CHEMICAL ANALYSIS AND PERCENT CEMENT

1Cristhofer Mejía – 20161150068

1Camilo Cano – 20152150910
2Alvaro Jiménez
1: Students
2: Instructor

ABSTRACT:

In the course of the following practices there is a sample of cement from 4 known brands in
Colombia [Argos, Holcim, CEMEX, Tequendama] with which the respective cations were separated
[SI, Ca, Al, Mg, Fe] by methods of mixing, precipitation and calcination in order to obtain also the
percentages that are in the sample and thus to be able to determine which brand of cement is the
sample problem.

KEYWORDS: Cations identification, precipitates, ions and solutions, cement.

1. THEORICAL FRAME:

Portland cement is obtained from the resistance to compression. Normally the

crushing, milling, dosing, calcining and
sintering of homogeneous mixtures of
limestone and clay, which produce a
material known as Clinker, consisting of
silicates and anhydrous calcium aluminates,
which is mixed and grinds with gypsum.
plastic mass is made by mixing the cement
with water and the hardening is produced by
chemical reaction of the components of the
cement with the water (hydrolysis) and by
the absorption of water forming the products
of hydration.

Portland cement is a hydraulic binder that MAIN COMPONENTS OF CEMENT:

has the property of setting and hardening in
the presence of water, experiencing a
chemical reaction due to hydration, which is
why they are called hydraulic cements.
When the cement is dosed and properly
mixed with water and aggregates, a mortar
or concrete is produced, which retains its
workability for a while achieving good
strength and long-term volume stability.
The above definition includes a large
number of materials different from each
other, which have in common their
adhesiveness. This way you have inorganic
and organic cements.
The most important inorganic cements are
those natural or artificial products, whose
main constituents are calcium compounds,
which have the property that when mixed
with water, they form plastic masses that, as
time passes, they harden and increase
The chemical composition of the raw
materials used in the manufacture of
Portland cement are calcium oxide (CaO)
supplied by lime, Silicon dioxide (SiO2)
found in the clay together with aluminum
oxide (Al2O3) and Iron oxide (Fe2O3), and
the addition of the setting regulator which is
sulfur trioxide (SO3) containing gypsum.
In the sintering stage during the
manufacture of the clinker, the main or
potential components that constitute 95% of
the clinker are produced and are called by
the mineral name, due to impurities of the
raw materials in such a way that the
tricalcium silicate is known as Alita (C3S),
the dicalcium silicate is called Belita (C2S),
the ferrite tetracalcium aluminate (C4AF) is
ferrite and celite to the tricalcium aluminate
(C3A). These compounds exhibit properties
which have an effect on the cement of which
they form part as set out below.
Tricalcium silicate or alite (𝑪𝟑𝑺): Its
chemical composition is the combination of
two oxides 3CaO.SiO2, this constituent of
Portland cement controls the initial
resistance and hardening, due to this has a
moderate heat of hydration of 120 cal / g.
the compound that releases the most CaO.
The hydration of this compound develops at
a rate of 2cal / gr / hr. The hydration of C3S
when it is low produces a calcium silicate of
low basicity and has as final product
C3S2H3 (gel of tobermorita). In performing
the hydration process with a limited amount
of water, the C3S undergoes hydrolysis and
consequently causes the initial release of
the calcium hydroxide into a mixture to
influence the outer layer approximately 0.01
μm thick of the calcium silicate hydrate.
In addition, a cement containing more than
60% C3S will have a very fast hardening
with high initial resistance that will allow,
under equal conditions, a faster stripping in
the work.
Dicalcium or biolytic silicate (𝑪𝟐𝑺): The
composition of the oxide is 2CaOSiO2, this
compound releases under heat of hydration
60 calgr /, with an intrinsic reaction rate of
1cal / gr / hr being slow its hydration and
hardening, reason why the increase in the
resistance is acquired after the first week
approximately.
The belite is known to have three or perhaps
four crystalline forms: α-C2S, occurs at high
temperatures, and is inverted into β-form at
a temperature of 1450˚C, this form
undergoes a γ-C2S transformation at less
than 650˚C, since this is the most stable, [β -
γ] in this transformation there is an increase
of approximately 10% in volume, which is
the cause of clinker disintegration, however,
this change can be avoided, stabilizing β
belite by including other ions within its
network and with a rapid cooling.
Tricalcium aluminate or celite (𝐂𝟑𝐀): This
interstitial material is often in the form of flat
sheets and its composition of the oxide is
3CaOAl2O3. The reaction of pure 𝐶3 con
with water is very violent and leads to an
immediate hardening of the paste,
accompanied by a high heat of 207 calgr / m
with an average rate of heat release of 3 cal
/ gr / hr.
To retard the setting of C3A, the amount of
gypsum required to be added to the clinker
is used in a maximum amount of 2.5% when
the content of 𝐶3𝐴 is less than 5% and 3%
when the content of 𝐶3𝐴 exceeds 5%. Also
an increase in fineness raises the amount of
gypsum required to provide a suitable
retarding effect, since in thinner cements
there is freer C3A for early hydration.
The C3A facilitates the combination of lime
and silica; due to this it is of vital importance
in the manufacture of cement.
In short, the C3A reacts very quickly with
water, generates a lot of heat, heals quickly
and contributes little to the initial resistance.
A high content of C3A in the clinker results
in pastes, mortars and concretes of low
resistance to attack by sulfates and other
aggressive agents.
Ferrite aluminate tetracalcium or ferrite
(𝐂𝟒𝐀𝐅): It is 5 - 15% in the cement, the
composition of the oxide is
4CaOFe2O3Al2O3, and this compound acts
as a flux and in this way reduces the firing
temperature of the clinker. The higher C4AF
in cement makes it more vulnerable to
chemical attack by sulfates (Aguilar
Mundaca, 2007). The C4AF is characterized
by a slow hydration rate, with moderate heat
of hydration (100 cal / gr), the average
speed of detachment being 1 calgrhr /, and it
contributes little to early resistance and to
advanced ages.
OTHER CHARACTERISTICS AND
TERMINOLOGIES OF CEMENT:
Autoclave: Equipment consisting of a
chamber in which the delayed potential
expansion, caused by the hydration of CaO,
or of MgO, or both, is measured.
Hydration Heat: The amount of heat,
expressed in calories per gram of hydrated
cement, after complete hydration at a given
temperature.
Cement: It is a pulverized material which in
addition to calcium oxide contains silica
alumina and iron oxide and which, by
addition of an appropriate amount of water,
forms a paste which is capable of hardening
both water and air. Hydraulic limes, air
lances and plasters are excluded.
Portland cement: Product obtained from
the spraying of Clinker Portland with the
addition of calcium sulphate. The addition of
other products is allowed provided that their
inclusion does not affect the properties of
the resulting cement. All added products
should be sprayed together with the Clinker.
Clinker Portland: It is a granular material,
consisting mainly of silicates, aluminates
and Ferro aluminates of calcium, obtained
by the cooking, until partial fusion
(clinkerizacion), of a suitable mixture
proportioned and homogenized of limestone
and clay properly selected.
Normal Consistency: It is the amount of
water that is added to the cement to achieve
certain fluidity.
Density of the hydraulic cement: It is the
mass of the unit volume of the solids.
Volume Stability: All cements have small
contraction and dilation deformations
according to the thermo-hygrometric
equilibrium in the construction zone;
predictable and controllable deformations.
These disturbances can be attributed to an
excess of the following compounds: Free
lime (Ca0), free Magnesia MgO especially
crystallized, Gypsum (SO4Ca2H2O).
Fineness: It is the size of the particles that
constitute a mass of cement.
It is the change of the plastic state to the
solid state of a cement paste and this is due
to the hydrolysis reactions that lead to the
setting and hardening.
Le Chatelier flask: It is a glass container of
defined shape in the standard NTC 221 that
has as main objective to determine the
density of the cement.
Permeabilimetre de Blaine: An apparatus
whose function is to determine the fineness
of the cement with the air permeability test,
through a cement layer of porosity already
defined. The pore is directly related to the
size of the particles and determines the
velocity of air flow through the layer. The
parts of the apparatus are: manometer,
permeability chamber, metal disk, filter
paper, etc.
Hydraulic property: The ability of a
pulverized material to set in the presence of
water to form stable compounds.
Pozzolanic property: Aptitude of a
pulverized material to react chemically with
the calcium hydroxide and in the presence
of water at room temperature, to form
hydraulic compounds.
Puzolana: Material that can be natural
(diatomaceous earth, opal rocks, schists,
volcanic ash, pumitas), or artificial that
contains silica and alumina with Pozzolanic
properties.
Mechanical strength of cement: It is the
ability of cement to withstand compressive
stresses.
2. METHODOLOGY:
The following diagrams show the procedure:
For the SiO2:
For this one we added HCl to the sample,
later we shake them to remove the lumps,
we heat the solution for six minutes, later we
added 7 ml of the jelly solution and 100 ml of
H2O and we filter that solution, the
precipitate was calcined for 45 minutes and
we make the calculations for this cation:
𝑃2 − 𝑃1
%𝑆𝑖𝑂2 =
𝑃
For the Fe2O3:
100 ml of solution is taken. They are
transferred to a glass of 250 ml capacity.
The mixture is heated to boiling and a
solution of stannous chloride is added to
reduce iron at ferrous state, stirring until
complete discoloration of the liquid. An
excess drop is added.
The solution is cooled as quickly as possible
and 10 ml of saturated, cold solution of
mercuric chloride. Shaken vigorously for 1
minute and 15 ml of the phosphorous-
sulfuric mixture is added. Five indicator
drops are added.
The liquid is titrated with potassium
dichromate standard solution until the
indicator turns, later we make the
calculations for this cation:
0,004 (𝑉1 − 0,05)
%𝐹𝑒2𝑂3 =
𝑃 We are taken 10 ml of solution with a
For the Al2O3:
We are taken with a
Pipette 50 ml of solution and pass to a 250
ml beaker.
Add a 0.01 M standard solution volume of
Complexone III, well known and measured
with burette. This volume may be 20 ml.
Next, we add 25 milliliters of the buffer
solution of pH 4.5. Boil the liquid for 5
minutes and is cooled with water as quickly
as possible. Once the solution dissolves,
add 80 ml of 96 ° ethanol, completely
recoiled and a small portion of the indicator
is added.
The liquid is titrated with standard solution of
Zn2 + 0.01 M until the green indicator turns
To red. The indicator will consume, in the
exposed working conditions, 0, 1 ml of
Standard solution of Zn 2 + 0.01 M.
We make the calculations for this ion:
%𝐴𝑙2𝑂3
𝑉2 − 𝑉3 − 𝑉1 + 0,05
= 0,637
𝑃
For the CaO:
We are taken 20 ml of solution with a
pipette. They are passed down to a
glass, of 250 mi of capacity. S ml of 4N
sodium hydroxide solution and 80 ml of
Water. Shake vigorously. 0.10 g
indicator is added. The liquid is titrated
with standard solution of 0.01 M
Complexone 111 until indicator turn
from yellowish green to persistent pink.
The calculations for this cations are:
𝑉4
%𝐶𝑎𝑂 = 1,7525
𝑃
For the MgO:
pipette. They are passed down to a
glass, of 250 ml capacity. 25 ml of
buffer solution of pH 10 are added and
80 ml of Water. Next, no more than two
drops of indicator Methyl red and one
pe burn off the indicator portion Black
until the solution takes a color Red
wine. The liquid is titrated with standard
solution of 0.01 M Complexone III, for
which give first about 13 ml of it. A new
indicator portion is then added, if
necessary, until the dissolution re-takes
the red wine former color. Continue to
value until the indicator turns from red
to green. (The Turn of the Negro of
eriochrome T is red to light blue, but in
the presence of methyl red, which at pH
10 is yellow, the final key is green.)
The calculations are:
𝑉5 − 𝑉4/2
%𝑀𝑔𝑂 = 2,52
𝑃
3. REACTIVES AND MATERIALS: but this changes do not affect the results of
the practice.
The reactive and material used in this For the Si4+:
practice are:
15, 25 − 15, 14
%𝑆𝑖𝑂2 = 𝑥 100%
REACTIVE MATERIAL 0,5
SnCl2 Beaker 50ml = 22%
HgCl2 Beaker 250ml %𝑆𝑖𝑂2 = 22%
H2SO4 Heating Plate
H3PO4 Glass Stirrer For the Fe3+:
MnSO4 Pasteur Pipette
KMnO4 Clock Glass
HCl Measured 0,004 (6 − 0,05)
Balloon %𝐹𝑒2𝑂 = 100 % ( )
2
ZR Reagent Spatula 5
Methyl Red Burette = 5, 95%
NaOH Universal %𝐹𝑒2𝑂3 = 5,95% ≈ 6%
Support For the Al3+:
Erlenmeyer 100
ml
%𝐴𝑙2𝑂3
4. DATA CHART: (0,4 − 0,31) − 0,1 + 0,05)
= 100% (0,637 )
0,5
ION PERCENTAGE = 5,096%
Si4+ 22% %𝐴𝑙2𝑂3 = 5,096%
Fe3`+ 6% For the Ca2+:
Al3+ 5,096%
Ca2+ 4,55% 5,608 · 10−4 · 1,3
Mg2+ 0,945% %𝐶𝑎𝑂 = 100
1
31,25𝑃
The sample belongs to CEMENTOS 1,3
= (1,7525 )
TEQUENDAMA S.A 0,5
5. RESULTS ANALYSIS: = 4,55%
%𝐶𝑎𝑂 = 4,55%
CALCULATIONS: For the Mg2+:

We are used the methods and determinate 0,075

0,05 −
the cations in the problem sample here we %𝑀𝑔𝑂 = 100 (2,52 2 )
have the calculations for each one cation in 0,5
this sample, we used some valuations and = 0,945
calcinations for the determination of certainly %𝑀𝑔𝑂 = 0,945%
cations for example the Silicon (Calcination)
and Iron, Aluminum, Calcium and The results are close to the percentages of
Magnesium (Valuation), some reactive are CEMENTOS TEQUENDAMA S.A.
changed as the Complexone III we change
that for EDTA and the calceine for murexide,
6. CONCLUSIONS:

 It is inferred after the practices that the

cement in analytical questions has its
degree of difficulty to obtain the
percentages taking into account the
interferences by the handling of the
marches of the cations and the obtained
precipitates, and although it is only a
qualitative experience, there are
variations in the procedures that do not
contribute the desired results and
possibly without knowing some
standards with which they make the
cement makes difficult the possible
determination of mark of the sample
problem
 Other alternatives for the determination
of the percentages of some of the
components of the cement that would
have been of great help in the practice
is the spectrophotometry or atomic
absorption that in the case of what
would be the Faith and the Ca would
give a greater success in the respective
percentages of these.
 For last conclusion the cement belongs
to CEMENTOS TEQUENDAMA S.A
.