ERTA ALIFAH FEBRIANTI | 431416014 | PK 1 2016

EXPERIMENT 3

EXTRACTION ALUMINA FROM ZEOLIT

Date : April, 23rd 2018

1. Introduction
1.1 Objective
Studying metal oxide extraction from mud and characterizing the produced
compounds by FTIR.
1.2 Theory
Much attention has recently been paid to the design and application of inorganic
membranes because of their high thermal resistance, high mechanical strength and
chemical inertness. Zeolites are of great interest as new materials for inorganic
membranes because the micropore systems of zeolites are inherent for the structure
and their pore dimensions are precisely controllable by ion-exchange and chemical
vapor deposition.
The natural mixture of minerals in the soil and rocks affects the stability because
nature will recognize its components in a natural way. The steps of mineral separation
require knowledge of the inorganic cations and their solubility and chemical reactions
necessary for chemical mineral extraction. Separation of minerals in general is not a
simple process natural rocks will contain a mixture of minerals in the form of highly
stable mixed compounds. (Surjani Rahardjo, 2013)
Aluminum is a good electrical conductor. However, Al2O3 acts as an acid oxidation
or alkaline oxidation. Oxidation with with this ability is called amphoteric
(amphoteric of the Greek word amphos, meaning both). Al2O3 insoluble in water but
exhibits its amphoteric properties through its reaction with both acidic and basic
solutions.
Al2O3(s) + 6 HCl(aq)→ 2 AlCl3(aq) + 3 H2O(l)
Base acid
AlCl3(s) + 2 NaOH(aq)+ 3 H2O(l)→ 2 Na[Al(OH)4](aq)
This amphoteric properties is signifies the point of exchange of the basic oxyadtion
to the acid oxidation in the elements of the third period. (Oxtoby, 2013)
2Al(s) + 2OH-(aq) + 2H2O → 2AlO2-(aq) + 3H2(g)
Alumina can be obtained from its hydroxide heating. The heating of this hydroxide
above 850oC produces oxides that are insoluble in both acid and base, but at heating
below 600oC is obtained oxide which is soluble in both acid and base or is
amphoteric.(Kristian,2010)
Aluminum oxide is alumina (Al2O3). Nevertheless, this simplicity is offset by the
presence of polymorphic and hydrated ingredients of a nature depending on the
conditions of manufacture. There are two forms of Al2O3 anhydrous α- Al2O3 and
γ- Al2O3. Other trivalent metals (eg Ga, Fe) form the oxides both the same
structure. Both have a densely packed order of ionine oxide but differ in their cation
arrangements. α- Al2O3 is stable at high temperatures and is also infinitely
metastable at low temperatures. Its contained in nature as corundum minerals and
can be prepared by heating γ - Al2O3 or any anhydrous oxide above 1000⁰C. γ-
Al2O3 is obtained by dehydration of the dihydrate oxide at low temperature (~
450⁰C). α- Al2O3 is hard and resistant to hydration and acid absorption. γ- Al2O3
easy to absorb water and dissolve in acid; alumina used for chromatography and the
condition set for various reactivities is γ- Al2O3.
Reaction with water
Alumina can not react simply with water and is not soluble in water. Although
alumina still contains oxide ions, but the solid lattice is too strong to react with
water. Reaction with Alumina acid contains oxide ions, so it can react with acids.
For example, alumina will act with hot aqueous chloride acid to give an aluminum
chloride solution.
Al2O3(s) + 6HCl(l) → 2AlCl3(l)+ 3H2O(l)
In this case (and similar in reaction with other acids), alumina shows the basic side
of its amphoteric properties. Reactions with Alumine bases may also exhibit acid
properties, can be seen in reaction with a base such as a sodium hydroxide solution.
Hot concentrated sodium hydroxide solution can react aluminum oxide to give a
colorless sodium 10 tetrahydrosoaluminate solution.
 ERTA ALIFAH FEBRIANTI | 431416014 | PK 1 2016

Al2O3(s)+ 2NaOH(aq)+ 3H2O(l)→ 2NaAl(OH)4(aq)

(Jim Clark. 2007)

2. Methods
2.1 Apparatus and Materials
Equipments - Beaker glass 50 mL, Measuring glass 10 mL, Magnetic stirrer,Hot
plate,Analytical balance, pH universal indicator, Glass funnel, Glass watches,Oven,
thermometer.
Materials - For the materials you need Dry mud, Distilled water, NaOH , HCl 2 M,
Paper filter.

2.2 Procedure
• 2,5 grams dry mud weighed and 15mL NaOH 2M added in the beaker glass then stirred
for 30 minutes. The precipitation is separated using filter paper then the filtrate moved
into beaker glass 50 mL. HCl 2M solution added till pH 8, and checked using pH
universal. The solution heated (70⁰C) till the precipitation formed , then cooling it. The
precipitate washed by aquadest to a neutral washwater pH, then the precipitate is heated
again in the oven at 110 ° C to a constant weight. The final precipitation mass weighed
and analyzed by FTIR.

3. Discussion and Results

3.1 Observation and Result
No Procedure Observation
1. Dissolve dry mud Dry mud = powder
a. Weighing the dry mud Mass = 2,5355 grams
b. Dissolving the dry mud V. NaOH = 15 mL
with NaOH using Dissolved 2,5355 grams dry mud with 15 mL
magnetic stirrer NaOH in beaker glass
Solution color = grey
Time = 30 minutes
2. React the filtrate with HCl V. HCl= 10 mL
 Reaction
AlO2- + HCl Al(OH)3 + Cl
Before rx After rx
Color transparant murky
Precipitation - √ ( ph 8)
3. Heat the solution Color of the precipitate = white
Degree = 70⁰C
Time = 1 hours
Volume after the adding of HCl = 30 mL
4. Wash the precipitate Color of the precipitate is white in filter paper
5. Drying the precipitate use oven Color of the precipitate = white
Degree = 110 ⁰C
6. Weigh the precipitate Mass = 0,0074 grams
7. Analyze with FTIR
Peak Area (cm-1) Functional Group

3471.01 O-H

3736.35 O-H

2320.98 O-H*

1642.72 O-H*

1051.86 Al-OH

462.8 Al-O

718.09 Al-O

787.80 Al-O
 ERTA ALIFAH FEBRIANTI | 431416014 | PK 1 2016

19
18

16

14 2320.98cm-1
718.09cm-1
12 787.80cm-1
%T

10
3840.03cm-1 1642.72cm-1

8 3736.35cm-1
461.55cm-1

4 1051.86cm-1
3471.01cm-1
3
4000 3500 3000 2500 2000 1500 1000 500 370
cm-1
Graphic 1 . FTIR alumina from zeolit

3.2 Discussion

In this experiment , the mud is calcined (heating) first, the aim of this treatment to
removing water and other organic / volatile substances for 1 hours. These impurities are
separated so as not to affect production. Mixing the mud with concentrated NaOH
solution(15ml), then Al2O3 dissolved and produces aluminate ions. Reaction :
Al2O3 + 2OH- 2AlO2- + H2O.
Stir with a magnetic stirrer. After stirring with a magnetic stirer then acidified with the
addition of HCl solution 2 M drop by drop till pH 8, check it using pH universal. In this step,
you must be careful because the addition of HCl excess can lowered pH value and then
influenced the yield (more lowered pH will produce small yield). HCl is the highest degree of
reactivity than other acids and the alumina in this mud will dissolve easily in HCl in both
high concentrations (concentrated) and low concentrations (dilute).
The reaction: AlO2- + HCl Al (OH) 3 + Cl
Then heated using hot plate with temperature 70⁰C (constant) for 30 minutes till formed the
precipitation (White precipitation). Produces:
2Al (OH) 3 Al2O3 + H2O
 The purification stage of mude is done to remove the main impurities in the mude The
main impurities of mude usually consist of SiO2, Al2O3, and TiO2.After that , separate the
precipitation from filter using filtered paper, then wash it using aquades to remove the
impurities. And dried the precipitation witrh oven in 110 ⁰C for 2 hours. Carefully, move the
precipitation and using analytical balance weighing the drying precipitation, we get 0,0074
grams. The main impurities of sludge (bauxite) usually consist of SiO2, Fe2O3, and TiO2. And
after the calculation we can get the % yield of alumina is 1,15%
FTIR test for alumina

Using FTIR to test the alumina to know what the bonding in the compounds. Before test the
sample, FTIR must be cleaning using aceton then use plat KBr. After that, the sample test .
from the graphice of FTIR about the alumina, we know that the bonding in the alumina
showed in every peaks of the graphic.

Peak Area (cm-1) Functional Group

3471.01 O-H
3736.35 O-H
2320.98 O-H*
1642.72 O-H*
1051.86 Al-OH
462.8 Al-O
718.09 Al-O
787.80 Al-O
Peaks area of 3471.01 cm-1 indicates absorption of the O-H group vibration. In the alumina
crystals this group may be derived from hydrate. While 3736.35 cm-1 region are absorption areas
O-H bound to Al octahedral atoms on alumina surfaces. The new absorption bands appear at
2320.98 cm-1 to 1642.72 cm-1 which is the -OH buckling vibration of the H2O molecule . This
absorption band appears due to absorption of water from the air caused by the properties of
alumina is quite hygroscopic. The peak area of 1051.86 cm-1 indicates absorption of the Al-OH
group. The area of 500-420 cm-1 shows the existence of Al-O bonding vibration that is the area
of 462.8 cm-1. The absorption at 850-650 cm-1 that is the area of 718.09 and 787.80 cm-1
represents the vibration absorption of Al-O with a symmetric spacing vibration.
 ERTA ALIFAH FEBRIANTI | 431416014 | PK 1 2016

4. Closing
-Conclusion
From the experiments about the extraction alumina from zeolite(mud) we get % yield of
Al2O3 is about 1,15% that’s mean the impurities in the sample substance is still a lot.
-Suggestion
Must be careful, especially when the adding of HCl to get pH 8. And always paid
attention.
5. References
- Clark, Jim. 2007. Sifat Asam-Basa dari Oksida-Oksida Periode 3. http://www.chemis-
try.org/materi_kimia/kimia_anorganik1/unsur-unsur_periode_3/
sifat_asam_basa_dari_oksida_oksida_periode_3/.
- Oxtoby, D.W., H.P. Gillis and N.H.Nachtrieb, 2003. Prinsip-Prinsip Kimia Modern.
Edisi Keempat jilid II. Terjemahan S.S. Achmadi. Erlarngga, Jakarta.
- Sugiarto, H. Kristian dan Retno D. Suyanti. 2010. Kimia Anorganik Logam. Yogyakarta:
Graha Ilmu
6. Appendix

Calculation
𝑚1 𝑚2
SiO2 : Al2O3 = ∶
Moles SiO2 : Al2O3 60 102
5 : 1 𝑚1 𝑚2
Mr 60 : 102 5 : 1 = ∶
60 102

2,5355−𝑥 𝑥
Massa 300 : 102 5 : 1 = : 102
60
6.1 discussion 2,5355−𝑥 102
5 : 1 = x
60 𝑥

258,621−102 𝑥
5 = 60𝑥

300x + 102x= 258,621

402x= 258,621
x= 0,6433 gram

experomental yield
% Yield = 𝑥 100%
theoritical yield
0,0074
= 𝑥 100%
0,6433

= 1,15%
 ERTA ALIFAH FEBRIANTI | 431416014 | PK 1 2016

Ph test using ph universal filtering the solution

Filtering the solution to get yield yield after heating in the oven

Weighing the yield after the addition of HCl

The precipitation in the filtered paper