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Experiment 33: Colorimetric determination of iron
PURPOSE To become aquainted with the principles of colorimetric analysis.
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THEORY When mixed with phenanthroline , Fe2+ ions reacts to form an orange red complex The color of the solution is directly proportional to the concentration of Fe3+ ions present. The concentration of these ions can be determined by measuring the absorbance of a unknown Fe2+ complex solution and comparing it with the absorbance of a solution of known concentration. Colorimeters measure the amount of light that is transmitted or absorbed by a solution. A description of how they work can be found in your text book Fe3+(aq) needs to be reduced to Fe2+ by adding hydroxlyamine
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SAFETY PROCEDURES Follow all instructions for using the equipment in this activity. 2. Wear safety glasses and a laboratory coat for this experiment. 3. Do not throw any waste down the sink.
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Part 1. Preparation of calibration curve
Pipet 1.00, 2.00, 3.00, 4.00, and 5.00 ml of standard Fe solution into a 50 ml volumetric flasks 1 – 5 respectively Add to each flask 1ml of 1M ammonium acetate 1ml of 10% hydroxylamine 10 ml of .30% phenanthroline Dilute the rest to 50 ml with water
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Part 1. Preparation of calibration curve
Mix well Let sit for 40 minutes for the color to develop Clean six cuvettes Add water to one cuvette ½ way and calibrate spectrophotometer to 510 nm Fill the other 5 cuvettes ½ way with a solution of increasing concentration Record absorbance
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Part 1. calibration curve
graph concentration of Fe+2 complex (mg/ml) vs absorbance Absorbance on y axis and concentration on x as seen on page 425 concentration of Fe+2 complex (mg/ml) Absorbance 1 .001 .15 2
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calibration curve Prepare calibration curve by plotting absorbance vs concentration
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Part B: Determination of Fe+3 complex
Create Fe +2 ion Weigh 0.1 g to 4 sig figs of Fe unknown into a 50 ml volumetric flasks Add 5 drop of 6 M sulfuric acid Dilute the rest to 50 ml with water Transfer to a 125 erlenmeyer flask
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Part B: Determination of Fe+3 complex
Convert Fe +2 ion to Fe+3 complex Pipet 1ml of Fe +2 ion from the erlenmeyer flask into three 50 ml volumetric flasks Add to each flask 1ml of 1M ammonium acetate 1ml of 10% hydroxylamine 10 ml of .30% phenanthroline Dilute the rest to 50 ml with water
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Part B: Determination of Fe+3 complex
Mix well Let sit for 40 minutes for the color to develop Clean 3 cuvettes Fill the 3 cuvettes ½ way with each Fe+3 complex solution Record absorbance at 510 nm Using the absorbance determine concentration of Fe+2 complex (mg/ml) by extrapolating from your graph
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