Complex Salt

Diyah Ayu Anggraeni

Erta Alifah Febrianti
Intan Cahyaningrum
Nurul Aisyara
2
Storyboard
Complex Salt

References
Introduction Results &
Discussion

1. Objectives 1. Results
2. Theory 2. Discussion
Closing
Procedure
Experiment
1. Conclusion
1. Apparatus and 2. Suggestion
Reagent
2. Flow Chart

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Section 1 Introduction
Objectives and Basic Theory
4
Objectives
-Introduction

The Objectives of This Experiments:

Studying the complex salt production tetra amin

copper (II) sulphate [Cu(NH3)4SO4.xH2O]. as a
result of reaction between cupric sulfate bunch of
ammonia and its properties.

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 Transition metals can form complex ions. An example is copper metal. Copper is a pink-red metal, which is soft,
malleable, and tough. These metals are capable of forming salts are generally blue, either in the form of hydrates, solid,
or in aqueous solution. Examples of the salt is in the form of ions tetraakuokuprat (II) [Cu(H2O)4]2+.

It is insoluble in hydrochloric acid and dilute sulfuric acid, although in the presence of oxygen it can dissolve slightly.
There are two rows of copper compounds. Copper compounds (I) are derived from copper (I) oxides of red Cu2O, and
contain Copper (I), Cu2+ ions. These compounds are colorless, most Copper salts are insoluble in water, their behavior
is similar to the silver compound (I). They are easily oxidized into Copper (II) Oxide, CuO black compounds. Copper (II)
salts are generally blue, either in hydrate, solid, or in aqueous solutions. Anhydrous (II) aqueous salts, such as Copper
(II) sulphate anhydrous CuSO4, are white (or slightly yellow).

Basic Theory
-Introduction
Most Cu (I) is quite easily oxidized to Cu (II), but subsequent oxidation to Cu (III) is difficult. The solubility
of copper hydroxide produces hydrate crystals, the best known CuSO4.5H2O blue sulfate, it can be
hydrated into a completely white anhydrous substance. The addition of the ligand to the aqua solution
leads to the formation of the complex by the exchange of water molecules sequentially with NH3. For
example the species [Cu(NH3)(H2O)5]2+.

If the ammonia solution is added to the Cu2+ ion solution, the blue solution turns dark blue due to the
occurrence of water ligand accidents by the ammonia ligand. This reaction is take place at ph = 8.

Basic Theory
-introduction
Section 2 Procedure Experiments
Apparatus-Reagents and Flow Chart
8
Apparatus
-Procedures Experiments
and Reagents
Apparatus
– Measuring cup 50 ml – Glass watches
– The glass beaker 100 ml – Funnel glass
– Pipette drops – Allumium Foil
– Mixer glass – Paper Filter

Reagents
Crystalline solid CuSO4.5H2O
Aquades
Ethanol
Concentrated Amonia

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9
Flow Chart
Synthesis of tetra amin copper (II) sulphate complex

2 3
1 Add drop by drop of concentrated NH3, stir it Add 20 mL of ethanol slowly through the walls of the
Weigh 1.25 g CuSO4.5H2O then dissolved until homogeneous (Amonia excess) and the beaker until formed 2 layers. Do not be stirred or
in 5 mL aquades in a glass beaker 50 mL precipitate is dissolve shaken.

4
Cover with a alumunium foil.
6 5 Store it in refrigerator for
Weigh the dry crystals that produced and
Dry the crystals in the oven at 60oC overnight to crystallize.
determine how many moles of ammonia are
used as well as the calculated yield of the until the water content is lost (about
results obtained. 2 hours)

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10
Flow Chart
Study the properties of the complex salt tetrammintembaga (II) sulphate

Weigh a number of times of the obtained complex salt and then dissolve
1. it with 10 mL of distilled water. Measure the absorption spectrum at area
300-800 nm

Studying the properties 2.

Reaggregate 2 mL of the solution with 1 mL KSCN 0.5 M. Observe the
change and measure the absorption spectrum at 300-800 nm
through Spectophotometry
UV-VIS, Conductivity Tools, and
3. Make a solution of NaCl, CuSO4, MgCl2, FeCl3, and the synthesized compounds,
FT-IR make it with a concentration of 0.025 M and measured it conductivity.

Place a small amount of the complex salt obtained in the ATR-FTIR sample
4. holder. measure the IR spectra of the sample. Compare with its constituent
compounds.

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Section 3 Results and Discussion
Results and Discussion
12
Results
-Results and Discussion

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 Discussion : The Synthesis of Complex Salt
13
Results and Discussion
If the ammonia solution is added to the Cu2+, ion solution, the blue solution turns dark blue due to the occurrence of water ligand accidents by the ammonia
ligand, according to the reaction.

[Cu(H2O6)]2+ (aq) + 5 NH3 (aq) → [Cu(NH3)(4-5)(H2O)(2-1)]2+ + 5 H2O (l)

Experiment of making complex salty of tetramin copper (II) sulfate hydrate ([Cu(NH3)4]SO4.xH2O) is principled in the manufacture of complex compounds by
recrystallization principle. Where a crystal is dissolved in aquades of heat until dissolved and then added NH4OH and ethanol to trigger the formation of
the precipitate and the mixture is cooled and filtered where the precipitate is taken and then dried in the oven and a salt of tetramin copper (II) sulfate
hydrate is formed.

The first step in the lab is to dissolve the pentahydrate copper (II) sulfate into the aquadest. Copper to be reacted as much as 1.2573 g and light blue. The
addition of copper (II) sulfate pentahydrate to this aquadest will form a hydrate ligand i.e. [Cu(H2O6)]2+ with coordination number 6. The color of the
solution in this step is light blue and sediment formed at the bottom of the test tube.

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 Discussion : The Synthesis of Complex Salt
14
Results and Discussion
The next step is to add concentrated ammonia or NH3 to the solution drop wise while stirring to accelerate the reaction due to the presence of large kinetic
energy, then settle at room temperature until the soluble dissolves completely. In this stage there is a change that is the color change to dark blue and
soluble sediment. This occurs because if the ammonia solution is added to the Cu2+ ion solution, the blue solution turns dark blue due to the occurrence of
H2O ligand crowding by the ammonia ligand (Sugiharto, 2003). The addition of ligand in the hydrated solution causes the formation of complex
compounds due to the exchange of water molecules with NH3 in sequence.

[Cu(H2O)4]2+ (aq) + 4 NH3 (aq) → [Cu(NH3)4]2+ (aq) + 4 H2O(aq)

Dark blue

After dropping of ammonia, the salt solution then begins adding ethanol 20 mL, to form 2 layers. In the experimental results, there are 2 layers with a clear
top layer of dark undercoat. The addition of 20 mL of ethanol aims to concentrate the solution so as to trigger the formation of the precipitate. After that
the solution is covered with aluminum foil and cooled for 3 days to lower the temperature so that the solubility is reduced and the precipitate is formed.
After cooling is re-formed 3 layers, the crystals [Cu(NH3)4]SO4.5H2O is precipitated and which is marked by dark blue layer located at the top of the layer.

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 Discussion : The Synthesis of Complex Salt
15
Results and Discussion

The precipitate formed was filtered off and then dried in an oven (60oC) to evaporate the remainder of the filtrate to
obtain the hydrothermal (II) sulfate hydrate ([Cu(NH3)4]SO4.xH2O) crystal. Having obtained pure crystals in the absence
of a solvent, the crystals are then weighed. The resulting crystals were 0.2761 g.

However, in our experiments after the cooling process of crystals that forms a light blue color crystal. It is suspected
that the salt crystals of the tetra amin copper (II) sulfate hydrate complex follow in with the mixture of ethanol and
ammonia. This error is likely to occur in the salt crystallization process after forming 3 layers, because at the time of
filtration of salt crystals do not use the pipette but dredged with a spatula so that the sediment becomes mixed and
cannot be separated again.

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 Discussion : The Properties of Complex Salt
16
Conductivity Tool
The formed salt crystals will be tested for conductivity by conducting the conductive test apparatus. Conductivity is the
ability of a material (solution, gas, or metal) to conduct an electric current. In this calibration test, the
comparative solution and sample experiment solution will be tested its ability to conduct the electricity. The comparative
solutions to be tested were also CuSO4, NaCl, KSCN, FeCl3, and sample salts from the tetra amin copper (II) sulfate
hydrate lab. The results of the conductivity of each sample are:
CuSO4 0.25 M : 16.75 µS atau 0.035 mS
NaCl 0.25 M : 24 mS
KSCN 0.1 M : 26.4 mS
FeCl3 0.25 M : 55 mS
Original sample (the resulting salt from experiment) 0.005 M : 2 µS atau 0.002 mS
Sample from lab 0.25 M : 1.02 µS atau 0.102 mS

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 Discussion : The Properties of Complex Salt
17
Conductivity Tool

The calibration tool is 1413 μS, its means the calibration start on buffer standard point 1413 μS. Comparative solution with
sample is difficult to compare the conductivity level because each concentration of each solution is different so it cannot
be compared. Using conductivity tools, the solution must have the same concentration so that the number of
conductivity can be measured, volume of solution is same, and the solubility. Based on theory, increasing the
concentration of chemicals in a solution will increase the conductivity. Looking the result of experiment, FeCl3 0.25 M
have the highest number of conductivity, its reach 55 mS. FeCl3 is the salt that can easily dissolved in water so that the
electrolyte power of water to drain electricity becomes higher, because the more dissolved salts the better the
electrical conductivity of the water.

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 Discussion : The Properties of Complex Salt
18
FT-IR

The second test uses FT-IR. The purpose of testing using FT-IR is to know the difference in spectra and absorption in the
infrared region of the ligands found in the complex salts. The sample tested is a sample of experimental results and
samples from the lab.

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 Discussion : The Properties of Complex Salt
19
FT-IR

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 Discussion : The Properties of Complex Salt
20
FT-IR

The FTIR is using to analyze the wavelength of certain bonding energy on spectra IR range. On wavelength 3235.92 is the
range of N-H bonding on NH3 and on 3328.38 there is overlapping with O-H bonding on H2O molecules. It is because Cu2+
makes ligand bonding with H2O and NH3. After that there is O-H stretching on wavelength 1623.94. On wavelength 1404.54
there is S-O bonding is SO4 molecules. On wavelength 1270.32 there is Cu-S bonding in CuSO4 molecules. On 719.06 there
is Cu-N bonding in [Cu(NH3)4]2+ molecules. The FT-IR results shown all of wavelength on bonding energy of tetra amin
copper (II) sulphate.

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 Discussion : The Properties of Complex Salt
21
UV-Vis

(2) Spectrum Absorbance Complex Salt (3) Spectrum Absorbance Complex Salt Tetra amin
Tetraamin copper (II) sulphate as Experiment copper (II) sulphate as Sample from Lab
Results

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 Discussion : The Properties of Complex Salt
22
UV-Vis

Figure 2. is from experiment results, it is produce noise because in the cuvet there is still precipitate that cannot
dissolved in aquades. This is because complex salt in dissolved in methanol, so when complex salt of the result of
experiment is being dissolved in aquades and putting it in cuvet, there are probably still left some soft particles or small
precipitate and produce noise on the curve.
Meanwhile figure 3 is coming from the examination of good samples from lab. Those curve stated that the number of
absorbance is started on 3.0.

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Section 4 Closing
Conclusion and Suggestion
24
Conclusion
-Closing
and Suggestion
Conclusion
The nature of the complex salts that if dissolved in water will decompose into complexes and
ions. Crystalline salt of tetra amin copper (II) sulfate hydrate [Cu(NH3)4SO4.xH2O] formed
0.2671 g with remendment of 23.48%.

Suggestion
• Students may focus and understanding when doing experiment
• Understand the basic theory of experiment
• Not in hurry when doing experiment

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Section 5 References
 References
26

Cotton and Wilkinson. 1989. Kimia Anorganik Dasar. UI-Press : Jakarta.

Goldberg, D. E. 2007. Fundamentals of Chemistry. 5th edition. New York: McGraw-Hill Production.
Sugiharto. 2003. Dasar-dasar Kimia Anoraganik Logam. UI-Press : Jakarta.
Sukardjo. 1985. Kimia Koordinasi. PT. Bina Aksara : Jakarta.
Svehla, G. 1990. Vogel : Buku Teks Analisis Anorganik Kualitatif Bagian I. PT Kalman Media Pusaka : Jakarta

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Section 6 Appendix
28
Appendix

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That’s all! Thank you! 
Any questions?

Inorganic Chemistry
By 1st Groups
---Diyah, Erta, Intan, Nurul