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Preparation Of Complex Salts And Double Salt

A. BACKGROUND
1. General Review
In the 1970s, Creep and damage of salt rock was the most research which focused
under different stresses and temperatures for the study of nuclear waste disposal. For gas and
hydrocarbon liquid storage are used the most salt caverns. In generally, gas injection rates (for
storage) and withdrawal rates (for consumption) are different from the loading rates
associated with radioactive waste storage, and are also different from time to time (injection is
generally slower than withdrawal) (Liang,et al., 2014: 166).
According toBronsted-Lowry, base is a hydrogen ion acceptor. After the hydroxide ion
itself, ammonia is the next most important Bronsted-Lowry base. This compound reacts with
water to produce the hydroxide ion. Here water is acting as an acid with hydroxide ion its
conjugate base, and the ammonium ion is the conjugate acid of ammonia. It is the production
of the hydroxide ion that makes ammonia solutions a useful glass cleaner (the hydroxide ion
reacts with fat molecules to form water-soluble salts) (Canham, and Overton, 2010: 147).
Atoms or molecules in which the total number of electrons is different from the
number of protons and therefore carries a positive or negative chargeis used with the term ion.
An anion is an atom or molecule that has a negative charge (has more electrons than protons).
In contrast to this, a cation is defined as an atom or molecule with a positive charge, that is, it
has more protons than electrons. Ionic bonds are strong but short-range bonds and they have
no defined direction in space, as they are ‘only’the result of electrostatic attraction. Therefore,
these attractions are not only limited to one directional partnereach but also with each ion
around them. As a result, a whole network of ions will be formed with anionsand cations
occupying specified spaces. The result is called a salt, which typically have high melting
points (Strohfeldt, 2015: 12-13).
The FT-IR analysis was charterized and confirmed formation of molecular salt. The
crystal structure of the salt is mainly stabilized by N+−H⋅⋅⋅ O−, O−H⋅⋅⋅O, C−H⋅⋅⋅F, and 𝜋-𝜋
interactions. The 3D Hirshfeld surface analysis and 2D fingerprint maps analysis revealed that
N–H⋅⋅⋅O and O–H⋅⋅⋅Ohydrogen bonding intermolecular interactions are more prominent in
the salt (Nagalapalli and Bheem, 2014: 4).
The salt production process would be success depends on the density. Initially, the
stabilization pond was filled with sea water (0°BE), after rising up to 5°BE, it flowed to the
evaporation pond. In the evaporation pond, evaporated sea water became 11°BE and flowed
to the concentration pond. After sea water reached 22°BE, it was poured to the crystallization
pond until 29°BE was achieved. The sea water in the crystallization pond became sodium
chloride crystal salt and was ready to harvest. The sea water is poured into the pond in the
sequence starting from stabilization-evaporation-concentrationcrystallization. Salt harvesting
was conducted in crystallization ponds. The salt deposit on the crystallization pond floor is
piled up next to pond and left to dry (Apriani,et al., 2018: 5).
Inorganic materials are made through methods that are grouped into three basic types.
Solid liquid-based interface; solid and liquid, has the same chemical properties known as two
processes, namely solidification and vitrification. The solid and liquid phases do not have the
same chemical properties known as crystallization and precipitation. In special cases, the
liquid phase is pure ionic liquid or liquid salt (molten salt). Ionic liquids can be activated as
solvents given by the agent template and the liquid component may not be incorporated in the
final solid product. Crystallization originating from the state of melt (liquid state) is analogous
to the solvent phase. Crystallization is a process of making solid materials by depositing
solution, melting, or gas. The crystallization material consists of solid liquid. In the process
there is a transfer of solute from the liquid to the solid crystal phase. The characterization of
crystallization is determined by thermodynamics and kinetic factors, which can make the
process very varied and difficult to control (Ningsih, 2016: 76-77).
2. Review of Results
In the unstable area could be occurred crystallization phenomenon. The viscosity and
temperature change of the inorganic hydrated salt are both important factors which affect the
nucleation.Crystallization process is a process closely related to the supercooling. Before the
temperature returns to the original freezing point, the liquid solidifies below its normal
freezing point and continues to decrease until complete solidification. When the degree of
supercooling increased, the degree of the deviation from the equilibrium state has risen, and
the critical dimension of the ice core and the formation energy also decrease dramatically,
which ultimately increases the probability of forming the nucleus (Liang and Chen, 2018: 4-
5).
During mechanicaltests on specimens of salt rock comprised of laminated halite and
non-salt interlayers. At ɛ = 1 × 10-4= S, a ‘‘stress drop’’ phenomenon was observed before
the axial stress reached peak value. The stress drop was about 4 MPa, and it was concluded
that the hard-brittle interlayer was suffering fracture while the halite remained intact. The
stress drop thus resulted from the mechanical differences between halite and the interlayer
material. To explore the deformation properties atɛ = 2.0 × 10-5= S, we conducted
supplementary tests with another three rock salt specimens; unfortunately, we did not have
identical samples from the same salt deposit as the former specimens 1 and 2. The
supplementary tests were carried out with three new specimens from the Hongze salt deposit,
also in Jiangsu Province, but the burial depth is similar to that of the thenardite, about 2000 m.
In the latter uniaxial compression experiment, the ‘‘stress-fluctuation’’ phenomenon was not
found for the stress–strain curves of new specimens (Liang, et al., 2014: 166).
At the point where the discharge is in contact with the liquid so crystals are readily
formed. The control sample crystallizes in a more dispersed layout. That difference is caused
by the orientation promoted by the electric field, that makes possible to crystallize in a
specific point on the liquid surface. So, the electric discharge crystallization allows the
formation of crystals that are not in contact with solid surfaces, and in a place with different
composition and energy (Baraunaa,et al., 2017: 217-218).
In ionic crystals, such as metal halides, oxides, and sulfides, cations and anions are
arranged alternately, and the solids are bound by electrostatic bonds. Many metal halides
dissolved in polar solvents such as NaCl dissolve in air, while metal oxides and sulfides,
which contain significant covalent bonds, are usually insoluble in the most polar solvents. The
basic structure of ionic crystals is that larger ions (usually anions) form a tight array and
smaller ions (usually cations) enter the octahedral or tetrahedral holes between the anions.
Ionic crystals involve several types of structures based on the cations and anions involved and
the ionic radius. Each type of structure is called the name of its distinctive compound, so the
structure of the salt is not only representing the structure of NaCl but also other compositions
(Ismunandar, 2008: 21-22)
When an ionic compound crystallizes from an aqueous solution, water molecules often
become incorporated in the solid crystal. These water-containing ionic compounds are known
as hydrates. In some hydrates, the water molecules are simply sitting in holes in the crystal
lattice, but in the majority of hydrates, the water molecules are associated closely with either
the anion or the cation, usually the cation. As an example, aluminum chloride crystallizes as
aluminum chloride hexahydrate, AlCl3∙6H2O. In fact, the six water molecules are organized in
an octahedral arrangement around the aluminum ion, with the oxygen atoms oriented toward
the aluminum ion, and so, the solid compound is more accurately represented as
[Al(OH2)6]3+∙3Cl-, hexaaquaaluminum chloride (the water molecule is written reversed to
indicate that it is the δ- oxygen that forms an ion-dipole interaction with the positive
aluminum ion). Thus, in the crystal of hydrated aluminum chloride, there are alternating
hexaaquaaluminum cations and chloride anions(Canham, and Overton, 2010: 95-96).
In a coordination complex, a central atom or ion is coordinated by one or more
molecules or ions (ligands) which act as Lewis bases, forming coordinate bonds with the
central atom or ion; the latter acts as a Lewis acid. Atoms in the ligands that are directly
bonded to the central atom or ion are donor atoms. The formation of complexes in aqueous
solution may be studied by a number of methods, of which testing the modifications of
chemical properties is only one, and a somewhat unreliable one at that. All reactions are
equilibria, and chemical tests are often only investigationsof relative values of equilibrium
constants. For example, in an aqueous solution of an Ag+ salt saturated with NH3, nearly all
the Ag+ is present as the complex [Ag(NH3)2]+ (Housecroft and Sharpe, 2005: 179).
B. THE OBJECTIVES
To learn the preparation and properties of ammonium sulphate copper double salt and
tetramintembaga (II) sulfate monohydrate sulfate complex salt.
C. APPARATUS AND CHEMICALS
1. Apparatus
a. Analytical balance (1 Unit)
b. Big test tube (3 Units)
c. Small test tube (3 Units)
d. Measuring glass 25 mL (1 Unit)
e. Evaporation disk (1 Unit)
f. Beaker glass 100 mL (2 Units)
g. Beaker glass 250 mL (1 Unit)
h. Watch glass (1 Unit)
i. Stirrer (1 Unit)
j. Funnel Buchner (1 Unit)
k. Vacuum pump (1 Unit)
l. Spiritus burner (1 Unit)
m. Tripod (1 Unit)
n. Asbes (1 Unit)
o. Spray Bottle (1 Unit)
2. Chemicals
a. Crystals copper sulphate pentahydrate, (CuSO4. 5 H2O )
b. Crystals ammonium sulfate ((NH4 )2SO4)
c. Etanol solution (C2H5OH)
d. Ammonium hydroxide 6M solution (NH4OH)
e. Ammonium hydroxide 15 M solution (NH4OH)
f. Aquadest (H2O)(l)
g. Filter paper
D. WORK PROCEDURES
1. Preparation of double salt kupri amonium sulfate, CuSO4.(NH4)2SO4.6H2O
2. Preparation of tetramincopper (II) sulfate monohydrate, Cu(NH3)4SO4.H2O.

3. Preparation several properties single salt, double salt, and complex salt.

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