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Spectroscopic Determination of Iron by 1,10-Phenanthroline Method

This document describes a spectroscopic method for determining iron concentration using 1,10-phenanthroline. Iron(II) reacts with 1,10-phenanthroline to form an orange-red complex with maximum absorbance at 510 nm. The method involves preparing standard iron solutions, reducing any iron(III) to iron(II), adding buffer and 1,10-phenanthroline, and measuring absorbances to generate a calibration curve to determine iron concentration in an unknown water sample. The limit of detection is 0.3 ppm iron according to EPA and BIS drinking water standards.

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164 views5 pages

Spectroscopic Determination of Iron by 1,10-Phenanthroline Method

This document describes a spectroscopic method for determining iron concentration using 1,10-phenanthroline. Iron(II) reacts with 1,10-phenanthroline to form an orange-red complex with maximum absorbance at 510 nm. The method involves preparing standard iron solutions, reducing any iron(III) to iron(II), adding buffer and 1,10-phenanthroline, and measuring absorbances to generate a calibration curve to determine iron concentration in an unknown water sample. The limit of detection is 0.3 ppm iron according to EPA and BIS drinking water standards.

Uploaded by

ancuta.lupaescu
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© © All Rights Reserved
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Spectroscopic determination of iron by 1,10-phenanthroline method

Presentation · April 2020


DOI: 10.13140/RG.2.2.12030.74568

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Spectroscopic determination of iron by 1,10-phenanthroline method
By
Dr. Santosh Bahadur Singh
Department of Chemistry, NIT Raipur, Raipur-492010, Chhattisgarh, India
E-mail: singhsbau2012@gmail.com
Introduction

Iron occurs in the minerals and leaches to natural water bodies. Elevated iron contents/levels

in water can cause stains in plumbing, laundry, cooking utensils, and can impart

objectionable taste and colour to food materials. US EPA (United State Environmental

Protection Agency) and BIS (Bureau of Indian Standards) approved the iron contents for

drinking water i.e. 0.3 ppm.

Materials

1. 1,10-phenanthroline (C12H8N2): 0.25 per cent solution of the monohydrate in water

2. Hydroxylamine hydrochloride (H2NOH.HCl): 10 per cent aqueous solution

3. Iron(II) standard solution [FeSO4.(NH4)2SO4.6H2O]

4. Ammonium acetate ((CH3COONH4) buffer solution: 1 % solution in an acetic acid buffer

of pH (mix 65 mL of 0.1 M acetic acid and 35 mL of 0.1 M ammonium acetate solution)


Theory/Principles

Iron(II) reacts with 1,10-phenanthroline (ortho-phenanthroline) to form an orange-red

complex {Ferrous ortho-phenanthroline-[(C12H8N2)3Fe]2+} which shows maximum

absorbance at wavelength (λmax) 510 nm. The colour intensity is independent of the acidity in

the pH range 2-9, and is stable for long periods. First, all the iron(III) contents may be

reduced with hydroxylamine solution to iron(II).

2+

N N

+ Fe2+
N Fe N
N N

1,10-phenanthroline N N

Orange-red colour

Maximum wavelenght = 510 nm

Procedure

1. Using a burette, transfer requisite volume of stock iron solution into separate 100 mL

volumetric flasks to prepare 10, 20, 30, 40, and 50 ppm solution. Fill each flask about half

full with deionized or distilled water.

2. Add 2mL of conc. HCl solution and 1 mL hydroxylamine solution to each flask, then heat

upto boiling to convert all Fe(III) into Fe(II), then cool it.

3. Add 10.0 mL of the ammonium acetate buffer solution to each flask and mix properly.

4. Finally, add 4.0 mL of the 1,10-phenanthroline solution to each flask. Fill each flask to the

100 mL mark with distill water.

5. Mix thoroughly and wait for few moments to complete colour development.
6. Similarly blank solution can be prepare: add 10.0 mL of buffer, 2.0 mL of hydroxylamine

hydrochloride solution, and 4.0 mL of 1,10-phenanthroline solution to a 100 mL flask. Dilute

to the mark with distilled or deionized water and mix. This is your blank solution.

7. You now have five standard iron solutions and one blank. Record the absorbance of all

standard and blank solution by UV-Vis spectrophotometer at λmax 510.

7. Plot the calibration curve between iron concentration v/s absorbance. By using the plot and

linear line equation (y = mx + c) conversion factor to convert absorbance to concentration can

be obtained.

8. Same procedure applied with unknown water sample containing iron and records their

absorbance.

9. By correlating with calibration graph, one can calculate iron concentration from unknown

water sample.
Procedure Chart

Results: Given water sample contains iron………………ppm.

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