Loss On Ignition (L.O.I) : Concrete Technology (I) Lecture 3

Concrete Technology (I) Lecture 3
Loss on Ignition (L.O.I)

It is the loss of the cement sample weight when it expose to the red temperature (at
1000°C). It shows the extent of carbonation and hydration of free lime and free
magnesia due to the exposure of cement to the atmosphere. Also, part of the loss in
weight comes from losing water from the gypsum composition. The maximum loss
on ignition permitted by Iraqi specification no. 5 is 4% by weight.
Insoluble residue (I.R)

It is that part of cement sample that is insoluble in HCl. It comes from the
unreacted silica, to form soluble cement compounds diluting in this acid, largely
arising from impurities in gypsum. The maximum insoluble residue permitted by
Iraqi specification no. 5 is 1.5% by weight of cement.
Hydration of cement
It is the series of chemical reactions for cement with water to form the binding
material. In other words, in the presence of water, the silicates (C3S and C2S) and
aluminates (C3A and C4AF) form products of hydration which in time produce a
firm and hard mass called the hydrated cement paste.
There are two ways in which compounds of the type present in cement can react
with water:
I. In the first, a direct addition of some molecules of water takes place, this
being a true reaction of hydration
II. The second type of reaction with water is hydrolysis , in which its nature
can be illustrated using the C3S hydration equation:
02
3CaO.SiO2 + H2O → Ca(OH)2 + xCaO.ySiO2 (calcium silicate hydrate)

2 C3S + 6H → 3Ca(OH)2 + C3S2H3
The reaction of C3S with water continue even when the solution is saturated with
lime and the resulted amounts of lime precipitate in crystals form Ca(OH)2 .
Calcium silicate hydrate → remains stable when it is in contact with the solution
saturated with lime.
Calcium silicate hydrate→ hydrolyzed when being in water – some of lime form,
and the process continues until the water saturate with lime.
If the calcium silicate hydrate remains in contact with water → it will leave the
hardened compound only as hydrated silica due to the hydrolysis of all of the lime.
The rates of the chemical reactions of the main compounds are different:
 Aluminates:
1- React with the water in the beginning,
2- Affect the route of the chemical reactions at early periods of
hydration.
 Silicates:
 Affect the later stage reactions.
02
The main hydrates of the hydration process are:

 Calcium silicates hydrate, including hydrated products of C3S (not
pure) named as Alite, and C2S (not pure) named as Belite.
 Tricalcium aluminate hydrate (C3A).
 C4AF hydrates to tricalcium aluminate hydrate and calcium ferrite
CaO.Fe2O3 in amorphous form.
Since calcium silicates (C3S and C2S) – are the main cement compounds (occupies
about 75% of cement weight) – they are responsible for the final strength of the
hardened cement paste.
With time:
 The rate of hydration decreases continuously.
 The size of unhydrated cement particles decrease. For instance, after 28 days
in contact with water, grains of cement have been found to have hydrated to
a depth of only 4 μm, and 8 μm after a year.
This is due to:

1. Accumulation of hydration products around the unhydrated cement grains
which lead to prevent water from channeling to them.
2. Reduction of the amount of water either due to chemical reaction or
evaporation.
3. Reduction of the amount of cement due to reaction.
00
The progress of hydration of cement can be determined by different means:

 The measurement of the amount of Ca(OH)2 in the paste resulted from the
hydration of the silicates.
2 C3S + 6H = C3S2H3 + 3 Ca(OH)2
2 C2S + 4H = C3S2H3 + Ca(OH)2
 The heat evolved by hydration.

 The specific gravity of the paste.
 The amount of chemically combined water.
 The amount of unhydrated cement present (using x-ray quantitative analysis)
 Also indirectly from the strength of the hydrated paste.
Tricalcium aluminate (C3A) hydrate and the action of gypsum:

The amount of C3A present in most cement is comparatively small but its behavior
and structural relationship with the other phases in cement make it of interest. The
tricalcium aluminate hydrate forms a prismatic dark interstitial material in the form
of flat plates individually surrounded by the calcium silicate hydrate.
The reaction of pure C3A with water is very violent with evolution of large amount
of heat, forming calcium aluminates hydrate in the form of leaf hexagonal crystals.
In Portland cement, this reaction leads to immediate stiffening known as "flash
setting". Gypsum, added to the clinker through grinding process cause delaying
the reaction of C3A with water by its reaction with C3A to form insoluble calcium
sulfoaluminate (3CaO.Al2O3.3CaSO.30-32H2O) - ettringite around C3A particles,
which permits enough time for the hydration of C3S that its reaction is slower than
C3A and permits the occurring of natural setting.
02
But eventually tricalcium aluminate hydrate is formed, although this is preceded by

a metastable (CaO.Al2O3. CaSO.12H2O), produced at the expense of the original
high-sulfate calcium sulfoaluminate.
The reaction of gypsum with C3A continues until one of them exhausted, while
C3S continue in hydration.
 If C3A exhausted before gypsum: The surplus gypsum → expand → become
an agent assist the disruption and deterioration of cement paste.
 If gypsum exhausted before C3A The remaining C3A begins in hydration:
C3A + 6H → C3AH6 … were this form (C3AH6) is stable - cubical crystals -
with high sulfate resistance.
Calcium aluminate hydrate – Be at many forms before transforming to the stable

state (C3AH6). It is probably forming hexagonal crystals (C4AH8, C4AH10, C4AH12)
before the cubical crystals. When the hexagonal crystals expose to sulfates (inside
concrete from sand or external from soil or ground water) → react with it forming
calcium sulfoaluminate → with increase in volume, depending on the amount of
remaining aluminates and the concentration of sulfates → leading to crack and
deteriorate of the hardened concrete.
The transformation of calcium aluminates hydrate from the metastable

hexagonal form to the stable cubical form is accompanied with – change in the
density and size of the crystals – leading to decrease in the late ages strength
of the cement paste due to:
02
1- Lose the adhesion and cohesion in the microstructure,

2- Increase the porosity of the hardened cement paste.
The presence of C3A in cement is undesirable

1) It contributes little to the strength of cement except at early ages (1-3 days)
and,
2) When hardened cement paste is attacked by sulfates, expansion due to the
formation of calcium sulfoaluminate from C3A may result in a disruption of
the hardened paste.
But it is useful in the cement industry

I. work as flux material to reduce the temperature needed to form the
clinker; and
II. Also it facilitates the combination of lime with silica.
C4AF compound: Gypsum reacts with C4AF to form calcium sulfoaluminate

and calcium sulfoferrite. C4AF work
1- as flux material and also
2- it accelerates the hydration of silicates.
Using the optimum percentage of gypsum is very important , because:

I. It regulates the speed of the chemical reactions in the early ages.
II. Prevent the local concentration of the hydration products.
02
The necessary gypsum content increase with the increase of:

1) C3A content in the cement;
2) Alkalis content in the cement; and
3) Fineness of cement.
 Iraqi specification No. 5 limits the maximum gypsum content (expressed as

the mass of SO3 present) to be not more than 2.5 % when C3A ≤ 7 % and 3
% when C3A > 7%.
Calcium silicates hydrate:

C3S:
C3S + water lime and silica ions in the solution with molecular
weight of 3:1;
Ca(OH)2 crystals; and
Calcium silicate hydrate gel (C3S2H3) - tobermorite.

2C3S + 6 H = C3S2H3 + 3Ca(OH)2
2C2S + 4 H = C3S2H3 +3Ca(OH)2
The product of hydration is called is called Tobermorite (CSH) and C3S

produce more than twice as much Ca(OH)2 as formed by the hydration
C2S
 Hydration of C3S – take about one year or more.
02
This initial gel form an external layer over C3S causing the delay of the reaction.
After few hours, this initial C-S-H undergo hydrolysis to form the second product
of the gel CSH I with C:S equal 1.5 then form the stable C-S-H II form with C:S
equal (1.4-1.6).
The full hydration of C3S can be expressed approximately by the following
equation:
2(3CaO.SiO2) + 6H2O •→ 3CaO.2SiO2.3H2O + 3Ca(OH)2
2C3S + 6H •→ C3S2H3 + 3Ca(OH)2
(100) (24) (75) (49)
C2S:
There are three main crystal forms of C2S (α , β, γ) but the β-form is the only one
occurred in the Portland cement and it react slowly with water.
 Its reaction is slower than C3S.
 The amount of Ca(OH)2 from its hydration is less.
Its formed gel is similar to that produced from C3S, but there is difference in the
route of the chemical reactions between the two compounds - the lime: silica
during the hydration of C2S differs than that formed during the hydration of C3S. It
is in the initial product formed as external layer at the surface about 2, and after 12
hours the initial product transform to CSH I with C:S equal 1.1-1.2 then form the
stable C-S-H II form with C:S equal 1.65-1.8 at 25 °C.
 Hydration of C2S - takes more than 4 years.
02
The full hydration of C2S can be expressed approximately by the following

equation:
2(2CaO.SiO2) + 4H2O → 3CaO.2SiO2.3H2O + Ca(OH)2
2 C2S + 4H •→ C3S2H3 + Ca(OH)2
(100) (21) (99) (22)
The rates of hydration of the two compounds are different as shown in the Figure
(1.6).
Fig (1.6) Typical development of hydration of pure compounds
02
Main characteristics of the major compounds of Portland

cement
Property C3 S C2S C3A C4AF

Rate of reaction Fast Slow Fastest Fast
Heat liberated per unit
Much Little Most More
compound
At early age strength Good Poor Good Poor
At later age strength Good Good Poor Poor
02

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Concrete Technology (I) Lecture 3

Loss on Ignition (L.O.I)

Insoluble residue (I.R)

3CaO.SiO2 + H2O → Ca(OH)2 + xCaO.ySiO2 (calcium silicate hydrate)

The main hydrates of the hydration process are:

This is due to:

The progress of hydration of cement can be determined by different means:

 The heat evolved by hydration.

Tricalcium aluminate (C3A) hydrate and the action of gypsum:

But eventually tricalcium aluminate hydrate is formed, although this is preceded by

Calcium aluminate hydrate – Be at many forms before transforming to the stable

The transformation of calcium aluminates hydrate from the metastable

1- Lose the adhesion and cohesion in the microstructure,

The presence of C3A in cement is undesirable

But it is useful in the cement industry

C4AF compound: Gypsum reacts with C4AF to form calcium sulfoaluminate

Using the optimum percentage of gypsum is very important , because:

The necessary gypsum content increase with the increase of:

 Iraqi specification No. 5 limits the maximum gypsum content (expressed as

Calcium silicates hydrate:

Calcium silicate hydrate gel (C3S2H3) - tobermorite.

The product of hydration is called is called Tobermorite (CSH) and C3S

 Hydration of C2S - takes more than 4 years.

The full hydration of C2S can be expressed approximately by the following

Fig (1.6) Typical development of hydration of pure compounds

Main characteristics of the major compounds of Portland

Property C3 S C2S C3A C4AF

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