Chemistry Lab Manual

Prof. Mostafa Radwan

Chemist: Sameh Haridi
Chemist. Mohamed Hammam
Eng. Rana Adel
Chemist: Ibrahim Hamad
Chemist:2022
Ibrahim Hamad
 Chemistry Lab Manual 2022/2023

Table of Contents
Introduction ............................................................................................................................ 5

Safety Practices in the Laboratory ......................................................................................... 6

1.1 General safety precautions in the laboratory ............................................................. 6

1.2 Contents of first aid kit .............................................................................................. 9

Chemical Analysis ................................................................................................................ 10

Quantitative analysis ............................................................................................................ 10

1.3 Volumetric methods of analysis .............................................................................. 10

1.3.1 Fundamentals requirements and main types of Volumetric Analysis ............... 10

1.3.2 The basic requirements of a volumetric method: .............................................. 11

1.3.3 Standard solutions ............................................................................................. 12

1.4 Main Concentration Expressions............................................................................. 13

1.4.1 Weight /volume:-............................................................................................... 13

1.4.2 Weight / Weight:- .............................................................................................. 13

1.5 Calculation of the Equivalent point of a titration .................................................... 16

1.6 Dilution calculations ................................................................................................ 16

EXPERIMENT (1): Acid-Base Neutralization Titration, Determination of the concentration

of HCl solution ......................................................................................................................... 20

1.1 Introduction: ............................................................................................................ 20

1.2 Acid-base indicators:- .............................................................................................. 20

1.2.1 Indicator for strong acid Vs strong base titration:............................................. 21

1.2.2 Indicator for strong acid Vs weak base titration ............................................... 21

1.2.3 Indicator for weak acid Vs Strong base titration............................................... 22

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1.3 Reagents and materials ............................................................................................ 23

1.4 Glassware................................................................................................................. 23

1.5 Procedure ................................................................................................................. 24

Lab Report 1 ......................................................................................................................... 25

Experiment (2): Oxidation-Reduction Titration (Redox Reaction), Standardization of

KMnO4 solution by using standard oxalic acid solution ......................................................... 28

1.1 Basic principles to a redox equation........................................................................ 28

1.2 Reagents and material.............................................................................................. 29

1.3 Glass ware & apparatus ........................................................................................... 29

1.4 Procedure ................................................................................................................. 29

Lab Report 2 ........................................................................................................................ 31

Experiment (3): Complexometric Titration (Complex formation), Determination of the total

hardness of water using EBT indicator .................................................................................... 35

1.1 Introduction: ............................................................................................................ 35

1.2 Principle ................................................................................................................... 36

1.3 Reagents and material.............................................................................................. 36

1.4 Glass ware................................................................................................................ 36

1.5 Procedure ................................................................................................................. 37

1.6 Calculation ............................................................................................................... 37

Lab Report 3 ........................................................................................................................ 39

Qualitative Analysis ............................................................................................................. 42

1.7 Detection of a simple salt ........................................................................................ 43

1.8 Physical properties................................................................................................... 43

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1.9 Identification of the acidic and basic radicals of the salt ........................................ 43

Experiment 4: Qualitative Analysis ..................................................................................... 44

I- Detection of the acidic radical (Anion) ....................................................................... 44

II- Detection of the basic radicals (Cations) ..................................................................... 46

Lab Report 4 ......................................................................................................................... 47

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Introduction
Chemical analysis is the most important method for investigation and is widely used in all
branches of science which are related to chemistry.
At present on large scale, no material is taken into production or released without analytical
data, which characterize its quality and suitability for various purposes.

Course objectives
After completing this course, the student will be able to:
1. Understand volumetric analysis.
2. Master neutralization and oxidation-reduction titrations.
3. Understand different concentration expressions.
4. Identify acid and base radicals.
5. Identify simple salts.

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Safety Practices in the Laboratory

1.1 General safety precautions in the laboratory

1. Wear safety glasses and white protective coats.
2. Drinking, eating or smoking in the laboratory is strictly forbidden.
3. Do not use mouth suction to fill pipettes.
4. Do not perform unauthorized experiments.
5. Never work in the laboratory alone.
6. Handle every chemical with care.
7. Do not taste chemicals.
8. Use care in smelling chemicals.
9. Avoid the inhalation of organic vapors.
[Link] contact of chemicals with skin and clothes.
[Link] spills immediately on the bench, near the balance and everywhere
[Link] caps on bottles as soon as possible.
[Link] away the opening of your test tube from your colleague’s face
[Link] the use of loose clothes while working.
[Link] the location of safety shower.
[Link] the location and contents of first aid kit.
[Link] lenses should never be worn in the laboratory.
[Link] the area near you for flames if you are about to use organic solvents.
[Link] over your equipment joined together before work.
[Link] not leave the equipment joined together for long period of time.
[Link] that glassware and the laboratory equipment are expensive.
[Link] not heat organic solvents on the open flame.
[Link] not hesitate to ask your instructor when you feel doubtful.
[Link] case of accident or if you feel unwell, seek medical advice immediately.

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In case of accident, you must notify the laboratory instructor immediately.

A) Handling chemicals after contact with the skin:
 In case of acids, wash the skin with plenty of water, then apply saturated sodium
bicarbonate solution and then again with plenty of water and finally get prompt medical
attention.
 In case of bases such as hydroxides, wash the skin with plenty of water, then apply 1%
acetic acid solution and then again wash using plenty of water and finally get prompt
medical attention.
 In case of organic material, wash with ethyl alcohol then with soap followed with hot
water and seek medical advice.
B) Chemicals in contact with the eye:
 Flush with large amounts of water for 15 min. using a special bottle and placing the
person face up on the floor.
 Hold the eye open to wash behind the eyelids.
 Prompt medical attention must be taken whatever the severity of the injury is.
C) Cuts:
 Wash the cut.
 Remove any pieces of glass.
 Apply pressure to stop bleeding.
 Get immediate medical attention.
D) Burns:
 Flush the burned area with cold water for at least 15 min.
 Wash of chemicals with 1% sodium bicarbonate solution then mild detergent and water.
 Remove contaminated clothes.
 Get prompt medical attention.

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E) Burning clothes:
 Prevent the person from running and fanning the flames.
 Roll the person on the floor to help extinguishing the flame.
 Hold the person under the shower until flames are extinguished and chemicals washed
away.
 Remove contaminated clothes.
 Wrap the person in a blanket to avoid shock.
 Get quick medical attention.
 Do not use toxic fire extinguisher.
F) Burning reagent:
 Extinguish all nearby burners.
 Remove combustible materials and solvents.
 Cover the fires in beakers with asbestos-wire gauze square or a watch glass.
 Use dry chemical fire extinguisher directed at the base of the flame.
 Do not use water.

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1.2 Contents of first aid kit

1. 1% aqueous solution of acetic acid.
2. 1% aqueous solution of boric acid.
3. Saturated solution of sodium bicarbonate.
4. 1% aqueous solution of sodium bicarbonate.
5. Glycerin.
6. Pure ethyl alcohol.
7. Cotton.
8. Disinfectant (dettol).
9. Mercurochrome.
[Link] for burns.
[Link].
[Link] plaster.
[Link] ointment.
[Link] dropper.

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Chemical Analysis
Chemical analysis is divided into: Quantitative analysis and Qualitative analysis

Quantitative analysis
Quantitative analysis is used to determine the concentration of element or compound in
solution or mixture. There are several techniques which may be used, such as (Volumetric
analysis, Gravimetric analysis, Spectrophotometeric analysis, Chromatography... etc)

1.3 Volumetric methods of analysis

1.3.1 Fundamentals requirements and main types of Volumetric Analysis
Volumetric analyses are quantitative analytical techniques which employ a titration, in
comparing an unknown solution sample with a standard.
A Solution: is a mixture of two or more components, one of them usually has the greatest
amount called solvent and the other is called solute. The solvent is usually a liquid and the
solute is a solid.
In a titration, a volume of a standard solution containing a known concentration of
reactant "A" is added incrementally to a sample containing an unknown concentration of
reactant "B" or vice versa.
The titration proceeds until reactant "B" is just consumed (stoichiometric completion),
which is known as the “Equivalence Point”. At this point the number of equivalents of "A"
added to the unknown equals the number of equivalents of "B" originally present in the
unknown.
Typically a burette is used to measure the volume of the titrant required to reach the
Equivalence point. Regardless of the type of titration, an indicator is always used to detect the
equivalence point.

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Most common are the internal indicators, compounds added to the reacting solutions that
undergo an abrupt change in a physical property (usually absorbance or color) at or near the
equivalence point.

Figure 1: the apparatus used for carrying out titration

Sometimes the analyte or titrant will serve this function (auto indicating). External
indicators, electrochemical devices such as pH meters, may also be used.
1.3.2 The basic requirements of a volumetric method:
1. A standard solution (i.e., titrant) of known concentration, which can react with the
analyte with a known and repeatable stoichiometry
2. An apparatus to measure the mass or volume of sample (e.g., pipette, graduated
cylinder, volumetric flask and analytical balance)
3. An apparatus to measure the volume of the titrant added (i.e., burette)
4. A suitable indicator by which the endpoint can be determined. This may be an internal
indicator (e.g., phenolphthalein) or an external indicator (e.g., pH meter).

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1.3.3 Standard solutions

There are two types of standard solutions,
Primary standard solution
It is a solution prepared by dissolving a primary standard substance in a solvent. A primary
standard substance should satisfy the following requirements:
1. The substance must be chemically pure.
2. The composition of the substance must correspond exactly to its formula.
3. The substance must be stable on keeping and its mass is unaltered in air. (not
hygroscopic)
4. The equivalent weight of the substance should be as large as possible.
5. The substance should be readily soluble in water.
The substances commonly employed as primary standards are:

 Oxalic acid (H2C2O4.2H2O)

 Potassium chromate (K2CrO4)
 Sodium borate (Na2B4O7.10H2O)
 Magnesium sulphate (MgSO4.7H2O)
Secondary standard solution
It is a solution that cannot be prepared in exact concentration such as HCl, NaOH, H2SO4,
CH3COOH, NH4OH, etc. A secondary standard solution should be standardized by a primary
standard solution prior using it to determine the concentration of unknown solutions

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1.4 Main Concentration Expressions

1.4.1 Weight /volume:-
1- Titer of a solution: is the mass in grams of solute per milliliter of solution

[Link]-1

2- Weight/volume percent: It is the mass in grams of solute dissolved per100 milliliter (dl)
of solution

Weight/volume percent = Titer × 100 (%)

3- Strength: the Strength of a solution is the mass of solute in grams dissolved per liter of
solution

Also, strength = Titer × 1000 (g/L)

1.4.2 Weight / Weight:-

1- Weight / Weight (percent): is the mass in grams of solute dissolved per100 g of solution

2- Parts per thousand: is the mass in grams of solute dissolved per kg of solution

For aqueous solutions mass of solution in kg is very close to volume of solution in liters
and hence

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3- Parts per million: is the mass in milligrams (mg) of the solute present in one kg of
solution. Or is the mass in milligrams (mg) of the solute present in one liter of aqueous
solution (mg/L)

For aqueous solutions

4- Molality (m): is the number of moles of a solute dissolved per one kilogram (1000g) of
solvent.

5- Molarity (M): is the number of moles of a solute per one liter of solution.

6- Normality: is the number of gram-equivalents of a solute per one liter of solution.

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Equivalent weight: is the number of grams of substance which react or replace one gram of
hydrogen, 8 grams of oxygen, 35.5 grams of chlorine, or the equivalent weight of any other
material.
Calculation of equivalent weight:-

For an Acid

For a Base

For a Salt

For an Oxidant/Reductant

It must be kept in mind that a reagent may have different equivalent weights for different
reactions. Thus, a balanced reaction equation must be applied to calculate the correct
equivalent weight. The following reactions illustrate this concept:

MnO 4
-
+ 4H
+ 3 e- MnO 2 + 2H 2O

+7 +4
Mn 3 e- Mn

Equivalent weight of KMnO4 = Molar mass/3

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- +
5 e- +2
MnO 4 + 8H Mn + 4H 2O

+7 5 e- +2
Mn Mn

Equivalent weight of KMnO4 = Molar mass/5

1.5 Calculation of the Equivalent point of a titration

In an experiment, 4 mL of H2SO4 of unknown concentration, were added to 10ml of NaOH of
a concentration of 0.1 mol.L-1 to reach the end point, find out the molar concentration of
Sulphuric acid.

1.6 Dilution calculations

One of the dilution problems is to dilute a solution like acid of high concentration to a
solution of lower concentration. Taking into account that the number of mole of the solute has
not changed by dilution, accordingly for the solute it is safe to assume that,
Number of moles before dilution = number of moles after dilution

Or
M.V initial = M.V final

Or

[V(ml) × [Link]. × concentration(%)] beforedilution

= [V(ml) × [Link]. × concentration(%)] after dilution

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Practice Problems
1- Calculate the number of moles, and number of gram-equivalents in:-
 80 g NaOH
 49 g H2SO4
 212g Na2CO3
 73 g HCl
(Na = 23, C = 12, O = 16, H = 1, S = 32, & Cl = 35.5)

2- Calculate the following for produced solution when dissolving 10g of NaOH in water
and complete the solution up to 500 ml:-
 Molarity
 Normality
 Molality
 Titer
 Strength
3- The concentrated sulphuric acid used in laboratory is 98% H2SO4 by mass. Calculate the
molality, molarity, & normality of the solution if [[Link]. = 1.83]
(Note [Link]. = density ρ in g/ml)
4- Calculate the titer of 2.9 ml H2SO4 of concentration 96% & [Link]. 1.84 when diluted with
water to one liter .
5- Calculate the molarity (M) of produced solution when:
 424 g Na2CO3 dissolved in water and the volume was completed to 200.
 49 g H2SO4 dissolved in water and the volume was completed to 100 ml.
 234 g Al(OH)3 dissolved in water and the volume was completed to 250 ml
6- Select suitable indicator for the next acid base titration and explain your reasons
 HCl versus NaOH

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 HCl versus NH4OH

 CH3COOH versus NaOH

7- Calculate the strength of KMnO4 when it was standardized by using 0.1 mol.L-1 Oxalic
acid and the volume of oxalic acid in the flask was 10 ml and that of KMnO4 at the end
point was 23 ml if the reaction was:
MnO4 + 8 H+ MnO
KMnO4 + 4 H+ MnO2

8- It is required to prepare 6 liters of 30% conc. HNO3 (of sp. Gr. 1.0) by using a bottle of
HNO3 of conc. 95% (sp. Gr. 1.4). Calculate the N, M, m of HNO3 before and after
dilution and calculate the amount of 95% conc. acid needed and the amount of water
should be added.
9- Explain briefly how you can determine the concentration of unknown NaOH solution
using internal and external indicator.
10- Give example for an oxidation-reduction titration.
11- Define and mention the differences between primary standard and secondary standard
solutions giving examples for both.
12- Calculate the amount of water in grams that must be added to 5 g Oxalic acid to prepare
17% weight /weight solution.
13- A 5 ml sample of Vinegar was diluted and titrated with 0.1104 M NaOH requiring 32.88
ml to reach the end point. If the Vinegar has density of 1.055 g/ml calculate the acidity of
Vinegar as acetic acid concentration%.
14- Show how you can differentiate between:
 Chloride and Sulphate anions and mention confirmatory tests.
 Carbonate and Phosphate anions and mention confirmatory tests.
 Lead, Aluminum and Ferric cations and mention confirmatory tests.

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 Copper and Lead cations and mention confirmatory tests.

 Aluminum chloride and Ferrous sulphate salts.

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EXPERIMENT (1): Acid-Base Neutralization Titration,

Determination of the concentration of HCl solution

1.1 Introduction:
Neutralization – in any reactions between acid and bases, is typically defined as when one
mole of the hydrogen ion of the acid (H+) combines with one mole of the hydroxide ion of the
base (OH-) to form one mole of neutral water
Generally, ACID + BASE = SALT + WATER
Complete formula equation of neutralization
NaOH(aq) + HCl(aq) NaCl (aq) + H2O(l)
Net ionic equation (after eliminating spectator ions):
OH-(aq) + H+(aq) H2O(l)

1.2 Acid-base indicators:-

The color change of an indicator can be used to follow the course of titration. However,
indicators do not all change color at the same pH, so the choice of indicators for particular
titration depends on the PH at which the equivalence point is expected to occur.
Table 1: various acid-base indicators and their typical pH ranges

Indicator Acid form Base form PH range

Thymol blue Red Yellow 1.2 – 2.8
Methyl orange Orange Yellow 3.0 – 4.6
Methyl red Red Yellow 4.2 – 6.3
Litmus Red Blue 5.0 – 8.0
Phenol phthalein Colorless Reddish pink 8.3 – 10.0

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1.2.1 Indicator for strong acid Vs strong base titration:

A strong acid/base, is simply a compound that shows a complete irreversible dissociation,
which can be shown by the most infamous example
NaOH(aq) + HCl(aq) NaCl (aq) + H2O(l)
The product NaCl does not hydrolyze, and a neutral species is obtained at end or
equivalence point at a pH value of about 7, in this case methyl orange, methyl red, litmus or
phenol phthaleine can be used.

Figure 2: Titraion of a strongbase with a strong acid

1.2.2 Indicator for strong acid Vs weak base titration

Consider the neutralization reaction between HCl and ammonium hydroxide:
HCl(aq)+ NH4OH(aq) NH4Cl(aq) + H2O(l)
The salt produced contains ammonium ion, which is capable of hydrolysis as follows
NH4+ + H2O NH4OH + H+
Therefore, at the equivalent point of the titration, the corresponding pH will be below 7,
which is attributed to the presence of excess H+ and hence, the suitable indicators for this
titration are methyl orange and thymol blue (check table 1).

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Figure 3: Titration of a weak base with a strong acid

1.2.3 Indicator for weak acid Vs Strong base titration

Consider the neutralization reaction between acetic acid and sodium hydroxide.
CH3COOH (aq) + NaOH (aq) CH3COONa (aq) + H2O(l)
The acetate undergoes hydrolysis as follows:

CH3COO- + H2O CH3COOH + OH-

Accordingly, and due to the abundance of excess hydroxide ions (OH-) at the equivalence
point, the pH is expected to be above 7, and consequently phenol phthaleine is the ideal
indicator to be employed in this case

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Figure 4: the titration of weak acid Vs Strong base

1.3 Reagents and materials

1- 0.1mol.L-1 standardized NaOH solution
2- Phenol phthaleine indicator

1.4 Glassware
1- 25 ml burette
2- 10ml pipette
3- 250 ml conical flask
4- 250 ml beaker
5- 100 ml beaker
6- Funnel
7- Washing bottle

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1.5 Procedure
 Transfer 10 ml of 0.1 mol.L-1 NaOH solution into conical flask, and 2-3 drops of
[Link] indicator. The solution turns to pink color.

 Fill the burette with the provided unknown HCl solution, start the titration by adding
HCl to the conical flask dropwise till the pink color is discharged (pink → colorless),
and record the volume of acid added.

 Carry out a rough titration, followed by at least three accurate titrations and compute
the average volume of the acid. Account the concordant readings only.
 Calculate the actual molar concentration as well as the strength of the unknown HCl
solution.
Some hints
 Rinse the burette with distilled water followed by small portion of titrant before filling
it
 Fill the burette to higher level than zero mark then remove the funnel and adjust it to
the zero mark..

Figure 5: accurate reading of the volume of a liquid inside the burette

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Lab Report 1
Name: ID: Date: Sample no:

Pipette exactly 10 ml of 0.1 mol.L-1 NaOH solution in the conical flask, fill the burette with the
provided solution of HCl, then add few drops of phenol phthalein indicator, and start the
titration until the colour changes into very faint pink, stop the titration.

Record your results in the following table

Experiment Experiment Experiment Experiment

Volume/cm3 Rough
1 2 3 4

Final
volume

Initial
volume

Titre volume

From the data above show clearly how to obtain a mean value for the calculations

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Answer the following questions, show your work and write down all required units

1- Write down a balanced equation for the reaction between HCl and NaOH

2- Calculate the number of moles of NaOH that were added into the conical flask.

3- Accordingly, calculate the number of moles of HCl ran from the burette

4- Calculate the molar concentration as well as the strength of the unknown HCl solution.

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Experiment (2): Oxidation-Reduction Titration (Redox

Reaction), Standardization of KMnO4 solution by using
standard oxalic acid solution

1.1 Basic principles to a redox equation

The main idea of balancing a redox equation is to take into consideration that number of
electrons lost by the reducing agent = the number of electrons gained by the oxidizing agent

 Oxidation half reaction

O OH + -
2.5 C C 5CO 2 + 5H + 5e
HO O

 Reduction half reaction

K+Mn+7O4-8 + 3H2SO4 + 5e- Mn+2O +KHSO4+2HSO4-+3OH-

Manganese in potassium permanganate gains 5 electrons (which were lost by oxalix acid),
which makes potassium permanganate an oxidizing agent

 Oxidation –Reduction reaction


K+Mn+7O4-8 + 3H2SO4 + 2.5 H2C2O4 KHSO4 + MnO + CO2 + 2 H2SO4 + 3 H2O

Note that: it is crucial that the reaction mixture is heated prior titration so as to vaporize the
carbon dioxide produced from the decomposition of the oxalic acid (according to Le Chatelier
principle).

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1.2 Reagents and material

1- A primary standard 0.01 mol.L-1 oxalic acid solution.
2- KMnO4 sample solution of unknown concentration.
3- 1 mol.L-1H2SO4 solution.

1.3 Glass ware & apparatus

1- 25 ml burette
2- 10ml pipette
3- 250 ml conical flask
4- 250 ml beaker
5- Water bath
6- Funnel
7- Safety filler
8- Washing bottle

1.4 Procedure
1- Transfer 10 ml of oxalic acid solution into conical flask, and add 20 ml of 1M H 2SO4
solution (to provide an acidic medium which prevents the formation of a brown ppt of
MnO2).
2- Heat the solution to 60-70ºC in a water bath, why?
3- Titrate the hot oxalic acid by dropwise addition of the unknown sample solution of
KMnO4 from the burette, till a faint violet color is obtained, and record the volume
added.
4- Repeat the titration at the same temperature range to a consistent reading, after each
titration; make sure that the colour obtained is permanent by putting the conical flask in a
water bath for 2 minutes.

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5- Use the balanced equation to form a stoichiometric relationship between the number of
moles of permanganate Vs the number of moles of oxalic acid
6- Use the previous relation in determining the concentration of the unknown sample
solution of permanganate (both in molarity and strength).

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Lab Report 2
Name: ID: Date: Sample no:

Transfer exactly 10 ml of oxalic acid solution into conical flask, and add 20 ml of 1M H2SO4
solution, then heat the solution to 60-70ºC in a water bath.
Titrate the hot oxalic acid by dropwise addition of the unknown sample solution of KMnO4
from the burette, till a faint violet color is obtained.

Record your results in the following table

Experiment Experiment Experiment Experiment

Volume/cm3 Rough
1 2 3 4

Final
volume

Initial
volume

Titre volume

From the data above show clearly how to obtain a mean value for the calculations

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Answer the following questions, show your work and write down all required units
1- State the reason why H2SO4 has to be added to acidify the medium of the reaction.

2- A very important and a crucial step during titration, was to heat the reaction mixture in a
water bath over a temperature range of 60-70ºC. state why it is important to heat the
reaction mixture. Also state the reason why the reaction mixture can’t be heated above
that temperature range.

3- Write down a balanced Ionic Equation depicting the reaction between potassium
permanganate and oxalic acid by answering the following questions
 Determine the oxidation number of Mn in MnO4-
 Determine the electrons gained/lost in MnO4-/Mn+2

 Determine the oxidation number of carbon in H2C2O4

 Determine the oxidation number of carbon in CO2

 Determine the electrons gained/lost in H2C2O4/CO2

4- Calculate the number of moles of oxalic acid that were added into the conical flask.

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5- Accordingly, calculate the number of moles of potassium permanganate that were run
from the burette.

6- Calculate the molar concentration as well as the strength of the unknown potassium
permanganate solution.

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Experiment (3): Complexometric Titration (Complex

formation), Determination of the total hardness of water
using EBT indicator

1.1 Introduction:
Complexometric titration or complex formation depends on the formation of a complex
between a ligand and metal ion.
A ligand is an atom, ion, or molecule that generally donates one or more electrons through
covalent or coordinate bonds.

Covalent = Sharing of electrons between both moieties.

Coordinate = Sharing of electrons where only one moiety donates
(Doner = Lewis base & Acceptor = Lewis acid)

Example of ligand or complexing agent = EDTA & EBT

Instead of EDTA (water insoluble), the sodium or potassium salt of EDTA (water soluble) is
used.

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The reaction is always 1 : 1 mol for any metal with EDTA, hence

(M×V) EDTA = (M×V) metal

Notes : (i) M is the Molarity
(ii) Up to 200 ppm the water is safe (valid) for drinking with
respect to hard salts.

1.2 Principle
The hardness of water is generally due to dissolved calcium and magnesium salts, EDTA
(Ethylene Diamin Tetra Acetic acid) form complex with calcium & magnesium ions, so
hardness of water can be determined by complexmetric titration.

1.3 Reagents and material

1- Standard (0.01M) EDTA solution.
2- Buffer (PH10) solution [(NH4OH + NH4Cl) or (Sodium borate)].
3- Eriochrom black T. (EBT) indicator (It is solid crystals mixed for work with KNO3 or
NaCl).
Note: EBT is the sodium salt of 1-(1-hydroxy-2-naphthylazo)-2-naphthol-6-nitro-4-
sulphonic acid.

1.4 Glass ware

 25 ml burette
 10ml pipette
 250 ml conical flask
 250 ml beaker
 Glass rod
 Funnel
 Safety filler
 Washing bottle
 Spatula

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1.5 Procedure
1. Transfer about 50 ml of tap water (which contains hard salts Of Mg ++ and Ca++) into a
beaker at first and then by pipette to conical flask, and add 5ml buffer PH 10 (to provide
Alkaline medium necessary for indicator work )
2. Add just few crystals of EBT indicator using spatula, the color will be red or pink.
3. Add standard EDTA 0.01 M solution, drop by drop, from the burette during shaking the
conical flask, until a pure blue color is obtained, and record the volume of EDTA added.
4. Repeat the titrations three times at least and compute the average volume of the EDTA.

1.6 Calculation
Hardness of water is expressed in ppm CaCO3

Applying equation (M×V) CaCO3 = (M×V) EDTA

(M × V) EDTA
M CaCO3 (Majority salt solution) = = Molar
V (Sample of salt solution)

0.01 × V EDTA
Molarity = ………………….(1)
50 (ml)

Mass of solute (g) mass (mg)

Molarity = =
Molar mass × Volume (L) 1000 × Molar mass ×Volume (L)

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Molar mass of CaCO3 = 100

ppm
Molarity of water solution = ………………….(2)
1000 × 100

From (1)&(2)

0.01 × V EDTA ppm

=
50 (ml) 1000 × 100

Hardness of water (ppm) = V EDTA× 20

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Lab Report 3
Name: ID: Date: Sample no:

Transfer exactly 50 ml of tap water into conical flask, and add 5 ml of buffer solution, then add
few crystals of EBT.
Titrate the mixture by dropwise addition of the of 1M EDTA Solution from the burette, till a
faint blue color is obtained.

Record your results in the following table

Experiment Experiment Experiment Experiment

Volume/cm3 Rough
1 2 3 4

Final
volume

Initial
volume

Titre volume

From the data above show clearly how to obtain a mean value for the calculations

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Answer the following questions, show your work and write down all required units
1- What is the cause of hardness in water?

2- State the reason why buffer solution has to be added to the medium of the reaction.

3- EDTA solution is not colored, however the color changes from red to blue due to the
indicator (explain why?).

4- Calculate the Value of the hardness of water. Is this water safe?

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Qualitative Analysis
A qualitative analysis shows what elements or ions a given substance contains, in the
following section we are concerned about the identification of inorganic substances.
An inorganic substance may be an element, compound or a complex compound.
Furthermore, inorganic compounds can be classified into acids, bases and salts.
An Acid (HA) is a compound that dissociates in the presence of water to give H+ ion and an
anion (called the Acid radical A-) as follows
HA H+ + A-
HNO3 H+ + NO3-
HCl H+ + Cl-
H2SO4 2 H+ + SO42-
A Base (BOH) is a compound capable of dissociation in the presence of water, to give OH-
ion and a cation (called the Basic Radical B+) as follows
BOH B+ + OH-
NaOH Na+ + OH-
A Salt: is a compound that is produced from acid-base neutralization reaction as follows
Acid + Base Salt + H2O
HA + BOH BA + H2O
HNO3 + NaOH NaNO3 + H2O
H2SO4 + 2NH4OH (NH4)2SO4+ 2H2O
Therefore, it is clear that any salt consists of two radicals, an Acid Radical such as Cl-, NO3-
,SO42-, and a Basic Radical such as Na+, K+, Ca2+.

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1.7 Detection of a simple salt

In order to detect a simple salt we have to follow the following steps:

 Study the physical properties.

 Identify and detect the acid radical.

 Identify and detect the basic radical.

1.8 Physical properties

There are some physical properties which are usually studied for any solid salt:

 Color (white, yellow, green, blue …etc.)

 Shape (powder, or crystals)

 Solubility (water soluble, or water insoluble)

 Melting point.

 Odor.

 Hygroscopicity

1.9 Identification of the acidic and basic radicals of the salt

A separate set of experiments will be carried out to identify the acidic radical of the salt,
followed by a separate set of experiments to identify the basic radical of the salt. Finally both
radicals will be combined in appropriate proportions to obtain the proper formula of the salt.

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Experiment (4): Qualitative Analysis

I- Detection of the acidic radical (Anion)
Detection of (CO32-, S2O32-, Cl-, Br-, SO42-, PO43-)
 Note that it is very important to work the experiments according to the mentioned
sequence, because the anions in the following table are arranged in a certain order, so
that the anions in the bottom cannot give any result with the reagents at the top of the
table.

 However, an anion from the top can possibly give a result with a reagent from the
bottom, so again it is very important to work them in the mentioned sequence.
 The main idea about the detection is involving the substitution of the anion from the salt,
and the formation of a gas, a colour, or a precipitate having a distinctive property.

 All the experiments are carried on the salt solutions.

Table 2: A scheme for identifying the acid radicals

Ion Reagent reaction

Effervescence with the evolution of a
Carbonate (CO32-) colourless gas that turns lime water milky
CO32- + 2HCl 2Cl- + CO2 + H2O
HCl dil. A colourless gas with a pungent odor is
evolved along with the formation of a
Thiosulphate(S2O32-) yellow ppt.
2-
S2O3 + 2HCl 2Cl- +SO2 + S+
H2O
A white ppt. is formed which is insoluble
Sulphate (SO42-) in dilute acids.
Barium chloride 2-
SO4 + BaCl2 BaSO4 + 2Cl-
(BaCl2) A white ppt. is formed which is soluble
Phosphate (PO43-) in dilute acids.
3-
HPO4 + BaCl2 BaHPO4 + 2Cl-
A white ppt. of lead chloride is formed
Chloride (Cl-) Lead Acetate
2Cl- + Pb2+ PbCl2
(CH3COO)2Pb A bright yellow ppt. of lead iodide is
Iodide(I-)
formed 2I- + Pb2+ PbI2

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Figure 6: a scheme showing the sequence of identification of the acid radicals

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II- Detection of the basic radicals (Cations)

Detection of (Pb2+, Cu2+, Al3+, Fe2+, Fe3+, Mn2+,Mg2+,Zn2+ )
Most of the metal cations form water insoluble [Link] hydroxides either have
distinctive colours, or do acquire different solubilities in excess of the reagent.
The reagents used to precipitate the hydroxides are sodium hydroxide and ammonium
hydroxide. Both of the tests have to be performed to deduce the identity of the cation.
Table 3: A scheme for identifying the Basic Radicals

Ion Reaction with NaOH Reaction with NH4OH

1- Gives a pale blue ppt.
Gives a pale blue ppt. which is insoluble
in excess reagent Cu2++2NH4OH Cu(OH)2+ 2NH4+
Cu2++2NaOH Cu(OH)2+ 2Na+ 2- It dissolves in excess reagent into a deep
Cu2+ blue colour
Cu(OH)2+4NH4OH [Cu(NH3)4](OH)2 +
4H2O
Gives a dirty green ppt. insoluble in Gives a dirty green ppt. insoluble in excess
2+ excess reagent reagent
Fe
2+ +
Fe +2NaOH Fe(OH)2+ 2 Na Fe2++2 NH4OH Fe(OH)2+ 2 NH4+
Gives a reddish brown ppt. Gives a reddish brown ppt.
Fe3+ 3+ +
Fe +3NaOH Fe(OH)3+ Na Fe3++ NH4OH Fe(OH)3+ 3 NH4+
Gives a white ppt. which is soluble in Gives a white ppt. which is insoluble in
3+ excess reagent excess reagent
Al
3+ +
Al +3NaOH Al(OH)3+ 3 Na Al3++3 NH4OH Al(OH)3+ 3 NH4+
Gives a white ppt. which is soluble in Gives a white ppt. which is insoluble in
2+ excess reagent excess reagent
Pb
2+ +
Pb +2NaOH Pb(OH)2+ 2 Na Pb2++2 NH4OH Pb(OH)2+ 2 NH4+
Gives off white ppt. of Mn(OH)2 Gives off white ppt. of Mn(OH)2 insoluble in
Mn2+
insoluble in excess reagent excess reagent
Gives white ppt. of Mg(OH)2 insoluble Gives white ppt. of Mg(OH)2 insoluble in
Mg2+
in excess reagent excess reagent
White ppt. of Zn(OH)2 soluble in excess White ppt. of Zn(OH)2 soluble in excess
Zn2+
reagent reagent
[Lead(II) ions can be distinguished from aluminium ions by the insolubility of lead(II) chloride.]

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Lab Report 4
Name: ID: Date: Sample no:

1- Physical properties:
Color :
Shape :
Solubility:
2- Chemical properties:

Experiment Observation Result

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Name: ID: Sample no:

Date:

1- Physical properties:
Color :
Shape :
Solubility:
2- Chemical properties:

Experiment Observation Result

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Name: ID: Date: Sample no:

1- Physical properties:
Color :
Shape :
Solubility:
2- Chemical properties:

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Experiment Observation Result

Name: ID: Date: Sample no:

1- Physical properties:
Color :
Shape :
Solubility:
2- Chemical properties:

Experiment Observation Result

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