Chem File

PROFESSIONAL Chemistry Lab Manual
EXPERIMENT 1(A)
AIM: To determine temporary and permanent hsardness of water by using EDTA
titration method. You
are provided 1 ml of S.H.W. =1 mg of CaCO.
CHEMICALS REQUIREMENT: Hard water sample, EDTA solution, Buffer solution of NH,OH +
NH,C
having pH 10 +0.1.
INDICATOR: Eriochrome Black-T (Erio-T or EBT)
OH OH
Na0 -N=N
NO2
Sodium salt of Erichrome Black-T (represented as NaH,In)

END POINT: Color change from wine red to pure blue.
THEORY: Originally, water hardness may be defined as the measure ofthe capacity of
the water to precipitate
soap. Hard water is due to metal ions (minerals) such as Ca2t, Mg2*, Fe3t, so; and
HCO, that are dissolved
in the ground water. The determination of water hardness is a useful test that
provides a measure of quality of
water for households and industrial uses. Hard water does cause soap scum, clog
pipes and clog boilers.
There are two types of water hardness which are temporary hardness (due to the
bicarbonate ions (HCO) of
calcium and magnesium) and permanent hardness (due to the presence of the chiorides
and sulphates of calcium
and magnesium).
Complexometric Titration
The EDTA is a complexing or chelating agent used to capture the metal ions. This
causes the water to become
softened but the metal ions are not removed from the water. EDTA simply binds the
metal ions to it very tightly.
EDTA can form four or six bonds with a metal ion. In this method, total hardness is
determined by titrating a
known' volume of hard water, buffered to a pH -10 with NH,OH + NH4CI buffer, with a
standard solution of
disodium salt of ethylene diamine tetra acetic acid (Na, EDTA) in presence of
Erichrome Black-Tindicator (an
azo dye). Prolanged boiling of hard water followed by filtration and titration of
ihe filtrate against EDTA gives
permanent hardness. The diference in two hardness gives the temporary hardness of
water.
Erio-T indicator is an organic azo dye having two phenolic ionizable hydrogen
atoms. It has three different forms
depending on pH:
H, ,In pH> 6.3 HIn2 pH>11.5 In
Red Blue Yellowish Orange
When added to hard water at a pH 10 (maintaincd with ammonical buffer), it forms
unstable wine red
coloured complexes with bivalent metal ions (especially Mg ions) of water.
M'2 HIn2 pll=10 MIn H (Here; M = Ca", Mg")
(From waler) (Indicator) (Metal-EBTcomplexes)
Wine r

EDTAis taken in the form ofits disodium salt due to higher solubility in water. It
ionizes in aqueous solution to
give a strong chelating ion.
HOOCH,C... CHCOONa
Na0OCHC N-CH2-CH-N CHCOOH 2H,0
Disodium salt of EDTA (NazH2 Y)
Na,H,Y 2Na+ H,Y
Chelating ion
When added from burette to wine red solution, EDTA combines with free metal ions of
hard water to form their
respective soluble complexes. These are more stable than corresponding metal
indicator complexes.
M + H,Y2 MY2 2H
(From water) (EDTA) (Metal-EDTA complexes)
Colorless
When all free metal ions of hard water have complexed with EDTA, a slight excess of
EDTAremoves metal ions
from weak metal indicator complexes to form strong metal-EDTA complexes. This
releases the indicator in free
form which iš blue in colour. This makes the end point of titration i.e. color
change from wine red to pure blue.
MIn + H,Y2 My2 HIn2 2H
Metal-EBT complexes (Excess) Metal-EDTA complexes Free Indicator
(Less stable) (Colorless, Imore stable) (Blue)
PROCEDURE:
Step 1. Standardization of EDTA solution
Rinse and fill the burette with standard EDTA solution and note down its initial
reading. Transfer 10 ml of
given standard hard water (S.H.W.) sample in a conical flask. Add 1/3td test tube
(i.e. 5 ml) of buffer
solution and 3-4 drops of Erichrome Black-T indicator. Solution becomes wine red in
colour. Titrate this
solution against EDTA solution till wine red colour changes to pure blue. Note down
the final burette
reading. Repeat to get concordant readings. Let V, ml of EDTA used in this step.
Step 2. Determination of total hardness in sample
Transfer 10 ml of given hard water sanple in a conical flask. Add 1/3rd test tube
the final burette
Step 3. Determination of permanent hardness in sanıple
Transfer 100 ml of water sample in a 250 ml glass beaker. Boil it on burner flame
to near dryness. Cool
it slightly and add small amount of distilled water. Filter the solution into a 100
ml volumetric flask. Make
the volumec oftitrate 100 ml by adding more distilled water. Shake the solution
very well. Transfer 10 ml
of this solution in a conicat flask. Add 1/3d test tube (i.c. 5 ml) of buffer
solution and 3-4 drops of
Erichrome Black-T indicator. Solution becomes wine red in colour. Titrate this
solution against EDTA
solution till wine red colour changes to pure blue. Note down the volume of EDTA
used. Repeat to get
concordant readings. Let V, ml of EDTA used in this step

OBSERVATIONS:
Table 1: Standardization of EDTA Solution
S.No Initial Burette Reading Final Burette Reading Volume of EDTA Used (ml)
1. lo.O
2.
3. o.0 300
Concordant volùme =V, ml
Table 2: Total Hardness of Water Sample
S.No Initial Burette ReadingFinal Burette Reading Volume of EDTA Used (ml)
1. 3. 3.
2. 30 2-8
3. 60 30
Concordant volume =V, ml

Table 3: Permanent Hardness of Water Sample
1.
2.
3. .
Concordant volume = V, ml
GENERAL CALCULATIONS: 0Y
Volume of standard hard water (S.H.W.) taken for titration 10 ml
V ml of EDTA= 10 ml of S.H.W.
10 mg of CaCO3
10
1 ml of EDTA V, mg of CaCO3 (Given: 1 ml of S.H.W. = 1 mg of CaCO)
Volume of water sample taken for titration 10 ml
10 ml ofhard water = V, ml of EDTA
10
V,xmg of CaCO3
M
PROFESSIONAL 'Chemistry Lab Manual

I ml of hard water=xmg of CaCO3
10
1000 ml ofhard water = x1000 mg of CaCo
Total hardness = X ppm (say)

Step 3. Determination of permanent hardness in sample
Volume of boiled and filtered water sample taken for titration= 10 ml
10 ml of boiled, cooled & filtered water- V3 ml of EDTA
10
V,xmg of CaCO
I ml of boiled, cooled & filtered water = xmg of CaCO

10 V
1000 ml of boiled, cooled & filtered water 1000 mg of CaCO3

10 V
Permanent hardness= Y ppm (say)
Temporary hardness in water sample= Total hardness - Permanent hardness
= (X - Y) = Z ppm in terms of CaCO,
RESULTS: The given water sample contains
Permanent hardness =Y ppm (in terms of CaCo)
Temporary hardness =Z ppm (in terms of CaC0,)
PRECAUTIONS:
The same amount of indicator should be added each time.
2. To obtain sharp end point, magnesium ion (MgCl,) mnay be introduced to the EDTA
solution before its
standardization.
3 The reaction mixture should be briskly shaken during titration.
INSTRUCTIONS FOR PREPARING REAGENTS
1. Standard Hard Water (S.H.W.) (1 ml= 1 mg CaC0): Take 1 gm ofanhydrous CaCO,
(A.R. grade)
in a conical flask and add slowly a small amount of dilute hydrochloric acid into
it. Heat it gently upto
dryness (to remove CO,). Dissolve in distilled water and dilute to one litre.
2. Standard Disodium Ethylenediaminetetraacetate Dihydrate (Na, EDTA.2H,0) solution
(Formula
weight 372.2): Dissolve about 3.723 g of the salt in one litre of distilled water.
3. Water Sample: Dissolve about one gram each of MgCl, and CaC1, in a litre
ofordinary (i.e. tap) water.
4. Eriochrome Black T Indicator Solution (0.5% w/v): Dissolve 0.5 g of the dyestuff
in 100 ml of
absolute ethanol.
5. Ammonium Chloride-Ammonium Hydroxide Buffer Solution (pH = 10): Dissolve 7 g of
NH,CI
(A.R. Grade) in 57 ml of concentrated ammonia solution (Specific gravity = 0.88-
0.90). Stir and make
up the volume to one litre with distilled water.
PROFESSIONAL Chemistry Lab Manual EXPERIMENT 1
AIM: To determine calcium (Ca2*) and magnesium (Mg*") hardness separately in the
given wo
Sample by EDTA titration method. You are provided 1 ml of S.H.W. = 1 mg of CaCO, at
CHEMICALS REQUIREMENT: Hard water sample, EDTA solution, Buffer solution of NH,OH+N
having pH 10+0.1, Calcium precipitating buffer solution of (NH,),C,0,+ NH,OH + NH
CI.
INDICATOR: Eriochrome Black-T (Erio-T or EBT)
OH OH
Na0-S- -N=N
NO2
Sodium salt of Erichrome Black-T (represented as NaH, In)
END POINT: Color change from wine red to purc blue.
THEORY: Originally, water hardness may be defined as the measure of the capacity of
the water to precipita
soap. It arises due to presence of dissolved salts of Ca2*, Mg, Fest and some other
heavy metal ions in wat
Calcium hardness means all the hardness due to soluble calcium salts whereas the
hardness due to solu
magnesium salts is termed as magnesium hardness. It may be temporary or permanent.
EDTAmethod of hardness determination: It is a complexometric titration method. The
principle involves t
formation of 1:1 complexes of hadness causing metal ions ofwater with EDTA. The
total hardness (calciuman
magnesium hardness) is determined by titrating a known volume of water sample,
buffered to a pH ~10 wi
NH OH+NH CI buffer, with a standard solution of EDTA in presence of Erichrome
Black-T indicator (an a
dye).
Erio-T indicator is an organic azo dye having two phenolic ionizable hydrogen
atoms. It has three different form
depending on pH:
H,In pH>6.3 HIn2 pH>11.5 In

Red Bluc Yellowish Orange
When added to hard water at a pH~10 (maintained with ammonical buffer), it forms
unstable wine red
coloured complexes with bivalent metal ions (especially Mg" ions) of water.
M*2 + Hln pH=10 MIn + H (Here; M = Ca3, Mg"
(From. water) (Indicator) (Metal-EBT complexes)
Wine red
EDTA is taken in the form ofits disodium salt due to higher solubility in water. It
ionizes in aqueous solution
givea strong chelating ion.
HOOCHC CHCOONa
N-CH;-CH2-N. 2H,O
Na0OCHC CH2CO0DH
Disodium salt of EDTA (NazH2Y)

Na,H,Y 2Na + HY
Chelating ion
indicator complexes
M2 + H,Y2 MY2 2H
(From water) (EDTA) (Metal-EDTA complexes)
Colorless
EDTA removes metal ions
form which is blue in colour. This makes the end point of titration i.e. color
change from wine red to pure blue.
MIn H,Y2 MY? + HIn 2H
Mctal-EBT complexes (Excess) Metal-EDTA complexes Free Indicator
(Less stable) (Colorless, Imore stable) (ISluc)
After finding the total hardness of water sample, Ca2t ions in hard water can be
precipitated as calcium oxalate
by adding calcium precipitating buffer solution of (NH4),C,0,+ NH,OH +NH,CI.
Ca2 COO pH-10 COO Ca
COO CO0
(From hard water) (Oxalate ion) (Calcium Oxalate)
(white ppt)
The solution is filtered to remove white ppt. i.e. calcium hardness. Titration
offiltrate against standard EDTA
solution using EBT indicator gives magnesium hardness in water sample. From the
difference oftotal and magnesium
hardness, calcium hardness in sample is obtained.
Mg HIn Mgin H
(From hard water) (Indicator ) (Mg-Indicator complex)
Mg2 H,Y MgY2 H
(From hard water) (EDTA) (Mg-EDTA complex)
Mgln H,Y MgY HIn 2H
(Mg-EBT complex) (Excess) (Mg-EDTA compiex) (Free Indicator)
Less stable More stable Pure Blue
PROCEDURE:
reading. Transfer 20 ml of
given standard hard water (S.H.W.) sample in a conical tlask. Add 1/3 test tube
the final burette
reading. Repeat to get concordant readings. Let V, ml of EDTA uscd in this step.
Transfer 20 ml of given hard water sample in a conical flask. Add 1/3 test tube
the final burette
Step 3. Caions precipitation and determination of Mg* hardness in sample
Pipette out 100 ml ofwater sample in a 250 ml beaker. Add 25 ml of calcium
precipitating buffer solution
with constant stirring by glass rod. Allow the white ppt. to settle down for 20-30
minutes. Filter the
solution through a dry Whatman-42 filter paper in a dry flask. Transfer 25 ml of
this filtrate in a conical
PROFESSIONAL Chemistry Lab Manual 0

flask. Add 1/3rd test tube (i.e. 5 ml) of buffer solution and 3-4 drops of
Erichrome Black-T indiea
Solution becomes wine red in colour. Titrate this solution against BDTA solution
til wine red colo
changes to pure blue. Note down the volume of EDTA used. Repeat to get concordant
readings. Let v
ml of EDTA used in this step.
OBSERVATIONS:
Table 1:Standardization of EDTA Solution
S.No Initial Burette Reading Final Burette Reading Volume of EDTAUsed (ml)
1.
2.
3.
V 9.S Concordant volume = V, ml
S.No Initial Burette Reading Final Burette Reading Volume of EDTAUsed (ml)
1. :5 2S
2. 22
3. 2:7
V 21* Concordant volume = V, ml|

Table 3: Mg2* Hardness of Water Sample
2 S.NoInitial Burette Reading Final Burette Reading Volume of EDTA Used (ml)
1. S
3. 2S
GENERALCALCULATIONS: V 12s Concordant volume = V, ml

Volume of standard hard water (S.H. W.) taken for titration = 20 ml
V ml of EDTA = 20 ml of S.H.W.
20 mg of CaCO3
20
1 ml of EDTA = mg of CaCOg
V (Given: 1 ml of S.H.W. = 1 mg of CaCO,)
Step 2. Estimation of total hardness in sample
Volume of water sample taken for titration= 20 ml

20 ml of hard water V2 ml of EDTA
= V, xmg of CaCO
V, 20
1000 ml of hard water = 2xx 1000 mg of CaCO
20 V
Total hardness = X ppm (say)
Step 3. Estimation of Mg?* hardness in sammple
Volume of solution prepared 100 +25 125 ml
Hardness of 125 ml of prepared solution = Mg? hardness of 100 ml.hard water sample
20 ml filtrate= 100/125 x 20 = 16 ml of hard water
Concordant volume of EDTA solution used =V, ml
16 ml hard water = V, ml ofEDTA solution
20
= V,x mg of CaCcO
V
1000 ml hard water =xx1000 mg CacO

Magnesium hardness = Y ppm (say)
Ca2 hardness in water sample = Total hardness- Mg hardness

= (X - Y) ppm = Z ppm in terms of CaCOD,
Results: The given water sample contains
Ca hardness in water sample = Z ppm
Mg2 hardness in water sample= Y ppm
PRECAUTIONS:
1. The same amount of indicator should be added each time.
2 To obtain sharp end point, magnesium ion (MgCl,) may be introduced to the EDTA
solution before its
standardization.
3. The reaction mixture should be briskly shaken during titration.
1. Standard Hard Water (S.H.W.) (1 ml= 1 mg CaCO,): Take 1 gm ofanhydrous CaCO,
(A.R. grade)
2. Standard disodium ethylenediaminetetraacetate dihydrate (Na, EDTA.2H,0) solution
(Formula
weight= 372.2): Dissolve about 3.723 g of the salt in one litre of distilled water.
3. Water Sample: Dissolve about one gram cach of MgCl,and CaCI, in a litre
ofordinary (i.e. tap) water.
4. Eriochrome Black T Indicator Solution (0.5% w/v): Dissolve 0.5gofthe dyestuff in
100 ml of
absolute ethanol.

Ammonium Chloride-Ammonium Hydroxide Buffer Solution (pH=10): Dissolve 7 g of NH,C
(A.R. Grade) in 57 ml ofconcentrated ammonia solution (Specifie gravity=0.88-0.90).
Stir and
make the volume to one litre with distilled water.
6. Calcium Preipitating Bufer (pH = 8): Dissolve 6 g of ammonium oxalate i.e.
(NH,,C o, in about
100 ml of distilled water. Add 144 g ofNH CI(A.R. Grade), 13 ml of concentrated
ammonia solution
and make the volume to one litre with distilled water.
/EXPERIMENT 1(C)
AIM: To determine caleium (Ca*") and magnesium (Mg*) hardness separately in the
given water sample
by EDTAtitration method. You are provided 1 ml of EDTA=1 mg of CaC0,
CHEMICALREQUIREMENTS: Hard water sample, EDTA solution, Bufler solution of NH OH
+NH,CI
having pH 10+0.1, Diethyl amine.
INDICATORS: () Erichrome Black-T Indicator (Erio-T or EBT)
(i) Calcon or Solochrome dark blue
O OH QH OH OH
NaO-S N=N- NaO,S -N=N-
NO2
Sodium salt of Eriochrome Black - T Calcon
(represented as NaH,In)
END POINTS: (i) Color change from wine red to pure blue (with EBT)
i) Color change from pink to purple (with Calcon)
THEORY: Originally, water hardness maybe defined as the measure of the capacity of
the water to precipitate
soap. It arises due to presence of dissolved salts of CaT, Mg", Fe"" and some other
heavy metal ions in water.
Calcium hardness mcans all thc hardness duc to soluble calcium salts whereas the
hardness due to soluble
magnesium salts is termed as magnesium hardness. It may be temporary or permanent.
EDTAmethod of hardness determination: It is a complexometric titration method. The
principle involves the
formation of 1:1 complexes of hadness causing metal ions of water with EDTA. The
total hardness (calcium and
magnesium hardness) is determined by titrating a known volume of water sample,
buffered to a pH -10 with
NH OH+ NH,CI buffer, with a standard solution of EDTA in presence of Erichrome
Black-T indicator (an azo
dye).
Erio-T indicator is an organic azo dye having two phenolie ionizable hydrogen
atoms. It has three different forms
depending on pH:
A,In . pH> 6.3 HIn2 pH>11.5 In
Red Blue Yellowish Orange

When added to hard water ata pH -10 (maintained with ammonical buffer), it forms
unstable wine red
coloured complexes with bivalent metal ions (especially Mg2* ions) of water.
M2 HIn2 pH=10 MIn + H (Here; M = Ca", Mg)
(From water) (Indicator) (Metal-EBT complexes)
Wine red
EDTA is takcn in the form ofits disodium salt due to higher solubility in water. It
ionizes in aqucous solution to
givea strong chelating ion.
HOOCHC N-CH-CH-N CHCOONa .2H,O

Na0OCHc CHCOOH
Disodium salt of EDTA (NazH» Y)
Na,H,Y 2Na 2Na + H,Y2
Chelating ion
indicator complexes.
M*2 + H,Y MY 2H
(From water) (EDTA (Metal-EDTA complexes)
Colorless
EDTA removes metal ions
form which is blue in colour. This makes the end point of titration i.e. color
change fromn wine red to pure blue.
MIn +H,Y MY2 HIn2 + 2H

Metat-EBT complexes (Excess) Metal-EDTA complexes Free Indicator
(Less stable) (Colorless, more st:able) (Blue)
After finding the total hardness of water sample, Mg4T ions in hard water can be
suppressed as magnesium
hydroxide by adding diethyl amine which makes the pH of solution around 12.5.
Mg +20H pH=12.5 Mg(OH),
(From hard water)
Titration of solution against standard EDTA solution using Calcon indicator gives
calcium (Ca*) hardness in
water sampłe.
Ca + Calcon Ca-Calcon complex + H
(From hard water) (Indicator) (Light pink)
Ca-Calcon complex + H,Y CaY2 Calcon +2H
(Light pink. ess stable) (Excess) (Ca-FDTA complex, more stable) (Free Indicator,
Purple)
From the difference of total and calcium hardness, magnesium hardness in sample is
obtained.
PROCEDURE:
reading. Transfer 10ml of
given standard hard water (S.H.W.) sample in a conical flask. Add 1/3d test tube
(i.e. 5 ml) of buifer
SOuion and s-4 drops of Erichrome Black-T indicator. Solution becomes wine red in
colour. 1 itrate this
SOIution against EDTA solution till wine red colour changes to pure blue. Note down
the final burette
reading.Repeat to get concordant readings. Let V, ml of EDTA used in this step.
PROFESSIONAL Chemistry Lab Manua

Transfer 10 ml of given hard water sample in a conical flask. Add 1/5" test tube
(i.e. 5 ml) of bu
colour. Titrate th
the final buret
Step 3. Mg*ions suppression and determination of Ca2* hardness in sample
Pipette out 10 ml of water sample in a conical flask. Add 3-4 ml of diethyl amine
and 4-5 drops of calco
indicator. Solution becomes light pink in colour. Shake the solution thoroughly
for2 minutes. Titrate th
pink solution against EDTA solution till colour changes to purple. Note down the
volume of EDTA used
Repeat to get concordant readings. Let V, ml of EDTA used in this step.
OBSERVATIONS:
Table 1: Standardization of EDTA Solution
1.
2.
3.
Concordant volume = V, ml
S.No Initial Burette Reading Final Burette Reading Volume of EDTA used (ml)
1.
2.
3.
Concordant volume = V, mR
Table 3: Ca* Hardness of Water Sample
S.No Initial Burette Reading Final Burette Reading Volume of EDTA Used (ml) P
2.
Concordant volume = V, m
GENERALCALCULATIONS:
Volume of standard hard water (S.H. W.) taken for titration = 10 ml

V, ml of EDTA = 10 ml ofS.H.W.
= 10 mg.of CaCO
10
1 ml of EDTA = V mg of CaCOD3 (Given: 1 ml of S.H.W. = I mg of CaCO)

Volume of water sample taken for titration= 10 ml
10 ml of hard water = V, ml of EDTA
10
=V, mg of CaCO3
V
1000 ml of hard water x x1000 mg of CaCO

10 V,
Total hardness X ppm (say)
Step 3. Determination of Ca in sample
Volume of water sample taken for titration 10 ml
10 ml of diethylamine treated water = V ml of EDTA
10
= V, xmg of CaCO
V
1000 ml of diethylamine treated water 1000 mg of CaCO3

10 V,
Ca2t hardness = Y ppm (say)
Mg hardness in water sample = Total hardness - Ca" hardness

(X- Y) ppm= Z ppm in terms of CaCO,
Results: The given water sample contains
Mg hardness in water sample=Z ppm
Ca* hardness in water sample= Y ppm
PRECAUTIONS:
. The same amount of indicator should be added each time.
2. To obtain sharp end point, magnesium ion (MgCI.) may be introduced to the EDTA
solution before ts
standardization.
3. The reaction mixture should be briskly shaken during titration.
1. Standard Hard Water (S.H.W.) (1 ml= 1 mg CaCO,): Take 1 gm ofanhydrous CaCO,
(A.R. grade)
EXPERIMENT 2
AIM To determine the alkalinity of given water sample. You are provided N/20 H,SO.
CHEMICALS REQUIREMENT: Standard H,SO, (N/20) solution.
INDICATOR: () Phenolphthalein (ii) Methyl orange
O CH3
Na O-S N=N-
CH3
HO OH
END POINTS: (i) Disappearance ofpink colour (with Phenolphthalein).

(ii) Colour change from light yellow to reddish orange (with Methyl Orange).

THEORY: Alkalinity of water means the total amount of those substances in water
which cause an increase in
OH ion concentration due to dissociation in water or due to hydrolysis. Alkalinity
is mainly due to the presence
of hydroxide ions (OH), carbonate ions ( CO ) and bicarbonate ions (HCO;) present
in the given sample of
water. These ions may be present alone or in combination e.g.
) OH (i) Co only (i) HCO% only
(iv) OH+ co (v) CO +HCO
The possibility of OH and HCO existing together is ruled out since
OH +HCO co+H,O
The type and amount of alkalinity can be estimated by titrating a known volume of
water against standard acid
using phenolphthalein and methyl orange as indicator in same order. The
phenolphthalein end point (P) marks the
neutralization of OH and halfneutralization of CO to HCO ions. The sample is
further titrated with standard
acid in presence of methyl orange as indicator which neutralizes all HCO ions
whether present originally or
obtained from CO.The titration of water upto methyl orange end point (M) gives
total alkalinity of water. The
reactions involved are
) OH + H H,O P
i) CO + H HCO% M
(ii) HCO+ H' CO, + H,O
Phenolphthalein alkalinity (P) =OH + co
Methyl orange or total alkalinity (M)=OH + CO; + HCO

From the calculated values of P and M, following alkalinity corrections can be
made:
Alkalinity-(in ppm)
S.No. Case OH co HCO
1. P 0 0 0 M
P M P or M 0 0
3. P M 2 P or M 0
4. 2P M 2 (M - P)
5. PM 0 2P M-2P
PROCEDURE:
Rinse and fill the burette with standard acid and note down its initial reading.
Pipette out 10 ml of water
sample in a conical flask. Add 2-3 drops of phenolphthalein indicator. Solution
becomes pink in colour.

Titrate this solution against acid till the colour disappears. Note down the final
burette read
colourless solution so obtained, add2-3 drops ofmethyl orange indicator. The colour
of solt own the o fi
ion become
light yellow. Titrate it further against acid till the colour changes to reddish
orange. Note dou
burette reading again. Repeat to get concordant readings.
OBSERVATIONS:
Table: Titration of Water Sample against Standarised N/20 H,SO,
FBR with FBR Volume of acid used (ml)

S. No. 1BR(x)|Phenolphthalein with Methyl Upto Phenolphthalein Upto Methyli Orange
(y) Orange (2) end pointA=y-x end point B=zx
1.
2.
3.
Concordant volumc of acid used ypto phenolphthalcin end point A (y-x) ml

Concordant volume of acid used upto methyl orange end point B (z-x) ml
GENERAL CALCULATIONSS:
For Finding Phenolphthalein Alkalinity (P)
Concordant volume of acid used=A ml
Applying Normality Equation
N,V, NV,
(water) (Acid)
N, *10 N XA
20
A
N,200 N
20
Strength in terms of CaCO, = Normality x Equivalent wt. of CaCO,
A
- x 50 g/L
200
A
So phenolphthalein alkalinity (P) = x50 x 1000 mg/L
200
= 250A ppm
For Finding Methyl Orange Alkalinity (M)
Concordant volume of acid used=B ml
N,V, N,V,
(water) (Acid)
PROFESSIONAL Chèmistry Lab Manual 23
N, X10 N xB
20
B
N200 N
Strength in terms of Cacoj= Normality.x Equivalent wt. of CaCO,
B: x50 g/u
200
B
So methyl orange or total alkalinity (M)= 50x 1000 mg/L
200
250B ppm
Types of alkalinity:
Since P is related to M as... .. , the water sample contains the following
alkalinity:
(1). .. Alkalinity=. Ppn
(ii). . ... Alkalinity=... Ppn
RESULTS: Phenolphthalein alkalinity (P) =, .. ppmn
Methyl Orange alkalinity (M) =, ppmn
PRECAUTIONS:
1. All glass wares (burette, pipette and conical flask) should be rinsed with
distilled water.
2. After rinsing with distilled water, burette and pipette should be rinsed with
desired solution.
3. Funnel should be removed from the burette during titration.
4. The end point of the titration should be observed carefully.
1. N/20 H,SO,: Dilute 1.33ml of concentrated H,SO, to one litre with distilled
water.
2. Phenolphthalein Solution (2%%): Dissolve 1 gofphenolphthalein in 50 ml of
ethanol (i.e. rectified
spirit) and add 50 ml of distilled water. Shake well and filter if necessary.
3. Methyl Orange Solution (0.1%): Dissolve 0.1gofsodium salt of methyl orange in
100 ml ofhot water
and filter ifnecessary.
VIVA- VOCE).
Q.1. What is acidimetry?
Ans. Acidimetry is a method to determine the strength of an acid bytitrating
against a standard alkali solution.
Ans.
Q.2. What is alkalimetry?
Ans. Alkalimetry is a method to determine the strength of a base by titrating
against a standard acid solution
Ans.
using suitable indicator.
EXPERIMENT 3
AIM: To determine the amount of Dissolved Oxygen (D.0.) in the given water sample
by using
Winkler's lodometric method. You are provided N/80 Hypo solution.
CHEMICALS REQUIREMENT: 48% Manganous sulphate solution (Mns0), 10% alkaline
potasium iodide
solution (KI+ KOH), Conc. H,S0, N/80 Hypo solution (sodium thiosulphate, Na,S,O0).
INDICATOR: Freshly prepared starch solution (added near the end point).
END POINT: Disappearance of blue colour (Hypo in burette).
THEORY: Dissolved oxygen (D.O.) is the amount of dissolved oxygen in mg present per
litre of water. It
depends upon the following:
1. Higher the temp. ofwater lesser is its D.o.The solubility of oxygen in fresh
water varies from 14.5 ppm
at 0°C to about 7.5 ppm at 30°C under one atmospheric pressure.
2. Higher the atmospheric pressure, more.is its D.O.
3. Higher the conc. of salts in water, lesser is its D.O.
The amount of D.O. in water can be determined by Winkler's iodometric method. In
this method, D.O. of water
oxidizes Mn*to Mn* (manganic oxide) in alkaline medium. It is called D.O. fixation.
2Mn+0, +40H) 2Mn Q(OH)
Basic Manganic Oxide o
Hydrated Mangancse Oxide
Then Mn" (manganic oxide) on acidification releases nascent oxygen which oxiddzes
iodide ions I to iodine
1 in acidic medium.
Mn' O(OH), + H + 2 1, + Mn+3H,0
The liberated iodine is titrated against std. hypo solution using starch as an
indicator.
1, +2e 21
2S,0 >S,O +2c
I,+2S,0; 21 + S,O;
(thiosulphate ion) (tetrathionate ion)
The amount of hypo solution used in the titration is equivalent to the D.0. present
in given water sample.
Chemical Equations:
MnSO, 2KOH Mn(OH), + KSO,
2Mn(OH), 0 2MnO(OH),
Basic manganic oxide
(Brown ppt)
MnQ(OH), + HS0_ > MnS0, + H,O +[O]
2KI +H,SO, +[O] K,SO, + H,0 + 1
+2Na,S,O, 2Nal +QNa,S,O,
Sodiun thioşulphate Sodium tetrathionate
Starch + Blue colourcd complex

PROCEDURE:
Fill the D.0. bottle upto brim with given water avoiding air bubbles. Fit the
stopper on the mouth of bottle and to
this add I ml 48% manganous sulphate solution (MnSO) andl ml ofalkaline potassium
iodide solution by taking
precaution that tip of the burette should be inside water. Now fit the stopper on
the mouth of bottle and shake it
well for approx. 2-3 minutes. This is called D.O. fixation. Now place the bottle
undisturbed for 5-10 minutes till
brown colour ppt. settle down. Add 2 ml of conc. H,SO, by taking the same
precaution that tip of the burette
should be inside water. Fit the stopper again and shake it very well till.brown
colour ppt. dissolve. Transfer 100
ml of this brown solution to a conical flask. Rinse and fill the burette with N/80
Hypo solution and note down the
initial burette reading. Now titrate with hypo till brown colour changes tó pale
yellow. Add 2 ml starch indicator
so that colour becomes blue. Now further titrate with hypo till blue colour
disappears which is end point and
which is equal to the amount of D.O. (in ppm) in given water samiple. Repeat the
only titration procedure to get
concordant readings.
OBSERVATIONS:
Volume of solution taken for each titration= 100 ml
Table: Titration of Water Sample against N/80 Hypo Solution
S.No Initial Burette Reading Final Burette Reading Volume of N/80 Hypo Used (ml)
2.
3.
Concordant volume = V ml
GENERALCALCULATIONSS:
Volume ofhypo solution used in titration=V ml
N
Normality ofhypo solution= 80
N,V, N,V,
(water sample) (Hypo)
N
N, x100 80 xV
V
N,8000 N
Amount ofD.O. present in given water sample= Normality x Equivalent wt. of oxygen
V x 8 g/L
8000

V x8x 1000 mg/L
8000
= X ppm
Result: The amount of D.O. present in given water sample = X ppm
PRECAUTIONS:
1. For reducing the contact of the sample with air, the stopper of the bottle
should be removed only wh
the reagents is to be added.
2. The bubbles should be removed from the water sample otherwise oxygen of the
bubble wil take parti
the reaction and this will lead to higher result.
3. While adding the various reagents, the tip ofthe pipette should be dipped below
the surface of the liqu
4. While adding the reagents and replacing the stopper, the bottle should be placed
in a basin as some liqu
will always overflow.
1. Water Sample: Collect the sample of water from any water source (such as pond or
sewage out flo
etc.) and decant it. Filter if necessary.
2. Sodium Thiosulphate (Hypo0) Solution (N/80): Dissolve 3.l gofsodium thiosulphate
in one litred
distilled water.
Note: Standardisation of sodium thiosulphate can be carried out with standard
potassium dichromate
or potassium iodate.
3. Manganous Sulphate (48%) Solution: Dissolve 480 g of manganous sulphate in one
litre of distilld
water.
4 Alkaline Potassium Iodide Solution: Dissolve 7g potassium hydroxide (KOH) pellets
and 15 gof
potassium iodide (KI) in distilled water and dilute it to 100 ml.
5. Starch Solution (1%): Make a paste of I gofsoluble starch with cold distilled
water in a beaker
with the help ofa glass rod. Add 100 ml distilled water slowly along with constant
stiring. Boil the
contents for 4-5 minutes and then cool.
Ti) To be kept for many days, add 0.5 g of salicylic acid or few drops of
chloroform or formalin.
(i) Keep it in a stoppered bottled to avoid bacterial action.
(VIVA -VOCE)
Q.1. What is dissolved oxygen (D.O).
Ans. It is the molecular oxygen that is dissolved in water.
Q.2. How oxygen enters into the water body?
Ans. It gets there by i) diffusion from the surrounding air. i) aeration of water &
ii) product of photosyntne
Q.3. The minimum Dissolved Oxygen required for aquatic life in general is_
Ans. 4 ppm.
EXPERIMENT 4
AIM: To Determine the flash point and fire point of an oil by Pensky-Marten flash
point apparatus.
APPARATUS/CHEMICALS REQUIRED: Pensky-Marten's flash point apparatus, Match Box,
Thermometer
and Lubricating oil sample.
THEORY: Flash point is the lowest temperature at

which the lubricating oil gives offenough vapours that Piolot burmer
ignite for a moment when tiny flame is brought near it. /
Fire point is the lowest temperature at which the vapours Test
of the oil burn continuously for at least five seconds flame Shutter
when a tiny flame is brought near it. Generally the fire burner control
point of oil is 5 to 40°C higher than its flash point. A Opening Oil level
good lubricant should always have flash point at least pointer
above the working temperature. This ensures safety
against fire hazard during storage, transport and use of
lubricating oil. -Stitrer
Flash and fire point of lubricating oils, fucl oils, solvents, Air bath
solvent containing material and suspension of solids are
determined by using Pensky-Marten's apparatus. It Oil cup
Consists of three parts. An oil cup (Material=Brass;
Height=5.5cm; Diameter=5cm) is surrounded by air
bath. Lid of the cup is provided with four openings of
standard sizes, first opening is for stirrer, second is for Fig. Pensky-Marten's
amission of air, third is for thermometer and fourth is flash point apparatus
for introducing test flame.

The shuter is provided at the top of the cup. By moving the shutter, opening in the
lid opens and flame is dipnad
into this opening, bringing the flame over the oil surface. As the test flame is
introduced in the opening. it Pe.
extinguished, but when the test flame is returned to its original position, it is
automatically lightened by the pile
burner. Stove consists of air bath and top plate on which the flange of the cup
rest. The assembly has an electri
heater which heats it in a controlled manner.
PROCEDURE:
Clean and dry all parts of the apparatus with the help of suitable solvent e.g.
CCl, ether, petroleum spirit o
benzene and dry it to remove any traces of solvent. Fill the oil cup with the test
oil up to the marki. Fix the lids on
on
the top through which arc inserted a thermometer and a stirrer. Ensure that the
flame exposure device is fixed on
the top. The test flame is lighted and the oil is heated at the rate of5°C/per
minute. Keep stiring the oil in the oit
cup. When the temperature rises up to 15°C of the probable flash point, the test
flame is introduced into the oit
vapours by moving the shutter and observe for any flash (a combination of weak
sound and light). Repeat this
process at every one degree rise of temperature. When test flame produces a
distinct flash in the oil cup, the
temperature is noted down as flash point (say t,°C). The oil sample is further
heated at a rate of about 1°C/per
minute and application of test flame is done after every 1°C rise in temperature of
the oil .The temperature at
which oil ignites and continues to burn for 5 seconds is noted down as fire point
(say t,°C).
RESULTS:
The flash point of the given oil sample = t,
The fire point of the given oil sample = tC
PRECAUTIONS:
1. The apparatus should be thoroughly dried. There should be no trace of moisture
inside the cup.
2 Water from the oil is removed by filtering it through filter paper containing
Plaster of Paris.
. The thermometer bulb should dip into the oil sample.
4 Fill the sample of the lubricating oil up to the mark. There should be no oil on
the outer part of the cup.
5. Stirring of the oil should be stopped at the time of the application of test
flame.
6 Avoid breathing over the surface of the oil.
7. A fresh portion of the oil sample should be used. Further determination on the
same portion of the oil
shows a higher flash point.
(VIVA- VOCE)
Q.1. What is flash point and fire point?

Ans. Flash point: Flash point is the lowest temperature at which the lubricating
oil gives offenough vapours
that ignite for a moment when tiny flame is brought near it.
Fire point: Fire point is the lowest temperature at which the vapours of the oil
burn continuously for at
least five seconds when a tiny flame is brought near it.
Q.2. Write the names of different parts of Pensky Marten's apparatus.
Ans. )Oil cup (ii) Stirrer ii) Oil level pointer
(iv) Test plane burner (v)Pilot burner (vi) Shutter Control.
EXPERIMENT5
AIM: Determinatiou of viscosity of lubricant by Red Wood viscometer (No. 1 and No.
2.
REQUIREMENTS: Redwood viscometer (No. I and No. 2), Stop watch, Thermometer, Given
lubricating oil
and Distilled water.
THEORY: Viscosity is the property of a fluid that determines its resistance to

flow. It is an indicator of flow
ability of a lubricating oil; the lowest the viscosity, greater the flow ability.
It is mainly due to the forces of
cohesion between the molecules of lubricating oil. Absolute Viscosity may be
defined as "the tangential force
per unit area which is required to maintain a unit velocity gradient between two
parallel layers. It is denoted by
7 (eta). Its unit in CGS system is poise. Mathematically,
F
A dvldx
where F Force, A = area, dv/dx = velocity gradient
The absolute or dynamic viscosity of a lubricant is determined by measuring the
time of flow of the oil througha
capillary ofdefinite dimensions at uniform temperature.
Viscosity generally decreases with increase in temperature. The maintenance of
viscosity over the range of
temperature is called the viscosity Index (V.). Viscosity oflubricating oil is
inversely proportional to the temperature
Le. with increase of temperature, viscosity decreases. This is due to the decreasc
in intermolecular attraction. At
higher temperature, oil must have su fficient viscosity to carry loads. Hence
heavier oils are used at higher temperature

Similarly, light oils are used at low ambient temperature. Lubricating oils are
subjected to extreme pressure at the
interphase between gears and rolling element. At such higher pressure, viscosity of
lubricating oil increases
considerably.Viscosity helps in selecting good lubricating oil.
REDWOOD VISCOMETER: It is of two types
a) Redwood viscometer No.1-Universal b) Redwood viscometer No.2- Admiralty
Both the above viscometers are identical in principle, shape and mode of testing.
The essential differences between
the two are
Description Redwood Viscometer No. 1-Universal Redwood Viscometer No. 2-Admiralt

Dimensions of Length-10 mm, Diameter-1.62 mm | Length-5Omm, Diameter-3.8mm
orifice
Kohlrausch flask| Smaller mouth Wider mouth
Useful for Less viscous oil having flow time between More viscous oils having flow
time greater
30s-2000s e.g. Kerosene oil and mustard oil than 2000s e.g. Fuel oil, mobile oil
The rate of discharge of oil through RW, is nearly 10 tmes the discharge through
RW, So, The RW, receiving
flask has a wider mouth.
Redwood viscometer is divided into

three parts: Thermometers
1. Oil Cup (Material- Silver plated Stimer
brass; Height-90mm; Diameter-
46.5mm) Water bath Pointer
It holds the test sample of lubricating Metallic oil cu Stirrer blade
oil. The bottom of the cup is fitted with Oil Value rod
polished-agate discharge tube Heating tube Watcr Water Water tap
containing an orifice of specified for emptying
dimension water
2. Water Bath: Oil cup is surrounded Agate jet of 1.62
diameter and
by water bath for adjusting the A 10mm length
temperature 5Oml Kohlrausch flask.
3. Kohlrausch Flask: It receives the Fig. Redwood Viscometer, -Levell ing screw
oil from polished-agate discharge tube
PROCEDURE:
eect the appropriate viscometer, either Redwood viscometer No.l or 2 depending upon
the nature of lubricating
1. Clean the viscometer cup properly with the help of suitable-solvent e.g. CCI,
ether, petroleum spirit or
enzene and dry it to remove any traces of solvent. Level the viscometer with the
help of leveling screws. Fill the
outer bath with water. Place the ball valve on the jet to close it and pour the
test oil into the cup up to the tip of

indicator (pointer). Place a clean dry Kohlrausch flask immediately below and
directly in line with discharging i
Insert a clean thermometer and a stirrer in the cup and cover it with a lid. Adjust
the temperature of water bath
until the oil attains the desired temperature. Lift the ball valve with one hand
and start the stop watch with the
other hand. Allow the oil to flow till the flask is filled upto 50 mL mark. Stop
the stop watch when lower menisci
of the oil reaches the 50 ml mark on the neck of receiving flask and note down the
time of flow in secon
Repeat the experiment 3-4 times and record the readings. Report the mean value in
Redwood seconds al
mentioning the viscometer used and the test temperature.
OBSERVATIONS:
Table: For Time of Flow
Sr. No. Temperature ('C) Time of flow (RW seconds)
1.
2s . 3
s 2 Mean = M.s.
RESULT: 2.18
Viscosity of given lubricant oil is .RW, or RW, sec. 2 2
2
PRECAUTIONS:
1 The oil should be filtered thoroughly a muslin cloth to remove solid particles
that may clog the jet.
To remove the moisture, the oil sample should be filtered through lintless filter
paper.
3. The receiving flask should be placed in such a manner that the oil stream from
jet strikes the neck of
receiving flask and do not cause any foaming.
The ball valve should be replaced immediately to prevent the overflow of oil.
After each reading; the oil should be completely drained out of receiving flask.
(VIVA-VOCE)
Q.1. Define the term viscosity.
Ans. Viscosity is the property ofa fluid that determines its resistance to flow.
Q.2. What is the unit of viscosity?
Ans. In S.I. system Nm's and in C.G.S. system dyne s cm? or poise.
Q.3. What is the coefficient of viscosity?
Ans. The viscosity ofa liquid cannot be measured directly. Therefore, it is
measured indirectly asa coefficient
of viscosity (7). It is defined as the force in dynes/cm? which is required to
maintain a difference in
velocities ofI cm/sec between two parallel layers of a liquid kept lcm apart from
each other.
Q.4. What are the units coefficient of viscosity?
Ans. C.G.S, unit is poise or dyne.sec.cm, Other smaller units are centipoises(10
poise), millipoise(10
poise) and micropoise(10 poise).

Q.13. How is the viscosity index of a lubricating oil is improved?
Ans. VI of a lubricating oil is improved by adding hexanol or linear polymers like
polvisa
jisoburylene
polymethacrylates etc.
Q.14. What is meant by the term 'viscous static'?
Ans. Itis the state of a liquid when its viscosity does not change with change in
temperature
Q.15. How can a viscous static lubricant be prepared?
Ans. Sucha lubricant can be prepared by adding appropriate amount of a suitable
linear polymer V.I. impr
prove
Q.16. What is meant by all weather lubricants?
Ans. The lubricants with high viscosity index undrego only a small change in
viscosity with change in temperat
Such lubricants can therefore be used over wide range of temperature and are termed
as all weathe
lubricants.
Q.17. Does molecular structure play any role in viscosity?
Ans. Viscosity increases with increase in branching and molecular size because as
branching increasés, crog
inking between molecules increases during the flow of liquid. Therefore; small and
unbranched spherical
molecules move faster and have lower viscosity as in petrol, ether, kerosene etc.
Q.18. What is the relation between viscosity of a lubricating oil and time of flow?
Ans. Highly viscous oil takes more time to flow while less viscous oil takes less
time to flow.
Q.19. How viscosity of a substance is related to its density?
Ans. Viscosity is directly proportional to the density of a substance.
EXPERIMENT 6
AIM: To determine the strength of HCl solution by titrating it with NaOH solution
conductometrically.
APPARATUS/CHEMICALS REQUIREMENT: Conductivity meter, Conductivity cell, N/10 Sodium
hydroxide solution (NaOH), N/100 Hydrochloric acid solution, Distilled water.
THEORY: End point of a volumetric analysis can also be found by conductometric
titration which involves
measurement of conductance of a solution during titration. The basic principle
involved is that electrolytic
conductance varies during the course of titration as its depcnds upon the number of
ions in solution and their
mobilities. The end point is found from a plot of conductance values against volume
oftitrant added which gives
two lines intersecting each other. The point of intersection gives the end point
oftitration.
Titration of HCl vs NaOH (strong acid vs strong base) is studicd by titrating a
known volume of acid against
standard alkali and measuring conductance of solution at di ferent times. Initally,
the conductance is high as HCI
isa strong electrolyte and is highly ionized. On adding NaOH from burette, the
conductance decreases.
PROFESiONAL Chemistry Lad Manual

Itis because fast moving H ons of HClare neutralized and are replaced by 39
slow moving Na' ions.
H'+CI + Na' + OH Na +Cl +H,O End point
After complete neutralization, added NaOH increases the conductance of
solution due to addition of highly mobile hydroxyl ions so the conduçtivity is
minimumat cquivalence point. On plotting conductance vs volume of NaOH
added, a V-shaped graph is obtained. The point of intersection of two lines
gives end point. From volume of NaOH used at end point, the strength of
HCl solution can be determined. Volume of NaOH added (ml)
PROCEDURE:
In conductometric titrations, conductance of solution is measured with the help of
a conductivity meter in
following two steps:
Step 1. Calibration of conductivity meter

1. Switch on the instrument and wait for 2-3 minutes.
2. Connect the conductivity cell to the terminals provided at the back of
instrument.
3. Take distilled water (D.W.) in a 100 mL beaker and dip the conductivity cell in
it.
4. Set the temperature control knob at 25 °C.
5. Put the cell constant knob to the value of cell constant given on the cell.
6. Select the proper conductance range by putting the multiplier switch in proper
range.
7. Adjust calibration control knob to get the desired value of conductivity of D.
W.
8. The instrument is now calibrated and the calibration control knob should not be
disturbed till experiment is
complete.
Step 2. Titration of HCI solution vs N/10 NaOH solution

1. Pipette out 50 mL of given HCI solution in a 100 ml. beaker.
2. Take out the cell from distilled water and dip in the HCl solution.
3. Push the cal/ meas knob to meas position ifrequired.
4. Note down the conductance value of solution.
5. Add I mL of N/10 NaOH solution from burette. Stir thoroughly and note down the
conductance of solution
when it becomes stablc.
. Add NaOH solution in I mlL lots and note the corresponding conductance values
till the conductance value
becomes constant.
Plot a graph betwcen conductance (along Y-axis) and volume of added NaOH solution
(along X-axis).
. Find out the volume of NaOH solution used at end point from point of intersection
oftwo lines in the graph.
PROFESSIONAL ChemmlLab Manual
OBSERVATIONS:
Volume of HCl solution aaken - 50 mlL
Nomality of NaOH solation=N

10
Table: For Titration of HCI Solution vś NaOH Solution
Sr. No. Volume of NaOH added (mL) Observed conduttance (mho)

0.0
2. 1.0
3. 2.0
3.0
4.0
6. 5.0
7. 6.0
8. 7.0
9. 8.0
10. 9.0
10.0
12. 11.0
13. 12.0
14 13.0
15. 14.0
Say volume of NaOH used at end point (frot graph) = V mL
Applying Normality equation
N, V, = N, V
(HCI) (NaOH)
N, x 50 xV
10
V
N 500 N
Strength of HCl solution Normality x Equivalent weight ofHCI

V x 36.5 = "X gm/lt
500
RESULT:
Strength of given HCI solution conductometrically= X gm/lt
PROFESSiONAL Chemistry Lab Manual

PRECAUTIONS:
. The titrant used should be ten times stronger then uhe solution tobe titratediso
that the volume change of
latter is negligible on the addition of the former solution.
2 After successive addition of NaOH from the burette, the salution shdbld benixied
thoroughly.
3. Tip of the cell should be dipped completely in the solution.
After calibrating the instrument, calibration control knobshould notbe distutbed.
(VIVA- VOCE)
Q.1. Define conductance (C).
Ans. The ease of flow of electric current through a body isl called its
donductante. It is reciprocal to the
resistance. Mathematically; C= R
EXPERIMENT 7
AIM: To determine the amount of sodium and potassium ions in a given water sample
by flame
photometer.
APPARATUS/CHEMICALS REQUIRED: Digital flame photometer, Standard NaCl solution,
Standard KC
solution and Distilled water.
THEORY: Photoelectric flame photometry, a branch of atomic spectroscopy is used for
inorganic chemical
anaiysis for determining the concentration of certain metal ions such as sodium,
potassium, lithium, calcium,
Lesaum, etc. In flame photometry the species (metal ions) used in the spectrum
arein the form ofatoms.
he basis of flame photometric working is that, the species of alkali metals (Group
1) and alkaline earth metals
(Group II) metals are dissociated due to the thermal energy provided by the flame
source. Due to this therma
cxcitation, some of the atoms are excited to a higher energy level where they are
not stable. The absorbance of
ght due to the electrons excitation can be measured by using the direct absorption
techniques. The subsequent
los
Or energy will result in the movement of excited atoms to the low energy ground
state with emission of some
PROFESSIONAL Chdmistry bath Mahudbnual

radiations, whichi can beisualized in the visible region of the spectrum. The
absorbance of light d
electrons excitation can beuisasured by àsing the direct absorption techniques
while the emitting radiation in
is measured using the emissium-techhiques, (Fhe wavelength of emitted light is
specific for specific eleme
A simple flame photometen comsisesvöfthe iftöllowing basic components: ients.
1. Source of flame 2. Nëbblišerland mixing chamber 3.Optical system (optical
filter) 4. Photo deta.
The intensity ofthe light enitted tould bd déscribed by the Scheibe-Lomakin
equation: deteck
I =kxo* wherelure liteásityof emitted light, c=the concentration of the element, A
stant of
proportionality.
At the linear part of the dàlibrdtion ourve
Then, =kxc
That is the intensitysof emitted: lightijs directly related to the concentration of
the sample. The
flame emissions of the'alkali and alkaline carth metals in terms of the emission
wavelength and the characteristic
color produced by baçh element is shown in table.
Name of thé ttemènteit Emitted wavelenght range (nm) Observed colour of the flame
Potassium (K) : } 766 Violet
Lithium(Li) 670 Red
Calcium (Ca) 622 Orange
Sodium (Na) 589 Yellow
Barium (Ba) 554 Lime green
A schematic representation of flame photometer is shown in figure.
Flame
Burner
Monochromator & uP-Based Printer
Mixing Photodetector Electronics &
Chamber Control
Atomizer
Sample- Compressed/ Compressed/ LCD
Regulated Regulated Alpha Numerical

Air Supply Fuel Supply
Fig.A schematic Representation of Flame Photometer

PROCEDURE: 45
Step 1. Preparation of standard solutions:
1. A stock solution of sodium and potassium is prepared by dissolving 2.542 gm and
1.907 gm of pure and
dry NaCl and KCl respectively in one litre of distilled water. This solution is
referred to as stock solution.
2. Prenare three standard solutions. To prepare 10 ppm solution, dilute the stock
solution 100 times. In the
same way other solutions can be prepared by appropriate dilution.
Step2. Instructions for use of the digital flame photometer:
1. Switch on the instrument and then compressor.
2. Place a beaker of distilled water and insert the narrow draw tube into it to
allow water to pass through the
photometer.
3 Adjust the gas control to give a flame with a large central blue cone, then, with
water passing through the
instrument slowly close the gas control until several (ten) separate blue cones
just form.
4. Make SET-UP by selccting the mode i.c. high concentration/low concentration;
mention the name and
number of elements to be detected; decide the number of standards used for
reference i.e. two or thre,
mention the concentration of standards in the descending order and then save the
SET-UP.
5 Now run the SET-UP by aspirating the distilled water followed by first, second
and third standards.
6. Aspirate the unknown sample and note down the concentration.
7. Finally, run water through the instrument until the flame appears free of colour
again.
7.
Step 3. Switch off the instrument:
1. Turn offthe gas control and the mains gas supply
2 Wait for the flame to die out.
3. Turn off the compressor.
4. Switch off the electricity
RESULT: The concentration of unknown solution of sodium and potassium in the given
sample solutions are
.and.........ppm respectively
PRECAUTIONS:
1. Do not lean over the instrument while lighting the gas burner.
2. Once the instrument is ready for measurement, the photometer must have water
running through it at all
times when a salt solution is not being measured.
3. The rate of uptake is fast, so make sure there is always enough water in the
beaker.
(VIVA-VOCE
Q.1. What forms the basis of atomic spectroscopy?

Basis of atomic spectroscopy is the radiation emitted from the flames depends on
the characteristic
Ans.
element present in tbe flame.
EXPERIMENT 8(A)
AIM: To determine the total iron content (Fe" and Fe*") in an iron ore by internal
indicator method.
CHEMICALS REQUIREMENT: 5% Stannous chloride solution (SnCI), Saturated mercuric
chloride solution
gCL). Standard potassium dichromate solution (N/40), Conc. HCI.
INDICATOR: N-Phenylanthranilic acid (NPA)
coOH
-NH-CsHs
PROFESSIONAL Chenmistry Lab Manual

END POINT: Color change fromlight green to reddish violet (K,Cr,0, in burette)
THEORY: An iron ore solution isprepared by treating the ore with acid. It contains
both ferro sium dichrom
errous (Fe
ferric (Fe )ions. The amount of iron in ore can be estimated by its titration with
standard potassi.
solution in acidic medium.
For finding total iron, the ore solution is first reduced with slight excess of
stannous chloride in medino .
nedium acid
with conc. HCI.
Sn2 Sn+ 2e (oxidation)
2Fe +2e 2Fe2 (reduction)
Sn2+2Fe* Sn t* +2Fe2
Sn" left in excess is destroyed by adding saturated mercuric chloride solution in
one lot.
Sn2 Sn 2e
2Hg +2+2C1 Hg,Cl

Sn+2Hg +2C1 Sn Sn*" + Hg,Cl,
Silky white ppt
Total iron present as Fe2* in reducėd solution is titrated against dichromate

solution in acidic medium usingN
phenylanthranilic acid as internal indicator.
CrO+14H' +6e 2 Cr3" + 7H,O

[Fe Fe +e] x6
Cr0 +14 H' +Fe 2C" +6 Fe" +7H,0
At the end point when all the Fe* jons get oxidized by dichromate, an excess drop
of dichromate oxidizes the
indicator to form a violet red dyc.
COOH COOH HOOC
2 NH- [O] N= N- +4H+ 4e
Violet red dye
From the volume of dichromate solution used in titrătion, total iron in ore
solution can be calculated.
PROCEDURE:
Rinse and fill the burette with dichromate solution. Note initial burette reading.
Pipette out 10 mL of ore solution
in a conical flask. Add3 mL conc. HCl into it and boil on flame to get yellow
solution. Add 5% stannous chloride
solution dropwise till yellow color disappears. Add 2-3 drops in excess. Cool the
solution to room temperature

49
nder tap water. Add 3 mL saturatedHgCl, solution in one lot and shake well till
silky white ppt are obtained.
Add 7-8 dròps of indicator and titrate against 'dichromate solution till light
green color changes to violet red.
Note final burette reading. Repeat the titration to record concordant values.
OBSERVATIONS:
Tablet Titration of Reduced Ore Solution vs K,Cr,O, Solution
S.No nitial Burette Reading Final Burette Reading Volume of K,Cr,0, Used (ml)
1.
2.
3.
Concordant Volume = V mL
Volume of ore solution taken for titration= 10 mL
Concordant volume of KCrO, solution = V mL
Normality of K,Cr,0, solution N

40
N,V, = N, V,
(Ore) (KCrO)
N,x 10 V
40
V
N,an N
400
Strength of total iron in ore solution = Normality x Equivalent weight ofiron
V
400 x 56 A gm// = Ax 10 ppm
RESULT: The given iron ore solution contains... of total iron.
PRECAUTiONS:
I. SnC1, solution should be added in a drop wise manner in hot condition.
2. Only a very small excess of SnC1, solution should be added during the reduction
of Fe otherwise a
much larger amount of HgCl, will have to be added to remove it.
To prevent the formation of grey or black precipitate of elemental mercury, HgC1,
should be added in one
lot in cold condition.
on adding HgC1,, grey or black precipitate ofelemental Hg forms, the reduction
should be repeated
with a fresh solution.
1. Iron Ore Solution:
N/20 Mohr's Salt Solution: Dissolve 18.6 g of ferrous ammonium sulfate (FeSO,
(NH),SO,6H.O)
distilled water. Add 10 ml of concentrated H,SO, and make up the volume to one
litre.
N/20 Potassium Permanganate (KMnO) Solution: Dissolve 1.58 g of potassium
permanganatei
one litre of distilled water.
Add one litre ofN/20 KMnO, solution to 3 litres of N/20 Mohr's Salt solution to
obtain 3:1 mixture of
Fe and Fe* ions in the sample.
Note: Instead of mixing N/20 KMnO, solution, add 2.75 g FeCl, into N/20 Mohr's Salt
solution.
2. Stannous Chlo ride Solution (5%): Dissolve 50 g ofstannous chloride diehydrate
(SnC1,2H,0) in 10
mlof concentrated HCl and dilute it to one litre using distilled water.
3. Saturated Mercurie Chloride Solution: Dissolve 80 g of HgC, in one litre of hot
distilled water. Cool
it to room temperature and filter.
4. N/40 Potassium Dichromate Solution: Dissolve 1.225 g of potassium dichromate
(K,Cr,0,) in one
litre of distilled water.
5 N-Phenyl anthranilic acid: Dissolve 3.25 gN-Phenyl anthranilic acid in 0.1 %
solution of NaOH and
make upto 250 ml with distilled water.
EXPERIMENT 8B)
AIM: To determine the total iron content in an iron ore by external indicator
method.
CHEMICALS REQUIREMENT: 5% Stannous chloride solution (SnCI), Saturated'mercuric
chloride solution
(HgC1,), Standard potassium dichromate solution (N/40),Conc. HC1.
INDICATOR: Potassium ferricyanide i.e K,[Fe(CN) J
END PQINT: Non appearance ofbluish green color externally.
THEORY: An iron orè solution is prepared by treating the ore with acid. It contains
both ferrous (Fež*) and
ferric (Fe*) ions. The amount of ireni in ore can be estimated by its titration
with standard potassium dichromate
solution in acidic medium.
For finding total iron, the ore solution is first reduced with slight excess of
stannous chloride in medium acidified
with conc. HCI.
Sn2 Sn + 2e (oxidation)
2Fe +2e 2Fe (reduction)
Sn2 +2Fe Sn + 2Fe
Sn left in excess is destroyed by adding saturated mercuric chloride solution in

one lot.

Sn Sn +2c
2Hg +2e +2C1 Hg,Cl
Sn2 2Hg" +2C1 Sn" + Hg,Cl,
Silky white ppt
l iron present as Fe* in reduced solution is titrated against dichromate solution
in acidic medium using N-
phenylanthranilic acid as internal indicator.
Cr0 +14 H' +6e 2 Cr*+7H,O
Fe Fe +e] x6
Cr,0+14 H' +Fe 2 Cr +6 Fe" +7H,O
Potassium ferricyanide is used as an external indicator to find out end point
oftitration. It reacts with Fe* ions
of ore solution to give prussian blue colour.
K,[Fe(CN),Jl 3K" + [Fe(CN),F"
3Fe+2[Fe(CN),I Fe,[Ee(CN),]2
Ferto ferricyanide
(pnissian blue colour)
At end point, when all Fe* ions get oxidized to Fe*" ions, bluish green color does
not appear with indicator.
Fe +[Fe(CN),J. Fe [Fe(CN),]
(Colourless)
From the volume of K,Cr,0,used at end point, the amount of total iron in ore
solution can be calculated in the
form of ferrous ions.
PROCEDURE:
Step 1. Reduction of ore solution
Pipette out 10 mL of iron ore solution into a conical flask. Add 3 mL conc. HCl and
heat to boiling to get yellow
solution. Add 5% SnCl, solution dropwise with shaking till yellow color just,
disappears. Add 2-3 drops in
excess. Cool the solution to room temperature under tap water. Add 3 mL of
saturated HgCl, solution in one lot
and shake well till silky white ppt is formed.
Step 2. Titration of reduced solution vs K,Cr,0, solution
(a) For long range reading:
Fll the burette with standard K,Cr,O, after rinsing. Add5 mL dichromate solution
from burette in one lot. Shake
contents well. Take out a drop ofthis solution with a clean glass rod and mix it
with a drop ofindicator placed on
Clean tile and check for end point i.e. non appearance ofbluish green colour. Add
dichromate solution in 5 mL
ES and check for end point till it comes. Record the volume of dichromate uscd as
long range reading8
(6) For short range reading:
COuce the iron solution as above. Acidify it and add dichromate solution from
burette in 1 mL lots starting fřom
wer end of long range reading. After every addition check for the end point
externally.

(c) For decimal reading:
Reduce the iron ore. Add dichromate solution in 0.5 mL lots starting from lower end
of short range
reading till end point is obtained.
(d) For concordant reading:
Take three concordant readings with reduced iron ore solution.
OBSERVATIONS:
Long range reading =.. mL of K,Cr,0, solution
Short range reading = ..mL of K,Cr,0, solution
Decimal reading ...mL of K,Cr,0, solution
Table: Titration of Reduced Ore Solution vs K,Cr,O, Solution.
S.No Initial Burette Reading Final Burette Reading Volume ofK,Cr,O, Used (mL)
1.
2.
3.
Concordant Volume = V mL
Volume ofore solution taken for titration = 10 mL
Concordant volume ofK,Cr,O, solution = V mL
Normality of K,Cr,0, solution = 1/40 N
N, V, = N, V,
(Ore) (K,Cr,0,)
N, x 10 xV
40
V
N, 400 N
Strength of total iron in ore solution = Normality x Equivalent weight of iron
V x 56 A gm/l = Ax 10 ppm
400
RESULT: The given iron ore solution contains.. of total iron.
PRECAUTIONS:
1. The glazed tile should be perfectly dried to get good drops.
2. After cach testing, the glass rod should be washed with distilled water
otherwise some indicator solution
sticking to the tip of the glass rod will get transferred to the reaction mixture
and spoil it.

NSTRUCTIONS FOR PREPARING REAGENTS
INS
N/20 Mohr's Salt Solution: Dissolve 18.6 gofferrous ammonium sulfate (FeSO
(NH,)SO,6H,O) in
distilled water. Add 10 ml of concentrated H,SO, and make up the volume to one
litre
permanganate in
Add one litre of N/20 KMnO, solution to 3 litres of N/20 Mohr's Salt solution to
Fe and Fe" ions in the sample.
Note: Instead of mixing N/20 KMn0, solution, add 2.75 g FeC, into N/20 Mohr's Salt
solution.
2. Stannous Chloride Solution (5%): Dissolve 50 g ofstannous chloride diehydrate
(SnCI,2H,0) in 100
ml of concentrated HCIl and dilute it to one litre using distilled water
3. Saturated Mercuric Chloride Solution: Dissolve 80g ofHgC1, in one litre ofhot
distilled water. Cool
it to room temperature and filter.
4. N/40 Potassium Dichromate Solution: Dissolve 1.225 gof potassium dichromate
(K,Cr,0,) in one
litre of distilled water.
5. Potassium Ferricyanide Solution: Dissolve 0.25 gof potassium ferricyanide i.e.
K.[Fe(CN)] in 12 ml
of 0.1 N NaOH and dilute to 250 ml.
EXPERIMENT 8(C)
AIM: To determine the total iron( Fe and Fe*) in an iron ore by self indicator
method. You are
provided N/20 KMnO, solution.
APPARATUS/CHEMICALS REQUIREMENT: Burette, Pipette, Titration flask, 100 mL
Volumetric flask,
Test tube, Filter paper, Zinc dust, Ammonium thiocyanate or Potassium sulphocyanide
solution and Dil. H,SO
INDICATOR: KMnO, (self indicator)
END POINT: Appearance of permanent pink colour
HEORY: The iron ore solution contains both Fe2 and Fes" ions. KMnO, reacts only
with Fe" and not with
because Fe" cannot be further oxidized. For the determination of Fe" a known volume
of iron ore
SOlution is directly titrated against standard KMnO, in acidic medium (dil. H,SO,).
MnO+ 8H + 5e Mn+ 4H,0
[Fe Fe+e]x5
MnO + 5Fe+8H > Mn* + 5Fe +4H,O
. t OT fe can be calculated from the volume of KMnO, consumed. To determine the
total iron, all the
The amou
produce n ron ore solution is reduced to Fe2 by adding Zn dust and H,SO. Zinc
reacts with H,SO, to
produce nascent hydrogen.
PPOFESSIONAL Chemistry Lab Manual

Zn Zn* +2e
[H'+ H] x2
Zn +2H Zn +H,
The nascent hydrogen so produced reduces Fc" to Fe"
Fe+e Fe2
H H +e
Fe +H Fe+ H
To ensure the complete reduction of Fe" into Fe" , the solution is tested with KSCN
or NH SCN as an
external indicator which produces red blood colouration with Fe" ion. Ifblood red
colour comes, reduction i
not complete and more zinc dust is added.
Fe+SCN [Fe(SCN)"
Ferric thiocyanate
(Blood Red Colour)
After the complete reduction excess zinc is removed by filtration or by boiling
until the whole of zinc
dissolves. The solution is then diluted to a definite volume with distilled water.
A known volume of this solution is
then titrated with standard KMnO, in acidic medium till the appearance of light
pink colour as end point. The
total iron can be calculated from the volume of KMnO, consumed. The amount of Fe"
is determined by subtracting
the amount of Fe" from total iron.
Amount of Fe" = Amount of total iron - Amount of Fe
PROCEDURE:
Step 1. Determination of Fe"
Pipette out 10 mL of iron ore solution in a titrating flask. Add to it 1/3rd test
tube of dilute H,SO, and
titrate against N/20 KMnO, solution till the appearance of pink colour as end
point. Repeat the experiment to get
concordant reading.
Step 2. Determination of total iron
(a) Reduction of Fe": 'Pipette out 20 mL of iron ore solution in a titration flask.
Add pinch ofzinc dust and
two test tube of dil. H,So, to it. Warm the mixture slightly and allow the reaction
to continue with occasional
shaking. When the reaction ceases, take a drop of reaction mixture with the help
ofglass rod and touch it with the
drop of NH,SCN drop taken on a glazed tile. Appearance of blood red colour
indicates the incomplete reduction.
In such case add one more pinch of zinc dust to the reaction mixture and test it
again as above to see complete
reduction. Now boil the mixture, cool and filter in a 100 mL measuring flask. Make
up the volume of the flask up
to the mark by adding distilled water. Stopper the flask and make the solution
homogeneous by shaking the flask
up and down.
(b) Titration of reduced solution: Pipette out 20 mL of the filtrate in a titration
flask. Add 1/3d test tube of
dilute H,SO, to it and titrate against N/20 KMnO, solution till the appearance of
pink colour as end point.
Repeat the experiment to get concordant reading.
PROFESSIONAL Chemistry Lab. Manual 55

OBSERVATIONS:
Table 1.Titration of Iron Ore Solution Vs N/20 KMn0, Solution
s.No Initial Burette Reading | Final Burette Reading Volume ofN/20 KMnO, Used (ml)
S.No
1.
2.
3.
Concordant reading=V, mL
TABLE 2. Titration of Reduced Solution Vs N/20 KMn0, Solution
S.No Initial Burette Reading | Final Burette Reading Volume ofN/20 KMnO, Used (ml)
1.
2.
3.
Concordant reading = V, mL
Step 1. Determination of Fe
Volume of solution taken each time = 10 mL
Volume of KMnO, used = V, mL
Applying Normality Equation:
N,V, N,V
(Fe*) (KMn0,)
N,x 10 20 xV
V
N, =: 200
Strength = N, x Eq. wt. of iron =N, * 56 = A gm/l
Step 2. Determination of Total iron
00 mL filtrate = 20 mL original iron ore solution
20
40 mL filtrate= x20 4 mL original iron ore solution
20 mL filtrate = 100
N,V, N,V,
(Fe&Fe) (KMnO)
N, x 4 20 *
N 80 x V
Strength N, x 56 = B gm/l
RESULTS: Total Iron = B gm/l
Fe-A gm/l
Fe- (B-A) gm/l
PRECAUTIONS:
1. Before titrating the reduced iron ore solution, all the zinc dust should be
removed by filtration or by boiling
2. After the complete reduction of iron ore solution, it should be titrated as soon
as possible to prevent th
atmospheric oxidation of Fe2 to Fe*.
|INSTRUCTIONS FOR PREPARINGREAGENTs
N/20 Mohr's Salt Solution: Dissolve I8.6 gof ferrous ammonium sulfate (FesO,
(NH),SO,6H,)
distilled water. Add 10 ml of concentrated H,S0, and make up the volume to one
litre.
permanganate in
Add one litre of N/20 KMnO, solution to 3 litres of N/20 Mohr's Salt solution to
Fe2 and Fe" ions in the sample.
Note: Instead of mixing N/20 KMn0, solution, add 2.75 g FeC1, into N/20 Mohr's Salt
solution.
2. N/20 Potassium Permanganate (KMn0,) Solution: Dissolve 1.58 gofpotassium
perrnanganate in
3. Ammonium Thiocyanate Solution (10%): Dissolve 10 gofammonium thiocyanate
(NH,SCN) (A.R.
Grade) in 100 ml of distilled water.
4. Potassium Sulphocyanide Solution (10%): Dissolve 10gof ptassium sulphocyanide
(KSCN) (A.R.
Grade) in 100 ml of distilled water.
(VIVA- VOCE)
Q.1. What is the difference between an ore and mineral?
Ans. Mineral is the combined form of metal which occur in earth's crust or rocks.
Amineral from which metal can be
extracted by metallurgical operation is called ore. So, all ores are minerals but
all minerals are not ores.
Q.2. How is iron ore solution prepared?
Ans. ron ore solution is prepared by decomposing ore with HCl or H,SO,,The
following reactions will occur

59
EXPERIMENT9
ATM: Determinatfion of concentration of KMnO, solution spectrophotometrically.
PPARATUS/CHEMICALS REQUIREMENT: Spectrophotometer, Standard KMnO, solution and
Distilled
API
water.
THEORY: Spectrophotometry is a technique that uses the absorbance of light by an
analyte (the substance to
he analyzed) at a certain wavelength to determine the analyte concentration. UV/VIS
(ultra violet/visible)
snectrophotometry uses light in UV and visible part of the electromagnetic
spectrum. Light of this wavelength
is able to effect the excitation of electrons in the atomic or molecular ground
state to higher energy levels, giving
rise to an absorbance at wavelengths specific to each molecule.
The absorption of light in the visible and near ultraviolet regions by a solution
is govermed by Beer-Bouguer-
Lambert law, commonly called Beer's law.
Beer's law: The intensity ofbeam of monochromes in light decreases exponentially
with increase in the concentration
of absorbing species arithmetically. In quantitative analysis mainly concened with
solutions i.e. the effect of
concentration of the coloured constituent in solution depends upon the light
transmissioı or absorption.
Mathematically I=I eke
Lambert's law: The rate of decrease in the intensity of the incident light with the
thickness of the medium is directly
proportional to the intensity of the incident light.
Mathematically; I= I, e*
By combining both Beer's and Lambert's equations, we get (converting natural
logarithm to base 10)
Kct or I= I 10-K
or I/T =10Kct
On inversing both sides
=10Ket
Taking log on both sides
log I/I= Ke
The quantity log I,/I is called the absorbance (A) and it is cqual to the
reciprocal of the common logarithm of
transmittance (T).
A=log 1/11,
Therefore A= log I
T log I/I= KcT
A KcTT
BEER-LAMBERT'S LAW
wnen C" is in moles/, the constant is called molar absorptivity (or) molar
extinction coefficient (& )
Ifas 1on obeys Beer-Lambert law, then the plot ofA vs c is a straight line passing
through the origin. This is
A= ecT
dias calibration curve. The calibration curve is plotted by measuring the
absorbance of standard solution fo
know
Ent concentrations. From the calibration curve, concentration ofunknown solution
can be obtained.
+AF.-1-
T t t t
Reading
Light Entrance Mono Exit Coloured Photocell Reading
source slit chromator slit solution device
Fig. Schematic Representation of the Components of a Spectrophotometer
PROCEDURE:
Step 1. Instruction for the use of Instrument
Part A
(a) Connect the instrument to power supply. Switch on the instrument and ensure
that red light indicator
glows.
(b) Put instrument on the tungsten filament lamp by rotating the knob marked with
°T and 'D' so that the
visible light passes through the shutter.
(c) Adjust the dark current to zero with the shutter oflight closed.
(d) Adjust the wavelength knob to the required wavelength region on the scale.
Choose the position of
wavelength between 400-960 nm.
(e) Adjust the "zero set" knob so that monitor reads zero on transmittance (T)
scale and 100 on optical
density (O.D) suale.
Part B
(a) Open the lid of the cell compartment (i.e. sample housing) and insert a cuvette
containing blank solution
(distilled water). Close the lid so that it fits properly.
(b) Adjust the control knob so that monitor reads 100 on "T' scale or zero on 'D'
scale.
(c) Open the lid and remove the cuvette. Close the lid tightly again.
(d) Check zero on the monitor. Adjust zero ifdisturbed.
(e) Repeat again (as in Part A (¢) and Part B(d)) for zero and 100% transmittance.
Step 2. Determination of E,m
(a) Place the cuvette containing standard solution in the cell compartment and note
the reading.
(b) Change the wavelength by about 20 nm every time and note down the corresponding
optical densities.
Plot a graph between wavelength (along X-axis) and O.D.(along Y-axis). Determine
the value of &, by
extrapolation of curve towards X-axis.
Step 3. Determination of concentration of sample solution
(a) Fix the wavelength at Em pOsition.
(6) Prepare 20 mL solution ofKMnO, with concentration 0.2%, 0.5%, 1.0%, 1.5%, 2.0%,
2.5% and 3.0%
etc.
(c) Note down the optical density of cach solution prepared above.
(d) Plot the absorbance against concentration of solution to get a straight line.
(e) Now takea solution of unknown concentration of KMnO, and note down its optical
density. Find out the
concentration of unknown solution from the graph corresponding to absorbance of
this solution.
PROFESSIC Chemistry Lab Manual 51

OBSERVATIONS:
Table 1. Determination of Ema
max
S.No Wavelength (nm) Absorbance
1.
2.
3.
5.
1.
3.
Table 2. Verification of Beer's law
S.No Concentration of KMnO, solution Absorbance

1. 0.2
0.5
3. 1.0
4. 1.5
2.0
6. 2.5
7. 3.0
Unknown Solution
Absoreance o
uranewn solution
A max
Ccnenraticn f
unknown solution
Conc
RESULT: The concentration of given KMnO, solution spectrophotometrically is ..-ppm
Wavelength
ig.Plot between wavelength Fig. Plot between absorbance
and abserbance and concentration

PRECAUTIONS:
For preparing the standard ca libration curve, dilute solutions of unknown
concentrations should h
1. ld used
2. Cuvette should be cleaned properly with tissue paper and handled with great care
as it is very fragie
gile.
3. Should be carefully observed.
(VIVA- VOCE)
Q.1. What is spectroscopy?
Ans. Spectroscopy can be defined as the interaction between matter and
electromagnetic radiations. After
absorbing suitable radiation molecule undergo transition from lower energy level to
higher energy level
Q,2. What is a spectrophotometer?
Ans. It is an instrument u sed to measure absorbance or transmission of light
through a solution.
Q.3 Define a photometer.
Ans. It is an instrument that can measure the amount of light transmitted through a
sample.
Q.4 What is main difference between the spectrophotometer and the photometer?
Ans. The main difference between the two is the type of wavelength selector. In
photometer, the wavelength
selector is a filter while in the spectrophotometer, it is monochromator.
Q.5 What is the function of monochromator?
Ans. Itallows selection from the entire light spectrum.
PROFESsIONAL Chemistry Lab Manual

EXPERIMENT
AIM: To determine the viscosity coefficient of the given liquid by using Ostwald's
Viscometer,
APPARATUS: Ostwald's viscometer, Thermostat or Water bath, Stop watch, Thermometer
etc.
THEORY: Viscosity is a property ofa liquid which resists its flow. For example,
glycerine does not flow as ea
easily
as methanol or ethanol. Thus, glycerine is said to have more viscosity than
methanol or ethanol. The coefficeint
eint of
viscosity is defined as the force required per unit area to maintain unit
difference of velocity between two paral
layers of liquid one centimeter part.' Ilftwo layers that are dx cm apart have a
difference of velocity ofdv em. se
', then the force F, acting per sq. cm. can be given by: sec
dv
F dx
where 7coefficient of viscosity and is expressed in dynes/cm.
Ostwald's Viscometer Method: This methdod is based on the Poiseuille's equation.
According to Poiseuilles
law, the rate of flow ofliquid through a capillary tube having viscosity
coefficient 7 can be given as:
n=" P where: D= volume of liquid, t = flow time through capillary,
8lu r=radius of the capillary,l = length of the capillary and p=hydrostatic
pressure
The apparatus used, known as Ostwald's viscometer, is shown in Fig. It consists of
two bulbs A and B connected
through a fine capillary tube. The bulb A is ofbigger size whereas the bulb B is of
smaller size. A known volume
of liquid is taken in the bulb A and the liquid is sucked into the bulb B.The time
taker in seconds for the liquid to
flow from the mark a to mark b is noted down.
Since the hydrostatic pressure of the liquid is given by P= pPgh (whereh is the
height of the column and pis the
density of the liquid:
nc Pt or 7apght
If 7, and7, are the viscosity coefficients of the liquids under study; p, p,
their densities and , and 1, are their times of flow of equal volume of
liquids through the same capillary then
Pgh and P8ht, a B
Hence; P22 b
The flow time for the liquid and water are determined in a Ostwald Viscometer.
Knowing the densities of the liquid and water and also knowing the viscosity
coetficient of water, viscosity coefficient of liquid can be calculated. Ift, andt
are the times taken by the liquid and water to flow from mark a to mark b,
respectively, we have
P
P Fig. Ostwald Viscometer
OROFESSIONAL Chemistry Lab Manual

PROCEDURE: 65
Clean and dry the viscometer thoroughly.
2 Introduce a definite volume of distilled water into the bulb A and kep it in
thermostat or water bath for
10-15 minutes so that contents acquire the room temperature.
3. Suck the water from bulb A through the capillary into the smaller bulb B.
Now bring the water to touch the mark a and hold it there by placing your finger at
the top of the narrow
limb.
5. Remove your finger and start the stop watch.
6. Stop as soon as water touhces the mark b.
1. Repeat this process 3-4 times and take the mean value.
8. Now dry the viscometer and fill it with the same volume ofthe test liquid and
keep it also in the thermostat
for 10-15 minutes, so that the liquid attains the room temperature.
9. Note the time during the flow of the liquid between the marks a and b.
10. Repeat the process 3-4 times and take the mcan value.
11. Get densities of both the liquids at the temperature of the water bath.
OBSERVATIONS:
Temeperature of measurement C
Density of water at t "C, d (From table)
Viscosity of water at tC, 7. (From table)
Flow Time Readings:
Liquid Time of flow in seconds

2 Average
Benzene
Water
Mass of the empty weighting bottle = m, g

Mass of the weighing bottle+ 10 ml benzene= m,
Mass of the weighing bottle+ 10 ml water m,g
Cani the viscometer: The cleaning of the viscometer is of utmost importance. All
greasy matiter should be removed from the
COme at there is no obstruction to the flow of the hquid. For cean ing fill chromic
acid solution (K,CrD,+ Conc. HS0) into the
wash i nd allow it to stand ina warm place for abou halfan hour or more. Then wash
it througły by running water through it. Finalh
a stilled water, alcohol and ether or acetone. Drain the extra liquid and then dry
it by passimg a cuhrent ofdust free air fom
loyer or nitrogen fr
from a gas holder or by sucking air through the iscometer using a water pump.

CALCULATIONS:
P m-m
Relative viscosity of benzene= P A
Absolute viscosity of benzene = 7 7 P.

P
Absolute value of viscosity of benzene at t 'C= ... Pas (From Appendix Table)
PRECAUTIONS:
1. As the viscosity of the liquid changes by I to 2 percent for each degree change
in temperature, te
experiment should be carried out at a constant temperature by suspending the
viscometer with the liqui
in a thermostat. Before measuring the flow time, the liquid should be allowed to
acquire the temperatur
of the bath. This takes about 10 minutes.
Exactly the same volume of liquids should be taken for viscosity measurements.
The volume of liquid taken in bulb A should be so much that when sucked through
capillary, it should fll
the bulb B and the U-bend at the bottom of the viscometer is full ofliquid.
The position, which can be reproduced repeatedly, is the vertical position. So
viscometer should be
clamped vertically.
CVIVA-VOCE
Q.1. Define viscosity.
Ans. Internal friction or resistance which resists the flow of the liquid is known
as viscosity.
Ans.
Q.2. Define coefficient of viscosity.
Ans. It may be defined as the force required to maintain a velocity difference of
unity between two layers of the
fluid unit distance apart and having unit area of contact.
Q.3. Define fluidity (¢).
Ans. Fluidity iş the case with which a liquid can flow. Mathematically; It is the
reciprocal of coefficient of
viscosity (7).
Fluidity (o)=
Q4. What is the unit of viscosity?
Ans. Poise (P). (1 Poise = 1 dynes s cm*)
Q.5. What do you mean by 1 Poise (P)?
Ans. When a force of dyne maintains a velocity difference of1 cm/sec between two
layers of a liquid I cm
apart and having an area of contact of I sq cm then the velocity of the liquid is
said to be 1 Poise.
EXPERIMENT 11
AIM: To determine the refractive index of given organic liquid using Abbe's
refractometer.
REQUIREMENTS: Abbe's refractometer, Temperature controller, Light source, Pure
sample of the given
liquid, Small quantity of rectified spirit and Distilled water.
THEORY: The refractive index (n) ofa sbstance is the ratio of the velocity oflight
in vacuum to its velocity in the
substance. Refraction occurs if the refractive indexes of the two media are
different and ifthe angle of incidence
is not zero. Liquids, gases and solids whose properites are identical in all
directions (cubic crystals) can be
characterised with a single refractive index; such substances are isotropic.
Crystals whose properties depend
upon the relative orientation of the light beam and the crystal axis pòssess more
than one refractive index. Such
anisotropic crystals may have two or three refractive indexes, one for each
optically different crystal axis. The
refractive indexes ofliquids fall in the range 1.3-1.7. Refractive index depends
upon the temperature as well as
the wavelength of light used. Generally, the D-line of sodium is used for standard
measurenements.

Refractive indices of liquids can be measured directly by means of an 69
festru ment known as refractomcter. Onc such refractometer is Abbe's
instru ment
ractometer as shown in figure. The refractive index of liquid is
n Veniently determined with an Abbe refractometer. In the Abbe Telescope
fractometer, the telescope is stationary and the prism is moved, but the Scale
fect is identical with that described. The angle through which the prism
effect is identic
mlst be moved to centre to the critical boundary in the field of view
mus Magnifying
corresponds to the critical angle of refraction. The Abbe refractometer Glass
Compensating Prism
ces white light, which produces a critical boundary with a rainbow like Arm R
appeamace becuase the different wavelengths of the light are refracted to
appearnac Water Jacket
slightly different extents (i.c. dispersion cffect). To eliminate the color band
Prism, P - Prism, R
and sharpen the boundary, an auxiliary optical system is incorporated that
is cabable of refracting the dispersed critical rays by exactly the same
amount that they originally diverged from the D line critical ray. This optical
"Compensator" thus sharpens the boundary and yiclds a critical ray with Mimor
white light that is equivalent to the ray that would be obtained with the Fig.
Abbe's refractometer
sodium D line. The refractive index measured with the Abbe refractometer
therefore isnp
Sample
Glass
Hemisphere
(a) (b) (c)

dtlaa
Fig.(a) The view into a refractometer when the /44
index knob is out of adjustment. (b) The view
into a refractometer when properly adjusted. (c)
The' view when the chromatic adjustemnt is Fig. Principle ofoperation ofthe Abbe
refractomerer
incorrect.
Table: Refractive indices of some liquids at 293 K for D-sodium line.
Liquid Refractive Index Liquid Refractive Index

Methyl alcohol 1.3289 Benzene 1.5005
Acetone 1.3585 Toluene 1.4950
Water 1.3330 Aniline 1.5859
Ethyl acetate 1.3725 Ethyl alcohol 1.3611
Ethylene glycol 1.4314 Cyclohexanol 1.4663
PROFESSIONAL Chemistry Lob Manual

PROCEDURE:
Step 1-Calibration with Water:
1. Set up the refractometer with the mirror facing away from you.
2 Position an ordinary tungesten light above the mirror.
3. Connect the constant temperature water bath (ifavailable) to the refractometer.
Adjust the angle ofte
telescope until you can look into it with comfort.
Unclamp the lower prism and swing itdown.
5. With a soft tissue moistened with alcohol, cleanse the faces of the upper and
lower prisms. (The uper
prism is the refracting prism; the lower one serves to hold the sample in place and
to transmit light to the
on Support it. the lower prism in an approximately horizontal position and place 2
or 3 drops of distilled wate
sample). Allow the prisms to air-dry.
6.
1. Siwing the prism to its closed position and clamp it firmly in place.
8. Permit the sample to stand for several minutes so it may reach temperature
equilibrium. Read the
temperature ofthe circulating water (ifused) or of the air in the vicinity of the
refractometer.
9. Move the arm along the curved scale until the critical boundary comes into the
view within the telescope
eyepicce.
10. When the boundary has been located, adjust the compensator knob on the barrel
of the telescope until
the boundary becomes colorles and sharp.
11. Then with the fine adjustment contorl on the long arm, bring the critical
boundary into exact coincidence
with the cross hairs.
12. Read the refractive index on the curved scale, sighting through the eyepiece on
the arm. The refractive
index is read to four decimal places, the final place being estimated.
13. Immediately after a measurement has been made, clean the prism faces with
ethanol and allow them to
dry
Step 2 -Measurement of Refractive Indexes: Using the same proceudre as in the
calibration with water,
measure the refractive indexes of four pure liquids. Compare your values with
literaure values.
OBSERVATIONS:
Organic liquid Wavelength of light used a Refractive index (n) at particular

temperature
Water
Benzene
Toluene
Ethanol
Referactive index of the material 'n' for given temperature is.
RESULTS: Refractive index of the given liquid sample at a particular trempratue
is..
PROFESsIONAL Chemistry Lab Manual

PRECUATIONS:
1. Take particúlar care not to scratch the faces of the prisms.
2. Always adjust the mirror to reflect the maximum light into the prism box.
3. Be careful not to allow the liquid to flow down.
A Ifthe liquid volatilises, introduce it through the groove provided in the prism
box.
VIVA-VOCE
Q1. Define refractive index.

Ans. The refractive index (n) ofa substance is the ratio of the velocity of light
travelling in air to the velocity of
Ans.
light moving in the liquid. Mathematically;
n=. velocity of light in the air

velocity of light in the liquid
Sini sine of the angle of incidence
Sinr sine of the angle of refraction
Q2. Define refraction.
Ans. The bending ofa light ray on passing from one medium to another is called
refraction.
Q3. Under what conditions, phenomenon of refraction takes place?
Ans. Refraction occurs if the refractive indexes of the two media are different and
the angle of incidence is not
zero.
What type of substances can be characterised with a single refractive index?
Ans. Isotropic substances whose properties are identical in all directions (cubic
crystals) can be characterised
Q4.
with a single refractive index.

Q5. What type of substances can be characterised with more than one refractive
index?2
Ans. Anisotropic substances whose properties depend upon the relative orientation
of the light beam and
crystal axis possess more than one refractive index.
Q6. What is the range of refractive indexes of liquids?
Ans. The refractive indexes of liquids fall in the range 1.3-1.7.
Q7. What happens to the refractive index with the increase in unsaturation and
chain length of fatty
acids in oils?
. t increases with the increase in unsaturation and chain length of fatty acids in
oils.
What do you mean by refractometer?
O ractive indices of liquids can be measured directly by means ofan instrument
known as refractometer
Q9. N e the most widely used instrument for the measurement of refractive index of
organic
liquid.
Ans. Abbe refractometer.
EXPERIMENT 12
AIM: To determine the strength of strong acid by titrating it with strong base
using pH meter.
APPARATUS/CHEMICALS REQUIREMENT: pH meter, Combined glass clectode, Beaker,
Burette, Stirrer,
Distilled water, 0.1N NaOH, Unknown HCl solution, Buffer solution of pH 4 and 9
(Acidic & basic).
THEORY: Most of the chemical and biochemical processes are profoundly affected by
the acidity or alkalinity
of the medium in which the reaction takes place. All acids dissociate in aqueous
solution to yield H ions. In order
1o express the acidity or alkalinity ofa solution, one can use the hydrogen ion
concentration. The ionic product of
water is 1014. Therefore, in water (ifit is neutral), we have: [H*]=[OH]= 107
Mathematically; pH = log 1/[H'] (or) pH= - log [H']
DC pH ofa solution can be measured accurately with the help ofa pH meter.
Measurement of pH is employed
to monitor the cause of acid-base titration.
The pH meter cons
nsists of combined glass electrode and indicator electrode which responds to H'
conc. and a
Clectrode (reference electrode). When glass clectrode is in contact with the
solution, it acquires some

potential which depends upon the concentration of H' ion in solution i.c., there
exist a potential difference at the
interface between the glass electrode containing H' and the solution.
The electrochemical cell is
H,(Pt)|HCI|Salt bridge| (N) KCI, Hg,Cl,6)|Hg
I atm (Sat.KCI)
The emf ofthe cell is given by
E E°+ log[H Jat 25°C
When an alkali is added to an acid solution, the pH of the solution X=volume of

base
increases slowly, but at the vicinity of the equivalence point, the 14 required for
complete
rate of change of pH of the solution increases very rapidly as at neutralizatio
the equivalent point H* ion'concentration is very small. Then it
flattens out after the end point. From the sharp jump in the curve, pH equivalence
point
we can find the equivalence point, from which the strength can be
calculated. The region of abrupt chnge ofpH in the titration curve
includes the equivalent point (end point or stochiometric point). X mL
The pH values of the solution at different stage of acid-base
neutralization are determined and plotted against the volume of Volume of base
added
alkali added on adding a base to an acid. However, the shape ofthe curve depends
upon the ionisability of the
acid and the base used and also on the acidity of base and basicity of the acid.
PROCEDURE:
1. First, standardize or calibrate the pH meter by using the buffer solutions of
appropriate pH*.
2 Transfer 50 ml of the given HCl solution in a 100 ml beaker.
3 Insert the electrode in the beaker containing above solution, so that they are
dipped in the acid solution.
Stir the solution well and measure the initial pH of the solution.
5. Add 0.5 or 1.0 ml portion of NaOH solution from the burette and stir the
contents thoroughly.
6. Measure the pH of the solution for cach addition of base. This is known as pilot
titration for equivalence
point determination.
1. Repeat the procedure for the accurate titration by adding 0.2 ml portions of
strong base from the burette
to get the exact end point near the neutralization point.
8 Plot a graph between pH and volume of NaOH added and find out the volume of NaOH
required (V, or
XmL) for complete neutralizatjon of HCI from the graph. Then find out the strength
of HCI.
During the titration, there uppears 2 pH-metric jumps. Near the end point, volume
of NaOH added should be as small as
possible because the acid is neutralized and there will a shurp increase in pH
values.
PROF OFESSIONA Chemistry Lab Manual

Volume ofHCl taken= 501 ml (say)
OBSERVATIONS: 75
Table: pH Metric Titration of HCI Solution vs NaOH Solution

S.No. Volume of NaOH added (mL)Observed pH
1. 0.0
1.0
2.0
3.0
5. 4.0
6. 5.0
6.0
7.0
9. 8.0
10. 9.0
11. 10.0
12. 11.0
13. 12.0
CALCULATIONS: A curve is plotted with pH values as ordinate and the volume of NaOH
added (ml) as
abscissa (Fig.). Find out the end point.
Suppose, volume of NaOH used at the end point = V, ml
N,V N,V2
(Acid) (Alkali)
Nx50= 10
N 1xV
10x50
,_x36.5 g/litre
Strength ofHCl solution= 10s36.5 glitre
10x50
RESULT:The strength of the given HCl solution is.. ghtre
PRECAUTIONS:
*Handle the instrument, electrodes (cell), glassware with care.
2. burning the set buffer control. Put back the selector at ero position. Wash the
electrode with distiled water and standardize the pH meter
Avoid parallax error while taking the readings.
solution h pH meter: Switch on the instrument and wait for 10-15 minutes so that
machine gets warmed up. Prepare the Dujer
dip the eledng buffer tablets ofpH=4 and přl = 9.2 in 100 mL of water separately.
Wash the electrode with distilled waler. 1nen,
temperotue ln the buffer solution (pH =4) taken in a beaker, so that the electrode
immersed to the solution properly. Measure ine
Controi. P e solution and set the temperature cotpensate control accordingly. Set
the pointer to pH= 7exactly means J se
using basicl ,eector switch to proper pH range 0-7 (as the buffer pH = 4). So the
pointers to the known pH value of ne
E Soution pH =9.2. Sameprocedure to be followed except the selector switch is put
to range of 7-4.
PROFESSIONAL 'Chemistry Lab Manual

3. The electrode should not touch the walls of the beaker.
Electrodes must be immersed in the solution properly and su fficient time to be
allowed for the electro
4. trodes
to obtain the temperature of the solution.
5. pH meter should bé calibrated before the experiment.
6 Magnetic stirrer maybe used or the solution be stirred mechanically from time to
time during pH met:
titration.
7. Leave the selectorin zero position where it is not in use.
(VIVA-VOCE
Q.1 Define pH.

Ans. pHis defined as the negative logarithm of hydrogen ion concentration.
pH=-loglH']
Q.2 Which electrode do you use in pH titrations?
Ans. Any electrode such as glass electrode, hydrogen electrode,quinhydrone
electrode etc.
Q.3 Name the indicator which you use in pH.titration.
Ans. We do not use any indicator in pH titration.
Q.4 What is the desirable pH range for drinking water?
Ans. The desirable płH range for drinking water is 7.0 to 8.5.
Q.5 Who suggested the term Ph value?
Ans. First of all Sorenson proposed the term pH value to measure the acidity of
solution.
Q.6 What is the efect of temperature on pH?
Ans. The pH vlaue of the solution increases with increase of temperature
Q.7 What is the effect of dillution on pH of an acidic solution?
Ans. On dillution pH increases towards 7.
Q.8 Which electrode is most suitable for the determination of pH?
Ans. Glaşs electrode is most suitable for the determinaton of pH.
Q.9 What is a combined electrode?
Ans. Electrode combining reference electode and a glass electrode is termed as
combined electrode.
Q.10 Why is hydrogen electrode not generally used in pH measurements?
Ans. (i) t is diflicult to set up. (ii) It cannot be used in redox systems.
Q.11 What would be the degree of ionisation of a strong clectrolyte?
Ans. It is nearly 100 percent.
Q.12 Define a reference electrode.
Ans. Standard hydrogen electrode isused as reference electrode. it is constructed
by dipping a Platinum foil
coated with platinum balck in I MHCI solution through which hdgrogne is passed at
298 Kunder 760 mn
pressure. Its electrode potential is assumed as zero.
OFESSIONAL Chemistry Lab Manual

PRO
Q.13 Why are soluti 77
are solutions acids and bases in water behaves as electrolytes..
Ans. They consist of hydrated ions and therefore canconduct electricity.
Q.14 what are the advatages in using glass electrode over quinhydrone electrode in
measuring pH
of of the solution?
Ans. Glass electrode is imple, not easily oxidiscd and attains cquillibrium
rapidly.
o15 Why is it necessary to knwo the pH of the solution?
Ans. tis very importatn to determine the pH of the solution because most of the
chemical and bichemical
Drocesses are highly affected by the acidity or alkalinity of the medium.
Q.16 List the desirable pH range for drinking water?
Ans. The desirable pH range for drining water is 7.0-8.5.
Q.18 Define buffer action.
Ans. The resistance of a solution to any change in its pH value is known as its
buffer action.
EXPERIMENT 13
AIM: To determine the surface tension of a given liquid at room temperature by
means of a
stalagmometer by drop number method.
APPARATUS AND CHEMICALS REQUIREMENT: Stalagmometer, Beaker, Rubber tubing, Pinch
cork,
Relative density bottle, Thermometer, Water, Given organie liquid.
THEORY: The resistance of a liquid to an increase in its surfacc arca is called the
surface tension ofthe liquid.
Substances with large attractive forces between molecules have high surface
tensions. The stalagmometer method
is the one; most often used in chemical laboratories.
Stalagmometer Method:
It consists ofa capillary tube with a thick wall and a ground glass flattened end
with sharp edges. This helps in
giving large well-formed drops. The function of capillary tube is only to slow down
the rate of flow of the liquid.
At the upper end of capillary is a bulb above to which a small glass tube is fused.
Above and below; the bulb of
the instrument carries two marks A and B. These marks define the volume of the
liquid to be delivered for
counting the drops. The rate of flow is adjusted by altering the screw pressure on
the rubber tube. In any case,
tne rate of formation of drops should not exceed 15 drops per minute. This
adjustment can be altered to readjust
ate offlow of various liquids and will be rcquired to exert different pressure for
different liquids. There are
wO methods to measure surface tension with stalagmometer. (i) Drop weight method
and (ii) Drop number
In thesc methods, the weight and number of drops are compared to those froma
reference liquid.
Drop Number Method:
dlSurtace tension force supporting the drop is 2Try, where r is radius of the outer
circumference of the
The
th nd of the capillary tube. It is along this line that the liquid, glass and air
meet and force of surface
drop
perates. The drop will fall when its weight force (mg) just excceds surface tension
force acting along the
Circumference. Hence mg= 27r

In case of two liquids; we have
m,g = 27ry, m,g = 2Try2 Capillary
With two different liquids, the masses of equal volumes are Wall
proportional to their densities. If n, and n, are the number of Thicknesss
drops produced from the same volume v of two liquids, then A
Volume ofa single drop ofone liquid= n
Mass of its single drop, m, V -xd, Surface tension

B acting along the
circumference
2ryxd, 8 )
and for the second liquid,
Force
V (a)
2nry, =-xd, g (i) (a)
Dividing (i) by (iü), we get (a) Stalagmometer with end fattened and
carefully ground and polished, (b) Liquid
drop for mation at stalagmometet
where and 7, are the surface tensions and d,and d, are the densities of
the respective liquids. One of the liquid is usually water as its surface tension
Air leak
data at different temperatures is easily available.
Hence, it is concluded that for the determination of surface tension
ofa liquid by this method, one should know the number of drops produced
from equal volumes of two liquids and the densities of the two liquids. In A
addition to this, surface tension of water (one of the liquid) should also be
known. The experiment should be performed in a thermostat as the surface
tension of a liquid is greatly reduced by a small increase in temperature.
PROCEDURE:
1. Clean the stalagmometer by chromic acid solution to remove grease

etc.; then wash it with distilled water and finally with ether. Dry it
2 by passing air or compressed nitrogen.
Now, tightly fit a rubber stopper having two holes of the wide mouth
weighing bottle.
3. Fig. Arrangement of Apparatus
Insert the stalagmometer in one of the hole and through the other, for the
Determination of
pass a glass tube (this tube serves as an air leak). Surface Tension

Attach a small rubber tube having a screw pinch cock to the upper end of the
stalagmometer (this is
4. 79
attached to regulate the flow rate of the liquid). A small glass tube may be fixed
in the free end of rubber
tube as a mouth piece for hygenic suction.
5. Take out the stalagmometer from the weighing bottle along with the stopper. Fill
it by immersing the lower
end into distilled water and sucking the water above mark A.
6. Close the pinch cock and insert the stalagmometer in the weighing bottle.
7. Now clamp the stalagmometer in a thermostat. Allow the stalagmometer to acquire
the temperature of
the water bath.
8. Count the number of drops obtained from a volume of water between the marks A
and B. Record it; take
similar readings thrice.
9. Remove the stalagmometer from the weighing bottle and thoroughly dry it.
10 Fill it with the alcohol and reset the stalagmometer in the weighing bottle as
done for water.
11. Replace the whole assembly in the thermostat. Count the number of drops for the
volume of alcohol
betwen the marks A and B. Repcat the counting process thrice. Determine density of
alcohol.
OBSERVATIONS:
Table Determination of Surface Tension of the Given Liquid
S.No Water (n,) Given Liquid (n,)

No. of drops Mean No. of drops Mean
2.
3.
By Drop Number Method
1,d
or
n,d
Similarly; = Y
RES
ESULT: The relative surface tension of the given liquid with respect to water at
room temperature is.
PRECAUTIONS:
Washing of stalagmometer should be done thoroughly, so that there may not remain
any trace ofgrease in
2. the capillary, particularly on its end.
Ater washing and drying, great care must be taken to ensure that the tip of the
stalagmometer does not
me in contact with hands or working table. Keep it covered with a clean dry test
tube.

3. The rate of dropping should be less than 15 drops per minute. Drops should be
allowed to fall only under
the weight force and should not be pushed away.
4. Whilc counting the drops, the apparatus should not be disturbed; disturbance may
cause the drops to fall
off before they develop to their full size.
5. Same stalagmometer should be used for water and liquid.
(VIVA-VOCE
Ans. The resistance of a liquid to an increase in its surface area is called the
surface tension of the liquid. It is
Q.1. Define surface tension.
usually represented by a Greck letter .

Q.2. What are the units of surface tension?
Ans. Newtons per meter i.e. Nm" or dynes per cm.
Q.3. What are the units of surface energy?
Ans. Ergs cm (C.G.S.) or Jm (S.I.)
Q.4. What are the effects of surface tension?
Ans. (i) It tends to decrease the surface area of the liquid to minimum.
(ii) The rise ofa liquid in a capillary is also due to surface tension.
Q.5. What is the effect of temperature on surface tension?
Ans. Surface tension decreases with increase in temperature. This is due to the
fact that with increase in
temperature, kinetic energy of the molecules of liquid increases. As a result, they
move with greater
velocities and force ofattraction between them decreases.
Q.6. Atcritical temperature, what happens to the surface tension?
Ans. Surface tension becomes zerò at the critical temperature. This is because at
the critical temperature, the
forces of attraction are just overcome by the kinetic energy of the molecules.
Q.7. Give some applications of surface tension.
Ans. i) Use of soaps and detergents as cleansing agents is based on their property
of lowering the interfacial
tension between water and oily or greasy substances.
(i) In metallurgy, the froth flotation process for the ore concentration is based
on surface tension reduction.
(ii) Surfactants are added in preparations like tooth paste in order to enable them
to spread evenly.
Q.8. Name the various methods used for the measurement of the surface tension of a
liquid.
Ans. The surface tension ofa liquid can be measured by the following methods:
(a) Stalagmometer method (b) Capillary rise method
(c) Maximum double pressure method (d) Torsion balance method
Q.9. What is Traube's Stalagmometer?
Ans. The, pipette like apparatus used for the determination of surface tension by
the drop weight or drop
number method is known as Traube's Stalagmometer which means by a drop measurer.
Q.10. What is the major use of a stalagmometer?
Ans. This is especially useful for comparing surface tensions ofliquids.

/EXPERIMENT 14
AIM: To determine saponification value/number of the given oil sample.
CHEMICAL REQUIREMENTS: Standard alcoholic KOH solution (N/2), Standard HCI(N/2),
Ethyl methyl
ketone as solvent, Given oil sample
INDICATOR: Phenolphthalein
HO OH
END POINT: Disappearance of pink colour with Phenolphthalein (HCl in burette).
THEORY: Saponification value of an oil is defined as the number of milligrams of
KOH required to saponify
fatty material present in one gm of oil. The vegetable or animal oils are ester of
higher fatty acids and they react
with KOH to form the potassium salt of fatty acids. For the determination of
saponification value, a known
weight of oil is dissolved in ethyl methyl ketone solvent and refluxed with a known
excess of standard alcoholic
KOH solution. The hydrolysis of oil or fat with caustic alkalies called
saponification can be represented by
following equation:
CHOCOR CHOH
CHOCOR KOH retlux CHOH + RCOOK +RCOOK +R,COOK
CHOCOR (ac) CH,OH Pot. salts of fatty acids
Glycerol (Soaps)
Triglyceride or
(oil or fat) Glycerine
where R, R, R, are same or different long chain alkyl groups

The unreacted standard alcoholic KOH is determined by titrating it against standard
HCl using phenolphthalein
as an indicator. Disappearance of pink colour of solution marks the end point of
titration.
OH+H >H,O
A blank titration is also performed in the same above manner and under same
conditions except using oil sample.
From the volumes of standard HCI consumed in both the titrations, saponification
value can be calculated using
following formula:
Saponification valuc of oil Vol. of KOH used to saponify x Normality of KOH x Eq.
wt. of KOH
Weight of oil sample
The ification number of some of the fats is given below:

PROF SIONAL Chemistry Lab Manual 83
Fat Saponification Number Fat Saponification Number

Butter fat 210-230 Linseed oil 188-195
Human fat 195-200 Coconut oil 250-260
Olive oil 185-195 Castor oil 175-185
Cottonseed oil 194-196
PROCEDURE:
Tabe two 250 ml conical flasks and label them A and B. Weigh the empty conical
flask labelled A. Then, weigh
a
ceurately about 1-2 gm of given oil sample into flask A. Difference in two weights
is the exact weight of o
accu
sample taken in flask A. Add 25 ml of ethyl methyl ketone and 25 ml of N/2
alcoholic KOH solution to both the
Hask A and B separately (Flask B is for blank determination, so no oil is taken in
it).
Put a small piece of boiling chip in both of the flask and fit air condensor on the
mouth of the flasks. Now place
the flask on water bath (temp. 100C) for 45 minutes. Wash the inner walls of each
condensor with some distilled
water into the respective flasks and cool the flasks to room temperature (or under
tap water) Add 9-10 drops of
phenolphthalein indicator to each flask by which pink colour is obtained. Rinsc and
fill the burette with standard
N/2 HCI solution and note down its initial reading. Titrate this pink colour
solution against N/2 HCI till pink
colour just disappears. Note down the final burette reading. Same titration
procedure is adopted for blank
titration.
OBSERVATIONS:
Weight of conical flask A+ oil sample = W, g
Weight of empty conical flask A = W,g
Weight of oil sample= (W, -W,)=W g
Volume of N/2 alcoholic KOH added to cach flask = 25 ml
Volume of ethyl methyl ketone added to each flask = 25 ml
Table 1. For sample Titration (Titration of unreacted KOH Vs N/2 HCI)
S.No | Initial Burette Reading Final Burette Reading| Volume of N/2 HCI used (ml)
S.No
1.
Table 2. For blank Titration(Titration of total KOH Vs N/2 HCI)
S.No Initial Burette Reading Final Burette Reading Volume of N/2 HCI used (ml)
S.No
1.
ume of N/2 HClused by unreacted KOH in sample flask A =x ml

Volume ofN/2 HCl used by unreacted KOH in sample flask B = y ml
Volume of N/2 HCl equivalent to volume of N/2 KOH used for
saponification of (W, -W) = Wg ofoil = (-x) ml
Saponification value ofoil = VO. or KOH used to saponify x Normality of KOH x Eq.
wt. of KOH
Weight of oil sample
y-x)x N/2x 28 Z
W
RESULT: Saponification value/number ofthe given oil sample is found to beez.
PRECAUTIONS:
. High boiling solvent such as ethyl methyl ketone should be preferred as it raises
the boiling point and thus
speed up the saponification.
2. To prevent the loss of oil vapours to the atmosphere, the slow boiling should be
carried out and the water
condenser should preferably be used in place of air condenser.
3. To enhance the rate of reaction, the reaction mixture should occasionally shaken
during reflux.
4. To get the acCurate results, the blank titration and the sample titration should
be carried out under similar
conditions.
1. N/2 HCI: Dilute 43.1 ml of concentrated HCl to one litre with distilled water
and standardise with N/2
sodium carbonate solution using methyl orange indicator.
2. Standardized N/2 Alcoholic KOH: Dissolve 28 g of KOH (A.R. Grade) pellets in one
litre of 95%
alcohol. Mix thoroughly and keep the solution for some time so that carbonate, if
any, get settled down.
Decant the clear supernatant solution and standardize it with N/2 oxalic acid.
3. N/2 Oxalic Acid: Dissolve 31.5 gof oxalic acid (C,0,2H,0) in one litre of
distilled water.
N/2 Sodium Carbonate Solution: Dissolve 13.25 g of Na,C0, (A.R. Grade) dried at
250°C, in distilled
water and dilute to 500 ml.
(VIVA-VOCE
Q.1. Defjne Saponification number of an oil.

Ans. Itisthe number of milligrams of KOH required to completely saponify 1 gof the
oil.
Q.2. How the saponification value of an oil/fat can be determined?
Ans It can be determined by refluxing a known amount ofa sample with excess of
standard alcoholic KOH
solution and titrating the unuscd alkali against a standard acid solution.
Q.3. What are soaps?
Ans. Soaps are generally the mixtures ofsoap and potassium salts of higher fatty
acids such as stearic, palmitic
and oleic acids.
NAL Chenmistry Lab Manual

AIM To prepare Phenol Formaldehyde (PF) resin.
PROFESS
87
balance, Phenol, Formalin, Glacial acetic acid and conc. HCI. EXPERIMENT 15(A)
APPA US/ CHEMICALS REQUIRED: Glass beaker, Glass rod, Measuring cylinder, Digital
electronic
DV- Resins are in general raw materials, for example for binders, curable moulding
compositions, adhesives
ORY: Resins are in
T inos. They normally have melting or softening range, are brittle in the solid
state. Resins can be divided
anral resins and synthetic resins. Phenolic resins are condensation polymerisation
product of phenolic
natura
ives with aldehyde (like formaldchyde or furfural). These are formed by
condensation polymerization off
kenol and formaldehyde in acidic or alkaline medium. Following steps are involved:
pheno.
Cen 1, Fornmation of ortho and para hydroxy benzyl alcohol derivatives
Tnitially; the monomers combine to form methylol phenol derivatives depending upon
phenol to formaldehyde
(P/F) ratio.
OH OH OH
O H CHOH
C
H H
o-Hydroxybenzyl CH;OH
alcohol p-Hydroxybenzyl
alcohol
(P/F 1:1)
H H
OH OH
HOH2C CH2OH H H CHOH
CH2OH CHOH
2,4,6-Trihydroxymethyl 2,4-Dihydroxymethyl
phenol phenol
(P/F= 1:3) (P/F =1:2)
onof products depend on the (i) phenol used (i1) the stochiometric ratio of phenol
to formaldehyde
Format
Step 2. Fomation of Novolac and Bakelite
linear polyme or a highly cross linked polymer.
and (ii) the pH during the reaction
nar pol phenol (i.e. hydroxy benzyl alcohol) derivatíves react among themselves or
with phenol to give a
The methylol

(a) Linear polymer (Novolac)
These are phenols that are linked by alkylidene (methine) bridges, without
functional groups (apart
rt fromt
phenolic hydroxyl groups). These can be cross linked by addition of curing agents
such as formalde
hexamethylene tetraamine. aldehyde
QH OH
CH;OH H
n
-nH0
OH OH OH
-CH2" CH2 -CH2
Novoac
(b) Cross linked polymer (Bakelite)
These are excellent heat resistant and having high OH QH
dimensional stability with good dielcctric property. QH
QH OH -CH2 -CH2-
CH,OH Condensation
polymerization
m
ÇH2 ÇH2
ČHOH
-CH2- -CH2
OH OH OH
Bakelte
(eross linked polymer)
PROCEDURE:
Place S mL of glacial acetic acid and 2.5 mL of 40% aqueous formaldehyde (i.c.
formalin) solution in a 100 m
glass beaker. Now, add 2 gm phenol to it safely. Add conc. HCl dropwise with
vigorous stirring by a glass rod t
a pink coloured gummy mass appears. Wash the pink residue several times with water
to make it free from acid
Filter the product and weight it after drying in the folds of a filter paper or in
an oven. Report the yield of resi
formed.
OFESSION Chenmistry Lab Manual

OBSERVATIONS: 89
Weight of empty watch glass= W, gm
Weight of watch glass + resin formed= W, gm
Weight of resin formed l=W,-W, gm
RESULT: Weight of phenol formaldehyde resin=W gm (say)
PRECAUTIONS:
. The reaction is sometimes vigorous and it is better to be a few feet away from
the beaker while adding the
HSO, and until the reaction is complete.
The experiment should be preferably carried out in fume cupboard.
EXPERIMENT 15(B)
AIM: To prepare Urea Formaldehyde (UF) resin.
APPARATUS/CHEMICALS REQUIRED: Glass beaker, Glass rod, Funnel, Urea, Formalin and
Conc. HSO
THEORY: Resins are in general raw materials, for example for binders, curable
moulding compositions,
adhesives and coatings. They normally have melting or softening range, are brittle
in the solid state. Resins can
be divided as natural resins and synthetic resins. Urea formaldehyde (UF) resins
are thermosetting amino
polymers which are formed by condensation ofurea and formaldehyde in acidic medium
by following steps:
Step 1. Formation of mono and di methylol urea derivatives
Iniially, urea and formaldehyde react to form methylol urca derivatives depending
upon urea to formaldehyde
(U/F) ratio.
H-NCH2OH
UF 1:1
NH2 NH2
Monome thybl urea
C=0 H H-N-CH%OH
NH2
UF=12 H-N-CH%OH
N, N'-Dimcthylol urca
Oll, grease and weak acids alongwith good adhesive properties.
Several lecules of dimethylol
Folymerization of dimethylol urea
inked cules of dimethylol urea derivatives condense with loss of water molecules to
form a highly cross
Brease naldehyde resin. These possess good electrical insulating properties and
having resistance to
linked urea
H-N-CH:OH H-N-CH,OH -nHhO -N-CH2-N

=o c=o
H-N-CHOH H-NCH,OH -N-CH-N
UF-resin
PROCEDURE:
Place 5 mL of 40% aqueous formaldehyde (i.e. formalin) solution in a 100 mL glass
beaker. Now, add 2.5 on
urea powder to it safely. Stir with a glass rod until a saturated solution is
obtained. Add few drops of cone
H,SO, (2-3 drops) dropwise with vigorous stirring by a glass rodtill a voluminous
white solid mass is formed
Filter the residue and wash it several times with distilled water to make it free
from acid.Filter the product and
weight it after drying in the folds of a filter paper or in an oven ( Above 80'C,
ifkept continousty, UF
resin gets discoloured). Report the yield ofurca formaldchyde polymer formed.
OBSERVATIONS:
Weight of empty watch glass W, gm
Weight of watch glass + resin formed= W, gm
Weight of resin formed= W,- W, gm
RESULT: Weight of urea formaldehyde resin = W gm (say)
PRECAUTIONS:
1. The reaction is sometimes vigorous and it is better to be a few feet away from
the beaker while adding the
H,SO, and until the reaction is complete.
2. The experiment should be preferably carried out in fume cupboard.
(VIVA- VOCE)
Q.1. Define a polymer.

Ans. Polymer is a high molecular mass giant molecule which is formed by linking
together ofa large number o
small molecules of monomers.
Q.2. What is a monomer?
Ans. It is a small molecule which combines together to form a giant molecule known
as polymer.
Q.3. What is meant by degree of Polymerization?
Ans. Number of repeating units of monomers in a chain of polymer is known as degree
of polymerization.
Q.4. Differentiate between a polymer and a macromolecule.
Ans. Both are giant molecules. Polymers has a repeat unit which a macromolecule may
not have. Hence all te
polymers are macromolecules but all the macromolecules are not the polymers.
Q.5. Give the name of some naturally occurring polymers.
Ans. Some naturally occurring polymers are: Starch, proteins, cellulose, natural
Rubber.

EXPERIMENT 16
AIM: Estimation of calcium in limestone and dolomite.
APPARATUS/CHEMICALS REQUIREMENT: 500 mL Beaker, Burette, Pipette, Measuring
cylinder, 100
mL Measuring flask, Titration flask, Funnel, Filter paper, N/20 Standard potassium
permanganate solution, 8%
Ammonium oxalate solution, 1:1 Ammonia solution, dil. H,SO-, dil. HG1, dil. HNO,
Silver nitrate solutionand
Methyl red indicator solution.
INDICATOR: KMn0,(Selfindicator)
END POINT: Light pink colour
THEORY: Limestone is the important source of CacO, and contain small amount of
MgC0, Dolomite contains
cquimolar amount of CaCO, and MgCO. These ores are generally contaminated with
minor amounts of oxides
of iron, alumnium, silicon (free or combined) and organic matter. The minerals havc
large umber ofindustrial
applications and the quality of the mincrals as woll as its suitability for a
particular commercial applications
depends upon the amounts of CaCO,, MgCO, and the other constituents present. Hence,
complete analysis is
often necessary.
To estimate the calcium in limestone, the limestone powdered is dissolved first in
HC1. Calcium in a solution is
precipitated as calcium oxalate by adding ammonium oxalate in a medium made
slightly alkaline using ammonia:
CaCO, +2HCI » CaCl, + H,O + co,
CaCl, +(NH,),C.O, CaC.O, + 2NH CI
Calcium Oxalate
(White ppt.)
The white precipitate is filtered, washed free of oxalate and chloride ions and
dissolved in dilute sulphuric acid.
CaC,O, +H,SO, (COOH), + Caso,
The liberated oxalic acid, which is equivalent to calcium in the original solution,
is titrated against standard
KMnO, in acidic medium.
(COOH), 2CO, + 2H' + 2e] x5
MnO + 8H* + 5Se Mn2+4H,O]x 2
2MnO+ 5(COOH), + 6H* 2Mn+ 10Co, + 8H,O

From the volume ofKMnO, consumed for the titration, the amount of calcium in the
ore can be calculated.
PROCEDURE:
1. Take 20 mL of sample solution in a 500 mL beaker. Add 60 mL distilled water to
dilute it.
2 Warm the solution and add 20 mL of8% ammonium oxalate solution with continuous
stirring with a glass
rod. A slight white coloured precipitate appears.
3. Add 2 drops of methyl red indicator to the white coloured precipitate.
To this solution, add 1:1 ammonia solution drop wise until the red colour of
solution changes to yellow.
K.cep the solution as such for half an hour to allow the precipitate settle down.

5. Filter the precipitate and discard the filtrate. Now,wash the precipitate
repeatedly with 5 mL of0.10
0.1%
ammonium oxalate solution until the filtrate is free from chloride (removal of
chloride is confirmed
the filtrate does not give white precipitate with AgNO, solution acidified with
dil. HNo)
6. Wash the precipitate with cold distilled water until the filtrate is free from
oxalate ion (removal ofoxalats
is confirmed if the filurate does not decolourizes hot solution of very dilute
KMnO). late
7. Now place the funnel on the mouth of 100 ml measuring flask, make a hole in the
filter paper with a ga
rod and the transfer the precipitate into the flask with the help of 25 mL dil.
H,S0, Open the filter paper
to check if any precipitate is sticking with it.
8. Now shake the flask to dissolve the precipitate (add more dil. H,SO, if
necessary) and make up the
volume of the flask up to the mark by adding distilled water.
9. Take 20 ml of this solution into the titration flask, add 10 mL of dil. H,so,
heat to about
60° C and titrate it against N/20 KMnO, until a light pink colour appears.
10. Repeat the titration to get the concordant readings.
OBSERVATIONS:
Table. Titration of Contents Vs N/20 KMnO,
S.No Initial Burette Reading | Final Burette Reading Volume of N/20 KMnO, Used (ml)
2.
3.
GENERALCALCULATIONS: Concordant reading = V mL
Volume of prepared solution = 100 mL
Volume of solution taken for each titration = 20 mL
100 mL prepared solution contains 20 mL calcium ion
20 mL prepared solution contains 20 20 = 4 mL calcium ion

100
N,V, N,V
(Calcium (KMnO)
N, x 4 = 1/20 V
V
N,R0N
Strength =N, * Eq. wt. of CaO
V
0 x 28

V 100
Weight of calcium in the sample=onx28 x 10008
80
80 x 28 xx 1000 mg
RESULT: Amount of calcium as CaO in the given sample solution is ...
PRECAUTIONS:
1. The presence of chloride and oxalate should be tested with a few drops of
filtrate taken directly from the
funnel.
2 The solutions used for washing should be taken in a beaker in which the
precipitation was carried out and
then it should be transferred to the filter paper.
3. Any precipitate remained stick in the beaker or in the filter paper should be
completely transferred into
the measuring flask with the help of dil. H,SO, or distilled water.
4 A process of washing the precipitate should be repeated only when the first
portion of washing has
completely passed through the filter paper.
1. Sample Solution: Dissolve 5.5 gof CaCl, in one litre of distilled water.
2 N/20 Potassium Permanganate (KMnO) Solution: Dissolve 1.58 gof potassium
permanganate i
3. Ammonium Oxalate Solution (8%): Dissolve 8 g of ammonium oxalate in 100 ml of
distilled water.
4. 1:1 Ammonia Solution: Mix equal volumes of ammonia and water.
5. Methyl Red Solution (1%): Dissolve 0.1 gof methyl red (free acid) in 100 ml
ofhot distilled water and
cool. Filter, if necessary. OR
Dissolve 0.1 g in 60 ml of distilled alchol and add 40 ml of distilled water.
6. Silver Nitrate Solution (1%): Dissolve 1 g of AgNO, CA.R. Grade) in boiled-out
100 ml distilled
water. OR
Silver Nitrate Solution(0.1 N): Dissolve 1.7 gofsilver nitrate in 100 mi of
distilled water.
Note: Always store silver nitrate solution in brown bottle.
(VIVA-VOCE)
Give two important ores of calcium.

0 Dolomite (an eauimolar mixturc of CaCO, and MgCO)
lime stone (mainly CaCO, with small amount of MgCO0)
is 1S Insoluble in water and does not directly react with ammonium oxalate. That is
why tne or
Why the calcium ore is dissolved in HCI.
A Ovol SOlved in dil. HCl to convert CaCO, into soluble CaCl, which easily reacts
with ammoniun
Oxalate.
EXPERIMENT 17
AIM: To determine the total dissolved solid in a waste water sample.
APPARATUS/CHEMICALS REQUIREMENT: Silica (porcelain or nickel or platinum) crucible,
Beaker,
Measuring cylinder, Whatmann filter paper no. 44 (or glass fibre filter disc or
Gooch crucible), Analytical balance,
Steam bath, Oven, Desiccator.
THEORY: Sewage or the waste water contains solids in suspended, colloidal or
dissolved fom. The "Solids"
refers to the matter that remains as residue upon evaporation and drying at 103-105
°C or 179-181 °C
."Dissolved solids" is the portion of solids that passes through a filter of 2.0 mm
(or smaller) nominal pore size
under specified conditions. The "Suspended solids" are those which can be filtered
out by a filter paper. The
suspended solids are of two. type, settelable and non- settleable. "Total solids"
is the term applied to the
material residue left in the vessel after evaporation ofa sample and its subsequent
drying in an oven at a defined
temperature. Total solids includes "total suspended solids," and "total dissolved
solids,".

It is difficult to remove the dissolved solids. Sewage normally contains 99.9
percent of water and only 0.1
percent of solids. Solids have the nuisance value because of their
biodegradability. The organic matter in the
sewage is highly susceptible of decay. During the decomposition, the organic matter
gets converted into inorganic
matter. The decomposition of organic matter depends upon
i) Temperature of the reaction:-Higher is the temperature, faster is the reaction.
(ii) pH: If the pH goes below 5, the anaerobic decomposition ceases.
The treatment of wastewater is necessary before it is disposed into a water body to
protect them by the foul
effects of the solid matter present in the wastewater. Better characterization of
organic matter can be made by
such tests as total organic carbon, BOD and COD. Biochemical Oxygen Demand. (B.O.D)
is the requirement of
oxygen imposed by the acrobic bacteria for the decomposition of biodegradable
organic matter at some certain
temperature. Water has dissolved oxygen in it that is required for the very
existence of the aquatic animals and
plants. When sewage is discharged in water, its Biochemical oxygen demand is
satisfied by the dissolved oxygen
of the water and ultimately the water becomes deficient of oxygen and the aquatic
life is endangered. So to
reduce the BOD first ofall the settleable solid are removed may it be organic or
inorganic by sedimentation. Then
the colloidal and dissolved organic solids are supplied with the oxygen to get
converted into inorganic solids and
come out of the solution and thus get 'Bio-flocculated'. Now they get settled and
can be removed leading to a
less harmful waste water. This is the reason of determination of total solids in
wastewater.
PROCEDURE:
Take a clean and dry silica crucible and note down its weight.
Filter a known volume of water sample by using Whatmann filter paper no. 44.
Transfer the filtrate in already dried, weighed silica crucible and evaporate to
dryness on a steam bath.
(Evaporation may also be performed in a drying oven)
3. Now; further dry it for one hour at 180 UC in an oven and then cool the crucible
in a desiccator and
weigh it.
4. Repeat the process of drying (if necessary) until there is no further loss in
weight.
OBSERVATIONS AND GENERAL CALCULATIONS:
Volume of the sample filtered = VmL
Weight of crucible = W,g
Weight of crucible + residue= W, g
Weight of residue (dissolved solids)= (W,-W,)g
Total Dissolved solids (mg/L)= (W-W)xI1000 = A ppm
V
RESULT: The total dissolved solid of water sample is A ppm.
PRECAUTIONS:
1. The outer surface of the crucible should be wiped before placing it in the oven
for drying.
2. During evaporation care should be taken to avoid spattering.
3. Cool the hot sample in a dessicator.
4 Switch off the oven when not in use.
5. After weighing measurements, clean the crucible immediately.
EXPERIMENT 18
AIM: To find out the melting point and eutectic point for a two component system by
the method of
cooling eurve.
APPARATUS/CHEMICALS REQUIREMENT: Corning glass tubes, Thermometer, Liquid paraffin
or
glycerine bath, Beaker, Small ring stirrer, Cork-10, Ice bath, Stop watch.
THEORY: Thermal analysis is a branch of phase diagram showing cooling curves of
various composition of a
system during solidification. The form of cooling curve indicates the composition
ofthe solids. In the eutectic
mixture, there are two solids capable of forming solutions with each other. They
depress freezing point and the
melting point is also lowered. The coling curve is a representation of phase
diagram in terms of temperature
along Y-axis and time along X-axis as shown in Figure.

When a solid solution is cooled at freezing point, a solid phase appears, the rate
of cooling is altered and the
hereis
a break in the cooling curve. The temperature decreases continuously but at
different rate but at freezing pain
int. If
the mixture becomes eutectic the temperature falls until the eutectic point is
reached. The system becom
omes
invariant and temperature remains constant until total solidification occurs (along
C'D) and again temperah
ature
falls uniformly (along D'E').
The purpose of the experiment is to obtain data by thermal analysis for
constructing a phase diagram whih
indicates the solid and liquid phases that are present at each temperature and
composition. The temperatureca
res at
which solid phases appear upon cooling various solutions of the two components are
detected by observation of
the changes in slope of the plot of temperature versus time. A slower rate of
cooling is obtained while a solid
phasc is separating out because the heat evolved by solidification partly off sets
the heat lost by radiation and
conduction to the colder surroundings. A time-temperature graph is obtained by
recording the temperature asa
function of cooling time. A sampling rate of 0.2 times per scconds and total time
of 2000 seconds is recommended
for recording the results using the temperature probe.
Following are the few combinations of chemicals which can be utilized to find the
eutectic point ofa two component
system:
Sr. No. ComponentA Component B

Diphenylamine Benzophenone
2 Pure naphthalene Benzoic acid
3 Pure naphthalene Diphenyl
Naphthalene B-naphthol
5 Tin Lead
6. Acctamide Salicylic acid
7. Benzoic acid Cinnamicacid
8. Cinnamicacid Naphthalene.
9. Urea Phenol
10. Naphthalene Nitrophenol
PROCEDURE:
Prepare mixture in any ratio of given two components A and B and tabulate in Table
1.
2. Take the melting point of the pure compounds A and B on the thermometer.
3. Take 10 test tubę of equal size with a cork having holes to provide stirrer and
thermometer.
4. Melt the mixtures by placing the test tube in a bath of liquid paraffin. Take
the melting point of each
mixture containing different proportions of component A and component B.
5. Transfer the test tube one by one in an ice bath. Start the stop watch and note
the temperature at the
different intervals oftime (say every halfa minute or minute).
6 Note the temperature at which first crystal of the solid appears.
7 Cooling is further proceed by adding more ice in ice bath. The exact temperature
was noted at which th
solid liquid system shows temperature halt before complete solidification. Lowest
temperature halt wi
be the eutectic temperature.
PROFESSIONAL Chenmistry Lab Manual

OBSERVATIONS: 101
Table 1
Sr. No. Mixture of component ofA and B( in grams) Temperature Time in
B (C) Seconds
11 1
2 10 2
3 09 3
08
5 07 5
6 06 6
7 05 7
04 8
10 03 9
02 10
Graph: Agraph is plotted by drawing a cooling curve by plotting the time of cooling
in seconds or minutes (as X-
axis) against temperature (as Y-axis). From the cooling curves, find the transition
temperature on freezing point
for each mixture and tabulate them in Table 2.
Table 2
Mixture No. % of B Transition Temperature (°C) Eutectics
A'
.. cp' B
Solid A Solid B
E D +Liquid C +Liquid E
Solid A+Solid B+Eutectic
Time 20 40 60 80 100
Composition (percentage)
Fig. Cooling Curves

RESULTS: M.pt. of component A ,°C
M.pt. of component B .°C
Eutectic temperature ..°C
Eutectic Composition
PRECAUTIONS:
1. It is important to use pure materials for preparing the mixtures.

2. The temperature of the mixture should fell slowly.
3. Cooling curve should be obtained from a large number of mixtures as possible.
(VIVA-VOCE)
Q.1. State phase rule?
Ans. According to the Gibb's phase rule, "In a heterogeneous system in equilibrium
at a definite temperature
and pressure, the sum of number of degrees of freedom (F) and number of phases (P)
is equal to number
of components (C) plus two provided equilibrium is influenced only by temperature,
pressure and
concentration and not by other factors such as gravity, magnetic forces etc."
Mathematically; F C P+2
Q.3. What do you understand by reduced Phase Rule?
Ans. For a two component solid-liquid cquilibrium, the gas phasc is not of much
significance and effect of
pressure on such system is very small which is negligible. This reduces the number
of degrees of freedom
to two and the system can be studied to take into account the remaining temperature
and concentration
variables. Such system is known as the condensed system and the phase rule equation
becomes: F=C
P+1(i.ce reduced phase rule cquation).
Q.5. What is meaning of eutectic?
Ans. The term eutectic means casy melting.
Q.6. What is meant by eutectic mixture?
Ans. Eutetic mixture is a solid solution of two or more substances which possess
the lowest freczing point of
all the possible mixture of the components.
Q.7. Define eutectic system.
Ans. Abinary mixture forming an cutectic mixture ofa particular composition is
called an eutectic system.
Q.8. Define eutectic point.
Ans. It is the maximum temperature upto which a solid phase can exist.
Q.9. Give some applications of eutectic.
Ans. Low melting alloys are used in safety devices, fire sprinklers, freezing
mixtures etc.
Q.12. What is cooling curve?
Ans. Itis a curve plotted between time of cooling on x-axis and temperature on y-
axis.
Q.13. What is meant by transition temperature?
Ans. The temperature at which two forms of a substancc are in equilibrium is called
transition temperature.
Q.14. What is supercooling?
Ans. Sometimes on cooling a liquid, separation of the solid phase may not occur at
the actual freezing point of
the liquid phase and the liquid may be cooled below its freezing point. This is
called supercooling

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PROFESSIONAL Chemistry Lab Manual

Sodium salt of Erichrome Black-T (represented as NaH,In)

PROFESSIONAL Chemistry Lab Manual

PROFESSIONAL Chemistry Lab Manual

Concordant volume =V, ml

PROFESSIONAL 'Chemistry Lab Manual

1000 ml ofhard water = x1000 mg of CaCo

Total hardness = X ppm (say)

I ml of boiled, cooled & filtered water = xmg of CaCO

1000 ml of boiled, cooled & filtered water 1000 mg of CaCO3

PROFESSIONAL Chemistry Lab Manual EXPERIMENT 1

H,In pH>6.3 HIn2 pH>11.5 In

Disodium salt of EDTA (NazH2Y)

PROFESSIONAL Chemistry Lab Manual

PROFESSIONAL Chemistry Lab Manual 0

V 21* Concordant volume = V, ml|

GENERALCALCULATIONS: V 12s Concordant volume = V, ml

PROFESSIONAL Chemistry Lab Manual

1000 ml hard water =xx1000 mg CacO

Ca2 hardness in water sample = Total hardness- Mg hardness

PROFESSIONAL Chemistry Lab Manual 12

PROFESSIONAL Chemistry Lab Manual 13

HOOCHC N-CH-CH-N CHCOONa .2H,O

MIn +H,Y MY2 HIn2 + 2H

PROFESSIONAL Chemistry Lab Manua

PROFESSIONAL Chemistry Lab Manual 15

Step 2. Determination of total hardness in sample

1000 ml of hard water x x1000 mg of CaCO

1000 ml of diethylamine treated water 1000 mg of CaCO3

Mg hardness in water sample = Total hardness - Ca" hardness

END POINTS: (i) Disappearance ofpink colour (with Phenolphthalein).

PROFESSIONAL Chemistry Lab Manual 21

Methyl orange or total alkalinity (M)=OH + CO; + HCO

PROFESSIONAL Chemistry Lab Manual

FBR with FBR Volume of acid used (ml)

Concordant volumc of acid used ypto phenolphthalcin end point A (y-x) ml

PROFESSIONAL Chèmistry Lab Manual 23

PROFESSIONAL Chemistry Lab Manual 27

PROFESSIONAL Chemistry Lab Manual

THEORY: Flash point is the lowest temperature at

PROFESSIONAL Chemistry Lab Manual 32

Q.1. What is flash point and fire point?

THEORY: Viscosity is the property of a fluid that determines its resistance to

PROFESSIONAL Chemistry Lab Manual 35

Description Redwood Viscometer No. 1-Universal Redwood Viscometer No. 2-Admiralt

Redwood viscometer is divided into

PROFESSIONAL Chemistry Lab Manual

PROFESSIONAL Chemistry Lab Manual

PROFESiONAL Chemistry Lad Manual

Step 1. Calibration of conductivity meter

Step 2. Titration of HCI solution vs N/10 NaOH solution

Nomality of NaOH solation=N

Sr. No. Volume of NaOH added (mL) Observed conduttance (mho)

Strength of HCl solution Normality x Equivalent weight ofHCI

PROFESSiONAL Chemistry Lab Manual

PROFESSIONAL Chdmistry bath Mahudbnual

A schematic representation of flame photometer is shown in figure.

Sample- Compressed/ Compressed/ LCD