Thesis for the Degree of Doctor of Philosophy - DTU Orbit
Thesis for the Degree of Doctor of Philosophy - DTU Orbit
Thesis for the Degree of Doctor of Philosophy - DTU Orbit
You also want an ePaper? Increase the reach of your titles
YUMPU automatically turns print PDFs into web optimized ePapers that Google loves.
0.2 M KNO3. The effluent and <strong>the</strong> washes were combined <strong>for</strong> <strong>the</strong> determination <strong>of</strong> iodate. Iodide on<br />
<strong>the</strong> column was eluted using 40 mL <strong>of</strong> 10% NaClO.<br />
Total iodine including organic and inorganic species determination. To a certain volume <strong>of</strong> fresh<br />
water sample (100 mL) spiked with about 50 Bq <strong>of</strong> 125 I - tracer, 5mL <strong>of</strong> 15% NaClO and 5mL <strong>of</strong> 3M<br />
NaOH was added. This mixture was heat at 150 0 C <strong>for</strong> 3h.<br />
Extraction <strong>of</strong> iodine from all separated fractions. About 50 Bq <strong>of</strong> a 125 I - solution was added to<br />
effluent plus wash from <strong>the</strong> anion exchange chromatographic separation procedure above (iodate<br />
fraction) as chemical yield tracer. About 2.0 mg <strong>of</strong> stable iodine (prepared from Woodward iodine) was<br />
added to all separated fractions as a carrier. To convert all iodine to iodide, 0.2 mL <strong>of</strong> 2.0 M NaHSO3<br />
was added and pH was adjusted to 2 using 3.0 M HNO3. Iodine was first extracted with CCl4 after<br />
oxidation <strong>of</strong> iodide to molecular iodine using NaNO2, and <strong>the</strong>n back-extracted with NaHSO3 solution.<br />
The extraction and back-extraction was repeated to purify <strong>the</strong> iodine solution. The chemical yields <strong>of</strong><br />
iodide and iodate were measured by counting 125 I in <strong>the</strong> separated solution using a NaI γ-detector, and<br />
were found to be 50-70% and 72-98% respectively. The chemical yields <strong>of</strong> total iodine were found to<br />
be 44-92%.<br />
127 I and 129 I preparation <strong>for</strong> ICP – MS and AMS measurement. One milliliter <strong>of</strong> iodide fraction was<br />
taken and diluted to 20 mL with 0.1 M NH4OH. About 10 mL <strong>of</strong> original lake water and 10 ml from<br />
iodate fraction was taken and NH4OH solution was added to a NH4OH concentration <strong>of</strong> 0.1 M. Cs + as<br />
(CsCl) was added as an internal standard to a concentration <strong>of</strong> 2.0 ng/mL. The concentration <strong>of</strong> 127 I was<br />
determined using an X-SeriesII ICP-MS (Thermo Electron Corporation). The detection limit,<br />
calculated as 3SD <strong>of</strong> blanks, was 0.23 nM.<br />
5