Shara N K.

Khan GN& Chari VD

S. Testing of Raw materials

3.1 Chemical testing

3.1.1 Limestone testing

3.1.1.1 Testing of total carbonate and magnesium carbonate

Method-1 (Using 0.5N HCI and 0.25N NaOH solutions)

Total Carbonate (TC)

Weigh 0.50 gm of sample in a clean and dried 250 ml conical flask.

Add 10 ml of distilled water and add 25 ml of 0.5N HCI. Boilthe
solution for 2 minutes. Remove it wash the sides of the conical flask
with distilled water. Cool the solution to room temperature.
Titrate against 0.25N NaOH solution using phenolphthalein
indicator. End point is light pink. Titrate against (N/4) NaOH.

N= Normality of HCI
N; = Normality of NaOH
V =
volume of NaOH consumed

Total Carbonate% = 10x N, x

MgCO, (MC)
Followed by above test of TC (after reaching the end point) add
Add
excess 3 ml of 0.25N NaOH in a same conical flask .
Thymolphthalein indicatior into it. Boil the solution for 3
minutes.
then
tnsure the colour is voilet (if voilet colour is not coming
till voilet
additional amount of 0.25N NaOH is added and boiled
Colour). Cool the solution to normal temperature. Titrate against
0.5N HCI till pink colour.

V= Volume of NaOH Consumed

V=Volume of HCl consumed
N= Normality of HCI
N Normality of NaOH
=

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 CEMENT LABORATORY MANAGEMENT

MgCO,% =V,-N N2XV2xN,Ngx8.43

8.43 x

Reactions involed in this testing method

CaCO+ 2HCl = CaCl2 + H20+ CO2

MgCO3 +2HCl = MgCl2 + H,0 + CO

NaOH+HCl = NaCI + H,0

MgCl2 + 2NaOH = Mg(OH), + 2NaCl

Mg(OH)2 + HCl =MgCl2 + H20(back titration)

Explanation for the calculation for TC (total carbonate) and MC

magnesium carbonate)
When 25 ml of HCI is used, some part of it reacts with the sample
and remaining part of HCI is calculated for determination of TC.

Remaining part of HCl = V, = 25 - X, where X

=
reacted part of HCI

(25 X) x N, =
V2 x N2

(25-X) = N2 xV2
N1
X=
25-(xV2,consumption of HCl in ml

05 1000/
(100)
as
CaCO and MgCO3
Since the total
carbonate is expressed
3, t h e formula

becomes, as
Caco3

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 Sharma N K, Khan GN& Chari V D

=10N,x (25N.
If Sample has higher percentage of
MgCO, (Dolmite) the addition
of NaOH is to be increased to get a voilet colour after
thymolphelene. boiling with

Method-2 (Using 0.4N HCI and 0.IN NaOH

solutions)
Total Carbonate (TC)

Weigh 0.5 gm of sample in a clean and dried 250 ml conical flask.

Add 10 ml of distilled water and add 25 ml of 0.4N HCI.
Boil the
solution for 2 minutes. Remove it wash the sides of the conical flask
with distilled water. Cool the solution to
room temperature.
Titrate against 0.1N NaOH solution
using phenolphthalein
indicator. End point is light pink.

Total Carbonate as CaCO % =

Acid Alkali factor -

BR

Determination of Acid alkali factor

Weigh 0.5 gm of oven dried pure CaCO3 (of known

purity)
sample in a clean and dried 250 ml conical flask. Add 10 ml of
distilled water and add 25 ml of 0.4N HCI. Boil the solution for 2
minutes. Remove it wash the sides of the conical flask with distilled
water. Cool the solution to room
temperature. Titrate 0.1N against
NaOH solution using phenolphthalein indicator. End point is light
pink.

Acid alkali factor = %Purity of CaCO3 +BR of NaOH

Explanation for acid alkali factor

CaCO3 2HCI
= CaCl2 + H20 +CO, T
100gm 73gm
100 gms of CaCO3 reacts with 73
gms pf HCI
. 5 gms of 100%
pure CaCO3 can react with

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 CEMENT LABU 1EMENNT

0.5 x 73= 0.365 gm of HCI

100

contains
25 ml of 0.4N HCI
25
x0.4 x 36.5 = 0.365 gm of HCI.
1000

Let the purity of CaCO; be 98.5%

98.5 % pure CaCO3 will react with

98.5
0.365 Xon0.3595 gm of HCI
Balance unreactedHCI present in the solution

0.365 0.3595 =
0.0055gm ofHCI
14.6 gms of HCl is present in 1000 ml of 0.4N HCI

0.0055 gms of HCI is presentin

1000
0.0055x4. 0.3767 ml of 0.4N HCI
0.3767 ml of 0.4N HCI
=0.3767 x = 1.50 ml of 0.1N Na0O

Factor =
Purity of CaCO + BR of NaOH =98.5 + 1.5 =
10
MgCO, (MC)
Followed by above test of TC oint) a
excess 10 ml of (after
0.IN NaOH in a reaching the end Ad*
Ad
Thymolphthalein same conical
Ensure the colourindicatior into it. Boil the solution for 3 minutes
inutes
is voilet
additional amount of (if voilet colour is m i n g then

colour). 0.1N NaOH is added andn dd tillvoile

Do T e a gvoa i n s
Cool the
0.4N HCI till solutionto normal
pink colour. temperature.
%MgCO =
3.36 x (M- Rof 0.4N HCI)

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 Sharma N K, Khan GN & Chari V D

M factor for NaOH solution used after testing of TC, If 10 ml

NaoH is used the factor is 2.5, for 20ml it is 5, for 30 ml it is 7.5.

The factor 3.36 can be derived by the calculation

Factor= Normalityx
Eq.Wt of MgCO3 1
x 100
1000 Wt of sample
42 1
0.4 x * 100 =
3.36
1000 05
5

Reactions involed in this testing method

CaCOg +2HCI = CaCl2 +H20 + CO2

MgCO +2HCl = MgCl2 + H,0+CO2

NaOH+ HCl = NaCl +H20

MgClh +2NaOH = Mg(OH)2 + 2NaC

Mg(OH) + HCl =
MgCl2 + H,0(back titration)
If the sample has higher percentage of MgCO, (Dolmite) the
addition of NaOH is to be increased to get a voilet colour after
boiling with thymolphelene.

3.1.2 Test of raw materials by Fusion method

in a
0.50 gm of raw material sample (passing 150u) is weighed
clean platinum crucible and about 2 to 4 gm of Fusion mixture (A
of equi-molecular ration of Na2CO3 and KCO:) is added.
mixture
It is mixed uniformly and additional fusion is added to cover it.

Fuse the material with a lower flame for 10 tol5 minutes. (Shake
at higher
the crucible at 5 minutes' time interval) Keep the crucible the
ame for 30 to 40minutes. Take the crucible out and quench
it to normal
ernal of the crucible with water25 to bring
to
Emperature. Extract the whole mass in 30 ml of (1:1) HCI in
d evaporating dish. Clean the crucible with distilled water in the

wire gauge and evaporate to dryness

vaporating dish on a

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