FINALDRAFT4
FINALDRAFT4
FINALDRAFT4
ABSTRACT
This study presents the physical and thermal properties, rheological behavior, chemical
and mineralogical composition and morphological structure of clay deposits at km 584, Brgy.
Pasaleng, Pagudpud, Ilocos Norte. The physical properties include are moisture content,
plasticity, particle size distribution and classification by sieve analysis (dry method) and
sedimentation method, which were determined based on ASTM. The thermal property being
determined was loss of ignition by subjecting the clay powder samples to heat treatment in the
laboratory box furnace at 1000℃ for four hours. The rheological behavior includes specific
gravity, density and viscosity by mixing clay powder with distilled water in 1:1 and 1:2 ratio and
with deflocculant and without deflocculant. The rheological behavior was measured in the clay-
water system according to Clays & Ceramic Raw Materials. The chemical and mineralogical
composition were determined by subjecting the clay sample to x-ray fluorescence and x-ray
diffraction analysis respectively. The morphological structure of clay was determined by
subjecting the clay powder sample to scanning electron microscopy analysis. The crude clay
sample undergone beneficiation process by elutriation to improve the quality in terms of its
chemical and mineralogical composition.
The results of physical properties having 0.73% moisture, for the plasticity test the clay
sample was low plasticity. In particle size distribution using dry method analysis and
sedimentation method determined the clay sample was contained dominantly of fine particles as
clay minerals.The thermal property which was the loss of ignition has a weight percentage of
11.58.
The results for the rheological behavior in density with a clay-water system 1:1 without
deflocculant, 1:2 without deflocculant and 1:2 with deflocculant, the density of the three clay-
water system was 1.39g/ml, 1.16g/ml and 2.07g/ml. And for the specific gravity was also the
same value with respect to each clay water system but the unit for specific gravity was unitless.
the result for the clay-water system having a ratio of 1:1, and 1:2 in viscosity with and without
deflocculant. The behavior of the clay-water system with no deflocculant and with deflocculant,
the MPa.S of with no deflocculant was started to decreased to increased while in without
deflocculant was inversed to the result in with deflocculant.
The chemical properties, different treatments were used in identifying the chemical
components of the clay, which is the moisture content, passing 200 mesh, sedimentation,
elutriation and the loss of ignition samples. The x-ray fluorescence analysis results showed that
the major chemical constituent oxides are silica and alumina with the value of 39.04% to 43.07%
and 35.41% to 44.65% respectively. The x-ray diffraction analysis result showed that the mineral
content of the clay was dominated by kaolinite, then hematite and anorthite.
The finding of the study, it showed the clay deposit of Brgy. Pasaleng, Pagudpud, Ilocos
Norte was suit for academic study.
Keywords: clay powder samples, physical and thermal properties & rheological behavior
I.INTRODUCTION
The oldest ceramic raw material is undoubtedly clay. Clay has been defined as an earth
that forms a coherent, sticky mass when mixed with water; when wet, this mass is readily
moldable, but if dried it becomes hard and brittle and retains its shape. Moreover, if heated to
redness, it becomes still harder and is no longer susceptible to the action of water. Clay may take
various form; it is easily recognized as the sticky, tenacious constituent of soil, but it frequently
occurs as a rock which, owing to compression, is so hard and compacted that it is not initially
plastic and is almost impermeable to water [1].
The objective of the study for moisture content is to determine the amount of water
present in a clay expressed as a percentage of the mass of dry clay, for density and also for the
specific gravity to determine the Pasaleng clay density and specific gravity. For plasticity test to
determine whether it has a low or high plasticity, the objective for particle size distribution
analysis is a necessary classification test for clay, in that it represents the relative portions of
different sizes of particles. To determine the fine, moderate and coarse particle of the Pasaleng
km 584 clay and also aims the process by which the particles are formed by accumulation of
sediment. For viscosity is to determine the measurement of the internal friction of a liquid. For
loss of ignition it was to determine the weight between before and after drying in the high
temperature furnace. The X-Ray Diffraction was to determine the diffraction pattern of Pasaleng
clay and for X-Ray Fluorescence is to determine the chemical composition of all kinds of
materials. The materials can be in solid, liquid, powdered, filtered or other form.
The clay used in conducting the experiment was Pasaleng clay. It was also done through
experimentation by evaluating the physical property such as moisture content, plasticity test,
particle size distribution by sieve analysis (dry method) and sedimentation method. Loss of
ignition for the thermal property. For rheological behavior such as density, specific gravity and
viscosity. And for the chemical property such as X-Ray Diffraction and X-Ray Fluorescence.
II.EXPERIMENTAL METHODOLOGY
Physical Characterization
Figure 1. The experimental flow chart of the study for moisture content determination
Fig 3. The experimental flow chart for particle size distribution by sieve analysis.
15 minutes. Wait for 24 hours before measuring the samples with a ruler. For the three remaining
samples, repeat the procedure by using distilled water.
Fig 4. The flow chart for sedimentation using tap and distilled water
Thermal Property
Rheological Behavior
2.8 Viscosity
Viscosity may be defined as the resistance of a liquid to flow. As a general rule, when a
liquid flows all parts of it must be in motion, so that successive planes of molecules slide over
each other. The objective for viscosity is to determine the measurement of the internal friction of
a liquid [8].
In viscosity two samples of 100 grams was used. The two samples were mixed with water
in a beaker, with a ratio of 1:1, 100 grams of clay and 100 ml of distilled water. The clay-water
system of the one sample was mixed with 0.01ml of sodium silicate. After it was stirred
manually for thirty minutes, the digital viscometer was set up and the samples were put into the
viscometer and started showing the results in the screen of the digital viscometer.
Fig 7. The flow chart using the clay-water system with a ratio of 1:1, with deflocculant and
without deflocculant of Pasaleng clay
Chemical Properties
A.
B.
B.
Fig 9. Experimental flow chart for a.) X-Ray Diffraction and b.) X-Ray Fluorescence analysis
Morphological Structure
Figure 10 Showed the results in Cumulative Percent Finer Than and % in class of the Pasaleng
clay sample. The CPFT or Cumulative Percent Finer Than is the percent passing. The % in class
is the percent retained which the inverse of CPFT, and as the screen opening decreases the
cumulative size increases.
% in Class CPFT
100
90
80
70
60
CPFT %
50
40
30
20
10
0
pan 45 53 75 125 250 600 2000
# SIZE OF MICRONS
Table 2 presents the particle size separation by sedimentation method using a tap and
distilled water. The result of percentage for the left part was using the tap water. And percentage
for distilled water to the right part. On tap water the percentage of coarse was 16% on medium
26% and for fine it was 58% a total of 100%. And for distilled water the percentage for coarse
was 22%, 34% for the fine and it was 44% for fine. In the observed experiment, the clay sample
using tap water is faster to settle down than the distilled water used.
Table 3 presents the results for beneficiation process by elutriation using 1:1 ratio. For
the elutriation method there wasfive parts, the #20mesh, #100 mesh or coarse, #200 mesh or
medium, #300 mesh or the fine and the passing -300 mesh. The percentage for the total of #20
mesh was 28.61%, for the coarse was 13.16%, the percentage for medium was 2.92%, 3.89% for
fine and 51.41% for the passing -300.
For the density and specific gravity of the clay, H 2O was the substance used for easier
calculations using the density of the clay. The result of the density in the clay water system for
1:1 ratio was 1.39 g/ml, for the clay-water system 1:2 the average density was 1.16 g/ml, the
average density in the clay-water system 1:2 with deflocculant was 2.07 g/ml.
For the ratio 1:1 the specific gravity was 1.39, for 1:2 without deflocculant its specific
gravity was 1.16, the specific gravity of 1:2 with with deflocculant was 1.16.
Fig 12 Showed the results for the viscosity of clay-water system with and without deflocculant.
At the left as shown in the graph the clay-water system with deflocculant, the ratio used was 1:1
added with 0.01 ml of sodium silicate. The graph shown that in the clay-water the average for the
first was 22.9 MPa.S. For the second, 24.2 MPa.S and for the third reading the MPa.S was 29.7.
The graph shown in the clay-water system without defloccculant the three average for the three
readings was 328.1 MPa.S, 684.7 MPa.S and 683.6 MPa.S.
80 1000
70 900
800
60
Viscosity (MPa.S)
Viscosity (MPa.S)
700
50 600
40 500
30 400
300
20
200
10 100
0 0
0 50 100 150 200 250 300 350 0 50 100 150 200 250 300 350
Time (Seconds) Time (Seconds)
A. B.
Figure 11. Graph of viscosity vs time of the 1:1 clay-water system. A.) With deflocculant B.)
Without deflocculant
3.3 Thermal Characterization
Table 5. The result of % loss on ignition
Before After
Clay+Crucible Porcelain % LOI
Sample Porcelain
Clay (g) (g) Crucible Clay (g)
No. Crucible (g)
(g)
1 10.8736 1.0266 11.9002 11.7819 0.1183 11.5235
2 8.7892 1.0974 9.8866 9.7587 0.1279 11.6548
3 10.4816 1.2282 11.7098 11.5679 0.3397 11.5535
Table 5 presents the results for loss of ignition the clay sample was subjected to high
temperature of 1000°C. The result for the percentage loss of weight for the first sample was
11.52, for the second sample the percentage was 11.65 and for the third sample has a percentage
of 11.55. The total average of the percentage for loss of ignition 11.58%.
Table 7 Presents the results for probable mineral analysis of Pasalenng clay. Different
conditions of clay sample used in determining the probable mineral analysis. For the undergo
Moisture content, extracted from sedimentation and undergo for Loss of ignition the 100
percentage was greatly part of kaolinite. For the passing 200 mesh screen 57% of kaolinite and
31% for anorthite and a little bit percentage for Hematite and rutile. From the extracted for the
elutriation process, 91% of kaolinite and 7% part of anorthite, 6.95% for hematite and 3.82% for
rutile. For the clay powder in different conditions, the result for the Pasaleng clay has the highest
part was kaolinite.
Figure 12 Shows the diffraction of the Pasaleng clay. The different pattern of the loss of
ignition, sedimentation and moisture content was determined, mostly the detected amount was
quartz and kaolinite with a low content of hematite. However, the passing 200 mesh and
beneficiation process by elutriation shows the great amount of quartz and kaolinite and some
parts are anorthite and it is due to the clay sample that screened using 200 mesh for passing 200
and 300 mesh for the elutriation. It was reveal that the clay samples were composed of
crystalline phases of quartz, kaolinite hematite and anorthite.
Figure 12. X-Ray Diffraction pattern of the Pasaleng clay of different preparations methods.
Figure 14 Shows the image results of image for elutriation and sedimentation for SEM.
The morphological structure of the clay powder to the extracted from elutriation in sedimentation
clay. The formation of the images has been demonstrated through the results.
The morphological structure for the elutriated powder A & B, the image of the clay sample for
1000x(A) the powder was like granules and for the 5000x(B), the part of the sample which
having a white and clearer determined as quartz.
A
For the extracted powder from the sedimentation C & D, the limage at 1000x(C) the powder was
just like a granules and for the 5000x(D) the determined part was quartz and it was like a page of
book.
Morphological Structure
Fig 13. SEM micrograph image of Pasaleng Clay. A & B Elutriated clay powder and C & D
Extracted powder from the sedimentation
IV. CONCLUSION
Clay from Pasaleng, Pagudpud, Ilocos Norte was determined by physical and thermal
properties, rheological behavior, chemical and mineralogical composition and morphological
structure of clay deposits at km 584, Brgy. Pasaleng, Pagudpud, Ilocos Norte.
For the physical property which was the moisture content the clay has an average percentage
moisture of 0.73% and for plasticity the clay was poor.The thermal property which was the loss
of ignition has a weight percentage of 11.58.
The rheological behavior in density with a clay-water system 1:1 without deflocculant, 1:2
without deflocculant and 1:2 with deflocculant, the density of the three clay-water system was
1.39g/ml, 1.16g/ml and 2.07g/ml. And for the specific gravity was also the same value with
respect to each clay water system but the unit for specific gravity was unitless. the result for the
clay-water system having a ratio of 1:1, and 1:2 in viscosity with and without deflocculant. The
behavior of the clay-water system with no deflocculant and with deflocculant, the MPa.S of with
no deflocculant was started to decreased to increased while in without deflocculant was inversed
to the result in with deflocculant.
The chemical properties, different treatments were used in identifying the chemical
components of the clay, which is the moisture content, passing 200 mesh, sedimentation,
elutriation and the loss of ignition samples. The x-ray fluorescence analysis results showed that
the major chemical constituent oxides are silica and alumina with the value of 39.04% to 43.07%
and 35.41% to 44.65% respectively. The x-ray diffraction analysis result showed that the mineral
content of the clay was dominated by kaolinite, then hematite and anorthite.
The finding of this study showed that the clay deposit of Brgy. Pasaleng, Pagudpud, Ilocos
Norte was only suit for academic study.
V. REFERENCES
[1] W.E. Worall. Clay and Ceramic Raw Materials. Second Edition, Elsevier Applied Science
Publishers. (1986). P1
[2] ASTM Standards 2974-87 Standard Test Methods for Moisture Content, Ash, and Organic
Matter of Peat and Other Organic Soils.
[3] DensityDeterminationManual.pdf
[4] A. Rule & S. Guggenheim (2007). A Standards-based Curriculum for Clay Science
[5]
http://www.ninolab.se/fileadmin/Ninolab/pdf/retsch/documents/af_sieving_basics_2004_en.pdf
[6] A. Arizzi Novelli, C. Losso, G. Libralato, D. Taglaprieta, C. Pantani, A. Volpi Ghirardini.
(2005) Ecoxictocology and Environmental Safety, Is the 1:4 elutriation ratio reliable?
Ecotoxicological comparison of four different sediment: water proportions.
[7] http://www.cpsinstruments.eu/pdf/Introduction%20Differential%20Sedimentation.pdf
[8] W.E. Worall. Clay and Ceramic Raw Materials. Second Edition, Elsevier Applied Science
Publishers. (1986). P 127
[9] https://www.ecn.nl/docs/society/horizontal/hor_desk_17_annex1.pdf
[10] P. Brouwer (2003). Theory of XRF Getting acquainted with the principles, PANalytical
BV, The Netherlands.
[11] https://www.nanoscience.com/technology/sem-technology
ACKNOWLEDGEMENT
After all the days of hard works, efforts and sacrifices, finally the authors successfully
finished this study. This paper is the fruit of all waiting. Through this piece, the authors would
like to extend her gratitude and thanks to the following:
Engr. Dionesio C. Pondoc, for sharing his time and priceless suggestions and also greatly
helped in improving the paper.
Engr. Andrew C. Dono, for helping us to analyze our data in X-Ray Diffraction (XRD)
using Match 2 Software. He provided valuable input and perspective.
CIMEA (Center for Innovative Materials in Emerging Applications) for the free of
charge on the different state-of-the-art equipment including X-Ray Fluorescence (XRF), X-Ray
Diffraction (XRD), and Scanning Electron Microscopy (SEM).
Engr. April Mae Patac, for operating those equipment for our samples to be analyzed.
Engr. Rotsen Pasion, for being our laboratory aid and for providing the materials needed
in our laboratory works.
To our parents, for all the kindness and supports, for extending their helping hands.
The God almighty who gives wisdom, knowledge and strength to finish this study, for his
guidance during the time that we’re down and depress. We will lift up your name and worship
you Lord Jesus because of who you are.
VI.APPENDICES
Detailed calculations
(141.19−140.16)
Moisture Content = ×100
14 o .16
Moisture Content = 0.73%
Sample #2
(142.01−141.06)
Moisture Content = × 100
141.06
Moisture Content = 0.67%
Sample #3
(139.77−178.68)
Moisture Content = ×100
138.68
Moisture Content = 0.79%
DISTILLED WATER
Detailed Calculation
(11.9002−11.7819)
LOI (weight%) = ×100
(11.9002−10.8736)
LOI (weight%) = 11.5235g
Sample #2
(9.8866−9.7587)
LOI (weight%) = × 100
(9.8866−8.7892)
LOI (weight%) = 11.6548g
Sample #3
(11.7098−11.5679)
LOI (weight%) = ×100
(11.7098−10.4816)
LOI (weight%) = 11.5535g
TRIAL Weight of the Weight of the SPG Volume of the Density Mass of the
SPG Cup (g) Cup + clay (g) SPG Cup (g) (g/ml) clay slurry (g)
1st 36.82 47.17 8.36 1.24 10.35
2nd 36.82 45.67 8.36 1.06 8.85
3rd 36.82 46.63 8.36 1.17 9.81
Mass of Clay Slurry
Density =
Volume of Clay Slurry
1st trial 2nd Trial 3rd trial
10.35 g 8.35 g 9.81 g
D= D= D=
8.36 g /ml 8.36 g /ml 8.36 g /ml
= 1.24g/ml = 1.06g/ml = 1.17g/ml
Trial 1+ Trial 2+Trial 3
Total Average ¿
3
1.24 g /ml+1.06 g /ml +1.17 g/ml
=
3
=1.16g/ml
Viscosity