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Chemical Overview
Reactions:
HCl reacts with Fe2O3 to generate Fe+3 (iron III). Stannous chloride (SnCl2) is
added, to a slight excess, converting iron III, Fe+3 to iron II, Fe+2. The reaction mixture
now contains Fe+2, Sn4+, and Sn2+. (The iron II is relatively unstable and subject to air
oxidation). Since Sn2+ is subject to oxidation by K2Cr2O7, the Sn+2 must first be
converted to Sn+4 state before the titration is started. Mercuric chloride (HgCl2), a mild
oxidizing agent, is added to the solution which converts the excess Sn2+ to the Sn4+
state while leaving iron II unreacted and forms Hg2Cl2, a milky white precipitate as a
product. This step also tests if:
1) Too large an excess of Sn II was added (reaction (4) takes place) and Hg0
(black precipitate) forms. This sample must be discarded as Hg0 can be oxidized by
K2Cr2O7.
2) Insufficient Sn II has been added, which results in no Hg2Cl2 (a white
precipitate) forming. This indicates that all of the Fe3+ was not converted to the Fe2+
state. This sample must also be discarded.
Purpose
1. Test of procedual skills learned in Experiments I and II. Since this experiment
uses a primary standard solution directly, both your weighing techniques and how
precisely you detect your end point will effect your results.
2. To learn the subtleties of redox reaction which allow selective reaction in a
solution containing several different ions.
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Terms: Direct titration, oxidation, reduction, primary standard.
Procedure Overview
Procedure
1) On a clean, dry, preweighed unribbed watch glass, weigh 2.452X grams ± 0.1
gram of primary standard potassium dichromate (That is, weigh between 2.352X and
2.552X grams.) Record the weight to four decimal places.
4) Calculate the molarity of solution: Note that if the weight is not exactly 2.452
grams, the normality will not be exactly 0.1000. You are calculating molarity.
Formula:
1 mole K2 Cr 2 O7
grams K 2 Cr 2 O7 × × Purity
M.Wt. K 2 Cr2 O 7
Molarity K2 Cr 2 O7 =
Volume in liters
1) Weigh 0.35XX gram ( ± 0.1 gram) samples of the iron oxide unknown into 4
flasks. You may have to discard the other three samples and adjust the grams of
unknown used if the first titration uses more or less than 35 ml ± 5 ml. This is a
time saver gamble. If your first reduction of iron III fails you have back up unknown
samples prepared. However because the amount of iron varies in different unknowns,
the milliliters of titrant, potassium dichromate, used per unknown sample may fall out
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side the range of 30 to 40 milliliter. If this occurs, you will need to scrap the remaining
weighed unknowns and adjust your sample weights according to the ml/wt. ratio of
your first titration.
4) Dilute each solution to 15 ml with distilled water. This will usually dissolve any
precipitated salts.
Samples may be covered with plastic wrap and stored at this point.
From here on do each solution individually to completion.
1) In the hood, heat flask #1 with the Iron (III) solution to boiling. While the
solution is heating, prepare the chemicals for the prereduction step.
4) DROPWISE, add 0.5 M. Stannous chloride until the yellow iron solution is
reduced to light green ( Iron (II) ). You may not be able to detect the light green color of
the iron (II) unless your initial solution was very concentrated. The solution may simply
go from yellow to colorless or very faint green. Do not add more than 2 drops excess.
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8) Wait 3 minutes. If your reduction was carried out properly, the precipitate in
the flask will appear to be "silky white" at this point. The actual appearance depends on
the amount of excess stannous chloride added. Too much causes greying of the
precipitate and the loss of the silky appearance. A white precipitate should form, but
may appear cloudy. If no precipitate at all forms, there was no excess stannous
chloride, discard the sample. If the precipitate is dark grey or black, mercury metal
is present, discard the sample. While waiting the 3 minutes, clean and fill buret with
K2Cr2O7.
1) Prepare:
3) Place the flask on a magnetic stirrer and put a clean stirring bar in the
solution. Titrate slowly with potassium dichromate solution. The end point is a color
change from blue-green to grey to purple. At the grey point proceed titrating dropwise
to purple. After the endpoint is reached the color may revert back to grey or blue-green
if the solution stands for a while.
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5) Repeat steps from III. Prereduction of Iron (III) with the 3 remaining samples,
if titration of first was about 35 ml.
6) Calculations:
Formula:
6 mole Fe
Vol.(L)K 2 Cr 2 O 7 × M K 2 Cr 2 O 7 × × At. Wt. Fe × 100%
1 mole K 2 Cr 2 O7
% Fe =
gms unknown
Notes
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Notes
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Notes
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Notes
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