CHEMICAL INDUSTRY CORPORATION

MUGHER CEMENT FACTORY

Training on Quality Control and Quality

Assurance in Cement Production

By: Endeshaw Mogninet (BSc: Chemistry

& Masters: Business Administration)

November 2024
 1. Introduction
1.1 What is cement?
 Cement is a finely ground, non-metallic, inorganic powder
when mixed with water forms a paste that sets and
hardens.
 This hydraulic hardening is primarily due to the formation
of calcium silicate hydrates as a result of the reaction
between mixing water and the constituents of the cement.
 It means when a finely ground inorganic material like
cement, is mixed with water it forms a paste which sets
and hardens by means of hydration reactions and which,
after hardening and setting, retains its strength and
stability even under water.
… Cont’d

 Setting and hardening of cement are not due

to a drying process but due to a hydration
process.
 Cement is seldom used on its own, but rather
to bind sand and gravel together.
 Cement mixed with fine aggregate produces
mortar for masonry, or with sand and gravel,
produces concrete.
… Cont’d

1.2 Types of cement

1. Ordinary Portland Cements (OPC):
 It is the basic Portland cements and manufactured in
large quantities than all other cements;
 It is presently available in three different grades viz. C33,
C43 and C53;
 The numbers 33, 43 and 53 correspond to the 28 days
compressive strength of cement as obtain from standard
tests on cement -sand mortar specimens;
 It is used in general concrete construction.
… Cont’d

2. Rapid Hardening Cements (RHC):

 It is finer than ordinary Portland cements;
 It contains more C3S and less C2S than OPC;
 The one day strength of this is equal to the 3 days
strength of OPC with the same water cement ratio;
 The main advantage of rapid hardening cement is that
shuttering may be removed much earlier, thus saving
considerable time and expenses;
 RHC is also used for road work where it is imperative to
open the road traffic with the minimum delay.
… Cont’d

3. Extra Rapid Hardening Cements (ERHC):

 It is obtained by mixing calcium chloride with RHC;
 Addition of CaCl2 imparts quick setting properties in
extra RHC;
 The acceleration of setting, hardening and evolution of
heat in the early period of hydration makes this cement
very suitable for concreting in cold weathers;
 The 1 or 2 days strength of extra RHC is 25% more than
that of RHC;
 The gain of strength disappears with age and 90 days
strength of extra RHC and RHC are nearly the same.
… Cont’d

4. Low Heat Portland Cements:

 It is a Portland cement which obtained by reducing the more
rapidly hydrating compounds, C3S and C3A and
increasing C2S;
 Since, the rate of gain of strength of this cement is slow, hence
adequate precaution should be taken in this use such as with
regard to removal of formwork;
 LHC is used in massive construction works like abutments,
retaining walls, dams, etc. where the rate at which the heat
can be lost at the surface is lower than at which the heat is
initially generated;
 It has low rate of gain of strength, but the ultimate is
practically the same as that of OPC.
… Cont’d

5. Portland Slag Cements (PSC):

 PSC is made by inter-grinding Portland cements clinker and
granulated blast furnace slag;
 The proportion of the slag being not less than 25 % or more
than 65 % by weight of cement;
 In general blast furnace slag cement finds to gain strength more
slowly than the ordinary Portland cement;
 The heat of hydration of Portland blast furnace slag cements is
lower than that of OPC. So, this cement can be used for mass
concreting but is unsuitable for cold weather;

 It has fairly high sulphate resistance, rendering it suitable for use

in environments exposed to sulphates
… Cont’d
6. Portland Pozzolana Cements (PPC):
 It is produced by grinding together Portland cement
clinker and pozzolana with the addition of gypsum;
 PPC produces less heat of hydration and offers great
resistance to the attack of impurities in water than OPC;
 The disadvantage of using PPC is that the reduction in
alkalinity reduces the resistance to corrosion of steel
reinforcement;
 It evolves less heat and its initial strength is less but
final strength is equal to OPC;
 It has lower rate of development of strength than OPC.
… Cont’d

7. Sulphate Resisting Cements (SRC):

 The Portland with low C3A and C4AF and ground
finer than OPC is known as sulphate resisting
cements;
 It is used in marine structures, sewage treatment
works, and in foundations and basements where soil
is infesting with sulphates;
 However, recent research indicates that the use of
sulphate resisting cement is not beneficial in
environments where chlorides are present.
… Cont’d

8. White Portland Cements:

 The process of manufacturing white cement is the
same but the amount of iron oxide which is
responsible for grayish colour is limited to less than 1
%;
 Sodium Alumino Ferrite added to act as flux in the
absence of iron oxide;
 The properties of white cement are nearly same
as OPC;
 Grey colour of OPC is due to the presence of iron
oxide. Hence in white cement, Fe2O3 is limited to 1 %.
… Cont’d

9. Coloured Portland Cements:

 It is a type of mixture of white cements along

with the desired colour and color determines
its original presence.

 The cost of this cement is higher than OPC.

… Cont’d

10. Hydrophobic Cements:

 It is obtained by inter-grinding OPC with 0.1 –
0.4 % of water repellant film -forming substance
such as oleic acid or stearic acid;

 The properties of hydrophobic cements are

nearly the same as that of OPC;

 The cost of this cement is higher than OPC.

… Cont’d

11. High alumina Cements (HAC):

 It is very different in composition from Portland cements;
 It is characterized by its dark colour, high early strength,
high heat of hydration and resistance to chemical attack;
 The raw material used for its manufacture consists of
limestone and bauxite which is a special clay with high
alumina content;
 High alumina cement is very expensive to manufacture.
 It is used where early removal of the framework is
required;
 Its rapid hardening properties arise from the presence of
calcium aluminate.
… Cont’d

12. Super Sulphated Cements (SSC):

• It is obtained from well granulated blast furnace
slag, calcium sulphate and OPC;
• It is ground finer than OPC;
• It has low heat of hydration;
• It is used for construction of dams and other mass
concreting works;
• It has high resistance to chemical attack.
… Cont’d

13. Special cement:

 It has some specific functions such as altering the

setting or hardening behavior of a concrete.

 The 5 classes of common cement defined by EN

197-1 are then dependent on the other
constituents of the cement, besides Portland
cement clinker and gypsum for regulation of
setting time and summarized below:
… Cont’d
… Cont’d

• Type I: Normal (OPC Ordinary Portland cement) Comprising Portland

cement and up to 5% of minor additional constituents: Portland cement

• Type II: Moderate heat/moderate sulphate resistance. Portland cement

and up to 35% of other single constituents: Portland-composite cement
• Type III: High early strength Portland cement and higher percentages of
blast furnace slag: Blast furnace cement

• Type IV: Low heat of hydration Portland cement and up to 55% of

pozzolanic constituents (volcanic ashes): Pozzolanic cement

• Type V: High sulphate resistance Portland cement, blast furnace slag or

fly ash and pozzolana: Composite cement
… Cont’d

Requirements on the compressive strength after 2 days and 7 days:

A 32.5N cement should attain a compressive strength of ≥16 MPa at 7 days,

A 32.5R cement should attain a compressive strength of ≥10 MPa at 2 days,
A 42.5N cement should attain a compressive strength of ≥10 MPa at 2 days,
A 42.5R cement should attain a compressive strength of ≥20 MPa at 2 days,
A 52.5N cement should attain a compressive strength of ≥20 MPa at 2 days,
A 52.5R cement should attain a compressive strength of ≥30 MPa at 2 days.
… Cont’d

1.3 Cement raw materials

 Cement raw materials composed mainly of CaO,
Sio2, Al2O3, Fe2O3 with little MgO;
 Can be those used in the calcinations of the cement
clinker and those fed to the finishing mill along with
the clinker at time of grinding;
 Those used for calcinations are lime components
which are rich with CaCO3 called calcareous
components and Argillaceous compounds which are
rich with silica, Alumina and ferric Oxide;
… Cont’d

 Examples of calcareous components: limestone,

Chalk, marl;
 Examples of Argillaceous components: Shale, Clay;
 Clays are elastic elements, i.e. they consist mainly of
the remains of pre-existing rocks which have been
broken down by weathering and/or erosions of alkali
& alkaline earth containing aluminous silicate and of
their products mainly feldspar & mica;
 Kaolinite is the most desirable clay mineral for
cement because of it is naturally finely divided &
easy to burn.
… Cont’d

 The raw materials for the manufacturing of

cement can be grouped in to three broad
categories. These are:
the major (basic),
the corrective constituent, and
 additives & admixtures.
… Cont’d

1.3.1 The major (basic) raw materials:

 CaCO3 rich calcareous rocks like limestone, chalk
& marl;
 Argillaceous rock like clay & shale which supply
the balance of silica, iron & alumina;
 The raw mix for making of Portland cement
clinker is generally obtained by blending a
calcareous material typically limestone, with a
smaller amount of argillaceous one, typically clay
or shale.
… Cont’d

1.3.2 Corrective raw materials

 Are materials with high content of specific oxides;

 Used before raw mill to balance chemical composition of
raw mix;
• The correction of iron oxide in raw mix done with iron ore;
• The correction of Alumina oxide in raw mix done with
Bauxites;
• The correction of Silicon oxide in raw mix done with
Sandstone or quartz;
• Pure limestone to bear CaO.
… Cont’d

1.3.3 Additive and admixtures

 Additives: are constituents which are typically added to
improve the manufacturing or the properties of cement. These
are added to clinker of OPC to reach the desired physical
character of cement.
 Example: Gypsum is added to cement mainly for the purpose of
regulating its setting time.
 Admixtures: are constituents which are added to Portland
cement clinker and gypsum to produce blended
(composite) cements.
 Example: Pumice is Pozzonlanic material left from the
Volcano consists essentially reactive amorphous SiO2& Al2O3
which is used for the production of PPC.
… Cont’d

 Fillers: Due to the higher consumption of non-

renewable resources & energy for the production of
OPC, concerned bodies around the world tried to
found out some cement additives which do not
significantly alter the physical and chemical
properties of OPC.
 MCF tried to check the physical & chemical
parameters for % of CLS as an additive (filler) to
normal OPC and proceed to mass production of 5%
addition.
… Cont’d

The addition of CLS (5% by weight) as a filler in

OPC clinker results:
 relative increase in cement fineness;
 Comparative marginal decrease in water
requirement due to filling of void spaces;
 Saving in grinding time;
 Improvement in cement performance such as
workability, increase in early strength, denser
micro structure & energy saving.
2. Cement manufacturing process
 Cement production involves processes like:
• Raw material preparation,
• Pyro processing,
• Finish grinding and packaging.

 The above processes can be presented in the

following process flow block diagram:
… Cont’d
… Cont’d

2.1 Raw material preparation

 Raw material preparation involves the following
operations:

• Mining & quarrying,

• Pre-homogenization/blending,
• Crushing,
• Raw milling.
… Cont’d

 Mining: is the process of extracting buried

material below the earth surface.
Quarrying: refers to extracting materials directly
from the surface.
 Mining operations:
• Core drilling (bore) holes to explore the mines;
• Blasting;
• Excavation and haulage;
• Transportation to crusher;
• Size reduction for process requirements
… Cont’d

Homogenization samplings
Core drilling samples to explore the mines quality
pattern:
• To ensure that the required quantity and quality are
met for daily, weekly and year productions for the
plant;
• To minimize the total operation cost for milling;
• To optimize the limestone quality for the raw mills.
… Cont’d

On line analyses of the limestone going to the

limestone stockpile:

• To ensure that the required quality is met

according to the mining plan after blasting and
crushing.
… Cont’d

What is quarry blast?

• Blasting is the breaking of rock masses using
explosives to obtain the fragments and
separate rock materials for further processing.
• It is the primary stage of rock size reduction
after drilling and it is followed by crushing and
grinding actions.
• The main objective of blasting action in the
mine is to produce a fragmented rock with
sizable and cost-effective way.
… Cont’d

Crushing
 Crushing is the process of size reduction.
 Crushers are chosen depending upon the material
characteristics such as hardness, abrasiveness, feed input size,
moisture content etc.
 The commonly used crushers are:
• hammer crushers,
• impact crushers,
• roll crushers,
• gyratory crushers,
• jaw crushers.
 Size reduction depends upon the grinding system to be adopted
i.e.., ball mill or vertical mill.
… Cont’d

Limestone stockpile stacking and storage

 Blending: is the function integration of a number
of raw materials with different chemical and/or
physical characteristics in such proportion that a
completed pile represents the requisite
composition.

 Homogenization: defined as the function of a

systematic transformation of the input flow of the
pile into the output flow, so that the fluctuations
of a property in the flow are evened out.
… Cont’d

• The quarry fluctuations are smoothed early in the raw

meal preparation process, namely at the pre-blending
beds.
• Stacking/blending of raw materials in preparation for raw
grinding process is pre-homogenization.
• Storage is the final opportunity for raw material feed
uniformity.
• Product from crushing operation is stacked & later
reclaimed specifically to improve material uniformity.
• The stockpile material normally has a maximum particle
size of up to 25mm in the case of cement production, to
reduce the effect of segregation.
Circular storage
Linear storage
… Cont’d

Raw milling
What is the function of Raw Milling?
• The function of raw milling is to produce sufficient quantities,
a raw meal of optimum fineness and consistent composition
for good burnability in the kiln.
• Maximum fineness would give easiest burning (lowest fuel
cost) but grinding costs would be prohibitive.
• Since raw materials vary chemically, the feed rate of various
components also changes and overall grindability also
changes.
• Coarse particles affect clinker quality the most - these are
controlled by keeping the 90μm residue of the raw meal
typically between 10 and 15%.
… Cont’d
 Mill types can be:
 VRM (Vertical Roller Mills):
• Energy consumption is less compared to ball
mills;
• Flexibility in operation as all forces can be
controlled;
• Drying capacity is better than ball mills;
• Noise level (noise pollution) is much less than
ball mills;
• Particle size distribution better than ball mills.
… Cont’d

 Ball mills:
• Cost of installation is relatively low;
• Replacement of grinding media and liners is
relatively cheap;
• Not sensitive to the entry of trap metal;
• Can be operated in either open or closed
circuit;
• Long periods between maintenance work;
• Non-specialised maintenance staff required.
… Cont’d

Raw mix control during raw milling

 Raw mix preparation is the quality key control

parameter for stable, continuous manufacture
of high quality clinker and cement.
… Cont’d
Objectives of raw mix control:
• To produce clinker with uniform and predicted quality;
• To have smooth kiln operation;
• Stable coating in the kiln with stable raw meal feed to
the kiln;
• Formation of favorable clinker phases grown from raw
meal with consistent properties;
• A kiln feed that permits effective energy conserving
production of a quality Portland cement clinker;
• To improve pozzolana addition in cement grinding;
• To reduce production cost.
… Cont’d

The raw mix chemical composition corresponds to the

quality requirements expressed either by the specific:
 Lime saturation factor (LSF),
 Silica module (SM) and
 Alumina module (AM), or
 By the potential clinker phases: C2S, C3S, C4AF, C3A.
 Both groups of magnitudes can be derived from the
main raw mix oxides CaO, SiO2, AI2O3 and Fe2O3.
 Well controlled raw mix during raw milling results
consistent clinker mineral composition resulted from
pyro processing.
… Cont’d

Cement clinker mineral composition

Cement clinker is composed of calcium
silicates, calcium aluminates and calcium
alumino-ferrites.

Tricalcium silicate Ca3SiO5 C3 S Alite

Dicalcium silicate Ca2SiO4 C 2S Belite

Tricalcium aluminate Ca3Al2O6 C 3A Celite

Tetracalcium alumino-ferrite Ca4Al2Fe2O10 C4AF Felite

… Cont’d
 The raw meal can be controlled by the following oxide
ratios:

Silica ratio (SM):

 The amount of total silicates in the cement is controlled
by cement chemists via the silica ratio.
 This is one of the most important ratios used as a target
and control in cement manufacturing.
 It is also commonly referred to as the “silica modulus”
(SM).
 Silica Ratio = %SiO2/ (%Al2O3 + %Fe2O3)
 Silica ratio (or modulus) is typically 2.50.
… Cont’d

Lime saturation Factor (LSF):

 Used to calculate the maximum combinable lime
 If LSF is greater than 100%, then all the lime cannot
be combined and some residual free lime will be
present in the clinker after burning in the cement
kiln.
 This effectively defines the maximum C3S content
which can be achieved in clinker and cement, and
therefore the maximum strength potential.
 Lime saturation is greater than 90% in commercial
Portland cement clinkers, and typically ~95%.
… Cont’d
… Cont’d

Alumina ratio (AM):

 The alumina ratio or alumina modulus (AM)
is the ratio of the Al2O3 to the Fe2O3 content
in cement raw mix, clinker or the cement
itself.
 0.64 is the minimum alumina ratio for
production of Portland cements, as below
that value there will be insufficient Al2O3
available to combine with the Fe2O3 in C4AF.
… Cont’d

 Below that alumina ratio (0.64), there would

be free FeO3 present in the cement.

 Alumina ratio= %Al2O3/% Fe2O3

 Alumina ratio (or modulus) can vary from

0.70 in sulphate resisting cements to >10.0 in
white cements, but is typically ~1.5 in ordinary
cements.
… Cont’d

 The major oxides CaO, SiO2, Al2O3 and

Fe2O3 will typically make up 98% of the
composition of Portland cement clinker.
… Cont’d

Burnability:
 Burnability is the relative ease or difficulty with
which feed is changed into clinker.
 It can be related to the time that it takes to
produce C3S, it is the time taken to fully combine
C2S + C to produce C3S.
 The burnability decreases with increasing LSF,
and increasing silica ratio (SR). Increase in LSF
implies more CaO that has to react and increase
SR implies less liquid at a given temperature.
… Cont’d

 The burnability also depends on the

mineralogical composition of the raw
materials.
 Silica present as quartz is less reactive than
that present in clay minerals and a limestone
with high silicate minerals content is likely to
be more reactive than nearly pure calcite.
 Minor components such as MgO or fluxes can
reduce the melting temperature then have a
positive influence on burnability.
… Cont’d

The impact of liquid phase:

Higher liquid phase Easier to burn

Too high liquid phase:
 The clinker porosity decrease;
 Grindability decreases (harder);
 1-day strengths reduces.
Too low liquid phase:
• The C3S formation speed decreases;
• The clinker nodule size reduces.
… Cont’d

Burnability factor (BF):

 Considers the components of lime, alumina,
silica, iron, magnesia, and alkalis, which all
directly influence burnability.
 BF = 100 X LSF + 10 X SR -3 (MgO + Alkalis)
 Higher BF Harder to burn
 BF is typically: 110-115
… Cont’d

Burnability vs LSF:
 Too high LSF is:
• Hard to burn which will lead to high fuel consumption
thus more Sulphur entry;
• Tend to have high free lime and C3S values in clinker which
will result in high early strength.

 Too low LSF is:

• Easy to burn;
• Tend to have low free limes, low C3S and high C2S values in
the clinker which will result in reduced cement strength.
… Cont’d
Burnability vs SM:
 The SR target is between 2.2 and 3.2%. For values
less than 2.2% the raw mix is very easy to burn and
the value of the C3S and the C2S compared to the
fluxes becomes very low and the cement strength
will decrease.

 The Silica ratio is the main indicator of the

burnability of the raw mix.
 The standard deviation should not be higher than
0.05
… Cont’d

Too high SM:

 Weakens the burnability of the clinker that
results in hard burning;
 Reduces liquid phase content;
 Causes thermal load in the kiln;
 It creates no coating or strip/remove the
coating;
 Kiln stays dusty and unstable;
 Creates a high free lime;
 Causes a slow setting and hardening of cement.
… Cont’d

Too low SM:

• Increases liquid phase content;
• Improves burnability of clinker;
• A tendency of brick infiltration;
• Create hard clinker and sometimes create
large clinker balls;
• Improves formation of coating in the kiln;
… Cont’d

Burnability vs AM:
 When AR ≤ 0.638, both oxides present in their
molecular ratios, therefore only C4AF can be formed
in the clinker and there will be no C3A in the clinker;
 C3A is typically 8-12% in the clinker anything less
that this will influence the early or initial strength of
the cement;
 The more iron the darker the cement;
 This ratio has a more important impact on the
coating formation in the kiln.
… Cont’d

Too high AM:

• Weakens the burnability of the clinker that results in
hard burning
• Reduces liquid phase content
• Increase the C3A and reduces the C4AF contents

Too low AM:

• Leads to easier burning, i.e. less fuel consumption;
• Makes the clinker sticky and tends to create large
clinker balls if there is no free silica.
The effect of SM and AM on coating
… Cont’d
Burnability vs fineness:
 The burnability is proportional to the raw mix fineness;
 The finer the material the easier it is for the reaction to occur;
thus less fuel is required for the reactions.

 With large particles, there is fewer spots. This means there is

less heat exchange between the particles thus less
combination of particles;
 With smaller particles, there is more connection spots.

 By increasing the number of contact areas for heat exchange,

a lower burning zone temperature is needed for the same
reaction.
Causes for poor raw mix uniformity
… Cont’d
2.2 Pyro processing
Pyro processing is:
• an important stage in cement manufacturing process;
• materials are subjected to high temperatures so as to cause
a chemical or physical changes;
• Its control improves efficiency in energy utilization and
hence enhances production for good quality assurance;
• is a thermal processing unit;
• Steadily increasing temperatures from 100/8500C to 14500C;
• Raw feed transitions through distinct zones in the whole
system;
• For the creation of a new artificial mineral called……Clinker
Raw material transformations in pyro processing
… Cont’d
… Cont’d

Major components in pyro processing:

 Pre heater and cyclones,
 Pre calciner,
 Kiln,
Cooler
… Cont’d

Major minerals of clinker resulted from

pyro processing:
C3S/ Alite:
 Typically, 55 to 65% C3S of clinker;
 Main strength constituent in cement;
 High initial strength and good final strength;
 Rapid hydration;
… Cont’d

C2S/ Belite:
 Typically, 10 to 20% of clinker;
 Low early strength but good final strength: +1
% C2S = up to + 0.5 MPa (at 28 days);
 Slow hydration;
 Clinker grindability is badly impacted by higher
C2S.
… Cont’d

C3A/ Aluminates:
• Rapid hydration with heat development:
gypsum is added to control hydration rate;
• Early strength (at 1d and before);
• Typically, 8 to 10% of clinker;
• Important effects on concrete quality:
workability- Resistance to sulphates in
soil/water exposure.
… Cont’d

C4AF / Ferro Aluminates:

• No impact on strength;
• Typically, 7 to 11% of clinker;
• Colour of cement: higher C4AF = darker
cement.
… Cont’d

Fuels used in cement production

Types of fuels:
 Solid fuels (coal, pet coke);
 Liquid fuels (furnace oil, Diesel oil);
 Gas fuels (natural gas);
 Alternate fuels (shredded tires, waste wood,
chemical waste, animal meal, rice husk, coffee
husk).
… Cont’d
 Fuel lumps are crushed to suitable size depending on
the grinding system and hard groove index of fuel.
The residue depends on the volatile matter.
 Hardgrave Index:
 The usual method of determining coal grindability;
 50 gram of sample is ground for a specified period in
a laboratory mill under standard conditions and the
product then sieved on a 75 µm sieve. If R is the
percent residue remaining on the sieve, then:

 Hardgrave Index (HGI) = 13 + 3.456 (100 – R)

… Cont’d

Coal fineness:
 To ensure complete combustion of the coal
dust, it must be ground to a fineness which is
dependent on the volatiles content;
 A rule of thumb is that the 90μm residue
should be approximately 0.5 x % volatiles;
 It should be noted that for calciner firing, the
sieve residue of the coal should be finer for
more rapid burnout.
… Cont’d

2.3 Finish grinding and packaging

 The finish grinding of cement can be using:
• Ball mills,
• Vertical Roller Mills (VRM)

 Cement dispatch can be either:

• Packed, or
• Bulk loading
3. Quality Control and Quality Assurance in
Cement Production

3.1 Quality control

 Cement quality is defined in terms of:

 Chemical composition (Oxides content limits);
 Physical properties (Strength, Workability,
setting behaviour etc.) in Standard Norms
(ASTM, ISO) and is measured using standard
method.
… Cont’d

Factors influencing cement quality:

 Chemical & mineralogical composition of raw
mix;
 Chemical & mineralogical composition of
clinker;
 Burning process;
 Chemical composition of fuels;
 Mechanical handling of clinker (grinding).
… Cont’d
Quality control: Monitoring the product quality at
different production stages so that the required
quality level is finally achieved.
 A detailed control plan for quality control of each
raw material, intermediate & final product is setup
by a thorough analysis of the following
questionnaire:
• What should be examined?
• What information is required for the control?
• How often must the test be performed?
• How accurate must the result of the testing be?
… Cont’d

Quality control activities include:

 Sampling the raw materials, clinker & cement
products produced at the factories;

 Checking their conformities with relevant

standards after testing in lab;

Issuing the right to use.

… Cont’d

Sampling:
• Sampling is the process of collecting a
representative & sufficient quantity of
material (sample) to be analysed.
• It is the act, process or technique of selecting
a suitable sample, or is representative part of
a population for the purpose of determining
parameters or characteristics of the whole
population.
… Cont’d
 Cement raw materials and cement products
can be sampled either manually or
automatically or both.
 Stationary materials mostly sampled in the
field either by taking them from the surface or
from the drill holes. Raw materials from their
quarries are sampled in this way. While
conveyed materials are materials that
transported continuously, can be sampled from
the belt conveyor, the air slide or slurry pipe.
… Cont’d
 Lime stone, sand stone, Clay and
Gypsum transported by belt conveyor to
their storage and sampled from belt
conveyor.
 Raw meal, kiln meal & cement meal
sampled from air slide.
… Cont’d

Sampling techniques:

• Three types of Samples:

• Convenience,
• Judgment, and
• Random Sample.
… Cont’d

The methods used for selecting the sample units can

be:
• Quota: samples selected from units arranged in a
block of predetermined size. It is used to select
sample units so as to capture the detailed
behaviour of the process.
• Systematic: samples selected over the extended
period of time. Data designed to select at fixed or
count intervals & samples must be in sequence
and serially numbered.
… Cont’d
 Example: - If there are 48 raw meal samples
per day and if you want to check 8 samples for
total carbonates, the sampling interval will be
6 i.e. for every 6th sample you perform the
test.
K=T/n =48/8 =6
Where, T= total collected samples per day,
n= design to check the process, and
k = sampling interval
… Cont’d
• Probability sampling: refers to the selection
of a sample from a population, when this
selection is based on the principle of
randomization, that is, random selection or
chance.
Probability sampling is more complex, more
time-consuming and usually costs more than
non-probability sampling.
… Cont’d
Probability sampling system also consists of:

 Simple random sampling,

 Stratified random Sampling, and
 Systematic random sampling.
… Cont’d
Sample Preparation:
The general and accepted steps to prepare any sample
includes:
 Crushing,
 Drying in the lab oven,
 Weighing and registering of the received sample,
 Splitting of the sample to obtain smaller representative
samples,
 Fine grinding by grinding mill,
 Sieving,
 Homogenizing,
 Fill to the bottle & labelling.
… Cont’d

Labelling the sample includes:

• Sampling date, place and time;

• Type of sample, method of sampling;
• Possibly sampled by whom and what is
required to be done for it.
… Cont’d

Chemical analysis in cement production

 Chemical analysis in cement production can

be either classical (traditional) especially the
gravimetric & the titrimetric (volumetric)
methods or instrumental. One of them or both
can be engaged to check the quality
parameters.
… Cont’d
 Classical method:
 involves taking samples from different processing
points and analysing them in a central laboratory
manually or in some cases automatically.

 Provide an analyst with an outline (procedure) of

analysis complete with preparation of reagents,
calculations;
 Great attention is required to the human factor and
method in order to minimize the error;
 Examples: wet gravimetric or titrimetric procedure.
… Cont’d
Modern methods/on-line measurement systems:
have the following advantages:

 Higher frequency & more time controls;

 Resulting in energy savings;
 Better & more stable product quality;
 Cheaper and simpler to operate than central automatic laboratory;
 Examples:
 gamma- metrics CBX- on line PGNNA Elemental analyser for raw
materials,
 On-line free lime analyser,
 On-line loss on ignition analyser
 CO2/SO3 analyser to monitor gypsum & limestone additions.
… Cont’d

 The quality control activities in MCF are

performed based on the predetermined
frequencies and methods.
… Cont’d
Tests performed by samplers:

• Moisture determination for different raw

materials, coal and other samples;
• Sieve test of RM, KM, Coal, Cement, and other
samples;
• Litter weight (bulk density) of clinker.
… Cont’d
Tests performed in process control lab:

 This laboratory is opened for 24 hours.

 It has closer contact with Raw meal, kiln and

Cement meal, coal operators in order to control the
daily quality of the parameters.

 It has major role in tacking action on operations so

that, statistically controlled process attained with
efficient and effective means of production.
… Cont’d
Tests performed in this lab are:

 Checking of solutions prepared by chemists (0.25N NaOH, 0.5N

HCl, 0.1N HCl): volumetric method
 Determination of free lime of clinker: volumetric method
 Determination of total carbonate of LSOB, CLS, filler and other
materials (by a method of back titration): volumetric method
 Determination of sulphates of cement, gypsum and other raw
materials: gravimetric method
 Determination of cement fineness by air permeability method
(Blaine method): specific surface area of cement
 Pozzolancity test (pumice content) for PPC: Volumetric
 Proximate analysis of coal: moisture, VM, ash & fixed carbon (3rd
process control)
… Cont’d
Question:

OPC/PPC have higher Blaine? Why?

… Cont’d
 Pozzolancity test for PPC:

• PPC is blended cement and it is mix of Portland Clinker with

mineral additive (natural pozzolana or pumice in our case);
• Its pumice content is tested hourly;
• Pozzolanas are siliceous or siliceous & aluminous materials
which in itself possesses little or no cementitious
properties, when finely ground they react in presence of
water at ambient temperature with dissolved Ca(OH)2 from
lime or Portland clinker to form strength developing
calcium silicate & calcium aluminates compounds. They are
natural substances or industrial activated products.
… Cont’d
Tests performed in analytical lab:

 Checking the purity of distilled water;

 Preparation, standardization and correction of solutions (0.5N
HCl, 0.25N NaOH, 0.1N HCl, ethylene glycol, 0.01M EDTA, etc.);
 Preparation of reagents and indicators (phenolphthalein,
Congo-red, Thymol fluoroxone, PAN, PAR, Copper
complaxmate, Buffer PH 3 & PH 10, 10% barium chloride, etc.);
 Complete analysis of cement raw materials, clinker, cement,
coal ash, and other materials: by complete analysis, it means
the total content (chemistry) of the material out of 100%, the
parameters are: LOI, SiO2, AL2O3, Fe2O3, CaO, MgO, SO3, and
other trace oxides;
… Cont’d
Tests performed in Instrumental lab (XRF/XRD lab):

 Complete analysis of cement raw materials, clinker,

cement, and other materials with hourly, 8 hours and
daily basis.
 The calorific value of local and imported coal also
tested instrumentally using bomb calorimeter (3rd
line XRF room).
… Cont’d
Tests performed in physical lab:

 Fineness of cement by sieve & Blaine method;

 Initial and final setting time;
 Standard consistency test: consistency refers to the
relative mobility (ability to flow) of a freshly mixed
cement paste or mortar.
 Expansion test;
 Flexural and compressive strength;
 Soundness test
… Cont’d

Cement soundness:
 By “soundness” is understood the ability of cement
to maintain a constant volume.
 Soundness refers to the ability of hardened paste to
retain its volume.
 a cement is to be rated as sound if, after it
hardened, it remains free from expansion effect
which may crack, loosen and destroy the hardened
paste.
 Unsoundness i.e. lack of volume stability is caused
by high content of MgO.
… Cont’d

Factors affecting soundness of cement:

 High MgO content,

 High free lime of clinker;
 Fineness of raw meal (more fine RM reacts
better);
 Chemical composition of clinker;
 Clinker burning and cooling;
 Fineness of cement;
 Storage of cement, etc.
… Cont’d
Hydration of cement:

 A chemical reaction that takes place between water &

cement or the process in which water is combined with
the reacting substance is called hydration.
 C3S and C2S hydrate to form calcium hydroxide (CH) &
calcium silicate hydrate (C-S-H).
 During hydration reaction, the volume swells, i.e. CaO +
H2O Ca(OH)2.
 Solidification is the change of the liquid or plastic system
(cement paste) into a stone like solid progressively by the
process of setting and hardening.
… Cont’d
 By setting to mean cement paste stiffens into a solid
without enough strength & hardening refers to the gradual
development of required strength.

 The overall result of hydration reaction is hardened

cement possessing high strength, the more rate of
hydration faster the development of strength.

 The finer the cement the higher the rate of hydration

hence faster strength development, because finer cement
offers greater surface area of particles for hydration.
 Generally, the strength of cement concrete or mortar
develops with the rate of hydration.
… Cont’d
3.2 Quality assurance

 Quality assurance is the establishment of standards

for processes, materials and finished products that
meet applicable regulatory requirements.
 It covers all aspects of product development and
manufacturing from raw material control to process
validation and final product release.

 In other words, quality assurance is the act of

verifying that the quality requirements you planned
for will be fulfilled as your product is made.
… Cont’d
 Quality assurance also involves corrective action
when deviations or errors occur, so that the product
is still safe and effective.
 It requires a combination of planning, testing and
monitoring.
 It helps companies avoid costly recalls and maintain
a good reputation.
 Ultimately, it is the key to producing high-quality
products for customers.
 Quality assurance is a key part of your quality
management plan.
… Cont’d
Quality Assurance Vs Quality Control

Quality control is the inspection phase of quality

assurance. It’s a series of test procedures used
to verify that a product is safe and effective after
mass production.
… Cont’d
Differences between QA and QC:
1) Proactive (QA) Vs Reactive (QC):

 Effective QA is proactive. It aims to prevent defects before

they occur through process design. QC is reactive and exists
to identify defects in the quality of products after they have
happened.
 QA involves the design of processes, such as documenting
standard operating procedures (SOPs).
 QC involves the testing of products to ensure they meet
standards for safety and efficacy. If QC testing uncovers
quality issues, it should result in reactive steps to prevent an
unsafe product from being shipped and distributed.
… Cont’d

2) Process (QA) Vs Product (QC):

 QA is process-oriented, and it focuses on preventing
quality issues. QC is product-oriented and focused on
identifying quality issues in manufactured products
that could affect customer satisfaction.

 Another way to understand this distinction is actions

vs. results. QA involves the actions which create the
product, while QC is focused on the resulting
product.
… Cont’d
 QA Processes:

 Documentation
 Audits
 Supplier management
 Personnel training
 Change control
 Investigation procedures

 QC Procedures:

 Batch inspection
 Product sampling
 Validation testing
 Laboratory testing
 Software testing
… Cont’d
3) System (QA) Vs Parts (QC):

 Quality assurance control systems are the methods and

procedures which are used to safeguard quality standards.
Quality control systems measure parts, including the
outputs of the system.

 QC efforts may also be focused on parts used to create

the final product, such as raw materials from a supplier.
The QA system for quality management may dictate
various activities to make sure inputs are consistently safe
and effective, such as auditing suppliers and batch
sampling raw materials.
… Cont’d
4) Creation (QA) Vs Verification (QC):

 The result of QA activities is a roadmap for

creating high-quality products. It involves defining
standards for product design, manufacture,
packaging, distribution, marketing, and sales.

 QC involves verification of products post-

manufacture and before distribution, or
confirming safety and efficacy.
… Cont’d
5) Entire team (QA) Vs Dedicated personnel (QC):

 Quality assurance activities involve the entire team.

Every member of a life sciences organization is
responsible for QA activities by following SOPs.

 QC is generally the responsibility of certain personnel

within the organization whose duties include following
SOPs for product testing. QC staff follow SOPs for
quality control and document their findings based on
standardized procedures for product testing and
process validation.
… Cont’d
3.3 Quality norms of MCF

The factory set quality norms considering the following

issues:

 Ethiopian standards requirements;

 the quality of clinker and types of cement being
produced in the factory;
 company’s resources;
 inputs from suppliers;
 company’s long year data analysis results and
experiences.
THANK YOU !!