve.<br />
See Appendix for column preparation.<br />
Vitrosil tall-form beaker nominally 50 ml capacity in fact has a<br />
volume of about 75 ml.<br />
145