13.
dissolve residue in 1:1 HNO 4 and wet ash to a clean white ash,
convert to chloride form by the addition of 10-15 ml conc. HCl and dake
dry,
dissolve residue in 40-50 ml of 0.08N HCl and stir for 10-15 minutes,
16.
adjust the pH to 1.1 = 0.1,
17.
if any solids remain at this point,
filter sample through a glass fiber
paper using 0.08N HCl as a wash solution,
18.
transfer sample solution into a 125 ml separatory funnel,
19.
rinse the sample container with 60 ml of 20% HDEHP and add to
separatory funnel,
extract the sample by shaking vigorously for 2 minutes.
Allow the
phases to separate and drain off the icwer aqueous phase into a second
125 ml separatory funnel containing 60 ml of 20% HDEHP,
2l.
extract the sample again by shaking for 2 minutes and allow phases to
separate,
22.
drain off the aqueous pnase.
The aqueous phases of 3 to 6 samples may
be combined to make a composite sample of 7.5 to 15 liters,
23.
evaporate the combined sample slowly until salting out occurs.
Dilute
to 40-50 ml with distilled H,0 and adjust pH to 1.1 + 0.1,
if any solids remain at this poinc,
filter sample through glass fiber
paper using 0.08N HCl as a wash solution,
25.
transfer sample solution to a 100 ml polyethylene bottle, add 40 mg of
yttrium carrier, gamma count for 8. strontium recovery and store for 18
days for Oy erriua ingrowth,
26.
proceed to Step 6 of the HDEHP procedure.