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Thesis for the Degree of Doctor of Philosophy - DTU Orbit

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espectively. The iodine was leached from <strong>the</strong> ashed samples 100 mL <strong>of</strong> double distilled water<br />

at 100 0 C and filtered. A known amount <strong>of</strong> <strong>the</strong> solution (0.1-0.5 mL) was removed <strong>for</strong> ICP-MS<br />

determination <strong>of</strong> 127 I and <strong>the</strong> remaining solution were subject to 129 I analysis. About 2.0 mg <strong>of</strong><br />

stable iodine (prepared from Woodward iodine) was added to leached fraction as a carrier. To<br />

convert all iodine to iodide, 0.2 mL <strong>of</strong> 2.0 M NaHSO3 was added and pH was adjusted to 2<br />

using 3M HNO3. Iodine was first extracted with CCl4 after oxidation <strong>of</strong> iodide to molecular<br />

iodine using NaNO2, and <strong>the</strong>n again reduced and back-extracted using NaHSO3 solution. The<br />

extraction and back-extraction step was repeated once to purify <strong>the</strong> iodine solution. The<br />

chemical yield <strong>of</strong> iodine in <strong>the</strong> whole procedure, measured by <strong>the</strong> added 125 I tracer, ranged from<br />

56% to70%.<br />

127 I and 129 I preparation <strong>for</strong> ICP – MS and AMS measurement. The aliquot <strong>for</strong> 127 I was<br />

diluted to 10 - 25 mL with 0.1 M NH4OH and stable Cs + as (CsCl) was added as an internal<br />

standard to a final concentration <strong>of</strong> 2.0 ng/mL. The concentration <strong>of</strong> 127 I was determined using<br />

an X SeriesII ICP-MS (Thermo Electron Corporation).<br />

Iodine as iodide in <strong>the</strong> final back extracted solution was transferred to a centrifuge tube, and<br />

1.5mL <strong>of</strong> 3M HNO3 was added. To <strong>the</strong> solution 1mL <strong>of</strong> 1M AgNO3 was added and mixed.<br />

The AgI precipitate was dried at 60-70 °C, and <strong>the</strong>n ground to powder, mixed with niobium<br />

powder and pressed into a copper holder <strong>for</strong> measurements <strong>of</strong> 129 I by accelerator mass<br />

spectrometry (AMS) at <strong>the</strong> Tandem Laboratory, Uppsala University using a terminal voltage<br />

<strong>of</strong> 3.5MV. The statistical error <strong>of</strong> <strong>the</strong> analysis, including mainly measurement errors at 1<br />

standard deviation was

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