Experiment No 1 PDF
Experiment No 1 PDF
Experiment No 1 PDF
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Spectrophotmetric Determination of Stoichiometry of a Complex by Jobs Method
1. Aim__________________________________________________________ In this experiment you will determine the the composition of the complex formed by thiocyanate and ferric ions, using Job's method of continuous variation. 2. Safety________________________________________________________ Do not pipette by mouth. Solutions of Hydrochloric acid at which you will be using it (0.004M) present a negligible risk. Ferric nitrate nonahydrate is harmful if swallowed or inhaled, causes irritation to skin, eyes and respiratory tract and affects the liver. Sodium thiocyanate is harmful if swallowed, may be harmful by inhalation or through skin contact and is irritant. 3. Requirements_________________________________________________ UV-Vis Spectrophotometer, 10 test tubes, test tube stand, 2 burettes (50mL), 2 stands, 2 burette clamps, wash bottle with distilled water, a pair of cuvettes, 410-3 M Ferric nitrate and 410-3M Sodium thiocyanate in 410-3M Hydrochloric acid solution, tissue paper.. 4. Theory_______________________________________________________ Job's method of continuous variation is a simple method for finding the stoichiometry of a complex. It is most effective when only a single complex is formed. The success of a Jobs method experiment depends upon how well Beers law is followed. The absorbance A of a sample (the fraction of incident light that it absorbs) is defined in terms of the light incident upon it, Io, and that transmitted, I. A = log10 Io / I The absorbance is related to concentration of the solution, c, through Beers law, which is A = cl is the molar extinction coefficient for a species and l is the optical path length.
Jobs method can be used to find the stoichiometry of the compound formed by two reacting species. The spectra of solutions containing both species in varying proportions are recorded, each solution containing the same total reagent concentration. In this experiment the reagents are Fe3+ and SCN-, so [SCN ] + [Fe3+] = constant (1) A wavelength at which the complex absorbs strongly is selected and the absorbance of each solution at this wavelength is determined. As the concentration of one of the reactants, say the Fe3+, increases from zero, so does the amount of complex, so that the absorbance rises. Absorbance reaches a maximum in the solution in which metal ion and ligand are in the same ratio as in the complex, since this solution will contain the highest concentration of complex. Further additions of metal ion are balanced by a reduction in the amount of ligand because of the need to satisfy equation (1), so absorbance due to the complex then falls. A plot of absorbance as a function of the amount of added ligand should give two straight lines, provided Beers law is obeyed. Extrapolation of the two lines (in the direction away from zero concentration of each species) gives the stoichiometry of the complex directly, since, where the two lines cross, ligand and metal are in the correct proportion to give maximum complex formation. 5. Procedure____________________________________________________ Prepare the following solutions which will be used throughout the experiment. A solution of 410-3M Fe3+ made by dissolving appropriate amount of Fe3(NO3)3.9H2O in 410-3M HCl. A solution of 410-3M SCN made by dissolving appropriate amount of NaSCN in 410-3M HCl. Keep these solutions in two different burettes, after washing and rinsing. Mix them well as follows in the test tubes. 1 2 3 4 5 6 7 8 9 Test Tube No. Volume of Fe(NO3)3 1mL 2mL 3mL 4mL 5mL 6mL 7mL 8mL 9mL 9mL 8mL 7mL 6mL 5mL 4mL 3mL 2mL 1mL Volume of NaSCN Allow to stand for half an hour. Using the the solution in test tube number 5 (the 5+5mL solution) determine the wavelength of maximum absorption max by
Experiment Number:1
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obtaining the spectra 350 and 550nm. At max determine the absorbance of each of the solutions prepared as in the above mentioned table. 6. Experimental Readings_________________________________________ Temperature of the experimental solution = Strength of Fe(NO3)3.9H2O = Strength of NaSCN = = max Test Volume of Fe3+ Volume of SCN tube no. solution (A) solution (B) 1. 1mL 9mL 2. 2mL 8mL 3. 3mL 7mL 4. 4mL 6mL 5. 5mL 5mL 6. 6mL 4mL 7. 7mL 3mL 8. 8mL 2mL 9. 9mL 1mL Ratio of Absorbance volumes(=A/B) 0.111 0.250 0.429 0.667 1.000 1.500 2.333 4.000 9.000
Experiment Number:1
7. Calculation___________________________________________________ Plot the absorbance as a function of the composition (that is ratio of volumes of 3+ Fe and volumes of SCN ). The ratio of the reagents corresponding to the maximum absorption in the curve gives the stoichiometry of the complex. 8. Results_______________________________________________________ Ratio of metal ion and the thiocyante ligand in the complex = Expected formula of the complex formed =
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