Experiment # 5
DETERMINATION OF IRON IN IRON SUPPLEMENTS BY REDOX TITRATION
De Jesus, Mirra P.
Group Mates:
Bautista, Angelic Russel
Macañas, Micah
October 10, 2014
Introduction An oxidizing agent oxidizes the other
substance by stripping off electrons from it
while a reducing agent reduces the other
In this experiment, it involves a type of substance by donating electrons to it. Oxidation
reaction which is the oxidation and reduction or and reduction reactions always occur
simply redox reaction. It exhibits the titration of simultaneously. One cannot take place in
an oxidizing agent (or oxidant) with a reducing isolation from the other. During a redox
agent (or reductant) or vice versa. There must reaction the oxidizing agent itself undergoes
be a sufficiently large difference between the reduction while the reducing agent undergoes
oxidizing and reducing capabilities of these its oxidation.
agents for the reaction to undergo completion
with a sharp end point. Oxidation process
involves loss of electrons The objectives of this experiment is (1)
while reduction process involves gain of to learn the technique and calculations
electrons, thus an oxidizing agent is one which involving back titration, (2) to illustrate the use
accepts electrons while a reducing agent is one of self-indicating agent; and (3) to determine
which loses the electrons. the iron content of a sample using an oxidation-
reduction type of reaction.
A useful mnemonic for this is:
Methodology
LEO (the lion) goes GER, which means
that:
Loss of Electrons is Oxidation Before doing the procedures of the
experimentation, the following materials were
Gain of Electrons is Reduction
prepared by our group and some by the
Or, facilitator: 600 mL beaker, 250 mL beaker, 50
mL graduated cylinder, 250 mL Erlenmeyer
OILRIG, which is: flasks to be used as a container for the analyte
Oxidation Is Loss of electrons during titrations, 100 mL volumetric flask, 50 mL
burette, 10 mL pipets, watch glass, sintered
Reduction Is Gain of electrons
glass or Gooch filtering crucible, suction or
filtering flask, vacuum pump, thermometer,
stirring bar, top-loading balance, analytical
1
balance, hot plate, mortar and pestle to grind and kept in the dark
the tablets, AR grade KMnO4, AR grade Na2C2O4, except when it was not
18 M H2SO4, glass stoppered amber bottle and used.
iron supplements tablets.
Setting aside the
Figure 1: Illustration of the brand of Iron KMnO4 solution,
tablets used approximately three 0.2
grams of dry sodium
oxalate or Na2C2O4 were
indirectly weighed and Figure 2 Standardized
transferred to three 0.02 N KMnO4 solution in
labeled 250 mL a glass-stoppered amber
Brand name of the
Erlenmeyer flasks bottle
iron tablet
respectively. To
prepare for the sulfuric acid, from the 18 M
H2SO4 that was given 28 mL had to be pipet out
and moved into a beaker filled with 500 mL
distilled water to obtain 1 M of sulfuric acid. 75
ml of the prepared acid was consequently pipet
out and allocated to each of the Erlenmeyer
flasks containing sodium oxalate to dissolve the
solids. These three were heated to 80-90
Illustration of the degree Celsius on a hot plate and using a
iron tablet thermometer to regulate the temperature. Into
another Erlenmeyer flask, only 75 mL of the
prepared 1 M sodium oxalate was pipet out and
boiled with the other 3 Erlenmeyer flasks under
the same conditions in able to perform the
blank titration. The blank titration was first
performed to opt to know when the moles of
The first to be done was ‘Procedure A’ the solution of the sodium oxalate will equate
which is the preparation and standardization of to the moles of the solution of the potassium
0.02 N KMnO4 solution. From the prepared permanganate. Maintaining the required 80 to
materials, reagent-grade potassium 90 degree Celsius, the Erlenmeyer flasks,
permanganate crystals were weighed up to 1.6 containing mixed solutions of sodium oxalate
grams out on a watch glass using an analytical and sulfuric acid, were reheated before titrating
balance. The crystals were transferred on an it with potassium permanganate. Obtaining an
empty 600 mL beaker to be filled with 500 mL endpoint wherein a faint pink color persists for
of distilled water to dissolve the potassium about 30 seconds, the subsequent readings of
permanganate crystals and boiled for about 10 each trials were recorded to compute for the
to 15 minutes. After boiling the solution the normality of potassium permanganate.
beaker was covered and left overnight in the
locker for the particles to settle. Continuing the
procedure, it was filtered through a filtering
crucible connected to a vacuum pump then
stored in a clean, glass-stoppered amber bottle
2
In the next step which is the analysis of
iron tablets in ‘Procedure B’, about 1 gram of
the summation of weights of the tablets were
needed and three tablets were used in this case
because each of the tablets weighs about 325
mg. These tablets were first weighed in the
analytical balance to record its original weight,
after confirming that it does not exceed 2 grams
it was grind up using mortar and pestle. The
ground iron tablets were then placed in a
beaker and poured with 50 mL of the acquired 1
Figure 3 Ground Iron M H2SO4 and was swirledFigure 4 Volumetric
to dissolve theflask
solids
tablets with dissolved Iron
in the solution. It was left to stand for a short
tablets
time to let the residues settle at the bottom,
then filtered into a 100 mL volumetric flask. The
beaker, where the iron tablets were dissolved,
as well as the filter paper were washed several
times, adding the washings to the volumetric
flask. 1 M H2SO4 was added to fill it up to its
indicated mark in the volumetric flask. 10 mL
aliquot was pipet out to each of the three 250
Erlenmeyer flasks added with 10 mL of 1 M of
sulfuric acid. The mixed solutions inside the
Erlenmeyer flasks were titrated with the
standardized potassium permanganate until
there was an observed faint pink color and the
endpoint was achieved.
Result and Discussion
Figure 5:
Standardization of Trial 1 Trial 2 Trial 3
0.02N KMnO4
Final Mass of Na2C2O4
46.3194 g 46.1199 g 45.9145 g
and vial (±0.0001g)
Initial Mass of Na2C2O4
46.5128 g 46.3194 g 46.1199 g
and vial (±0.0001g)
Mass of Na2C2O4,
0.1934 g 0.1995 g 0.2054 g
(±0.0001g)
Initial burette reading
14.71 mL 0.00 mL 17.50 mL
(±0.05mL)
Final burette reading
42.15 mL 28.51 mL 46.96 mL
(±0.05mL)
Volume KMnO4 used
27.44 mL 28.51 mL 29.46 mL
(±0.05mL)
3
Initial burette reading
in blank titration 14.53 mL
(±0.05mL)
Final burette reading in
blank titration 14.43 mL
(±0.05mL)
Volume KMnO4 used in
blank titration 0.10 mL
(±0.05mL)
Corrected KMnO4
27.34 mL 28.41 mL 29.36 mL
(±0.05mL)
Normality of KMnO4 0.1056 ± 0.001901 N 0.1048 ± 0.001834 N 0.1044 ± 0.001771 N
Mean Normality
0.1049 ± 0.001835 N
KMnO4
Standard Deviation 0.0006124
Relative Standard
0.5838
Deviation
Figure 6: Analysis of
Trial 1 Trial 2 Trial 3
Iron Tablets
Generic and Brand
RHEA: Ferrous Sulfate
name of sample
Mass of sample 1.3747 g
Number of tablets used 3 tablets
Initial burette reading
15.12 mL 18.00 mL 24.00 mL
(±0.05mL)
Final burette reading
17.56 mL 21.00 mL 26.81 mL
(±0.05mL)
Volume KMnO4 used
2.44 mL 3.00 mL 2.81 mL
(±0.05mL)
Mass of Iron in sample 142.9 ± 0.02694 mg 175.7 ± 0.02416 mg 164.6 ± 0.02495 mg
Mass of Iron per tablet 47.63 ± 0.02694 mg 58.57 ± 0.02416 mg 54.87 ± 0.02495 mg
Mean mass of Iron per
53.69 ± 0.02702 mg
tablet
Manufacturer’s
indicated weight per 325 mg
tablet
Manufacturer’s
indicated amount of 65 mg
iron content per tablet
Relative Error (ppt) 174.0 ppt
4
Figure 7: Results of Titration of sodium
oxalate and sulfuric acid with potassium
permanganate
Endpoint of titration
of trial 3 in
standardization of
KMnO4
Endpoint of blank
titration of 1 M H2SO4
and KMnO4 solution
Regarding the procedure of preparation
and standardization of potassium
permanganate, the dissolution of KMnO4
crystals in distilled water had to be boiled
because the water added to it may contain
Endpoint of titration some impurities that reduces permanganate. In
of trial 1 in order to eradicate this, it is done through
standardization of boiling because it will hasten the oxidation and
KMnO4 coagulate the precipitate of manganese dioxide
which is a reducing agent, then filtered to
eliminate MnO2. In standardizing the
concentrated sulfuric acid, 28 mL had to be
used because of the subsequent equation:
( Χ ) ( 18 Μ ) =( 500 mL ) (1 Μ )
Χ =(500
( mL )( 1 Μ )
Endpoint of titration 18 Μ )
of trial 2 in Χ =27 .78≈28 mL
standardization of
KMnO4 The corrected volume used in the succeeding
computations had to be taken into
consideration for accurate measurements,
which is illustrated below:
5
CV =V standardization −V blank titration 2 KMnO 4 +5 Na2 C2 O 4 +8 H 2 SO4 →
T 1=27 . 44−0. 10=27. 34mL K 2 SO 4 +2 MnSO 4 +5 Na 2 SO 4+10 CO 2 +8 H 2 O
T 2=28 . 51−0. 10=28. 41mL In this reaction, MnO4- is reduced to
T 3=29. 46−0. 10=29 . 36mL Mn+2 and Na2C2O4 is oxidized to CO2.
And to compute for the normality of potassium Taking note that the substance that
permanganate, meq of the C2O42- had to be oxidized is known as reducing agent
equated to that of the meq of MnO 4-, with the while on the contrary, the substance
given equivalent weight of sodium oxalate that reduces is known as an oxidizing
which is (134 mg/mmole)/2. agent in the redox reaction. Thus, we
can conclude that the oxidizing agent is
Wt NaC2 O 4 the permanganate ion and sodium
=N KMnO V KMnO oxalate as the oxidized substance is the
EW NaC O 2 4
4 4
reducing agent.
Wt NaC O
N KMnO = 2 4
4
( 67 mg
mmole ) ( V KMnO )
4 To determine the percentage by mass
of iron (II) sulfate in each tablet, mass of iron in
T 1=193mg. 4mg =0 . 1056 N sample was calculated first, minding that the
( 67 mmole ) (27 . 34 mL ) EW of Fe is (55.845 mg/mmole)/1.
199 .5 mg
T 2= =0 .1048 N
( 67 mg
mmole )
( 28. 51 mL) Mass Fe in sample
EW Fe
=
4 4
100
( N KMnO ) ( V Analysis of Fe KMnO ) ( 10 )
205. 4 mg
T 3= =0 . 1044 N
( 67 mg
mmole )
( 29 .36 mL ) Obtaining their respective results, these values
were used to attain the mass of iron per tablet,
The standard deviation obtained is 0.0006124
Χ1
which dictates how minimally spread our data M Fe =
was and to represent it in percentage, relative Number of Fe tablets used
standard deviation was used wherein, 142.9
T 1=3 =47.63mg
RSD=SD
Χ
×100 T 2=175
3
.7
=58.57mg
0. 0006124
¿ 0. 1049 ×100 T 3=164.6
3
=54.87mg
¿ 0 .58 % Computing for the relative error expressed in
Since RSD deals with the precision of the data, ppt,
the smaller the RSD yields a precise data. Solved Fe-Expected Fe
RE=Expected Fe ×100
|47 . 63−65|
T 1=65 ×100=267 . 2 ppt
1. What chemical species is the reducing |58. 57−65|
agent in the standardization step? The T 2=65 ×100=98 . 92 ppt
oxidizing agent? . 87−65|
T 3=|54
65
×100=155. 8 ppt
( 267. 2)+( 98 . 92)+(155. 8 )
In the standardization step, the reaction Χ =3 =174 .0 ppt
involved is:
MnO−4 +8 H + +5 e− →Mn +2 + 4 H 2 O
6
2. Other oxidizing agents are also oxidized to iron (III) ions by potassium
employed for the determination of iron permanganate in acidic solution. In acidic
in an unknown sample. What is one conditions the deep purple solution of
obvious advantage of KMnO4 over permanganate ions is reduced to a very pale
K2Cr2O7 and Ce (SO4)2 as oxidant in the pink solution of manganese (II) ions. This
determination of iron? solution is so pale as to appear colorless when
The potassium permanganate solution dilute and, in practice, the marked difference in
that was added from the burette to the color between these two oxidation states is
solution of the reducing agent was useful as an end-point for this redox reaction.
immediately decolorized.
Permanganate acts as self-
–
indicator. Since MnO4 is intense purple Although the calculated mass of iron in
while Mn+2 is colorless, the reaction each tablet were less of that compared to the
mixture at equivalence point is colorless original, it was due that during the preparation
and even a single drop of the it was filtered first before adding sulfuric acid to
permanganate would impart sufficient the medium, as a consequence not all of the
pink color to the solution acting as self- iron were included in the solution and possible
indicator and no other indicator is errors were accounted unto it.
required.
3. What are the reasons for using 1M
H2SO4 in the standardization of KMnO 4
and in the preparation and analysis of References
iron tablets?
H2SO4 or sulfuric acid is
“Oxidation & Redution”. Web. 10 October 2014.
considered to be a strong acid and
<http://fc.sjsd.net/~gjohnson/FOV1-
conventionally, permanganate ion in
00053FB3/Chapter%2009.pdf>.
the acidic medium is a very strong
oxidizing agent. The main reason for
using acid in the titration is that it
"Redox titrations". Web. 10 October 2014.
transforms oxalate to oxalic acid and
<http://alevelchem.com/aqa_a_level_c
this acid solution reduces the KMnO4.
hemistry/unit3.6/inorg01.htm>.
Any side reaction may hamper the
result. So only sulfuric acid should be
used to maintain a strongly acidic
solution. Also, it should always be in Jain, Manisha. "Redox Titration". Web. 10
excess otherwise insoluble brown October 2014.
manganese (IV) oxide (MnO2) will form. <http://eduframe.net/andc/chemistry/
Che01/Redox%20Titrations%20only
%20-%20Final.htm#1>.
Conclusion
Wasserman, Robin. "Does Sodium Oxalate
React With Potassium Permanganate?".
All of the objectives indicted in the
Web. 10 October 2014.
introduction were met. Iron (II) ions can be
7
<http://www.livestrong.com/article/28
6203-does-sodium-oxalate-react-with-
potassium-permanganate/>.
Islam, Nashid Noor. "Standardization of
Potassium Permanganate solution with
Standard Sodium Oxalate Solution
". Web. 10 October 2014.
<http://alamsworld.weebly.com/upload
s/4/4/9/7/4497549/chemistry-07.pdf>.
"Redox Titration". Web. 10 October 2014.
<http://chemistry.tutorvista.com/analy
tical-chemistry/redox-titration.html>.
