Estimation of Iron by using photometric colorimetric method

Aim Estimation of Iron by using photometric colorimetric method Principal The absorbance of various solutions with known concentrations of iron (bound in a colored ironphenanthroline complex) was measured to determine a calibration curve. The absorbance of an unknown was then determined both quantitatively (with a spectrometer) and qualitatively (by sight comparison) to assess the amount of iron in the unknown. The relationship that links absorbance with concentration and path length is given by Beer Lamberts law: A = Ecl ______________________(1)

Where, A = absorbance of the sample E= extinction coefficient c = concentration l = pathlength of sample Iron is brought into solution, reduced to the ferrous state by boiling with acid and hydroxylamine, and treated with 1, 10 phenanthroline at pH 3.2 to 3.3. Three molecules of phenanthroline chelate each atom of ferrous iron to form an orangered complex. Use 510 nm, providing a light path of 1 cm or longer. The coloured solution obeys Beer's law; its intensity is independent of pH from 3 to 9. A pH between 2.9 and 3.5 insures rapid colour development in the presence of an excess of phenanthroline. Colour standards are stable for at least 6 months.
4 Fe+3 (aq) + NH2OH (aq) Fe+2 (aq) + 3 C12H2N2 (aq) 3 Fe+2 (aq) + N2O (aq) + 4 H+ (aq) + H2O (l) [(C12H2N2)3Fe]+2 (aq) (orange-red complex)

Materials used (beyond common lab glassware): Spec 20, set at 510 nm Total amount needed 50-mL 5-mL 5-mL 50-mL 10 drop Chemical Stock Fe solution (0.050 mg Fe+3/ ml) 1 M ammonium acetate (NH4C2H3O2), buffer to maintain pH = 3.5 10% Hydroxylamine HCl (NH3OHCl), reducing agent 0.3% o-phenanthroline (C12H2N2) 3 M H2SO4

Procedure to prepare solution Strong Oxidising agents, cyanide, nitrite, and phosphates (polyphosphates), and some metals in higher concentrations. The initial boiling with acid converts polyphosphates to orthophosphate and removes cyanide and nitrite. Adding excess hydroxylamine eliminates errors of strong oxidising agent. In the presence of interfering metal ions, use a larger excess of phenanthroline. When excessive concentrations of interfering metal ions are present, the extraction method may be used. Mix sample thoroughly and measure 50.0 mL ( < 200 g iron,) Add 2-mL conc. HCl and 1 mL hydroxylamine Hydrochloride (NH2OHHCl). Heat to boiling. Transfer sample to nessler tube and Add 10 mL Ammonium acetate(NH2O3H2C4) buffer and 4 mL phenanthroline solution and dilute to mark with water. Mix thoroughly and allow at least 10 to 15 min for maximum colour development. Experiment 1 In this experiment, a UV-Vis spectrophotometer was used for the analysis of the sample. 2 First, solutions of 5 ppm, 10 ppm, 15 ppm, 20 ppm were taken from a 50 ppm working solution and placed in a 50 ml-volumetric flasks. 3 The blank solution was put in a plastic cuvette and into the spectrophotometer to minimize the error caused by the reflected light then the analytical wavelength was set by using the most concentrated working standard. 4 The calibration curve was then prepared by using the prepared solutions and plotting their Absorbance (Abs.) vs Concentration. 5 Then, a sample of unknown concentration was obtained from the instructor and absorbance readings were taken and the concentration was determined. Thus, it can be said that this experiment was done to determine the concentration of Fe ions in a sample by taking the absorbance and using Beers law to compute the concentration.

Table 1. Observation of max Sr. No. 1 2 3 4 5 6 7 8 9 10 11 Wavelength nm 450 460 470 480 490 500 510 520 530 540 550 Absorbance of solution 0.25 0.38 0.42 0.55 0.73 0.88 1 0.9 0.81 0.62 0.49

2.0

Graph of Abs.
1.8 1.6 1.4 1.2

Concentration

Abs.

1.0 0.8 0.6 0.4 0.2

510 nm
0.0 440 460 480 500 520 540 560

Wavelength

Table 2. Absorbance of solution Sr. No. 1 2 3 4 5 Relative Concentration [ Cu (II) ppm] 5 10 15 20 Unknown
0.50 0.45 0.40 0.35 0.30

Absorbance at 606 nm 0.108 0.203 0.291 0.38 0.108

Graph of Abs.

Concentration

Abs.

0.25 0.20 0.15 0.10 0.05 0.00 0 5 10 15 20 25

Concentration (PPM)

Concentration of Unkown Solution

Take Concentration Sample = 9 ppm

Result:1. Concentration of Unknown sample in given solution = 7.5 ppm