Canada - Memorial University of Newfoundland

2.3.2 Single Crystal X-Ray Dif'fraction
Dr. John BridsoD and Mr. David Miller at the Department ofChemistrylMUN
analyzed the structure of the single crystal isolated in this study with a Rigaku AFC6S
diffractometer and a VAX3l00 workstation and the teXsan crystallographic software
package (Molecular Structure Corporation Inc.). A more detailed report ofthe analysis
can be found in Appendix II.
2.3.3 ICP Emission Spectroscopy
During the kinetic and solubility experiments, liquid samples were taken from the
autoclave at regular intervals and diluted by mass in order to obtain sodium and
phosphorus concentrations between 50-200 ppm. The diluted samples were analyzed
using a TJA Iris HR ICP-OE spectrometer with a TJA 300 sample changer, at the
Department ofMines and Energy by Mr. Chris Finch. The spectrometer was controlled
by ThennoSpec software.
To calibrate the instrument a blank solution was run that contained 0 ppm sodium
and phosphorus followed by a standard solution of 250 ppm sodium and phosphorus.
Two samples ofdeionized water were then run for baseline measurement, then another
125 ppm standard solution. Each sample was flushed through the sample line for a
minute to remove any possible contaminants before the concentrations ofthe sample was
mcasured, and the 125 ppm standard was rc-run aftcr cvery tcn samples to ensure the
instrument was giving accurate readings. Included in each batch ofunknown samplcs
were four known standard solutions which provided a second check for instrument
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