EXPERIMENT OF TOTAL IRON DETERMINATION & TOTAL MANGANESE

DETERMINATION

Introduction

The determination of total iron can be done by Phenanthronine method. While the total
manganese determination required Persulfate method. Iron (Fe) in  ground  waters  is  normally
present  in  the ferrous  (Fe++)  state  which  is  easily  oxidized  to  ferric  (Fe+++)  on the
exposure  to  air. Manganese (Mn) is less commonly found in groundwater than iron, rarely
found alone in a water source, and generally found with dissolved iron.

Oxidation of dissolved iron particles in water changes the iron to white, then yellow and finally
to red-brown solid particles that settle out of the water. Iron that does not form particles large
enough to settle out and that remains suspended and then leaves the water with a red tint.
Manganese usually is dissolved in water, although some shallow wells contain colloidal
manganese (black tint). These sediments are responsible for the staining properties of water
containing high concentrations of iron and manganese. These precipitates or sediments may be
severe enough to plug water pipes.

Objective

a) To determine the total iron concentration in the sample provided by using Phenanthroline
Method
b) To determine the total manganese concentration in the sample provided using Persulfate
Method
Method

Total Iron Determination

1. 50ml sample was placed into 125mL flask

2. 20ml of concentrated HCl, 1 Hydoroxylamine and a few of glass beads were added
3. Heat to boil until the volume reduced to 15~20ml. Then cool at room temperature.
4. Transfer to 50mlvolumetrik flask
5. 10ml Ammonium acetate buffer,4ml phenanthroline solution were added. Then, mixed
them well.
6. Dilute to mark with distilled water and mix well
7. Let 10-15minit for maximum color development
8. Measure absorbency at 510nm

Total Manganese Determination

1. 100ml sample was placed into 250 ml flask

2. 5ml special reagent and 1 drop H₂O₂ were added
3. Boiling until the concentrated reduced to 90ml
4. 1g of Ammonium Persulfate was added
5. Boil and prolonged boiled for 1 minute. Then, cool it immediately
6. Dilute to 100ml with distilled water and mix well
7. Absorbency was measured at 525nm.
Result

Total Iron at 510nm Total Manganese at 525 nm

(mg/L) (mg/L)
0.19 0.02

Discussion & Conclusion

Iron  in  ground  waters  is  normally  present  in  the ferrous  (Fe++)  state  which is
easily oxidized  to  ferric  (Fe+++)  one exposure  to  air. Iron  can  enter  a  water  system  by
leaching  natural deposits   from   iron-bearing   industrial   wastes,   effluents   from   pickling
operations, or  acidic  mine  drainage.

According to Environmental protection Agency (EPA), iron and manganese is secondary

pollutant. They are both classified under the Secondary Maximum Contaminant Level (SMCL)
standards. The SMCL for iron in drinking water is 0.3 milligrams per liter (mg/l), sometimes
expressed as 0.3 parts per million (ppm), and 0.05 mg/l (ppm) for manganese. Water with less
than these concentrations should not have an unpleasant taste, odor, appearance or side effect
caused by a secondary contaminant.

In this experiment, Iron and Manganese were measured by Spectroquant Nova 300 using
wavelength of 510nm for Iron and 525 nm wavelengths for Manganese. Total iron that has been
measured is 0.19 mg/L which is not exceed the standard of Secondary Maximum Contaminant
Level. Same goes to manganese which is measured by 0.02 mg/L of total determination
compared to SMCL standard which is 0.05 mg/L.

Question
1) What is the environmental significance of iron and manganese in water supplies?
- They cause reddish-brown (Iron) or black stains (Manganese) on clothes or household
fixtures. According to Environmental Protection Agency (EPA), iron and manganese are
considered secondary contaminants. Secondary standards apply to substances in water
that cause offensive taste, odor, color, corrosion, foaming, or staining but have no direct
affect on health.
-Besides, Iron and manganese deposits will build up in pipelines, pressure tanks, water
heaters and water softeners. This situation reduces the available quantity and pressure of
the water supply. Iron and manganese accumulations become an economic problem when
water supply or water softening equipment must be replaced. There also are associated
increases in energy costs from pumping water through constricted pipes or heating water
with heating rods coated with iron or manganese mineral deposits.

2) Discuss briefly how iron and manganese get into underground water supplies?
-Iron and manganese are common metallic elements found in the earth's crust. Water
percolating through soil and rock can dissolve minerals containing iron and manganese
and hold them in water supplies.

3) In what form must iron exist in order to be measured by the Phenanthroline method
and how is iron converted to this form?
-It is exist in form of ferric (3+) which is Iron (III). Iron (III) converted to this form by
the reaction of Iron (II) with the air.

4) In what oxidation state must the manganese be for calorimetric measurement?

-Mn (II)