General Instructions for Chemistry Laboratory

1. Students are instructed to come to Engineering Chemistry laboratory in time. Late

comers are not entertained in the lab.
2. Students are expected to come prepared at home with the experiments which are going to
perform.
3. Students are instructed to wear their identity cards and apron before entering into the lab.
4. Students are instructed not to bring mobile phones to the lab.
5. The glass apparatus and other instruments used in Engineering Chemistry lab should be
handled with care and responsibility.
6. Any damage of glassware and equipment during the lab session is student’s responsibility
and penalty or fine will be collected from the student.
7. Do not throw waste such as match sticks, filter papers etc. into the sink. They must be
thrown into the waste bin.
8. Keep the water and gas taps closed except when these utilities are needed.
9. Replace the reagent bottles on the reagent shelves immediately after use. They must
never be allowed to accumulate on the bench.
10. Students should update the records and lab manuals session wise. Before leaving the lab
the student should get his lab manual signed by the faculty.
11. Students should not move around in the lab.
12. If any emergency, the student should take the permission from faculty member concerned
in written format.
13. The faculty members have the authority to suspend any student from the lab session on
disciplinary grounds.
14. Never cook the result by recording false observations or by making manipulated
calculations.

Miscellaneous Policies and Procedures

Laboratory note book:

i. The one essential tool for any laboratory worker in any field is the laboratory
notebook. Its main purpose is to record observations, variations in procedures,
experimental results, conclusions and supplementary information from texts,
handbooks, and other printed source.
ii. Never attempt to remove the pages from the notebook nor to erase the entries. Simply
cross out neatly any entry you wish to delete and give the page reference for the
correction or type in the correction.
iii. Label the notebook on the outside and inside the front cover with your name, roll
number, batch number.
iv. Leave the first one or two pages blank for a Table of Contents which you must keep
up to date each week.
v. Always read the upcoming experiments carefully and thoroughly, being sure to
understand of the directions before entering the lab.
vi. It is essential that you come to the laboratory with a schedule of operations planned in
advance, and with all tables, equations, etc. completed. Tables for the recording of
observations should be clearly and neatly set-up advance.
vii. Take data during lab. Not after lab, on the assumption that it will be neater. Put data
directly in your lab book rather than transcribing from another source (e.g., notebook
or lab partner).

Homework and Lab Report Due Dates:

Lab reports are due one week from the date of performance, at the beginning of the lab
period. Only a verifiable illness (Doctor’s note) or prior permission of the instructor
counts as excused absences. Unexcused lab reports will receive a grade of zero.

Lab Partners:

For those experiments where students are to work in pairs, lab partners will be assigned
randomly as announced by the instructor at the beginning of the lab period. You may not
exchange lab partners. Both lab partners must be present for the entire experiment.

Copying:

All lab reports are to be your own. Lab partners are to independently produce their lab
reports. It is very easy for the grader to spot identical work among two or more students.
In the event of copying, all students involved will receive a grade of zero; therefore do
not give a copy of your lab report to another student.
Safety Instructions for Chemistry Laboratory

1. State-approved safety goggles must be worn in the laboratory at all times.

2. You must dress appropriately for the laboratory. Lab coats are required to be worn. Bare
feet, sandals, or other open-toed shoes are not permitted in the laboratory. Shorts and
short skirts are likewise not permitted; legs must be covered to below the knees.

3. Long hair should be tied back.

4. Learn the location and operation of the safety showers, emergency eyewashes and fire
extinguishers in the laboratory. In the case of spill onto a person or clothing, the
immediate action should be to flush with water and lots of it.

5. The fire extinguishers should only be used for real emergencies since the chemicals they
contain can cause considerable damage.

6. Become familiar with all of the exits from the laboratory.

7. Never attempt any unauthorized or unassigned experiments. Follow the experimental

procedures explicitly, checking and double-checking the identity of all reagents before
you use them.

8. Clean up spills immediately. The next person to come along has no way of knowing if the
clear liquid or white powder on the lab bench is innocuous or hazardous. Neutralize acid
spills with sodium bicarbonate (baking soda) before cleaning them up. Spills of sulfuric
acid solutions are particularly hazardous since only the water will evaporate, thereby
making the solution more concentrated upon standing.

9. Never return unused reagents to their storage container. If you take more than you need,
dispose of the excess in the appropriate manner. Use the reagents sparingly—they are
expensive and time-consuming to prepare.

10. Do not pick up hot objects. Be sure your apparatus is cool before picking it up. Do not
point the open end of a test tube or other vessel containing a reaction mixture toward
yourself or anyone else. If the procedure calls for you to observe the odor of the contents
of a vessel, hold it upright in front of you, gently fan some of the vapors toward your
nose and sniff cautiously. Most chemical vapors are at least irritating, and many are quite
toxic. Please do not taste any chemicals.

11. Do not eat, drink or smoke in the laboratory.

12. Playing of radios, tapes, CDs is not permitted. This includes small portable devices
used with earphones or headsets.
13. Keep coats, backpacks and other non-essential materials away from areas where people
are working.

14. Dispose of all broken glassware and other sharp objects in the cardboard glass disposal
boxes. Custodial personnel will stop collecting trash after they find broken glass in the
trashcans.

15. Wash hands often when working in lab, and always wash thoroughly before leaving.

16. Use the hood for evaporation of anything other than water. The vapors from your
procedure alone may not present a problem but those from all the students in the lab
could combine to create a hazard.

17. Do not leave a Bunsen burner or other heated apparatus unattended. The person working
next to you may not know what is involved with your setup and may be working with a
flammable material. Turn off open flames if you must leave your area. Make sure the gas
taps are completely off whenever the Bunsen burner is not lit.

18. Waste Disposal: Dispose of chemical reagents and other materials properly. The proper
disposal of chemical wastes is essential to the health and safety of Institute faculty, staff,
students and the surrounding community.

19. Chemical wastes must be managed and discarded in the most responsible and
environmentally sound method available.

20. Never use reagents from an un marked bottle.

21. If a fire is occurred in a beaker or some other container, cover it with a glass dish or other
flame-retardant item.
22. Notify instructor immediately in case of an accident.
Safety measures in accidental case

1. Eye accidents:

Flood your eyes immediately with water. For an acid, use dilutes Sodium bicarbonate
solution; for an alkali, use dilute boric acid solution.

2. Burns:

Acid burns: wash immediately with large quantity of water, then with dilute (8%) sodium
bicarbonate solution. If burn is severe, wash again with water and apply the acriflavine.
Alkali burns: wash immediately with water and 1% acetic acid solution.
Bromine burns: wash immediately with ample supply of petrol, when the bromine will be
completely removed from skin.
Organic substance: wash immediately with soap and warm water.

3. Cuts:

Wash the wound with sterile gauze, soap and water. Disinfect with an antiseptic and
apply a bandage.

4. Reagents in mouth:

If the reagents is in the mouth and not swallowed then spit out at once, wash the mouth
out repeatedly with water.
If the substance like acid or alkali is swallowed, dilute by drinking much water. Then for
acids follow by drinking much lime water. Milk may be given but not emetics.
For salts of heavy metals give milk or white of egg.
For arsenic or mercury compounds give emetic without any delay.

5. Gas poisoning:

Remove patient to fresh air and loosen clothing at neck. If breathing has stop give
artificial respiration until the doctor arrives.
List of Experiments

1. To determine the strength of given unknown ferrous ammonium sulphate solution by titrating
against standard N/40 K2Cr2O7 using diphenylamine as an internal indicator.

2. To determine the strength of given unknown ferrous ammonium sulphate solution by titrating
against standard N/40 K2Cr2O7 using potassium ferricyanide as an external indicator.

3. To determine the total, permanent and temporary hardness of given water sample by
complexometric titration using EDTA solution.

4 To determine the strength of sodium carbonate and sodium hydroxide in given alkali mix.
(water sample) hydrochloric acid is used as an intermediate solution, methyl orange and
phenolphthalein used as indicators.

5. To determine the strength of ferrous Ammonium Sulphate by titrating against KMnO4

solution.

6. To prepare urea formaldehyde resin.

7. To determine the strength of given HCl solution using a standard NaOH solution by
performing a pH-metric titration.

8. To determine the strength of given HCl solution using a standard NaOH solution by
performing a conductometric titration.

9. To determine the strength of given CH3COOH solution using a standard NaOH solution by
performing a pH-metric titration.

10. To determine the strength of phosphoric acid solution with 0.2N NaOH solution pH
metrically and verify that it is a tribasic acid.

11. Titrate a mixture of strong acid HCl and weak acid CH3COOH and determine the unknown
strength of HCl and CH3COOH pH-metrically.

12. To determine the equivalent conductance of given an electrolyte.

13. To determine the viscosity of a given lubricating oil at various temperatures using Redwood
Viscometer No. 1 or No. 2.

14. To determine cloud and pour point of a given sample of lubricating oil using cloud and pour
point apparatus.

15. To determine the water equivalent of benzoic acid by Using Bomb calorimeter.
EXPERIMENT: 1 Date:

Object: To determine the strength of given unknown ferrous ammonium sulphate (FAS)
solution by titrating against standard N/40 K2Cr2O7 using diphenylamine as an internal indicator.

Principle: K2Cr2O7 acts as an oxidizing agent in the presence of dil. H2SO4

K2Cr2O7 + 4 H2SO4 K2SO4 + Cr2 (SO4)3 + 4 H2O + 3 (O)
The liberated (O) oxidize ferrous ion to ferric ion.
6 FeSO4 + 3 H2SO4 + 3 (O) 3 Fe2 (SO4)3 + 3 H2O
-2 + +2
Cr2O7 + 14 H + 6 Fe 2 Cr+3 + 6 Fe+3 + 7 H2O

The complete reaction is

6 [FeSO4. (NH4)2 SO4.6H2O] + K2Cr2O7 + 7H2SO4
3 Fe2 (SO4)3 + K2SO4 + Cr2(SO4)3 + 6 (NH4)2SO4 + 43H2O
The color exhibited by diphenylamine change from greenish to purple at the end point.

Procedure:

Standardization of K2Cr2O7 solution:

1. Firstly wash all the apparatus with distilled water

2. Rinse and fill the burette with K2Cr2O7.
3. Pipette out 10 ml N/40 FAS solution into conical flask.
4. Add 5 ml of mixture [dil. H2SO4 + H3PO4] into conical flask.
5. Now add 2-3 drops of indicator, diphenylamine to the solution
6. Titrate the FAS solution with K2Cr2O7 solution from the burette.
7. At the end point, color of the solution will turn to purple blue from light green.
8. Note the burette reading and repeat the titration until two concordant readings are
obtained.

Estimation of ferrous ammonium sulphate:

Follow the same procedure for the unknown FAS solution.

Observations:

Standardization of K2Cr2O7:

Sr.No. Volume of Burette reading (ml) Volume of Concordant

FAS solution K2Cr2O7 readings
taken (ml) Initial Final consumed (ml) (ml)

Estimation of unknown FAS solution:

Sr.N Volume of Burette reading (ml) Volume of Concordant

o. FAS solution K2Cr2O7 readings
consumed (ml) Initial Final consumed (ml) (ml)

Calculations: The equivalent weight of FAS = 392

Standardization of K2Cr2O7 solution:

N1V1 = N2V2

N1 = Normality of ferrous ammonium sulphate solution (N/40)

V1 = Volume of ferrous ammonium sulphate solution

N2 = Normality of potassium dichromate solution

V2 = Volume of potassium dichromate solution

N2 = N1V1/V2

N2 = ------------N

Estimation of Ferrous ammonium sulphate:

N3V3 = N4V4

N3 = Normality of ferrous ammonium sulphate solution

V3 = Volume of ferrous ammonium sulphate solution

N4 = N2 = Normality of potassium dichromate solution

V4 = Volume of potassium dichromate solution

N3 = N4V4/V3

N3 = -----------N

Strength = N3 × Equivalent weight of FAS

= N3 × 392

= -------------gm./L

Result: The strength of given unknown ferrous ammonium sulphate solution = ----------- g/L

Precautions:

1. Potassium dichromate acts as an oxidizing agent in acidic medium, add some dil. H2SO4.
2. End point should be observed carefully.
EXPERIMENT: 2 Date:

Object: To determine the strength of given unknown ferrous ammonium sulphate solution by
titrating against standard N/40 K2Cr2O7 using potassium ferricyanide as an external indicator.

Principle: The oxidizing agent K2Cr2O7 in presence of dil. H2SO4 gives three atoms of nascent
oxygen [O]

K2Cr2O7 + 4 H2SO4 K2SO4 + Cr2 (SO4)3 + 4 H2O + 3 [O]

The liberated [O] oxidizes ferrous ion (Fe+2) to ferric ion (Fe+3)
6 FeSO4 + 3 H2SO4 + 3 [O] 3 Fe2 (SO4)3 + 3 H2O
The complete reaction is:
6 [FeSO4.(NH4)2SO4.6H2O] + K2Cr2O7 + 7 H2SO4
3 Fe2(SO4)3 + K2SO4 + Cr2(SO4)3 + 6 (NH4)2SO4 + 43 H2O
Or ionically,
Cr2O7-2 + 14 H+ + 6 Fe+2 2 Cr+3 + 6 Fe+3 + 7 H2 O
The end point on potassium dichromate titration is usually determined by using two types of
indicator, external and internal. External indicator was once employed when no internal indicator
was available. Here the indicator cannot be added to the solution to be titrated, but is placed in
the depressions of a white glazed tile. About 0.1 % solution of potassium ferricyanide acts as
external indicator. Freshly prepared potassium ferricyanide indicator is used because the old
solution of it becomes contaminated with potassium ferrocyanide. The use of potassium
ferricyanide as an external indicator is the best known example in the titration of iron with
dichromate. As long as ferrous ion is present in the titration mixture, the indicator will turn blue
on the transfer of solution. The appearance of blue color is due to the formation of
ferroferricyanide (Turnbull’s blue) according to following reaction:

2 K3Fe(CN)6 + 3 FeSO4 Fe3[Fe(CN)6]2 + 3K2SO4

Ferroferricyanide
(Dark blue complex)

Usually at the end point (all Fe+2 ions are oxidized to Fe+3) the color of the indicators drop
becomes light brownish yellow due to reaction of indicator with Fe+3 ions to produce brown
colored ferricferricyanide complex.

Fe2(SO4)3 + 2 K3[Fe(CN)6] 3 K2SO4 + 2 Fe[Fe(CN)6]

Ferricferricyanide
Brownish yellow
Thus, at the end point, the indicator fails to produce blue color when treated with a drop of
titration mixture.

Reagents: Ferrous ammonium sulphate solution, N/40 potassium dichromate solution, 0.1 %
solution of potassium ferricyanide, dil. Sulphuric acid.

Apparatus: Burette, pipettes, conical flask, glass rod, funnel, white glazed tile, test tubes.

Procedure:

Standardization of K2Cr2O7 solution:

1. Wash all the apparatus with distilled water.

2. Rinse and fill the burette with N/40 K2Cr2O7 solution.
3. Pipette out 10 ml of FAS solution (N/40) in a clean conical flask and add 5 ml of dil.
H2SO4.
4. Put a series of drops of indicator (potassiumferricyanide solution) with the help of glass
rod on a white tile.
5. Titrate the FAS solution against K2Cr2O7 solution.
6. Near end point, take a drop of titration mixture and put it on one of indicators drops on
tile and see the color.
7. A strong blue color will be produced. Continue the titrations and repeat the process at
different intervals and when the color of indicator drop does not give blue color, the end
point is reached.
8. Note the reading of the burette and repeat the titration until two concordant readings are
obtained.

Estimation of FAS:

Follow the same procedure for the unknown FAS solution.

Observations: Standardization of K2Cr2O7 solution:

Sr. No. Volume of Burette Readings (ml) Volume of K2Cr2O7 Concordant

Initial Final
FAS taken (ml) consumed (ml) Reading(ml)
Estimation of Ferrous ammonium sulphate:

Sr. No. Volume of Burette Readings (ml) Volume of K2Cr2O7 Concordant

FAS taken (ml) Initial Final consumed (ml) Reading (ml)

Calculations:

Standardization of K2Cr2O7 solution:

N1V1 = N2V2

N1 = Normality of ferrous ammonium sulphate solution (N/40)

V1 = Volume of ferrous ammonium sulphate solution
N2 = Normality of potassium dichromate solution
V2 = Volume of potassium dichromate solution

N2 = N1V1/V2

N2 = ------------N
Estimation of ferrous ammonium sulphate:

N3V3 = N4V4

N3 = Normality of ferrous ammonium sulphate solution

V3 = Volume of ferrous ammonium sulphate solution
N4 = N2 = Normality of potassium dichromate solution
V4 = Volume of potassium dichromate solution

N3 = N4V4/V3
N3 = -----------N

Strength = N3 × Equivalent weight of FAS

= N3 × 392

= -------------gm./L

Result: The strength of given unknown ferrous ammonium sulphate solution = ----------- g/L

Precautions:

1. Potassium dichromate acts as an oxidizing agent in acidic medium, add some dil. H2SO4.

End point should be observed carefully

EXPERIMENT: 3 Date:
Object: To determine the total, permanent and temporary hardness of given water sample by
complexometric titration using EDTA solution.

Principle: Hard water is due to metal ions (minerals) that are dissolved in the ground water.
Generally water contaminated with Ca or Mg salts is called hard water. When impurities are in
form of bicarbonate salts, they are easily removed by boiling as boiling decomposes bicarbonates
to insoluble carbonates. It is said to be temporary hardness. When they are in the form of
chlorides and nitrates etc. it is called permanent hardness.

A complex is a molecule or ion formed by the reaction of two or more ions or molecules capable
of independent existence. A metal atom can usually form a bond with one or more donor atoms
which have at least one unshared pair of electrons. The number of donor atoms which bond with
a given atom depends on the number of electron pairs that the metal ion can accept, in other
words, the coordination number of the metal ion. Complexing agents, or ligands, which can
provide more than one pair of electrons (multidentate ligands), are also called chelating agents.

Many metals forms complexes with such reagents as contain appropriate ligands. The most
important chelating agent in analytical chemistry is ethylenediaminetetraaceticacid (EDTA). The
tetra basic form of this acid forms complexes with virtually all metal ions. EDTA is a
hexadentate ligand; each of the acid oxygen and each of the amine nitrogen can donate one
electron pair. The metal ion is usually held in a one-to-one complex with EDTA. The complexes
have four or five 5-membered rings, contributing significantly to their stability. Dissociation
constant values indicate that EDTA behaves like a dicarboxylic acid. That is two of its carboxyl
groups are strongly acidic and other two hydrogen are released during formation of complex. In
forms of its disodium salt, it is used to estimate Ca+2 and Mg+2 ions.

It is important to realize that the electron pair of the carboxylic acid groups of EDTA are only
available to the metal ion when the acid is dissociated. This means that the effectiveness of the
complexing agent is strongly affected by pH. At low pH EDTA will be in the acid form and will
not be an effective complexing agent. Additionally, many metal ions form complexes with
hydroxide ions. Hydroxide ions compete with the chelating agent for coordination sites in the
metal ion. Therefore, the effectiveness of the complexing agent will also be reduced at high pH.
For a given chelating agent and metal ion, there will be an optimum pH for the titration which
will depend on the pKa values for the chelating agent and the formation constants for the metal-
hydroxide complexes. Therefore, suitable buffer solution is added to keep pH of the solution
nearly constant and pH sensitive indicators are used. In the estimation of hardness with EDTA,
an azo dye called Eriochrome Black-T is used as an indicator. This forms a metal indicator
complex, the stability of which is lower than that of the metal EDTA complex. The solution is
initially red due to metal ion indicator complex. As the titration proceeds, the metal ions forms
more stable complex with EDTA, hence the indicator anion goes in to solution. As the indicator
accumulates the color changes from wine red to blue at the end point.
EDTA is normally used as di sodium salt or tetra sodium salt because of their greater solubility.
If EDTA is assigned the formula H4Z the disodium salt will be Na2H2Z, which gives H2Z-2, a
complex forming ion. It reacts with metal ions in 1:1 ratio.

EDTA forms complexes with Ca+2 and Mg+2, as well as other metal cations in solution. Such
complexes have the general structure

The reaction with M+2 ions (Ca+2 or Mg+2) may be represented as:

M+2 + H2Z-2 MZ-2 + 2 H+

Eriochrome Black-T

When solution having pH 10 the indicator EBT react with Mg+2 and gives wine red color

Ca+2/Mg+2 + EBT [Ca+2/Mg+2 – EBT]

Blue Wine red

Reagents: EDTA solution (0.1N), buffer solution (pH=10) (NH4Cl+NH4OH), Eriochrome
black-T, unknown water sample.

Apparatus: Pipettes, burette, conical flasks, hot plate.

Procedure:

Total Hardness:

1. Clean the burette and fill with standard EDTA solution and note the initial reading.
2. Pipette out 10 ml of given hard water into a clean conical flask.
3. Add 5 ml of buffer solution (pH=10) and 2-3 drops of EBT indicator.
4. Titrate it against standard EDTA solution.
5. At the end point color changes from wine red to clear blue.
6. Note the burette reading and repeat it for two concordant readings (total hardness).

Permanent hardness:

1. Take 250 ml hard water in to 500 ml beaker and boil it gently for an hour, filter the
solution in to a 250 ml measuring flask and make the solution up to 250 ml with distilled
water and shake it thoroughly.
2. Now take 10 ml of above water sample into a conical flask, add 5 ml of buffer solution
and 2-3 drops of EBT indicator. Titrate it against standard EDTA solution value
corresponds to the permanent hardness.
3. To measure temporary hardness subtract the value of permanent hardness from total
hardness.

Observations:

Total Hardness:

Sr. Volume of Burette Readings (ml) volume of Concordant

No.
Water sample Initial Final EDTA solution Reading (ml)
taken (ml) consumed (ml)
Permanent Hardness: -

Sr. Volume of Burette Readings volume of Concordant

No.
Water sample Initial Final EDTA solution Reading(ml)
taken (ml) consumed (ml)

Calculations:

1mole EDTA ≡ 1mole of Ca+2

1 ml of 1 M EDTA ≡ 100 mg of CaCO3

Total hardness of water in 10.0 ml sample

Volume of 0.1N EDTA ≡ 100 × ( B.R. / 1) × 0.1 mg of CaCO3

≡ … X……mg of CaCO3

Hence the hardness in 1 lt. of water sample ≡ X × 1000/10

= …………. mg of CaCO3/ lt.

Total hardness = ……………mg /liter or ppm

Permanent hardness of water sample in 10.0 ml

B.R. of 0.1N of EDTA ≡ 100 × (B.R. / 1) × 0.1 mg of CaCO3

≡ ……Y……mg of CaCO3

Hence the hardness in 1 lt. of water sample = …………… mg of CaCO3 × 1000/50

So = Y × 1000/50

Permanent hardness = …………… mg / l or ppm

Temporary hardness = Total hardness – permanent hardness

= …………… mg. / l or ppm

Result: The hardness of given water sample is

Total hardness = ……….. ppm

Permanent hardness = ……….. ppm

Temporary hardness = ……….. ppm

Precautions:

1. The amount of EBT indicator should be the same in each titration.

2. pH 10 of the reaction mixture should be maintained throughout the experiment.

Experiment No. 4 Date:

Object:- To determine the strength of sodium carbonate and sodium hydroxide in given alkali
mix.(water sample) hydrochloric acid is used as an intermediate solution, methyl orange and
phenolphthalein used as indicators
Required apparatus and reagents:- burette, pipette, conical flasks, volumetric flask, funnel etc.
[Sodium hydroxide-sodium carbonates (alkali mix)] (water sample) N/10 sodium carbonate,
hydrochloric acid methyl orange phenolphthalein
Theory: - Determination of NaOH and Na2CO3 method double indicator method is generally
employed.
The principle involved in this method is that when Na2CO3 solution is titrated with HCl the
neutralization occurs in two stages. The first step is hydrogen carbonate step
CO3-2 + H+ HCO3-
The equivalence for the first step on ionization of carbonic acid is at pH 8.3 ; which may be
detected by phenolphthalein indicator.
The second step corresponds to the displacement of all carbonic acid.
CO3-2 + H+ HCO3

HCO3- + H+ H2CO3
H2CO3 H2O + CO2
The equivalence point can be detected by using methyl orange indicator. The methyl orange
indicator end point comes in the pH range 3.1 to 4.4 ; whereas the phenolphthalein end point
occurs in the pH range 8.3 to 10
NaOH + HCl NaCl + H2O
Na2CO3 + HCl NaCl + NaHCO3
If the titration is continued with methyl orange, the neutralization of the bicarbonate to the
carbonic acid takes place:
NaHCO3 +HCl NaCl + H2C
H2CO3 H2O + CO2

[P] ≡ NaOH +1/2 Na2CO3

And [M] ≡ NaOH + Na2CO3
So, [M - P] ≡ 1/2 Na2CO3
And [M] – 2 [M – P] or [2p – M] ≡ NaOH
Procedure:
i. Standardization of HCl
Pipette out 10 ml of standard sodium carbonate solution and transfer it into a conical
flask, add 2-3 drops of methyl orange indicator into the conical flask and titrate it against
HCl solution until a sharp color change from yellow to red at end point. Repeat the
procedure for concordant readings
ii. Estimation of NaOH and Na2CO3 :
Pipette out 10 ml of alkali mix and transfer it into a conical flask and add 2 – 3 drops of
phenolphthalein indicator, pink color is appear Into the conical flask
Now titrate it against HCl solution the pink color will disappear at the end point i.e.
phenolphthalein end point [P]
Now add 2-3 drops of methyl orange indicator into the same flask and continue the
titration until a sharp color change from yellow to red occurs at the end point. This titrate
value is known as methyl orange end point [P]
Observation: -

Standardization of HCl: -

Sr.No. Volume of Burette reading Volume of HCl Concordant

sodium (ml) reading (ml)
carbonate (ml) Initial (ml) Final (ml)

Calculation: -

N1 V1 =N2 V2, N2 = N1V1/V2 Where N1 = normality of Na2CO3

V1 = volume of Na2CO3
N2 = normality of HCl
V2 = volume of HCl

Analysis of given alkali mixture: -

 Sr. Volume of Volume of HCl (ml)
No. alkali mixture
Phenolphthalein end point Methyl orange end point [M] (ml)
[P] [ml]

Calculation: -
Hence [P] ≡ NaOH + ½ Na2CO3
………………….ml

[M] ≡ NaOH + Na2CO3

……………………ml

Na2CO3 ≡ 2 {[M] – [P]}

And NaOH ≡ 2[P] – [M]
Equivalent weight of NaOH = 40
Equivalent weight of Na2CO3 = 53
HCl equivalent of NaOH present in 10 ml of the given alkali mixture = …………….ml
HCl equivalent of Na2CO3 present in 10 ml of the given alkali mixture = ……………ml
Normality of the given alkali mixture with respect to NaOH = N2X B.R. /10
Strength of NaOH = eq. wt.* normality
= ……………….g /L
Similarly,
Normality of the given alkali mixture with respect to Na2CO3 = N2X B.R. /10
Strength of Na2CO3 = eq. wt.* normality
= ……………. g /L
Result: - The alkali mixture contains:
NaOH = ……….. g /L
Na2CO3 = ……….. g /L
Precautions: -
i. All readings must be repeated until concordant readings are obtained.
ii. To obtained the satisfactory results the solutions must be cold enough.
iii. Observe carefully the Decolorization of phenolphthalein end point.
iv. Loss of CO2 must be prevented by6 keeping the tip of the burette immersed in the
solution present in the conical flask.
Experiment No.5 Date:
Object: To determine the strength of ferrous Ammonium Sulphate by titrating against KMnO4
solution.

Theory: In the present experiment, potassium permanganate acts as a powerful oxidizing agent.
Although KMnO4 acts as an oxidizing agent in alkaline medium also, for quantitative analysis
mostly acidic medium is used. The oxidizing action of KMnO4 in the acidic medium can be
represented by the following
Equation:
MnO4- + 8H+ +5e– → Mn2+ + 4H2O

Chemical equations
Reduction half reaction : 2KMnO4 + 3H2SO4 → K2SO4 + 2MnSO4 + 3H2O + 5 [O]
Oxidation half reaction : H 2C 2O4 + [O] → 2CO2+ H2O] × 5 (at 600 temp.)
______________________________________________________________________________
__
2KMnO4 + 3H2SO4 + 5H2C2O4 → K2SO4 + 2MnSO4 + 8H2O + 10 CO2
______________________________________________________________________________
__

Like oxalic acid, ferrous ammonium sulphate also acts as a reducing agent in the titration against
potassium permanganate. The reaction which takes place is given below:

Chemical equation
Reduction half reaction : 2 KMnO4 + 3H2SO4 → K2SO4 + 2 MnSO4 + 3H2O + 5 [O]
Oxidation half reaction : 2 FeSO4 (NH4)2 SO4 . 6H2O + H2SO4 + [O] → Fe2 (SO4) 3 + 2
(NH4)2 SO4
+ 13 H2O] x 5
______________________________________________________________________________
__
2KMnO4 + 8H2SO4 + 10FeSO4 (NH4)2 SO4 . 6H2O → K2SO4 + 2MnSO4 + 5Fe2(SO4)3 +
10(NH4)2SO4 + 68H2O

Potassium permanganate oxidizes ferrous ion into ferric ion in acidic medium in cold and is itself
reduced to colorless manganous ions.

Reduction half reaction : MnO4– + 5e– + 8H+ ⎯Mn2+ + 4H2O

Oxidation half reaction : Fe2+ → Fe3+ + e– ] 5
______________________________________________________________________________
__
MnO4– + 5Fe2+ + 8H+ →Mn2+ + 5Fe3+ + 4H2O
______________________________________________________________________________
__

Apparatus/Reagents Required:
Burette, Pipette, conical flask, Measuring Cylinder, Dilute Sulphuric Acid, FAS Solution, Oxalic
Acid, KMnO4 solution.

Procedure:

Standardization of KMO4 solution:

Pipette out 10mL of standard N/10 oxalic acid solution into a 100mL conical flask. Add 10mL of
dil. Sulphuric acid and heat the solution to about 600C to 700C then titrate this solution slowly
against the KMnO4 solution from the burette until a faint but permanent pink color persist in the
solution. Repeat the titration until at least two concordant readings.

Estimation of FAS solution:

Pipette out 10mL FAS solution into the conical flask. To this add about 10mL of dil. Sulphuric
acid. Now titrate it against KMnO4 solution continue adding of KMnO4 solution drop by drop till
the color of the solution just changes to permanent pink. Note down the volume of KMnO4.
Repeat the titration to get at least two concordant readings.

Observation Table:

Standardization of KMO4 solution:

Sr.No. Volume of Burette reading(mL) Vol. Concordant

Oxalic Consumed of reading(mL)
acid(mL) Initial(mL) Final(mL) KMnO (mL)
4

Estimation of FAS solution:

 Sr.No. Volume of Burette reading(mL) Vol. Concordant
FAS (mL) Consumed of reading(mL)
Initial(mL) Final(mL) KMnO (mL)
4

Calculation:

Standardization of KMO4 solution:

N1V1=N2V2

N1= Normality of Oxalic acid; V1= Volume of Oxalic acid

N2= Normality of KMnO4; V2= Volume of KMnO4

Estimation of FAS solution:

N3V3=N4V4

N3= Normality of FAS; V3= Volume of FAS

N4= Normality of KMnO4 V4= Volume of KMnO

N4= N2 (Normality of KMnO4)

Strength: Normality of FAS x Equivalent of FAS (392)

……………….. g /L

Result:

The strength of given FAS solution =………….. g /L

Precautions:
1. Titration is carried out at room temp. i.e. FAS solution should not be heated.

2. All the volumetric apparatus should be washed with distilled water before used.

3. Rinse the burette with a solution of KMnO4 solution.

4. Rinse the pipette with a solution to be taken in the conical flask.

5. Wash the titration (conical flask) with distilled water after every titration.

6. KMnO4 solution should not be added fast.

EXPERIMENT: 6 Date:
Object: To prepare urea formaldehyde resin.

Principle: Amino resins are obtained by condensation reaction of urea or melamine with
formaldehyde. Such resins find uses in packaging, water tumblers, unbreakable dishes, buttons
etc. They are also used in paper industry to improve the strength of paper.

Reagents: formaldehyde (40%), urea, conc. H2SO4, distilled water.

Apparatus: Beakers, measuring cylinder, glass rod,

Procedure:

1. Take 4.5 gm of urea in a 250 ml beaker and add 10 ml of 40% formaldehyde solution in it
with constant stirring.
2. Add few drops of conc. H2SO4 to the reaction mixture with constant stirring.
3. Suddenly white voluminous mass appears in the beaker.
4. When the reaction is complete, wash the residue with distilled water and filter it.
5. Dry the product in between folds of filter paper and calculate the yield of the resin
formed.

Observations:
Weight of empty watch glass = W1; Weight of watch glass with product = W2

Weight of product (W) = W2 - W1

Result: - Weight of urea formaldehyde resin = …………….. gm.

Precautions:

Since the reaction is quite vigorous so it is better to remain quite away from the beaker while
addition of conc. H2SO4 until the reaction is complete.

First aid measures:

Conc. H2SO4:

Inhalation: Remove to fresh air. If not breathing, give artificial respiration. If breathing is
difficult, give oxygen. Call a physician immediately.

Ingestion: DO NOT INDUCE VOMITING. Give large quantities of water. Never give anything
by mouth to an unconscious person. Call a physician immediately.

Skin contact: In case of contact, immediately flush skin with plenty of water for at least 15
minutes while removing contaminated clothing and shoes. Wash clothing before reuse. Excess
acid on skin can be neutralized with a 2% solution of bicarbonate of soda. Call a physician
immediately.

Eye contact:

Immediately flush eyes with gentle but large stream of water for at least 15 min., lifting lower
and upper eyelids occasionally. Call a physician immediately.

Formaldehyde:

Eye contact: Check for and remove any contact lenses. Immediately flush eyes with running
water for at least 15 min., keeping eyelids open. Cold water may be used. Get medical attention
immediately.

Skin contact: In case of contact, immediately flush skin with plenty of water. Cover the irritated
skin with an emollient. Remove contaminated clothing and shoes. Cold water may be used.
Wash clothing before reuse. Thoroughly clean shoes before reuse. Get medical attention.

Inhalation: If inhaled, remove to fresh air. If not breathing, give artificial respiration. If
breathing is difficult, give oxygen. Get medical attention immediately.

EXPERIMENT: 7 Date:
Object: To determine the strength of given HCl solution using a standard NaOH solution by
performing a pH-metric titration.

Principle: Water can act both as an acid and as a base, aqueous solution is characterized by the
auto ionization processes in which one H2O molecule transfers a proton to another H2O molecule
and also weakly ionized in to H+ and OH- ions as:

H2O H+ + OH-

H2O + H2O H3O+ + OH-

Methamatical difinition of pH :

The negative logarithm (to the base of 10 ) of the hydrogen ion concentration of the given
solution.

pH = -log [H+]

similarly the alkalinity also be termed as;

pOH = -log [OH-]

Kw = [H+][OH-] = 1x10-14 at 25°C

For pure or neutral solution:

pH = 7.0 i.e. [H+] = [OH-] = 1 X 10-7 gm. ions per liter.

For an acidic solution:

pH < 7.0 i.e. [H+] > 1 X 10-7

For a basic solution:

pH > 7.0 i.e. [H+] < 1 X 10-7

In this experiment, the pH of a solution is utilized as an indicator for determining the end-point
of a strong acid-strong base titration. The base solution is standard while the concentration of
acid is unknown.

A fixed quantity of solution of strong acid is taken in a beaker and its initial pH is recorded. To
this, if we start adding a strong base solution, we find that the pH of the reaction mixture follows
a graph of the following type:

Strong acid and strong base curve:

When a base is added to an acid the pH rises slowly first, and then it changes rapidly at the end
point. Ionization of the base is responsible for the shape of the inflexion point and symmetry of
the curve.

Reagents: Hydrochloric acid (Strong acid), sodium-hydroxide (strong base), buffer solutions of
pH 4 & 9

Apparatus: Burette, pipette, beaker (100 ml), funnel, pH meter, pH electrode.

Procedure:

1. Calibrate the pH meter first.

2. Fill the burette with 0.2 N NaOH.
3. Take out 50 ml of given HCl solution into a 100 ml beaker.
4. Dip the pH electrode into the beaker and measure the initial pH of the acid solution.
5. From the burette, start adding the NaOH solution in 0.5 ml increments with constant
stirring. Note down the pH after each increment.
6. Continue with the previous step till 45 ml.
7. Plot a graph between the observed pH value and the volume of NaOH solution added.
Locate the end point as the point of maximum slope on the graph.
8. Calculate the strength using the data obtained.

Observation:
 Sr. Volume of NaOH added (ml) pH meter reading (pH)
No.

Calculations:

N1V1 = N2V2

N1 = Normality of acid

V1 = Volume of acid

N2 = Normality of NaOH

Strength = N2 × Equivalent weight of HCl

 = ----- × 36.5

= --------------gm./L

Result: The strength of HCl = -------- g /L

Precautions:

1. In general, be very careful when handling expensive glassware.

2. pH reading should be noted when the electrode has attained the temperature of the
solution.
3. The glass bulb should not be touched the walls and bottom of the beaker, when it is
dipped.
4. Concentrated reagents are very corrosive to human skin; exercise extreme caution while
handling them.
EXPERIMENT: 8 Date:

Object: To determine the strength of given HCl solution using a standard NaOH solution by
performing a conductometric titration.

Principle: The specific electrical conductivity and the electrical conductance are a measure of
the ability of a solution; a metal or a gas- in briefs all materials-to conduct an electrical current.
In solutions, the current is carried by cations and anions whereas in metals it is carried by
electrons. If a substance has a high electrical conductance C, the electrical or ohmic resistance R
is low.

“Conductance is the reciprocal of the resistance”

C = 1/R

Unit of R is ohm and the unit of C is ohm-1 or mhos or Siemens

Electrolytic conductors obey ohm’s law

I = E/R

Where: I = current

E = potential difference between electrode

R = resistance

In this experiment, the conductivity of a solution is utilized as an indicator for determining the
end-point of a strong acid-strong base titration. The base solution is standard while the
concentration of acid is unknown.

A fixed quantity of the solution of strong acid is taken in a beaker and its initial conductivity is
recorded. Being a strong electrolyte, the conductivity value will be large. To this, if we start
adding a strong base solution, we find that the conductivity falls slightly in the beginning. This is
because the added strong electrolyte is consumed completely in the neutralization reaction, and
hence the ionic concentration doesn’t appreciate much.

H+Cl- + Na+OH- Na+Cl- + H2O

On the other hand, dilution of the existing ions due to increase in volume causes the conductivity
to decrease. However, as soon as the equivalence point is reached, the added ions of the strong
base remain free in solution and hence beyond this point, further addition of base leads to a sharp
rise in the conductivity of the solution.
To determine the end point, the observed conductivity of the solution is plotted against the
volume added. Conductivity values follow two distinct linear trends before and after the
equivalence point, as can be seen in the following schematic diagram:

Conductometric titration of strong acid-strong base

Apparatus: Burette, pipette, beakers, measuring cylinder, conductivity meter with electrode.

Reagents: HCl solution, NaOH solution, phenolphthalein indicator.

Procedure:

1. Calibrate the conductivity meter.

2. Wash all of the glass wares with distilled water.
3. Fill the standard NaOH (0.2N) solution into the burette and note the initial volume level
in the burette.
4. Take 100 ml of given unknown HCl solution in 250 ml beaker.
5. Dip the conductivity cell into the solution of HCl acid and note the initial conductance of
HCl solution.
6. From the burette, start adding the strong base solution in 1.0 ml increments.
7. Shake the solution properly and note down the conductivity after each increment.
8. Continue with the previous step till about 45 ml and then empty the burette into a waste
container.
9. Plot a graph between volumes of NaOH added verses observed conductivity value.
Locate the end point as the intersection of the two lines.
Observation:

Sr. No. Volume of NaOH added (ml) Conductance (mhos)

Calculations:

N1V1 = N2V2

N1 = Normality of acid solution,

V1 = Volume of acid solution,

N2 = Normality of NaOH solution,

V2 = Volume of NaOH solution

N1 = N2V2/V1

Strength = N1 × equivalent weight of HCl

= -------- × 36.5

Result:

The strength of the given unknown HCl acid = --------------- g /L

Precautions:

1. In general, be very careful when handling expensive glassware.

2. Concentrated acids are very corrosive to human skin; extreme caution while handling
them.
3. NaOH should be added by accurate volume from burette.
4. Addition of acid to the base should be slow enough to keep the effervescence in control,
otherwise it could cause spillage.
5. All solutions should be prepared in conductivity water having conductivity of 0.3 to 0.5
X 10-6 mhos.
6. The conductivity solution should be dipped in a given solution.
Experiment 09: Date:

Object: - To determine the strength of given unknown acetic acid (weak) by titrating it with
sodium hydroxide (strong base) pH metrically.

Required apparatus and reagents: - Burette, pipette, beaker (100 ml), pH meter with electrode,

Standard NaOH solution, CH3COOH acid, buffer solution of the pH of 4 & 9.

Theory: - In acid base titrations, measurement of pH is done by neutralization of acid by base.

On addition of a base the concentration of H+ ions will be removed by OH+ ions and hence the
pH will increase. In the beginning the pH increases slowly but at the equivalence point, it
changes rapidly, the H+ ions removed by constant addition of alkali solution. After equivalence
point the pH changes slowly and when solution will be saturated by OH- ions then the pH value
will be constant. The plot of pH verses the volume of alkali will be “S” shaped. The point of
inflection will give the equivalence point.

Procedure: -

i. Calibrate the pH meter first.

ii. Wash the electrode by distilled water properly and wipe it with tissue paper,
iii. Fill the burette with standard NaOH solution.
iv. Take 50 ml of unknown acid solution in a beaker (100 ml) and dip the electrode in it.
v. Now insert the electrode in to the beaker and note down the reading display on pH meter.
vi. Now add standard NaOH solution from burette to the unknown solution with the
difference of .05 ml and note the pH after each addition.
vii. Plot a graph between pH value and the volume of NaOH to find out the equivalence
point.
Observation: -

Sr. Volume of (pH)

No. NaOH
Added (ml)

Weak (CH3COOH) acid strong base (NaOH) curve: -

Calculation: - N1V1 = N2V2

N1 = Normality of CH3COOH acid, V1 = Volume of CH3COOH acid,
N2 =Normality of NaOH solution, V2 = Volume of NaOH solution,
N2 = N1V1/V2
Strength = Normality X equivalent weight of CH3COOH acid
= N2 X 60.05
Result: - The strength of the given unknown CH3COOH acid = ---------- g /L
Precautions: -
i. Instrument should be warmed sufficiently.
ii. Lower end of the bulb of the electrode must be immersed properly in the solution.
Experiment No.10 Date:

Object : To determine the strength of phosphoric acid solution with 0.2N NaOH solution pH
metrically and verify that it is a tribasic acid.

Apparatus and Reagent required: pH meter with electrodes, beaker, pipette, phosphoric acid,
and 0.2N NaOH.

Theory: Neutralization of phosphoric acid takes place in following steps-

H3PO4 + NaOH NaH2PO4 + H2O

NaH2PO4 + NaOH Na2HPO4 + H2O

Na2HPO4 + NaOH Na3PO4 + H2O

In the titration curve as shown in the fig.6.01 three inflections will be observed. First and second
inflection points will be clearly seen but the third will not be observed so clearly. The solution
remains acidic after the first neutralization step but owing to the salt hydrolysis, it becomes
mildly alkaline after the second neutralization step and strongly alkaline after the third
neutralization step.
 Procedure:

1. Calibrate the pH meter first.

2. Take 50 ml of phosphoric acid (of unknown strength) in 100 ml beaker and immerse
the electrode in to the solution and note down the reading.

3. Fill the burette with 0.2N NaOH.

4. Select the switch on PH mode in PH meter and note the PH of the solution.

5. Add NaOH solution in batch of 0.5 ml into the acid solution with constant stirring and
note the PH meter reading.

6. PH will appreciably change near the neutralization point as, small amount of NaOH
added.
Observation Table:

Sr.No. Volume of alkali added pH

(mL.)

Calculation: -
N1V1 = N2V2
N1 = Normality of acid
V1 = Volume of acid
N2 = Normality of NaOH
V2 = Volume of NaOH
N2 = N1V1/V2
N2 = -----------N
Strength = N2 X Equivalent weight of phosphoric acid
 = --------------gm. /L
Result: - The strength of phosphoric acid = --------gm. /L
In the titration curve, three inflections are observed. It verifies all the three steps in the
neutralization of phosphoric acid i.e. ortho phosphoric acid is a tribasic acid.

Precautions: -
1. Instruments should be wormed sufficiently.
2. Since glass membrane is very sensitive as may break, electrode must be handled
carefully.
3. pH reading should be noted when the electrode has attained the temperatures of the
solution.
4. The glass bulb should not be touched the walls and bottom of the beaker, when it is
dipped.
Experiment No.11 Date:

Object: Titrate a mixture of strong acid HCl and weak acid CH3COOH and determine the
unknown strength of HCl and CH3COOH pH-metrically.

Apparatus and Reagent required:

PH-meter with electrodes, standard solution of alkali, unknown solution of acids, beaker, pipette,
Burette.

Theory:

When a mixture of two acids with dissociation constants well separated is titrated, the stronger
acid with larger dissociation constant will be neutralized first, and after the completion of
neutralization of stronger acid, the second one weak acid will be neutralized. That means in the
titration curve, there will be two inflection points, first corresponding to the neutralization of
stronger acid and the second of that to weaker acid. Plot a graph between pH and volume of
titrant. The titration curve will be as shown.

Strong acid = V1 ml of a alkali

Weak acid = (V2 – V1) ml of alkali

Procedure:

1. Standardize the pH-meter, clean and dry the electrode properly.

2. Take 25 ml of strong acid and 25 ml of weak acid in a beaker and dip the electrode in it.

3. Note the temperature of the solution and set apparatus accordingly.

4. Fill the burette of the standard solution of alkali (NaOH).

5. The pH value shown on the pH-meter is the pH value of unknown solution.

6. Titrate the acids solution with alkali, stir thoroughly and take the reading of pH after each
addition. Make smaller and smaller additions near the equivalence points.

7. Plot pH against volume of alkali added and find the equivalence points for HCl and
CH3COOH solutions separately.

Observations:

Temperature of the solution= ………………..0C

Sr.no. Volume of alkali pH

added(ml.)

1.

2.

3.

4.

5.

6.

7.

8.
Calculation:

Volume of alkali consumed for complete neutralization of strong acid = V1 ml of alkali (HCl)

Volume of alkali required for complete neutralization of weak acid = (V2-V1) ml

N1V1=N2V2

N1=Normality of acid

V1= Volume of acid (ml.)

N2= Normality of alkali

V2= Volume of alkali (ml.)

(It is equivalent to V1 in the case of strong acid and (V2-V1) for weak acid)

The strength of an acid = Normality X Equivalent weight

Result:

The strength of given HCl solution is ………………. g /L

and CH3COOH solution is …………. g /L

Precautions:

1. Temperature should be maintained throughout the experiment.

2. Addition of titrant should be made smaller and smaller near the equivalence points.

3. Electrodes must be dipped properly in the solution.

EXPERIMENT: 12 Date:

Object: To determine the equivalent conductance of an electrolyte.

Theory: - Equivalent conductance is the power of all the ions produced by one gm. Equivalent
conductance of an electrolyte at any particular concentration and represented by λc.

Λc = ƙ.V = 1000k /C ohm-1cm2gm equv-1

Where ƙ = specific conductivity; V = volume in which one gm. of equivalent is present.

Specific conductance ƙ = l/a X observed conductance (Where l/a = cell constant)

Cell constant = specific conductance / observed conductance

Required apparatus and reagents: - Conductivity meter with electrode, wash bottle, beakers,
electrolytes etc.

Procedure:

1. Connections are made according to the manual of the instrument.

2. Prepare 0.1N/0.01N KCl solution by dissolving an accurate amount of pure and dry KCl
in conductivity water.
3. Wash the conductivity cell with distilled water and rinse the conductivity cell with KCl
solution.
4. When equilibrium temperature has been attained, measure the conductivity. Wait for
some time and again measure the conductivity of the solution
5. Prepare the stock solution of 0.1 N of electrolyte (HCl) and determine the equivalent
conductivity by quantitative dilution of the solutions of 0.05, 0.02, 0.01, 0.001, 0.002 and
0.005N are prepared from stock solution.
6. Now wash the electrode with distilled water and rinse it with 0.1 N KCl solution, dip the
conductivity cell in to 0.1 N HCl solution and measure the conductivity of the solution.
7. Now measure the conductivity of the other solutions in similar way, care should be taken
that every time cell must be washed and rinsed properly with respective solutions.
8. The conductivity cell should be washed and kept in to the distilled water after each
reading.
Observations:

Strength of Conductivity Cell constant =

KCl solution specific Conductance /
(N) Specific conductance Observed observed conductance
of KCl conductance

0.1 0.01289

0.01 0.001412

Strength of Observed Specific conductance ƙ = Equivalent conductance

solution (N) conductance cell constant X observed = Λc = 1000 ƙ / C
conductance

0.05

0.02

0.01

0.005

0.002

Calculations:

1. λc = 1000 k/0.1
2. λc = 1000 k/0.05
3. λc = 1000 k/0.02
4. λc = 1000 k/0.01
5. λc = 1000 k/0.002
6. λc = 1000 k/0.005

Result:

1. The cell constant = -----------/ cm.

2. Equivalent conductivity for different solutions =--------mhos.
Precautions:

1. Temperature should be constant within ± 0.5 0C throughout the experiment.

2. Sufficient time should be given to the solutions to attain the equilibrium temperature.
3. Electrolyte should be of good quality.
4. Conductivity water should be free from CO2
 EXPERIMENT: 13 Date:

Object: To determine the viscosity of a given lubricating oil at various temperatures using
Redwood Viscometer No. 1 or No. 2.

Principle: Viscosity is a measure of the internal resistance to the motion of a fluid and is mainly
due to the forces of cohesion between the fluid molecules.

Absolute Viscosity may be defined as “the tangential force per unit area required to maintain
unit velocity gradient between two parallel planes in the fluid at a unit distance apart. It is
denoted by η(eta). Its Unit in CGS system is poise. Poise is equal in one dyne/second/cm2
(Dimensions of absolute viscosity are ML–1T-1).

The ratio of absolute viscosity to density for any fluid is known as its absolute kinematic
viscosity.

η Absolute viscosity
Absolute kinematic viscosity ν = =
ρ density of the fluid
Viscosity Index: Viscosity generally decreases with increase in temperature. The maintenance of
viscosity over the range of temperature is called the viscosity Index (V.I). A relatively small
change/no change in viscosity with temperature is indicated by high viscosity index whereas low
viscosity index shows relatively large change in viscosity with temperature.

The instrument used for measuring the viscosity is known as viscometers. Different types of
viscometers are: Saybolt Viscometer, Angler’s Viscometer, Ostwald Viscometer, Kinematic
Viscometer, Redwood Viscometer.

Redwood Viscometer: It is of two types

a) Redwood viscometer No.1 b) Redwood viscometer No.2

Both the above viscometers are identical in principle, shape and mode of testing. The essential
differences between the two are:

Redwood viscometer No.1 Redwood viscometer No.2

Dimensions of orifice Length-10mm, Dia-1,62mm Length-50mm, Dia-3.8mm
Kohlrausch flask Smaller mouth Wider mouth
Useful for Low viscous oil having flow Higher viscous oils having
time flow
between 30s-2000s time greater than 2000s
e.g. Kerosine oil and mustard oil e.g. Fuel oil, mobile oil
Description of the Redwood viscometer

It is divided in to three parts

1. Oil Cup: Material- Silver plated brass. It holds the test sample of lubricating oil. The bottom of
the cup is fitted with polished-agate discharge tube containing an orifice of specified dimension

2. Water Bath: Oil cup is surrounded by water bath for adjusting the temperature

3. Kohlrausch Flask: It receives the oil from polished-agate discharge tube

Reagents and apparatus: Redwood Viscometer, Thermometer 0-100°c (2 Nos), Stop watch, 50
ml standard narrow necked flask, Given Sample of oil.

Procedure:

1. Select the Redwood viscometer according to the nature of oil (RW1 for light oil and RW2
for heavy oil).

2. Level the viscometer by leveling screws.

3. Clean the cylindrical oil cup and ensure the orifice tube is free from dirt.
4. Seal the orifice by means of the brass ball and put the receiver (Kohlraush’s flask-50 ml)
below the jet.

5. Fill the bath with water or oil according to the temperature of the experiment.

6. Maintain the desired temperature and stirr the water and oil in bath and cup respectively.

7. At particular temperature lift the ball and simultaneously start the stopwatch.

8. Collect the oil in the 50 ml flask and note the time taken in seconds for the collecting 50
ml of oil.

9. Repeat the whole process at five different temperature and note respective times.

Observations:

S. No. Temperature Time t (sec) Viscosity

(mean)
(oC) Trial 1 Trial 2 Trial 3
Calculations:

The ratio of absolute viscocity to density for any fluid is known as its absolute kinematic
viscocity. Because the instruments used sre of standard dimensions, the kinematic viscocity
of the oil in centistokes can be calculated from the time taken by the oil to flow through the
standard orifice of the instrument with the help of the following equation.

The viscocity of the given oil sample with the help of the redwood viscometer at t oC =
………………Redwood seconds.

B
ν = At –
t

where ν = Kinematic viscocity (in centistokes, cst)

t = time of flow in sec.
A and B are instrument constants
A = 0.264 and B = 190 for t = 40-85 seconds
A = 0.247 and B = 65 for t = 85-2000 seconds
Note: 100 cst = 1 stoke
And 1 poise = stoke × density

Result: The kinematic viscosity of given oil at different temperatures were determined.

Precautions:

1. The cup and receiver should be properly washed with appropriate solvent.

2. The temperature of bath and oil cup should be the same.

3. The oil should be filtered thoroughly to remove solid particles that may clog the jet.

4. 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.

5. After each reading the oil should be completely drained out of receiving flask.
EXPERIMENT: 14 Date:

Object: To determine cloud and pour point of a given sample of lubricating oil using cloud and
pour point apparatus.

Principle: Cloud point and pour point are important physical properties of any liquid. Cloud
point, as the name suggests is the temperature at which a cloud of wax crystals first appear in a
liquid fuel when it is cooled under special testing conditions. The cloud point of any petroleum
product is an indicator of how well the fuel will perform under cold weather conditions. Pour
point is just the opposite of cloud point as it refers to the lowest temperature at which movement
of oil is observed and the fuel can be pumped easily.

Fig. Cloud and pour point apparatus

The cloud point and pour point apparatus consists of the following parts:

i) Test tube: it is made of glass having flat bottom and standard dimensions.
ii) Cooling bath: It consists of an insulated jacket of glass or copper containing cooling
mixture.
iii) Thermometers: In given sample and cooling mixture, there are two thermometers
fitted.

Reagents: lubricating oil, freezing mixtures

Apparatus: Cloud and pour point apparatus

Procedure:

1. Thoroughly dry and clean the flat bottomed glass tube.

2. Fill the oil sample to form a film of 5 cm thickness and fit the cork.
3. Adjust the dipped bulb of thermometer in the oil and in the cooling bath properly.
4. The tube is kept in the freezing mixture.
 5. Prepare freezing mixture as mentioned below:

Mixture Composition Temperature range

A Ice + water Upto 10 oC

B Ice + NaCl Upto -10 oC
C Ice + CaCl2 Upto -25 oC
D Solid CO2 + Acetone Upto -60 oC

6. The temperature of oil falls on cooling (when cooling bath filled with freezing mixture).
7. Take out the tube after every 1 oC fall in temperature and inspect for a moment. It may
restore if the cloudiness has not formed. This step should be completed in 3 Seconds.
8. For cloud point, note the temperature for hazy appearance.
9. And for pour point, continue the cooling process. After every 3 oC fall, the tube is
withdrawn and tilted to horizontal position for about 5-10 seconds. When oil stops
flowing out of the jar, note the temperature. It is the pour point for the given sample of
lubricating oil.

Result: The cloud point of the given sample is ………..oC and pour point is ……oC.

Precautions:

i. The observation of tube should be completed within 3 to 5 seconds.

ii. According to the pour point of oil, suitable freezing mixture should be chosen.
iii. The test oil should not be disturbed during the process which may delay the
observation.
iv. Temperature of the cooling bath and the jacket should be maintained in equilibrium.
EXPERIMENT: 15 Date:

Object: To determine the water equivalent of fuel sample by using bomb calorimeter.

Principle: Bomb calorimeter is used for determining the calorific value of solid and liquid fuels.

Fig. Bomb Calorimeter

It consists of a strong stainless steel vessel, called bomb, capable of withstanding high pressure.
The bomb is provided with a lid, which can be screwed firmly on the bomb, so as to make a
perfect air tight seal. The lid in turn is provided with two electrodes and an oxygen inlet value.
One of the electrodes is provided with a ring to accommodate the silica crucible.
The bomb is placed in a copper calorimeter having a known weight of water. The copper
calorimeter in turn, is surrounded by an air jacket and water jacket to prevent heat loss due to
radiation. The calorimeter is also equipped with an electrical stirrer and a Beckman thermometer.
Procedure:
1. Weighed amount of fuel is taken in the silica crucible and supported it over the ring.
2. A fine magnesium wire touching the fuel sample is stretched across the electrodes and oxygen
supply is forced into the bomb till a pressure reached to 25-30 atm.
3. Initial temperature of the water in the calorimeter is noted after thorough stirring.
4. The electrodes are then connected to 6 volts battery and circuits completed.
5. The current is switched on and the fuel in the crucible burns and transferred heat to water,
which is stirred throughout the experiment by the electric stirrer.
6. Maximum temperature shown by the Beckman’s thermometer is recorded and the calorific
value

Reagents: Solid or liquid fuel given

Apparatus: Bomb calorimeter

Observations:
1. Weight of the fuel taken in the crucible = x gm
2. Weight of water taken in the calorimeter = W gm
3. Water equivalent* of the calorimeter, stirrer, thermometer and bomb = w gm
4. Initial temperature of water in calorimeter = t10C
5. Final temperature of water in calorimeter = t20C
6. Higher (cross) calorific value of the fuel = L cal/gm
7. Amount of H2SO4 formed = a gm.
8. Amount of HNO3 formed = b gm.
9. Amount of fuse wire = c gm.
10. Weight of calorimeter = d gm.
11. Mass of benzoic acid a fuel of known calorific value = e g.

Calculations:
Heat gained by water = W × (t2-t1) cal.
Heat gained by water equivalent = w × (t2-t1) cal.
Total heat gained = W (t2-t1) + w (t2-t1) cal.
= (W+ w) (t2-t1) cal. …… (i)
Heat liberated by fuel = x × L cal. .….. (ii)
Since, heat liberated by the fuel = heat gain by water and water equivalent.
i.e. from eq. (i) and (ii) we get-
x × L = (W + w) (t2-t1)
Higher calorific value (HCV), L = (W + w) (t2-t1)/x cal/gm ………(1)
x
Let the percentage of hydrogen in fuel = H
Wt. of water produced from 1 gm of fuel = 9 H/100 gm
= 0.09 H gm
Heat taken by water in forming steam = 0.09 H × 587 cal.
(where 587 cal/gm is latent heat of steam)
Hence, the lower (net) calorific value = HVC – latent heat of water formed
LCV = (L – 0.094 × 587) cal/gm.
* For determining the water equivalent of the calorimeter, a fuel of known calorific value (e.g.
H.C.V. of benzoic acid = 6325 kcal. H.C.V. of naphthalene = 9688 kcal/kg.)
For benzoic acid data (same with naphthalene)
e x 6325= (W + w) (t2-t1)
Water equivalent w = [e x 6325/(t2-t1)]-W

Corrections:
(i) Sulphuric acid correction = a x 144/4 cal
(ii) Nitric acid correction = b x 14.29 cal
(iii) Fuse wire correction = 35 cal/gm (Ni-Cr wire) = 100 cal/gm (Pt wire)
(iv) Cooling correction (tc)- note the time taken to cool the water in calorimeter from maximum
temperature to room temperature

Cooling correction(tc) = dt x t
where dt = rate of cooling in 0C/minutes
Add this value to the rise in temperature.
To get more results of the calorific value the following eqn. can be used

L = (W + w) (t2-t1+ tc) –(CS+CN+CF)/x

Where CS = Sulphuric acid correction

CF = fuse wire correction
CN = Nitric acid correction

Results:
(i) Higher calorific value of the given sample = ………………….cal/gm
(ii) Lower calorific value of the given sample = ………………….cal/gm

Precautions:
1. Take only one gram of coal sample for more accurate results.
2. Fill only required necessary amount of oxygen in the bomb for complete combustion.
3. Do not fire the bomb if there is any gas bubble leaking from the bomb when it is submerged in
water.
4. Follow the procedure strictly to avoid any accident.