03.04.2013 Views

THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org

THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org

THE RADIOCHEMISTRY OF PLUTONIUM - Sciencemadness.org

SHOW MORE
SHOW LESS

You also want an ePaper? Increase the reach of your titles

YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.

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

Hooray! Your file is uploaded and ready to be published.

Saved successfully!

Ooh no, something went wrong!