Analysis of Iron Ore by Titration with Potassium Dichromate

Purpose: A standardized solution will be prepared by the direct method by dissolving

an accurate weight of primary standard potassium dichromate in deionized water up to
the pre-calibrated mark of your volumetric flask. The percentage of iron in an unknown
sample will be determined by an oxidation-reduction titration.
Solutions and Chemicals Required
unknown iron ore sample to be dried at 110°C for at least one hour predried primary
standard K2Cr2O7concentrated HCl SnCl2 solution, HgCl2 solution, syrupy H3PO4
diphenylamine sulfonate indicator
Special Equipment: calibrated 250 ml volumetric flask
PROCEDURE
1.Preparation of K2Cr2O7
Precisely weigh by difference from a weighing bottle, between 0.55 to 0.65 g
of the predried, primary standard K2Cr2O7. Carefully dilute the K2Cr2O7 solution with
deionized water up to the calibration mark of the 250ml volumetric flask. The exact
volume contained in the 250ml volumetric flask was determined in part II of Analytical
Techniques and Measurements experiment. Write the balanced equation for the reaction
of Fe2+ with K2Cr2O7. Calculate the molarity of the K2Cr2O7 solution.(FW of
K2Cr2O7 = 294.19)
2.Solution of the Iron Ore Sample
Transfer the unknown iron ore sample to a clean weighing bottle and dry for one hour at
110°C. After the sample has cooled, weigh by difference, to the nearest 0.1mg, a 0.20
gm sample into a 250 ml Erlenmeyer flask. To dissolve this and subsequent samples,
add 15ml of concentrated HCl (ALWAYS ADD ACID TO WATER) to the sample in
the flask. Heat the solution to just below boiling on the hot plate until the ore dissolves.
Make sure the exhaust fan is on. This first 0.20gm sample is a trial to become familiar
with the end point and to determine a sample weight which will result in the delivery of
30-45ml of K2Cr2O7 solution. Go through the entire procedure with this sample and
then calculate an optimum weight for the remaining trials. Remember that three good
trials must be done.
3.Reduction of Fe(III) to Fe(II) and Titration of Fe(II)
The reduction step must be done one trial at a time and the titration of that
sample must be done immediately after the reduction. This is because the reduced Fe2+
is readily oxidized in air to Fe3+. Note the oxidized form of the iron does not react with
K2Cr2O7.
Heat each solution containing the iron sample almost to boiling. Carefully add
SnCl2 solution dropwise until the yellow Fe(III) color just disappears. Then add only 2
drops excess of SnCl2 solution. Cool by running the outside of the flask under cold
water (until the flask can be comfortably held, <40°C). Next rapidly add 10ml
(measured in a graduated cylinder) of the HgCl2 solution. A small quantity of a white
precipitate should appear. If no precipitate forms or if the precipitate is gray or black,
the trial must be discarded.
After waiting only about 2 to 3 minutes, add to the pre-reduced solution, about
5ml of concentrated sulfuric acid and 7ml of syrupy phosphoric acid (measured in a
graduated cylinder). Dilute with distilled water to bring the volume to about 125ml.
Again cool the solution to room temperature by running the outside of the flask under
cold water. Add 8 drops of diphenylamine sulfonate indicator and slowly titrate with
your standard K2Cr2O7 solution from a blue-green, through a greyish tinge to the first
permanent violet, which is the end point. The titration should be conducted dropwise
when the grey tinge is noted because the oxidation of the indicator is somewhat slow at
this point. Do the trial run first to see the end point and determine the sample weight.
Then do three good trials. The average relative deviation should not exceed 2 ppt.
Blank
There is a significant indicator blank for this titration. To run a blank, all the
reagents except for the iron unknown should be added to a 250ml Erlenmeyer flask and
the volume should then be brought up to the approximate volume at the end point using
distilled water.
Hence add 15ml of distilled water, 15ml of con HCl, 2 drops of SnCl2, 10ml of
HgCl2, 5ml con H2SO4, 7ml of syrupy H3PO4, and dilute with deionized water to an
approximate end point volume. Cool. Add 8 drops of diphenylamine sulfonate indicator
and titrate with K2Cr2O7 through the greyish tinge to a permanent violet.
Remember the actual end point change is slow. The blank should be no more than 1 to 4
drops (about 0.20ml) and its value needs to be subtracted from the volume of K2Cr2O7
required to titrate each iron sample. Do the blank twice.
CALCULATIONS
1. Calculate the molarity of the K2Cr2O7 solution.
2. Calculate the percentage of Fe in the iron ore sample for each trial.
Calculate the average relative deviation for this experimental step.
Formula Weights:
Fe 55.847
Fe2O3 159.69
K2Cr2O7 294.19