408CHP06 CHEMICAL ANALYSIS LAB 0 0 3 2

OBJECTIVE
To learn basic principles involved in estimation and characterization of industrially
important materials.

I. Soap Analysis
a. Estimation of total fatty acid.
b. Estimation of percentage alkali content.

II. Oil Analysis

a. Estimation of free acid
b. Determination of Saponification value
c. Determination of iodine value

III. Cement Analysis

a. Estimation of Silica content
b. Estimation of mixed oxide content
c. Estimation calcium oxide content
d. Estimation of calcium oxide by rapid method

IV. Coal Analysis

a. Estimation of Sulphur present in coal
b. Ultimate analysis of coal
c. Proximate analysis of coal

V. Analysis of Bleaching Power

a. Estimation of Available Chlorine

VI. Analysis of Glycerol

a. Estimation of purity of glycerol

VII. Analysis of fuels

a. Flash point
b. Fire point
c. Cloud point
d. Pour point
e. Aniline point

TOTAL : 45 PERIODS
REFERENCES
1. Technical Analysis Manual, Chemistry Division, Chemical Engineering
Department, A.C. Tech. Anna University (2007).
2. Hand book of Chemical Analysis by Griffin.
 Estimation of Silica content of Cement

Aim

To estimate the silica content in the given cement sample

Apparatus Required

Crucible, Desiccator, Beaker, Water bath, No 40 Watt man filter paper, Pipette, Electric Bunsen
Burner, Stirrer

Chemicals Required

Given sample of Portland cement, 1:1 HCl.

Procedure:

1) 2 gm cement was weighed and transferred into china dish.

2) 2 ml of water was added to prevent lumping.
3) 10 ml of 1:1 HCl was added to this and digested for 10 minutes.
4) 50 ml of water was added to it and the contents were transferred from china dish to a beaker.
5) 50 ml of 1:1 HCl was again added to this beaker to make the medium acidic.
6) The solution was filtered through No 40 Watt man filter paper
7) The residue was incinerated in the pre weighed crucible using an electric Bunsen burner
8) Then it was cooled in a desiccator.
9) The crucible with its content was weighed.
10 From the difference in the weight the amount of silica was found.

Calculation

Weight of cement taken (w) = g

Weight of empty crucible (a) = g
Weight of silica + crucible (b) = g
% of silica = ( b – a ) x100 w
% of silica = ____________

Result

The amount of silica content in cement was found to be =______________.

 Estimation of Mixed Oxide content of Cement

Aim

To estimate the mixed oxide content in the given cement sample

Apparatus Required

Crucible, Desiccator, Beaker, Water bath, No 40 Wattman filter paper, Pipette, Bunsen burner,
Stirrer

Chemicals Required

Given sample of Portland cement, 1:1 HCl, 15% NaOH solution, NH4Cl, NH3

Procedure

1) 2 gm cement was weighed and transferred into china dish.s

2) 2 ml of water was added to prevent lumping.
3) 10 ml of 1:1 HCl was added to this and digested for 10 minutes.
4) 50 ml of water was added to it and the contents were transferred from china dish to a beaker.
5) 50 ml of 1:1 HCl was again added to this beaker to make the medium acidic.
6) The solution was filtered through No 40 Watt man filter paper
7) Then the filtrate was collected in a beaker and made it up to 250 ml using water in a graduated
flask.
8) 100 ml of above solution was pipetted out into a beaker and boiled.
9) 2 gm of NH4Cl was added to it to avoid the precipitation of Ca and Mg compounds
10) 20 ml of NH3 was added to the boiling solution to make the solution alkaline
11) The solution was boiled for about 5 minutes until a pale brown jelly precipitate was formed
12) The solution was cooled and the solution was filtered through No 40 Watt man filter paper.
13) Then the residue was incinerated using Bunsen burner using a preweighed crucible and
cooled in desiccator.
14) The amount of mixed oxide (Fe2O3 + Al2O3) content was found by the difference in weight.

Calculations

Weight of cement taken (w) = g

Weight of empty crucible (a) = g
Weight of mixed oxide content + crucible (b) = g
% of mixed oxide content (Fe2O3 + Al2O3) = ( b – a ) x 250 x 100 /(w x 100)
% of Mixed oxide content = ____________

Result

The amount of mixed oxide content was found to be=_____________.

 Estimation of Calcium Oxide Content of Cement

Aim

To estimate the calcium oxide content in the given cement sample

Apparatus Required

Crucible, Desiccator, Beaker, Water bath, No 40 Watt man filter paper, Pipette, Bunsen Burner,
Stirrer.

Chemicals Required

Given sample of Portland cement, 1:1 HCl, 15% NaOH solution, NH4Cl, NH3, Ammonium
oxalate etc.

Procedure

1) 2 gm cement was weighed and transferred into china dish.

2) 2 ml of water was added to prevent lumping.
3) 10 ml of 1:1 HCl was added to this and digested for 10 minutes.
4) 50 ml of water was added to it and the contents were transferred from china dish to a beaker.
5) 50 ml of 1:1 HCl was again added to this beaker to make the medium acidic.
6) The solution was filtered through No 40 Watt man filter paper
7) Then the filtrate was collected in a beaker and made it up to 250 ml using water in a graduated
flask.
8) 100 ml of above solution was pipetted out into a beaker and boiled.
9) 2 gm of NH4Cl was added to it to avoid the precipitation of Ca and Mg compounds
10) 20 ml of NH3 was added to the boiling solution to make the solution alkaline
11) The solution was boiled for about 5 minutes until a pale brown jelly precipitate was formed
12) The solution was cooled and the solution was filtered through No 40 Watt man filter paper.
13) The collected filtrate was heated.
14) 1 gm of ammonium oxalate was added in 10 ml of boiling water and emptied into the boiling
Filtrate.
15) White precipitate of oxalate was formed during the above procedure.
16) Then it was again filtered through No 40 Watt man filter paper.
17) The preweighed crucible was incinerated in a Bunsen burner and cooled in desiccator.
18) The amount of calcium oxide content was found by the difference in weight.

Calculation

Weight of cement taken (w) = )g)

Weight of the empty crucible (a) = (g)
Weight of crucible + calcium oxide (b) = (g)
% of calcium oxide content = ( b – a ) x 250 x 100 /(w x 100)

Result

The amount of calcium oxide content was found to be =_______________

 Estimation of Total Alkali Content of Soap

Aim
To analyze the given soap sample and to determine the total alkali content

Apparatus Required
Beaker, Stirrer, Glass plate, conical flask, Pipette, Burette, Standard flask, Separating funnel,
Bunsen Burner, Funnel

Chemicals Required

Given sample of soap, water, chloroform, 0.5 N NaOH, Methyl orange, Sodium carbonate,
concentric H2SO4
Procedure

1) 5 gm of soap was weighed accurately in a glass plate and transferred into a 250 ml beaker
2) 100 ml of water was added to completely dissolve the soap.
3) The mixture was heated directly till the fatty matte comes floating above. (Approximately 20-
30 minutes)
4) Then concentrated H2SO4 was added to the beaker using a pipette carefully to the sides of the
container until the fatty acids were floating as a layer above the solution. The volume of H2SO4
was noted.
5) 50 ml of chloroform was added to the remaining solution and transferred to the separating
funnel.
6) The solution was shaken thoroughly until it separates into 2 layers
7) Separate fatty acid dissolved chloroform layer again from the aqueous solution.
8) The aqueous solution volume was measured accurately in a measuring cylinder and 10 ml of it
was taken into a conical flask.
9) 2 or 3 drops of methyl orange indicator was added and titrated against NaOH from the burette.
10) Yellow to pale pink color indicates end point
11) Then the total alkali content was calculated.

Calculation
Total volume of the aqueous solution =V=__________ml
TITRATION
Standard NaOH Vs soap sample

Volume of Burette reading(ml) Volume of Concordant

Soap NaOH(ml) titer value Indicator
sample(ml)
Initial Final
10 0 t t Methyl
10 0 t t t orange

10 ml of aqueous solution required t ml of NaOH

V_ml of aqueous solution requires = V*t /10 = V1 ml.
Amount of NaOH required by acid in aqueous solution =V1 ml
Normality of NaOH= 0.5N
Volume of H2So4 required V2= 1 ml ( 1- 3 ml)
Normality of H2So4 N2= 46 N
Weight of soap taken = m g

[ ( V2N2- V1N1)]/ m
% of alkalinity = 4X
= ________________

Result

The total alkali content of the given soap sample was found to be___________
 Estimation of Total Fatty Matter Content of Soap

Aim

To analyze the sample of the given soap and to determine the total fatty matter content

Apparatus Required

Beaker, Stirrer, Glass plate, conical flask, Pipette, Burette, Standard flask, Separating funnel,
Bunsen Burner, Funnel, China dish.

Chemicals Required

Given sample of soap, Water, Chloroform, Sodium carbonate, 0.5 N HNO3

Procedure

1) 5 gm of soap was weighed accurately in a glass plate and transferred into a 250 ml beaker
2) 100 ml of water was added to completely dissolve the soap.
3) The mixture was heated directly till the fatty matter comes floating above. (Approximately 20-
30 minutes)
4) Then concentrated H2SO4 was added to the beaker using a pipette carefully to the sides of the
container until the fatty acids were floating as a layer above the solution. The volume of H2SO4
was noted
5) The fatty matter collected was filtered using a filter paper and transferred to a preweighed
china dish.
6) The contents were allowed to evaporate in an electric oven and the residue was weighed.
7) From the difference in weight, the % of fatty matter in the given soap sample was calculated.

Calculation

Weight of the china dish (x) = _____________

Weight of china dish + Soap after drying (y) =______________
% of fatty mater = (y – x) * 100* Weight of soap sample
% of fatty matter = ___________.

Result

The percentage of total fatty matter present in the given sample of soap was found to
be_________
 Estimation of Iodine Value of Oil

AIM

To determine the amount of unsaturation present in the given oil. (To determine the iodine
value of an oil)

PRINCIPLE

The Iodine number is defined as the number of grams of iodine which will add to 100 grams of
fat or oil. Iodine value shows the degree of unsaturation of the constituent fatty acids in an oil or
fat and is thus a relative measure of the unsaturated bonds present in the oil or fat. Iodine value is
expressed in grams of iodine absorbed by 100 gms of oil or fat. Unsaturated compounds absorb
iodine (in suitable form) and form saturated compounds. The amount of iodine absorbed in
percentage is the measure of unsaturation in the oil. No oil has zero iodine value and oils are
classified as drying, semi drying and non drying on the basis of iodine value..

CHEMICALS REQUIRED

Wij’s Solution:
Dissolve separately 7.5 gm of AR Iodine tetrachloride and 8.5 gm of resublimed iodine in
glacial acetic acid by warming on a water bath. Mix the two solutions and dilute to 1 litre with
glacial acetic acid in cold.

Potassium iodide solution ( 15%)

Dissolve 15 gm of AR potassium iodide in 100 ml of water.
Sodium thiosulphate solution (0.1 N)
Dissolve 25 gm of AR sodium thiosulphate crystals (Na2S2O3 .5H2O) in a 1 litre of
distilled water.

Starch indicator solution

1 ml of starch in 100ml boiling water.

PROCEDURE

Standardization of Sodium Thiosulphate Solution

1. 20 ml of 0.1 N potassium dichromate solution was pipetted out accurately into a clean conical
flask.
2. 10 ml of dilute H2SO4 was added to the conical flask followed by 10 ml of 15% KI solution.
3. Then it was titrated against thiosulphate from the burette until it turns into pale yellow.
4. 1 ml of starch indicator was added and titrated against thiosulphate solution.
5. End point is disappearance of blue color.

EXPERIMENTAL PROCEDURE

1. 0.5 gm of oil was weighed accurately and transferred into Iodine flask.
2. 10 ml of chloroform was added and warmed slightly and cooled for 10 minutes
3. Then 25 ml of Wij’s solution was added in the same flask and shaken vigorously.
4. Then the flask is allowed to stand for half an hour in dark place.
5. Then 10 ml of KI solution was added and the solution was titrated against 0.1 N Sodium
thiosulphate solution until the appearance of yellow color.
6. 1 ml of starch indicator was added and again it was titrated against the sodium thiosulphate
solution from the burette.
7. Disappearance of blue color indicates end point.
8. The above procedure was repeated without taking sample (ie Oil) and the corresponding
reading was noted for blank titration.

CALCULATION

Titration I
Standardisation of Sodium thiosulphate:
Burette solution: Sodium thiosulphate
Pipette solution: Potassium dichromate
Additional solution: 10ml of dil H2SO4 solution
Indicator: Starch
End point: Disappearance of blue colour

Volume of Burette reading(ml) Volume of Concordant Indicator

K2Cr2O7 Thiosulphate titer value
(ml)) solution(ml)
Initial Final
20 0 Starch
20 0

Volume of K2Cr2O7 ( V1) =

Normality of K2Cr2O7 (N1) =
Volume of sodium thiosulphate solution (V2) =
Normality of sodium thiosulphate solution ( N2) = (V1 x N2) / V2

Titration II
ESTIMATION OF IODINE VALUE:
Burette solution: Std. Sodium thiosulphate solution
Pipette solution: 20 ml of oil
Additional solution: 25 ml of Wij’s solution + 20 ml of KI ( 15%)+50 ml of water
Indicator: Starch
End point: Disappearance of blue color

Blank titre value V1 =

Sample titre value V2=
Iodine value = (V1 – V2) x N1 x Equivalent weight of Iodine x 100
W x 1000
where
V1 = Volume of thiosulphate required by blank,ml N1 = Normality of thiosulphate
V2 = Volume of thiosulphate required by sample,ml W= Weight of the sample
Iodine value = _____________mg of KOH/ Gm of oil.

RESULT

The iodine value of the given oil sample was found to be =___________ mg of KOH/ Gm of oil.
 Estimation of Saponification Value of Oil

AIM

To calculate the number of milligrams of potassium hydroxide required to completely

saponify 1 gm of Oil.

THEORY

Saponification value indicates the average molecular weight of a fat or oil. The saponification
value may be defined as the number of milligrams of caustic potash required to neutralize the
fatty acids obtained by complete hydrolysis of one gram of oil or fat. Thus saponification value
gives us information whether an oil or fat contains high proportion of lower or higher fatty acids.
Applications of saponification value: Saponification value gives us an idea about the molecular
weight of fat or oil.
Oil x Saponification Value = Amount of Lye needed to make soap.

PROCEDURE
STANDARDIZATION OF KOH

1) 20 ml of 0.1 N oxalic acid solution was transferred in to a 250 ml conical flask.

2) 1 or 2 drops of phenolphthalein indicator was added to this solution.
3) This solution was titrated against KOH taken in a burette.
4) The appearance of pink color indicates the end point.
5) From the volume of the KOH solution in burette the normality of KOH was found.

ESTIMATION OF SAPONIFICATION VALUE

1) 1 gm of oil was weighed accurately and transferred into the round bottomed flask.
2) 20 ml of 0.5 N alcoholic KOH solution was added to the round bottomed flask.
3) The above procedure was followed without taking oil for blank titration.
4) Both contents were refluxed in round bottomed flasks for 1 hour.
5) After refluxing both the round bottomed flasks were allowed to cool.
6) Both the samples were titrated against 0.5 N HCl with phenolphthalein indicator.
7) The disappearance of pink indicates the end point.

CALCULATION
Titration I: STANDARDISATION OF KOH:

Burette solution : KOH

Pipette solution : Oxalic acid
Indicator : Phenolphthalein
End point : Appearance of pink colour
Volume of Burette reading(ml) Volume of Concordant Indicator
Oxalic acid KOH(ml) titer value
(ml)
Initial Final
20 0 Phenolphthalein
20 0

Volume of oxalic acid (V1)=

Normality of oxalic acid (N1)=
Volume of KOH consumed (V2)=
Normality of KOH consumed (N2)= V1 N1 / V2
Normality of KOH (N2) = _______________.

TITRATION II: ESTIMATION OF SAPONIFICATION VALUE

Burette solution: HCl

Flask solution: Alcoholic KOH (with and without oil)
Indicator: Phenolphthalein
End point: Disappearance of pink colour
Blank titre value:
Titre value of sample:
Saponification Value= (Titre value of blank in ml – Titre value of sample in ml) x NKOH x
Equivalent wt of KOH)/Weight of the sample=___________________
Saponification value = ________________mg of KOH/ Gm of oil

RESULT

The saponification value of the given oil sample was found to be_________ mg of KOH/ Gm of
oil .
 ESTIMATION OF ACID VALUE OF OIL
AIM

To calculate the number of milligrams of potassium hydroxide required to neutralize the

free fatty acid in 5 gm of oil.

THEORY

Acid value indicates the proportion of free fatty acid present in an oil or fat and may be defined as
the number of milligrams of caustic potash required to neutralize the acid in 1 gm of the sample.
The normal acid value for most samples lies within 0.5. If any titrable acid other than a fatty acid
is present in the sample, it will be an error. A high acid value indicates a stale oil or fat stored
under improper conditions.

PROCEDURE
STANDARDIZATION OF KOH

1) 20 ml of 0.1 N oxalic acid solution was transferred in to a 250 ml conical flask.

2) 1 or 2 drops of phenolphthalein indicator was added to this solution.
3) This solution was titrated against KOH taken in a burette.
4) The appearance of pink color indicates the end point.
5) From the volume of the KOH solution in burette the normality of KOH was found.

EXPERIMENTAL PROCEDURE

1) 5 gm of oil was weighed accurately and transferred into a 250 ml conical flask.
2) 50 ml of neutralized alcohol solution was added to the oil solution.
3) This mixture was heated for 10 minutes by using the heater.
4) Then the solution was taken after 10 minutes and 1 or 2 drops of phenolphthalein indicator was
added to it.
5) This was titrated against the KOH solution from the burette.
6) The appearance of pink color indicates the end point

Calculation

Titration I: STANDARDISATION OF KOH:

Burette solution : KOH

Pipette solution : Oxalic acid
Indicator : Phenolphthalein
End point : Appearance of pink colour
Volume of Burette reading(ml) Volume of Concordant Indicator
Oxalic acid KOH(ml) titer value
(ml)
Initial Final
20 0 Phenolphthalein
20 0

Volume of oxalic acid (V1)=

Normality of oxalic acid (N1)=
Volume of KOH consumed (V2)=
Normality of KOH consumed (N2)= V1 N1 / V2
Normality of KOH (N2) = _______________.

TITRATION II: ESTIMATION OF ACID VALUE

Burette solution: KOH

Pipette solution: Oil + 50 ml of neutralized alcohol
Indicator: Phenolphthalein
End point: Appearance of pink colour
Titre value or Volume of KOH =
Acid value = (Volume of KOH x Normality of KOH x Eq. wt x 1000) / Weight of Oil sample
Acid Value = _________ mg of KOH/ Gm of oil.

RESULT

The acid value of the given oil sample was found to be__________ mg of KOH/ Gm of oil.
 ANALYSIS OF BLEACHING POWDER
ESTIMATION OF AVAILABLE CHLORINE

AIM :

To estimate the amount of available chlorine in the given bleaching powder sample.

THEORY:

Bleaching powder is a mixture of CaCl2, Ca(OCl)Cl, and Ca(OCl)2 and is prepared by the
reaction of Cl2 and slaked lime, Ca(OH)2. The commercial bleaching powder consists
essentially of a mixture of calcium hypochlorite Ca(OCl)2 and the basic chloride
CaCl2,Ca(OH)2,H2O; some free slaked lime is usually present. The active constituent is
the hypochlorite, which is responsible for the bleaching action. Upon treating bleaching
powder with hydrochloric acid, chlorine is liberated:

ClO- +C1- + 2H+ = C12 + H2O

The available chlorine refers to the chlorine liberated by the action of dilute acids on the
hypochlorite, and is expressed as the percentage by weight in the case of bleaching
powder. Commercial bleaching powder contains 36-38 per cent of available chlorine. The
hypochlorite solution or suspension is treated with an excess of a solution of potassium
iodide, and strongly acidified with acetic acid:

ClO- + 2I- + 2H+ = Cl- + I2 + H2O

The liberated iodine is titrated with standard sodium thiosulphate solution. The solution
should not be strongly acidified with hydrochloric acid, for the little calcium chlorate
which is usually present, by virtue of the decomposition of the hypochlorite, will react
slowly with the potassium iodide and liberate iodine:

ClO3- +6I- + 6H+ = Cl- + 3I2 + 3H2O

CHEMICALS REQUIRED:
0.1 N Potassium dichromate, Potassium iodide, 0.1N Sodium thiosulphate solution,
bleaching powder, glacial acetic acid.
Starch Indicator solution:
1mg of starch in 100 ml of boiling water.

APPARATUS REQUIRED:
Pestle and mortar, 500 ml volumetric flask, burette, pipette, Iodine flask.

PROCEDURE:

STANDARDIZATION OF SODIUM THIOSULPHATE SOLUTION

1. 20 ml of 0.1 N potassium dichromate solution was pipetted out accurately into a clean conical
 flask.
2. 10 ml of dilute H2SO4 was added to the conical flask followed by 10 ml of 15% KI solution.
3. Then it was titrated against thiosulphate from the burette until it turns into pale yellow.
4. 1 ml of starch indicator was added and liberated iodine was immediately titrated against
thiosulphate solution till the disappearance of blue colour.

EXPERIMENTAL PROCEDURE:

1. 5.0 g of bleaching powder was weighed accurately in to a clean mortar.

2. A little amount of water was added and the mixture was ground to a suitable paste.
3. The milky liquid suspension was poured off into a 500 ml volumetric flask.
4. The residue in the mortar was ground again with little water and the above operation was
repeated until whole of the suspension has been transferred into the flask as a very fine
suspension and the mortar was washed clean.
5. The volumetric flask was then filled with water up to the mark and shaken well and 50 ml of
turbid liquid was transferred into a Iodine flask .
6. 25 ml of water was added to it followed by 10ml of 15% Potassium iodide solution and 10 ml
of glacial acetic acid.
7. The liberated iodine was titrated against standard 0.1 N sodium thiosulphate solution until it
turns into pale yellow colour.
8. Then 1 ml of starch indicator solution was added and liberated iodine was immediately titrated
against thiosulphate solution till the disappearance of blue colour.

TITRATION I

STANDARDIZATION OF SODIUM THIOSULPHATE SOLUTION

Burette solution : 0.1 N Thiosulphate solution

Pipette solution : 0.1N K2Cr2O7
Additional solution: 10ml of 15% KI+ 10ml of glacial acetic acid
Indicator : Starch
End point : Disappearance of blue colour

Volume of Burette reading(ml) Volume of Concordant Indicator

K2Cr2O7 Thiosulphate titer value
(ml)) solution(ml)
Initial Final
20 0 Starch
20 0

Volume of K2Cr2O7 ( V1)=

Normality of K2Cr2O7 (N1)=
Volume of Thiosulphate solution (V2) =
Normality of Thiosulphate solution consumed (N2) = V1N1/ V2
Strength of Thiosulphate solution = ---- N

TITRATION II
ESTIMATION OF AVAILABLE CHLORINE
Burette solution : 0.1 N Thiosulphate solution
Pipette solution : 50ml of sample
Additional solution: 10ml of 15% KI+ 10ml of glacial acetic acid
Indicator : Starch
End point : Disappearance of blue colour

Volume of Burette reading(ml) Volume of Indicator

bleach Thiosulphate
sample solution(ml)
Initial Final
(ml))
50 0 Starch

Calculation:
Volume of thiosulphate solution ( V1)=
Normality of thiosulphate solution (N1)=
Volume of bleach sample (V2) = 50 ml
Normality of bleach sample consumed (N2) = V1N1/ V2
Strength of bleach sample consumed = ---- N
Amount of available chlorine}
in 50 ml bleach sample = strength of bleachX equivalemt wt of chlorineX 100
1000
Percentage available chlorine in the bleach sample = Amt of Cl2 X 100/ weight of sample taken
= __________%

RESULT:
The percentage of available chlorine in the given sample was found to be __________
 COAL ANALYSIS- PROXIMATE ANALYSIS
AIM:
To assay the given sample of coal and determine the moisture content, volatile matter content,
ash content and fixed carbon content.

THEORY:

Coal is classified into three types namely, anthracite, bituminous and lignite. The
common coal used in Indian industry is bituminous and sub-bituminous. There are two methods
for analysis of coal: Proximate and Ultimate analysis. Ultimate analysis determines all coal
components – solid or gaseous whereas Proximate analysis determines only the moisture content,
volatile matter content, ash content and fixed carbon content.

APPARATUS REQUIRED:

Mortar and Pestle, Silica crucible, dessicator, muffle furnace

PROCEDURE:

MOISTURE CONTENT:

Determination of moisture is carried out by placing 2 grams of powdered raw coal of size 200-
micron size in an uncovered crucible and it is placed in the oven kept at 108+2 oC for about one
hour along with the lid. Then the sample was cooled to room temperature in a dessicator and
weighed again. The loss in weight represents moisture.

VOLATILE MATTER:

Powdered raw coal of about 2 grams was accurately weighed and placed in a covered crucible
and kept in a Muffle furnace maintained at 900 oC for exactly 7 minutes. Then the sample was
cooled to room temperature in a dessicator and weighed again. The loss in weight represents
volatile matter content.

ASH CONTENT:

Powdered raw coal of about 2 grams was accurately weighed and placed in an uncovered
crucible and kept in a Muffle furnace maintained at 400- 450 oC for about 60 – 80 minutes. Then
the sample was cooled to room temperature in a dessicator and weighed again. The weight of the
residue remaining in the crucible corresponds to the ash content . It is usually expressed as a
percentage.
FIXED CARBON CONTENT:

The sum total of the percentages of moisture, volatile matter and ash, subtracted from 100
gives the percentage of fixed carbon.

CALCULATION:

MOISTURE CONTENT:
Weight of empty crucible W1=
Weight of crucible+ sample W2=
Weight of crucible+ sample after heating W3=

Percentage moisture = (W2-W3)/ (W2-W1) X 100

VOLATILE MATTER:
Weight of empty crucible W4 =
Weight of crucible+ sample W5=
Weight of crucible+ sample after heating W6=

Percentage volatile matter = (W5-W6)/ (W5-W4)x100

ASH CONTENT:

Weight of empty crucible W7 =

Weight of crucible+ sample W8=
Weight of crucible+ sample after heating W9=

Percentage ash content = (W9-W7)/ (W8-W7)x100

FIXED CARBON CONTENT:

Percentage fixed carbon content = 100 – (%moisture+ % volatile matter+ % ash)

RESULT:

THE PROXIMATE ANALYSIS OF GIVEN COAL SAMPLE IS TABULATED BELOW:

S.NO PARAMETER PERCENTAGE

1 MOISTURE CONETNT
2 VOLATILE MATTER
3 ASH CONTENT
4 FIXED CARBON CONTENT