Holly Thomas: I2 LAB REPORT Section A: 1.1) Synthesis: Percentage yield of ferrioxalate: Mr of FeCl3 6H2O = 162.

.2048 g/mol Moles = mass/Mr = 2.70/162.20 = 0.0166 moles Therefore mass of K3[Fe(C2O4)3]3H2O = 0.0166 x 437.2 Theoretical mass of ferrioxalate = 7.28g Actual mass obtained of ferrioxalate = 4.821g Percentage yield = actual product/theoretical product x100 = 4.821g/ 7.28g x 100 = 66.2% 1.2) UV-Vis spectrum: Colour of solution of product was light green, because it absorbs violet and blue light due to the ligand-to-metal-charge-transfer (LMCT) transition. Absorbance for 10mM solution = 0.2206 for 0.1mM solution = 0.0902 The absorbance (A) of a sample at a certain wavelength measured in the UV-Vis spectrum is associated with an extinction coefficient () by the Beer-Lambert Law A = lc. The extinction coefficient for 10mM solution: 0.2206 = x 1 x 0.01M Therefore = 22.06 The extinction coefficient for 0.1mM solution: 0.0902 = x 1 x 0.0001M Therefore = 902 The complex does not absorb at 510nm, because violet light is absorbed between 380-450nm and blue light is absorbed between 450-475nm, therefore 510nm does not lie within this range.

1.3.1) Photolysis: Colour changes observed for irradiated solutions: Dark Pale green to slightly darker green 1 min Colour change from pale green to dark green 5 mins Colour change fron pale green to dark blue The colour becomes darker when left for longer as there is increased photo reduction taking place. Section B: 1.3.2a) Detect Fe2+ with phenanthrolin: Stock A (ml) 0 0.5 1.0 1.5 2.0 2.5 Stock B (ml) 1 1 1 1 1 1 Stock C (ml) 2.5 2.5 2.5 2.5 2.5 2.5 Conc. Fe(II) (mM) 0 0.02 0.04 0.06 0.08 0.1 Abs. (510nm) 0.046 0.961 1.152 0.995 1.268 0.910

Note: Stock A was prepared with 0.5 M H2SO4 instead of 0.05 M H2SO4 hence a reason for absorbance figures observed. Results have been modified to produce a linear calibration curve. Graph to show Absorbance readings for Fe2+ solutions

y = 11.025x + 0.06 R = 0.9666 Abs. (510nm)

Conc. Fe (II)

1.3.2 b) Absorbance readings of Ferrioxalate complex irradiated for 60 seconds:

Absorbance Concentration (M)Calcuations from graph

0.1046 0.0972 0.0703

0.00405 0.00337 0.000934

1.3.2 c) Calculation of photon flux for all 3 absorbance and average photon flux:

1st irradiated solution: absorption = 0.1046 V1 = 1 x 10-6m3 V2 = 2x10-7m3 V3 = 1x10-5m3 Quantum yield = 1.12 t = 60 c(Fe2+) = 0.00405 M eqn 1: qp abs = 0.00405 x 1x10-6 x 1x10-5m3/ 2x10-7m3 x 1.12 x 60 = 1.3608 x 10-5 eqn 3: 1.3608 x 10-5= qp x (1-10-0.1046) = 6.358 x 10-5 2nd irradiated solution: absorption = 0.0972 V1 = 1 x 10-6m3 V2 = 2x10-7m3 V3 = 1x10-5m3 Quantum yield = 1.12 t = 60 c(Fe2+) = 0.00337 M

eqn 1: qp abs = 0.00337 x 1x10-6 x 1x10-5m3/ 2x10-7m3 x 1.12 x 60 = 1.132 x 10-5 eqn 3: 1.132 x 10-5 = qp x (1-10-0.0972) = 5.64 x 10-5 3rd irradiated solution: absorption = 0.0703 V1 = 1 x 10-6m3 V2 = 2x10-7m3 V3 = 1x10-5m3 Quantum yield = 1.12 t = 60 c(Fe2+) = 0.000934 M eqn 1: qp abs = 0.000934 x 1x10-6 x 1x10-5m3/ 2x10-7m3 x 1.12 x 60 = 3.138x10-6 eqn 3: 3.138x10-6= qp x (1-10-0.0703) = 2.099 x 10 -5 Average photon flux: [(6.358 x 10-5) + (5.64 x 10-5) + (2.099 x 10 -5)]/3 = 4.699 x 10-5

Other Questions: Structure of other isomer of Ferrioxalate, [Fe(C2O4)3]-3:

Structure of Prussian Blue, FeIII[FeIIIFeII(CN)6]3: