Andrew Li 101258492 Fe short report, TA-Maram Bakiro, 11-03-22 (1)

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Feb 20, 2024

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Spectrophotometric determination of iron Date submitted: 11-03-2022 By: Andrew Li (101258492) Lab section:L4 TA: Maram Bakiro Procedure: 1. You’ll be given a CONCENTRATED STANDARD IRON solution that contains 0.2500 g/L of iron. Pipette 25.00ml of this into a 500.00ml volumetric flask and dilute up to the mark with distilled water. Mix well as you fill the volumetric flask. This is your DILUTE STANDARD IRON solution. 2. Prepare a set of six calibration standards using this DILUTED STANDARD IRON SOLUTION, containing the following total amounts of iron: 0.00 mg (the “blank” with no iron in it), 0.05 mg, 0.10 mg, 0.15 mg, 0.20 mg, 0.25 mg.NOTE: do NOT fill these six flasks to their marks. Set them aside for now. These are your calibration standards. 3. Obtain an unknown iron sample and note the sample number. Pipette 10.00 ml of your unknown iron sample into a 250.00 ml volumetric flask and dilute it to the mark with distilled water. Mix it properly as described in step 1. 4. Pipette two 25.00 ml aliquots of this solution into two individual 50.00 ml volumetric flasks. Note the dilution factor for these solutions relative to the original unknown. This value will be needed to calculate the original concentration of iron in the unknown (which is the objective of this lab.) 5. You now have eight 50 ml volumetric flasks: your blank, five flasks with increasing amounts of your standard iron solution in them, and two with samples of your unknown solution. Add to each one, by pipette:4.0 ml 10% hydroxylamine hydrochloride 4.0 ml 0.3% ortho-phenanthroline 6. Swirl each and allow them to sit for at least 10 minutes. 7. After 10 minutes have passed, dilute each flask to the mark with distilled water, using proper technique (as in step 1). 8. Set the wavelength on the spectrophotometer to the value you chose based on the spectrum of the iron(II) ortho-phenanthroline complex. ONCE YOU SET IT, DO NOT CHANGE THIS WAVELENGTH DURING THE LAB.
9. Fill a cuvette about 2/3 full of your blank solution and run the blank in the spectrophotometer to zero it. 10. Empty the blank solution out of the cuvette and rinse it with your most dilute solution. Fill the cuvette about 2/3 full and measure the absorbance. 11. Empty this solution, and rinse with the next one in order of increasing concentration. Fill it 2/3 full with this second solution, and measure the absorbance. 12. Repeat this step for each of the calibration solutions, going up in concentration from least to most concentration. Make sure each absorption is recorded. 13. Rinse the cuvette with distilled water, and then rinse with a small amount of your first unknown solution. Measure the absorption of your first unknown. Rinse the cuvette with a small amount of your second unknown solution, then fill it and measure the absorption of your second unknown. Data: Iron amount (mg) Absorption 0.00 -0.022 0.05 0.154 0.10 0.352 0.15 0.540 0.20 0.739 0.25 0.937 Unknown 1 0.651 Unknown 2 0.646 Table 1. Absorptions of different concentration of diluted iron Calculations: 1.
Graph 1- Concentration(mg/50ml) vs Absorbance (excluding unknown samples) 2. Beer-lambert’s Law: A= εlc l=1 cm (cuvette) Equation of the line: y=mx+b y=absorption value x= concentration Unknown #1 y=3.85x-0.0313 0.651=3.85x-0.0313 0.6823=3.85x x=0.1772207792 x=0.177mg/50mL or 0.00354mg/mL Unknown #2 0.646=3.85x-0.0313 x=0.1759220779 x=0.176mg/50mL or 0.00352mg/mL
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3. Unknown sample Amount of iron in the undiluted= (0.00354+0.00352)/2 =0.00353mg/ml= 0.00353g/L 0.00353 g/L x 50(Dilution factor)= 0.1765g/L=0.177g/L Amount of iron in undiluted is 0.177g/L 4. Relative spread=((higher value-lower value)/average value)x1000 Relative spread=((0.00354-0.00352)/0.00353)x1000 Relative spread= 5.67 ppt 5. Accepted value of unknown iron sample= 0.1735g/L Relative error= ((Calculated Result-Accepted Result)/Accepted Result)x 100% Relative error= ((0.1765-0.1735)/0.1735)x100% Relative error = 1.72910663 Relative error=1.73% 6. Slope of the curve is : 3.85 m=A= εl ε=m/l ε=3.85/1 ε=3.85L/mol*cm Results: The concentration 1.73% higher than the accepted value of the unknown iron sample, of 0.1735 g/L. The margin for error is very low, and some possibilities of errors come from slight smudges on the cuvette causing some added absorption of light. It also could be the account that the measuring equipment all have margins of error, and that slight error caused a slight increase in measured concentration of iron.
Conclusion: The results of the experiments show that the amount of measured iron in the unknown sample was 0.177 g/L. That measured value was 1.73% higher than the accepted value, and the spread of data was 5.67 ppt. The extinction coefficient is 3.85 L/mol*cm. References Carleton University, Fe: SPECTROPHOTOMETRIC DETERMINATION OF IRON, p. 1 to 5. Skoog and West, Fundamentals of Analytical Chemistry, 2nd ed., Chapter 29. Vogel, A Textbook of Quantitative Inorganic Analysis, 3rd Ed., p. 294, 310 and 787.