Determination of Percent Potassium and Percent Iron

During the analysis of a green crystalline compound, KxFey(C2O4)z.aH2O will determine

both the percent potassium and percent iron. The % K and % Fe will be obtained by carrying out
a pH titration after passing a solution containing a known mass of the compound through an ion
exchange column to prepare for analysis. The ion exchange column contains a resin which are
solids that are insoluble in water. Ion exchange resins are made up of large molecules containing
ionizable groups. The ionizable portion of the resin molecule to be used in this experiment is a
sulfonic acid group (-SO3-H). This group ionizes in the presence of water.
X-SO3-H ---------------> X-SO3-1 + H+1
The X represents the resin. H3O+ is the hydronium ion which ends up bonding with the
sulfonate on the resin. The resin is the cation this is because other cations can be substituted for
H3O+ (the acid form of the resin). When a combination of the resin and water is poured into a
glass tube, plastic column or buret, with a cotton plug at the bottom to hold the resin in and let
excess water flow out, a workable ion exchange column is obtained. When a massed sample of
the green crystalline compound is dissolved in water, the salt dissociates by the equation:
KxFe(C2O4)y zH2O -----------------> xK+(aq) + Fe(C2O4)yx-(aq) + zH2O
The number of moles of K+ in the solution of the green crystalline compound
is equal to the number of moles of H3O+ in the solution that comes off the
resin column. The number of moles of H3O+ and thus the number of moles
of K+ can be determined by doing an acid-base titration using a standardized
solution of NaOH:
mol K+ = mol H3O+ = molNaOH used in titration = VNaOH(in liters)
MNaOH
The mass of K+ can be obtained from the number of moles:
mass K+ in sample = mol K+ 39.1 g/mol
The percent potassium can be calculated:
%K = [(mass of K+ in sample)/(mass of sample of crystal)] x 100
Notice that iron comes through the ion exchange column in the form of
Fe(C2O4)yx- . When the solution from the ion exchange column is titrated with
standardized NaOH solution, the reaction that takes place first is given by the
equation:
H3O+ + OH------------>2H2O
Once all of the acid (H3O+) has reacted, further addition of NaOH results in
the reaction of Fe(C2O4)yx- by the following equation:

Fe(C2O4)yx-(aq) + 3OH-(aq) ---------------->Fe(OH)3(s) + yC2O42-(aq)

The Fe(OH)3 precipitates from solution as a rust colored precipitate. The
equation shows that three moles of OH- from the NaOH are needed to react
with one mole of Fe in Fe(C2O4)yx-.
mol Fe = VNaOH(in liters) MNaOH 1 mol Fe
3 molNaOH
The mass of Fe can be calculated from the number of moles.
mass Fe = mol Fe 55.8 g/mol
Since the mass of the green crystalline compound is known, the percent iron
can be determined.
%Fe = [(mass Fe)/(mass of crystalline compound)]x100
The solution obtained from the ion exchange column is to be titrated with a
standard solution of NaOH. A pH meter is used to follow the reaction. A
titration curve of pH versus number of mL of NaOH solution added will be
graphed. The curve will have two equivalence points as shown in the figure
below:

The volume of NaOH solution needed to reach the first equivalence point (V1)
along with the molarity of the solution can be used to calculate the number
of moles of OH- needed to neutralize the H3O+. The volume of NaOH solution
required to go from the first equivalence point to the second equivalence
point (V2-V1) along with the molarity of the solution is used to calculate the
number of moles of OH- needed to combine with iron.
Using the same steps above with MNaOH = 0.10524M, sample 1 have
mass is 0.1538g, V1 is 8.80mL and V2 is 17.60mL. And sample 2 have mass is
0.1570g, V1 is 8.6mL and V2 is 17.50mL. the result is:
Sample 1

Sample 2

% K+
%Fe

23.54%
11.05%

22.55%
10.80%

Determine percent of H2O

From the formula of Green Cystal, KxFey(C2O4)z.aH2O, it should be apparent that
the substance is a hydrate. Hydrates are inorganic compounds with water molecules bound to
them. In hydrated compound a fixed number of water molecules, called the water of hydration,
are chemically combined with the metal ion. In this part of the analysis, the mass of water in the
hydrated Green Crystal will determine by measuring the mass of the substance before and after it
is dehydrated by heating in order to determine the mass of water lost in the process.
Sample 1
Sample 2
Mass of
44.0015g
44.2529g
empty
crucible
(gram)
Mass of
45.0799g
45.2615g
crystal and
crucible
Mass of
1.0784g
1.0086g
crystal
(gram)
Constant
44.8921g
45.0867g
mass of
crystal and
crucible
(gram)
Mass of
0.1878
0.1748g
anhydrous
Green crystal
(gram)
Percentage of 17.41%
17.33%
water in
Green Crystal
Determine the empirical formula of the Green Crystal
Assume there are 100 grams of the Green Crystal:
Sample 1
grams
Molar Mass
Moles
Relative
(grams/mol)
moles
Iron
11.05g
55.8
0.20
1
Potassium
23.54g
39
0.60
3
Hydrate
17.41g
18
0.97
5
(H2O)
Oxalate
48.00g
88
0.55
3
2(C2O4 )

The empirical formula: K3Fe(C2O4)3.5H2O

Sample 2

Grams

Ion
Potassium
Hydrate
Oxalate

10.83g
22.55g
17.33g
49.29g

Molar Mass
Moles
Relative
(grams/mol)
moles
55.8
0.19
1
39
0.58
3
18
0.96
5
88
0.56
3
The empirical formula: K3Fe(C2O4)3.5H2O

Theoretical yield and % yield

Sample 1
Sample 2
Mass of pure Green
6.7867g
Crystal synthesized
(grams)
A complete balanced chemical equation for the synthesis of the Green
Crystal.
FeCl3.6H2O
+ 3K2C2O4.H2O - K3Fe(C2O4)3.5H2O + 3KCl + 2H2O
8.00mL of 2.50M
0.02mol
0.02mol
Based on the exact masses of the two starting materials used for the
synthesis, the theoretical of the Green Crystal: (0.02mol crystal) x (527
g/mol)=10.54 g
%yield =(experimental yield / theoretical yield) x 100
%yield

Sample 1
64.39%

Sample 2

Ultraviolet light investigations

,nm
A
,nm
A
,nm
A
400
500
0.381
600
1.46
420
520
0.314
620
0.021
440
0.925
540
0.190
640
-0.045
460
0.622
560
0.081
660
-0.147
480
0.418
580
-0.032
680
-0.276
The maximum of absorbance was measured at 440nm. Therefore,
spectrophotometric analysis of the sample is carried out at 440nm. In
difference solvent, we have the difference physical properties; it is affected
to the absorbance increases or decrease at different wavelength.