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VPCOE
LAB MANUAL
OF
CHEMISTRY
(APPLIED SCIENCE II)
SECOND SEMESTER
FOR FIRST YEAR ENGINEERING DEGREE COURSES
Approved By HoD
Dr. A. P. Hiwarekar
Approved By Principal
Dr. S. B. Deosarkar
PREPARED BY
VPCOE
CONTENTS
Scope & Objectives
II
Safety rules
III
14
56
710
1114
1517
6. Analysis of mixture of phosphoric acid and hydrochloric acid using indicators and
pH meter.
1821
7. To determine moisture, volatile matter & ash content of a given sample of coal.
2225
Appendix
2627
References
28
Skills developed
28
Grid table
29
VPCOE
VPCOE
Burette
Pipette
Conical flask
Test-tube
Beaker
Desiccator
II
Measuring cylinder
Volumetric flask
VPCOE
SAFETY RULES
1) Keep your bags in the cupboards below the
working table
2) Keep your hands away from your face, while
working.
3) Wash your hands with soap while leaving
the lab.
4) Keep your working table neat and clean.
5) Read the procedure thoroughly
starting the experiment.
before
apparatus
and
chemicals
III
VPCOE
EXPERIMENT NO. 1
Aim: Determination of Alkalinity in given water sample by volumetric method.
Apparatus: Burette, Pipette, Conical flask, Dropper, measuring cylinder, Beaker etc.
Chemicals: 0.02 N HCl, phenolphthalein indicator & methyl orange indicator.
Theory: Pure water is neutral in nature with pH 7. Due to the presence of those minerals,
which increase the concentration of OH ions in water, the pH of water increases & it
becomes alkaline. These substances undergo dissociation or hydrolysis to form OH ions &
the total amount of such titrable bases in water expressed as equivalent of CaCO3 are
referred to as total alkalinity. Alkalinity is divisible into bicarbonate alkalinity, carbonate
alkalinity & in some cases hydroxide alkalinity. In most waters bicarbonates (HCO3-) and
carbonates (CO3=) are the major bases, but others can also be important under particular
conditions. Total alkalinity of natural waters may range from 5mg to several hundreds per
litre (as CaCO3). For biological purposes a total alkalinity over 40 mg of CaCO3/litre is
considered to indicate hard waters.
Alkalinity refers to the capability of water to neutralize acid. The presence of calcium
carbonate or other compounds such as magnesium carbonate contribute carbonate ions to
the alkalinity. Alkalinity is often related to hardness because the main source of alkalinity is
usually from carbonate rocks (limestone), which are mostly CaCO3. If CaCO3 actually
accounts for most of the alkalinity, hardness in CaCO3 is equal to alkalinity. Since hard water
contains metal carbonates (mostly CaCO3) it is high in alkalinity.
Environmental Impact: Alkalinity is important for aquatic life because it protects against rapid
pH changes. Aquatic life functions best in a pH range of 6.0 - 9.0. Higher alkalinity levels in
surface waters will buffer acid rain & other acid wastes & prevents pH changes that are harmful
to aquatic life.
Effect on boilers: If water having high alkalinity is used for steam generation in boilers, it will
lead to boiler troubles like caustic embrittlement, scale & sludge formation.
The above alkalinities can be determined volumetrically by titrating water sample against
standard acid using methyl orange and phenolphthalein indicators.
Detected by
Phenolphthalein Indicator
OH + H+
HCO3 + H+
CO3 2 + H+
HCO3 + H
VPCOE
Procedure:
Part A: Preparation of solutions
1) Standard 0.02 N HCl solution: Dilute 1.72 ml of concentrated AR grade hydrochloric acid
(11.6N) to 1 litre with distilled water in a volumetric flask.
2) Phenolphthalein indicator: Dissolve 500 mg of phenolphthalein in 50 ml ethanol & 50 ml
distilled water (100 ml 50%ethanol).
3) Methyl orange indicator: Dissolve 50 mg of methyl orange in 100 ml distilled water.
Part B: Determination of alkalinity
0 ml
V1 ml (phenolphthalein
end point)
V2 ml (Methyl orange
end point)
Reference table:
Alkalinity (ppm)
Relation between
Hydroxide
V1 & V2 / P & M
(OH )
(CO3 2 )
(HCO3 )
alkalinity
alkalinity
alkalinity
---------
--------
V1 = 0 / P = 0
V1 = V2 / P = M
Condition
If phenolphthalein end point is zero, then
alkalinity is due to only bicarbonate.
---------
-------
Carbonate Bicarbonate
2P
2( M P )
M
--------
-------
-------
VPCOE
V1 < V2 / P < M If phenolphthalein end point is less than half
the total titration, then alkalinity is due to
both carbonate & bicarbonate.
------2P
M 2P
Observations:
Readings (ml)
Sample No.
(Pink to Colourless)
Constant
Constant
1)
2)
3)
Calculations:
All kinds of alkalinity are expressed in terms of CaCO3 equivalents as parts per million.
1000 ml of 1N HCl 50 g of CaCO3
1 ml of 1N HCl
50 mg of CaCO3
= 2P = ______ ppm
VPCOE
4) Calculation for condition 4: water sample having both CO3 2 & OH alkalinity, V1 > V2
Phenolphthalein end point, V1 = _____ ml
Phenolphthalein alkalinity, P = 20 V1 ppm = ________ ppm
Methyl orange end point, V2 = _____ ml
Methyl orange alkalinity, M = 20 V2 ppm = ________ ppm
Alkalinity due to OH = 2P M = ___________________ =
Alkalinity due to CO3 2 = 2 ( M P ) = _________________ =
________
________
ppm
ppm
5) Calculation for condition 5: water sample having both CO3 2 & HCO3 alkalinity, V1 < V2
Phenolphthalein end point, V1 = _____ ml
Phenolphthalein alkalinity, P = 20 V1 ppm = ________ ppm
Methyl orange end point, V2 = _____ ml
Methyl orange alkalinity, M = 20 V2 ppm = ________ ppm
Alkalinity due to CO3 2 = 2P = ___________________ = ________ ppm
Alkalinity due to HCO3 = M 2P = ___________________ = ________ ppm
Result:
Water sample
Hydroxide (OH )
alkalinity, ppm
Carbonate (CO3 2 )
alkalinity, ppm
1)
2)
3)
Related Questions:
1) Define Alkalinity.
2) What are the types of alkalinities of water?
3) What are the pH transition ranges of the indicators used?
4) What are the ill effects of alkaline water on boilers?
Bicarbonate (HCO3 )
alkalinity, ppm
VPCOE
EXPERIMENT NO. 2
Aim: To determine chloride (Cl ) content of water sample by Mohrs method.
Apparatus: Measuring cylinder, conical flask, volumetric flask, burette, pipette, dropper, etc.
Chemicals: Standard 0.02N Silver nitrate solution & 5 % potassium chromate solution as
indicator.
Theory: Chlorides are present in water usually as NaCl, MgCl2 & CaCl2. Chlorides are not
harmful but their concentrations above 250 ppm impart a peculiar taste to the water thus
making the water unacceptable for drinking purposes. High concentration of chloride in a
water sample indicates pollution. MgCl2 & CaCl2 are responsible for permanent hardness of
water.
Mohrs method is used for the determination of chloride ions in water sample, which is neutral
or slightly alkaline. This method determines the chloride ion concentration of a solution by
titration with silver nitrate. As the silver nitrate solution is slowly added, a precipitate of silver
chloride forms.
Ag+(aq) + Cl (aq)
AgCl(s)
(White ppt)
The indicator used is dilute potassium chromate solution. When all the chloride ions have
reacted, any excess silver nitrate added will react with chromate ions to form a red-brown
precipitate of silver chromate. This procedure is known as Mohrs method.
2AgNO3(aq) + K2CrO4(aq)
Ag2CrO4(s) +
2KNO3
(Red-brown ppt)
The pH of the water sample should be between 7 - 8.5. At pH higher than 8.5, silver ions get
hydrated to form silver hydroxide. And at pH below 7 (acidic), potassium chromate is
converted to potassium dichromate.
Procedure:
Preparation of solutions:
1) Standard 0.02N silver nitrate solution: Dissolve exactly 3.3978g of dry solid AgNO3 in
distilled water & dilute it to 1 liter with distilled water in a volumetric flask, then store in a
brown bottle.
2) 5% Potassium chromate solution: Dissolve 5g of solid K2CrO4 in 100 ml distilled water.
Determination of chloride:
Back titration: Pipette out 50 ml of given water sample into a 250 ml conical flask & add 5
6 drops of potassium chromate as indicator. Now titrate this yellow coloured solution against
standard 0.02N silver nitrate solution taken in burette. Initially white precipitate of silver
chloride is formed which appears yellow due to the indicator. When all the chloride ions in
water sample gets precipitated then addition of an extra drop of silver nitrate forms a reddishbrown precipitate of silver chromate. Thus formation of reddish-brown precipitate indicates
the end point. Note down the burette reading & repeat the same titration for 2 more times.
Let the constant burette reading be X ml.
CHEMISTRY LAB MANUAL - II
VPCOE
Blank titration: A blank titration is also carried out as above with distilled water. In a 250 ml
conical flask pipette out 50 ml distilled water & add 5 6 drops of potassium chromate as
indicator. Now titrate it against standard 0.02N silver nitrate solution until the formation of
reddish-brown precipitate at the end point. Note down the burette reading & repeat the same
titration for 2 more times. Let the constant burette reading be Y ml.
Observations:
Blank titration
Reading in ml
II
III
II
III
Initial
Final
Difference
Back titration:
Reading in ml
Initial
Final
Difference
Calculations:
Volume of water sample taken for titration = 50ml.
Volume of 0.02 N silver nitrate that has reacted with the chloride ions = Y X = ____ = Z ml.
1 mole of AgNO3
1 mole of AgCl
1 mole of AgCl
1 mole of AgNO3
1000 ml 1N AgNO3
1 mole of Cl
1 mole of Cl
Z ml 0.02 N AgNO3
Weight of chloride ions
35.5 g of Cl
Z x 0.02 x 35.5 g of Cl
Z x 0.02 x 35.5
50
2)
Name the salts that contribute for the chloride content in water.
3)
4)
VPCOE
EXPERIMENT NO. 3
Aim: To determine temporary & permanent hardness of water sample by EDTA
method.
Apparatus: Burette, Pipette, Conical flask, Dropper, Beaker etc.
Chemicals: Ethylene diamine tetra acetic acid (EDTA) solution, zinc sulphate solution,
ammonia buffer of pH 10 & Eriochrome black-T indicator.
Theory: Hardness of water can be defined as the soap consuming capacity of water
resulting in the formation of white curdy PPT due to the presence of salts of Ca & Mg salts.
Ca/Mg + sodium stearate (C17H35COONa)
Salts
Soap
Ca (C17H35COO)2 / Mg(C17H35COO)2
Calcium/Magnesium stearate (curd)
Total hardness = It is due to the presence of all the salts of Ca & Mg.
= Temporary hardness + Permanent hardness
Temporary hardness: It is due to the presence of bicarbonates and soluble carbonates of
Ca & Mg. Also called as carbonate hardness & can be removed by boiling. Ca(HCO3)2,
Mg(HCO3)2, MgCO3.
Permanent hardness: It is due to the presence of sulphates, chlorides and nitrates of Ca &
Mg. Also called as non-carbonate hardness, which cannot be removed by boiling. It requires
lengthy treatment. CaCl2, MgCl2, CaSO4, MgSO4, Ca(NO3)2, Mg(NO3)2 etc.
For determining suitability of water for domestic and industrial purpose, type of hardness and
the amount of hardness is important. For the estimation of total hardness of a sample,
disodium salt of EDTA is used. Na2EDTA forms 1:1 complex with divalent metal ions like
Ca2+, Mg2+, Fe2+, Zn2+, etc.
NaOOCH2C
CH2COOH
N CH2 CH2 N
HOOCH2C
CH2COONa
Disodium-EDTA Structure
The anion of EDTA (H2Y4-) is a strong chelating agent, which forms a stable anionic complex
with divalent metal ions in basic medium.
Therefore alkaline buffer of NH4OH & NH4Cl of
pH-10 is used. In this complexometric titration, Eriochrome black -T is used as an indicator.
This indicator forms unstable wine red coloured complex with metal ions, which dissociates
on titration with EDTA solution. On dissociation, a strong metal ion- EDTA complex is formed
and indicator is set free which gives blue colour to the solution at the end.
VPCOE
M2+
HIn2
Metal ion
MIn
MIn
Indicator
Metal-Indicator complex
Blue
Wine red
H2Y4
MY2
HIn2
EDTA
Metalion-EDTA
Indicator
Ionic form
Complex
Blue
O
||
H+
C
O
||
C
O
CH2
CH2
N
CH2
Ca/Mg + EDTA
M = Ca / Mg
CH2
N
C
||
O
CH2
CH2
O
C
||
O
Soft
Below 50 ppm
Moderately hard
50-150 ppm
Hard
150-300 ppm
Very hard
H+
VPCOE
II
III
Initial
Final
Difference
M1V1 (ZnSO4) =
M2V2 (EDTA)
0.01 x 25
=
M2 x X
M2
= ( 001 x 25 ) /X
Molarity of EDTA = M2 = ______ M.
Part C: Total hardness of water sample:
Pipette out 50 ml of water sample in a conical flask, add 5ml of pH 10 buffer solution & then add 5
drops of Eriochrome black-T indicator. Titrate the wine red coloured solution against EDTA solution
taken in burette till the colour changes to blue at the end point. Repeat the same titration for 2 times
and note the constant burette reading as Y ml. Using this value calculate the total hardness of water
sample.
Observations and Calculations:
Reading in ml
II
Initial
Final
Difference
III
VPCOE
1 mole Ca2+/Mg2+
1 mole EDTA
100 g CaCO3
Thus 1000 ml 1M EDTA
100 g CaCO3
1ml 1M EDTA
1g CaCO3
1ml 0.01M EDTA
1mg CaCO3
Y ml M2 M EDTA
1 mole of CaCO3
( Y x M2 ) / 0.01 mg of CaCO3
_______ mg of CaCO3 = A
II
III
Initial
Final
Difference
1ml 0.01M EDTA
1mg CaCO3
P ml M2 M EDTA
(P x M2) / 0.01
mg of CaCO3
_______ mg of CaCO3
50 ml water sample contains B mg of CaCO3
= B
VPCOE
Result:
Determinations
Value
molar
ppm of CaCO3
ppm of CaCO3
ppm of CaCO3
VPCOE
EXPERIMENT NO. 4
Aim: Spectrophotometric / colorimetric estimation of ferrous ions (Fe2+) from the given
solution.
Apparatus: Spectrophotometer or colorimeter, 50 ml volumetric flasks, Beaker etc.
Chemicals: 0.25% ortho-phenanthroline solution, 10% hydroxylamine hydrochloride solution,
ammonium acetate buffer solution, 0.2% sodium acetate solution, concentrated HCl,
standard 0.1, 0.2, 0.3, 0.4 & 0.5 N iron solutions.
Theory: Colorimetry is the science of measuring colors. One useful and often used way of
determining the concentration of a chemical in a solution, if it has a color, is to measure the
intensity of the color and relate the intensity of the color to the concentration of the solution.
Several useful factors are very important.
The BeerLambert law, also known as Beer's law or LambertBeer law is an empirical
relationship that relates the absorption of light to the properties of the material through which
the light is traveling. It states that the optical absorbance of a chromophore in a transparent
solvent varies linearly with both the sample cell path length & the chromophore
concentration.
Absorbance is measured in a colorimeter or spectrophotometer by passing a collimated
beam of light at wavelength through a plane parallel slab of material that is normal to the
beam. For liquids, the sample is held in an optically flat, transparent container called a
cuvette. Absorbance (A) is calculated from the ratio of light energy passing through the
sample (I0) to the energy that is incident on the sample (I):
A = -log (I/I0)
Beer's Law follows:
A = bc
VPCOE
Fe2+ + 3phen
1,10-phenanthraline
(phen)3Fe(II)
A
(0,0)
CONCENTRATION, C (mg/ml)
VPCOE
Using the blank as a reference and any one of the iron solutions prepared above, measure
the absorbance at different wavelengths in the interval from 400 to 700 nm. Take reading
about 20 nm apart except in the region of maximum absorbance where intervals of 5 nm
should be used. Plot the absorbance vs. wavelength and connect the points to from a
smooth curve as shown in Fig-1. Select the proper wavelength to use for the determination of
iron with 1,10-phenanthroline. Also, calculate the molar absorption coefficient, , at the
wavelength of maximum absorption ( max) on the absorption curve (assume b = 1 cm).
Measure the absorbance of each of the standard solutions and the unknown at the selected
wavelength. Plot the absorbance vs. the concentration of the standards as shown in Fig-2.
Note whether Beer's law is obeyed. Using the absorbance of the unknown solution calculate
the % (w/w) iron in original solid sample.
Observations:
Serial No.
Volume of standard
Fe (II) solution
1.
5 ml
2.
10 ml
3.
15 ml
4.
20 ml
5.
25 ml
6.
Blank
7.
Unknown
Concentration In
mg/ml
Calculations:
Concentration of standard Fe solution = 0.01 mg/ml
Using C1V1 = C2V2, calculate the concentration of all solutions.
Now plot the graph of absorbance Vs. Concentration & from this standard graph, determine
the concentration of unknown Fe (II) solution as shown below:
A
B
S
O
R
B
A
N
C
Absorbance of
Unknown solution
A
Concentration of
Unknown solution
(0,0)
CONCENTRATION, C (mg/ml)
VPCOE
VPCOE
EXPERIMENT NO. 5
Aim: Study of corrosion of metals in medium of different pH.
Apparatus: Beakers, metal bars, pH meter, sand paper, weighing balance, etc.
Chemicals: Standard 2N hydrochloric acid and 2N sodium hydroxide (for preparing solutions
of different pH).
Theory: Corrosion is the primary means by which metals deteriorate or Corrosion is defined
as the destruction of metals through chemical or electrochemical reactions taking place at its
surface. Most metals corrode on contact with water (& moisture in the air), acids, bases,
salts, oils, aggressive metal polishes, and other solid & liquid chemicals. Metals will also
corrode when exposed to gaseous materials like acid vapors, formaldehyde, ammonia, and
sulfur containing gases.
Corrosion specifically refers to any process involving the
deterioration or degradation of metal components. The best example is that of the rusting of
iron/steel.
If a piece of metal is immersed in a polar solvent like water, some of the metal ions leave the
metal surface and go into the solution i.e., dissolution of metal starts. The metal continues to
dissolve, more and more electrons are left back and a net negative charge is built up in the
metal. Thus metal acquires a negative charge. The potential developed can be measured
under standard conditions using standard hydrogen electrode as a reference electrode. It is
called standard oxidation potential of metal. The metals having positive values are noble,
they do not dissolve readily (metals like gold, platinum, silver, etc.). The metals having
negative values of electrode potential are called active metals, which go into solution readily
(like iron, zinc, magnesium, etc.).
Metal
Gold (Au2+)
+ 1.498
2+
Platinum (Pt )
+ 1.18
Silver (Ag+)
+ 0.7996
2+
Copper (Cu )
+
Hydrogen (H )
2+
Iron ((Fe )
+ 0.3419
0
- 0.447
2+
Zinc (Zn )
- 0.7618
3+
Aluminium (Al )
- 1.662
2+
- 2.372
Magnesium (Mg )
This behaviour of metals depends upon the environmental conditions to which they are
exposed. It can be studied by immersing metal plates in the solutions of different pH for a
fixed or constant time.
pH = log [ H+ ]
VPCOE
Procedure: Take 5 metal plates (mild steel or zinc) of size 6cm x 2.5cm having same
thickness. Rub the metallic plates with sand paper to remove any corrosion product on it.
Weigh them separately and note down their respective weights.
Prepare solutions having different pH such as 1.5,
2.0, 3.0, 5.0 & 8.0 units by mixing standard 2N HCl
& 2N NaOH. Measure their pH using pH meter.
Take five 50 ml beakers, label them and take
about 30 ml above solutions in the beaker. Dip
the previously weighed metallic strips in the
beaker such that 4/5th portion is immersed in the
solution. Note down the time.
Beaker
Electrolyte solution
Metal plate
Corrosion assembly
After one hour take out the metallic plates from the
beaker, dry them in air and then weigh. Note
down the respective weights of the plates.
Observations:
Plate No.
pH of the
solution
1.
1.5 unit
2.
2.0 unit
3.
3.0 unit
4.
5.0 unit
5.
8.0 unit
Calculations:
After
Loss in weight
(In 1 hr)
Loss/gm/hr
Plate No. 1:
Plate No. 2:
Plate No. 3:
Plate No. 4:
Plate No. 5:
VPCOE
Result:
Conclusion:
Related Questions:
1) Define corrosion.
2) How does pH affects the rate of corrosion?
3) Name the series in which metals and their alloys are arranged according to their
anodic or cathodic nature.
VPCOE
EXPERIMENT NO. 6
Aim: Analysis of mixture of phosphoric acid and hydrochloric acid using indicators
and pH meter.
Apparatus: Burette, pipette, conical flask, burette stand, beaker, magnetic stirrer, pH-meter,
glass electrode, etc.
Chemicals: 0.1 N sodium hydroxide, standard buffer solution of Known pH and 3:1
phenolphthalein naphtholphthalein indicator mixture.
Theory: An acid or a base is quantitatively determined by titration using pH meter or acidbase indicators to detect the equivalence point/end point. pH-meter is frequently used
because the advantage that one actually monitors is the change in pH at the equivalence
point rather than just observing the colour change of a visual indicator. This eliminates any
indicator blank error.
The titration of a mixture of phosphoric acid and hydrochloric acid is complicated by the fact
that phosphoric acid is a triprotic acid with
Ka1 = 7.5x10-3, Ka2 = 6.2x10-8, and Ka3 = 4.8x10-13.
Ka1 is sufficiently large that the first proton from phosphoric acid cannot be differentiated from
strong acids like hydrochloric acid. The second dissociation of phosphoric acid is varies
significantly from the first. The second proton can be neutralized and differentiated from the
first phosphoric acid proton and the strong acid proton.
At the first equivalence point: pH = 4.7
H3PO4 (aq) + OH(aq)
H2PO4(aq) + H2O(l)
Neutralization of the third proton of phosphoric acid does not produce an appreciable break
in the titration curve. This is ultimately because Ka3 is very small and acids with small Ka' s
produce small breaks. Because Ka3 is so small, the basicity (proton accepting ability) of the
phosphate ion is large, and it undergoes hydrolysis producing hydroxide ion.
HPO42 (aq) + OH(aq)
Overall reaction: H3PO4 (aq) + 3OH(aq)
To express H+ ion concentration, pH scale is used. This pH can be measured directly using a
pH meter. pH = log H+ ion concentration Or pH = log [H+].
The titration curve for a mixture of phosphoric and hydrochloric acids are illustrated here.
The first break in the mixed acid curve indicates the amount of hydrochloric acid plus the
amount of the phosphoric acid. The amount of phosphoric acid in the sample is indicated by
the difference between first and second breaks in the titration curve. The first equivalence
point volume (25.0 mL) permits calculation of the total meq of HCl + (meq H3PO4)/3 since the
first proton of H3PO4 is neutralized.
VPCOE
ln [H+]
2.303 RT
E
log [H+]
F
2.303 RT
E
pH
F
Where -
E0
R
T
F
=
=
=
=
voltage that depends on the reactants and the products in the reaction.
Gas constant, 8.314 J mol-1 K-1
Absolute temperature in Kelvin.
Faraday, the charge on one mole of electrons (96485 coulombs).
1. Standard 0.1N sodium hydroxide solution: Weigh accurately 4 g of pure NaOH in a clean watch
glass and transfer it to a beaker. Dissolve it in distilled water and collect the washings of the watch
glass in the same beaker. Then transfer it to a 1liter volumetric flask & take washings of beaker
into the volumetric flask. Dilute this solution upto the mark with distilled water and make it
homogeneous.
2. 0.01% Methyl orange indicator: Weigh 0.01 g of solid methyl orange and dissolve it in 100ml
distilled water.
VPCOE
Standardisation of pH meter: Switch on the instrument by turning the control ON and set
the function switch to standard-by, STD BY position. Rinse the electrode pair with distilled
water and wipe them carefully with tissue or filter paper. Take the beaker containing
standard buffer solution of pH 7.00 and dip the electrodes in it. Set the function switch to the
pH position. Set the buffer value on digital display to read 7.00 by rotating the Standardise
knob. Put back the function switch to STD BY mode. Now without disturbing the
Standardise knob, complete all the pH measurements of titration.
Acid-Base titration using pH-meter: Pipette out 25ml of acid mixture (0.1N HCl + 0.05N
H3PO4) in a 100ml beaker. Rinse the glass electrode with distilled water and wipe it with
filter paper. Now dip the electrode in the beaker containing acid solution. Set the function
switch to pH mode and note down the pH of the solution displayed on the digital display of
pH meter. Fill the burette with standard 0.1N sodium hydroxide solution. Add 5 ml of NaOH
to the beaker containing acid solution and stir it using a magnetic stirrer. Note down the pH
of the solution. Similarly measure the pH of the reaction mixture after adding 10, 15, 20,
25,30,35,40 and 45 ml of NaOH from burette. Watch for the region where the pH begins to
change rapidly with each added portion of titrant. As the pH begins to change more rapidly,
add the titrant in smaller portions. When you have passed the equivalence point by several
ml, there is no reason to continue any further in the titration.
Then plot graphs of pH versus volume of NaOH added and pH/ml versus volume of
NaOH. From the graph, find out the end point of titration.
Acid-Base titration using indicator: Pipette out 25 ml of acid mixture (0.1N HCl + 0.05N
H3PO4) in a conical flask and add 2-3 drops of methyl orange indicator. Titrate this orange
red solution against standard 0.1N NaOH till the solution becomes yellow at the end point
(first).
After recording the burette reading, to the same flask add 2-3 drops of
phenolphthalein indicator and continue the titration till the solution turns pink at the end point
(second). Record the total burette reading. Repeat the titration and Compare the results
with the first method.
Observations: For pH-meter method
Volume of NaOH added, (ml)
05
10
15
20
22
24
26
28
30
35
40
45
50
CHEMISTRY LAB MANUAL - II
pH
pH
ml
pH / ml
VPCOE
Graph II (
ml Vs volume of NaOH)
(pH/
pH
ml
pH
(0,0)
ml of NaOH
ml of NaOH
From the graphs find out the end/equivalence points of the titration = ______ & _____ ml
Observations: For Indicator method
Reading in
ml
Readings (ml)
Methyl orange end point, V1 = M
(Colourless to Pink)
Constant
Initial
Final
Difference
End point of titration is = X = ______ & ______ ml
1)
2)
3)
4)
5)
1.1 x 5ml = C2 x 50
For 5 ml solution, C2 = (0.01 x
For 10 ml solution, C2 = (0.01 x
For 15 ml solution, C2 = (0.01 x
For 20 ml solution, C2 = (0.01 x
For 25 ml solution, C2 = (0.01 x
5) / 50 = 0.001
10) / 50 = 0.002
15) / 50 = 0.003
20) / 50 = 0.004
25) / 50 = 0.005
Result:
Related Questions:
1) What is the pH value at the first and the second equivalence point?
2) Why standard buffer solution of pH 7 is used?
3) Name the two indicators used in this titration.
4) How end point of titration is detected using pH meter?
CHEMISTRY LAB MANUAL - II
Constant
VPCOE
EXPERIMENT NO. 7
Aim: To determine moisture, volatile matter & ash content of a given sample of coal.
Apparatus: Silica crucible with vented lid, electric oven, Muffle furnace, spatula, desiccator,
pair of tongs, weighing balance, long legged tongs, etc.
Chemicals: Powdered coal sample.
Theory: Coal is a primary, solid, fossil fuel. Coal sample has to be analysed before using it
in any field/industry to find out its quality & suitability. Moisture, volatile matter & ash content
of coal are determined under proximate analysis. This method is simple & quick and is used
primarily to determine the suitability of coal for coking, power generation or for iron ore
smelting in the manufacture of steel. Coal comes in following main types or ranks: Peat,
lignite or brown coal, bituminous coal, anthracite & Graphite. Each type of coal has a certain
set of physical parameters which are mostly controlled by moisture, volatile content (in terms
of aliphatic or aromatic hydrocarbons) & carbon content. The carbon content is lowest in
peat and highest in anthracite.
Moisture
Moisture is an important property of coal, as all coals are mined wet. Groundwater and other
extraneous moisture is known as adventitious moisture and is readily evaporated. Moisture
held within the coal itself is known as inherent moisture & is analysed. Moisture reduces the
calorific value of coal and considerable amount of heat is wasted in evaporating it during
combustion. Moisture may occur in four possible forms within coal: Surface moisture,
Hydroscopic moisture, Decomposition moisture & Mineral moisture.
Total moisture is analysed by loss of mass of sample by Drying in air at 100 to 105 C (210 to
220 F) and relative loss of mass is determined. T otal moisture content of the coal should be
as low as possible.
Volatile matter
Volatile matter in coal refers to the components of coal, except for moisture, which are
liberated at high temperature in the absence of air. This is usually a mixture of short and long
chain hydrocarbons, aromatic hydrocarbons & some sulfur. Volatile matter of the coal is
related to the length of the flame, smoke formation & ignition characteristics. High volatile
matter coal gives long flame, high smoke & relatively low heating values. Volatile matter
content should be therefore as low as possible but minimum 20% is required for the ignition
of coal.
In Australian & British laboratories this involves heating the coal sample to 900 5 C (1650
10 F) for 7 minutes in a cylindrical silica cruci ble in a muffle furnace. American Standard
procedures involve heating to 950 25 C (1740 4 5 F) in a vertical platinum crucible.
Ash
Ash content of coal is the non-combustible residue left after coal is burnt. It represents the
bulk mineral matter after carbon, oxygen, sulfur and water (including from clays) has been
driven off during combustion. It consists of inorganic matter like silica, alumina, iron oxide,
lime, magnesia, etc. Ash reduces the heating value of coal, reduces air supply in furnaces
CHEMISTRY LAB MANUAL - II
VPCOE
and also requires labour (extra cost) for its regular disposal. Therefore ash content of coal
should be as low as possible. Analysis is fairly straightforward, with the coal thoroughly burnt
and the ash material expressed as a percentage of the original weight.
Fixed carbon
The fixed carbon content of the coal is the carbon found in the material which is left after
volatile materials are driven off. This differs from the ultimate carbon content of the coal
because some carbon is lost in hydrocarbons with the volatiles. More the fixed carbon
content, higher will be the calorific value of coal. Fixed carbon is determined by removing the
mass of volatile matter, moisture and ash determined by the above tests, from the original
mass of the coal sample.
Procedure:
A. Determination of Inherent Moisture: Transfer about 1g (known quantity) of powdered
air dried coal sample into a previously weighed silica crucible. Place the open crucible
with sample in an electric oven and heat it at about 105 110oC for an hour. Take out
the crucible after one hour from the oven and cool it in a desiccator (containing moisture
absorbing anhydrous calcium chloride). Then weigh the crucible with sample and repeat
the process of heating, cooling & weighing till constant weight is obtained. Calculate the
loss in weight.
B. Determination of Volatile matter: The dried sample of coal after determining moisture
content is closed with a vented lid. The closed crucible is then heated in a Muffle furnace
maintained at 925 20o C for exactly 7 minutes. The crucible is taken out from Muffle
furnace carefully with the help of long legged tongs. It is first cooled in air and then in a
desiccator. When the crucible attains room temperature it is weighed. Calculate the loss
in weight.
C. Determination of Ash: Transfer about 1g (known quantity) of powdered air dried coal
sample into a previously weighed silica crucible. Place the open crucible with sample in a
Muffle furnace maintained at 725 25o C for about 40 minutes or till constant weight is
obtained. Coal burns in open and the residue left is ash. Take out the crucible from
Muffle furnace carefully using long legged tongs. Cool the hot crucible first in air and then
in a disiccator. Weigh the crucible and find out the amount of unburnt residue left (ash).
D. Determination of Fixed Carbon: The percentage of fixed carbon is determined
indirectly by substrating the sum total of percentages of moisture, volatile matter and ash
from 100.
Observations and Calculations:
A. For Moisture:
1. Weight of empty crucible =
W1 = __________ g.
VPCOE
Weight of moisture
x 100 = W M x 100
Weight of coal (before heating)
W3
= _____ %
Observations and Calculations:
B. For Volatile matter:
1. Weight of empty crucible =
= _____ %
Observations and Calculations:
C. For Ash:
1. Weight of empty crucible =
W1
= __________ g.
Weight of Ash
Weight of coal (before heating)
x 100 =
WA
W3
= _____ %
D. For Fixed carbon (FC):
% Of Fixed Carbon = 100 (% Moisture + % Volatile matter + % Ash)
= 100 ( ________ )
= ______ %
x 100
VPCOE
Result:
The coal sample analysed contains: Moisture
= _______ %
= _______ %
Fixed Carbon
= _______ %
Conclusion:
Related Questions:
1) Define coal. What are the types of analysis of coal?
2) What is the temperature time limit of heating for volatile matter analysis?
3) For moisture content determination heating is carried out in which equipment?
4) What is the significance of proximate analysis of coal?
5) How does ash and fixed carbon affect the quality of coal?
VPCOE
APPENDIX
Table-I: pH Value (Refer Experiment No. 6)
Btu/lb
Anthracite
7762 - 8120
32,500 - 34,000
14,000 - 14,500
Bituminous coal
4060 - 5553
17,000 - 23,250
7,300 - 10,000
Charcoal
7069
29,600
12,800
Coal
3582 - 6448
15,000 - 27,000
8,000 - 14,000
Coke
6687 - 7404
28,000 - 31,000
12,000 - 13,500
Lignite
3893
16,300
7,000
Peat
3296 - 4896
13,800 - 20,500
5,500 - 8,800
Semi anthracite
6377 - 7762
26,700 - 32,500
11,500 - 14,000
Wood (dry)
3439 - 4155
14,400 - 17,400
6,200 - 7,500
VPCOE
Radiation /Rays
Wavelength range
Radio waves
3 x 10 5 cm
Micro eaves
30 cm
Far Infrared
0.01 cm
Near Infrared
1000 nm
Visible
400 750 nm
Red
750 nm
ii
Orange
650 nm
iii
Yellow
590 nm
iv
Green
530 nm
Blue
490 nm
vi
Indigo
420 nm
vii
Violet
400 nm
Ultraviolet
200 400 nm
Vacuum UV
200 5 nm
X - rays
5 - 0.01 nm
Gamma rays
0.01 - 0.0001 nm
Noble)
Cathodic
Gold
end
Platinum
VPCOE
REFERENCES:
1) Laboratory Manual on Engineering Chemistry, Sudharani (Dhanpat Rai Publishing
Company).
2) Vogels Textbook of Quantitative chemical analysis, J. Mendham et.al. (Pearson
Education).
3) Advanced Inorganic Analysis, Agarwal & Keemtilal, Pragati prakashan.
4) Chemical tables, Dr N. S. Gnanapragasam, (Sultan Chand & sons).
DEVELOPMENT OF SKILLS
This Lab Manual intends to develop the intellectual and motor skills of student. The skills
mentioned below will be developed through the experiments performed in this laboratory.
Intellectual Skills:
I-1 : To understand and identify the concepts.
I-2 : To Discriminate / Classify / Identify.
I-3 : To Investigate / Test / Verify properties or characteristics.
I-4 : To Interpret test results or numerical values.
I-5 : To locate faults.
I-6 : To plan and design.
Motor Skills:
M-1 : Skill to sketch the circuit diagram / block diagram / graph.
M-2 : Skill to select, handle and operate the equipment and reagents.
M-3 : Skill to measure the values / note down the observations.
M-4 : Skill to follow systematic procedure or sequence of operations step by step.
M-5 : Skill to observe the performance.
CHEMISTRY LAB MANUAL - II
VPCOE
In order to develop these skills for each experiment, important skills have been
identified. While performing the experiment, it is necessary to focus on such important
skills. Following table shows a grid of experiments and relevant skills.
GRID TABLE
No.
Intellectual skills
Motor skills
I1
I2
I3
I4
I5
I6
M1
M2
M3
M4
M5
Determination of Alkalinity in
given water sample by volumetric
method.
Spectrophotometric/colorimetric
estimation of ferrous ions (Fe2+)
from the given solution.