Experiment Ii Synthesis of Mohr Salt: A. Objectives

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EXPERIMENT II

SYNTHESIS OF MOHR SALT


26 Mei 2015
A. OBJECTIVES
Study the Mohr salt from the reaction between the iron with sulfuric acid and ammonia
solution
B. THEORETICAL BACKGROUND
The main iron ore is hematite Fe2O3, magnalie Fe3O4, limonite FeO(OH), and
sideritr FeCO3. Pure iron is quite reactive. In humid air quickly oxidized give iron (III)
hydrate oxidation (rust) are not sangggup protect, because these substances are destroyed
and leave open the new metal surface. Iron is a very delicate nature pirofor. Soluble metal
minerals. With the not-oxidizing acids without air, obtained Fe 2+. With the air or when
used in hot dilute HNO3, some iron into Fe3+. Very strong oxidizing media such as HNO3
or acids containing dichromate iron making passive. Ferrous ion [Fe(H 2O)6]2+ provides
crystalline salt. Mohr salt (NH4)2SO4.[Fe(H2O)6]SO4 sufficiently stable to air and to water
loss, and commonly used to make a standard solution of Fe 2+ for volumetric analysis and
as a substance pengkalibrasi in magnetic measurements. FeSO 4.7H2O should slowly decay
and turn into yellow brown if left in the air. The addition of the solution HCO 3- or sh Akua
Fe2+ consecutive FeCO3 and FeS precipitate. Fe2+ oxidized in acidic solutions by air to
Fe3+. With ligands other than water that is, a noticeable change in potential bias occurred,
and the system FeII-FeIII is an excellent example of the effect of the ligand to the relative
stability of the level of oxidation (Cotton and Wikinson, 1989).
Ammonium iron(II) sulfate, or Mohr's Salt, is the inorganic compound with the
formula (NH4)2Fe(SO4)26H2O. 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 Schnites
orTutton's salts. which form monoclinic crystals and have formula M2N(SO4)2.6H2O. This
group can mix metals and crystallise on other schnite crystals.
Ferrous ion [Fe(H2O)6]2+ provides crystalline salt. Mohr salt (NH4)2SO4.Fe(H2O)
6SO4 sufficiently stable to air and to water loss, and commonly used to make a standard
solution of Fe2+ to volumetric analysis, and as a substance calibration in magnetic

measurements. Instead FeSO4.7H2O slowly decay and turn into yellow brown if left in air
(Shukri, 1999).
Iron is a metal that ranks second from common metals found in the earth's crust.
Iron (II) sulfate salts of alkali metals can form a double salt of the general formula M 2Fe
(SO4)2.6H2O (M is K, Rb, S or NH4). If the same number, each of the iron (II) sulfate
dissolved in hot water until saturated, and a solution of iron (II) sulphate is added a little
sulfuric acid, then the solution is mixed, then the cooling will crystallize monoclinic form
bluish green , These salts, iron (II) ammonium sulfate or iron (II) chloride, salt crystals
Morh stable in the air and the solution is not easily oxidized by oxygen in the atmosphere
(Purwaka, 2007)
All salts of iron (II) contains hydrated ion [Fe(H2O)6]2+ is pale greenish, if partially
oxidized to iron (III) to yellow-brown color. Salt crystals of iron (II) sulfate heptahedrat,
FeSO4.7H2O, tend to lose some of the water molecules. In the solid phase, double salt of
ammonium iron (II) sulfate hexahydrate or more precisely ammonium hexa aqua iron (II)
sulfate or salt Mohr called, showing highest lattice stability. This salt in the open air is not
experiencing eflouresense and also not oxidized, so it is often used as a standard solution,
especially in the redox titration, for example, to standardize a solution of potassium
permanganate (Sugiyarto, 2003).
Pure iron is white-silver metallic, solid and tough. He melts at 1535 oC. There is
rarely a purely commercial iron, iron usually contain small amounts of carbide, silicide,
phosphide and sulphide of iron, and a little graphite. Contaminants have played a
significant role in the strength of the iron structure. Iron can dimagnitkan. Dilute or
concentrated hydrochloric acid and dilute sulfuric acid dissolves the iron. At which the
resulting salts of iron (II) and hydrogen gas (Svehla, 1979).
Ions of iron (II) can be readily oxidized to Fe (III), it is a strong reducing agent.
The less acidic the solution, the more obvious this effect, in a neutral or alkaline even
oxygen from the atmosphere will oxidize iron (II). Salts of iron (III) or ferry derived from
iron oxide (III), Fe2O3. They are more stable than the iron salt (II). In the solution, there
are Fe3+ cations are pale yellow; if the solution containing chloride, the color becomes
stronger. Reducing agents transform ion iron (III) to iron (II). Ferrous ion [Fe(H 2O)6]2+
provides crystalline salt.
Forming two rows of iron salt that is important. Salts of iron (II) (or ferro) derived
from iron (II) oxide, FeO. In solution, these salts containing cations Fe 2+ and tinted
slightly green. Ions combined and complexes old color are also common. Ions of iron (II)
can be readily oxidized to iron (III), it is a strong reducing agent. The less acidic the
solution, the more obvious this effect, in a neutral or alkaline even oxygen from the

atmosphere will oxidize iron (II). Then a solution of iron (II) should be slightly acidic
when you want to save for a longer period of time (Svehla, 1990).
Mohr salt was made by mixing two sulphate salts of iron (II) and ammonium,
wherein each salt is dissolved till 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 molecular formula (NH4)2FeSO46H2O or (NH4)2(SO4)26H2O.
For double salt with M is NH 4, 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 molecular
formula (NH4)2FeSO4.6H2O or (NH4)2(SO4)2.6H2O.
Mohr salt, ferrous ammonium sulfate, a double salt of iron sulfate and ammonium
sulfate with molecular formula [NH4]2[Fe][SO4]2.6H2O. Mohr salt is widely used in
analytical chemistry, namely in volumetric analysis, to standardize a solution of potassium
permanganate or potassium bikrom.
Ferrous
ion
[Fe(H2O)6]2+

provides

crystalline

salt.

Mohr

salt

(NH4)2SO4.Fe(H2O)6SO4 sufficiently stable to air and to water loss, and commonly used to
make a standard solution of Fe 2+ to volumetric analysis, and as a substance pengkalibrasi
in magnetic measurements. Instead FeSO4.7H2O slowly decay and turn into yellow brown
if left in the air (Sunardi, 2006).
C. EQUIPMENT AND MATERIALS
Equipment :
Evaporating dish
Beaker
Round bottom flask
Materials :
20% sulfuric acid
Iron powder
Solution of ammonia
D. WORK INSTRUCTION

Synthesis of Mohr Salt

Neutralize 25 ml 20% sulfuric acid with 20 ml ammonia


25%

ammonium sulfate solution was evaporated until


saturated

Dissolve 3,5 gr of iron powder into 50 ml of 20% sulfuric


acid in beaker by heating and let the iron powder
dissolve by stirring

Filter the solution in hot conditions

evaporate dish so so that the solution begins to form


crystal on the surface

Mix with solution from neutralization of sulfuric acid in


hot conditions

Refrigerate the mixture, so that it from crystal of


ammonium ferrous sulphate with light green color

Purified the crystal by recristallization process with a


little hot wate
E. RESULT OF OBSERVATION
a. Color and structure (solid, liquid, gas) of H2SO4 :

Colorless and liquid


b. Color and structure (solid, liquid, gas) of iron powder :
Dark grey and smooth solid
c. Color and structure (solid, liquid, gas) of NH3 :
Colorless and liquid
d. Reaction occurred in the experiment :
H2SO4(aq) + NH3(aq) (NH4)2SO4(aq)
Fe(s) + H2SO4(aq) FeSO4(aq) + H2(g)
FeSO4(aq) + (NH4)2SO4(aq) + 6 H2O(l) (NH4)2FeSO4.6H2O(aq)
(NH4)2FeSO4.6H2O(aq) (NH4)2FeSO4.6H2O(s)
e. Weight of Mohr salt
14,8908 grams
f. Color and structure crystal of Mohr salt
Light green color and crystal form is monoclinic
g. Purity of Mohr salt
Theoretical Mass=

3,5053 gram x 392 gram . mol1


56 gram . mol1

= 24,5371 gram
14,8908
Purity of Mohr salt =
x 100
24,5371
= 60,68%
F. DISCUSSION
This lab is the synthesis of the salt Mohr aims to study the formation of salt
crystals Mohr, (NH4)2Fe(SO4)2.6H2O of reaction between iron with sulfuric acid and
ammonia solution. First create a solution that is between 25 mL solution of 20% sulfuric
acid with 20 mL of 25% ammonia. Then the solution is evaporated to saturated, or the
solution is reduced to half of the original. The reaction occurs:
H2SO4 (aq)+ 2NH4OH (aq) (NH4)2SO4 (aq)
Then make the solution B, ie dissolving 3.5 grams of powdered iron in 50 mL of
20% sulfuric acid and then heated. Blackish gray colored solution and precipitates in the
form of iron to be dissolved, which H2SO4 is a solvent containing protons that can be
ionized and acidic. The solution is heated until almost all the iron dissolves, so the
solution turns blue, then the solution is filtered using a filter paper while still hot. Into a
solution of sulfuric acid was added little to the filtrate and evaporating the solution until
crystals formed on the surface of the solution. Reactions that occur:
Fe(s) + H2SO4(aq) FeSO4(aq) + H2(g)

The goal of screening is to avoid the formation of crystals at low temperatures and
the purpose of heating to accelerate the reaction so that almost all of the iron can be
dissolved. This solution is continuously evaporated in order to reduce the water molecules
in solution. This solution is used to stabilize the vitrol crystals formed. This experiment
manghasilkan salts of iron (II) sulphate which is a salt of iron (II) which is important. In
solution, these salts containing cations Fe2+ so green and FeSO 4 Formation of Fe metal is
based on the principle of thermochemical reaction electrons.
After that A and B are mixed in hot conditions. Mixing the two solutions A and B
is intended to be able to make salt Mohr. The second solution is mixed with the hot
conditions to maintain in order to avoid crystallization solution at a low temperature, it
will produce a light green solution. To obtain crystals, solution was cooled in a refrigerator
for several days. Once cooled, the salt crystals obtained Mohr blue. The crystals are then
recrystallized by adding hot water. The addition of hot water to dissolve pengotot
substances which may be contained in the crystal. Then the crystals are dried and salt
crystals obtained Mohr weighing 14.8908, with randemen of 60.68%. Mohr salt crystal
form is monoclinic with a light green color. In the complex compounds of Fe 2+ acts as a
central atom with H2O as ligands. The reaction takes place, namely:
FeSO4(aq) + (NH4)2SO4(aq) + 6 H2O(l) (NH4)2Fe(SO4)2.6H2O(aq)
Once cooled, the reaction occurs:
(NH4)2Fe(SO4)2.6H2O (aq) (NH4)2Fe(SO4)2.6H2O (s)
Mohr salt
G. CONCLUSSION
1. Synthesis Mohr salt is a reaction between the iron with sulfuric acid and ammonia
2. Salt Mohr lab results obtained at 14.8908 grams with randemen 60.68%
H. SUGGESTION
1. Before the practitioner should understand the material lab practicum
2. Should the practitioner be more careful and thorough when doing lab
I. REFERENCE
Cotton dan Wikinson. Kimia Anorganik Dasar. UI-Press. Jakarta. 1989.
Sunardi. 116 Unsur Kimia. CV. Yrama Widya. Bandung. 2006.
Shevla, 1979. Analisis Anorganik Kualitatif Makro dan Semimikro Bagian I. PT Kalman
Media Pustaka. Jakarta.
Svehla, G. 1990. Vogel: Buku Teks Analisis Anorganik Kualitatif Makro dan Semimikro
Bagian II. PT Kalman Media Pusaka. Jakarta.
Syukri. 1999. Kimia Dasar 3. ITB. Bandung.

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