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EXPERIMENT 20

I. Identity
a. Title

Determination of iron ion concentration in Sangobion by


permanganometric titration.

b. Objective

To determine concentration of iron ion in Sangobion by


permanganometric

c. Day/Date

Monday, 13th May 2011

d. Department/Faculty

Chemistry education department/ Mathematic and Sciences

e. Names of group

II. Background
Theorytical
Iron is one mineral that is needed by the body. In the human body there are
approximately 3.5 to 4.5 grams of iron, in which two thirds are found in the blood, while the rest
are found in the liver, bone marrow, and muscle. It is role in the production of red blood cells are
very famous. The recommended amount of iron per day is 18 mcg. Iron is useful to help the
formation of hemoglobin in red blood cells and prevents of anemia.
Red blood cells are containing a protein called hemoglobin, and each has one atom of
hemoglobin iron. This is the iron in hemoglobin that binds oxygen in the blood in the lungs to be
distributed throughout the body. After removing oxygen, hemoglobin is binding of carbon
dioxide (CO2) to be secreted by the lungs.
Function
1. Iron has a role in the process of cell respiration, namely as a cofactor for the enzyme
involved in the oxidation reduction reaction.
2. Energy metabolism, in each cell, iron work with electron transport chain proteins that has a
role in the final step of energy metabolism. A total of more than 80% iron in the body is in
hemoglobin.
Impact
Disadvantages
The reduced work ability, lack of energy in general causes pale, weakness, fatigue, dizziness,
loss of appetite, reduced fitness, immunity and impaired wound healing, and the ability to
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regulate body temperature decreased, and difficulty breathing (gasping breath), a beating heart
faster, fatigue, difficulty concentrating, can not sleep well, pain during menstruation, the tip of
chapped lips, eye irritation, and even hair loss.
Livron B Plex and supra livron are the food supplements that contain iron. Iron contained
in Livron B Plex and supra livron are the form of ferrous gluconate (C12H24FeO14). To
examine the content of Fe2 +, then the experiment was conducted using the titration
permanganometri.

Ferrous gluconate

Dasabion is also one of the food supplements that contain iron. Iron contained in
dasabion is the form of iron (II) fumarat (C12H24FeO14). To examine the content of Fe2 +, then
the experiment was conducted using the titration permanganometri.

Iron (II) Fumarat

Permanganometri titration is oxidationmetric titration using standard solution of


potassium permanganate (KMnO4). In the redox reaction of KMnO4 as an oxidator will occur a
reduction reaction. One drop of 0.1 N permanganate gives a clear pink color on the volume of
solution which is used in a titration. This color is used to indicate the excess reagent.
Permanganate undergoes various chemical reactions because manganese can be present with
oxidation number +2, +3, +4, +6, +7. Its ability to capture the electron is determined by the
acidity of the solution ion-MnO4. Reduction reactions experienced by ion MnO4 are as followsMnO4-(aq) + 8H+ (aq) + 5e

Mn2+(aq) + 4H2O(l)

Permanganate reacts rapidly with many reducing agents based on the reaction, but some
substances require heating or the use of a catalyst to accelerate the reaction. Permanganate is an
oxidizing agent element that is strong enough to oxidize Mn (II) to MnO2 in accordance with the
equation
3Mn2+(aq) + 2MnO4-(aq) + 2H2O(l)

5 MnO2(s) + 4H+(aq)

Little excess of permanganate is present at the titration end point is sufficient to result in
the precipitation of MnO2. However, given the slow reaction, MnO2 not normally precipitated at
the end point of the titration of permanganate.
Permanganate solutions are unstable acidic because the permanganate acid decomposes
according to the equation:
MnO4-(aq) + 4H+ (aq) + 5e

MnO2(s) + 2H2O(l)

MnO4-(aq) + 2H2O(aq) + 3e

MnO2(s) + OH-(aq)

From the equation above can be seen that KMnO4 most powerful oxidizing properties
occur in a very sour mood. For the reduction reaction of KMnO4, Mn2+ is necessary to prevent
the formation of the intermediate results in the form of a brown MnO2 by titration in hot
conditions.
Aquades used to dissolve the solid KMnO4 must certainly have been free from organic
substances capable of reducing KMnO4. To prevent this, a solution of KMnO4 boils it first.
Furthermore, after the cold it is filtered using a glasswol filter or sinterglas. To avoid KMnO4
decompose by air, this solution is stored in dark bottles.
As a secondary standard solution, before being used to standardize a reducing, KMnO4
will be standardized with primary standard solution. Primary standard solution is a reducing
agent, such as sodium oxalate (Na2C2O4). This reaction was slow at room temperature, so the
solution is usually heated to around 60-70oC. Even at higher temperatures the reaction started
slowly, but speed increases when the ion manganese (II) is formed. Manganese (II) acted as a
catalyst and the reaction is called autocatalytic gripped, because the catalyst is produced in the
reaction itself. Ions can provide catalytic effect in a way to react quickly with permanganate to
form manganese oxidation conditioned medium (+3, +4), whereas in turn rapidly oxidizes
oxalate ion to the divalent state. Standardized potassium permanganate can be used to determine
the concentration of reducing agent, such as ferrous ions. Redox reactions that occur are as
follows:
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2 MnO4-(aq) + 16H+ + 5C2O4 (aq)

2 Mn2+(aq) + 8H2O(l) + 10CO2(g)

MnO4-(aq) + 8H+ + 5Fe2+(aq)

Mn2+(aq) + 5Fe3+(aq) + 4H2O(l)

Based on the redox reaction is occurred, then the indicator will show that the equivalent
point has been achieved, indicated by the color change from transparent solution became purple.
This change occurs when KMnO4 is used as titrant (Selamat and Lanang, 2004).
III. Experiment Methods
Chemical Apparatus
Apparatus
- Measuring flask 250mL

Number
1 unit

Volumetric Pipette 10mL

1 unit

Analytical balance

1 unit

Erlenmeyer flask 100mL

1 unit

Erlenmeyer flask 250mL

3 unit

Burette

1 unit

Beaker glass 500mL

1 unit

Beaker glass 100mL

1 unit

Small funnel

1 unit

Drop pipette

2 units

Statif and clem

1 set

Watch glass

2 units

Spatula

2 units

Erlenmeyer flask 250mL

3 units

Heater

1 unit

Petri disk
Materials

Materials
- Na2C2O4 (s)

Amount
1,675 gram

KmnO4 p.a

0,813 gram

Aquades

Enough

C12H24Fe O14

gram
4

C4H2FeO4

H2SO4 1N

10 mL

Procedures
1. 0.790 gram of KMnO4 was weighting and was entered into the beaker glass 500 mL.
2. It was added by 250 mL of aquades and was stirred until it was dissolved completely. The
solution was boiled in 10 minute in closed condition (beaker glass was closed by using
watch glass).
3. After cooled, it was filtered by using funnel in glasswol. The filtrate that got was saving
in dark bottle (brown).
4. Sodium oxalate was dried in oven in temperature is 110 0C in 1-2 hours and was cooled in
decicator until room temperature.
5. Aquades 50mL was poured into measuring flask. Sodium oxalate was weighting 1.675
gram and was entered into the measuring flask 250mL. It was added by aquades until the
volume is 250mL.
6. 25mL of Na2C2O4 solution was entered into the measuring flask and was added by 3mL
of H2SO4 1 N. The solution was heated until the temperature was 700C.
7. The solution was titrated by KmnO4 solution until the color of solution is pale purple
(still purple in 30 second).
8. In this titration, the shaken was done completely.
9. The volume of titrant that was used was noted and was repeated in three times.
10. 25mL of Fe2+ salt solution (0.1N) was poured into Erlenmeyer 250 mL and was added by
3mL of H2SO4 1N.
11. The solution was heated until the temperature is 70 0C. It was titrated by KMnO4 solution
until the color of solution is pale purple (still purple in 30 second).
12. The volume of titrant that was used was noted and was repeat in three times
13. The concentration of Fe2+ was determined.
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IV.

Experiment Results and Discussion


Experiment Results

No
1

Procedures
Experiment Results
0.79 gram of KMnO4 was weighting and KMnO4 like crystal has dark violet color. The
was entered into the beaker glass 500mL

mass of KMnO4 is 0,790 gram

[KMnO4] = 0,1 N = 0,02 M (because n =


5)
Mr KMnO4 = 158
mass = mol x Mr
=0,02 M x 0,25 L x 158
= 0,790 gram

Picture 03. KMnO4 crystal


250 mL of aquades was added and the 0.790 gram of KMnO4 is dissolved into 250
solid of KMnO4 was stir until all of the mL aquades produce violet solution
solid of KMnO4 is dissolved. In close
condition that solution take place in
wacth glass was heated for 10 minutes

Picture 04. KMnO4 solution


Filtering that solution after cool by using Filtrate that violet color is produced and there
funnel and its glaswol. The filtrat that is little precipitate on filtering paper
get was save in the bottle.
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Picture 05. Little precipitate


Sodium oxalate was dried in oven in Na2S2O4 is white powder
temperature is 1100C in 1-2 hours and
was cooled in decicator until room
temperature.

Aquades

50mL

was

Picture 06. Na2S2O4 powder


into Na2C2O4 0.1 N

poured

measuring flask. Sodium oxalate was - [Na2C2O4] = 0,1 N = 0,05 M


weighting 1.675 gram and was entered N= M x n
into the measuring flask 250mL. It was M = 0.1/2
added by aquades until the volume is =0.05 M
250mL
[Na2C2O4] = 0,1 N = 0,05 M (because

- Mol Na2C2O4 = 250 x 0.05

the amount of electon thats released is 2) = 1.25 x 10-2 mol


follow by equation below:
C2O42-(aq)

2CO2(g) + 2e

Mr Na2C2O4 = 134
Massa

= Mol x Massa molar


=

M.

Na2C2O4

V.

Na2C2O4 x Mr. Na2C2O4


= 0,05 M x 0,25 L x 134 gram/mol
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= 1,675 gram
Picture 07. Na2S2O4 powder
25mL of Na2C2O4 solution was entered Na2C2O4 is colorless solution
into the measuring flask and was added
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by 3mL of H2SO4 1 N. The solution was


heated until the temperature was 700C.

Picture 08. Na2S2O4 solution


The solution was titrated by KMnO4 KMnO4 solution is violet color. Titration was
solution until the color of solution is pale stopped until the solution become pink.
purple (still purple in 30 second).
In this titration, the shaken was done When titration can be used stirer. This has
completely.

purpose that shacked done. It was used


magnetic stirred.

Pictures 09. KMnO4 Standardization


The volume of titrant that was used is Titration
Volume (mL)
I
24.45
noted and titration was repeated in three
II
24.48
times. In this titration the volume of III
24.52
average
24.48
titrate that was used is 25.00mL.
2M equivalent C2O4 = N x V
= 0.1 x 25.00
= 2.5 m equiv.
M equivalent C2O4 2-= M equivalent MnO4Meqiv = N MnO4- x V MnO4Meqiv = N MnO4- x 24.48
N MnO4- = 0.102 N

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Livron B Plex
25mL of Fe2+ salt solution (0.1N) was N Fe2+= 0.1 N
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, V Fe2+= 100 mL= 0.1 L

poured into erlenmeyer 250mL and was N Fe2+= M.n


added by 3mL of H2SO4 1N.

0.1 = 1 (( gr/Mr)/(1000/100))
Gram Fe 2+= (0.1 x 169.901x 100 mL)
= 1.69 gram
So, to make 100 mL of Fe 2+ solution must
dissolved 1.69 gram of Livron B plex is equal
with 9 capsule.

Dasabion
25mL of Fe2+ salt solution (0.1N) was

N Fe2+= 0.1 N

poured into erlenmeyer 250mL and was

, V Fe2+= 100 mL= 0.1 L

N Fe2+= M.n

added by 3mL of H2SO4 1N

0.1 = 1 (( gr/Mr)/(1000/100))
Gram Fe 2+= (0.1 x 448.156x 100 mL)
= 4.5 gram
So, to make 100 mL of Fe 2+ solution must
dissolved 4.5 gram of dasabion is equal with 9
capsule.

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The solution was heated until the The color of solution is


temperature is 700C. It was titrated by
KMnO4 solution until the color of
solution is pale purple (still purple in 30

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second).
The volume of titrant that was used is Livron B Plex
noted and titration was repeated in three
times. Volume of titrate is 25.00mL.

Titration
Volume (mL)
I
0.8
II
0.7
III
0.6
Average
0.6
M equivalent MnO4 = M equivalent Fe2+
N.V MnO4- = N .V Fe2+
0.102 x 0.7 = N x 25.00
N Fe 2+= 2.448 x 10-3 N

Dasabion
Titration
Volume (mL)
I
15.8
II
15.8
III
15.9
Average
15.9
M equivalent MnO4-= M equivalent Fe2+
N.V MnO4- = N .V Fe2+
0.102 x 15.9 = N x 25.00
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The

concentration

of

Fe2+

N Fe 2+= 0.064872 N
was Livron B Plex

determined.

N=Mxn
gr / ArFe 2
0.1L

N = 1

gr / 56

0.05L

2.856 x 10-3 N = 1

Mass Fe 2+= 0.00799 gram = 7.99 mgram


Dasabion
N=Mxn
gr / ArFe 2
N = 1
0.1L

gr / 56

0.1L

0.064872 N = 1

Mass Fe 2+= 0.363 gram = 363 mgram


Discussion
Making standard solution of KMnO4

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In this experiment will be the determination of Fe2+ ion in solution was done by titration
permanganometric. In this titration the titrant is acting as KMnO4 solution while the salt solution
Fe2 + as its titrate. Standard solution of KMnO4created by 0790 grams of KMnO4 was dissolved
in 250 mL aquades. From this process will form a purple solution. And then was boiled for 10
minutes. This warming aims to prevent the formation of the intermediate results in the form
MnO2 thats have brown color. After the solution is boiled and then is filtered. The filtrate
obtained from this screening are colored purple and there is little precipitate attached to the filter
paper. As a secondary standard solution, before being used to standardize a reductant will be
standardized KMnO4 solution prior to the primary standard. Primary standard solution is a
reducing agent, in this experiment the primary standard solution used is sodium oxalate
(Na2C2O4).
Preparation of Primary standard solutions of Na2C2O4 0.1 N
To making a primary standard solution Na2C2O4 done by weighing as much as 1.675 grams
of sodium oxalate and subsequent drying of the sodium oxalate is aiming to make the mass of
sodium oxalate into constant given the nature of the sodium oxalate is hygroscopic. Once that
phase is completed, the sodium oxalate is inserted into the 250 mL measuring flask previously
filled with 50 mL of water and whipped until it dissolves. The continually added by aquades to
limit the measuring flask.
Standardization of KMnO4 solution by the primary standard solution Na2C2O4 0.1 N
Standardization is a way to determine the appropriate concentration of standard solution. One
way that can be used to standardize is by titration. Terms of use titration for standardization is to
have available a solution whose concentration is known precisely. Solution in question is the
primary standard solution. This solution was made from the primary standard substance, that is a
substance concentration of the solution can be directly determined from weigh a certain amount
of these substances and dissolving it in a certain volume.
KMnO4 solution can be standardized with a solution Na2C2O4, where KMnO4 solution as
titrant and solution of Na2C2O4 as its titrate. 25.0 ml of Na2C2O4 0.1 N entered into the
erlenmeyer and added by 3 mL of concentrated H2SO4. The addition of concentrated H2SO4
was aimed to create an atmosphere of acid. Then the solution is heated to a temperature of about
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70oC. The purpose of this warming is to prevent the formation of the intermediate results in the
form of a brown MnO2. Titration was also carried out in hot conditions. In this acid solution of
permanganate ion is reduced by the 5 electrons, when the oxidation state of Mn changes from +7
to +2. The reaction was as follows:
MnO4- + H+ + 5 e-

Mn2+ + 2 H2O

Titration was stopped until the solution color changed to pink titrates. In the process of
standardization titration is done 3 times, where the number average volume of titrant (KMnO4)
is 23. 97 mL. The reactions that occur in the standardization process are as follows:
2 MnO4-(aq) + 16H+ + 5C2O42- (aq)

2 Mn2+(aq) + 8H2O(l) + 10CO2(g)

Titration of Morh Salt Solution


N Fe2+= 0.1 N

, V Fe2+= 100 mL= 0.1 L

N Fe2+= M.n
0.1 = 1 (( gr/Mr)/0.1 L)
Gram Fe 2+= (0.1 x 0.1 x 448.156)
= 4.5 gram
Mohr salt solution prepared by dissolving 4.5 grams of Mohr salt in 100 mL aquades. A mixture
of Morh salt with H2SO4 is then heated until the temperature 70o C. And then, titrated with
standard KMnO4 solution that has been standardized. The average volume of KMnO4 that used
is 22.81 mL. Titration was stopped when the color changed from light yellow of titrat into weak
purple. Titration performed 3 times.
The reactions occurring in this titration is as follows:
MnO4-(aq) + 8H+(aq) + 5Fe2+(aq)

Mn2+(aq) + 5Fe3+(aq) + 4H2O(l)

Then obtained concentration of Fe2 + in the solution of salts based on the calculation result is
observation 0.095 N and the percentage of Fe 2+ solution of salts is 13.40%
V. Conclusion

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From the experimental results above it can be concluded that the concentration of Fe2 + in
salts solution is 0095 N.
VI. Answer of questions
1.

Na2C2O4 solution is good primary standard solution for permanganate in very acidic
condition. In this experiment, addition of concentrated sulphuric acid into oxalate have
purpose to make acidic solution. Other strong acid cannot be used, for example used
HCl, Cl- will oxidized by KMnO4 to form Cl2 so the amount of KMnO4 that used is much,
it caused the concentration of KMnO 4 bigger than concentration that have to oxidized
oxalate. It also occurs when the strong acid that use is HNO3.

2.

Reaction between oxalate and permanganate occur slowly in room temperature. It is


caused the solution have to heat until the temperature is 70 oC. The temperature also
cannot more than 700C because if the temperature more than ith, reaction will occur
slowly too. But, the speed of reaction increase when manganese (II) ion already formed.
Manganese (II) ion has a function as catalyst, the reaction called by autokatalitik because
it catalyst is produce in that reaction. This ion also give an effect by react quickly with
permanganate to form manganese in midlle oxidation (+3 or +4), whereas it will quickly
oxidized oxalate back to divalent condition.

3.

Beside ferro ion standardisation, permanganometric titration also can be used to


standardized tin (II) ion. It is caused by tin (II) ion will oxidized to tin (IV) by KmnO4

References
Selamat, I Nyoman dan I Gusti Lanang Wiratma.2004. Penuntun Praktikum Kimia Analitik.
Singaraja: IKIP Negeri Singaraja.
Underwood, A.L dan RA day.2003.Analisis Kimia Kuantitatif .Jakarta: Erlangga

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