FACULTY OF PHARMACY

ANALYTICAL CHEMISTRY-I

LABORATORY

Prepared by

Asst. Prof. Dr. Tanem Garanti

Oluwasuyi Oba, MSc

 ANALYTICAL CHEMISTRY-I
LABORATORY CONTENTS
Student Evaluation ……………………………………………………………………….

General Rules …………………………………………………………………………….

Report Format ……………………………………………………………………………

General Laboratory Guidelines …………………………………………………….

Laboratory Safety ……………………………………………………………………

Laboratory Equipments ………………………………………………......................

Experiment 1: Solution Preparation………………………………………………….

Experiment 2: Gravimetric Analysis of Chlorine ……………………………………

Experiment 3: Identification of Cations ………………………………………………

Experiment 4: Identification of Anions ………………………………………………

Experiment 5: Acid-Base Titration …………………………………………………….

General Rules

 Laboratory work is compulsory. In the case of missing more than three laboratory
experiments and getting grades less than 10% would result in failure in Analytical
Chemistry.
 Students must attend all laboratory session only on the appropriate days allocated for their
groups. Changing groups will not be permitted, unless you have a reasonable excuse.
 Each lab sessions consist of:

 A quiz,

 A short discussion,

 The practical work which must be completed and individual reports submitted
afterwards. (See report format)
 Laboratory coats are compulsory in the lab. Nobody is allowed in the laboratory without
laboratory coats.
 You must have a scientific calculator with you in lab sessions, tutorials and in exams.
 Students are personally responsible for any equipment and glassware which they break.
 Students should leave the benches clean and tidy after the experiment.
 No practical work shall be carried out in the absence of instructor.
 Food and drinks are not allowed to be consumed in the laboratory.
Report Format:

1. Cover Page
2. Name of the Experiment
3. Aim of the Experiment
4. Introduction (Background information)
5. Materials (include hazard class for each chemical used)
6. Procedure
7. Results and/or Calculations (if there are any)
8. Discussion
9. Conclusion
10. References

Things to know!

 Cover page should include: Student name, Logo of the Uni, Lecturer’s name and Student
ID.

 Aim of the experiment, Introduction, Procedure, Discussion and Conclusion has to be

written on your own words, meaning you should NOT copy from a book/online
source/lab procedure leaflet and paste it. Find information from online/books, read and
understand it, then with your own words, re-write it to your report.

 All of the students MUST submit individual reports! (this means that each report will be
different than each other). Even though experiments might be done in groups.

 References should be either online articles, web pages (apart from Wikipedia) or
books. Please DO NOT reference lecturer’s notes or Google research. That is NOT
referencing!

 Finally, please submit your reports on time! Each delayed day will cut off 5 points from
your report marks.
GENERAL LABORATORY GUIDELINES

Cleanliness

It is important to keep the equipment and the laboratory clean at all times.

a) Glassware: This should be cleaned with a detergent, rinsed with tap water, and then with
small portions of distilled water.
b) Desks and Reagent Bottles: These should be cleaned at the conclusion of each laboratory
session.
c) Shelf Reagents: If materials are spilled on the shelves, clean it up immediately.
d) Balance Room: Do not spill material in the balance case. Keep the balance room clean.

Use of Acids and Reagents

a) No foreign objects of any kind (Spatula, dropper, pipet) should be introduced into the
reagent bottles at any time.
b) When pouring acids from the desk reagent bottles, do not lay the stopper on the desk. Hold
it between the fingers.
c) Reagents on the shelves are not to be taken to the desks. Pour what is needed of a dry
reagent onto a watch glass or piece of paper. Liquids should either be poured into the vessel
in which they will be used or into a small beaker for transfer. Replace stoppers and bottle
caps when finished.
d) Under no circumstances should a reagent, once removed from a stock bottle, be returned
to the stock bottle.
e) As reagents are expensive, students should learn to estimate their needs and avoid waste.
LABORATORY SAFETY

Potentially, all chemicals are hazardous for your health. In other words, many of them are toxic
and carcinogenic. Constant and excessive exposure of your body to these chemicals by different
means such as inhalation, digestion, skin contact etc. may cause unfortunate health problems.
Therefore, minimize any direct exposure to chemicals during the experiment.

The chemistry laboratory is not a dangerous place, but it demands a reasonable prudence on the
part of an experimenter to keep it safe. The following rules cover some important general
precautions and should be observed at all times.

Principal Safety Rules

 Never smoke, eat or drink in the laboratory.

 Wear your lab coats from the first to the last minute you spend in the lab.
 Learn the use and location of eye-wash bottles, fire blankets and fire extinguishers on the first
day.
 Make sure you are fully informed before attempting to use a Bunsen burner.
 You should never undertake any unauthorized experiments. You should carry out experiments
under the supervision of your laboratory assistants. The chances of accident are high,
particularly with an experiment that has not been completely checked to reduce the hazard.
 You should never work in a laboratory without presence of another person within calling
distance. Minor accidents can become disasters if help is not available.

Eye Protection

 Learn the location and use of eyewash bottles and other facilities. In case any chemical goes
into your eyes, go immediately to the eyewash bottle and flush your eyes with large amounts
of water. Be sure that the eyelids are kept open. Continue flushing the eyes in this way for 15
minutes.
 In the case of persisting pain or any other negative indications inform your assistant to get
medical help.
 Contact lenses should not be worn in the laboratory. If a splash occurs, the lens can act as a
trap for corrosive materials and greatly increase the likelihood of permanent injury. Moreover,
low levels of vapors that are present in the laboratory can cause severe irritation to your eyes
if you wear lenses.
Other Safety Rules Regarding Your Health

 Never taste or smell a compound. Students tend to act this way in order for quick identification
of compounds (especially unknowns). Remember that we have safer experimental techniques
for this purpose.
 Never pipette a chemical by mouth. Use the rubber bulbs supplied for this purpose.
 Avoid contact of the skin with any chemical. If a compound is spilled on your hands, wash
them thoroughly with soap and water. Do not rinse them with a solvent, since this may cause
more rapid adsorption.
 You should always wear shoes in the laboratory. Even open-toed shoes or sandals offer
inadequate protection against spilled chemicals or broken glass.
 Long hair should be tied back. Avoid loose-fitting sleeves and clothing that leaves expanses of
skin unprotected.
 Do not keep the liquids open to the atmosphere. Otherwise, they will be a constant source of
dangerous vapours. Once you finish your work with a liquid, put it in a safe container in a safe
place for further work or to the waste disposal bottles. For the same purpose, all bottles should
be kept tightly closed.
 Never heat a flask or any apparatus that is sealed or stoppered- make certain that there is an
opening to the atmosphere.
 When you feel any difficulty in setting up the apparatus, do not be persistent on exerting excess
pressure, immediately call for help of your assistant.

Poisonous Chemicals

Most of the chemicals you will work with are poisonous to some degree. It is obvious that you
should never taste a chemical unless specifically directed to do so. However, there are more subtle
ways of being poisoned. One of these is breathing toxic vapors. Be careful to work in a ventilating
hood whenever instructed to do so. Even such common substances as carbon tetrachloride,
benzene, and mercury are poisonous and potentially dangerous. Avoid prolonged exposure to these
liquids or the accompanying vapors. Since heating favors the vapor state, these and other
poisonous liquids should be heated only in a hood or with use of a backflow condenser.

Occasionally, you will be directed to test odour of a substance. The proper way to do this is to waft
a bit of the vapor toward your nose. Do not stick your nose in and inhale vapor directly from the
test tube. A possible poisonous danger, frequently overlooked, is contamination through the hands.
Some poisons e.g benzene is rapidly absorbed through the skin and some can stick to the hands,
eventually carried into your mouth. Immediately scrub your hands thoroughly and get into the
habit of washing your hands before leaving the laboratory.

Essential Precautions

Follow all directions with utmost care especially those having to do with hazardous conditions.
Do not perform any unauthorized experiment. If you go to change or supplement the assigned
material, first consult your instructor and get this permission. Irresponsible behavior will result in
immediate expulsion from the laboratory.

First Aid

Keep always in mind that an injury, no matter how much small, must be reported to your assistant
as soon as possible.

Emergency Equipment: Learn the location of eye-wash bottles, fire blankets, and fire
extinguishers, and how these equipments are used.

Chemical Spills on the Skin: Immediately flush with running water for several minutes; if the eyes
or face are involved, use an eye-wash bottle. For any severe chemical burn consult a physician as
soon as possible after the initial thorough water flushing.

Fire: If there is fire, the best advice is to get away from it and let the instructor, assistant or
laboratory technician take care of it. DON’T PANIC! Move quickly and carefully. If it is a small
fire in a flask, it usually can be extinguished quickly by placing wire gauze or, possibly, a watch
lass, over the mouth of the flask. It is a good practice to have a wire screen or watch glass, over
the mouth of the flask. It is a good practice to have a wire screen or watch glass handy whenever
you are using a flame. If this method does not take care of the fire and if help from an experienced
person is not readily available, then extinguish the fire yourself with a fire extinguisher. If the
clothing is ignited, immediately extinguish it with a fire blanket or safety shower or, if necessary,
a coat or anything else available. DO NOT RUN. Walk purposefully toward the nearest fir blanket
or fire shower station. Running will fan the flames and intensify them. Wrapping yourself in the
fire blanket will smoother the flames quickly. If the fire blanket is not readily available, lay down
and revolve around your body.
Chemical Hazard Symbols

Hazard Name Definition Symbol

Flammable Any substance that will burn if exposed to an open
flame.

Explosive A substance that may explode if exposed to heat or

flame.

Teratogenic/ A substance that have adverse effects on

Health effect development of embryo or fetus.

Toxic/poison A substance that can lead to death if inhaled,

ingested, or absorbed by the skin.

Corrosive A substance that can destroy or burn living tissue

and can eat away at other materials

Irritant A substance that causes inflammation upon contact

with skin or mucous membranes.
 Toxic to the Substances that are harmful to the environment.
environment They must be disposed of properly, not washed
down the drain.

Material Safety Data Sheet (MSDS)

A Material Safety Data Sheet (MSDS) is designed to provide both workers (students and staff at
SHS) and emergency personnel with the proper procedures for handling or working with a
particular substance (chemical or element). MSDS's include information such as physical data
(melting point, boiling point, flash point etc.), toxicity, health effects, first aid, reactivity, storage,
disposal, protective equipment, and spill/leak procedures. These are of particular use if a spill or
other accident occurs.

NFPA (National Fire Protection Association)

CHEMICAL HAZARD LABEL
0 4

Least Most
Serious Serious
 Laboratory Equipment
Laboratory equipments are important part of chemistry and science in general. In this section,
you can find information about laboratory equipments and their uses.

Name Description Picture

Beaker Used to hold and heat liquids. Multipurpose and
essential in the lab.

Bottle Bottles can be used for storage, for mixing and for
displaying.

Bunsen burner Bunsen burners are used for heating and exposing
items to flame.

Burette The burette is used in titrations to measure precisely

how much liquid is used.

Crucible Crucibles are used to heat small quantities to very

high temperatures.

Erlenmeyer Flask The Erlenmeyer Flask is used to heat and store

liquids. The advantage to the Erlenmeyer flask is that
the bottom is wider than the top so it will heat
quicker because of the greater surface area exposed
to the heat.
Evaporating Dish The Evaporating Dish is used to heat and evaporate
liquids.
Funnel The Funnel is a piece of equipment that is used in the
lab but is not confined to the lab. The funnel can be
used to target liquids into any container so they will
not be lost or spilled.
Micro spatula The Micro spatula, commonly called a spatula, is
used for moving small amounts of solid from place to
place.

Pipette The pipette is used for moving small amounts of

liquid from place to place. They are usually made of
plastics and are disposable.

Mortar and Pestle The Mortar and Pestle is used to crush solids into
powders for experiments, usually to better dissolve
the solids.

Ring Stand Ring Stands are used to hold items being heated.
Clamps or rings can be used so that items may be
placed above the lab table for heating by Bunsen
burners or other items.

Stir Rod The Stir rods are used to stir things. They are usually
made of glass. Stir Rods are useful in the lab setting.

Test tube Holder The Holder is used to hold test tubes when they are
hot and untouchable.

Test tube Rack It is used to hold test tubes while reactions happen in
them or while they are not needed.

Thermometer The thermometer is used to take temperature of

solids, liquids, and gases. They are usually in 0C, but
can also be in 0F.
Tongs Tongs are used to hold many different things such as
flasks, crucibles, and evaporating dishes when they
are hot.

Volumetric Flask The Volumetric Flask is used to measure one specific

volume. They are mostly used in mixing solutions
where on liter or one half liter is needed.

Watch Glass The watch glass is used to hold solids when being
weighed or transported. They should never be heated.

pH meter A pH meter is an electronic instrument used to

measure the pH (acidity or basicity) of a liquid
(through special probes are sometimes used to
measure the pH of semi-solid substances).
Analytical balance An analytical balance is a device for measuring the
weight of an object.

Heating magnetic A heating magnetic stirrer is a type of laboratory

stirrer equipment consisting of a rotating or stationary
electromagnets creating a rotating magnetic field and
heats the liquid.
Drying ovens Laboratory ovens are for high-forced volume thermal
convection applications. These ovens generally
provide uniform temperatures throughout.

Melting Point Measures the melting point of substances.

Meter (Meltemp
Apparatus)
Fume Hood A fume hood or fume cupboard is a large piece of
scientific equipment common to chemistry
laboratories designed to limit a person’s exposure to
hazardous fumes.
 EXPERIMENT 1: SOLUTION PREPARATION

A solution is a homogeneous mixture created by dissolving one or more solutes in a solvent. The
chemical present in a smaller amount, the solute, is soluble in the solvent (the chemical present
in a larger amount). Solutions with accurately known concentrations can be referred to as
standard (stock) solutions.

Preparing a Standard Solution from a Solid

A solution of known concentration can be prepared from solids by two similar methods.
Although inherent errors exist with each of the methods, with careful technique either will
suffice for making solutions in Chemistry Laboratory.
In the first method, the solid solute is weighed out on weighing paper or in a small container and
then transferred directly to a volumetric flask (commonly called a "vol flask"). A funnel might be
helpful when transferring the solid into the slim neck of the volumetric flask. A small quantity of
solvent is then added to the volumetric flask and the contents are swirled gently until the substance
is completely dissolved. More solvent is added until the meniscus of the liquid reaches the
calibration mark on the neck of the volumetric flask (a process called “diluting to volume”). The
vol flask is then capped and inverted several times until the contents are mixed and completely
dissolved. The disadvantage of this method is that some of the weighed solid may adhere to the
original container, weighing paper, or funnel. Also, solid may be spilled when it is transferred
into the slim neck of the volumetric flask.

Finally, the volumetric flask is diluted to volume (additional solvent is added to the flask until
the liquid level reaches the calibration mark) as shown in figure 1. The flask is capped and
inverted as before until the contents are thoroughly mixed. The disadvantage to this method is
that some of the solution may adhere to the beaker, stirring rod, or funnel if not washed
thoroughly. Also, a possibility of contamination exists from the beaker, rod, or funnel if they
have not been washed carefully.

Figure 1: Preparing a solution of known concentration from a solute.

In general chemistry molarity is the most commonly used concentration unit:

(1) Molarity = moles of solute = grams of solute

liters of solution molar mass solute x liters of solution

Example: A student weighs 0.563 g of FeCl3 and dissolves it in enough deionized (DI) water to
make 100.0 mL of solution. (FeCl3 is the solute and water is the solvent; the mixture of FeCl3
and water is called the solution.) The molarity of the FeCl3 (aq) solution is:

0.563 g FeCl3 = 3.47 x 10-2 M

162.2 g /mol FeCl3 x 0.1000 L

Diluting a Solution of Known Concentration

Dilution is the addition of more solvent to produce a solution of reduced concentration. Most often
a diluted solution is created from a small volume of a more concentrated stock solution. To make
such a solution, a volumetric pipet is used to deliver an exact amount of the stock solution into a
clean volumetric flask, which is then diluted to volume. To prevent extra dilution or contamination,
prerinse the vol pipet with the stock solution to remove any water droplets or impurities. (The
rinsings should be placed in an appropriate collection container.) As shown in figure 2.

Figure 2: Dilution a solution

The diluted solution’s molarity is less than the stock solution it was created from. The moles
present in the volume of stock solution delivered by the volumetric pipet is equal to the moles
present in the diluted solution created:

(2) (Moles of solute)before dilution = (Moles of solute) after dilution

The moles of solute is also equal to the molarity (M) of the solution times the volume (V) of the
solution (note that the volume units cancel):

(3) Moles of solute = M x V = mol/liter x liter So

equation (2) can be rewritten:
(4) M1V1 = M2V2 (where 1 = "before dilution" and 2 = "after dilution")

Example: A student pipets exactly 5.00-mL of 3.47 x 10-2 M FeCl3 solution into a vol flask and
adds enough water to make 250.-mL of solution. What is the concentration of the diluted solution?
Answer: Let M2 be the concentration of the new solution. By using equation (4) and substituting
known values for M1, V1 and V2, solve for M2:

-2
M2 = M1V1 = (3.47 x 10 M)(5.00 mL) = 6.94 x 10-4 M

V2 (250 mL)
 EXPERIMENT 2
GRAVIMETRIC ANALYSIS OF CHLORINE

Theory:
Gravimetric analysis is a technique through which the amount of an analyte (the ion being
analyzed) can be determined through the measurement of mass. Gravimetric analysis depends on
comparing the masses of two compounds containing the analyte. The principle behind gravimetric
analysis is that the mass of an ion in a pure compound can be determined and then used to find the
mass percent of the same ion in a known quantity of an impure compound. In order for the analysis
to be accurate, certain conditions must be met:
1. The ion being analyzed must be completely precipitated.
2. The precipitate must be a pure compound.
3. The precipitate must be easily filtered.

An example of a gravimetric analysis is the determination of chloride in a compound. In order to

do a gravimetric analysis, a cation must be found that forms an insoluble compound with chloride.
This compound must also be pure and easily filtered. The solubility rules indicate that Ag+, Pb2+,
and Hg2+ form insoluble chlorides. Therefore, silver chloride could be used to determine % Cl -,
because it is insoluble (that is, about 99.9% of the silver is converted to AgCl) and it can be formed
pure and is easily filtered.

Procedure:
1. You will obtain an unknown amount of NaCl solution in a beaker ~ 20mL.
2. Add a precipitating agent (AgNO3 solution) to the solution (see Fog.1 below). Cl- will
precipitate quickly after forming AgCl water-insoluble compound.

Figure 1: The addition of a precipitating agent.

 3. Test for complete precipitation by adding a drop of the precipitating agent and looking for
any sign of precipitate.
4. Weigh out a filter paper and record weight of the filter paper in your notebook.
5. Filter the solution using a funnel and the filter you weighed in previous step. It is important
that the precipitate is quantitatively transferred to the filter. If any remains in the beaker,
the mass obtained will be inaccurate.
6. Add extra distilled water into the beaker and filter it on top of your sample to be able to
obtain the remaining part of AgCl from the beaker.
7. Dry (in the oven) and weigh the precipitate (one day later).
Weight of the precipitate = (Weight of the filter paper + precipitate) – (Filter paper)

Calculations:
1. Use stoichiometry to determine the mass of the ion being analyzed.
2. Find the unknown amount of NaCl that was given to you at the beginning of the in terms
of gram.

The following example calculations would be done for the gravimetric determination of
chloride (this is only an example for you to help you with your calculations):
Mass of sample of unknown chloride after drying: 0.0984 g
Mass of AgCl precipitate: 0.2290 g
One mole of AgCl contains one mole of Cl-, therefore:
𝑔
(0.2290 𝑔 𝐴𝑔𝐶𝑙)⁄(143.323 𝑚𝑜𝑙) = 1.598 × 10−3 𝑚𝑜𝑙 𝐴𝑔𝐶𝑙
𝑔
(1.598 × 10−3 𝑚𝑜𝑙 𝐴𝑔𝐶𝑙) × (58 𝑁𝑎𝐶𝑙) = 0.092 𝑔 𝑁𝑎𝐶𝑙
𝑚𝑜𝑙
 EXPERIMENT 3
IDENTIFICATION OF CATIONS

Introduction

Qualitative analysis is used to identify and separate cations and anions in a sample substance.
Unlike quantitative analysis, which seeks to determine the quantity or amount of sample, qualitative
analysis is a descriptive form of analysis. The common cations may be divided, for purposes of qualitative
analysis, into a number of groups which are distinguished by the fact that the cations of any group are
precipitated by a particular group reagent. Thus, by addition of a slightly excess of dilute hydrochloric acid
to a solution containing all the common cations, a precipitate is obtained. Similarly, by the use of the
appropriate group reagents, the remaining cations are separated into different groups. In general, it may be
stated that the classification is based upon the varying solubilities of the chlorides, sulphides, hydroxides
and carbonates.

The table below shows some of the various groups and the precipitates formed with the reagents used:

Group Group reagent Ions Formula of Distinguishing

precipitates features
I Dilute HCl Ag+, Pb2+, Hg22+ AgCl, PbCl2, Chlorides
Hg2Cl2 insoluble in cold
HCl
II H2S in the Hg2+, Pb2+, Cu2+ HgS, PbS, CuS Sulphides
presence of dilute insoluble in dilute
HCl HCl
III NH3 in presence Al3+, Cr3+, Fe3+ Al(OH)3, Hydroxides
of NH4Cl Cr(OH)3, Fe(OH)3 precipitated by
NH3 in presence
of excess of
NH4Cl

Procedure:

Ag+ ion determination

1. Add 1 mL distilled water and 3-4 drops of 3M HCl to 3mL of Ag+ ion solution
 Ag+ + HCl- AgCl + H+
2. Add 1 mL of 2M NH3 solution to the precipitate. The precipitate (AgCl) is solubilized by forming
a complex molecule.

AgCl + 2NH3 [Ag(NH3)2]+ + Cl-

3. Take 3mL of the Ag+ ion solution, add 2-3 drops of 2M NaOH. Observe the color change and
solubility in few drops and in excess.

Hg22+ ion determination

1. Take 10 drops of Hg22+ ion solution. Add about 8-10 drops of 6M HCl. White Hg2Cl2 precipitates.
Wait for the precipitate to settle for about 5mins.

Hg22+ + 2HCl Hg2Cl2 + 2H+

2. Add 3-4 drops of 2M NH3 solution to the precipitate. Observe color change. The mixture includes
NH2Cl2 + 2NH3 NH2HgCl + Hg + NH4+ + Cl-

Fe3+ ion determination

1. Take 3mL of Fe3+ ion solution, add few drops of 2M NaOH and in excess. Observe the color
change and solubilities.

Fe3+(aq) + 3OH-(aq) Fe(OH)3 (s)

2. Add 3-4 drops of 2M NH3 solution to Fe3+ ion solution.

Fe3+(aq) + 3NH3(aq) Fe(OH)3(s) + 3NH4+(aq)

QUESTIONS

1. Observations of reactions including color changes, precipitation and the colour of the precipitate
must be reported
2. Write the reaction mechanisms of the experiments
3. Write on which of the ions is more soluble and why (Consider Ksp values at this point)
4. The solubility product (Ksp) of AgCl is 1.8 x 10-10, find out the solubility products of the
remaining precipitates.
5. Why is Ksp important for solubilty?
 EXPERIMENT 4

IDENTIFICATION OF ANIONS

Introduction

Qualitative analysis is used to identify and separate cations and anions in a sample substance.
Unlike quantitative analysis, which seeks to determine the quantity or amount of sample, qualitative
analysis is a descriptive form of analysis. The anions are negatively charged ions produced by the ionization
of acids and salts. With the exception of the fluoride, chloride, bromide, iodide and sulfide ions, the anions
are composed of two or more elements bound in chemical combination. Such combinations vary widely in
stability and reactivity. Oxidizing anions tend to react with reducing anions, and in the reactions, the ions
lose their identities as a result of the oxidation- reduction reaction. Reactions of this type are avoided by
maintaining pH above 7 through the first three groups of the anion scheme

The table below shows some of the various groups and the precipitates formed with the reagents used:

Group Group reagent Ions Formula of Distinguishing

precipitates features
I Ca(CH3COOH)2 CO32-, PO43-, CaCO3 (white), Calcium salts
Ca3(PO4)2 insoluble in
(White) neutral or slightly
basic solution
II Ba(CH3COOH)2 CrO42-, SO42-, BaSO4 (White) Barium salts
BaCrO4 (Yellow) insoluble in
slightly basic
solution
III Cd(CH3COOH)2 S2- CdS (yellow) Cadmium salts
insoluble in
neutral or slightly
basic solution

Procedure:

Cl- ion determination

1. Add 4-5 drops of 0.1M AgNO3(ag) to 3mL of Cl- ion solution

Cl-(aq) + Ag+(aq) AgCl(s)

 2. Add few drops of 2M NH3 solution to the precipitate and then in excess.

When excess NH3 is added;

AgCl(s) + 2NH3(aq) [Ag(NH3)2]+(aq) + Cl-(aq).

(Diammine silver(I) ion)

I- ion determination

1. Add 4-5 drops of 0.1M AgNO3(ag) to 3mL of I- ion solution

I-(aq) + Ag+(aq) AgI(s)

2. Add 3-4 drops of 2M NH3 solution to the precipitate. Observe color change and solubility.

SO32- ion determination

1. Take 3mL of SO32- ion solution, add 5-6 drops of Acidified K2Cr2O7 and in excess. Observe the
color change.

2 SO32- (aq) + Cr2O72-(aq) + 8H+(aq) 3SO42-(aq) + 2Cr3+(aq) + 4H2O(L)

2. Take 3mL of SO32- ion solution, add 5-6 drops of Acidified KMnO4 and in excess. Observe the
color changes.

5 SO32- (aq) + 2MnO4-(aq) + 6H+(aq) 5SO42-(aq) + 2Mn2+(aq) + 3H2O(L)

QUESTIONS

1. Observations of reactions including color changes must be reported

2. Write the reaction mechanisms of the experiments

3. Write on which of the ions is more soluble and why

4. Which of the reactions is a reduction reaction and what is the oxidizing agent?
 EXPERIMENT 5
ACID – BASE TITRATION

Theory:

Titration is a technique that chemists use to determine the

unknown concentration of a known solution (we know what
chemical is dissolved, but not how much in a solution). Because
we know what the chemical is, we know how it will react with
other chemicals and we can use that reaction to determine the
concentration of the solution by measuring the formation of
product(s). This type of reaction is a neutralization reaction, where
salt and water are products of the reaction:
Acid + Base Salt + H2 O

Standardization is the process of determining the exact concentration (molarity) of a

solution. Titration is one type of analytical procedure often used in standardization. A titration is
a technique where a solution of known concentration is used to determine the concentration of an
unknown solution. Typically, the titrant (the know solution) is added from a burette to a known
quantity of the analyte (the unknown solution) until the reaction is complete. The equivalence
point in a titration is a theoretical point reached when the amount of added titrant is chemically
equivalent to the amount of analyte in the sample. We cannot determine the equivalence point of
a titration experimentally. Instead, we can only estimate its position by observing some physical
change associated with the condition of chemical equivalence. The position of this change is called
the end point for the titration.

The end point is the point in a titration when a physical change occurs that is associated with the
condition of chemical equivalence. The difference in volume or mass between the equivalence
point and the end point is the titration error.
Indicators are often added to the analyte solution to produce an observable physical change
(signaling the end point) at or near the equivalence point. A chemical substance known as
an indicator is used to indicate (signal) the endpoint. The indicator used in this experiment is
phenolphthalein. Phenolphthalein, an organic compound, is colorless in acidic solution and pink
in basic solution.

Procedures:

1. Preparation of standard solutions; prepare 0.1M NaOH in 100ml distilled water. This
would be the titrant.
2. Standardization of NaOH with 0.1MHCl: Using a pipette, take 10ml of 0.1M HCl into an
Erlenmeyer flask.
3. Add two drops of phenolphthalein into the acid solution
4. Place the flask under the burette and start adding the base solution to the Erlenmeyer flask.
Have one lab partner swirl the flask while the other controls the stopcock. When pink starts
to develop, add the solution more slowly. At this point you should add one drop at a time
followed by swirling until a very light pink color persists. Remember, the lighter the pink
the better!!!
5. Record the final reading of the burette.
6. From the unknown Dilute HCl solution, take 10ml of the solution into the Erlenmeyer
flask.
7. Add two drops of the indicator and titrate against the base as repeated above to determine
the concentration of the unknown acid solution.

CALCULATIONS OF UNKNOWN CONCENTRATION

Use this formula for calculation of the unknown concentrations;
C1 V1 = C2 V2
Where,
C1 = Molarity of acid V1 = volume of acid
C2 = Molarity of base V2 = Volume of base

1. Calculation of molarity of unknown dilute HCl solution