Step | Protocol (in anoxic glovebag with anoxic solutions) | Purpose/Importance |
---|---|---|
1 | Wash ~2-5 g of Dowex® 1x8 resin (100–200 mesh, chloride form) with ~20 mL 0.1 M HCl, repeat 4x | Pre-wash to remove any residual material from resin production that can interfere with uranium analysis via KPA |
2 | Use final rinse from Step 1 to slurry-pack a suitable column (such as a Thermo Scientific® Pierce polystyrene column, 0.7 cm ID with top and bottom frits) to 1.5-2 mL bed volume | Use a bed-height to column diameter ratio >3. In this study, bed-height to column diameter ratios between 5 and 7 were used with success |
3 | Flush resin-packed column with 4 M HCl (~10 bed volumes) | Pre-flush to ensure resin column is completely saturated with 4 M HCl |
4 | Add two successive flushes of 1x10-2 M Ti(III) (2 bed volumes each) in 4 M HCl and, using end caps, seal in a final 1.5-2 bed volumes of Ti(III) and allow the packed resin column to soak for 3 or more days | Pre-treat resin to reduce oxidants associated with the resin that cause oxidation of U(IV) |
5 | Drain the resin column and flush with at least 10 bed volumes of 4 M HCl | To flush out residual Ti(III) prior to sample addition |
6 | Add uranium-containing solution in 4 M HCl (1 mL). Elute column with a total of 9 bed volumes of 4 M HCl and collect fraction(s) | To collect U(IV) fractions, which pass through the resin at 4 M HCl |
7 | Elute column with a total of 9 bed volumes of 0.1 M HCl and collect fraction(s) | To collect U(VI) fractions, which adsorb to resin at 4 M HCl but are eluted at 0.1 M HCl |
8 | Flush column with a total of 7 bed volumes of 0.1 M HCl | Post-flush to ensure all U(VI) is flushed away and clean resin for future use |
9 | Flush column with a total of 7 bed volumes of 4 M HCl | Post-flush to ensure all U(IV) is flushed away and resin column is in 4 M HCl state for future use |
Column is ready to be re-used by repeating Steps 6–9 (Steps 1–5 need only be completed once) |