Title

Preparation of colloidal dispersions

Objectives
1. To prepare a ferric hydroxide sol.
2. To prepare silver hydrosol by reduction with ferrous citrate and by reduction
with dextrin.
3. To understand several methods of preparation of colloid.
4. To perform a general investigation and verification of the properties of the
colloidal system.

Apparatus:

50 ml measuring cylinder
500 ml beaker
hotplate
glass rod
retort stand
cellophane
250 ml beakers
100 ml volumetric flask
dropper
blue litmus paper

Chemicals:

2% ferric chloride solution

Distilled water
silver nitrate
0.004 M sodium thiosulphate solution
0.004 M hydrochloric acid
0.02 M sodium bromide solution
0.018 M silver nitrate solution

10% silver nitrate solution

30% ferrous sulphate (FeSO4.7H2O)
40% sodium citrate (Na3C6H5O7.2H2O)
Ammonium nitrate solution
Concentrated sodium hydroxide solution
Dextrin

Introduction

Colloid chemistry is a branch of physical chemistry and is connected with the

chemical properties and the production of colloidal system. Colloidal system or
colloidal dispersion is a heterogeneous system which made substance is dispersed a
very fine particles in another substance called dispersion medium.
Preparation of the colloid
The colloid is a dispersion system of matter. When the particles of 1nm100nm of
matter disperses in the another medium, it will become a dispersed system of
colloid. The dispersed system of colloid mainly includes two types: a sol and a
macromolecular solution. For the preparation method of colloid, there is a
condensation method and a dispersion method. Matter can be put into the colloidal
state by means of dispersion methods, in which large pieces of the substance are
broken up into particles of colloidal size, and condensation methods, in which
molecules or ions or atoms are made to cluster together to form particles of the
desired size. The preparation of colloid is preceded usually with some chemical
reaction or the physical condensation.
Ferric Hydroxide Sol
Ferric hydroxide forms a lyophobic sol with water which is the dispersion medium. It
is prepared by the hydrolysis of ferric chloride with boiling distilled water as per the
reaction:
FeCl3 (aq) + 3H2O Fe(OH)3 + 3HCl (aq).
The HCl formed during the reaction tries to destabilize the sol and therefore should
be removed from the sol by dialysis. A wine red sol of ferric hydroxide is obtained.

Silver hydrosol
Silver hydrosols are one of the most attractive inorganic materials due to its
remarkable applications. Moreover, a multitude researchers in many laboratories
have been exposed the synthesis of different morphologies of advanced silver
nanoparticles. Reduction in solutions is one of the methods were used from the past
for the synthesis of silver nanoparticles. A large number of chemical reduction
methods have been applied by using different reducing agents to synthesize stable
and various shapes of silver nanoparticles in water. To reduce the silver salts, the
shape and size as well as the size distribution sturdily depended on the strong and
weak tendency of organic substrates. The chemical reduction of metal salts is the
simplest and the best frequently used of bulk-solution synthetic method for metal
nanoparticles. The surface of silver metal having free electrons in the conduction
band and positively charged nuclei due to a one-step process of producing a colored
silver sol through reduction of silver hydrosol by chemical methods. Ferrous citrate
is slightly water soluble which be prepared by reacting sodium citrate with iron(II)
sulfate. It is well known as weak reducing agent since it has an ability of one-step
reduction and coordinates with silver ions. Silver hydrosol contains around 96%
charged silver atoms, slightly lower than that of colloidal silver. While hydrosol silver
may still provide similar benefits, its considered by many to be ineffective for some
conditions. Hydrosol silver carries a greater risk for argyria than colloidal. Most
silver hydrosol on the market, however, contain no protein additives or salts. This is
a slight benefit, as silver should always be in a pure solution free of
contamination.Metal nanoparticles, especially gold and silver, are currently among
the most attractive nanomaterials due to their applications. silver nanoparticles are
being incorporated into clothes, bandages, coatings, and food containers as
deodorizers and disinfectants. Most of the above-mentioned applications of silver
nanoparticles are due to their size and shape-dependent unique chemical and
physical properties. Several protocols already exist to prepare silver nanoparticles,
the reproducible production, stability and control over their size, shape and surface
chemistry is still less established compared to gold nanoparticles. This is probably
due to easier oxidation of reduced silver and its complex interaction with a variety
of currently used stabilizers for such nanomaterials.

Discussion

In this experiment, we are going to prepare a colloidal dispersion. For the first part,
we are preparing the ferric hydroxide sol and the solution prepared has to undergo
dialysis process. Ferric chloride is also known as iron (III) chloride is one type of
metals. As ferric chloride is a metal, although we heated it until boiling it will still
remain the solid residue in the water and cannot evaporates but as we see the
boiling solution, there was no suspended solid that can be seen thus we can say
that the ferric chloride solution that was prepared is a colloidal solution.
If a concentrated iron (III) chloride solution is boiled, it will produce a small amount
of hydrogen chloride gas which is very toxic to human and has corrosive properties.
When the concentrated solution of iron (III) chloride was heated, hydrolysis occur
producing hydrogen chloride, some of which will escape as a gas and some will
remain in water and form hydrochloric acid.

Ferric Hydroxide Sol

In the first procedure, ferric hydroxide formed a lyophobic sol with water which was
the dispersion medium. It was prepared by the hydrolysis of ferric chloride with
boiling distilled water as per the reaction:

FeCl3 (aq) + 3H2O Fe(OH)3 + 3HCl (aq)

The HCl formed during the reaction tried to destabilize the sol and therefore should
be removed from the sol by dialysis. A wine red sol of ferric hydroxide is obtained.
This proved that the ferric hydroxide molecules diffused out from the cellophane
into the distilled water in the beaker.

For this experiment, we are preparing 2% of ferric oxide in 100mL of water. Thus the
solution was added to 250mL of distilled water. As the ferric chloride has low
concentration therefore it is not very harmful if the solution is heated. Then the
ferric chloride solution prepared has to undergo dialysis to remove hydrochloric acid
produce. Dialysis process is where a true solution is pass through a semipermeable
membrane while the colloidal particle not. The pore size of the semipermeable
membrane permits the passage of small molecules or ions.
The colloid solution which is the ferric chloride is placed in a cellophane bag and the
bag was suspended in a large water bath. The cellophane bag has to be tied tightly
as to prevent from the ferric solution enter the water bath. This dialysis process is
very slow. Thus it has to be leaved for about 24 hours. After 24 hours solid AgNO3
was added to the water bath. After several minutes, we can see the formation of
white precipitate at the bottom of the beaker.
The white precipitate is the

Silver Hydrosol

In the experiment, the preparation of silver hydrosol was from the reaction of
ferrous sulfate with sodium citrate and produced ferrous citrate which acts as
reducing agent to silver nitrate. Some elements have electrons that absorb certain
wavelengths as it provides energy to the elements that will often emit another
wavelength to get rid of the extra energy. The energy state of the electron is related
to the wavelength that it absorbs. The bonding in this element affects the energy
state of these electrons. Consequently, bonds to different elements will produce
different colors. From the first observation, the combination of this chemical
reaction made the solution turned to brown in color. The solution was neutralized by
adding some trace amount of concentration sodium hydroxide and the blue litmus
papers were used as indicator to make sure the solution became neutral. The use of
sodium hydroxide is most suitable since it is soluble in water. The second

observation was realized when the solution turned into precipitate with changed
color to lilac. This is due to the immediate reaction of neutral aqueous ferrous
citrate and silver nitrate respectively. Nevertheless, the lilac-colored precipitate was
tossed down and successively turned dark blue when we stirred vigorously the
solution. This is because silver halide are sensitive to blue light so it absorbed all
the blue light and sent only the green and red light separately when it exposed to
the light. During the filtering process, the retained silver precipitate was washed
using prepared ammonia nitrate solution. The ammonia cation neutralized the
charge on the silver micelles accordingly inhibiting their dispersion by coagulating
all the charges in the solution as it act as the stabilizing agent.

The precipitated colloidal silver was reversible because it was dispersed by

removing the neutralizing cations. On the other hand, we washed the precipitate
with distilled water and consecutively it attacked the precipitate and passed through
the filter paper due to the characteristic of distilled water as hydrophilic solution.
The color was ranging from bright red to a very deep red-brown color. The
precipitate was washed using two or three small quantities of 7% ammonium nitrate
and it was turned to red in color. We added the 7% ammonium nitrate once again
because we need reprecipitated it again. The precipitate was washed with distilled
water and resumed silver hydrosol. The silver hydrosol was bright red in color and
when we transmitted it to the light, it was turned to chocolate brown. The next
method was proceeded to determine whether the process is irreversible or
reversible. The yield precipitate was added with a few drops of calcium chloride as
calcium chloride acts as hydrophobic. Hence, the yield precipitate that was added
with calcium chloride changed from red to colorless and was filtered from filter
paper. So, the process called irreversible achieved our second objectives.

Next we proceed with the silver hydrosol experiment. Silver hydrosol can be
prepared as to be a suspended solution or a colloidal solution. To make a suspended
solution of silver hydrosol it is by the reduction with ferrous citrate.

In the fourth procedure, preparation of silver hydrosol by reduction with

ferrous citrate, a dark brown solution was formed. When silver nitrate was added to
ferrous citrate, ferrous ion (Fe2+) reduced silver ion (Ag+) to solid silver (Ag) and
became ferric ion (Fe3+). What caused the silver solid to disperse was citrate ion
that "stick" outside the silver solid causing it to be negatively charged and Ag
repelled each other. Mechanism for dextrin was where the silver was reduced by
reducing sugar (dextrin) to form a silver solid. The solid then bound on the complex
chain of dextrin to stay dispersed in medium that caused formation of brown
precipitate.