1 Determination Of Silica (SiO2) :

A. For un-fused materials (Limestone, Raw Meal, Kiln Feed, Silica Sand, Gypsum, Clay,
Iron Ore etc.) :

(1) Weigh appx. 0.5 gm sample in a platinum crucible. Add approximately 2 gm of fusion
mixture. Mix thoroughly with the help of a glass rod. Spread more fusion mixture in a
thin layer over the sample and fuse the contents at 950-1000 C in a muffle furnace for an
hour.

(2) Cool the crucible and place it in a beaker. Add 20 ml of conc. HCl and equal amount of
distilled water to dissolve the fused mass. Rinse and remove empty crucible from the
beaker.

(3) Place the beaker on a hot plate (temp. 60-70C) and allow the contents to evaporate to
complete dryness. Now bake the dried mass for about 30 minutes at 100 to 120 C.

(4) Cool the mass upto room temperature.

(5) Add 10 ml of 1:1 HCl and 20 ml of distilled water and heat it for 2-3 minutes on 60-70C
and filter through Whatman # 40 filter paper. Wash the precipitate with hot distilled
water and the filterate is preserved in 250 ml volumetric flask and made the volume upto
the mark for subsequent determination of Fe 2O3, CaO & MgO given in para 2, 4 & 5.

(6) Dry the precipitate along with filter paper in an oven and ignite it in a pre-weighed
porcelain crucible in a muffle furnace at 1150  50C for 1 hour. Cool it in a desiccator
and weigh.

(7) Calculation :

% SiO2 = Weight of precipitate x 100 / weight of the sample

B. For fused materials (Clinker, Cement, Slag or above materials after fusion) :

(1) Weigh approximately 0.5 gm sample in 100 ml beaker. Add approximately two grams solid
ammonium chloride and mix it with a glass rod till smell of ammonia is observed. Add
10 ml of conc. HCl and again mix it. Keep it on a hot plate at the temperature of 60-70C
for 30 minutes. Now bake the dried mass for 30 minutes at 100 – 120 C.
(2) Now follow the step No.5, 6 & 7 of 1 A as given above.
2. Determination of Iron oxide (Fe2O3):

(1) Take out 10 ml of the filterate preserved in the test of SiO 2 (given in clause No.5 of para 1
page 1) and add approximately 50 mg of Sulphosalicylic Acid with constant stirring.
(2) Add dilute ammonium hydroxide (1:6) solution drop by drop till colour changes from pink
to yellow.

(3) Add dilute HCl (1:3) till colour changes back to pink. Add 2-3 drops of HCl in excess.
(4) Shake well and titrate with 0.01M standard EDTA solution to a colourless or pale yellow
solution. Let the EDTA solution consumed be V 2. Please note that the solution of titration
is to be preserved for Al2O3 determination.
(5) Calculations :

1 ml of 0.01 M EDTA = 0.7985 mg

0.7985 x 10-3x M x V2 x 250 x 100

% Fe2O3 = -------------------------------------------
W x 0.01 x 10
where V2 = Volume of EDTA used, and
W = Weight of the sample in gms (taken initially for SiO2 determination i.e.
approx. 0.5 gm..
M = Molarity of EDTA used
3. Determination of Alumina :

(1) Take the solution left after the determination of Fe 2O3 (as given in Clause No.4 of Para2
Page 2) and add 15 ml of excess EDTA solution, 1 ml phosphoric acid ( 1:3 ), 5 ml
sulphuric acid (1:3) and a drop of thymol blue indicator.
(2) Add ammonium acetate drop by drop until the colour changes from red to yellow. Add
25 ml of ammonium acetate in excess.
(3) Heat the solution to just boiling and cool. Add appx. 50 mg of solid xylenol orange
indicator and Bismuth nitrate solution slowly with stirring until the colour of the
solution changes from yellow to red. Add 2 to 3 ml of bismuth nitrate solution in excess.
(4) Titrate with EDTA to a sharp yellow end point.
(5) Calculation :
V = V1 - V2 - (V3 x E)
where V = Volume of EDTA for Alumina in ml
V1 = Total volume of EDTA used in the titration (Clause No.4 para No.2)
this plus excess EDTA (i.e. 15 ml)
V2 = Volume of EDTA used for Iron Oxide determination in ml
V3 = Total volume of bismuth nitrate solution used in the titration in ml
E = Equivalence of bismuth nitrate solution

0.5098  10-3 x M x V  250  100

% Al2O3 = ----------------------------------------------
W x 0.01 x 10
W = Weight of sample in gm (taken initially for SiO2 determination i.e. approx. 0.5 gm).
M = Molarity of EDTA solution used in titration.
4. Equivalence of Bismuth Nitrate Solution :
(1) Transfer 100 ml of Bismuth Nitrate solution to a 500 ml conical flask and dilute it with
about 100 ml distilled water. Add a few drops of Thymol Blue solution and ammonium
acetate solution until the colour changes from red to yellow. Add 50 mg of Xylenol
Orange indicator and titrate with 0.01M EDTA solution until the colour changes from
red to yellow. The equivalence ( ml of EDTA of 1 ml of Bismuth Nitrate solution is
calculated as follows :
(2) Calculation :
Volume of EDTA consumed
E = ------------------------------------------
100
4. Determination of CaO :

(1) Take 10 ml of silica free acid sample solution (preserved in clause No.5 of para 1 page 1)
into a 250 ml conical flask.
(2) Add 5 ml 1:1 glycerol with constant stirring and then 5 ml of triethanolamine.
(3) Add 6-8 pellets of NaOH and shake well.
(4) Add about 50 ml of distilled water and 50 mg of Patton & Reeder’s indicator.
(5) Titrate against 0.01M EDTA solution till the change in colour from wine red to clear blue.
(6) Calculation :
0.5608  10-3 x M x V x 250 x 100
%CaO = --------------------------------------------
W x 0.01 x 10
Where : V = volume of EDTA used
W = weight of the sample in gm (taken initially for SiO 2
determination i.e. approximately 0.5 gm.)
M = Molarity of EDTA solution
5. Determination of Magnesia MgO :

(1) Take 10 ml of silica free acid solution (preserved in clause No.5 of para 1 page 1) in a 500
ml conical flask. Add 5 ml of 1:1 triethanolamine with constant shaking and 20 ml of
buffer solution of pH 10.
(2) Add appx. 50 mg of solid Thymol Phthalexone/mixed indicator (0.08 gm naphthol
green B + 0.05gm O-Cresol Phthalein + 0.06 gm Eriochrome Black- T + 20 gm
Ammonium Chloride) and appx. 50 ml of distilled water.
(3) Titrate it against standard 0.01M EDTA solution until the colour changes from blue to
clear pink or colour less.
(4) This titration gives the sum of CaO and MgO. Titre value of MgO is obtained by
subtracting the titre value of CaO as in previous section from the total titre value.
(5). Calculation:
0.4032 x 10-3  ( V1 - V ) x 250 x 100 x M
% MgO = -------------------------------------------------------
W x 0.01 x 10
Where :
V1 = Volume of EDTA used in this titration
V = Volume of EDTA used in CaO determination (Clause No. 5 Para 4 Page 4)
W = Weight of the sample in gm (taken initially for SiO2 determination i.e.
approximately 0.5 gm.).
M = Molarity of EDTA solution used in titration.
6. Calculation of LSF

(a) For Cement

CaO – (0.7 x SO3)

LSF = --------------------------------------------------------
(2.8 x SiO2) + (1.2 x Al2O3) + (0.65 x Fe2O3)

(b) For Raw mix and Clinker

CaO
LSF = --------------------------------------------------------
(2.8 x SiO2) + (1.2 x Al2O3) + (0.65 x Fe2O3)

7. Calculation of A/F or AM

Al2O3
A/F or AM = --------
Fe2O3
8. Calculation of S/R or SM

SiO2
S/R or SM = ---------------------
Al2O3 + Fe2O3