Applied Chemistry (Ar23) Student Manual

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Department of Chemistry

(AR-23)
APPLIED CHEMISTRY LABORATORY
STUDENT MANUAL CUM OBSERVATION BOOK
(Common to EEE,ECE,CSE,CSM,CSD,CSC &CSO)

Prepared by
Dr.G.V.Siva Prasad (HoD) Dr.Anindita Chatterjee Dr.M.Ravikumar Dr.D.Vasundhara
Professor Professor Professor Associate professor

Dr.R.S.K.Sharma Dr.M.Naresh Kumar


Dr.V.Anita Mr. K.Satyam Naidu
Associate professor Associate professor Associate professor Associate professor

Dr.D.Varaprasad Dr.G.Jaishree
Associate professor Associate professor
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CERTIFICATE

This to certify that it is a bonafied record of practical work done by


kum/sri _______________________________________________________________bearing the
Regd.No ______________________ of __________________class _____________branch/section
in the_______________________________________ laboratory during the academic year
_________________under our supervision.

No. of experiments held _______________

No. of experiments done _______________

Signature of faculty Head of the department


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EVALUATION SHEET
(Day to Day Assessment)
Name of the Student: Branch/Section:

Register No: Academic Year:

SI. Date of Max Signature


No Date of Name of the Experiment submission marks
Issue (10)
1.

2.

3.

4.

5.

6.

7.

8.

9.

10.

11.

12.

No. of Expts. Held


No. of Expts. Done
Avg. marks/grade obtained

Signature of Instructor
|3
I-I 23BS203 APPLIED CHEMISTRY LABORATORY L T P C
I-II 23BS203 LIST OF EXPERIMENTS 0 0 2 1

Ex.No Name of the experiment Page No.

0 Introduction to chemistry laboratory-molarity, normality, primary, 7-12


secondary standard solutions, volumetric titrations, qualitative analysis,
quantitative analysis etc.,
1 Determination of Hardness of a groundwater sample. 13-17

2 Determination of Strength of an acid in Pb-Acid battery 18-21

3 Estimation of Ferrous Iron by Dichrometry 22-24

4 Determination of percentage Moisture content in a coal sample 25-26

5 Preparation of nanomaterials by precipitation method. 27

6 Conductometric titration of strong acid vs. strong base 28-32

7 Conductometric titration of weak acid vs. strong base 33-36

8 Determination of cell constant and conductance of solution 37-38

9 pH metric titration- determination of strength of strong acid vs. strong 39-42


base
10 Verify Lambert –Beer’s Law 43-45

11 Preparation of a polymer (Bakelite) 46-47

12 Adsorption of acetic acid by charcoal 48-52


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General Instructions

 Be punctual.
 Bring manual, record, notebook, calculator etc.
 Maintain discipline and cleanliness in the laboratory.
 Handle the apparatus and reagent bottles with almost care.
 Report, breakage of glass wares to the laboratory Assistant immediately.
 Keep the reagent bottles in their respective places after use.
 Do not misplace the stoppers of the bottle.
 Do not throw waste paper, match - stick, broken glass wares etc., inside the sink; put them
into the dust bin.
 Do not discharge concentrated acid into the sink, dilute it before discharging.
 In case of accident, inform the faculty immediately
 Before taking any liquid in the burette or the pipette, these should be rinsed with the liquid.
 The conical flask should not be rinsed with any liquid. It should simply be washed with
distilled water.
 Read the lower meniscus in case of colorless liquids and the upper one in the case of colored
liquids.
 The solution should be filled in the burette by means of a funnel which must be removed
before titrations.
 The readings should be entered immediately in the practical note-book and not on some piece
of paper.
 When the experimental is over, wash all the glass wares and handover to the laboratory
assistant before you leave the lab.
 Playing of radios, tapes, CDs is not permitted.
 Do not eat, drink in the laboratory.
 Never attempt any unauthorized or unassigned experiments
 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.
 All lab reports are to be your own. Lab partners are to independently produce their lab
reports.
 Lab reports are due one week from the date of performance, at the beginning of the lab
period.
 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.
 Using mobiles phones are strictly prohibited in laboratory.
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COMMON LABORATORY GLASSWARES
|6
SAFETY SYMBOLS

*Not hazardous, but these compounds need to be stored in anhydrous conditions. While
preparing reagents, due to their hygroscopic nature, their weight may vary and have effect on
calculations.
|7
Expt. No Date
0
BASIC CONCEPTS OF VOLUMETRIC ANALYSIS

Chemical analysis of the compounds is carried out in two ways


1. Qualitative analysis.
2. Quantitative analysis.
Qualitative analysis shows what element a given contains.
Quantities analysis determines the quantity of a particular component present in substance.
It is carried out in two ways
1. Gravimetric analysis.
2. Volumetric analysis or Titrimetric analysis.
Gravimetric analysis involves the estimation of the amount of a given compound from the results of
weighing.
Volumetric analysis is based on the measuring the volume of the solution of a substance.

Terms involved in volumetric analysis

Titration: The process of finding out the volume of one of the solution (titrant) required to react
completely with the definite volume of other solution (analyte).
Titrant: The solution of known strength. (Usually taken in burette)
Titrate (analyte): The solution which contains a substance whose strength is to be estimated. (Taken
in conical flask)
Indicator: The substance which indicates the end point of titration by changing its color is called
indicator. Eg: Phenolphthalein, methyl orange, EBT, FSBF, Starch, potassium chromate etc.,
End point: the point where the titrant is added to slightly excess to the equivalence point and the
indicator changes its color is known as end point.
Equivalence point: the point where the titrant is added until it chemically equivalent to the analyte is
known as equivalence point. It is an exact point.
Strength: The amount of substance dissolved in one liter of a solution expressed in termed as
strength of a solution. Strength of solution can also be expressed in any of the following ways.
i. Normality: It is the number of gram equivalents of the substance dissolved per liter of the solution.
It is denoted by N.

Weight of solute per litre of the solution Weight 1000


N= (OR) N = Gm.eq.wt
×
Equivalnt weight of the solute V(ml)

ii. Molarity: It is the number of moles of solute per litre of the solution. It is denoted by M.

Weight of solute per litre of the solution Weight 1000


M= Molecular weight of the solute
(OR) M = Gm.wt
×
V(ml)

iii. Molality: It is the number of moles of the substance dissolved in 1000gm or 1kg of the solvent. It
is denoted by m.

Grams of solute per kg of the solvent


m=
Molecular weight of the solute

iv. Percentage by weight: It is the weight in grams of a solute present in 100gms of the solution.
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Weightof solute×100
Percentage weight =
Weight of solute + weight of solvent
v. Equivalent Weight: The equivalent weight of a substance is defined as the number of parts by
weight of it that combine with or displace one part by weight of hydrogen or eight parts by weight of
oxygen.

Atomic weight
Equivalent weight of a metal =
Valency

Molecular weight of an acid


Equivalent weight of an acid =
Basicity of an acid

Molecular weight of base


Equivalent weight of a base =
Acidity of base

Basicity: It is the number of replaceable hydrogen atoms in an acid.


Acidity: It is the number of replaceable OH groups in one molecule of a base.

Standard Solution: A solution of exactly known concentration is known as standard solution.


Eg: 0.05 N Na2CO3 (or) 0.05 EDTA solution etc.,

Primary Standard substance: A standard solution is one which is prepared by dissolving an exactly
weighed quantity of a (such as K2Cr2O7, Na2CO3, H2C2O4 etc.,) in a known volume of distilled
water.

A primary standard substance should confirm to the following requirements.


i) It should be stable, non-hygroscopic and must be of fixed composition.
ii) It should not gain or lose weight.
iii) It should be non-corrosive.

Solutions can also be prepared by dissolving an approximate weight of secondary standard


substances (like HCl, H2SO4, hypo, NaOH, Mohr’s salt etc.,) in a known volume of distilled water.

However, strength of these solutions should be ascertained by titrating against a standard solution
referred above, before using.

There are four types of reactions in titrimetric analysis:

1) Neutralization reactions or acidimetry and alkalimetry: These reactions involve the


combination of H+ and OH- ions to form water. That means simple acid - base reactions will
come under this class.

HCl + NaOH→NaCl + H2O

H2C2O4+ 2NaOH → (COONa)2 + 2H2O

2) Complexometric reactions: The titration involving the formation of a stable soluble complex
between the metal and the complexing agent (ligand).

2CN- + Ag+→ [Ag(CN)2]-


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EDTA + [Ca/Mg]+2→ [Ca-EDTA] or [Mg-EDTA]


3) Precipitation reactions: These depend upon the combination of ions to form a simple
precipitation. In this no change in oxidation states among reacting substances

AgNO3+ NaCl→ AgCl↓ + NaNO3

4) Oxidation – Redox reactions: These reactions involve the change in oxidation number or
transfer of electrons among the reacting substances.

2KMnO4+ 3H2SO4 + 5H2C2O4→K2SO4 + 2MnSO4 + 8H2O + 10CO2

A reaction involved in volumetric analysis must fulfill the following requirements.

i) The two solutions should react completely in stoichiometric proportions.


ii) The reaction should be simple and take place instantaneously.
iii) There must be a definite change in physical or chemical property of a solution.
iv) An indicator should be available for the reaction.

Click on:
1. https://youtu.be/IbkreR5VDmo
2. https://youtu.be/sFpFCPTDv2w

TITRATION ERRORS

Many errors occur due to analyst or method or reagent or uncalibrated glassware and
interference of the indicator. To avoid these errors statistical treatment of the titration values is
necessary. Hence, ‘Most Probable value’ is taken as the result.

MOST PROBABLE VALUE: Even when a quantity is measured with possible accuracy,
the results of a successive observation differ among themselves. The average value of these results is
taken as most probable value. Hence, it is not a true value.

ABSOLUTE ERROR: The difference between observed or measured value to a true or


most probable value is known as absolute error. It is measure of accuracy.

ACCURACY: It is the concordance between measured value and most probable value or
true value.

RELATIVE ERROR: It is the absolute error divided by true or most probable value. It is usually
expressed in terms of % ppm.

MEAN DEVIATION: It is an agreement between a series of results. It can be evaluated by


determining arithmetic means of the results, then calculating the deviation of each individual
from the mean, finally dividing the sum of the deviations by the number of measurements.
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RELATIVE MEAN DEVIATION: It is the mean deviation divided by the mean. It is expressed in
% or ppm. It is a measure of precision.

PRECISION: Precision is a measure of reproducibility of measurements.

STANDARD DEVIATION: It measures the closeness of the results with the mean. Smaller
the Standard deviation, more closely are the results to the mean value.

RELATIVE STANDARD DEVIATION (RSD): It is a measure of the quality of the sample. Large
the RSD, shows the poor the quality of the sample.

Probable viva-voce questions

1. What is meant by titration?


Ans: It is the process of determining the volumes of reagents required to bring about a definite
reaction to just completion.
2. Distinguish between titrant and titrate?
Ans: The reagent of known concentration is called the titrant and the substance being titrated is
termed as titrate.
3. What is a standard solution?
Ans: A standard solution is a solution of a definite concentration/ solution whose concentration is
known.
4. What is an indicator?
Ans: It is a substance, which produces a visible change in color at the commencement of end point.
5. What is end point?
Ans: It is that point which confirms the completion of the chemical reaction involved in titration.
6. What does an internal indicator mean?
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Ans: An indicator, which is added to the reaction mixture in the titration flask is called internal
indicator.
7. What is the relationship between normality and strength?
Ans: Strength is gm/lit = normality × grm Eq.wt
8. What are the primary and secondary standard substances?
Ans: A substance, which is having the following properties.
 It is available to a high degree of purity
 It is stable and unaffected by air
 It does not gain lose moisture in air
 It is readily soluble and its solution remains such as for a long time.
On the other hand a substance, which does not possess the above said characteristics is called
secondary standard.
9. Name some of the primary standard and secondary standard substances?
 Crystalline oxalic acid, anhydrous Na2CO3, Mohr’s salt green vitriol etc. are primary
standard substances.
 HCl,HNO3, NaOH,KMnO4 etc., are secondary standard substances.
10. What is meant by molarity and normality?
Ans: Molarity: it is the number of gram molecular weights of solute dissolved per litre of the
solution.
Normality: it is the number of gram equivalents of solute dissolved in 1 litre of a solution.
11. What are the types of titrations?
Ans: Titrations are of 4 types. Acid – Base titrations, Redox titrations, complexometric titrations and
precipitation titrations.
12. What is meant by standard solution?
Ans: Standard solution is a solution whose concentration is known.
13. What is equivalence point? Ans: The point where the titrant is added until it chemically
equivalent to the analyte is known as equivalence point. It is an exact point.
14. What is end point?
15. What is the basic formula used to calculate concentration or volume? Ans: V1N1=V2N2
16. What is a standard solution?
17. What is primary standard solution?
18. What is secondary stranded solution?
19. What is volumetric analysis?
20. What is meant by internal indicator, external indicator and self indicator? Give one
example of each.
Ans: Internal indicator: An indicator which is added to the reaction mixture to indicate the end point
of titration. Ex. Phenolphthalein in acid-base titration.
External indicator: An indicator which is not added to reaction mixture. But it is used externally to
indicate end point of titration. Ex. K2[Fe(CN6 )] is used as an external indicator in titration of Fe+2
ions with K2Cr2O7 solution.
Self indicator: When one of the reactants it acts as indicator and no external substance is required to
indicate the end point of titration. Ex. KMnO4 acts as self indicator in its titrations.
21.What is the colour change/ end point of the titration carried out with the help of
phenolphthalein indicator?
22.What is the colour change/ end point of the titration carried out with the help of methyl
orange indicator?
23.What is the colour change/ end point of the titration carried out with the help of starch
indicator?
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Exercise Problems:

1. Calculate the weight of sodium carbonate required to prepare 250 ml of 0.05N solution.

2. Calculate the normality of oxalic acid solution when 0.63 g of substance is dissolved in
100ml of the solution.

3. Calculate the amount of EDTA required preparing 1000ml of 0.01M solution.

4. What is the amount of NaOH required to prepare 1lit of 0.1N solution.

5. Calculate the volume of HCl required to prepare 1 lit of 0.1N solution.

6. 21ml of 0.05M Na2CO3 Solution is titrated with HCl solution for standardization of HCl and
11.3mLof HCl is consumed when methy orange indicator is used. Calculate the molarity of
HCl.

Marks awarded
Signature of the Instructor
| 13
Expt. No 1 Date

DETERMINATION OF HARDNESS OF A GROUNDWATER SAMPLE.


AIM:
To estimate the total hardness, permanent hardness and temporary hardness of water by using
standard solution of EDTA

APPARATUS CHEMICALS
1. 250ml conical flask, 1. Standard MgSO4
2. 50ml Burette, 2. EDTA solution
3. Burette stand, 3. Water sample
4. Wash bottle 4. Buffer solution (NH4Cl+NH4OH) (pH-10)
5. 10ml,50ml measuring cylinders, 5. Eriochrome black-T,
6. 250mlVolumetric flask
7. 250ml Beaker
8. Hot plate
9. Funnel
10. Filter paper

PRINCIPLE:

EDTA is a well known complexing agent, forms stable complex with Ca and Mg ions as well as
many other metal ions in aqueous solution. It reacts with metal ions 1:1 ratio.

Hard water which contains Ca2+ and Mg2+ ions react with EBT forms unstable wine red color
complex at pH 9-10.
Ca2+ (or) Mg2+ + EBT→ [Ca-EBT] (or) [Mg-EBT]
(Wine red color complex)
During the titration, the wine red coloured complexes [Ca-EBT] (or) [Mg-EBT] react with EDTA
and forms a stable colorless complexs [Ca-EDTA] (or) [Mg-EDTA] by releasing blue colour
indicator into the solution. Hence the color change at end point is wine red to blue.

[Ca-EBT] (or) [Mg-EBT] + EDTA→ [Ca-EDTA] (or) [Mg-EDTA] + EBT


(Wine red color complex) (Colorless stable complex) (Blue)

PROCEDURE:

Step-1: Preparation standard MgSO4:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Molarity (M) = Molecular weight of the substance ×
volume of the solution required(ml)
=
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Step-2: Preparation of 0.01M EDTA: dissolve 3.72 g of EDTA in 1000 ml of distilled water

Step-3: Standardization of EDTA:

 Rinse the burette with EDTA and fill the same solution up to the mark avoiding air gaps.
 Pipette out 10 ml of standard MgSO4 into a conical flask, add 3 ml of buffer solution, 2-3
drops of Eriochrome Black-T indicator and 20ml distilled water.
 Titrate the above wine red solution with standard EDTA solution taken in the burette, till the
wine red color changes to blue and tabulate the volume.
 Repeat the same procedure until two concurrent values are obtained.
End Point: Wine red color solution changes to pale blue

OBSERVATIONS:

Volume of Burette Reading Volume of EDTA


S. No
standard MgSO4 Initial Final consumed(V2)
in(ml) (V1)
Trail-1
Trail-2
Trail-3

Concordant volume of EDTA (V2)= ml


M1= Molarity of standard MgSO4= M
V1 = volume of standard MgSO4 = ml
M2= EDTA Molarity = ----------- ?
V2= volume of EDTA consumed = ml

M1V1 M2V2
= ;
𝑛1 n2

n1=n2=1

M2= Molarity EDTA = M

Step-4: Determination of Total Hardness:


 Take 50ml of water sample into a conical flask add 2 ml of buffer solution add 2-3drops of
EBT indicator.
 Titrate the wine red color solution with EDTA taken in burette, till a blue color end point is
obtained.
 Repeat the titration to get concurrent values.

End Point: Wine red color solution changes to pale blue


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OBSERVATIONS:

Volume of Hard Burette Reading Volume of EDTA


S. No
water in(ml) (V3) Initial Final consumed(V4)

Trail-1 50.0
Trail-2 50.0
Trail-3 50.0

Concordant volume of EDTA (V4) = ml


CALCULATIONS:

M3= Molarity of water sample = ?


V3 = volume of water sample = 50ml
M4= EDTA Molarity = M (obtained in previous step )
V4= volume of EDTA consumed = ml

M3V3 M4V4
𝑛3
= ; n3=n4=1
n4

M3= Molarity of water sample = M

Total hardness= M3×100 × 1000 = ppm

RESULT: The hardness of the given water sample has been found to be as follows:

Total hardness = ppm

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10

Application of the Experiment:


 Estimation of calcium in milk
 Estimation of calcium in calcium supplement tablets
 Estimation of calcium in eggshell
 Determine the percentage of mg in talcum powder
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 Determine Magnesium in Epsom Salt
 Estimation of calcium, magnesium in antacids
 Estimation of CaO in cement solution by rapid EDTA method
Probable viva-voce questions
1. What is hardness of water?
Ans: Hardness is defined as the characteristics which prevents the lathering of soap.
2. How hardness is expressed?
Ans: Hardness is expressed in terms of CaCO3 equivalent.
3. Why hardness is expressed in terms of CaCO3 equivalent?
Ans: It is due to two reasons: (i) Mol. wt. of CaCO3 being100 make calculation easier. (ii) It is the
most insoluble compound precipitated out in water treatment.
4. How water becomes hard?
Ans: Water becomes hard due to its action on rock and minerals. This may involve hydrolysis,
dissolution, disintegration, oxidation etc. of minerals by water.
5. What are various units of hardness?
Ans: Hardness of water can be expressed in following units:
(I) Parts per million (ppm) (II) Milligram per litre (mg/lt) (III) Degree Clarke(˚C)
(IV) Degree French(˚F)
6. Name some methods for removing permanent hardness of water.
Ans: There is (i) lime–soda (L-S) method (ii) zeolite method (iii) ion –exchange resin method
7. Which of the above methods is best for removing permament hardness?
Ans: Ion –exchange resin method is best as it gives water for almost zero hardness.
8. Give few disadvantages of using hard water.
Ans: Some of the advantages of using hard water is:
(i) It takes more time and consumes more soap for washing clothes.
(ii) Use of hard water results into scale and sludge formation inside boilers
(iii) It takes more time for cooking with hard water.
9. Why does hard water not lather with soap.
Ans: Ca+2 and mg+2ions of hard water from insoluble soaps on treating hard water with soap
2RCOONa (soap) + M+2 (from hard water)→(RCOO)2 M +2Na +(metallic soap ,white ppt or scum)
Lather is only formed when all hardness causing metal ions are removed from water. So more soap is
consumed.
10. What is a chelating agent?
Ans: It is a poly dentate ligand which coordinates with metal ions to form a stable ring complex The
complex so formed is called a chelate . eg. EDTA is a chelating hexadentate ligand.
11. What is temporary hardness? how it can be removed?
Ans: Hardness of water due to presence of carbonates and bicarbonates of Calcium and magnesium
is called temporary hardness. It can be removed by simple boiling of water.
12. What is permanent hardness?
Ans: Hardness of water due to presence of chlorides, sulphates and nitrates of calcium and
magnesium is called permanent hardness.
13. What is the other name for temporary and permanent hardness?
Carbonate and non – carbonate hardness.
14. What is the role of buffer solution? Ans: To maintain pH 9 – 10.
15. What is the name of the buffer used in EDTA titration?
Ans: Ammonium chloride - Ammonium hydroxide.
16. Why hardness is expressed in equivalents of calcium carbonate?
Ans: Calcium carbonate is most insoluble salt and its molecular weight and equivalent weights are
100 and 50 respectively.
| 17
17. What is hard water and soft water?
Ans: Water which readily forms lather with soap is called soft water and which does not produce
lather is known as hard water.
18. What are complexometric titrations?
Ans: Titrations which involves the formation of soluble, undissociated, stoichiometric complex at the
equivalence point are called complexometric titrations.
19. What is EDTA? Ans: EDTA is Ethylene Diamine Tetra Acetic Acid.
20. What is structure of EDTA?

21. What is EBT? Ans: Eriochrome Black-T


22.What is the structure of EBT? Ans: ( 1-(hydroxy 2-naphthhylazo) 6 nitro-2-napthol-4-
sulphonate)

23. What are the constituents of the ammonia buffer?


Ans: A mixture of ammonium chloride and ammonium hydroxide
24. What type of titrations are EDTA titrations? Ans: Complexometric titrations
25. What does it mean ppm? Ans: Parts per million. 1ppm = 1 mg/lit
26. What are the types of hardness?
Ans: Hardness is of two types 1. Temporary hardness - it is due to bicarbonates of Ca &Mg.
Temporary hardness can be easily removed by boiling the water sample
2. Permanent hardness-it is due to chlorides, sulphates and nitrate of Ca and Mg.
Total hardness = permanent hardness+ temporary hardness
27. Write down the chemical reaction which taking place during the titration.
28. What is carbonate hardness? Ans: temporary hardness
29. What is non carbonate hardness? Ans: permanent hardness
30. What are the major problems of hardness in water?
31. Name the methods to estimate the hardness of water. Ans: EDTA method, soap titration
method
32. What is the color of EBT indicator? Ans: Blue
33. What is the color of Ca/Mg-EDTA complex? Ans: colorless
34. What is the color change at end point?
35. Why sodium salt of EDTA (Na2-EDTA) is used but not EDTA?
Ans: EDTA is least soluble in water. Hence its disodium salt is used for preparing solution
36. Why ammonia buffer is used? Ans: The pH is to be maintained between 9 – 10.
37.Name the most widely used indicator in EDTA titrations. How does it act?
38.What is an acidic buffer? Give an example.
Ans: It is solution of a mixture of weak acid and salt of weak acid with a strong base.
(Ex. CH3COOH+CH3COONa)
39.What is a basic buffer? Give an example.
Ans: It is the solution of a mixture of a weak base and a salt of this weak base with a strong acid (Ex.
NH4OH + NH4Cl).
| 18
Expt. No 2 Date

DETERMINATION OF STRENGTH OF AN ACID IN LEAD-ACID BATTERY


AIM: To determine the strength of acid in Lead-Acid battery
APPARATUS CHEMICALS
1. 250ml conical flask, 1. H2SO4
2. 50ml Burette, 2. NaOH
3. Burette stand, 3. standard Oxalic Acid
4. 10ml Pipette, 4. Phenolphthalein indicator
5. Wash bottle

THEORY

Strength of acid in Lead-Acid battery, measure of its ability to neutralize with bases to resist change
of pH value of acid due to presence of mineral acids like H2SO4.

H2SO4 + NaOH → Na2SO4 + H2O

PROCEDURE:
Step-1: preparation of standard Oxalic acid:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Normality (N) = Equvalent weight of the substance ×
volume of the solution required(ml)

Step-2: standardization of NaOH:

 Rinse the burette with NaOH solution; take NaOH solution into the burette.
 Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
 Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
 Repeat the titration to get concurrent values.

End Point: colorless solution changes to pale pink.

OBSERVATIONS:
| 19
Volume of oxalic acid Burette readings Volume of NaOH
S.No. solution taken in ml. Initial Final Solution
(V1) consumed in ml.( V2)
Trail-1
Trail-2
Trail-3

Concordant volume of NaOH (V2) = mL

CALCULATIONS:

Volume of oxalic acid (V1) = ml


Normality of standard oxalic acid (N1 )= N
Volume of NaOH (V2) = ml (titre value)
Normality of NaOH (N2) = ?

By volumetric principle V1 N1 = V2 N2

Normality of NaOH (N2) = N

Step-3: Standardization of unknown H2SO4


 Make up the given H2SO4 solution up to the mark with distilled water and shake the flask
well for uniform concentration.
 Rinse the burette with given standard NaOH solution and fill it with same solution up to
zero mark without air bubbles then it is clamped to burette stand.
 Now pipette out 10ml of H2SO4into a clean conical flask, add 2-3drops of phenolphthalein
indicator and 20ml distilled water.
 Titrate the colorless solution with NaOH taken in burette, till pink color end point is
obtained.
 Repeat the titration to get concurrent values.

End Point: colorless solution changes to pink.

OBSERVATIONS:

Volume of H2SO4 Burette readings Volume of NaOH


Trails solution taken in ml. Initial Final Solution
(V3) consumed in ml.( V4)
Trail-1 0.0
Trail-2
Trail-3
| 20
Concordant volume of HCl (V2) = mL

CALCULATIONS:

Volume of H2SO4 (V3) = ml (titre value)


Normality of H2SO4 (N3 )= ?
Volume of NaOH (V4) = ml
Normality of standard NaOH (N4) = N

By volumetric principle V3 N3 = V4 N4

Normality of H2SO4 (N3) = N

Amount of H2SO4 present in100ml of given solution= N3× Eq.Wt H2SO4 × 100/1000

= × 49/10 gms/100cc

Amount of H2SO4 present in100mlof given solution= N3 × Eq.Wt of H2SO4 × 100/1000

= × 49 /10 gms/100cc

RESULT:

1. Normality of H2SO4 solution=


2. Amount of H2SO4 present in100ml of given solution = gms/100cc.

Amount of substance present % Error


S.No Given Reported
1.
Calculation of error percentage:
│given value−reported value│
% Error = ×100
given value

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 21

Application of the Experiment


 To measure the quantity of stomach acid that can be neutralized by a tablet of Tums.
 To estimate the percentage of acetic acid in store bought vinegar

Probable viva-voce questions


1. In which titration the pH of the end points exactly 7?
Ans: In titration of a strong acid against a strong base.
2. What is the working pH of phenolphthalein?
Ans: Phenolphthalein works in pH range of 8-10. It is pink in alkaline medium and is colorless in
acidic or neutral medium.
3.What is the working pH of methyl orange indicator? Ans: pH of 3.1 to 4.4
4.Why should you carry out the titration for 3 or 4 times? Ans: To get concordant values.
5. Which type of titration it is? Ans: Acid –base (or) neutralization titration.
6. What is an acid? Ans: It is an any substance that gives H+ ions when it is dissolved in water.
Eg: HCl, H2SO4, HNO3,H3PO4, CH3COOH, H2C2O4etc…
7. What is base? Ans: It is an any substance that gives OH- ions when it is dissolved in water.
Eg: NaOH, KOH, Ba(OH)2, Mg(OH)2, Na2CO3,Al(OH)3 etc…
8. Write down the chemical reaction which taking place during the titration.
9. What is the color of phenolphthalein in basic medium?
10. What is the color of phenolphthalein in acidic medium?
11. What is the color change at end point?
12. What is the molecular weight of sodium carbonate?
13. Does sodium carbonate is primary standard or secondary standard?
14. Sodium carbonate is acid or base?
| 22
Expt. No 3 Date

ESTIMATION OF FERROUS IRON BY DICHROMETRY


AIM: To Estimate the amount of ferrous iron in the given sample solution using standard potassium
dichromate solution
APPARATUS CHEMICALS
1. 250ml conical flask, 1. Ferrous ammonium sulphate
2. 50ml Burette, 2. Standard K2Cr2O7solution
3. 100ml volumetric flask 3. H2SO4 + H3PO4 acid mixture
4. Burette stand, 4. Diphenylamine indicator
5. 10ml Pipette,
6. Wash bottle

THEORY/ PRINCIPLE:

Ferrous iron is oxidized to ferric iron by potassium dichromate in acid solution. The completion of
the oxidation of reaction is marked by the appearance of blue violet color of the diphenylamine
which is used as an internal indicator.

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


3[2FeSO4 + H2SO4 + (O) → Fe2(SO4)3 + H2O ]
K2Cr2O7 +6 FeSO4 + 7H2SO4→ K2SO4 +3Fe2(SO4)3 +Cr2(SO4)3 + 7H2O

PROCEDURE:
Step-1: preparation of standard K2Cr2O7:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Normality (N) =
Equvalent weight of the substance
×
volume of the solution required(ml)
=
Step-2 standardization of ferrous solution:
 Rinse the burette with K2Cr2O7 solution and fill the burette with K2Cr2O7 without air
bubbles.
 Make up the given ferrous solution upto the mark of 100ml flask with distilled water.
 Pipette out 10ml of ferrous solution into a 250ml conical flask add 3ml of acid mixture and
2 drops of diphenylamine indicator. Titrate the resulting solution with potassium dichromate
solution taken in burette drop by drop till blue violet color end point is obtained. Repeat the
titration to get concurrent values.
End Point: orange-yellow color solution changes to blue violet color
| 23
OVSERVATIONS:

Volume of ferrous iron Burette readings Volume of


Sl.No. solution taken in ml. Initial Final K2Cr2O7
(V1) consumed in ml.(V2)
Trail-1
Trail-2
Trail-3

Concordant volume of K2Cr2O7 (V2) = mL

CALCULATIONS:
Volume of ferrous iron solution (V1) =10 ml
Normality of ferrous iron solution (N1) = ?
Volume of K2Cr2O7 (V2) = ml (titre value)
Normality of K2Cr2O7 (N2) =0.05N

By volumetric principle V1 N1 = V2 N2

Normality of ferrous iron (N1) = N

Amount of ferrous iron present in 100ml of the given solution = N1× Eq.wt of ferrous iron×
100/1000

= × 55.85 /10

RESULT: Amount of ferrous iron present in given solution = gms/100cc

Amount of substance present % Error


S.No Given Reported
1.

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 24
Application of the Experiment:

 To estimate the amount iron of Fe+2 in test solution by preparing a Standard FAS solution &
using K2Cr2O7.
 To Estimation of Iron in haematite ore solution using standard K2Cr2O7 solution
 To Estimation of Iron in rust solution using standard K2Cr2O7 solution

Probable viva-voce questions

1. Write the structure of potassium dichromate?

2. What is meant by oxidation?


3. What is an oxidising agent?
4. What is meant by reduction?
5. What is an reducing agent?
5. What is redox reaction?
6. What is an oxidizing agent in this experiment? Ans: K2Cr2O7
7. What is a reducing agent in this experiment? Ans: ferrous iron
8. What is the indicator used in this experiment? Ans: Diphenylamine.
9. Why acid mixture is added before the starting of titration process? Ans:
10. What is the equivalent weight of potassium dichromate? Ans:
11. What is the oxidation number of Cr in potassium dichromate? Ans: +6
12. What is the color change at end point? Ans: pale yellow to blue violet
| 25
Expt. No Date
4
DETERMINATION OF PERCENTAGE OF MOISTURE CONTENT IN A COAL SAMPLE

AIM: To Determination of percentage Moisture content in a coal sample

APPARATUS CHEMICALS
1. Crucible 1. Anhydrous Calcium chloride
2. Muffle furnace
3. Electric oven
4. Desiccator
5. Tongs

Theory:
Coal is fossil fuel which occurs in large the earth crust. It was been formed by the partial decay of
plant materials accumulated millions years and further altered by action of heat and pressure. Coal is
highly carbon matter and important fuel. The process of conversion of wood into coal be represented
as
Wood ------> Peat ------->Lignite---> Bituminous---------->Anthracite
The coal is classified according to rank which measure of change. It has underground in the
transition from wood to anthracite rank based on carbon content. The composition of coal varies
widely and hence it is necessary to analyze and interpret the result from the point of commercial
classification , the price fixation and proper industrial utilize, the following methods are analyze can
be used for moisture content in coal.
PROXIMATE ANALYSIS
This includes the determination of moisture, volatile matter, ash and fixed carbon content, which
give value information regarding the commercial classification. This is known as proximate analysis.
Procedure:
Determination of Percentage Moisture:

 Take one gram of sample in weighed crucible.


 Place the crucible with coal sample in the hot air oven.
 Maintain the oven at temperature of 105-110oC.
 Keep the crucible in oven for 1 hour.
 Remove the crucible with the help of tongs and place it in desiccators.
 Again weigh the sample.
 Loss in weight is reported as the moisture content.
 % Of Moisture = (Loss in weight/wt. of coal taken) X 100

Weight of Weight of the Weight of Crucible along with Weight of crucible along with
crucible Sample (W3) substance (Before Heating) W1 substance (After heating) W2
| 26
Calculation of moisture content:
Calculate the present of moisture in the analysis in the sample as follows
Loss in wt.of coal
% of moisture in coal = ×100
wt.of coal initially taken

W1−W2
% Moisture content = W3 ×100
Where
W1= mass of the crucible and sampler
W2=mass of crucible
W3= mass of sample in grams

Result: the percentage Moisture content in a given coal sample is =

Significance of proximate analysis:


Moisture Increase the transport cost, reduce the caloric value. Considerable amount of heat is wasted
in evaporating the moisture during the combusted of moisture. Hence, high percentage of moisture is
undesirable.

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 27
Expt. No 5 Date

PREPARATION OF NANOMATERIALS BY PRECIPITATION METHOD


AIM: To prepare nano particles by precipitation method
APPARATUS CHEMICALS
1. Magnetic stirrer 1. zinc nitrate
2. Graduated pipette 2. KOH
3. Centrifuge 3. Alcohol
4. Furnace 4. AgNO3
5. Beakers 5. Na2CO3
6. Starch

Procedure:
1. ZnO nano particles:
The aqueous solution (0.2M) of zinc nitrate (Zn (NO3)2.6H2O) and the solution (0.4 M) of KOH were
prepared with deionized water, respectively. The KOH solution was slowly added into zinc nitrate
solution at room temperature under vigorous stirring, which resulted in the formation of a white
suspension. The white product was centrifuged at 5000 rpm for 20 min and washed three times with
distilled water, and washed with absolute alcohol at last. The obtained product was calcined at 500
°C in air atmosphere for 3 hr.

2. Silver nano particles:


AgNO3 and Na2CO3 were used as a precursor and the starch acting as a reducing agent. Silver Nitrate
0.05 M and 50 mg of starch were dissolved in aqueous medium, the obtained solution was stirred for
one hour at room temperature. 0.025 M of sodium carbonate in aqueous solution is used as basic
medium, and is added drop wise to the above solution. Thus, the AgNO3 splits into positive silver
ions (Ag+) and negative oxide ion (NO3-). Due to the splitting of ions the color of the solution
changes to yellow which is unstable. This solution was stirred for 5 hours at room temperature and
there is a complete transformation of Ag+ ions with the indication of dark gray precipitates. The
precipitate is separated by centrifugation process and other impurities are washed out by ethanol and
the residues are dried at room temperature.
Result:
In this experiment, ZnO nano particles were successfully synthesized by direct precipitation method
using Zinc nitrate as Zinc source and KOH as precipitating agent in aqueous solution. The size range
of the generated ZnO powder was approximately ________nm.

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 28
Expt. No Date
6
CONDUCTOMETRIC TITRATION OF STRONG ACID VS. STRONG BASE

AIM: To determine the amount of strong acid (HCl) present in the given sample by conductometric
titration with NaOH solution of strength 0.1N.

APPARATUS CHEMICALS
1. Conductivity meter 1. 0.1N standard oxalic acid
2. Conductivity cell 2. 0.1N NaOH solution
3. 50ml Burette, 3. HCl solution,
4. 100ml Beaker, 4. Distilled water
5. Glass rod,
6. 20ml Pipette

PRINCIPLE

The conductmetric titration is a volumetric analysis based upon the measurement of conductance
during the course of titration. Conductance of the solution (electrolyte) depends on the number of
ions and their mobility. When one electrolyte is added to another electrolyte, the change in number of
free ions causes a change in the conductance.
For example when a strong acid (HCl) is titrated against a strong base (NaOH), before NaOH added
from the burette, the acid solution has high conductivity due to the highly mobile H+ ions. When
NaOH added is added to the acid, the conductivity of the acid solution decreases due to the
neutralization of highly mobile H+ ions of the acid with OH- ions of base.

HCl + NaOH→NaCl + H2O + NaOH (excess)

Thus the conductance of the solution continues to decrease until the equivalence point reached.
Further addition of NaOH will increase the conductance by highly mobile OH- ions.
The point of intersection of the graph plotted by conductance of the solution against volume of base
added corresponds to the end point of the titration.

PROCEDURE
Step-1: preparation of standard Oxalic acid:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Normality (N) = Equvalent weight of the substance ×
volume of the solution required(ml)
| 29
Step-2: standardization of NaOH:

 Rinse the burette with NaOH solution; take NaOH solution into the burette.
 Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
 Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
 Repeat the titration to get concurrent values.

End Point: colorless solution changes to pale pink.

OBSERVATIONS:

Volume of oxalic acid Burette readings Volume of NaOH


S.No. solution taken in ml. Initial Final Solution
(V1) consumed in ml.( V2)
Trail-1 0.0
Trail-2
Trail-3

Concordant volume of NaOH (V2) = mL

CALCULATIONS:

Volume of oxalic acid (V1) = ml


Normality of standard oxalic acid (N1 )= N
Volume of NaOH (V2) = ml (titre value)
Normality of NaOH (N2) = ?

By volumetric principle V1 N1 = V2 N2

Normality of NaOH (N2) = N

Step-3: standardization of unknown HCl:

 Fill the burette with standard NaOH solution and clamp it to burette stand.
 20 ml of the given HCl is pipetted out in to a clean 100 ml beaker and then diluted to 50 ml
by adding distilled water.
 The conductivity cell is washed with water and then immersed in the solution.
 Initial conductance is read in the instrument for the acid alone without the addition of NaOH.
 Now 0.5 ml of NaOH solution from the burette is added to the solution taken in the beaker,
stirred and then conductivity is measured.
 The process is continued up to the end point i.e at least five points beyond the equivalence
point.
 After the end point, further NaOH is gradually added and few more readings are noted.
| 30
S.No Vol.of Measured Corrected S.No Vol.of Measured Corrected
NaOH Conductance conductance NaOH Conductance conductance
(V1) (C) C1 = (C) C1 =
C(V+V1/V) C(V+V1/V)
1 16
2 17
3 18
4 19
5 20
6 21
7 22
8 23
9 24
10 25
11 26
12 27
13 28
14 29
15 30

GRAPH:

A plot is made between volume of NaOH added along X-axis and the conductance of solution along
Y- axis. The end point is intersection of the two lines.
| 31
CALCULATION:

Step - 1: Calculation of normality of HCl:

Volume of NaOH (V1) = ml (titer value from graph)

Normality of NaOH (N1) = N (given)

Volume of HCl (V2) = ml (taken in beaker)

Normality of HCl (N2=----------------? (to be find)

By volumetric principle V1 N1= V2 N2

= N

Concentration of HCl(N2) = N

Step - 2: Calculation of amount of HCl

The amount of HCl present in the whole of the given solution =N2 × Eq.wt. of HCl

= ×36.45

= g/lit

RESULT:The amount of HCl present in the whole of the given solution (or)

Strength of given unknown HCl solution = g/L

Amount of substance present % Error


S.No Given Reported
1.

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 32
Probable viva-voce questions
1. What are conductometeric titrations?
Ans: The volumetric titration which involves the determination of strength of given solution by
measuring conductance of the solution is called conductometric titration
2. Give the factors on which conductance of a given solution depends ?
Ans: Conductance depends on two factors:-
1. No’s of ions
2. Mobility of ions
3. In the experiment you have done, what is the pH of the solution before & after the titration?
Ans: In metal the conductance is due to movement of free ions. Before titration solution contains
HCl therefore pH is acidic, after titration solution contains NaOH therefore pH is basic.
4. What is specific conductivity ? Give its units
Ans: Specific conductivity is defined as the conductance of ions per centimeter cube of solution.
 It is denoted by k { kappa }.
 Specific conductance = cell constant / absorbed resistance
 Its units are ohm-1cm-1 or mhocm-1 or scm-1
5. What is the difference between conductance of metal and electrolytic solutions?
Ans: In metals the conductance is due to movements of free electrons. In electrolytic solution, the
conductance is due to moving ions.
6.What are the advantages of conductometric titrations over volumetric titrations?
 More accurate results are obtained because the end point is determined graphically
 Titration can be carried out along with coloured solution
 These are successful even in weak acids and strong base
 This method gives more accurate results even with weak acids against weak bases.
7. What could be the shape of graph of strong acid vs strong base? Ans: V-shape
8. What is the equivalent weight of HCl? Ans: 36.5
9. What is a conductivity cell? Ans: The vessel in which the measurement of conductivity of the
solution is to be made is known as conductivity cell. They are of various shapes and sizes depending
upon the nature of the solution taken.
10. What is cell constant? Ans: It is the ratio between the distance of two parallel plates of the cell
and the area of the electrode. Its unit is cm-1.
11. What is the relationship between conductance and concentration of electrolyte?
12. What is an electrolyte?
13. What are the factors affecting conductance of an electrolyte?
14. What are the units of conductance?
15. What is the cell constant of a conductivity cell you used in this experiment?
16. What are the units of cell constant?
17. What is corrected conductance?
18. Discuss the pattern of graph obtained during this titration.
19. How the end point for a particular reaction is calculated using this, titration method?
Ans: Plotting a graph between conductance and volume of the base, the point of Intersection of the
straight lines gives the end point.
20.Why conductance decreases on addition of NaOH to HCI ?
Ans: During the titration the fast moving hydrogen ions are replaced by the slow moving Sodium
ions, as a result the conductance of the solution decreases.
21.What is the unit for conductance? Ans: The unit for conductance is mho.
| 33
Expt. No 7 Date

CONDUCTOMETRIC TITRATION OF WEAK ACID VS. STRONG BASE

AIM: To determine the amount of Weak acid (CH3COOH) present in the given sample by
conductometric titration.

APPARATUS CHEMICALS
1. Conductivity meter 1. 0.1N standard oxalic acid
2. Conductivity cell 2. 0.1N NaOH solution
3. 50ml Burette, 3. CH3COOH solution,
4. 100ml Beaker, 4. Distilled water
5. Glass rod,
6. 20ml Pipette

PRINCIPLE

The conductmetric titration is a volumetric analysis based upon the measurement of conductance
during the course of titration. Conductance of the solution (electrolyte) depends on the number of
ions and their mobility. When one electrolyte is added to another electrolyte, the change in number of
free ions causes a change in the conductance.

When weak acid is titrated with strong base, the conductance of the solution is low in the beginning,
since the dissociation of weak acid is very low. On addition of base, highly dissociated sodium
acetate is formed. Due to the common ion effect, the acetate ion tends to suppress the ionization of
acetic acid. Later the conductivity begins to increase due to the conductivity power of the highly
ionized salt exceeds that of weak acid. After end point, the addition of NaOH contributes sharp
increase in the conductivity of the solution. The point of intersection of the two cures gives the end
point of the titration.

CH3COOH + NaOH → CH3COONa + H2O

PROCEDURE
Step-1: preparation of standard Oxalic acid:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Normality (N) = Equvalent weight of the substance ×
volume of the solution required(ml)
| 34
Step-2: standardization of NaOH:

 Rinse the burette with NaOH solution; take NaOH solution into the burette.
 Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
 Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
 Repeat the titration to get concurrent values.

End Point: colorless solution changes to pale pink.

OBSERVATIONS:

Volume of oxalic acid Burette readings Volume of NaOH


S.No. solution taken in ml. Initial Final Solution
(V1) consumed in ml.( V2)
Trail-1 0.0
Trail-2
Trail-3

Concordant volume of NaOH (V2) = mL

CALCULATIONS:

Volume of oxalic acid (V1) = ml


Normality of standard oxalic acid (N1 )= N
Volume of NaOH (V2) = ml (titre value)
Normality of NaOH (N2) = ?

By volumetric principle V1 N1 = V2 N2

Normality of NaOH (N2) = N

Step-3: standardization of unknown CH3COOH:

 Fill the burette with standard NaOH solution and clamp it to burette stand.
 20 ml of the given CH3COOH is pipetted out in to a clean 100 ml beaker and then diluted to
50 ml by adding distilled water.
 The conductivity cell is washed with water and then immersed in the solution.
 Initial conductance is read in the instrument for the acid alone without the addition of NaOH.
 Now 0.5 ml of NaOH solution from the burette is added to the solution taken in the beaker,
stirred and then conductivity is measured.
 The process is continued up to the end point i.e at least five points beyond the equivalence
point.
 After the end point, further NaOH is gradually added and few more readings are noted.
| 35
S.No Vol.of Measured Corrected S.No Vol.of Measured Corrected
NaOH Conductance conductance NaOH Conductance conductance
(V1) (C) C1 = (C) C1 =
C(V+V1/V) C(V+V1/V)
1 16
2 17
3 18
4 19
5 20
6 21
7 22
8 23
9 24
10 25
11 26
12 27
13 28
14 29
15 30

GRAPH:

A plot is made between volume of NaOH added along X-axis and the conductance of solution along
Y- axis. The end point is intersection of the two lines.

CALCULATION:

Step - 1: Calculation of normality of CH3COOH:

Volume of NaOH (V1) = ml (titer value from graph)

Normality of NaOH (N1) = N (given)


| 36

Volume of CH3COOH (V2) = ml (taken in beaker)

Normality of CH3COOH (N2=----------------? (to be find)

By volumetric principle V1 N1= V2 N2

= N

Concentration of CH3COOH (N2) = N

Step - 2: Calculation of amount of CH3COOH

The amount of CH3COOH present in the whole of the given solution =N2 × Eq.wt. of CH3COOH

= × 60

= g/lit

RESULT:The amount of CH3COOH present in the whole of the given solution (or)

Strength of given unknown CH3COOH solution = g/L

Amount of substance present % Error


S.No Given Reported
1.

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 37
Expt. No 8 Date

DETERMINATION OF CELL CONSTANT AND CONDUCTANCE OF SOLUTIONS

AIM: To Determination of cell constant and conductance of solutions

APPARATUS CHEMICALS
1. Conductivity meter 1. Potassium chloride
2. Conductivity cell 2. Distilled water
3. Beaker
4. Standard flask
5. Glass rod

Theory: -
Conductance is the reciprocal of resistance. It is depend upon three factors, number of ions, and
nature of ions and mobility of ions towards their respective electrodes. The specific conductance of
electrolyte is decreased by increasing its dilution and equivalent conductance is increased by
increasing its dilution. The observed conductivity of an electrolyte will be equal to its specific
conductivity if cell constant is one.
Procedure: -
 Prepare 0.1M KCl solution by weighing accurately 0.7455gm of KCl into a clean 100ml
standard flask.
 From this 0.1M KCl solution prepare 100ml each of 0.05M, 0.02M, 0.01M, 0.005 and
0.001M KCl solutions.
 Take about 40ml of each solution in to a clean and dry 100ml beaker and dip the conductivity
cell and make necessary connections. Measure the conductance of each solution and note
down.

Observations: Room temperature =____ ◦C.

Part-A: Determination of cell constant:


Record the conductance of 0.1N, 0.01 N KCl by using conductometer and determine the cell
constant.
S.No Concentration Observed Specific Cell constant Mean of
-1
conductance conductance (k) (cm ) cell
(ohm -1) -1
(ohm cm ) -1 constant
1 0.1 N 1.288
2 0.01 N 1.413

Specific conductance
Cell constant =
observed conductance
| 38
Part-B: determine the conductance of all the prepared solutions of KCl and calculate the their
specific and equivalent conductance.

S.No Concentration Observed Specific Equivalent √𝑐


(c) conductance (ohm-1) conductance (k) conductance(ᴧ)
(ohm-1 cm-1) (ohm-1 cm2 gr.eq-1)
1 0.02 N
2 0.01 N
3 0.005 N
4 0.001 N
5 0.1 N

 Specific conductance (k) = Cell constant × Observed conductance


𝑘 ×1000
 Equivalent conductance (ᴧ)= 𝑁
Plot a graph of equivalent conductance against the concentration of solution

Result:
 Cell constant =_______________ cm-1
 Equivalent conductance of KCl at infinite dilution ( Λ0 ) =………………. ohm-1 cm2 gr.eq-1

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10

Probable Viva Voce questions

1. Define cell constant


2. State the factors that determine the conductance of electrolytic solution
3. What is the effect of dilution on specific conductance?
| 39
Expt. No Date
9
DETERMINATION OF THE CONCENTRATION OF ACETIC ACID USING SODIUM
HYDROXIDE (PH-METRY METHOD).
AIM: To determination of the concentration of acetic acid using sodium hydroxide

APPARATUS CHEMICALS
1. pH meter 1. 0.1N Oxalic acid
2. Glass electrode 2. 0.1N NaOH
3. Buffer solutions (pH-4.0, 9.0) 3. 0.1N Acetic acid
4. 100cc Beaker 4. Distilled water
5. 50cc Burette 5. Phenolphthalein indicator
6. 100cc Volumetric flasks(3)
7. 250cc Conical flask
8. 10cc Pipette
9. 50cc Measuring cylinder
PRINCIPLE

The titration of a weak acid with a strong base involves the direct transfer of protons from the weak
acid to the hydoxide ion. The reaction of the weak acid, acetic acid, with a strong base, NaOH, can
be seen below. In the reaction the acid and base react in a one to one ratio.

NaOH + CH3COOH → CH3COONa + H2O


PROCEDURE
Step-1: preparation of standard Oxalic acid:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Normality (N) = Equvalent weight of the substance ×
volume of the solution required(ml)
=
Step-2: preparation of NaOH solution:

Step-3: standardization of NaOH:

 Rinse the burette with NaOH solution; take NaOH solution into the burette.
 Pipette out 10ml of standard oxalic acid into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
 Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
 Repeat the titration to get concurrent values.

End Point: colorless solution changes to pale pink.


| 40
OBSERVATIONS:
Volume of oxalic acid Burette readings Volume of NaOH
S.No. solution taken in ml. Initial Final Solution
(V1) consumed in ml.( V2)
Trail-1 0.0
Trail-2
Trail-3

Concordant volume of NaOH (V2) = mL

CALCULATIONS:

Volume of oxalic acid (V1) = ml


Normality of standard oxalic acid (N1 )= N
Volume of NaOH (V2) = ml (titre value)
Normality of NaOH (N2) = ?

By volumetric principle V1 N1 = V2 N2

Normality of NaOH (N2) = N

Step-4: Calibration of a pH meter:


 Calibrate the pH meter by dipping the electrode into the buffer solution of known pH.
 Use basic and acidic buffers respectively to determine pH of solution.
 Take out the electrode wash with distilled water, dry and dip in test solution.
 Switch on the pH meter and note down the pH of solution directly.
Step-5: standardization of CH3COOH:

 Fill the burette with standard NaOH solution and clamp it to burette stand.
 Make up the given CH3COOH solution up to the mark with distilled water and shake the
flask well for uniform concentration.
 Pipette out 25.0 ml of the given CH3COOH in to a clean beaker and add 3-4 drops of
phenolphthalein indicator.
 Put the rinsed pH probe into the beaker of CH3COOH, swirl and record the initial pH.
 Add small quantity of NaOH from the burette using following scheme
| 41
S.No Volume pH ∆pH S.No Volume pH ∆pH S.No Volume pH ∆pH
of NaOH ∆V of NaOH ∆V of NaOH ∆V
added added added
1 0.0 16 31
2 17 32
3 18 33
4 19 34
5 20 35
6 21 36
7 22 37
8 23 38
9 24 39
10 25 40
11 26 41
12 27 42
13 28 43
14 29 44
15 30 45

Plotting graph: Plot a graph taking pH on ordinate and Volume of NaOH added on abscissa

CALCULATION:
Volume of NaOH (V3) = ml (titer value from graph)
Normality of NaOH (N3) = M (given)
Volume of CH3COOH(V4) = ml (taken in beaker)
Normality of CH3COOH (N4) =----------------? (to be find)

By volumetric principle V3 N3= V4 N4


= N
Concentration of CH3COOH (N4) = N
RESULT: Concentration of CH3COOH (N4) = N

Concentration of CH3COOH % Error


S.No Given Reported
| 42
SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 43
Expt. No 10 Date

VERIFICATION OF BEER’S LAW


AIM: To determine the concentration of given CuSO4 solution by verifying the Beer’s law using
colorimeter
APPARATUS CHEMICALS
1. Colorimeter 1. 0.2M CuSO4
2. Graduated pipette 2. Distilled water
3. Cuvettes
4. Standard flask
5. Glass rod
6. Filter paper

Principle: Beer’s law is applicable to only to dilute solutions. It states that when a monochromatic
light is passed through a solution intensity of light decreases with thickness and this decrease in
intensity is directly proportional to the intensity of incident light and the concentration of the
solution.
I = I0 e-ε c l
Where I = Intensity of the transmitted light;
I0 = Intensity of the incident light
C = Concentration of the solution;
l = Path length of the cuvette
ε = Molar extinction coefficient
ln (I/ I0)= -εcl
The value of ε (epsilon) depends on the nature of the absorbing solute but independent of the
concentration of the solution. Decrease in the intensity of the transmitted light is due to the
absorption of light, which may lead to photochemical reactivity.
In colorimetric studies transmittance is defined as the fraction of light passes through the sample.
% Transmittance (T) = (I /I0) x 100
A more useful and convenient quantity in performing analysis is the absorbance or negative log of
transmittance.
Absorbance or Optical density= A= log (1/T) = - log (T)
A linear relation exists between absorbance (O. D) and concentration of the sample is known as
Beer’s law.
Absorbance or Optical density= A= log (I0/I) = εcl
| 44
Before verification of Beer’s law, it is necessary to a select a suitable wave length and determines
whether Beer’s law is valid at the wavelength selected. The most suitable wavelength is that at which
maximum absorbance is observed, called λmax. The λmax will always be at the same wavelength for
a given solution under any condition.
Filter Selection: (Calculation of λmax)
 Prepare 100 ml, 0.2M CuSO4 solution (stock solution), fill it in a burette
 Switch on the instrument; wait for 10 minutes for ‘warmup’ of the instrument.
 Take one clean and dry glass (only for visible range scan) or quartz cuvette with a given
path length (say, 1 cm).
 Prepare a blank by filling a cuvette 3/4 full with distilled water
 By using blank cuvette (with distilled water) calibrate the colorimeter (absorbance = 0,
transmittance =100 %) at filter 1 and putout the blank cuvette.
 Then fill cuvette with the stock solution and measure absorbance, note the reading in table.
 Repeat the above step for all the filters (wave length range)
 From table we can see the λmax i.e. wave length at which solution show maximum
absorbance/ O.D.

S.No Wavelength(nm) Optical density


1 420
2 440
3 490
4 520
5 540
6 570
7 600
8 650
9 700

Beer’s law verification


Procedure:
 Colorimeter is switched on, wait for 10-15min so that the instrument acquires temperature
stability. The intensity of the light from the lamp depends on the environmental temperature.
 Now transmittance is adjusted to 100% or O.D is adjusted to zero with distilled water (Since
water is the solvent used in the preparation of CuSO4 solution), which is taken in a cuvette.
 By using various filters the λmax value of the CuSO4 solution (Bluish green colour solution)
can be determined.
 Different concentrations of CuSO4 solutions are prepared by mixing 10,9,8,7,6,5,4,3,2,1 ml
CuSO4 solutions from the stock with 0,1,2,3,4,5,6,7,8,9 ml of distilled water respectively.
 The O.D value is measured for each set at the λmax which is in the range of 650-700nm (Red
colour filter).
| 45
S. No of Volume of Volume of Concentration(mol/lit) Optical density
CuSO4 (ml) water(ml)
1 9 1 0.18
2 8 2 0.16
3 7 3 0.14
4 6 4 0.12
5 5 5 0.10
6 4 6 0.08
7 3 7 0.06
8 2 8 0.04
9 1 9 0.02
Unknown sample

Model graph: A graph is plotted between optical density and concentration of CuSO4 .A straight
line passing through the origin is obtained. Slope of the line is equal to Molar extinction co-efficient

Result: A straight line passing through origin is obtained in the graph. Hence, Beer’s law is verified.

 Concentration of Unknown sample=……………………..Mol/Lit


 The molar extinction co-efficient = ……….. Lit mol-1 cm-1

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 46

Expt. No 11 Date

PREPARATION OF BAKELITE
(DEMONSTRATION ONLY)

AIM: To prepare bakelite in laboratory

APPARATUS CHEMICALS
1. Beaker 1. 36-45% formaldehyde
2. Measuring cylinder 2. Phenol
3. Fume hood 3. Glacial acetic acid
4. Glass rod 4. Conc. HCl
5. Copper bath

Theory: Phenol formaldehyde resin or P-F resin or phenolic resins (also called phenoplasts) are
important class of polymers which are formed by condensation polymerization of phenol and
formaldehyde in acidic or alkaline medium. Following steps are involved
| 47
Procedure:
1. Place 5 mL of glacial acetic acid and 2.5 mL of 40 % aq formaldehyde solution in a 100 mL
beaker. Add 2 g phenol safely.
2. Wrap the beaker with a wet cloth or place it in a 250 mL beaker having small amount of
water in it.
3. Add conc. HCl drop wise with vigorous stirring by a glass rod till a pink coloured gummy
mass appears.
4. Wash the pink residue several times with to make it free from acid.
5. Filter the product and weigh it after drying in folds of a filter or in an oven. Report the yield
of polymer formed.

Precautions:-

1. While adding conc. HCl, it is better to stay little away from the beaker since the reaction
sometimes becomes vigorous.
2. The reaction mixture should be stirred continuously.

Observation:
Weight of empty watch glass = W1 g

Weight of watch glass + polymer formed = W2 g

Weight of polymer formed = W2 – W1 g

Result:

Weight of phenol formaldehyde resin = ________________g

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 48
Expt. No 12 Date

ADSORPTION OF ACETIC ACID BY CHARCOAL.


AIM: To study the adsorption of acitic acid from solution on active charcoal and to examine the
validity of freundlich & Langmuir adsorption isotherm.

APPARATUS CHEMICALS
1. Volumetric flask
2. Stoppered bottles 1. 0.25M Acetic acid
3. 50ml Burette, 2. 0.1M NaOH solution
4. 100ml Beaker, 3. Phenolphthalein indicator
5. Water bath 4. Distilled water
6. 20ml Pipette 5. Activated charcoal
7. Conical flask

PROCEDURE
Step-1: preparation of standard NaOH:

Weight of the empty bottle W1=


Weight of the bottle and substance W2 =
Weight of the substance transferred into flask W=(W2-W1)
Equivalent weight of the substance Eq.Wt=
Volume of the solution required V=

Weight of substance transferred 1000


Molarity (M) = Molecular weight of the substance ×
volume of the solution required(ml)

Step-2: standardization of CH3COOH:

 Rinse the burette with NaOH solution; take NaOH solution into the burette.
 Pipette out 10ml of CH3COOH into a conical flask, add 2-3 drops of phenolphthalein
indicator and 20ml distilled water.
 Titrate the colorless solution with NaOH till pale pink color is obtained as end point.
 Repeat the titration to get concurrent values.

End Point: colorless solution changes to pale pink.

OBSERVATIONS:

Volume of Acetic acid Burette readings Volume of NaOH


S.No. solution taken in ml. (V1) Initial Final Solution consumed in ml.( V2)
Trail-1 0.0
Trail-2
Trail-3
| 49
Concordant volume of NaOH (V2) = mL

CALCULATIONS:

Volume of NaOH (V1) = ml (titre value)


Molarity of NaOH (M1) = M
Volume of Acetic acid (V2) = ml
Molarity of Acetic Acid (M2 )= ?

M1V1 M2V2
By volumetric principle = ; n1=1; n2=1
𝑛1 n2

Molarity of Acetic Acid (M2 )= M

Step-3:
 Take well cleaned and dried 6 stoppered reagent bottles and label them
 With help of two burettes transfer the acetic acid and distilled water into these bottles as
shown below.
Bottle No 1 2 3 4 5 6
Acetic acid 50 40 30 20 10 0
Distilled water 50 60 70 80 90 100
Initial 50 40 30 20 10
concentration × 𝑀2 × 𝑀2 × 𝑀2 × 𝑀2 × 𝑀2
100 100 100 100 100
of acetic acid zero
(C1) a= b= c= d= e=

 Mix the solution well and keep all the six bottles in a water bath for some time to aquire the
temperature of the water bath.
 Weigh exactly 2 gms of activated charcoal and add the same to each bottle.
 Shake the bottle well and keep in the water bath for 1 hour while shaking the bottles from
time to time.
 Filter contents of all the six bottles into six different labelled, dried conical flasks.
 Titrate the six samples with 0.1M NaOH taken in the burette using phenolphthalein indicator
till pale pink coloured end point is obtained.
 Let the titre values be V3,V4,V5,V6,V7,V8 respectively for bottle numbers 1,2,3,4,5,6.
 Take 20ml of the stock solution into a clean 250ml conical flask add 2drops of
phenolphthalein indicator and titrate against 0.1M NaOH till pale pink coloured end point is
obtained.
 Repeat the titration to get concurrent values.
 Let the titre value be x ml.
| 50

Calculations:
M1V1 M2V2
= n2 ;
𝑛1

M1= Molarity of Acetic acid= M


V1 = volume of Acetic acid = ml
n1 = no.of moles of acetic acid reacted= 1
M2= Molarity of NaOH = ----------- ?
V2= volume of NaOH consumed = ml
n1 = no.of moles of NaOH reacted= 1

V1×M1×n2
M2 = =
n1×V2

Concentration of the acetic acid solutions after adsorption (C2):

Bottle No-1 Bottle No-2 Bottle No-3 Bottle No-4 Bottle No-5 Bottle No-6
M Acetic acid M Acetic acid M Acetic acid M Acetic acid M Acetic acid Zero
𝑀(𝑁𝑎𝑂𝐻)×𝑉3 𝑀(𝑁𝑎𝑂𝐻)×𝑉4 𝑀(𝑁𝑎𝑂𝐻)×𝑉5 𝑀(𝑁𝑎𝑂𝐻)×𝑉6 𝑀(𝑁𝑎𝑂𝐻)×𝑉7
= = = = =
50 50 50 50 50
=p =q =r =s =t

(𝐶1−𝐶2)×60×100 (𝐶1−𝐶2)×60
Amount of Acetic acid absorbed (X) = =
1000 10
Where C1=Initial concentration
C2= concentration after adsorption
Amount of the adsorbent (acetic acid) m = 2 gms
Initial concentration of six bottles (c) = a,b,c,d,e,f respectively

Bottle Initial concentration Amount of acetic acid X/m Log (X/m) Log c
No conc. C1 after absorbed
(𝐶1−𝐶2)×60
=X
adsorption C2 10

1 a= p= (𝑎 − 𝑝) × 60
=
10
2 b= q= (𝑏 − 𝑞) × 60
=
10
3 c= r= (𝑐 − 𝑟) × 60
=
10
4 d= s= (𝑑 − 𝑠) × 60
=
10
5 e= t= (𝑒 − 𝑡) × 60
=
10

Plotting graphs:

Freundlich adsorption isotherm:


| 51
 The Freundlich adsorption isotherm is, ln(X/m) = lnk + alnc.
 A graph may be plotted against lnX/m and lnc to test the Freundlich adsorption isotherm and
k values are calculated from the straight-line plot as slope = a, and intercept = lnk.

Log x/m log K

Log C
Langmuir adsorption isotherm:
 The Langmuir adsorption isotherm is, c/(X/m) = 1/(k1k2) + c/k2
 A graph may be plotted between c/(X/m) and c. A straight line indicates the validity of
Langmuir adsorption isotherm. k1 and k2 are obtained from the graphs as; Slope = 1/k1 and
intercept = 1/(k1k2).

RESULT:
The adsorption of acetic acid on activated charcoal is studied and the constants of the equations of
Langmuir and Freundlich isotherms are estimated and are:

Freundlich isotherm: slope (a) = -------


K = -------
Langmuir isotherm: k = -------
k2 = -------

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10

Application of the Experiment:


 To Study the Adsorption of oxalic acid on activated charcoal
| 52
Probable viva voce questions

1. Define Adsorption Isotherm?


2. Define Adsorption?
3. What is the pH range of Phenolphthalein indicator?
4. What is the indicator used in this experiment?
5. What is the color change of indicator used in this experiment?
6. Why did you use charcoal as an adsorbent?
7. Which isotherm is more suitable? Why?

SCHEME OF EVALUATION
S.No Skill tested Max Marks Awarded marks Signature
1 Skills in handling apparatus 2
2 Correctness of data/information 3
3 Analysis and calculations 2
4 Viva voce 3
Total Marks 10
| 53

Annexure-1

I. Equivalent weights of substances used in volumetric Analysis


Titration and Substances used Formula Eq. wights
ACID – ALKALI TITRATIONS:
1. Sodium carbonate Na2CO3 M.W./2 = 53.06
2. Sodium bicarbonate NaHCO3 M.W./1 = 84.00
3. Potassium carbonate K2CO3 M.W./2 = 69.00
4. Potassium bicarbonate KHCO3 M.W./1 = 100.00
5. Sodium hydroxide NaOH M.W./1 = 40.00
6. Barium hydroxide Ba(OH)2.8H2O M.W./1 = 157.75
7. Oxalic acid (hydrated) H2C2O4.2H2O M.W./2 = 63.03
8. Hydrochloric acid HCl M.W./1 = 36.46
9. Sulphuric acid H2SO4 M.W./2 = 49.04
REDOX TITRATIONS:
1. Potassium permanganate KMnO4 M.W./5 = 31.606
2. Potassium dichromate K2Cr2O7 M.W./6 = 49.03
3. Ferrous sulphate (hydrated) FeSO4.7H2O M.W./1 = 278.00
4. Ferrous sulphate (anhydrous) FeSO4 M.W./1 = 152.00
5. Ferrous ammonium sulphate FeSO4.(NH4)2SO4.6H2O M.W./1 = 392.12
6. Oxalic acid (hydrated) H2C2O4.2H2O M.W./2 = 63.04
7. Iron (ferrous) Fe At.W./1 = 55.84
8. Copper Cu Eq.Wt = 63.5
IODINE TITRATIONS:
1. Iodine I2 M.W./2 = 126.92
2. Hypo (sodium thiosulphate) (hydrated) Na2S2O3.5H2O M.W./2 = 124.09
3. Anhydrous sodium thiosulphate Na2S2O3 M.W./1 = 158.09
4. Arsenious oxide As2O3 M.W./1 = 49.45
5. Copper sulphate (hydrated) CuSO4.5H2O M.W./1 = 249.68
ARGENTOMETRIC TITRATIONS:
1. Silver nitrate AgNO3 M.W./1 = 169.89
2. Silver Ag At.W./1 = 107.88
3. Sodium chloride NaCl M.W./1 = 58.45
4. Chloride ion Cl- At.W./1 = 35.46
5. Potassium sulphocyanide KCNS M.W./1 = 97.17
| 54

II. Strength of Aqueous solutions of Concentrated Acids and Bases.

Approximate Volume for


Compound Molecular Molecular making1litre
formula weight % of Specific ofapprox1M
solute by gravity Molarity solution(ml)
weight
Hydrochloric acid HCl 36.5 35 1.18 12 84
Nitric acid HNO3 63.0 70 1.42 16 63
Sulphuric acid H2SO4 98.0 96 1.84 18 56
Acetic acid CH3COOH 60.0 100 1.05 17.5 58
Phosphoric acid H3PO4 98.0 >85 1.70 14.7 68
Sodium hydroxide NaOH 40.0 50 1.48 19 53
Ammonia NH3 17.0 28 0.90 15 67

III. Indicators used

Sl. Titration Approximate pH range Suitable pH at color


change of
No. at indicators indicator
1 Strong acid against 4 to 10 Methyl orange Litmus 3.1 – 4.4
strong base Phenolphthalein 4.5 – 8.3
8.0 – 9.6
2 Strong acid against 3.5 to 7 Methyl orange 3.4 – 4.4
weak base Methyl red 4.2 – 6.3
3 Weak acid against 6.5 to 10 Phenolphthalein 8.0 – 9.6
strong base
4 Weak acid against No sharp None
weak base inflection at
equivalence point
IV. PREPARATION OF STANDARD SOLUTIONS AND REAGENTS

1. 0.1N standard sodium carbonate: Dissolve exactly 5.3 grams of sodium carbonate in 1000
ml of distilled water in a standard volumetric flask (Eq.wt 53)
2. 0.1N standard potassium permanganate: Dissolve exactly 1.6 grams of potassium
permanganate 500 ml of distilled water in a standard volumetric flask (Eq.wt 158 )
3. 0.1N standard oxalic acid: Dissolve exactly 0.63 grams of oxalic acid in 100 ml of distilled
water in a standard volumetric flask. (Eq.wt 63)
4. 0.1 N standard potassium dichromate: Dissolve 0.49 grams of potassium dichromate in
100 ml of distilled water in a standard volumetric flask. (Mol.wt 294.18)
5. 0.1 N Hypo solution: Dissolve 12.4 gms of hypo into 1000ml of distilled water.
| 55
6. Preparation of KI: Dissolve 20 gms of KI in 100ml of water and stir well.
7. Preparation of dil.CH3COOH (2N): Dissolve 11.6 ml of glacial acetic acid in 100ml of
distilled water.
8. 0.01M EDTA: Dissolve 3.72 grams of EDTA in 1000 ml of distilled water in a standard
volumetric flask. (Mol.wt 372.24)
9. 0.01M Magnesium sulphateheptahydrate:Dissolve exactly 0.246 grams of magnesium
sulphatehepta hydrate in 100 ml of distilled water in a standard volumetric flask (Mol.wt 246)
10. 0.1M standard zinc sulphate solution: Dissolve exactly 2.87 grams of zinc sulphate in 100
ml of distilled water in a standard volumetric flask (Mol.wt 287)
11. 0.1 N sodium hydroxide:Dissolve approximately 0.4 grams of sodium hydroxide 100 ml of
distilled water in a standard volumetric flask (Mol.wt 40)
12. 0.1 N HCl : Use 8.6 ml of 11.6 M/N acid (36% HCI) in 1000ml (9.9 mL of acid in 1000mL
if 37% HCl)
13. Ammonium hydroxide (0.1 M, 0.1 N): Dilute 6.75 ml of concentrated solution (14.8 M,
28% NH3) to 1 liter.
14. Ammonium buffer of PH-10: dissolve 67.5 grams of ammonium chloride in 570ml of
ammonia solution and then make upto 1000ml
15. Methyl orange indicator. Dissolve 1 g of methyl orange in 1 liter of water. Filter, if
necessary.
16. Methyl red indicator. Dissolve 1 g of methyl red in 600 ml of alcohol and dilute with 400
ml of water.
17. Phenolphthalein. Dissolve 1 g of phenolphthalein in 50 ml of alcohol and add 50 ml of
water.
18. Diphenylamine: Dissolve 1 g in 100 ml of concentrated sulfuric acid.
19. EBT indicator: dissolve 0.5 grams of EBT in 100ml of alcohol
20. Fast Sulphone Black F: The indicator solution is 0.5% solution in water (or) dissolve 1 gm
of fast sulphone black-F indicator in 100ml of alcohol
21. 1% starch solution: In a 250ml beaker, place 100ml of distilled water and then add 1 grams
of starch. Heat the contents for about 10-15 min.
22. Murexide: This is the Ammonium salt of purpuric acid. Suspend 0.5g of the powdered
dyestuff in water, shake thoroughly and allow to settle. The saturated supernatant is used as
the indicator.
23. Preparation of acid mixture: Mix up 100 ml of phosphoric with 300ml of concentrated
H2SO4 in a reagent bottle and stopper it.
24. Conductivity standard (0.01N): dissolve 0.7459 g KCl in 1000ml. its conductivity at 25 OC
is 1413 microsemen/cm.
25. pH standard: 1. dissolve 10.12 g potassium hydrogrnphthalate in 1000ml distilled and its pH
is 4.004.
2. Dissolve 2.0992 g sodium bicarbonate in 1000ml distilled water (or) Dissolve 2.64 g
sodium carbonate in 1000ml distilled water (pH =10.014)
𝒘×𝒅×𝟏𝟎
26. Molarity =
𝒈𝒎𝒘
27. Molarity of Concentrated Acids & Bases
| 56

Dilutions to Make a 1 Molar Solution


Volume (mL)
required to
Molarity Normality make 1000 mL
Concentrated Reagents Density
(M) (N) solution:
1M 1N
Acetic acid 99.5% 1.05 17.4 17.4 57.5 57.5
Ammonia 35% 0.880 18.1 18.1 55.3 55.3
Ammonia 25% 0.910 13.4 13.4 74.6 74.6
Hydrochloric acid 36% 1.18 11.65 11.65 85.8 85.8
Hydrochloric acid 32% 1.16 10.2 10.2 98.0 98.0
Hydrofluoric acid 40% 1.13 22.6 22.6 44.2 44.2
Nitric acid 70% 1.42 15.8 15.8 63.3 63.3
Perchloric acid 60% 1.54 9.2 9.2 108.7 108.7
Perchloric acid 70% 1.67 11.6 11.6 86.2 86.2
Orthophosphoric acid 85% 1.7 15.2 45.6 65.8 21.9
Sodium hydroxide 47% 1.5 17.6 17.6 56.7 56.7
Sulfuric acid 98% 1.84 18.4 36.8 54.3 27.2
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