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Figure 3.3: Scanning electron micrograph ofa solid reaction product obtained from iron(IlI) tartrate and aqueous sodium phosphate (NafP04 = 2.8) at 200 °c for 3 weeks. 71
and reacted with aqueous sodium phosphate (NalP04 - 2.5, [P04] - 1.0 molal) at 250°C for a period of8 days to produce a red-orange, crystalline solid. The powder XRD results are listed in Table A.L6 in Appendix L No evidence for unreacled starting material could be found visually or in the powder XRD spectrum. This synthesis seemed to produce a solid product with little or no impurities however some extra peaks were observed that are not present in the SlHP XRD powder pattern from Quinlan (1996). The presence ofNa)P04 and FC3PO, in the sample accounts for some ofthe peaks, however the peaks observed at d-spacings 0£7.9707 A and 7.8460 A could not be accounted for. Figure 3.4 is the SEM image ofthe product. The SEM elemental analysis cantioned the presence of iron, sodium, and phosphorus. Distinct thin, needle-like crystals can be seen, much like thc SIHP products obtained from the FelllNTA reactions. While the crystals were bigger than in previous SIHP syntheses, they were still too small to perfonn single crystal XRD. The crystals were not unifonn and there appear to be many crystal [ragments scaltereO throughout the sample. However various areas ofthe SEM image show that the crystals grew in layers of smaller parallel crystals. Again this method gave better crystals than in the first approach, described in Section 3.2.1 but a few impurities were observed. Future work on this reaction could include trying the synthesis at a higher NalP04 mole ratio. J.J (NH4)Fc II Fe lll (p04h The mixed valence compound {NH4)Fe Il Fe Jll (P04h was synthesized by Boudin and Lii (1998) at 500 °C as a black crystalline product. The objective was to see jfthe mixed 72
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1"'1 National Library of Canada Bib
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y thcnnally dc
Page 11 and 12:
Gregory for his kindness and making
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LIST OF TABLES Table 1.1 Corrosion
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single crystals ofquartz (Nacken, 1
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phosphate control in the 19&Os was
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the standard Gibbs energies and ent
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consist ofortnophospllatcs. The bou
Page 41 and 42: 2 FcIlFc[[J204(S) + 26 Na+(aq) + 12
Page 44 and 45: solubility and phase relations ofpr
Page 46: where 11 equals the ionic state ofh
Page 49: '", g :£ 30
Page 55: 1.10 Project Objectives The objecti
Page 61 and 62: II - "7 /'7"7L 41 J n
Page 65 and 66: 2.3.2 Single Crystal X-Ray Dif'frac
Page 67 and 68: 2.4 Synthesis and Characterization
Page 69 and 70: Several solid starting materials we
Page 75 and 76: FeUlNTA(aq) + HPOl(aq) + NH/(aq) __
Page 77 and 78: All runs lasted up to to days at a
Page 79 and 80: 0.0 l--l_-L_l-....J.._-L_l-....J..-
Page 81 and 82: dissolution orSNHP and allowed the
Page 83 and 84: (a) (b) Figure 3.1a and b: Scanning
Page 87 and 88: and the equilibrium constant for ma
Page 89: groups. Oxidizing agents were previ
Page 94 and 95: (al (b) Figure 3.5a and b: Scanning
Page 97 and 98: Figure 3.7: Scanning electron micro
Page 99: Table 3.1: Positional parameters fo
Page 104: Figure 3.10: Scanning electron micr
Page 107 and 108: pattern is listed in Table A.LI3. E
Page 109: 4.0 SOLUBILITY AND REACTION KINETIC
Page 117 and 118: Table 4.1 Experimental C
Page 119: Table 4.3 Standard slale properties
Page 126 and 127: Table 4.6 HKF equation ofstate coef
Page 128 and 129: Equilibrium constants are listed in
Page 130: Table 4.9 Equilbrium constants for
Page 136: Table 4.10 Standard state propertie
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lower NalP04 mole ratio than the re
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Broadbent D., Lewis G.G., and Wetto
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Marshall W.L. (1982) Two-liquid-pha
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Welton E.A.M. (1981) Phase equilibr
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APPENDIX I: Powder X-ray Diffractio
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TABLE A.l.l: X-Ray Diffraction Resu
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TABLE A,I.3 (continued) Quinlan JCP
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TABLE A.1.4 (continued) Quinlan (19
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TABLE A.l.S (continued) JCPDS Quinl
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TABLE A.1.6 (continued) Quinlan (19
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TABLE A.L8 (continued) Boudin JCPDS
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TABLE A.I.9 (continued) Product RGH
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TABLE A.I.IO (continued) Ziemniak a
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TABLE AJ.11 (continued) Zicmniak an
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TABLE A.T.I2 (continued) Zicmniak a
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TABLE A.I.13 (continued) Ziemniak a
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Experimental A colorless irrcg.plal
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Slfuc!ure Solution Refinemenl Funct
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111
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TABLE A.1II.1: Summary of ICP ES Re
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TABLE A.lll.2: KinclicData Time m(N
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TABLE A.III.2 (continued) Time m(Na
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TABLE A.lll.2 (continued) Time m(Na
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TABLE A.lIl.l (continued) Time m(Na
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TABLE A.III.3 (continued) t "C m(p0
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