COMPLEX SALT

1. Preface

1.1 Objective

Study about reaction of making complex salt tetramincopper (II) sulphate

hydrate [Cu(NH3)4]SO4.xH2O.

1.2 Introduction

A double salt is a salt formed by crystallizing a mixed solution of an

equivalent amount of two or more specific salts. A double salt is formed when
two salts crystallize together with a certain molecular ration. The salts have their
own structure and should not be the same as the component salts structure.

A complex salt is a salt formed from an anion or a complex cation, for

example [Co(NH3)6]3+ and [Fe(CN)6]3-, otherwise known as a coordinating
compound. Example potassium hexacyanoferrat(III) or K3[Fe(CN)6].

Copper is a light-red metal, which is soft, malleable, and ductile. It melt at

1038o C. Because of its positive standard electrode potential ( +0.34 V for the
Cu/Cu2+ couple) it is insoluble in hydrochloric acid and in dilute sulphuric acid,
although in the presence of oxygen some dissolution might take place.

There are two series of copper compound. Copper(I) compounds are

derived from the red copper(I) oxide Cu2O and contain the copper(I) ion Cu+.
These compounds are colorless, most of the copper(I) salts are insoluble in water
their behavior generally resembling that of the silver(I) compounds. They are
readily oxidized to copper(II) compounds, which are derivable from the black
copper(II) oxide, CuO. Copper(II) compounds contain the copper(II) ions Cu2+.
Copper(II) salts are generally blue both in solid, hydrated from and in dilute
aqueous solution; the color is characteristic really for the tetraquocuprate(II) ion
[Cu(H2O)4]2+ only (Vogel, 1979).

One of the properties of the transition element is that it has a tendency to

form complex ions or complex compound. Ions of transition metal elements
 have empty orbitals that can accept electron pairs in bonding with certain
molecules or anions to form complex ions.

Complex ions composed of central metal ions surrounded by anions or

molecules forming a coordination bond. Central metal ions are called central
ions or central atoms. Anion or molecules that surround the central ions are
called ligands. The number of coordination bonds between central ions and
ligands is called coordination number. The central ion is the transition element
ion, can receive the free electron pair form the ligand. Free electron pair from
ligand occupy empty orbital in subshell 3d, 4s, 4p and 4d in central ions. Ligand
are molecules or ions that can donate free electron pairs to central ions. Ligand
are neutral and negatively charged or positive. Naming ligand adjusted to the
type of ligand. When there are two kinds of ligands or more then sorted
alphabetically (Maulana, 2007).

2. Methods

2.1 Apparatus and Reagent

Apparatus

In this labwork we using many apparatus to prepare the complex salt that
will be characterize. There are beaker glass 50 mL, graduated cylinder 50 mL,
volumetric pipet with pipet filler bulb, analytical balance, dropping pipet, watch
glasses, filter paper, aluminium foil, oven, and funnel. We also using an
instrument for test; FT-IR spectrometer, Conductivitymeter, and UV-Vis
spectrophotometer.

Reagent

The reagent that using is CuSO4.5H2O crystal, (NH4)2SO4 solution,

concentrated ammonia, ethanol, aquadest, and KSCN 0.5 M.

2.2 Skema Kerja

Preparation of Complex Salt

 1.25 grams of copper(II)
sulphate pentahydrate
diluted by 5.0 mL
aquadest in beaker glass
50 mL
solution added by
dropping excess
concentrated ammonia
until the precipitation
dissolved again
added 20 mL ethanol
through the glass wall
until two layer formed
(bottom = dark blue, top
= clear)

Close the beaker glass

the crystal or precipitate
with aluminium foil and
filter and put off watch
left at room
glasses. Dried crystals in
temperature, obseve the
the oven at  60o C for 2
crystal formation in next
hours, then weighed
day

Test or Characterizing

measuring conductivity.
measuring the absorbance
For the comparative
spectrum. The complex
solution, we used NaCl
salt dissolved by 10 mL
solution, CuSO4 solution,
aquadest. Then, 2 mL of
and FeCl3 solution each
this solution react with 1
with concentration 0.025
mL KSCN 0.5 M.
M.

FT-IR spectrophotometer.
A small amount of the
obtained complex salt is
placed on the sample
holder ATR-FTIR.

2.3 Procedure

Preparation of Complex Salt

First step, 1.25 grams of copper(II) sulphate pentahydrate diluted by 5.0

mL aquadest in beaker glass 50 mL. For weighed the copper(II) sulphate
pentahydrate mass, we using analytical balance.
 Second step, the solution added by concentrated ammonia dropping until
precipitate formed. Then, addition excess of concentrated ammonia until the
precipitation dissolved again.

Third step, added 20 mL ethanol through the glass wall until two layer
formed (bottom = dark blue, top = clear).

Close the beaker glass with aluminium foil and left at room temperature,
obseve the crystal formation in next day.

For last, the crystal or precipitate filter and put off watch glasses. Dried
crystals in the oven at  60o C for 2 hours. Then, the crystal that formed weighed
using analytical balance.

Test or Characterizing

There are 3 type of test or characterization. That is FT-IR spectrum, UV-

Vis spectrum, and conductivity test.

For the measuring the absorbance spectrum at 300-800 nm, first we

weighed a number of mass from complex salt. The complex salt dissolved by 10
mL aquadest. Then, 2 mL of this solution react with 1 mL KSCN 0.5 M.
Observe the change that happen and measure absorbance spectrum at 300-800
nm.

The second test is measuring conductivity. For the comparative solution,

we used NaCl solution, CuSO4 solution, and FeCl3 solution each with
concentration 0.025 M.

To measuring the IR spectrum of complex salt, we using FT-IR

spectrophotometer. A small amount of the obtained complex salt is placed on the
sample holder ATR-FTIR.

3. Results and Discussion

3.1 Results

Procedure Observation
1 Diluting 1.25 gram copper (II) sulphate  Mass of CuSO4.5H2O : 1.2540 gram
pentahydrate in 5.0 mL aquadest  Balance specs : analytical
 Vaquadest : 5.0 mL
 Solution color : blue

2 Addition of conc. Ammonia until  Precipitate color : light blue

precipitate formed dissolved again  Vammonia : 49 dropped
 Solution color : dark blue

3 Addition ethanol through the glass wall  Vethanol : 20 mL

until formed 2 layer  Top layer : clear solution
 Bottom layer : dark blue

4 Close the beaker glass with aluminium  Precipitate color : dark blue
foil and observe the crystal formation  Storage time : 2-3 days
 Vsolution :  35 mL

5 Filter and put on the watch glasses, then  Oven temperature :  60o C
dried crystals in the oven. And last,  Oven time : 2 hours
weighed  Crystal color : dark blue
 Crystal weight
= mtotal – mwatch glasses
= 21.6585 g – 21.3155 g
= 0.343 gram

Conductivity Test

𝑀𝑎𝑠𝑠 1000
Msampel = 𝑥
𝑀𝑟 𝑚𝐿

0.1556 1000
= 𝑥
317.5 50

= 0.0098 M

Because the molarity of sample solution different with comparative solution, so

the comparative solution is dilution;

V1 . M1 = V2 . M2

V1 . 0.25 = 50 (0.0098)

50 (0.0098)
V1 =
0.25
 = 1.96 mL

The results of conductivity test at T = 27.9o C;

No Solution Conductivity

1 Water 2.00 µs

2 CuSO4 609 µs

3 NaCl 637 µs

4 FeCl3 2.01 ms

5 Complex salt 931 µs

3.2 Discussion

Analysis Data

a) Mass of CuSO4.5H2O = 1.2540 gram

Mass result [Cu(NH3)4]SO4 = 0.3437 gram

𝑀𝑎𝑠𝑠
b) Mole of CuSO4.5H2O =
𝑀𝑟

1.2540
=
249.5

= 5.026 x 10-3 mol

c) Mole NH3,  = 0.899 g/mL

If we assume that 2 drop is 1 mL, so 49 drop = 24.5 mL

Mass of NH3 =xV

= 0.899 g/mL x 24.5 mL

= 22.0255 gram

22.0255 gram
Mole of NH3 = = 1.2932 mole
17,031 g/mL

d) Reaction between CuSO4.5H2O and NH3

 [Cu(H2O)5]SO4 + 4 NH3 [Cu(NH3)4]SO4 + 5H2O

m 0.0050 1.2932

r 0.0050 0.0200 0.0050 0.0250

s - 1.2732 0.0050 0.0250

e) Mass of [Cu(NH3)4]SO4 = mol x Mr

= 0.0050 mol x 227.5 gr/mol

= 1.1375 gram

practical weight
f) Rendemen = x 100%
theoretical weight

0.3437 gram
= x 100%
1.1375 gram

= 30.215 %

In the process make complex ion begins by reacting CuSO4.5H2O with a

ammonia solution with stirring until all crystal dissolve, result blue solution.
This reaction causes a stinging gas that comes from concentrated ammonia.
Ethanol classified as a volatile solvent, as well as other alcoholic properties.
Therefore, after the addition of ethanol, the glass is directly covered with
aluminium foil to reduce evaporation during the formation of crystals. This salt
formation process takes a long time to form a perfect crystal.

After the crystal formed do the filtration for separated the crystal from
solution and washed. The resulting crystals are blue and the mass of the complex
salt crystals is obtained 0.3437 grams.

4. Closing

4.1 Conclusion

 The complex tetramincopper(II) sulphate can made by reacting CuSO4.5H2O

with ammonia solution
 The ammonia, NH3, replacing the H2O position as a ligand in the central
aton.
  The mass of crystal that obtained is 0,3437 grams

4.2 Suggestion

 In the making complex ion process, the position of the beaker glass should
not be rocking
 Prepare the theory before do labwork
 Wisely in do procedure

5. Bibliography

Effendy, 1996. Sintesis dan Struktur Senyawa-Senyawa Kompleks Logam-logam

Alkali Tanah. Media Komunikasi Kimia, Vol 1, No 2.
Maulana, 2007. Senyawa atau Ion Kompleks. http://masterkimia.com
Vogel, 1979. Textbook of Macro and Semimcro Qualitative Inorganic Analysis.
Longman Group Limited. London.

6. Appendix