College of Engineering and Technology

Department of Materials and Resources ACTIVITY NO. 10

Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 1 of 3

A. PREPARATION

I. TOOLS
a. Clay Samples
b. Spoon
c. Wash bottle with Distilled water
d. Metal Mold
e. Drying Oven
f. Electric Furnace

II. MEASURING EQUIPMENT

a. Weighing Scale
b. Vernier Caliper

B. PROCESS (It is understood that Moisture Test, Residue Test, Plastic RangeTest and
Water of Plasticity Test , had already performed)

I. Drying Shrinkage Test

a. About 1 kg of dried clay is mixed with water with the amount corresponding to the water of
plasticity. Wedge the clay mass thoroughly and stay overnight for soaking.
b. Form a rectangular bar, 70 x 15 x 5 mm in dimension using the metal mold. At least 10 test
pieces per sample.
c. Make a mark on the test pieces as shrinkage reference lines 50 mm apart on the long axis.
d. Place the marked three pieces on a lightly oiled pallets and allow to dry at room temperature
for 24 hours. (Note : turn the test pieces every now and then to ensure even drying)
e. Further dry the specimens in the drying oven at 100 to 110 °C for 4 hours or until no
moisture is present.
f. Calculate the linear drying shrinkage as percent of dry strength as follows:

Sd (% linear drying shrinkage)=Initial length of the test piece (L¿ ¿1)−Dry lengthof the test piece
Initial length of th

g. Note and record any observation on the samples such as distortion, warping and etc.

II. Loss on Ignition and Firing Shrinkage Test

a. Utilized the test specimen from the drying shrinkage test for fired properties.
b. After forming the samples , initially weigh the sample test bars.
c. Then fire 5 test pieces at 800°C.
d. Examine thoroughly the test pieces and record your observation on any changes on the
samples such as cracks, warping, and etc.

Submitted by: Submitted to:

 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 2 of 3
e. Measure and record the changes in the dimensions and weight of the samples after firing and
determine the firing shrinkage and loss on ignition (LOI). Calculating the % LOI and %
Linear Firing Shrinkage is as follows:

Weight of dried samples ( Wd )−Weight of fired samples (Wf )

% LOI = × 100 %
Weight of dried samples ( Wd )

(L
Sf (% linear firing shrinkage)=Dried length o f thetest piece(L¿¿ d )−fired length of the test piece
Dried length of the te

f. Calculate the total linear shrinkage of clay by getting the sum of the linear drying shrinkage
and linear firing shrinkage.

C. AFTER PROCESS

I. ACTIVITIES AT THE END OF THE CLASS

C.I.1 Make sure that the working area is clean.

C.I.2 Make sure that tools are complete and kept in a proper place
C.I.3 Make sure the measuring equipments are in good working condition.

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 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 3 of 3

I. INTRODUCTION

1.1 Background of the Study

The purpose of this research is to investigate the Clay Samples utilizing the Loss on
Ignition Test and & Drying and Firing Shrinkage Test. This experiment was developed
through literature searches of previous studies.

1.2 Objectives of the Study

This experiment was performed to solely investigate the . It also investigates the Clay
Samples utilizing the Loss on Ignition Test and & Drying and Firing Shrinkage.

1.3 Significance of the Study

The percentage weight lost on ignition plays a significant role for materials like cement and clay
which gives a crude measure of the organic content of the sediment. Generally, percentage loss on
ignition values show an inverse relationship with percentage dry weight values. Furthermore, the
purpose of the Drying and Firing Shrinkage Test is to obtain values of shrinkage after drying and
firing of clays or bodies or both, under various processing conditions to enable designers to determine
the proper size of mold or die so as to produce a predetermined size of fired ware.

1.4 Limitations of the Study

 This test method covers the determination of linear shrinkage of ceramic whiteware clays, both
unfired and fired.
 The values stated in inch-pound units are to be regarded as standard. The values given in
parentheses are mathematical conversions to SI units that are provided for information only and
are not considered standard.
 This standard does not purport to address all of the safety concerns, if any, associated with its
use. It is the responsibility of the user of this standard to establish appropriate safety, health,
and environmental practices and determine the applicability of regulatory limitations prior to
use.

Submitted by: Submitted to:

 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 4 of 3
II. REVIEW OF RELATED LITERATURE

The Nature of Clay

Examination of data on North Wales soils shows that a good correlation exists between loss-
on-ignition and organic C values, determined by Tinsley's method. Ignition for half an hour at 850° C,
and for 16 hours at 375 f 5' C have both been employed. The latter has advantages over the former
procedure. Regression lines and prediction limits for organic C from loss-on-ignition are given from
the data obtained. Although these regressions are not necessarily expected to be generally applicable,
examination of some published data suggests that closely similar expressions may be. The method,
because of its simplicity, can be usefully applied in a wide range of survey, analytical, and ecological
studies, in spite of the known sources of error (Ball, 2015)

Drying

Water which is not consumed during the manufacturing and later hardening of some
materials (such as concrete, cement, plaster, ...) leads upon drying to a shrinkage of the
material. Drying from a free surface gives rise to an inhomogeneous shrinkage which in turn
produces stresses which may lead to cracking, when they exceed the material strength. It is
only in concrete pieces of a small size that shrinkage can be uniform enough to prevent crack
formation [1]. In general, surface elimination of water gives rise to tensile stresses in the skin
of the material which are partly released by the formation of surface cracks. The latter form a
characteristic polygonal pattern in brittle homogeneous materials (e.g. cement), and a more
complex dense array of branched cracks in more heterogeneous structures (standard concrete
and mortar). Indeed heterogeneities will favour [2–4] the nucleation of stable micro cracks
which progressively shields the stress, and gives rise to a “controlled” development of
cracking. In contrast, for homogeneous materials, the nucleation of cracks is the limiting
process. As soon as they are initiated, they tend to propagate extremely fast along the surface
in a more or less straight manner until they are stopped by other preexisting cracks. The latter
scenario gives a mosaic where at least past of the history of crack formation can be read from
the final pattern. It is crucial to understand the pattern formation of surface cracks in concrete
structures, in particular for their ageing properties. Surface cracks are easy paths for chemical
species which may react with the material or reinforcements. Thus estimating the depth and
opening of cracks is essential. The latter are however difficult to measure directly. It is thus of
interest to try to relate these properties to the surface crack pattern, which is much more easily
accessible.

Submitted by: Submitted to:

 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 5 of 3
III.METHODOLOGY

Figure 3.1 The Process Flow Chart

Prepare the
Materials/Equipment
needed

Loss on Ignition Test Drying and Firing

Shrinkage Test

Utilize the specimen from the 1 kg of dried clay is mixed

drying shrinkage test with water

Form a rectangular bar

Weigh the sample Test Bars

Make a mark on the test

pieces as shrinkage reference
Fire 5 test pieces at 800°C lines

Place the marked three pieces

on a lightly oiled pallets.
Examine thoroughly the test
pieces and record

Further dry the specimens in

the drying oven
Measure and record the
changes
Calculate the linear drying
shrinkage
Calculate the total linear Put the date in
shrinkage of clay Results

Submitted by: Submitted to:

 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 6 of 3

Analysis of Results.
3.1 The Pre-experimental Procedure

Prepare all the Materials and Measuring Equipment needed.

TOOLS
g. Clay Samples
h. Spoon
i. Wash bottle with Distilled water
j. Metal Mold
k. Drying Oven
l. Electric Furnace

MEASURING EQUIPMENT
c. Weighing Scale
d. Vernier Caliper

3.2 Main Experiment

PROCESS (It is understood that Moisture Test, Residue Test, Plastic RangeTest and Water
of Plasticity Test , had already performed)

Drying Shrinkage Test

h. About 1 kg of dried clay is mixed with water with the amount corresponding to the water of
plasticity. Wedge the clay mass thoroughly and stay overnight for soaking.
i. Form a rectangular bar, 70 x 15 x 5 mm in dimension using the metal mold. At least 10 test
pieces per sample.
j. Make a mark on the test pieces as shrinkage reference lines 50 mm apart on the long axis.
k. Place the marked three pieces on a lightly oiled pallets and allow to dry at room temperature
for 24 hours. (Note : turn the test pieces every now and then to ensure even drying)
l. Further dry the specimens in the drying oven at 100 to 110 °C for 4 hours or until no
moisture is present.
m. Note and record any observation on the samples such as distortion, warping and etc.

Loss on Ignition and Firing Shrinkage Test

Submitted by: Submitted to:
 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 7 of 3
g. Utilized the test specimen from the drying shrinkage test for fired properties.
h. After forming the samples , initially weigh the sample test bars.
i. Then fire 5 test pieces at 800°C.
j. Examine thoroughly the test pieces and record your observation on any changes on the
samples such as cracks, warping, and etc.
k. Measure and record the changes in the dimensions and weight of the samples after firing and
determine the firing shrinkage and loss on ignition (LOI). Calculating the % LOI and %
Linear Firing Shrinkage is as follows:

Weight of dried samples ( Wd )−Weight of fired samples (Wf )

% LOI = × 100 %
Weight of dried samples ( Wd )

(L
Sf (% linear firing shrinkage)=Dried length o f the test piece(L¿¿ d )−fired length of the test piece
Dried length of the te

3.3 Post Experiment

Drying Shrinkage Test

Calculate the linear drying shrinkage as percent of dry strength as follows:

Sd (% linear drying shrinkage)=Initial length of the test piece (L¿ ¿1)−Dry lengthof the test piece
Initial length of th

Loss on Ignition and Firing Shrinkage Test

Measure and record the changes in the dimensions and weight of the samples after firing and
determine the firing shrinkage and loss on ignition (LOI). Calculating the % LOI and % Linear Firing
Shrinkage is as follows:

Weight of dried samples ( Wd )−Weight of fired samples (Wf )

% LOI = × 100 %
Weight of dried samples ( Wd )

(L
Sf (% linear firing shrinkage)=Dried length o f the test piece(L¿¿ d )−fired length of the test piece
Dried length of the te

Calculate the total linear shrinkage of clay by getting the sum of the linear drying shrinkage
and linear firing shrinkage.

Submitted by: Submitted to:

 College of Engineering and Technology
Department of Materials and Resources ACTIVITY NO. 10
Engineering and Technology (DMRET)
Date : May 20, 2021
Course No. & Title : CER 127.2 Ceramic Measurements Due : May 24, 2021
Activity Title : Loss on Ignition & Drying and Firing Shrinkage Tests Page 8 of 3

III. RESULTS AND DISCUSSION

IV. CONCLUSION AND RECOMMENDATIONS

V. REFERENCES

ASTM C326 - 09(2018). ASTM International - Standards Worldwide. (n.d.).

https://www.astm.org/Standards/C326.htm#:~:text=Significance%20and%20Use,predetermined
%20size%20of%20fired%20ware.

Fatahi, B., Le, T. M., Fatahi, B., & Khabbaz, H. (2013, May 17). Shrinkage Properties of Soft Clay
Treated with Cement and Geofibers. Geotechnical and Geological Engineering.
https://link.springer.com/article/10.1007/s10706-013-9666-y.

Kingery, W. D., & Francl, J. (2006, June 2). Fundamental Study of Clay: XIII, Drying Behavior and
Plastic Properties. ACerS. https://ceramics.onlinelibrary.wiley.com/doi/pdf/10.1111%2Fj.1151-
2916.1954.tb13994.x.

Laird, D. (2001, September 1). Nature of Clay–Humic Complexes in an Agricultural Soil. ACSESS.
https://acsess.onlinelibrary.wiley.com/doi/abs/10.2136/sssaj2001.6551419x.

Assoc. Prof. Lori-ann I. Cabalo

BS CERE Faculty

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