PRACTICAL # 1

TITLE:

Determine the percentage purity of NaCl by Mohr’s Method.

OBJECTIVE:

To determine the pure amount of NaCl present in the impure sample provided.

APPRATUS:

 Burette
 Titration flask
 Pipette

CHEMICALS:

 Sample of Salt (NaCl)

 Standard solution of 0.025M AgNO3
 K2CrO4 as an indicator

RELATED THEORY:

PROCEDURE:

 Weigh exactly 2g of sample and transfer it into 500mL volumetric flask.

 Fill the flask up to the mark with distilled water and shake properly to dissolve the sample.
 Take 10mL of sample in titration flask and add 2 drops of indicator to it.
 Take a clean burette and rinse it first with distilled water and then with standard solution of
AgNO3.
 Fill the burette with the standard solution of 0.025M AgNO3, remove air bubbles and note the
initial reading.
 Slowly add titrant to the flask containing analyte with constant swirling till the appearances of red
brick precipitate.
 Take the three readings by repeating the same procedure with other sample of NaCl.

OBSERVATION & CALCULATIONS:

Sr.No Initial burette reading Final burette reading Vol of AgNO3 used
(mL) (mL) (mL)
1 0 10 10
2 10 20 10
3 20 30 10
Volume of AgNO3 used 10
Molarity of AgNO3 solution = M1 =0.025M

Volume of AgNO3 solution used = V1 = 10mL

No of moles of AgNO3 taking part in reaction= n1= 1

Molarity of solution of NaCl =M2= ?

Volume of solution of NaCl= V2 = 10mL

No of moles of NaCl taking part in the reaction=n2= 1

By formula,

M1V1/n1=M2V2/n2

By substituting values we get the value of M2 we get:

M2= 0.025M

NOW,

Molarity of NaCl solution = 0.025M

Amount of pure NaCl dissolved per liter = molecular weight *molarity

= 58.5 * 0.025

= 1.4625 g

Amount of impure NaCl dissolved per liter =2g/500ml

= (2*1000ml / liter)/500mL = 4g

%purity of NaCl =

= 1.4625/4 * 100

= 36.56%

RESULTS:

The purity percentage of NaCl of the given sample is 36.56%.

COMMENTS:
PRACTICAL # 2

TITLE:

The estimation of chloride ions in water.

OBJECTIVE:

To find the concentration of chloride ion in the sample of water.

APPRATUS:

 Titration flask
 Burette
 Beaker
 50mL cylinder
 Pipette

RELATED THEORY:

The chloride ion is the anion (negatively charged ion) Cl−. It is formed when

the element chlorine (a halogen) gains an electron or when a compound such as hydrogen chloride is
dissolved in water or other polar solvents. Chloride salts such as sodium chloride are often very soluble in
water.[4] It is an essential electrolyte located in all body fluids responsible for maintaining acid/base
balance, transmitting nerve impulses and regulating fluid in and out of cells.

Occurrence:
Sea water contains 1.94% chloride. Some chloride-containing minerals include the chlorides of sodium
(halite or NaCl), potassium (sylvite or KCl), and magnesium (bischofite), hydrated MgCl2.

The presence of chlorides, e.g. in seawater, significantly worsens the conditions for pitting corrosion of
most metals (including stainless steels, aluminum and high-alloyed materials) by enhancing the
formation, which, like most chloride salts, is colorless and water-soluble. chlorides is also found in
wastewater.

Effects of Chloride:
Chloride increases the electrical conductivity of water and thus increases its corrosivity. In metal pipes,
chloride reacts with metal ions to form soluble salts, thus increasing levels of metals in drinking-water.
In lead pipes, a protective oxide layer is built up, but chloride enhances galvanic corrosion. It can also
increase the rate of pitting corrosion of metal pipes.

Chloride concentrations in excess of about 250 mg/liter can give rise to detectable taste in water, but
the threshold depends upon the associated cations. The toxicity of chloride salts depends on the cation
present; that of chloride itself is unknown. Although excessive intake of drinking-water containing
sodium chloride at concentrations above 2.5 g/liter has been reported to produce hypertension. Also, if
we drink chlorinated water then it may cause many health issues like diarrhea and stomach problems.

PROCEDURE:

For concentration, less than 100 mg/L:

 Take 50 mL of the sample in a clean titration flask.
 Add 0.5 mL of mixed indicator (di-phenyl carbazone + Xylene cyanol FF)
 Color of the solution turns to purple.
 Then add drop wise concentrated HNO3 till solution becomes colorless
 Titrate this solution by 0.0141 N Hg(NO3)2 in burette till color changes to deep violet, which
indicates the end point.
 Hg combines with diphenyl carbazone and gives purple color
 Repeat the titration three times (to get concordant readings) for each of the three samples and
a blank. And now note down volume of Hg (NO3) and label it as “A” mL.

For concentration, greater than 100 mg/L:

 Take 50 mL of the sample in a clean titration flask.

 Add 0.5 mL of mixed indicator (diphenylcarbazone + bromophenol blue)
Color of solution turns to purple.
 Add 0.5 N solution of nitric acid drop wise through pipette until the solution turns to yellow
color.
 Titrate this solution by 0.141 N Hg(NO3)2 in burette till color changes to purple, which
indicates the end point.
 Note down volume of Hg (NO3) and label it as “A” mL. Hg combines with diphenyl
carbazone and gives purple color.
 Repeat the titration three times (to get concordant readings) for each of the three samples and
a blank.
 Record the data and calculate the amount of chlorides as follows

For Blank Solution

Take 50mL of distilled water.
For concentration, less than 100 mg/L:
Add pinch of HCO3-1. Then add 1 mL of mixed indicator (di-phenylcarbazone + Xylene cyanol FF)
in it.
For concentration, greater than 100 mg/L:
Add 0.5 mL of mixed indicator (di-phenylcarbazone + Bromophenol) in it. After indicator addition
solution becomes blue color.
For concentration, greater than 100 mg/L:
Then add drop wise concentrated HNO3 till solution becomes colorless. Start titrating it against
0.0141N Hg (NO3) for concentration less than 100 mg/L and 0.141N Hg (NO3) for concentration
greater than 100 mg/L. Keep on adding till deep violet color appears. Note down volume of Hg
(NO3) and label it as “B” mL.

OBSERVATION & CALCULATIONS:

FOR SAMPLE # 1:

Titration No. Initial burette reading Final burette Volume of titrant

(mL) reading (mL) Used (mL)

01
02
03
Average vol. of titrant used                  

FOR SAMPLE # 2:

Titration No. Initial burette Final burette reading Volume of titrant used
Reading (mL) (mL) (mL)
01
02
03
Average vol. of titrant used                       

FOR SAMPLE # 3:

Titration no Initial burette Final burette reading Volume of titrant used

reading (mL) (mL) (mL)
01
02
03
Average of vol. used                     

Chlorides (mg/l) =

RESULTS:

Given water contains                 chlorides.

COMMENTS:
PRACTICAL # 3
TITLE:

Determination of hardness of water.

OBJECTIVE:

To determine the total hardness of water samples by EDTA titration / complexometric titration.

APPRATUS:

 Titration flask
 Burette
 Beaker
 50mL cylinder
 Pipette

CHEMICALS:

 De-ionized water
 Ammonia buffer
 Eriochrome black T powder
 NaOH
 Eriochrome black blue R indicator
 EDTA titrant

RELATED THEORY:

Hardness:

water hardness is the amount of dissolved calcium and magnesium in the water. Hard water is high in
dissolved minerals, largely calcium and magnesium .

Causes of hardness:
Hardness of water is mainly cause by the multivalent metallic cations. The principle cations are the
divalent calcium and magnesium ions.

Sources of hardness;
Water's hardness is determined by the concentration of multivalent cations in the water. Multivalent
cations are positively charged metal complexes with a charge greater than 1+. Usually, the cations have
the charge of 2+. Common cations found in hard water include Ca 2+ and Mg2+. These ions enter a water
supply by leaching from minerals within an aquifer. Common calcium-containing minerals
are calcite and gypsum. A common magnesium mineral is dolomite (which also contains
calcium). Rainwater and distilled water are soft, because they contain few ions.

Types of hardness:
There are two types of hardness:

Temporary hardness
Temporary hardness is a type of water hardness caused by the presence
of dissolved bicarbonate minerals (calcium bicarbonate and magnesium bicarbonate). When dissolved,
these type of minerals yield calcium and magnesium cations (Ca2+, Mg2+) and carbonate
and bicarbonate anions (CO32-)and HCO3−. The presence of the metal cations makes the water hard.
temporary" hardness can be reduced either by boiling the water, or by the addition of lime (calcium
hydroxide) through the process of lime softening. Boiling promotes the formation of carbonate from the
bicarbonate and precipitates calcium carbonate out of solution, leaving water that is softer upon cooling.

Permanent hardness
Permanent hardness (mineral content) is generally difficult to remove by boiling.[6] If this occurs, it is
usually caused by the presence of calcium sulfate/ calcium chloride and/or magnesium sulfate/magnesium
chloride in the water, which do not precipitate out as the temperature increases. Ions causing permanent
hardness of water can be removed using a water softener, or ion exchange column.
permanent hardness = permanent calcium hardness + permanent magnesium hardness.
Effects on Health;

Hard water has no known adverse health effect, WHO says at its Geneva Conference. In addition, hard
water, particularly very hard water, could provide an important supplementary contribution to total
calcium and magnesium intake. The health effects of hard water are mainly due to the effects of the salts
dissolved in it, primarily calcium and magnesium. To a large extent, individuals are protected from excess
intakes of calcium by a tightly regulated intestinal absorption mechanism through the action of 1, 25-
dihydroxy-vitamin D, the hormonally active form of vitamin D. Although, calcium can interact with iron,
zinc, magnesium, and phosphorus within the intestine, thereby reducing the absorption of these minerals.
On the other hand, the major cause of hypermagnesemia is renal insufficiency associated with a
significantly decreased ability to excrete magnesium. Increased intake of magnesium salts may cause a
change in bowel habits (diarrhea). Drinking-water in which both magnesium and sulfate are present in
high concentrations (~250 mg/l each) can have a laxative effect. Laxative effects have also been
associated with excess intake of magnesium taken in the form of supplements, but not with magnesium in
the diet.

PROCEDURE:

CALCULATING TOTAL HARDNESS:

 Take 25mL of sample solution in the clean titration flask with distilled de-ionized water. Dilute
the sample with 50mL by adding 25mL distilled de-ionized water.
 Add 1-2mL buffer solution (ammonia buffer) to maintain pH of solution to 7-9 into sample into
titration flask.
 Add a small quantity of eriochrome black t powder to the diluted sample which in the presence of
hardness ions gives wine-red color.
 Titrate it against 0.01M standard EDTA solution till the appearance of blue colour.
 Take at least three concordant reading by repeating the same experiment.

CALCULATING HARDNESS DUE TO Ca & Mg:

 Take 25mL of sample and dilute it to 50mL by adding 25mL distilled water to it.
 Add 2mL of 1M of NaOH solution in it.
 Add a small quantity of eriochrome black blue R indicator.
 Add EDTA titrant (0.1M EDTA) slowly with continuous stirring until the appearance of blue
color.
 Take at least three concordant reading by repeating the experiment.

OBSERVATION & CALCULATIONS:

WATER SAMPLE # 1

Titration No Initial burette reading Final burette reading Volume of EDTA used
(mL) (mL) (mL)
01
02
03
Avg. of vol. of EDTA                

WATER SAMPLE # 2

Titration No Initial burette reading Final burette reading Volume of EDTA used
(mL) (mL) (mL)
01
02
03
Avg. of vol. of EDTA                

WATER SAMPLE # 3

Titration no Initial burette reading Final burette reading Volume of EDTA used
(mL) (mL) (mL)
01
02
03
Avg. of vol. of EDTA             

Total hardness (mg/l) =

Ca+2 hardness =

Total hardness = calcium hardness + magnesium hardness

Magnesium hardness= total hardness – calcium hardness

RESULTS:

The total hardness in the given sample of water is             and the calcium and magnesium hardness in the
given sample of water is            

COMMENTS:
PRACTICAL # 4
TITLE:

Determine the sulfate concentration in water sample.

OBJECTIVE:

To determine the sulfate content in the given sample of water.

APPRATUS:

 Conical flask
 Turbidity meter
 Beaker
 Sample tube
 Spatula
 Wash bottle and tissue paper

RELATED THEORY:

Sulphate is a naturally occurring substance that contains Sulphur and oxygen. It is one of the major
component in rain and it is second most abundant anion in seawater. It has very high concentration in
seawater so it combines with other water cations such as sodium, magnesium, and calcium and forms
salts and basically these salts are soluble in seawater.

High concentration in water leads to Laxative effect due to the combination with cations such as calcium
and magnesium and these cations are also contributors of hardness. When these contributors combine
with sulphate, they form permanent hardness in seawater which cannot be remove by simple boiling. It
needs chemical treatment. Hydrogen sulphide is form when bacteria act on the sulphur and reduces it to
hydrogen sulphide and it smells like rotten egg.

Sulphur entered in water supplies:

Sulphate enters in our water supplies through minerals that contains sulfate are sodium sulfate (Glauber’s
salt), magnesium sulfate (Epsom salt), and calcium sulfate (Gypsum), Water moves through these rocks
and get involved in water supplies.

Health risks for humans:

Sulphate is generally considered to be non-toxic. The consumption of drinking water containing high
amounts of magnesium or sodium sulphate may result in intestinal discomfort, diarrhea and consequently
dehydration. High amounts of various sulphate salts may give drinking water an offensive taste.
Depending upon the type of sulphate salt(s) present in the water, most people begin to notice an offensive
taste at concentrations ranging from 250 to 1,000 mg/L

Environmental Effects:
Sulfates occur as microscopic particles (aerosols) resulting from fossil fuel and biomass combustion.
They increase the acidity of the atmosphere and form acid rain. The anaerobic sulfate-reducing
bacteria Desulfovibrio  desulfuricans and D. vulgaris can remove the black sulfate crust that often tarnishes

Principle:
This turbidimetric method of determining sulfates is based upon the fact that barium sulfates tend to
precipitate in a colloidal form of uniform size.

SO4-2 +BaCl2  BaSO4

PROCEDURE:

 Stock solution was prepared in the calibration flask.

 Prepare 100ppm solution of SO4-2 in 100mL.
 CuSO4.5H2O: SO4-2
 249.5: 96
X: 100
 X = 259.89
 So, 259.85 mg CuSO4.5H2O required to dissolve 1000mL of water to make 100ppm SO4-2
solution.
 Now we have to prepare in 100mL flask so divide by 10.
 259.89/10 =1000/10
 So, 25.9mg CuSO4.5H2O is required to make 100mL solution. This gives 100ppm SO4-2 stock
solution.
 The calibration solutions were made up of 0,10,20,30,40 ppm.

Concentration Vol. from stock BaCl2 mL Distilled water Total volume Ml

ppm solution Ml mL
C1V1=C2V2
10 100*V1=10*100 10 80 100
V1=
10mL

 Now solutions are ready for calibration curve. For calibration curve , we will take unit as mg/l.
 Now determine the turbidities of all. Completely fill quartz cell with the calibration sample.
Using values draw standard graph.

OBESRVATION & CALCULATIONS:

Concentration (ppm) Turbidity (NTU)

RESULTS:
COMMENTS:
Practical # 5

TITLE:

Determine the percentage amounts of NaCl AND KCl in a mixture of the two salts by MOHR’S
method.

OBJECTIVE:

To determine the % amount of NaCl and KCl in a mixture of two salts by Mohr’s method.

APPARATUS:

 Burette
 Pipette
 Titration flasks

CHEMICALS:

 Sample of salt mixture (NaCI & KCI)

 Standard solution of 0.1M AgNO3
 K2CrO4 as an indicator

RELATED THEORY:

PROCEDURE:

 Weight  10.00 g of the salt mixture and transfer to 0 1000.0 mL volumetric flask.
 Add about 100 ml distilled water and swirl the flask to dissolve the salt.
 Then add more distilled water to bring the solution upto 1000.0 ml mark.
 The concentration of the solution will be 0.01 g/mL.
 Pipette out 10 mL of salt solution, which will have 0.1 g of salt mixture, in a titration flask and
add 2 drops of potassium chromate indicator to make it mixture of two salts.
 Titrate it against AgNO3 solution till the appearance of brick red precipitates.
 Repeat the process and get three concordant readings.
 Calculate the percentage amount of KCl and NaCl in the given mixture of given salt.

OBSERVATION & CALCULATIONS:

Sr.No Initial burette reading Final burette reading Vol of AgNO3 used
(mL) (mL) (mL)
1
2
3
Average volume of titrant used (Vavg)
Molarity of AgNO3 solution: M1= 0.1M

Volume of AgNO3 solution used=V1 = YmL

Molarity of salt mixture (NaCl & KCI) solution= M2= ?

Volume of salt mixture (NaCl & KCI) solution used=V 2= 10mL

By formula M1V1/n1=M2V2/n2

n1=n2

M2=M1V1/V2

M2=A

Molarity of (NaCl + KCl)=M2=Moles/volume in litres =A

Moles of 1L solution= M2 x Volume in liter (1000mL)

Calculations for 10ml solution:

Moles of 10ml solution= M2 x 10ml/1000(mL/L)

= 0.01A (moles/liter)

Amount of salt mixture in 10ml solution= 0.1g

Let Amount of NaCl in mixture=X

Amount of KCI in mixture= 0.1g-X

Moles of KCl +Moles of NaCl =Moles of 10ml solution= (KCI + NaCl)

(KCL in g/ (Molar mass of KCI)) + (NaCl in g/Molar mass of NaCl) =0.01A

(0.1-X /74.5 + X/58.5)= 0.01A

X=B

%age of NaCl= (X/0.1) × 100: X1%

%age of KCI=(0.1-X/0.1g) x 100: X2%

RESULTS:
%age of KCl= X2%

COMMENTS:
Practical#6

TITLE :

Determine the amount of free alkali (Percentage) in a soap sample.

OBJECTIVE:

To determine the % amount of free alkali in a given sample of soap.

APPARATUS:

 Burette
 Pipette
 Titration flasks
 Beakers

CHEMICALS:

 Soap samples
 0.01M HCI
 Phenolphthalein

RELATED THEORY:

PROCEDURE:

 Weight out 10.00 g laundry soap and transfer it into a beaker containing 150 mL distilled water.
 Heat for 30 min to dissolve soap into water.
 Transfer the prepared soap solution along with washings into a 250.0 mL volumetric flask and
make up the volume by adding distilled water up to the mark.
 Avoid shaking as that can produce froth (foaming) which can lead to wrong results.
 Take 10.00 mL of soap solution into a titration flask.
 Add 2 drops of indicator to it. Color will be changed to pink.
 Titrate it against 0.01 M HCI solution, taken in the burette, till solution become colorless.
 Repeat the procedure and take three readings.
 Repeat experiment for 3 different soap samples.

OBSERVATION & CALCULATIONS:

Sr.No Initial burette reading Final burette reading Vol of acid used
(mL) (mL) (mL)
1 0 10 10
2 10 20 10
3 20 30 10
Average volume of titrant used (Vavg) 10

Molarity of HCI solution= M1= 0.01M

Volume of HCI solution used=V1 = 10ml

No. of moles of HCI taking part in the reaction=n1=1

Molarity of NaOH solution=M2= ?

Volume of NaOH solution used=V2= 10ml

No. of moles of NaCI taking part in the reaction=n2=1

(M1V1)/n1=(M2V2)/n2

M2=(M1V1)/n1n2/V2

M2=0.01 M

Molarity of NaCI solution=0.01M

Moles of alkali NaOH = Molarity (M2) x Volume (L) = 0.01 x 0.25=0.0025

Moles = (Mass in g of NaOH)/Molar Mass

Molar mass in g of alkali (NaOH)= Moles x Molar Mass= 0.0025 x 40= 0.1g

%age of free alkali in soap= (free alkali in g)÷(soap in g )× 100.

%age of free alkali in soap=(0.1g÷10g )× 100

%age of free alkali in soap: 1%

RESULTS:

% of free alkali in soap= 1%

COMMENTS:
Practical# 7

TITLE:

Separate the mixture of liquid by paper chromatography.

OBJECTIVE:

To separate the liquid mixture by paper chromatography technique.

APPARATUS:

 Whatman's filter paper No.1

 capillary tube
 Beaker
 Thread & clips for hanging

CHEMICALS:

 Mixture of different inks

 solvent (water)

RELATED THEORY:

PROCEDURE:

 Take a solvent mixture (water) in beaker.

 Take 20cm long strip of Whatman's filter paper no. i and draw a pencil line at 2.5cm from one
end of paper strip.
 Spot a point of mixture solution (inks) in the center of pencil drawn line with the help of capillary
tube.
 Dry the spot and suspend the strip in beaker with the help of thread in such a way that lower end
dips into the solvent without touching the bottom. Note that spot remains out of the solvent .
 After some time solvent rises due to capillary action and the components get separated out as they
rises up with solvent at different rates.
 When the solvent covers 3/4th length of paper strip, then remove the strip.
 Mark the position of solvent (solvent front) with the help of pencil and dry the strip.
 The pattern on the paper is called chromatogram.

OBSERVATION & CALCULATIONS:

Note down the distance from base line to solvent front with the help of scale i.e., 81mm.

Mark center of each color and measure distance for each ink mark  from base line. For purple is 65mm
Component name Distance of solvent Distance of component RF (2/1)
from baseline (cm) from baseline (cm)
1 2
Red 15 8.5 0.56
Blue 15 10.5 0.7
Green 15 7.5 0.5
Purple 15 4.2 0.28

RESULTS:

Rf value of red is 0.56 , blue is 0.7 , green is 0.5 and purple is 0.28.

COMMENTS: