SYNTHESIS OF MOHR SALT

29 May & 1 June 2016

A. Objective
Study the Mohr salt from the reaction between the iron with sulfuric acid and
ammonia solution.

B. Theoretical Basis

Mohr’s salt i.e. ferrous ammonium sulphate [FeSO4.(NH4)2SO4.6H2O] is a

double salt. It can be prepared by making equimolar solution of hydrated ferrous
sulphate and ammonium sulphate in minimum amount of water. A few ml of dil.
H2SO4 is added to prevent the hydrolysis of FeSO4.7H2O. Cooling of the hot
saturated solution yields light green crystals of Mohr’s salt.

FeSO4.7H2O + (NH4)2 SO4 → FeSO4.(NH4)2SO4.6H2O + H2O

(Miscellaneous, 2013)

Containing two different cations, Fe2+ and NH4+, it is classified as a double salt
of ferrous sulfate and ammonium sulfate. It is a common laboratory reagent. Like the
other ferrous sulfate salts, ferrous ammonium sulfate dissolves in water to give the
aquo complex [Fe(H2O)6]2+, which has octahedral molecular geometry. This
compound is a member of a group of double sulfates called Schönites or Tutton's
salts. which form monoclinic crystals and have formula M2N(SO4)2.6H2O. This group
can mix metals and crystallise on other schönite crystals.

Mohr salt preferably of 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 . ( Svehla , 1990 )

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

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 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 fluid chemistry
itself, when the solidification conditions and ambient pressure. The process of
formation of the crystalline structure known as crystallization. ( Anonymous, 2013 )
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.
( Sugiyarto, 2004)

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 be magneted. 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, produces ions of iron (III) and sulfur dioxide:
2Fe (s) + 3H2SO4 (aq) + 6H + (aq) + 2Fe3 (s) + 3SO2 (g) + 6H2O (l)
Iron salts formed two important series.

To developing the process of education in laboratory, the experiment shyntesis

of mohr salt is done used Fe powder, sulphuric acid and ammonia. Mohr salt is more
stable than Ferro sulphate salt, so mohr salt is used in measurement of standart solution
Fe2= on measurement of substance that contained Fe by methode volumetri or
spektrofotometri. Beside to make sure the ability of oxidation from potassium
permanganate and potassium bicromate. But the proce of this salt in market is so
expensive. Mohr salt is the double salt that contains of ferro sulphate salt and
ammonium sulphate salt in a monocline crystall and has a blue-green colour. The
making process of mohr salt is by crystallization process, such as heating process,
cooling process, and filtration. Shyntesis process of this salt is through 2 steps, the first

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is forming of ferro sulphate salt and the econd step is forming of ammonium sulphate
salt.

( Ngatin, dkk, 2013)

C. Material and equipment

Equipment :
1. Evaporating dish
2. Beaker
3. Round bottom flask
4. Pipette volume
Material :
1. Sulfuris acid 20% 25 ml
2. Iron powder
3. Solution of ammonia 25% 20 ml

D. Methods

solution A solution B

Neutralized 27 ml sulfuric acid Dissolve 3,5006 g of iron

20% with 23 ml ammonia powder into 50 ml sulfuric acid
25%. 20%.

Heating and let the iron

powder dissolve by stirring
Ammonium sulfate solution
was evaporated until saturated

Filter the solution in hot conditions

and evaporated in evaporating dish
so that the solution begins to form
crystal on the surface

Mix solution A and solution B in hot conditions

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 Refrigerated the mixture, so that it form crystal of
ammonium ferrous sulphate with color light green

Purified the crystal by reccrystallization process with a

little hot water

Weigh the crystal as a product and count

the rendemen.

E. Observation data
1. Color and structure (s,l,g) H2SO4 : clear, aqueous
2. Color and structure (s,l,g) iron powder : grey-black, solid, mass = 3,5006 gr
3. Color and structure (s,l,g) NH3 : clear, aqueous
4. Reaction occurred in experiment :
Fe(s) + H2SO4(aq) FeSO4(aq) + H2(g) (light green solution)
H2SO4(aq) + 2NH3(aq) (NH4)2SO4(aq) (clear solution)
FeSO4(aq) + (NH4)2SO4(aq) (NH4)2 Fe (SO4 ) 2.6H2O(s)

5. Weigh of Mohr salt (as a product ):

3,5084 𝑚𝑜𝑙 𝑥 392 𝑔𝑟/𝑚𝑜𝑙
Weigh of Mohr (theoretical) = 56

=24,5 gr
6. Weigh of Mohr salt as a product : 14,6632 gr
7. Color and structure crystal of Mohr salt : green-bluish, crystal
8. Purity of Mohr salt :
𝑚𝑎𝑠𝑠 𝑜𝑓 𝐹𝑒
Mol Fe = 𝐴𝑟 𝐹𝑒
3,5006 𝑔𝑟𝑎𝑚𝑠
= 56
= 0,0625 mol

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 Mol Fe = mol (NH4)2 Fe (SO4 ) 2.6H2O

𝑚𝑎𝑠𝑠 (NH4)2 Fe (SO4 ) 2.6H2O

0,0625= 𝑀𝑟 (NH4)2 Fe (SO4 ) 2.6H2O

𝑚𝑎𝑠𝑠 (NH4)2 Fe (SO4 ) 2.6H2O

0,0625= 392

Mass (NH4)2 Fe (SO4 ) 2.6H2O = 0,0625 x 392

= 24,5 grams (theoretical)

𝑀𝑜ℎ𝑟 𝑠𝑎𝑙𝑡 𝑎𝑠 𝑎 𝑝𝑟𝑜𝑑𝑢𝑐𝑡 𝑥 100 %

Rendemen = 𝑤𝑒𝑖𝑔ℎ 𝑜𝑓 𝑚𝑜ℎ𝑟

14,6632 𝑥 100 %
=
24,5
= 59,85 %

F. Discussion

This experiment is about aynthesis of Mohr salt, the aim of this experiment is to
study the making process of Mohr salt from the reaction between the iron with sulfuric
acid solution and ammonia solution. Double salt is the salt that in the crystal contains 2
different kation with certain proportion, the double salt usually is easier to form big
crystal then the single salt. The example of double salt is Mohr salt. All of the solution
that used in this experiment is concentrated, so we have to do the steps of this
experiment in the acid cupboard, its because the gass that evaporated from the solution
is dangerous if smelled by the practician. To synthesis the mohr salt, we used iron in
powder form, the aim of used powder form of iron is to make the reaction is increase
and faster because the surface area is the one of the factors that influence the rate
reaction.

The Mohr salt is the double salt, so it is formed from 2 kinds of salt, the both salts
is in form solution, the A solution and B solution. The A solution is prepared by
neutralize sulfuric acid solution with ammonia solution and its result ammonium sulphate
solution. The function of ammonia is to serve the ligand that has an orbital that
contained unpaired electron to react with a metal, then the solution is heated until it is
saturated, the way to know if it is already saturated is the volume of the solution is still a
half from the total volume. The aim of the heating process is to evaporate the ammonia
that not bound with sulphuric acid, so that we get the ammonium sulphate solution with
clear solution. The reaction is;

H2SO4(aq) + 2NH3(aq) (NH4)2SO4(aq) (clear solution)

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 Then to prepared B solution is by reacting Fe powder with sulphuric acid solution,
the solution has to be heated and stirred during heating process, the heating process is
done until the Fe powder is solved perfectly, it is showed by the color of the solution
change from grey become green-bluish. The heating process is aimed to make the
reaction become faster and to release the H2 gass and to make the forming of ion Fe2+ is
become faster, forming of ion i Fe2+ is showed by the formation of little crystal / hablur.
After all of the Fe powder is solved then it should be filtered and must be evaporated in
evaporating dish so that it is formed the little crystall in the surface of the solution. The
reaction is;

Fe(s) + H2SO4(aq) FeSO4(aq) + H2(g) (light green solution)

When the both solution is ready, then the A and B solution is mixed in hot
conditions, the aim of mixed in hot condition is to prevent the crystallization in low
temperature of both solution before heated. The result is the light-green solution, then
the solution is stand in the refrigerator for 5 days so that the crystall of mohr salt can be
formed. After 5 days cooled in refrigerator, the mixture has to be filtered to separate the
solid phase and the liquid phase. So that we get the Mohr salt crystall that has blue-
green color because the reaction between Fe and (NH4)2SO4(aq) that formed complex
compound. The reaction is;

FeSO4(aq) + (NH4)2SO4(aq) (NH4)2 Fe (SO4 ) 2.6H2O(s)

Purifying of mohr salt crystall is done by recrystallization process by washing it

used hot water. The function of the hot water is to solve the impurities that still included
in the crystall. The recrystallization process is done by dropping the hot water drop by
drop and all of the part of crystall should be washed by hot water, the aim why it should
be drop by drop is to prevent the crystal of mohr salt is solved again, because the crystal
can solved in a high temperature of water. The final result of crystal of mohr salt is
14,6632 gr, and then the theoritical mass that is calculated is 24,5 gr so the rendement
of the crystal of Mohr salt is 59,85 %.

G. Conclusion

1. Mohr salt can be prepared from the reaction of iron with a solution of sulfuric acid
and ammonia solution.
2. Mohr salt that formed is light-green crystal
3. Purification Mohr salt crystals can be done by recrystallization using hot water
4. In this experiment produced Mohr salt of 14,6632 gr
5. The rendement obtained in this experiment is 59,85%

H. Suggestion
1. Should the practitioner be more careful during the practicum

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 2. Practician must understand the material before doing the lab
3. Practician should work well with the member group.
4. Practician should make sure all of the tools of practicum is in good condition

I. References
Miscellaneous.2013.https://sites.google.com/site/cbsehomework/practical/chemprac/
miscellaneous/mohr-s-salt-crystals (accessed 7 June 2016 in time 20.56)
Ngatin, dkk. 2013. Sintesis Garam Mohr. Prodi Teknik Kimia Polban
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.
Wikipedia. 2013. http://id.wikipedia.org/wiki/Kristal. (accessed 7 June 2016 in time
21.15)