Determination of Silicate

Minerals in Acid Sulfate

Soils Using X-ray
Diffraction Analysis
Najim Muhammad

Universiti Putra Malaysia
Department of Land
Management

Outline
Introduction

Materials and Methods

Results

Conclusion



Aluminum toxicity throughout the
world
Acid sulfate soils are categorized
by two things:
Having a pH less than 3.5
Having high Aluminum
concentration
Iron (Fe) and Aluminum (Al) give
acid sulfate soils a high toxicity,
and it affects the bio-chemical
properties of the soil.
It is difficult to grow in these soils
unless the soil is effectively
augmented.

Methods to
improve acid
sulfate soil include
liming (GML),
leeching and
drainage by water,
and submergence.
Acid Sulfate Soils in Malaysia
0
20000
40000
60000
80000
100000
120000
140000
Peninsular
Malaysia
Under rice
cultivation
Kelantan
A
r
e
a

(
h
a
)

110,000
20,000 10,000
X-ray diffraction can be used to
analyze results of soil samples.
The composition of a single
grain or crystal can be
determined
Small areas of the crystal can
have size, shape, and stress
measured.
Crystal structure of an unknown
material can be identified.
D-spacing

X-ray Diffraction
Materials and Methods
Two soil samples
were used.
Sample 1 is soil
from Semerak,
Kelantan,
Malaysia.
Sample 2 is soil
from Merbok
Kedah, Malaysia.
Both acid sulfate
soils.

Preparation of Sample
Collection of soil
Ground the soil
Sieve through 2mm sift
Weigh out 30g
Put in beaker and wet
with water
Add 50mL of hydrogen
peroxide
Let sit in beaker for 30
min

Had to let soil sit in peroxide
longer than 30 min.

Soil was continually bubbling to
the top of beaker, used alcohol to
neutralize the bubbling.

Placed samples on hot plate at
130C for increased reaction time.

After one hour took samples off
hot plate and put in sink with
water to cool off.

Added water to sample

Remove water from clay

Use pipette to collect
10mL of the sample and
put on sample slides

Let sample slides dry

Put samples in x-ray
diffraction machine


Saturation of Sample
Saturate soil samples in
Potassium Chloride
(KCl)
Determine how much
KCl to use for saturation.
250mL flask
74.56g KCl=1000mL
Combine KCl with
250mL of water
Weigh out 3g of soil in 3
containers. Two
containers contained 3g
of sample one and one
container had 3g of
sample two
Place three containers in
centrifuge

Wash saturated soil samples two times
with 30mL of alcohol and once with 30mL
of water
Used pipette to obtain sample then
released onto sample slides
Let sample dry for 24 hours
Put sample slides in x-ray diffraction
machine

Saturation of Sample
Saturate soil samples in
Magnesium Chloride
(MgCl
2
)
Determine how much MgCl
2

to use for saturation.
250mL flask
203.30gMgCl
2
=1000mL

I repeated same process
as I did for KCl saturation



Heated Magnesium Sample
Used pipette to obtain sample 2 then put
on sample slide

Let the slide dry for 24 hours

Put in furnace at 100 for 8 hours

Put in x-ray diffraction machine
Sample 1 Graph
Sample 1 Chart
Common Mineral D-spacing
D-spacings of mica are 10,5, and 3.33A. D-spacings of kaolinite are 7.2
and 3.57A. D-spacings of quartz are 4.26 and 3.3A.
Sample 2 Graph
Sample 2 Chart
Sample 1 KCl
Sample 1 KCl Chart
Sample 2 KCl Heated Graph
Sample 2 KCl Heated Chart
Sample 1 MgCl
2
Graph


Sample 1 MgCl
2
Chart
Sample 2 MgCl
2
Graph


Sample 2 MgCl
2
Chart


Conclusion
In conclusion, I have recorded that quartz
is the most prevalent mineral in all of the
samples I had. In this case it seems all
the samples had a similar make up of
100% quartz mineral. All the samples also
had appropriate amounts on mica and
kaolinite in them.
Acknowledgements
Dr. Shamshuddin Jusop
Dr. Qurban Ali Panhwhar
Dr. Azali
Dr. Ponzarina