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Chemistry Lab Manual & Record Book

JAIN COLLEGE OF ENGINEERING, BELAGAVI

Department of Chemistry

CHEMISTRY LABORATORY MANUAL

Subject Code: BCHES202/BCHEC202

(For CSE & CV Streams of Engineering)

NAME

USN

ROLL NO

DIVISION

BRANCH

SEMESTER
Chemistry Lab Manual & Record Book

INDEX

Sl. No. Experiment

1 Conductometric estimation of acid mixture

2 Determination of pKa of vinegar using pH sensor (Glass electrode)

3 Potentiometric estimation of FAS using K2Cr2O7

Estimation of Copper present in electroplating effluent by optical sensor


4
(Colorimetry)

5 Determination of Viscosity coefficient of lubricant (Ostwald’s viscometer)

6 Estimation of total hardness of water by EDTA method

Determination of Chemical Oxygen Demand(COD) of industrial waste water


7
sample

8 Estimation of iron in TMT bar by diphenyl amine/external indicator method

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Chemistry Lab Manual & Record Book

CONDUCTOMETRIC ESTIMATION OF ACID MIXTURE

Experiment No: 1 Date: .................................

Aim: Estimation of a strong acid (e.g. HCl) and a weak acid (e.g. CH3COOH) from
given mixture by conductometric titration.

Procedure: (This is to be written during the lab session ONLY)

Pipette out specified volume of acid mixture solution into a clean

100 mL Beaker. Dip the conductivity cell into it and connect it to the

conductivity bridge. Note down the specific conductance of this solution.

Add standard sodium hydroxide from the burette in increments of 0.5 mL

and measure the corresponding specific conductance. Record six readings

when specific conductance increases significantly (i.e. after the

neutralization of weak acid).

Plot a graph of specific conductance versus volume of NaOH. From

this graph, find out the neutralization points for strong and weak acids and

calculate their strength and amount.

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Chemistry Lab Manual & Record Book

Observations and Calculations:

Volume of acid mixture taken (Vmix) = …..……… mL

Strength of NaOH solution = N

Specific
Volume of NaOH
conductance
(mL)
(S / cm)
0.0
0.5

1.0

1.5

2.0

2.5

3.0

3.5

4.0

4.5

5.0

5.5

6.0

6.5

7.0

7.5

8.0

8.5

9.0

******

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Chemistry Lab Manual & Record Book

pKa OF VINEGAR
Experiment No: 2 Date: ...........................

Aim: Determination of pKa of vinegar using pH meter.

Procedure: (This is to be written during the lab session ONLY)

Pipette out specified volume of vinegar into a 100 mL beaker.

Immerse the combined glass electrode assembly into it and connect to a

calibrated pH meter and record the pH. Add NaOH in increments of 0.5 mL

and record the corresponding pH after mixing the solution thoroughly.

Sharp increase in pH indicates completion of neutralization reaction. From

this point onwards record six more readings.

Plot graphs of ∆pH / ∆V versus volume of NaOH and pH versus

volume of NaOH to determine pKa of given weak acid.

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Chemistry Lab Manual & Record Book

Observations and Calculations:

Volume of vinegar taken =...................Ml

Volume of pH ∆pH ∆V ∆pH / ∆V


NaOH (mL)
0.0 ----- ----- -----
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0

****

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Chemistry Lab Manual & Record Book

POTENTIOMETRIC ESTIMATION OF FAS


Experiment No: 3 Date: ............................

Aim: Potentiometric estimation of FAS using standard potassium dichromate


solution of ………….. N.

Procedure: (This is to be written during the lab session ONLY)

Pipette out specified volume of FAS solution into a 250 mL beaker

and add 25 ml of dil. H2SO4. Immerse calomel electrode and platinum

electrode assembly into the beaker. Connect this assembly to the

potentiometer and measure the potential. Add standard potassium

dichromate from the burette in increments of 0.5 mL and measure the

corresponding potential after thorough mixing. Take six readings after

sharp increase in the potential.

Plot a graph of ∆E/∆V versus volume of K2Cr2O7 and determine the

equivalence point. Knowing the strength and volume of K 2Cr2O7, the

normality & amount of FAS in the given solution is calculated.

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Chemistry Lab Manual & Record Book

Observations and Calculations:

Volume of FAS solution taken =...................mL

Normality of K2Cr2O7 =................... N

Volume of E (mV) ∆E ∆V ∆E / ∆V
K2Cr2O7 (mL)
0.0 ----- ----- -----
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0

******

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Chemistry Lab Manual & Record Book

ESTIMATION OF COPPER BY COLORIMETRY


Experiment No: 4 Date: ...........................

Aim: Estimation of copper in copper sulphate solution using photoelectric


colorimeter.

Procedure: (This is to be written during the lab session ONLY)

Using burette, add 5, 10, 15, 20 and 25 mL of copper sulphate

solution into five separate 50 mL volumetric flasks. Further, add 10 mL of

ammonia solution to each flask and make up to the mark with distilled

water and mix well. Blank solution is prepared by adding 10 mL of

ammonia solution to an empty 50 mL standard flask and make up to the

mark with distilled water and mix well.

Blank solution is taken in a Nessler tube and placed inside

photoelectric colorimeter. The variable diaphragm is adjusted to get zero

absorbance at 610 nm. The absorbance of each of the standard solution and

also for the test solution is measured. A graph of absorbance (OD) against

concentration is plotted and concentration of test solution is determined.

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Chemistry Lab Manual & Record Book

Observations and Calculations:

Concentration of CuSO4.5H2O solution =…..……………. M (X)

Volume of CuSO4 Concentration of Cu2+ (ppm)


solution in 50 mL
Sl. No. Concn=(X × V × 1000 × 63.54) / Absorbance
volumetric flask (‘V’
mL) 50

1 5

2 10

3 15

4 20

5 25

6 Test Solution By graph:

*****

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Chemistry Lab Manual & Record Book

VISCOSITY COEFFICIENT OF A LUBRICANT

Experiment No: 5 Date: .............................

Aim: Determination of coefficient of viscosity of a lubricant using Ostwald’s


viscometer.

Procedure: (This is to be written during the lab session ONLY)

Clamp vertically a clean & dry Ostwald’s viscometer. Fill the given

liquid to ¾ of the bulb B. Suck the liquid into the bulb A, so that the level

rises above the mark ‘x’ and allow it to flow down to bulb B through the

capillary tube. Start a stop-watch as the liquid level touches mark ‘x’, and

stop it when it crosses mark ‘y’. Note down the flow time and repeat the

procedure.

Clean the viscometer with acetone and dry it. Fill the viscometer with

same volume of distilled water and repeat the above method to get flow

time and calculate ηl.

Observations and Calculations:

Room Temperature = ............................ °C

Density of given liquid, dl = ............................ g/cm3

Density of water, dw = ........................... g/cm3

Viscosity of water, ηw = ........................... mP

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Chemistry Lab Manual & Record Book

Flow time (seconds)

Trial No.

For Liquid, tl For water, tw

Average

*****

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Chemistry Lab Manual & Record Book

TOTAL HARDNESS OF WATER

Experiment No: 6 Date: ..............................

Aim: Estimation of total hardness of water by EDTA complexometric method.

Procedure: (This is to be written during the lab session ONLY)

I. Preparation of standard EDTA solution:

 Dissolve accurately weighed EDTA disodium salt in 10 mL of ammonia

solution and transfer it into 250 mL standard flask.

 Then dilute it up to the mark with distilled water and mix thoroughly for

uniform concentration. Fill the burette with this solution.

II. Estimation of hardness of water:

 Pipette out 25 mL of given hard water into a clean conical flask.

 Add 10 mL of NH4Cl-NH4OH buffer to maintain pH of about 10 which is

required for stable EBT-Ca2+/Mg2+ complex (wine red color).

 Add a pinch of Eriochrome Black-T indicator.

 Titrate this solution against standard EDTA solution until wine red colour

changes to clear blue.

 Record the reading and repeat the titration for agreeing values.

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Chemistry Lab Manual & Record Book

Observations and Calculations:

Preparation of standard EDTA solution:

Mass of EDTA dissolved in 250 mL =…………………….. (W) g

Molarity of EDTA solution, MEDTA = (W × 4) / 372.24 = ---------------------------


(Mol. Wt. of EDTA is 372.24)

= ………………………. M (X)

Estimation of Total Hardness:

Burette :

Conical flask :

Indicator :

End Point :

Trial No. 1 2 3

Final burette reading (ml)

Initial burette reading (ml)

Difference (ml)

Agreeing value, V1 = ........................ mL

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Chemistry Lab Manual & Record Book

DETERMINATION OF CHEMICAL OXYGEN DEMAND OF


INDUSTRIAL WASTE WATER

Experiment No: 7 Date: ................................

Aim: To determine the chemical oxygen demand (COD) of the given industrial
waste water, using K2Cr2O7 solution supplied and pure solid Mohr’s salt.

Procedure: (This is to be written during the lab session ONLY)

I. Preparation of standard Mohr’s salt solution:

 Dissolve accurately weighed Mohr’s salt in 10 mL of dil. H2SO4 and transfer

into a 250 mL standard flask.

 Then dilute the solution up to the mark with distilled water and mix

thoroughly for uniform concentration. Fill the burette with this solution.

II. Back titration:

 Pipette out 25 mL of waste water into a conical flask.

 Add 25 mL of potassium dichromate solution by means of pipette, 25 mL

of 1:1 H2SO4 and 2 drops of Ferroin indicator.

 Titrate this solution with standard Mohr’s salt solution until the colour

changes to reddish brown. Record the reading and repeat the titration for

agreeing values.

III. Blank Titration:

 Pipette out 25 mL of potassium dichromate solution into a conical flask.

 Add 25 mL of 1:1 H2SO4 and 2 drops of Ferroin indicator.

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Chemistry Lab Manual & Record Book

 Titrate this solution with standard Mohr’s salt solution until the colour

changes to reddish brown. Record the reading and repeat the titration for

agreeing values.

Observations and Calculations:

Preparation of Mohr’s salt solution:

Mass of Mohr’s salt dissolved (W) =…………………….. g

Normality of Mohr’s salt solution, NMohr salt = [W × 4] / 392 = -------------------------


(Mol. Wt. of Mohr’s salt is 392)

= .......................... N (X)

Back Titration:

Burette :

Conical flask :

Indicator :

End Point :

Trial No. 1 2 3

Final burette reading (ml)

Initial burette reading (ml)

Difference (ml)

Agreeing value, V1 = ........................ mL

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Chemistry Lab Manual & Record Book

Blank Titration:

Burette :

Conical flask :

Indicator :

End Point :

Trial No. 1 2 3

Final burette reading (ml)

Initial burette reading (ml)

Difference (ml)

Agreeing value, V2 = ........................ mL

*****

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Chemistry Lab Manual & Record Book

ESTIMATION OF IRON IN TMT BAR


Experiment No: 8 Date: ........................

Aim: Estimation of percentage of iron in the given solution using standard


potassium dichromate solution (External indicator method)

Procedure: (This is to be written during the lab session ONLY)

I. Preparation of standard K2Cr2O7 solution:


 Dissolve accurately weighed potassium dichromate in distilled water and
transfer into a 250 mL standard flask.

 Dilute the solution up to the mark with distilled water and mix well for
uniform concentration. Fill the burette with this solution.

II. Estimation of iron:


 Pipette out 25 mL of iron solution into a conical flask.

 Add 10 mL of HCl solution and heat to boiling.

 To this hot solution, add SnCl2 (to reduce Fe3+ to Fe2+) solution drop wise
until the discharge of yellow colour. Add one or two drops of SnCl2 in
excess.

 Cool this solution to room temperature and add 10 mL saturated HgCl 2


solution (to remove excess SnCl2). Observe the formation of silky white
precipitate (Hg2Cl2) in the solution.

 If no precipitate or black precipitate appears, reject it and repeat the


above process with fresh iron solution.

 Then titrate above solution with standard K 2Cr2O7 solution, until a drop of
the titrated solution fails to give blue precipitate or green colour with a
drop of indicator taken on a wax paper / porcelain tile.

 Record the reading and repeat the titration for agreeing values.

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Chemistry Lab Manual & Record Book

Observations and Calculations:

Weight of rust in 250 mL of given solution= (a) = …………….g (Given)

Preparation of K2Cr2O7 solution:

Mass of K2Cr2O7 dissolved (W) =…………………….. g

Normality of K2Cr2O7 solution, NK2Cr2O7 = [W × 4] / 49 = ---------------------------


(Equiv. Wt. of K2Cr2O7 is 49)
= .......................... N (X)
Estimation of iron in haematite :

Burette :

Conical flask :

Indicator :

End Point :

Trial No. 1 2 3

Final burette reading (ml)

Initial burette reading (ml)

Difference (ml)

Agreeing value, VK2Cr2O7 = ........................ mL

*****

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