EXPERIMENT 2

Synthesis of Mohr Salt

14 April 2015

A. Objective
Study the Mohr salt from the reaction between the iron with sulfuric acid and
ammonia solution
B. Theory
Mohr salt is a double salt which has the chemical formula FeSO4.
(NH4)2SO4.6H2O. The physical form of salt Mohr is greenish crystals. The green color
is caused by the presence of Fe (II). Compounds Fe is one of the complex salt-forming
compounds or double salt Mohr. Fe compounds in the form of Mohr salt or K4Fe(CN)6
potential as a reducing agent in the reaction of iodate reduction in salt. Mohr salt or
ammonium ferrous sulfate (FeSO4.(NH4)2SO4.6H2O) can be used to study the reactions
that occur in the Fe (II). (Tri Wulandari, 2012)
Such as copper and zinc, iron in nature are as sulfide (Fe2S).
But it is not used as a mineral ore as remnants of trace sulfur
difficult to remove. Fe2O3 hematite after magnetite most abundant
Fe3O4 or FeOFe2O3 very valuable as because of the content of iron
ore. As stated by its name, magnetite is attracted by a magnet.
(Kristian, 2004)
Elemental iron (Fe) in a system Periodic Elements (SPU)
belonging to the Group VIII. Iron can be made from iron ore in a
furnace. Iron ore typically contains Fe2O3 were marred by sand (SiO2)
of about 10%, as well as a bit of sulfur compounds, phosphorus,
aluminum, and manganese. Iron can also be magneted.
Iron sand deposits, may have magnetic minerals such as magnetic (Fe 3O4),
hematite (-Fe2O3), and maghemit (-Fe2O3). These minerals have the potential to be
developed as an industrial material. Magnetite, for example, can be used as a base
material for dry ink (toner) on a photo-copy machines and laser printers, while
maghemit is the main ingredient for tape-cassette. Magnetic minerals in the upper
third digunakansebagai also dyes and mixtures (filler) for the paint as well as the basic
material for permanent industrimagnet. (Bijaksana, 2002)

The properties of very smooth iron is pyrophoric. Metal soluble in mineral

acids. With the not-oxidizing acids without air, obtained Fe 2+. The presence of air or
when used hot dilute HNO3, a number of iron to Fe (III). Dilute or concentrated
hydrochloric acid and dilute sulfuric acid dissolves the iron, in which the resulting
salts of iron (II) and hydrogen gas. Pure iron is quite reactive. In the damp air quickly
oxidized give iron (III) oxide hydrate (rust) are not able to protect, because this
substance is destroyed and let the new metal surface open.
The properties possessed of the element iron is easily corroded iron in moist air
with the formation of rust (Fe2O3.nH2O), which does not protect iron from further
perkaratan, therefore iron usually closed with a metal coating other substances such as
lead , nickel, zinc and others. An incandescent iron if in a state of iron can overtake O
and H2O (steam) to form H2 and Fe3O4. Whereas if left in the open air, the iron will
form Fe2O3 (ferric oxide), and if one is not consumed by the alkaline iron, the iron can
be dissolved in dilute sulfuric acid and hydrochloric acid to form H 2, and concentrated
sulfuric acid does not take the iron. (Annisa, 2008)
Pure iron is a silver-white metal, which is strong and tough. Melts at 1535 C.
There is rarely a purely commercial iron, iron usually contain small amounts of
carbides, silicides, phosphides, and sulfides of iron, and a little graphite. Contaminants
have played an important role in the strength of the iron structure. Iron can
dimagnitkan. Dilute or concentrated hydrochloric acid and dilute sulfuric acid
dissolves the iron, in which the resulting salts of iron (II) and hydrogen gas.
Fe(s) + 2H+(aq)
Fe2+(aq) + H2(g)
Fe(s) + 2HCl(aq)
Fe2+(aq) + 2Cl-(aq) + H2(g)
Hot concentrated sulfuric acid produced ions of iron (III) and sulfur
oxide :
2Fe(s) + 3H2SO4(aq) + 6H+(aq)

2Fe3+(s) + 3SO2(g) + 6H2O(l)

Iron formes two important salt series.

Salts of iron (II) (or ferro) derived from iron (II) oxide, FeO. In
these salts solution containing Fe2+ cations and slightly green color.
Ions and complexes combined colored old tongs are also common.
Iron (II) can be easily oxidized to iron (III), it is a strong reducing
agent. The less acidic the solution, the more obvious this effect, in a
neutral or even alkaline oxygen from the atmosphere will oxidize iron
(II). Then a solution of iron (II) should be slightly acidic when you
want to keep for a long time.
Salts of iron (III) (or ferric) derived from iron oxide (III) oxide,
Fe2O3. They are more stable than the salt, iron (II). In the solution,

there are Fe3+ cations are bright yellow. If the solution containing
chloride, the color becomes stronger. Reducing agents convert iron
(III) to iron (II). (G. Svehla, 1990)
Salts of iron (II) sulfate can join sulfate salts of alkali salts,
forming a double salt with a general formula that can be described
as M2Fe(SO4).6H2O, where M is a symbol of metals, such as K, Rb, Cs
and NH4. This formula is a combination of two salts with anions
similar or identical to that M2SO4FeSO4.6H2O.
For double salt with M is NH4, which made the number of moles
of iron (II) sulfate and ammonium sulfate same, then the result is
known as Mohr salt. Mohr salt was prepared by mixing both sulfate
salts of iron (II) and ammonium, wherein each salt is dissolved to
saturation and the iron (II) added a little sour. At the time of cooling
results in both salt mixture above will be obtained crystal bluish
green with monoclinicic form. Mohr salt is nothing but a double salt
of

iron

(II)

ammonium

sulfate

with

molecular

formula

FeSO4(NH4)2SO4.6H2O or (NH4)2Fe(SO4)2.6H2O.
(Aziz, 2007)
Mohr salt is preferred over the iron (II) sulfate to the Mohr
titration because salt is not easily affected by free oxygen in the air /
not easily oxidized by free air than iron (II) sulfate. Oxidation solution
of iron (II) is highly dependent pH, occurs much more easily at high
pH. Ammonium ions make Mohr salt solution slightly acidic, which
slows down the oxidation process. Sulfuric acid is generally added to
the solution to reduce the oxidation of iron. (Anonymous, 2013)
Crystal or crystalline solid that is an atom, molecule, or ion
constituent packed regular and repetitive pattern extends in three
dimensions. In general, a liquid form crystals when subjected to the
compaction process. In ideal conditions, the result can be a single
crystal, which all atoms in solids "attached" to the grid or the same
crystal structure, but in general, most of the crystals are formed
simultaneously resulting polycrystalline solids. For example, most
metals which we see everyday are polycrystalline.
Crystal structure which is formed of a liquid, depends on the its
fluid chemistry, when the solidification conditions and ambient
pressure. The process of formation of the crystalline structure known
as crystallization. (Anonymous, 2013)

In general, the ferrous ion [Fe(H2O)6]2+ to form salt crystals. Mohr

salt (FeSO4.(NH4)2SO4.6H2O) sufficiently stable to air and to water loss.
Based on these properties, Mohr salt is used to create a standard
solution of Fe2+ for volumetric analysis and as an astringent
pengkalibrasi (standard substance) in magnetite measurements, for
example, to standardize the KMnO4 solution. (Lecturer of Inorganic
Chemistry Team, 2014)
C. Apparatus and Reagents
Apparatus :
Evaporating dish
Beaker glass
Round bottom flask
Stirring
Funnel
Measuring glass
Filter paper
Reagents :
25 ml of 20% sulfuric acid solution
Iron powder
20 ml of 25% ammonia solution
Distilled water
D. Procedure
Solution A
E.
Neutralizing
25 ml of sulfuric
F.
acid 20% with 20 ml of
G.
ammonia 25%.

H.Evaporating ammonium
I.
sulfate solution until saturated

Solution B
Dissolving 3,5 g of iron
powder into 50 ml sulfuric
acid 20%.
Heating ang let the iron
powder dissolve by stirring

Filtering the solution in hot

condition. Then, evaporating
until the solution formed
crystal on the surface

Mixing solution A and solution B in hot condition

Refrigerating the solution until formed the crsytal of

ammonium ferrous sulfate with light green color

Purifying the crystalby recrystallization process with

a little hot water

Weighing the crystal and calculating the yield

E. Observation Data and Analysis Data

1. Color and structure of H2SO4
: no color, liquid
2. Color and structure of iron powder : black, solid (powder)
3. Color and structure of NH3
: no color, liquid
4. Reaction occured in the experimen :
Fe(s) + H2SO4(aq)
FeSO4(aq) + H2(g) (green light solution)
H2SO4(aq) + 2NH3(aq)
(NH4)2SO4(aq) (no color solution)
FeSO4(aq) + (NH4)2SO4(aq)
(NH4)2Fe(SO4)2.6H2O(aq

(bluish

green crsytal)
5. The calculation of the theoretical weigh of Mohr salt :
3,50122 mol x 392 gr /mol
Theoretical weight of Mohr salt =
56
= 24,5084 g
6. Weight of Mohr salt (as a product) : 5,0122 g
7. Color and structure crystal of Mohr salt : Bluish green (tosca), crsytal
8. Purity levels of Mohr salt :
Yield

weight of salt of experiment result x 100

theorytical weight of salt

5,0122 x 100
24,5084

20,45

F. Discussion

In this practicum, conducted the experiments of Mohr salt synthesis. This

experiment aims to study the Mohr salt from the reaction between the iron with
sulfuric acid, and ammonia. Mohr salt is made by reacting the iron with sulfuric acid
solution and ammonia solution. The iron used in this experiment is the iron powder.
The purpose of the use of iron powder is to accelerate the reaction, because the
reaction rate is proportional with the surface of a substance. In this experiment, all of
the solution that used is concentratd solution, so that this experiment is done in a fume
hood because of the concentrated solution will cause a pungent odor and dangerous for
practitioner. This is a standard and one of safety lab procedures.
The first step that we do in this experiment is make solution A, solution A is
made by neutralizing the sulfuric acid solution with ammonia solution, so that this
reaction produced the solution of ammonium sulfate. Ammonia solution is as a ligand
that has an orbital containing the unpaired electron to its interaction with the metal,
classic form coordination complexes with metals. Then the solution is evaporated until
the volume is reduced about a half of its volume before heating. The purpose of this
evaporating process the evaporate of ammoni solution which may not react with
sulfuric acid solution. Ammonium sulfate solution is colorless.
The reaction occured :
H2SO4(aq) + 2NH3(aq)

(NH4)2SO4(aq) (no color solution)

The next step is to make solution B by react the iron powder with sulfuric acid
solution. Sulfuric acid solution is a solvent containing ionizable protons and strong
acid or weak acid. Then heating this solution until all part of the iron is completely
dissolved and the color of solution is light green. This heating process is aims to
eliminate H2 gas and accelerate the formation of Fe2+ ions that are characterized by the
formation of bluish green crystal. In addition, heating is also as a catalyst to accelerate
the reaction, so that all the iron can be dissolved completely. After all part of iron
powder are dissolved, then filter the solution and evaporate the filtrate in a porcelain
cup, until forming a light green solution and there are crystal on its surface. The
purpose of filtering and evaporation of this is to avoid the formation of crystals at low
temperatures and to reduce the water molecules in the solution.
The reaction occurred :
Fe(s) + H2SO4(aq)
FeSO4(aq) + H2(g) (green light solution)
After that , solution A and solution B were mixed in hot conditions. This is
done to prevent crystallization solution at a low temperature and to accelerate the
reaction. So that this reaction produced light green solution. Then the solution is

cooled in the refrigerator for 3 days in order to form Mohr salt crystals. After cooled,
the mixture solution is filtered to separate the solution with Mohr salt crystals. Thus
obtained Mohr salt crystals with monoclinicic shape and has bluish-green color due to
contained Fe with (NH4)2SO4 which form complex compounds.
The reaction occurred :
FeSO4(aq) + (NH4)2SO4(aq)

(NH4)2Fe(SO4)2.6H2O(aq) (bluish green crystal)

After that, conducted purification of Mohr salt crystal by recrystallization

using hot water. The purpose of used hot water is to eliminate the impuritiy materials
that may be still present in Mohr salt crystals. So that this produced pure Mohr salt
crystals that has bluish green color. In this experiment obtained 5,0122 grams of Mohr
salt crystal. According to the data, the theoretical mass of Mohr salt crsytal should be
produced is 24,5084 grams. From the experiment data, the yield of Mohr salt crystal
that we obtained is 20,45%, so the purity levels of Mohr salt crsytal in this experiment
is 20,45 %. This purity levels is obtained from the calculation result (weight of Mohr
salt crystal from the experiment result : theoritical weight of Mohr salt) x 100%. The
purity levels of Mohr salt that obtained in this experiment is little (20,45%). This
happens due to several factors, such as the iron powder is not dissolved 100%, and the
solution A is less saturated when it heated, because it is difficult to know the solution
A has been saturated or not yet.

G. Conclusion and Suggestion

Conlusion :
Mohr salt can be prepared from the reaction of iron with sulfuric acid and

ammonia solution.
Mohr salt crystals shaped is monoclinic and has bluish-green color
Purification Mohr salt crystals can be done by recrystallization using hot

water
In this experiment produced 5,0122 grams of Mohr salt crystal
The theorytical weight of Mohr salt that produced is 24,5084 grams
The purity levels of Mohr salt that obtained in this experiment is 20,45 %

Suggestion :

Practitioner must understand the procedure and theory before doing the

experiment
Equipments and materials that will be used should be in good condition
Practitioner should be more careful in observe the solution A until it saturated
Practitioner should be more careful in stirring the solution B until Iron powder

dissolve perfectly
Practitioner should maintain the cohessiveness within the members of the
group

H. Reference
Bijaksana, S. 2002. Kajian Sifat Magnetik Pada Endapan Pasir Besi di
Wilayah Cilacap dan Upaya Pemanfaatannya untuk Bahan
Industri. Bandung: ITB.
Aziz, T. 2007. Penuntun Praktikum Kimia Anorganik Jurusan Kimia.
Kendari: Universitas Haluoleo.
Svehla, G. 1985. Analisis Kuantitatif Anorganik Makro dan Semi Makro. Jakarta: PT
Kalman Media Pustaka.
Sugiyarto, Kristian H. 2004. Kimia Anorganik II. Jogjakarta: JICA.
Tim Dosen Kimia Anorganik. 2015. Petunjuk Praktikum Kimia Anorganik. Semarang:
Laboratorium Kimia FMIPA UNNES
Tri

wulandari.

2012.

http://uwlankimura.blogspot.com/2012/01/garam-Mohr.html.
(Diakses pada tanggal 15 April 2015 pukul 20:05)
Annisa. 2008.
http://annisanfushie.wordpress.com/2008/12/26/garam-Mohrnh426h2o/.

(Diakses pada tanggal 15 April 2015 pukul

15:30)

Semarang, 15 April 2015

Bunga Mahardhika A

NIM. 4301413105
I. Appendix

H2SO4(aq) + NH3(aq)

Fe(s) + H2SO4(aq)

Kristal garam mohr