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Luke Steensen

Stephen Jackson

Tues 9:35 Desk 9

Preparation of an Iron Salt

Introduction

The purpose of this lab was to prepare potassium tris(oxalato) ferrate(III) trihydrate salt using a given
procedure and then determine the percent yield and the purity of the salt produced by that procedure.
The percent yield was determined by the final weight of the salt and its purity was established by
analyzing the oxalate, K+, and Fe+3 content.

Experimental

To prepare the salt, 7.5 g of Fe(NH4)2(SO4)2*6H2O was placed in a 250mL beaker and dissolved in 25mL of
warm water and 1mL of 6M sulfuric acid, followed by 35mL of prepared oxalic solution while stirring.
The mixture was then heated and stirred while yellow ferrous oxalate settled. The clear supernatant
liquid was then decanted from the mixture. The solid was washed with 25mL of hot water and decanted
a second time, and then 15mL of the prepared 1.8M potassium oxalate solution was added. This mixture
was heated to approximately 40*C. Then, 15-17mL of 7.5% H2O2 was slowly added with a dropping
pipette while stirring and maintaining temperature. The precipitate was then dissolved by heating the
solution to near boiling and adding first 8mL of oxalic acid and then up to an additional 6mL until the
dissolving completed. If this resulted in more than 60mL of solution, it was reduced to 50mL by heating
to near boiling. Finally, 15mL of ethanol was added to the solution before covering it with plastic wrap
and letting it cool to room temperature. Two weeks later, the crystals were gathered by using vacuum
filtration to dry out the solution.

The oxalate analysis was performed by first filling a clean buret with 0.1000N KMnO4. Approximately
0.10 grams of the salt were then dissolved in 20mL of 6M sulfuric acid and heated to boiling. The hot
solution was then titrated with the KMnO4 until it retained a permanent pink tinge. This analysis was the
repeated for a second trial.

The first step of the K + and Fe+3 analysis was to dissolve 0.20 grams of the salt in 10mL of warm water.
Two grams of the Dowex 50 resin was rinsed with deionized water until its pH matched that of the water
before being added to the salt solution. The mixture was swirled for about five minutes before being
poured into a 250mL beaker through filter paper contained in a funnel. The original beaker was washed
rinsed four to five times with the rinse always being poured through the filter paper before diluting the
resulting solution to 100mL of total volume. Two such samples were prepared. The beaker was placed
on the stirring motor and a stir rod was added. The electrode was lowered into the solution approximate
three quarters of an inch. The buret was prepared and positioned over the beaker for the addition of
0.1000M NaOH solution. The stirring motor was then started and the initial pH reading was near 2.20.
NaOH was added in 1mL increments, with the pH being recorded soon after each addition. Once the pH
reached 3.40, the addition was slowed to 0.5mL at a time. The increments returned to 1mL after the
reading reached 5.9 and until it reached 7.2, when it was again slowed to 0.5mL between readings. The
additions were continued until the pH was not changing by more than 0.1 from reading to reading. Each
of the pH values provided a point on the titration curve.

Results

Trial Mass of salt mL of KMnO4


1 0.10 10
2 0.10 10.2

pH Values
12

10

4
See appendix for table of values
2

0
0 5 10 15 20 25
mL NaOH

Calculations

Theoretical Yield

1 𝑚𝑜𝑙𝑒 𝐹𝑒(𝑁𝐻4 )2 (𝑆𝑂4 )2 ∙ 6𝐻2 𝑂 491.3 𝑔 𝐾3 𝐹𝑒(𝐶2 𝑂4 )3 ∙ 3𝐻2 𝑂


7.50 𝑔𝑟𝑎𝑚𝑠 × × = 9.40 𝑔𝑟𝑎𝑚𝑠
392.15 𝑔 1 𝑚𝑜𝑙𝑒

The actual weight was never measured, so percent yield cannot be calculated.
Oxalate Analysis

88 𝑔 𝐶2 𝑂4 2− 88 𝑔 𝐶2 𝑂4 2−
𝑉 (𝑁𝑀𝑛 𝑂4 − ) 0.0101 (0.1)
2 𝑒𝑞 2 𝑒𝑞
%𝐶2 𝑂4 = × 100 = × 100 = 44.4%
𝑠𝑎𝑚𝑝𝑙𝑒 𝑤𝑒𝑖𝑔ℎ𝑡 0.10

Ideal value: 53.8%

K+ Analysis
𝑔 𝑔
𝑉 𝑁𝑁𝑎𝑂𝐻 39.1 (100) . 0223 − 0.0118 0.1 39.1 (100)
𝑒𝑞 𝑒𝑞
%𝐾 = = = 20.53%
𝑠𝑎𝑚𝑝𝑙𝑒 𝑤𝑒𝑖𝑔ℎ𝑡 0.20

Ideal value: 23.9%

Fe3+ Analysis
𝑔 𝑔
𝑉 𝑁𝑁𝑎𝑂𝐻 55.85(100) . 0323 − .0223 . 1 55.85 (100)
3𝑒𝑞 3𝑒𝑞
%𝐹𝑒 3+ = = = 9.31%
𝑠𝑎𝑚𝑝𝑙𝑒 𝑤𝑒𝑖𝑔ℎ𝑡 0.20

Ideal value: 11.4%

Discussion and Conclusion

The given procedure for preparing the iron salt successfully produced the salt, but from the available
data it is difficult to determine just how effectively it did so. The mass of the salt product was never
weighed, so the percent yield value was never able to be determined. Instead, all insights must be
gleaned from the titration analyses. These experiments attempted to determine the purity of the
produced salt by finding out the mass ratios of its constituent parts. These values could then be
compared to the ideal molecular weight ratios to see how well they match up. If there were very little
difference between these values, it could be assumed that the salt being tested was very pure. In this
experiment, however, the mass ratios were consistently about fifteen to eighteen percent lower than
the ideal ratios. This seems to imply that the difference is made up of impurities in the salt, which would
mean that the percent yield of the process was around eighty to eight-five percent. This seems to be an
acceptably high value, but there are no other benchmarks for comparison.

In conclusion, the procedure being tested appears to produce a product that is over eighty percent pure.
Assuming the percent yield is a similarly high value, this process seems to be an entirely feasible method
for obtaining the desired salt.
Appendix

mL NaOH pH Values
0 2.27
1 2.31
2 2.36
3 2.43
4 2.53
5 2.66
6 2.9
7 3.25
8 4.33
8.5 4.69
9 5.04
9.5 5.4
10 5.71
10.5 5.91
11.5 6.16
12.5 6.35
13.5 6.45
14.5 6.6
15.5 6.75
16.5 6.95
17.5 8.06
18 9.32
18.5 9.8
19 10.09
19.5 10.27
20 10.37
20.5 10.46
21 10.53
21.5 10.59
22 10.63