Experiment 2

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May, 26th 2015

EXPERIMENT II
SYNTHESIS OF MOHR SALT
A. Objectives
1. Study the Mohr salt from the reaction between the iron with sulfuric acid and ammonia
solution
B. Theoritical Basic
Mohr salt is a double salt which has a chemical formula FeSO4.(NH4) 2SO4.6H2O. The
physical form of salt Mohr is greenish-shaped crystals. The green color is caused by the ion
Fe (II). Compounds Fe is one of the salt-forming complex compounds or double salt Mohr. Fe
compounds in the form of Mohr salt or K4Fe(CN)6 potential as a reducing agent in the
reduction reaction of iodine in salt. Mohr salt or iron (II) ammonium sulphate (FeSO4. (NH4)
2SO4.6H2O) can be used to study the reactions that occur in ion Fe (II) (Tri Wulandari,2012).
Such as copper and zinc, iron in nature are as sulfide (Fe2S). But this is not used as a
mineral ore since the remnants of trace sulfur difficult to remove. At most abundant hematite
Fe2O3 magnetite Fe3O4 or FeO, Fe2O3 after extremely valuable as due to the large content of
iron ore. As stated by its name, magnetite is attracted by the magnet (Kristian, 2004).
Salts of iron (II) sulfate can join sulfate salts of alkali salt, forming a double salt of the
general formula that can be described as M 2Fe (SO4) 6.H2O, wherein M is a symbol of metals,
such as K, Rb, Cs and NH4. This formula is a combination of two salts with the same anion or
identicalie 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 made by
mixing two sulphate salts of iron (II) and ammonium, wherein each salt is dissolved until
saturation and the iron (II) added a little sour. At the time of cooling results in the second
mixture above salt will be obtained crystal bluish green with monoclinic form. Mohr salt is
nothing but a double salt of iron (II) ammonium sulfate with a molecular formula FeSO 4.
(NH4) 2SO4.6H2O or (NH4) 2Fe (SO4) 2.6H2O. (Aziz, 2007)
In general, ferrous ion {Fe(H2O)6]2+ forms crystals salt. Mohr salt (NH4)2SO4.
[Fe(H2O)6]SO4 quite stable against air and against the loss of water. Based on these properties,
Mohr salt is used as a substance for calibration (standard substance) in the magnetic
measurements, for example to standardize a solution of KMnO4.
(Inorganic Chemistry Lecturer Team, 2015)
C. Equipment and Material
Equipment :
1. Evaporating dish
2. Beaker
3. Round bottom flask
Materials :
1. 20% sulfuric acid
2. Iron powder
3. Solution of ammonia
D. Work Instruction

25 mL 20% sulfuric
acid + 20 mL
ammonia 25%
neutralized,
evaporated until
saturated (Asolution)

Purified the
crystals by
recrystallization

Dissolve 3,5 g of
iron powder into 50
mL of sukfuric acid
20% by heating
and stirring (Bsolution)

The mixture
refrigerated

The solution
filtered in hot
condition and
evaporated to form
crystals on the
surface

The solution mixed


with neutralization
solution

E. Result of Observation
1. Color and structure (solid, liquid, gas) of H2SO4 : colorless and liquid
2. Color and structure (solid, liquid, gas) of iron powder : grey and solid
3. Color and structure (solid, liquid, gas) of NH3 : colorless and liquid
4. Reaction occured in the experiment :
H2SO4(aq) + 2NH3(aq)
(NH4)2SO4(aq) (solution-A)
Fe(s) + H2SO4(aq)
FeSO4(aq) + H2(g) (solution-B)
FeSO4(aq) + (NH4)2SO4(aq) + 6H2O
(NH4)2SO4.[Fe(H2O)6]SO4(s) (mohr salt)
5. Weigh of Mohr salt (as a product) :
Mass of Fe powder
= 3,5000 grams
Mass of Mohr salt (in experiment) = 14,8908 grams
Mass of Mohr salt (theory) = Mol of Mohr salt x Mr Mohr salt
3,5084
= 55,85 mol x 392 gr/mol

Purity of Mohr salt

= 24,5000 grams
mass of Mohr salt (experiment )
mass of Mohr salt ( theory)
=

x 100

14,8908
x 100
24,5000

= 60,68 %
6. Color and structure Crystal of Mohr salt : green and solid
7. Purity of Mohr salt : 60.68%
F. Discusion
This experiment is to synthesis of mohr salt. Synthesis mohr salt, it means produce salt
mohr in crystal (solid structure). Practicant must prepare two solution to form mohr salt. There
are solution of ammonium sulphate and ferrous sulphate. That solution make at same time.

Solution of ammonium sulphate as solution-A. That solution produced by H 2SO4 and


NH3 solution. Between of solution is colorless. Sulphate acid H2SO4 solution mix with
ammonium NH3 solution. Mixture of solution is colorless too. Then heated and stirr it. Heating
is to increase rate reaction between H2SO4 and NH3 solution. Stirring is to make solution
homogen. Heated until mixture of solution become more thick. That need long time until
mixture of solution become total volume in first time. The mixture produce ammonium
sulphate solution. Look at this reaction :
H2SO4(aq) + 2NH3(aq)
(NH4)2SO4(aq)
Solution of ferrous sulphate as solution-B. It produce use iron powder and sulphate acid
solution. The color of iron powder is grey. H2SO4 solution heated, so H2SO4 more easily to
dissolve the iron powder. But the boiling point of H2SO4 is high. To effective the time, so we
put iron powder into H2SO4 before boil, mix that iron podwer and H2SO4 still heated. Heating is
to increase rate reaction. The color of solution become grey after put iron powder into H 2SO4
solution. Stirring that mixture, there are bubbles on solution. That heated until all iron powder
dissolve, we can know if the solution change color become green and transparent. Green color
from Iron(II) sulphate. After that, the solution filter use filter papper. The filtrat evaporated use
evaporating dish by heating again. Hablur will formed if the solution become saturated. This
like as sugar solution, there are layer thick. The mixture produce ferrous sulphate solution.
Look at this reaction :
Fe(s) + H2SO4(aq)

FeSO4(aq) + H2(g)
If solution-A and solution-B already to formed, so that solution mix (solution-B put into
solution-A). After that the mixture of that solution covered using plastic, then save in
refrigerator. Low temperature make that solution become solid. It need long time, 3 days for
waiting.
The crystals formed after 3 days waiting. The color of crystals is green and it solid.
Crystals of mohr salt very dificult to dislocate from erlenmeyer, because it has freeze. So
practicant need powerful energy to dislocate the crystals, but must carefully too prevent broke
the erlenmeyer. Then the crystals washed use hot water. Washing with hot water to losing dirty
substance from crystals, hot water can dissolve another substance. Drying do after washing, it
because to evaporated another substance (H2O) from crystals, so we get pure mohr salt crystals.
Look at this reaction :
FeSO4 + (NH4)2SO4 + 6H2O (NH4)2Fe(SO4)2.6H2O

(bluish green crystal)

Based on theory the mass of mohr salt is 24.5..... gram, based on experiment the mass of
mohr salt crystals is 14.8908 gram. So we can know the rendement of mohr salt crystals is
60.68%. It not optimum, because :
1. Probability A-solution not yet thick, because its very long time to make the solution
thick.
2. NH3 evaporated so NH3 in little amount, so the A-solution not produce perfectly.
G. Conclusion
1. Mohr salt formed from reaction between the iron with sulfuric acid and ammonia solution.
2. Mohr salt is a compound of iron complexes (Fe as center atom) with ligands of ammonium
and sulfate with molecular formula (NH4)2Fe(SO4)2.6H2O.
3. Based on experiment the rendement of mohr salt is 60.68%.
4. Mohr salt include cluster salt.
5. High temperature and low temperature need in this experiment.
H. Suggestion

1. Making solution-A & B must in right procedure, so that can produce mohr salt
maximally.
2. Before put Fe into H2SO4, the solution of H2SO4 must heated.

I. Refference
Annisa. 2008. http://annisanfushie.wordpress.com/2008/12/26/garam-mohr-nh426h2o/.
Aziz, T. 2007. Penuntun Praktikum Kimia Anorganik Jurusan Kimia. Kendari : Universitas
Haluoleo.
Inorganic Chemistry Lecturer Team. 2015. Manual Work of Inorganic Chemistry Practicum.
Semarang : UNNES.
Sugiyarto, Kristian H. 2004. Kimia Anorganik II. Jogjakarta: JICA.
Svehla, G. 1990. Vogel Buku Teks Analisis Anorganik Kualitatif Makro dan Semimikro.
Bagian I Edisi kelima. Jakarta: PT. Kalman Media Pusaka.
http://digilib.itb.ac.id/files/disk1/628/jbptitbpp-gdl-mubarohnim-31358-3-2008ts-2.pdf

Documentation

H2SO4 solution

Making of solution-A

Iron powder

Making of solution-B

Heating H2SO4

Iron dissolve in H2SO4

Evaporating of mixture

Result of evaporating

Mohrs salt crystals

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