Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
CH402-CHEMICAL PROCESS INDUSTRIES
LAB MANUAL
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Acid Value
Aim: To Determine The Acid Value Of Given Oil Sample.
Theory:
 Oil or fat consists of various free acids.
 The portion of free acids can be measured as Acid value.
 Acid value is the no. of mg. of Potassium Hydroxide required to neutralize 1 gm. of
fat or oil.
Apparatus:




Weighing balance
Steam bath
Conical flask 250 ml.
Burette 50 ml.
Chemicals:

N Sodium hydroxide
 Neutral Alcohol (Absolute Alcohol)
 Phenolphthalein indicator
 Oil sample
Procedure:
 5 gm. of oil is taken in a conical flask. 50 ml. of neutral alcohol is added and the
mixture is heated up to boiling for 15-20 minutes.
 1 c.c. of phenolphthalein indicator is added and is titrated against 0.1 N NaOH. The
end point may be taken as the first persistence of pink color.
Observations:
 Final volume of titration =
 Normality of NaOH =
N
ml.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Calculation:
Acid value =
5.61 * ml. of NaOH used
wt. of sample taken
=
gm/gm
Result:
The acid value of given sample =
Conclusion:
gm/gm.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Roll No:
Practical No:
Preparation of Caustic Soda
Aim: To prepare the caustic soda by chemical method.
Apparatus: Weighing balance, measuring cylinder (500ml), Burette, Pipette, Beaker
(500ml), Stirrer, etc.
Chemicals: Soda ash (Sodium carbonate), Calcium hydroxide, Hydrochloric acid
solution, Distilled water, Phenolphthalein indicator.
Procedure:
 Take 10.6gm of Soda ash accurately by weight scale.
 Weight 7.4gm of Calcium hydroxide and add it with soda ash in a beaker with 200 ml
of distilled water.
 Mix the content of the beaker thoroughly
 Put the beaker on the heating mental and heat it for about 30 minutes. During heating
stir the content continuously.
 After heating allow the solution to settle down the precipitates.
 Separate the clear solution careful from the precipitates.
 Take 10ml of clear solution in a conical flask and titrate it against ______ N HCl
solution
 Use phenolphthalein as indicator. At the end color change is from pink to colorless.
 Measure the volume of clear solution.
Observations:
 Normality of Hydrochloric acid solution. N1 = _____N
 Volume of sample of clear solution taken for titration (V1) = ____ml
 Final burette reading (V2) = ______ ml
 Total volume of clear solution (V) = _____ ml
Calculations:
Normality of sodium hydroxide solution:
N2 
N2 
Now,
N 1  V1
V2
N2 
N
_____  _____ 
_____
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Normality 
gm equivalent
lit of solution
gm equivalent = N  lit of solution
= ______ ______= ______gm eq.
gm eq. 
Weight
Eq.Wt
Practical Yield (x) = ______ gm
Reaction:
Na2CO3 + Ca (OH) 2
For each gmol
grams
106
74
2 NaOH + CaCO3
2*( 40)
100
So, by Stoichiometric equation, 1 mole (=106 gms) of Sodium Carbonate produces 2
mole (=80 gms) of Sodium Hydroxide
Therefore, 10.6 gms of Sodium carbonate will produce
y = (10.6*80)/106 gm
= ______ gm
Yield of Sodium Hydroxide obtained
(x  100) / y = (______ / ______)  100
Yield = ______ %
Result: The percentage yield of Sodium Hydroxide =
Conclusion:
%
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Determination of the Sodium Carbonate in the Washing Soda
Aim: To determine the sodium carbonate content in the washing soda.
Apparatus Required:





Weighing Balance
Measuring Cylinder (1liter, 500 ml and 10 ml)
Burette (50 ml)
Graduated Pipette (25 ml)
Conical Flask (250 ml)
Chemicals Required:
 Washing Soda-crystals
 0.1 M Hydrochloric acid solution: 9 ml of concentrated Hydrochloric Acid is taken in
1 liter of measuring cylinder and dissolved by 500 ml. of distilled water. At last it is
diluted up to 1-liter quantity using distilled water. It is thoroughly mixed.
 Methyl orange-Indigo Carmine Indicator / Bromocresol green indicator.
Theory:
Washing soda is mainly consisting of Sodium Carbonate. It is used in washing clothes
and is also used for other domestic purpose. It enhances the cleaning action during
washing.
Procedure:
 3.6 gm. of Washing Soda crystals is accurately weighed. It is dissolved in 100 ml. of
distilled water in measuring cylinder (500 ml.) and is diluted up to 250 ml. using
distilled water and is mixed thoroughly.
 25 ml. of Washing soda solution is taken in 250 ml. of conical flask. Burette is filled
with std. 0.1 M Hydrochloric solution. Then Washing Soda solution is titrated against
0.1 M Hydrochloric solution by adding 2 drops of Bromocresol Green as indicator.
 The final end point is found out by color change and the final burette reading is noted
as V1 ml.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Observations:
 Weight of Washing Soda is taken (W3) =
 Final Burette reading (V1)
=
 Molarity of HCl used in burette (M)
=
gm
ml
Calculations:
Weight of anhydrous Sodium Carbonate Na2Co3, which, has reacted with the standard
HCl solution can be readily calculated from known weight of washing soda.
Na2CO3
106
+
2HCl
2NaCl
2(36.5)
(58.5)
1 ml of 1 N HCl
x ml of 1 N HCl
= 0.053 gm .of Na2CO3
=(?) gm of Na2CO3
Weight of Washing Soda in portion titrated = W3 * 25.0/250
= A gm
Percentage of Na2CO3 = (z * 100) /A
=
Result:
Percentage of Sodium Carbonate in Washing Soda =
Conclusion:
%.
+ H2 O
18
+ CO2
44
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Roll No:
Practical No:
Saponification Value
Aim: To determine the saponification value of given oil sample.
Theory:
A fat e.g. Tristearin obtained from beef and mutton tallow or a oil e.g. Tripalmitin present
in palm oil is treated with sodium hydroxide solution called lye to form soap and
glycerin. This process is called Saponification.
In brief, Saponification is the hydrolysis of an ester with an alkali to give alcohol and salt
of that acid.
CH2-CO-C17H35
CH2OH
CHO-CO-C17H35 + 3NaOH
CHOH
CH2-CO-C17H35
CH2OH
Tristearin
Lye
Glycerin
+ 3C17H35COONa
Sodium Stearate
Consumption of lye can be measured during reaction with fatty acids present in oil or fat
by saponification value.
Saponification value is the no. of mg. of KOH required to neutralize the fatty acids
resulting from the complete hydrolysis of 1 gm. of oil or fat.
Saponification value is used to estimate the requirement of lye for known amount of oil
or fat in making soap.
Apparatus:




250 ml. Conical Flask
Measuring Cylinder 100 ml.
Burette 50 ml.
Pipette 25 ml.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
 Measuring Cylinder 1 ltr.
 Weighing balance with weight box
Chemicals:
 0.5 M KOH solutions.
 Dissolve 30 gm. Of KOH in 20 ml. Of water and make the final volume up to 1 liter.
Using 95% alcohol
 Keep it for 24 hrs. and then filter it. Finally store it in bottle.
 0.5 M HCl solution.
 Phenolphthalein indicator
Procedure:
 25 ml. of 0.5 M KOH solution is taken in a conical flask. 2-4 drops of
phenolphthalein indicator is added. 0.5 M HCl is taken in burette.
 It is titrated against 0.5 M HCl solution. Note the titration value.
 Accurately weighted 2 gm. of oil is taken in 250-ml conical flask with round glass
joint.
 25 ml. of KOH solution. is added in it.
 Reflux condenser is attached on flask and the flask content is heated in a steam bath
for 25 minutes with occasional shaking.
 2-4 drops of phenolphthalein indicator is taken in flask while the solution is hot.
 In burette 0.5 M HCl solution is taken.
 Titration of final solution is done against 0.5 M HCl and the final value is reported.
 During titration color change from pink to colorless.
Observations:
 Weight of sample taken = W gm. =
 Vol. of HCl required for blank titration = x ml.=
 Vol. of HCl required for sample titration = y ml.=
 Normality of HCl solution = N1
Calculations:
1000 ml of 1N HCl = 1000 ml of 1 N KOH = 56 g of KOH
(x-y) ml of 1N HCl
=
56 * (x-y) * N1
__________
g of KOH
1000
Hence, Saponification value = (x-y) *N1*56
W
mg/g of sample
Result:
Saponification value for the given oil sample = ________mg / gm of oil.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Preparation Of Soap
Aim: To Study The Preparation Of Soap And Its Cost Analysis.
Theory:
 Soap - compounds are of the type RCOOM where, R.COO- Fatty acid radical
representing oleic, stearic, palmitic lauric and myristic acid.
 M - An alkali element such as Na or K.
 Soap is the mixture based on glyseride raw materials.
 The most commonly used oil or fats are Beef tallow, Coconut oil, Palm oil, Cotton
seed oil, Soyabean oil.
 It is two-step process:  Hydrolysis of oil
 Saponification
Reactions
(C17H35COO)3C3H5 + 3H2O
Glyceryl Stearate
Water
3C17H35COOH
Stearic acid
+ 3NaOH
Caustic
3C17H35COOH
Stearic acid
+ C3H5(OH)3
Glycerin
3C17H35COONa + 3H2O
Sod. Stearate
Water
 Methods of soap manufacturing process: 1. Batch saponification process
2. Acid hydrolysis of glycerides followed by alkali addition or direct saponification
using strong caustic in batch operation.
3. Continuous hydrolysis and saponification.
The main class of soap is toilet and industrial soaps. The types of bar soap are regular and
super fatted toilet soap, deodorant and anti microbial soaps, floating soap, transparent
marbleized and hard water soap.
Chemicals:
 Given oil sample
 Sodium hydroxide pellets
 Water
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Apparatus:





Weighing balance
50 ml. Beaker
Glass rod
Measuring cylinder 50 ml.
Hot plate
Procedure:




10 gm. of given oil sample is accurately weighed and is taken in beaker (50 ml.)
5 ml. of water is added in beaker.
3 gm. of Sodium hydroxide pellets is carefully weighed and is taken in to beaker.
After addition of sodium hydroxide the whole content is rigorously shaken till whole
mixture completely dissolved. At the same time reaction of hydrolysis and
saponification is initiated by the evolved heat of neutralization.
 After wards whole content is heated on hot plate till mixture is completely turned to
solid form.
 Solid soap is weighed and is noted down.
Observation:




Weight of oil taken x gm. =
Weight of sodium hydroxide taken
Volume of water taken z ml. =
Weight of soap formed a gm. =
Result:
Weight of soap =
gm.
y gm. =
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Preparation of Salicylic Acid
Aim: To Prepare Salicylic Acid From Methyl Salicylate.
Apparatus Required:







Round bottom flask
Heating mantle
Water reflux condenser
Thermometer
Water bath
Beakers
Measuring cylinder
Chemicals Required:
 Methyl salicylate
 Concentrated hydrochloric acid
 20 % w/w Sodium Hydroxide
Reaction
COOCH3
COONa
OH + NaOH
COOH
OH HCl
OH
-CH3OH
Methyl Salicylate
Sodium Salicylate
Salicylic Acid
OH
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Theory:
Salicylic acid is prepared from methyl salicylate. Methyl salicylate is reacted with
Sodium Hydroxide and finally is acidified with hydrochloric acid to convert into salicylic
acid.
Procedure:
 10 ml. of methyl salicylate and 10 ml. of w/w sodium hydroxide solutions are taken
in a small round bottom flask. Small pieces of glass or porcelain are also taken in the
flask to withstand over heating.
 Then water reflux condenser is joined to the round bottom flask. The whole mixture
in the round bottom flask is gently heated in water bath continuous reflux for about
30 min.
 After refluxing for 30 min. reflux condenser is removed and the flask is cooled. Then
the contents are transferred in to a beaker.
 Afterwards concentrated hydrochloric acid is added slowly with continuous stirring to
acidify the solution. Final condition is predicted by checking its pH using litmus
paper. The content is cooled under tap water. The cooled product is collected in the
paper is taken in glass funnel. The product is washed with water over this filter paper
and it is dried.
 The dried product is accurately weighed and is noted as final; product weight in the
observation table.
Observation:




Final weight of Salicylic acid dried =
gm.
Volume of Methyl Salicylate taken =
ml.
Density of Methyl Salicylate
= 1.184 gm/ml
Weight of Methyl Salicylate taken =
gm.
Calculation:
 Molecular weight of Methyl Salicylate = 152.15 gm/gmol
 Molecular weight of Salicylic Acid
= 138.12 gm/gmol
 Theoretical Yield is calculated as below from the reaction as
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Reaction
COOCH3
COONa
OH + NaOH
COOH
OH HCl
OH
OH
-CH3OH
Methyl Salicylate
Sodium Salicylate
Salicylic Acid
152.15 gm. of Methyl Salicylate is required to produce 138.12 gm. of Salicylic Acid.
 1.184 gm. of Methyl Salicylate is required to produce Salicylic acid
= (1.184 * 138.12) / 152.15
=
gm
= i.e. Theoretical Yield
 Practical Yield = Final weight dried Salicylic Acid =
gms.
 Percentage Yield =  Practical Yield / Theoretical Yield  * 100 =
Result:
Percentage yield of Salicylic Acid =
%
%
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Preparation of Phenylazo-2-Napthol
Aim: To prepare Phenylazo-2-Napthol
Theory:
 Azo compounds (ArN=NAr) are prepared by the interaction of a diazonium salt with
phenol in the present of Sodium Hydroxide, for example
C6H5NH2
NaNO2
C6H5N2Cl + C10H8O
HCl
Aniline
Diazonium
Chloride
2-napthol
Apparatus:








Round bottom flask
Heating mantle
Stirrer assembly
Thermometer
Water bath
Condenser
Beakers & Measuring cylinder
Ice
Chemicals:






Aniline
Hydrochloric acid
Sodium Nitrite
2-Napthol
Sodium hydroxide
Methylated spirit or methanol
NaOH
C6H5N=N (C10H8O) + HCl
Phenylazo-2-napthol
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Procedure:
Diazotization:
 Dissolve 5 gm of aniline in 60 ml of concentrated HCl and water (in equal proportion
to HCl) in a 250 ml beaker.
 Diazotize by the addition of 4 gm of Sodium Nitrate dissolved in 20 ml of distilled
water.
Coupling:
 Prepare a solution of 7.5 gms of 2-napthol in 45 ml of 10% NaOH solution. Cool the
solution to 50C by immersing it in ice bath assisted by direct addition of 50 gms of
ice.
 Stir the napthol solution vigorously and add the cold diazonium salt solution slowly
to it and a red color develops giving red crystals of phenyl azo-2-napthol, which
separates out very soon.
 When all the diazonium salt is added allow the mixture to cool in ice bath for about
30 min. with occasional stirring.
Isolation:
 Filter it through the funnel & wash well with water and drain thoroughly by pressing
the crystals with back of beaker. Wash the crystallized product with little alcohol and
dry upon filter paper.
Observation:
Final weight of the dry phenylazo-2-napthol obtained =
gms
Calculations:
Find the theoretical yield
NaNO2
C6H5NH2
C6H5N2Cl + C10H8O
HCl
Aniline
(93 gms)
Diazonium
Chloride
2-napthol
NaOH
C6H5N=N (C10H8O) + HCl
Phenylazo-2-napthol
(248 gms)
To produce 248 gms of phenylazo-2-napthol 93 gms of aniline is used. Therefore from 5
gms of aniline X gms of Phenylazo-2-napthol
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Theoretical yield = X gms = (5 * 248)/93 =
Practical yield obtained = Y gms =
 % Yield = (Practical yield / Theoretical yield)
= (Y/X) 100
Result:
The percentage yield of Phenylazo-2-Naphthol=_______%
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Roll No:
Practical No:
Iodine Value
Aim: To determine the iodine number of given oil sample
Theory:
 Oil is in liquid form due to its olefin instauration. Degree of instauration can be found
out by doing analysis of animal fat or oil. This degree of instauration is measured as
iodine number or bromine number.
 Iodine number is defined as the number of gm. of iodine, which combines, with 100
gm. of oil or fat. Bromine number is also defined in the same manner.
Apparatus:






500-ml. beaker
Measuring flask 1 ltr.
500-ml. Iodine flask
Burette 50 ml.
Pipette 25 ml.
Weighing balance with weight box
Chemicals:
Wij’s solution.
 Dissolve separately 7.9 gm. of A.R. Iodine Trichloride and 8.7 gm. resublimed iodine
in 250 ml. glacial acetic acid each, by warming in water bath.
 Mix the two solutions. and dilute to 1 ltr. With glacial acetic acid.
 Store the Wij’s solution. in a well-stopper amber bottle.
 It keeps for about a month.
Potassium Iodine solution. 15% w/w
 Dissolve 15 gm. of A.R. Potassium Iodine in 100 ml. of water.
Sodium Thiosulphate solution. 0.1 N
 Dissolve 25 gm. of A.R. sodium thiosulphate crystals (Na2S2O3, 5H2O) in one ltr. of
distilled water.
Starch powder solution.
 Make slurry of 0.1 gm. of soluble starch with 5-10 ml. of water and pour the
suspension with constant stirring into 100 ml. of boiling water.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
 Boil the mixture for 1 minute; allow cooling, after that adds 3 gm. of Potassium
Iodide. Store it in stoppered bottle.
Procedure:
For sample titration
 gm. of sample is taken in beaker. 20-25 ml. of chloroform or carbon tetrachloride is
also taken in beaker and is completely dissolved.
 Whole solution. is then transferred in a 500-ml. iodine flask. 25 ml Wij’s solution. is
added.
 Flask is stoppered and is shaken well.
 Flask is kept in dark for 30 minutes with occasional shaking.
 After that 20 ml. Of potassium iodine solution and 100 ml. Of water are added in it
and the mixture is thoroughly mixed.
 Burette is filled up with 0.1 N sodium thiosulphate solutions.
 Starch solution. is added and titration is completed in usual manner. Color turns from
blue to white. Note the titration value.
For Blank Titration
 25 ml. of Wij's solution. is also taken in it and whole mixture is kept in dark for 30
minutes with occasionally shaking.
 20 ml. of KI solution. is added along with the starch indicator and titration is done
against 0.1 N sodium thiosulphate as described above. Note the titration value.
Observations:




Weight of sample taken w gm.=
Normality of Sodium Thiosulphate solution. N1= N
Vol. of thiosulphate solution consumed during sample titration x ml.=
Vol. of thiosulphate solution consumed during blank titration y ml. =
Calculation:
1000 ml of 1N thiosulphate solution = 1000 ml of 1N I2 solution = 127 gm of I2
(y-x) ml of N1 thiosulphate solution = (y-x) * N1 * 127
____________
w * 1000
gm of I2
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Hence, Iodine number = (y-x) * N1 * 127 * 100
w * 1000
=
Result:
Iodine number of given oil sample =
Conclusion:
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Roll No:
Practical No:
Analysis Of Sulfa Drug
Aim: To find the purity of sulfa drug.
Theory:
 In medical line, to perform the analysis of various Sulfa drugs is of prime interest.
 There are many example of the sulfa drug such as Sulfa pyridine, Sulfa dyagin, Sulfa
thiazol and sulfa marazine.
 They have one characteristic to give insoluble precipitates with silver nitrate solution.
 Their purity is measured by dissolving it in the mixture of acetone and sodium acetate
with the use of potassium dichromate as indicator. Afterwards the dissolved mixture
is titrated against standardized silver nitrate solution.
 In other way, precipitation is done in more amount of silver nitrate solution to get the
silver salt. This silver salt is filtered and is dried. Its purity is found out based on
gravimetric analysis.
Apparatus:





Beaker 500 ml. and 1000 ml.
Conical flask 250 ml.
Measuring cylinder 100 ml. and 10 ml.
Burette & Pipette
Water bath
Chemicals:
 0.1 N Silver Nitrate solution
17 gm. Silver Nitrate is dissolved in 1 liter of distilled water.
 0.1 N Ammonium Thiocyanate solution
7.6 gm. Ammonium Thiocyanate is dissolved in 250 ml. of distilled water. Dilute
the solution up to 1-liter volume using distilled water.
 10% w/w Sodium acetate solution
20 gm. Sodium acetate is dissolved in 200 ml. distilled water.
 10% v/v Nitric Acid solution
20 ml. concentrated nitric acid is dissolved in 200 ml. distilled water.
 0.5% w/w Sodium Dichromate solution (indicator)
0.5 gm Sodium Dichromate is dissolved in 100 ml. of distilled water.
 10% w/w Ferric Ammonium Sulphate solution
10 gm Ferric Ammonium Sulphate is dissolved in 100 ml. of distilled water.
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
 Acetone
Procedure:
Sample titration
 0.2 gm. of sulpha medicine (e.g. Sulfa pyridine, Sulpha dyajol or Sulfa thiajol) is
accurately weighed.
 Accurately weighed sample is taken in 250 ml. of conical flask. 25 ml. of Acetone
and 20 ml. of 10% Sodium Acetate solution are taken in the same flask. Whole flask
content is shaken till it become uniform solution.
 Note: If required solution is heated to make completely uniform solution.
 1 ml. of 0.5% Sodium Dichromate solution (as indicator) is added.
 The whole solution of the flask is titrated against 0.1 N Silver Nitrate solution. At the
end point the yellow color of the solution is turned to permanent red color. Final
burette reading is noted as V1.
Blank titration
 25 ml. of Acetone and 20 ml. of 10% Sodium Acetate solution is taken in the 250 ml.
of conical flask. 1 ml. of Sodium Dichromate solution is added as indicator.
 Afterwards, the whole content is titrated against 0.1 N Silver Nitrate solution. Finally
the yellow color changed to permanent red color. This final end point is noted as V2.
Observations:





Burette reading for sample titration (V1) =
Burette reading for blank titration (V2) =
Normality of Silver Nitrate solution (N1) =
Molecular Weight of sulfa drug (M)
=
Weight of sulfa drug (W)
=
ml.
ml.
Calculations:
Purity of sulfa drug is found out using below equation,
Substitute the required values from the observations
Purity of Sulfa drug = [(V1 - V2) * N1 * M * 100]/ (W * 1000)
Result: Purity of Sulfa drug =_______ %
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Proximate analysis of Coal
Aim: To study the proximate analysis of given coal sample.
Theory:
 Coal is coming in various qualities. It is classified mainly on the basis of the fixed
carbon and its heating value.
 Coal is widely used from domestic purpose of heating to its various applications in
the industries like in power generation, in mfg. of organic chemicals.
 Coal is analyzed to its quality before coal is taken into use.
 Coal is analyzed in two ways.
 Proximate analysis
 Ultimate analysis
 Proximate analysis is the simplest way of analyzing the coal. The following contents
are found in analysis.
 Fixed Carbon
 Volatile Matter
 Moisture
 Ash (Mineral Matter)
 Ultimate analysis is the specific method of analyzing the coal. The following contents
are found out.
 Carbon
 Hydrogen
 Nitrogen
 Oxygen
 Sulphur
 Its Heating Value
Apparatus Required:







Muffle Furnace
200 mesh size sieve
Weighing Balance
Silica Crucible with air tight lid
Asbestos hand gloves
Desiccators
Pair of tongs
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Procedure:
 First small pieces of coal were crushed and are passed through 200 mesh size sieve.
 From the under flow of the sieve, accurately weighed 2 gm of sample in the crucible
and a lid is weighed and total weight is noted
 Moisture Content
 Crucible is kept in furnace and temperature in the furnace is raised up to 110 0 C. to
remove the moisture.
 Now the crucible is taken out carefully and is kept in the desiccators with CaCl2 to
cool down up to room temp. Then whole crucible is weighed again and weight is
noted down.
 The weighed crucible is kept again in the furnace.
 Volatile Matter
 Now, temp. in the furnace is raised up to 900 0 C. and temp. is kept constant for 7
minutes to remove the volatile matter.
 Crucible is taken out and is kept in the desiccators to cool down up to room temp.
Crucible is again weighed and note down the weight.
 Ash content
 Lid over the crucible is removed and is heated from 5000 C. to 815 0 C. for 1 hrs.
 Again the crucible is kept in the desiccators to cool down up to room temp.
 This crucible is weighed and weight is noted
Observations:






Weight of the empty crucible = a gm. =
Weight of a lid = b gm.=
Weight of the crucible with the sample = c gm. =
Weight of the crucible after heating up to 1100 C. = d gm. =
Weight of the crucible after heating up to 9000 C. e gm. =
Weight of the crucible after heating up to 8150 C. = f gm. =
Calculations:








Weight of crucible with sample and the lid = a+b+c gm. = w gm.
Weight of moisture gone out = (w-d) gm. =
Weight of the volatile matter gone out = (d-e) gm. =
Weight of the ash remaining after the final heating = f- (a+b) gm. =
Moisture fraction in the sample = (w-d)/c = x* 100 =
Volatile Matter fraction in the sample = (d-e)/c =y* 100 =
Ash fraction in the sample = (f- (a+b))/c = z* 100 =
Fixed carbon fraction in the sample = (1- (x+y+z))* 100 =
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Result:
Proximate analysis of the given coal sample:
Moisture percent =
Volatile Matter percent =
Ash percent =
Fixed Carbon percent =
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Hardness of Water
Aim:
To determine the hardness of given water sample.
Apparatus: Burette, pipette, conical flask, heater, measuring cylinder etc.
Chemicals: 0.01 N EDTA solution, EBT solution (Eriochrome Black 1), Buffer
solution, water.
Theory:
 One of the important chemicals used in chemical industries is water, which is used as
raw material & as utility also. So the quantity and quality of available water are
important.
 Groundwater is generally hard which may cause scale. Hard water is the water
containing objectionable amount of dissolved salts of calcium and magnesium. These
are usually present as bicarbonates, chlorides, sulfates & nitrates.
 Hardness of water can be divided in to two classes: Carbonate (temporary) and Noncarbonate (permanent). Temporary hardness is caused by bicarbonates of calcium and
magnesium & it can be reduced by heating. Permanent hardness is due to sulfates and
chlorides of calcium and magnesium, which can be reduced by chemical
agents.
Hardness is conventionally expressed in the units of mg/1 or ppm of CaCO3.
Procedure:
Part – A (Estimation of total hardness of given water sample)
 Fill the burette with 0.01 N EDTA solution.
 Take 25 ml of given water sample in the conical flask. Add 2 ml of buffer solution
and 2 drops of indicator, a dye, EBT.
 In the presence of hardness in water EBT gives wine red color at pH 10 and in
absence of hardness color is blue.
 Titrate the sample against 0.01 N EDTA solution till color changes from wine red to
light blue, which indicates the end point.
 EDTA will form stable complex ions with Ca & Mg.
PH = 10
Ca + Mg
+ EDTA
Ca EDTA + Mg EDTA
EBP
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Part – B (Estimation of permanent hardness of given water sample)
 Take 25 ml of water sample in to a conical flask and put it on to a heating mental, boil
gently for 10 minutes (Around 95oC).
 Cool it to room temperature and repeat the procedure of part A for titration.
 Calculate the temporary hardness of water by subtracting the permanent hardness
from the total hardness calculated in part A.
Observations:
Burette : 0.01 N EDTA solution
Pipette : 25 ml given water sample
Indicator : EBT
End point: Colour change from red to light blue
OBSERVATION TABLE:
Before Heating:
Sr.No.
Burette Reading
Final
Initial
After Heating:
Average
Reading
Difference
Sr.No.
Burette Reading
Final
Initial
Difference
Calculation:
 Total Hardness:
1 lit = 1000 ml 1 N EDTA = 1 mole of CaCO3
= 100 gm of CaCO3
V (B.R) ml 0.01 N EDTA = V ×0.01 × 100
= A gm CaCO3
1000
If 25 ml of hard water contain ‘A’ gm of CaCO3, therefore 1000 ml hard water sample
contain,
= A× 1000
25
Total Hardness of water = B.R × 1000 = ______________
25
Average
Reading
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
 Permanent Hardness:
Permanent Hardness of water = B.R × 1000 =
25
Result:
Permanent Hardness = _____________
Temporary Hardness= _____________
______________
Nirma University
Institute of Technology
Chemical Engineering Department
Lab Manual -Chemical Process Industries
Date:
Practical No:
Roll No:
Determination of Total Solids
Aim: Determine the total solids in given water sample.
Apparatus:
1.
2.
Usual glassware
Hot air oven
Theory:
 The sources refer to domestic water supply domestic & industrial wastes, soil erosion
and inflow infiltration.
 Total solids can be broadly classified as filterable and non-filterable solids. The
filterable solids are classified in to colloidal solids (10-3 to 10-6 mm) and dissolved
solids (<10-6 mm).
 Non filterable solids (suspend solids) having size more than 10-3 mm is classified in
to settable solids.
Procedure:




Take initial weight (W1) of empty dry container.
Take 25 ml sample of water / waste into this container.
Keep this container in Hot air oven at temperature of 103 – 105 oC for 24 hours.
After 24 hours, take final weight (W2) of container after taking it from hot air oven.
Calculations:
Total weight of solids present in 25 ml sample = W2 – W1
= ______ gms
Hence, total weight of solids present in 1 litre of sample = W2 – W1 x (1000 / 25)
= __________ gms.
Result: