Foundation Academy for Sciences and Technology

FAST
Chemistry Lab Manual
2012-2013

1
 TABLE OF CONTENTS

I. Preface 3

II. Proper Laboratory Techniques and Safe Handling . 4

III. Laboratory Safety Rules .. 12

IV. First Aid .. 17

V. Common Laboratory Apparatus and Their Uses . 20

VI. Students Activity Marks .. 27

VII. Solubility Test for Organic Compounds .. 28

VIII. Baeyers Test for Unsaturation.... 31

IX. Bromine Test for Unsaturation . 33

X. Properties of Arenes (Benzene) .. 35

XI. Lucas Test for 10, 20, and 30 Alcohol ... 37

XII. Classifying Alcohols Using Acidified Potassium Dichromate. 39

XIII. Properties of Aldehydes and Ketones .. 42

XIV. Tollens Test for Aldehydes .. 44

XV Fehlings Test for Aldehydes 46

XVI. Iodoform Test for Methyl Ketones 48

XVII. Oxidation of Carbonyl Compounds by Acidified Potassium Dichromate. 51

XVIII. Oxidation of Carbonyl Compounds Using Fehlings Solution .. 53

XIX. Fehlings Test for Carbohydrates . 55

2
 PREFACE

This Chemistry Laboratory Manual is designed specifically for the students in the
Foundation Year to be able to equip them with the knowledge and skills in conducting
experiments following the scientific investigations and guidelines. The manual aims to
help the students to have full understanding of the theoretical concepts being introduced
in the class by having them performed related experiments in the laboratory. Proper
Laboratory Techniques are discussed and by understanding these, the level of safety
in the laboratory will be increased. Safety Rules that should be observed in the lab are
also included. A section on First Aids which explains the things that should be done in
case of accidents is also included. Apparatus that are commonly used in the laboratory
as well as their functions are also given in a separate section. Activities included in this
manual are those related to Organic Chemistry such as Solubility Test for Organic
Compounds, Tests for Unsaturated Hydrocarbons, Properties of Arenes or Aromatic
Compounds, Classifying Alcohols, Oxidation of Carbonyl Compounds by Acidified
Potassium Dichromate, Fehlings Test for Aldehydes , Iodoform Test for MethylKetones,
and Fehlings Test for Carbohydrates.

The students are expected to benefit from this manual by having them experience the
excitement and fun of performing every experiment in the laboratory. It will surely
improve their learning ability because activities are prepared in parallel with the lessons
they will have in the class.

So learn and have fun!!!

Maria Leila S. Basas, Chemistry Lecturer
Mylene Lourdes L. Delmo, Chemistry Laboratory Instructor

3
 PROPER
LABORATORY
TECHNIQUES
&
SAFE
HANDLING

4
 PROPER LABORATORY
TECHNIQUES & SAFE HANDLING

Working in the chemistry laboratory, you will be handling potentially

dangerous substances and performing unfamiliar tasks. This section provides you with a guide to
the safe laboratory techniques needed in this course. While performing experiments throughout
the year refer back to this section any time you are unsure of proper laboratory techniques.

Read with understanding the procedure of the experiment or activity.

Make sure that you have the proper equipment, and that you know how to use it.
Always read the label on a reagent bottle before using its contents.
Always wear safety goggles when handling corrosive chemicals.
Always wear face masks when handling chemicals emitting unpleasant odor.
Never touch chemicals with your bare hands. Wear gloves to protect your hands.
Never return unused chemicals to their original containers. To avoid waste, do not take
excessive amounts of reagents.

A. Transferring Solid Chemicals

Solid chemicals are generally kept in reagent bottles. Dark-colored (or Amber) reagent bottles
are used to protect some chemicals from bright light. The following are some techniques in
transferring solid chemicals from reagent bottles:

1. Stoppers of reagent bottles should be laid with the flat side on the table to prevent
contamination.
2. Solid chemicals are spooned out from the reagent bottle using a clean and dry spatula. A
dirty spatula will not only contaminate the portion taken but also that which is left in the
bottle.
3. Use a piece of paper to transfer solids to a small-mouthed container, like a test tube.

Practice the technique of transferring solids to a test tube using common table salt in a sample
reagent bottle.

a. Get a piece of clean paper. Fold it lengthwise. Cut it in such a way that it is about 2 cm
longer than the test tube and slightly wider than its diameter.
b. Place the solid chemical you obtained from the reagent bottle with a spatula near the edge
of the paper.

5
 c. Hold the test tube in a horizontal position. Slide the paper into the test tube until it
touches the bottle.
d. Incline the test tube and tap the paper gently. In this way, the solid is deposited at the
bottom of the test tube and not along the sides.

B. Transferring Liquid Reagents

Liquid reagents are usually stored in properly labeled reagent bottles. Liquid reagents should be
poured into clean and dry vessels. To avoid contamination, do not pour reagents directly to a
reaction mixture and do not return excess liquid reagents to their bottles after performing an
experiment.

Ways of transferring liquid reagents depend on the type of receiving vessel. The following are
techniques in transferring liquid reagents into different types of glassware:

1. When pouring a liquid reagent into a wide-mouthed container, the neck of the reagent
bottle must touch the rim of the receiving vessel. A glass rod may also be used to prevent
the liquid from running down the outside surface of t he bottle. The glass rod is held
against the lip of the bottle to direct the liquid into the receiving container.
2. Use a glass rod or a funnel when transferring a liquid reagent into a narrow-mouthed
container.
3. If only a small amount of liquid reagent is needed, a pipette or a medicine dropper may
be used. A pipette is a glass tube calibrated to deliver specific volumes of liquids. When
using more than one liquid reagent, use a separate pipette for each reagent, to avoid
contamination.

Practice the techniques of transferring liquid reagents using a reagent bottle filled with water.

a. Transfer a definite volume of water from the reagent bottle into a beaker by pouring.
b. Use a glass rod in transferring water from the reagent bottle into the beaker.

6
c. Use a glass rod or a funnel to transfer a definite volume of water from the reagent bottle
into an Erlenmeyer flask.
d. Using a pipette, get a definite amount of water from the reagent bottle and transfer it to
the beaker.

7
C. Separating a Solid from a Liquid

Sometimes it is necessary to separate a solid from a liquid. The most common method of
separating such a mixture is filtration.

1. Fold a filter paper circle in half and then quarters. Open the folded paper to form a cone, with
one thickness of paper on one side and three thicknesses on the other.

2. Put the paper cone in a filter funnel. Place the funnel in an iron ring clamped to a ring stand.
Moisten the filter paper with a small volume of distilled water, and gently press the paper against
the sides of the funnel to achieve a good fit. (If the correct size of filter paper has been used, the
top edge of the cone will be just below the rim of the filter funnel.)

3. Place a beaker beneath the funnel to collect the filtrate. The tip of the funnel should touch the
inside surface of the beaker and extend about one inch below the rim. Guide flow of liquid with a
glass rod.

4. Decant the liquid from the solid by pouring it down

a glass stirring rod into the funnel. Be careful to keep
the liquid below the top edge of the cone of filter paper
at all times; the liquid must not overflow. Finally, use
distilled water from a wash bottle to wash the solid into
the filter.

5. When the filtration is complete, wash the solid

residue on the filter paper with distilled water to
remove traces of solvent. Dry the solid.

6. If the filtrate contains a dissolved salt, it may be

recovered by evaporation if desired.

8
D. Measuring Mass

In many experiments you are required to determine the mass of a chemical used or produced in a
reaction. An objects mass is determined by measuring it on a balance. When you determine the
mass of an object, you are comparing its mass with a known mass. In the SI (International
System), the base unit of mass is the kilogram.

1. Check the balance before you start. The balance pan should be empty and clean, and all
masses (or dials) should be set on zero. The balance must be level. Check the bubble level on the
base.

2. Objects to be placed directly on the balance pan must be clean, dry, and at room temperature.
Solid chemicals and liquids must never be put directly on the balance pan. Liquid samples
should be placed in beakers or sealed containers. Solid chemicals can be conveniently placed in
beakers, disposable plastic weighing boats, or on a piece paper.

3. TARE the container before weighing the sample.

4. The balance is a precision instrument that must be handled with care. To avoid damaging it,
always be sure that the balance is in an arrested position when objects are placed on or removed
from the pan.

5. Never move or jar either a balance or the balance table.

6. If you spill a chemical on or near the balance, clean it up immediately.

7. Never attempt to measure an object with a mass greater than the maximum capacity of the
balance.

8. When you are done, return all the masses to zero, and make sure the balance pan is clean.

E. Measuring Volume

Volume measurements are important in many experimental procedures. Sometimes volume

measurements must be accurate; other times they can be approximate. Most volume measures in
the laboratory are made using equipment calibrated in milliliters. Although some beakers have
graduation marks, these marks are designed only for quick, rough estimates of volume.
Accurate volumes must be measured with pipettes, burettes, or volumetric flasks.

9
1. Using a Graduated Cylinder

Half-fill a 100-mL graduated cylinder with water, and set the cylinder on your laboratory bench.
Examine the surface of the water. Notice how the surface curves upward where the water
contacts the cylinder walls. This curved surface is called a meniscus.

A volume measurement is read at the lower meniscus, with your eye at the same level as the
colorless liquid surface. To make the meniscus more visible, you can place your finger or a dark
piece of paper behind and just below the meniscus while making the reading. A volume
measurement is read at the upper meniscus, with your eye at the same level as the colored liquid
surface.

2. Using a Pipette

A pipette is used to accurately measure and deliver volumes of liquids. Two types are in
common use: volumetric pipettes and graduated, or measuring, pipettes.

A volumetric pipette has a single calibration mark and delivers the volume printed on the bulb of
the pipette at the temperature specified.

A graduated pipette has calibrations along the length of the pipette.

Volumes can be measured more accurately with a volumetric pipette than with a graduated
pipette.

10
 Practice the techniques of transferring liquid reagents using
pipettes and pipette aids/ filler with water.

1. Place the tip of the pipette below the surface of the liquid
to be dispensed.
CAUTION: Never fill a pipette by applying suction with
your mouth.

2. Put the pipette aid/filler at the end of the pipette. Roll the adjustable thumb wheel down to take
the liquid until the required volume.

3. Now, deliver the liquid in the pipette into the designated receiver. When releasing liquid from
a volumetric pipette, press the valve lever. Let it drain completely by pressing more the valve
lever.

11
LABORATORY
SAFETY
RULES

12
 LABORATORY SAFETY RULES

Dress Appropriately
When working in the laboratory, always wear your buttoned laboratory coat. Do
not wear unbuttoned long sleeves. Take note of loose clothing
or synthetic garment that may be a fire hazard.

Wear shoes that completely cover your feet to protect them from spilt corrosive,
broken glasswares, or hot liquids. Do not wear open shoes or sandals in the
laboratory.

Tie back long hair. Take off any jewellery or

accessories, such as bracelets or necklaces,
which may get in the way of your work.

Wear protective glasses or safety goggles when carrying out

experiments involving concentrated chemicals or while
heating chemicals.

Wear protective gloves especially when handling chemicals.

Dont Taste or Sniff Chemicals

Never touch, taste, or smell chemicals. Many chemicals are poisonous. If you are
instructed to note the fumes in an experiment, always gently wave your hand over the
opening of a container and direct the fumes toward your nose. Do not inhale directly
from the container. This isnt a cooking class dont taste your experiments!

13
Don't Play Mad Scientist
Don't haphazardly mix chemicals! Pay attention to the order in which chemicals are to
be added to each other and do not deviate from the instructions. Even chemicals that
mix to produce seemingly safe products should be handled carefully. For example,
hydrochloric acid and sodium hydroxide will give you salt water, but the reaction could
break your glassware or splash the reactants onto you if you aren't careful!

Do Not Pipette by Mouth

You say, "But it's only water." Even if it is, how clean do you think that glassware really
is? Learn to use the pipette bulb or automated pipetter. Don't pipette by mouth at home
either. Gasoline and kerosene should be obvious, but people get hospitalized or die
every year, right?

Heating Procedure
When heating a test tube, hold it at an angle of 450 with a test
tube holder and slowly move it back and forth across the flame.
Point the test tube away from yourself and from others.

Never heat chemical that you are not instructed to heat.

Never reach across a flame.

Never leave a lighted burner unattended.

Always use a clamp or tongs when handling hot containers.

Turn off burners that are not in use.

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Precautions About Acids and Bases
When making dilute acids, slowly add acid to the water, not the other way
around.
Wear protective glasses or safety goggles to protect the eyes when handling
acids and bases.
When dilute acids or bases are spilled on the skin or in the eyes, immediately
wash the eyes or skin with plenty of water. Strong bases can cause burns. Weak
bases can cause burns when they are left in contact with the skin.

Fire Safety
Know where to locate water sources, gas outlets, and fire exits.

Know where to find the fire extinguishers, first aid kits, emergency showers, and
fire blankets in case of fire or injury.

If your clothes catch fire, do not run. Cover yourself with a wet blanket or roll on
the floor or use the shower.

If a persons clothes have caught fire, lay the person down, roll the person over,
and smother the flames with a fire blanket.

Do not play with electrical sockets, gas fittings, or flammable chemicals in the
laboratory.

Completely extinguish matches after use an place them in a nonflammable

container. Do not throw matches into a waste basket.

Apparatus used in heating should be allowed to cool before storing them.

Hot objects should not be placed directly on the bench tops, paper, or other
flammable substances. A cool gauze mat should be used.

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Disposal and Clean-Up

Note carefully the method of disposing chemicals in each activity.

Do not return excess chemicals back to their containers.

Clean up spills immediately, even if they are just water, to prevent accidents.

Before you leave the laboratory, do the following:

(1) Clean up the equipment you have used.

(2) Wipe your working table clean.

(3) Check that the water and gas outlets are closed.

(4) Place your stool under the table.

These safety rules should strictly be followed.

Better be safe than sorry . . .

16
FIRST AID

17
 FIRST AID

Injury: Burns

What To Do: Immediately flush with cold water until

burning sensation is lessened.

Injury: Cuts, bruises

What To Do: Do not touch an open wound without

safety gloves. Pressing directly on minor
cuts will stop bleeding in a few minutes. Apply cold compress to
bruises to reduce swelling.

Injury: Fainting

What To Do: Provide fresh air and have the person recline
so that his head is lower than the rest of his
body.

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 First Aid

Injury: Poisoning

What To Do: Find out what substance was responsible for the
poisoning and alert the teacher immediately.

Injury: Spills on the skin

What To Do: Flush with large quantities of water. For acid spills, apply
baking soda solution. For base spills, apply vinegar or boric acid.

Injury: Electrical shock

What To Do: Shut off the current at the source. Remove wire with rubber
gloves. Alert the teacher immediately.

19
 COMMON
LABORATORY
APPARATUS

20
 COMMON LABORATORY APPARATUS

TEST TUBES as containers for holding chemicals

during heating or other reactions.

TEST TUBE RACKS used to support the test tubes.

TEST TUBE HOLDER used to hold the test tube

while heating

STIRRING ROD/ used for stirring or mixing chemicals

GLASS ROD

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ERLENMEYER FLASKS / used as mixing vessels or
CONICAL FLASKS as containers for heating. They
give only approximate volumes.

VOLUMETRIC FLASKS used to measure one

specific volume of liquid.

GRADUATED CYLINDERS / used to measure volumes

MEASURING CYLINDERS of liquids in milliliters (ml)

BEAKERS used as containers for chemicals. They do not

give exact volumes of liquids.

22
PIPETTES measure and deliver exact volumes of liquid.

Graduated Pipette Volumetric Pipette

Pasteurs Pipette (dropper)

PIPETTE AIDS / used with the pipette to take

PIPETTE FILLERS and deliver exact amount of liquid.

FUNNELS used to aid in the transfer of liquid from one

vessel to another

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BUNSEN BURNER used for heating

DIGITAL BALANCE used to measure the mass of an

object in grams.

HOT PLATE STIRRER used as a heat source.

TRIPODS a three-legged stand used to

support the glass apparatus when heating

SPATULA used to spoon out or dispense solid

chemicals from their containers.

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WIRE GAUZE used to protect glass apparatus
from direct application of heat

RINGSTAND/ IRON STAND used to support the burette,

and the burette clamp, and iron ring.

BURETTE CLAMP holds the burette

BURETTE used to dispense volumes of liquid in

titration.

BEAKER TONGS used to move beakers

containing hot liquids.

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MEDICINE DROPPER used to transfer a small volume
of liquid. On top of each medicine
dropper is a rubber bulb.

WASH BOTTLES have spout that deliver wash

solution to a specific area.
Distilled water is the only liquid
that should be used in a wash
bottle.

REAGENT BOTTLES used to store small amount of chemicals

TEST TUBE BRUSH used to clean test tubes and

graduated cylinders.

EVAPORATING DISH are made from glazed porcelain

and are used to hold samples
under high heat conditions.

26
 StudentS Activity MArkS
No. Experiment Title Mark
1 Solubility Test for Organic Compounds

2 Baeyers Test for Unsaturation

3 Bromine Test for Unsaturation

4 Physical Properties of Arenes (Benzene)

5 Lucas Test for 1o, 2o, and 3o Alcohols

6 Classifying Alcohols Using Acidified K2Cr2O7

7 Physical Properties of Aldehydes and Ketones

8 Tollens Test for Aldehydes

9 Fehlings Test for Aldehydes

10 Iodoform Test for Methyl Ketones

11 Oxidation of Carbonyl Compounds by Acidified Potassium Dichromate

12 Oxidation of Carbonyl Compounds Using Fehlings Solution

13 Fehlings Test for Carbohydrates

Average

27
 Batterjee Medical College for Science and Technology
Department of Chemistry
Experiment No. 1 Chemistry Practical
SOLUBILITY TEST FOR ORGANIC COMPOUNDS
Name : _____________________________________

Class : ________________ ID No. _____________

Experiment No. 1
SOLUBILITY TEST FOR ORGANIC COMPOUNDS

I. Introduction :

1. Hydrocarbons

Hydrocarbons are organic compounds that contain only carbon and hydrogen. Hydrocarbons can
either be aliphatic or aromatic. Aliphatic hydrocarbons contain either straight chains,
branched chains and/or certain cyclic arrangements of carbon atoms. Aromatic hydrocarbons
contain at least one aromatic ring, most commonly the benzene ring.

Alkanes are insoluble in polar solvents like water, but very soluble in non-polar solvents such as
other alkanes, diethylether, or carbon tetrachloride. Alkenes are insoluble in water but soluble in
organic solvents. The density of an alkene is less than that of water. Alkynes are colorless,
soluble in water and have a pleasant odor when pure.

2. Alcohol

The general formula of an alcohol is R-OH, where R is an organic group and OH is the
hydroxyl group.
In general, alcohols with one OH group and fewer than five carbon atoms are soluble in water,
but as the hydrocarbon chain gets longer, hydrogen bonding through the single OH group is
not sufficient to keep the entire molecule in solution.

3. Aldehydes and ketones

Aldehydes and ketones are organic compounds which contain a carbonyl group (a
carbon-oxygen double bond).
In aldehydes, the carbonyl group has a hydrogen atom attached to it together with either:
a second hydrogen atom
a hydrocarbon group which might be an alkyl group or one containing a benzene ring.

28
In ketones, the carbonyl group has two hydrocarbon groups attached. Ketones never have a
hydrogen atom attached to the carbonyl group.

In general, aldehydes and ketones with fewer than five carbon atoms will be completely soluble
in water, but as the number of carbon atoms increases, the solubility decreases.

4. Carboxylic Acid

Carboxylic acids are Bronsted-Lowry acids because they are proton (H+) donors.
Smaller carboxylic acids (1 to 5 carbons) are soluble in water, whereas higher carboxylic acids
are less soluble due to the increasing hydrophobic nature of the alkyl chain. These longer chain
acids tend to be rather soluble in less-polar solvents such as ethers and alcohols.

Carboxylic Acid Ester

5. Esters

The small esters are fairly soluble in water but solubility falls with chain length.
The reason for the solubility is that although esters can't hydrogen bond with themselves, they
can hydrogen bond with water molecules.
One of the slightly positive hydrogen atoms in a water molecule can be sufficiently attracted to
one of the lone pairs on one of the oxygen atoms in an ester for a hydrogen bond to be formed.

29
II. Objective:
Describe the solubility of organic compounds in polar and non-polar solvents.
III. Materials :
Test tubes (12) test tube rack acetaldehyde
Pasteurs pipette water oxalic acid
Hexane methanol acetone
Sodium benzoate diethylether
IV. Procedure :
1. Put 1 ml of hexane in the first tube, and 1 ml in the second tube. Add 1 ml of water in
the first tube. Add 1 ml of diethylether in the second tube.

2. Note the observation. Record in the report sheet below.

3. Do the step one for the rest of the compounds listed in the report sheet. Record your
observations below.

Report Sheet:
Organic Compound Water Diethyl Ether

Hexane

Methanol

Acetaldehyde

Acetone

Oxalic acid

Sodium benzoate

Note :
miscible - clear solution with no layering
immiscible - cloudy mixture or two separate layers

30
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _________________ ID No. ______________

Experiment No. 2
BAEYERS TEST FOR UNSATURATION

I. Introduction :

Alkenes and alkynes are both unsaturated hydrocarbons. Baeyers permanganate test
is a test used to distinguish whether the hydrocarbon is saturated or not. In this test, the
hydrocarbon is made to react with dilute potassium permanganate, KMnO4. As the reaction
proceeds, the characteristic color of the permanganate ion is destroyed and replaced by a brown
to black suspension of finely divided manganese (IV) oxide, MnO2. The color change of the
solution from purple to brown (or black) indicates the presence of an alkene or an alkyne.

H H

C =C + KMnO4 C - C + MnO2(s)_

H H OH OH

potassium manganese
alkene permanganate a diol (IV) dioxide

(colorless) (purple) (colorless)

31
II. Objective:

Distinguish saturated from unsaturated hydrocarbon using Baeyers permanganate test

III. Materials :

saturated hydrocarbon 2 test tubes

unsaturated hydrocarbon test tube rack (small)

0.5% KMnO4 solution plastic droppers

IV. Procedure :

1. Put 3 ml of compound A and 3 ml of compound B in two separate test tubes.

2. Add 2 3 drops of 0.5% KMnO4 solution into each of the two labeled test tubes.

3. Shake the mixture for about 1 minute. The color change of the solution from purple to brown
(or black) indicates the presence of an unsaturated hydrocarbon.

V. Report Sheet :

Saturated or Unsaturated
Compound Tested Observations Hydrocarbon

32
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : ____________________________________

Class : _______________ ID No. _______________

Experiment No. 3
BROMINE TEST FOR UNSATURATION

I. Introduction :

Alkanes are saturated hydrocarbons because of the presence of carbon to carbon single
bond. Alkenes are unsaturated hydrocarbons which contain double carbon carbon covalent
bonds.

Bromine test is a test used to determine whether the hydrocarbon is saturated or not.
The decolorization of bromine is a test to distinguish between saturated and unsaturated
hydrocarbons. Only unsaturated ones will decolourise bromine water easily.

II. Objective :

Distinguish saturated from unsaturated hydrocarbon using bromine test.

III. Materials :

saturated hydrocarbon test tube rack

unsaturated hydrocarbon 2 test tubes

bromine solution plastic dropper

33
IV. Procedure :

1. Put 3 ml of compound A and 3 ml of compound B in two separate test tubes.

2. Add 5 drops of bromine solution into each of the two test tubes.

3. Shake both solutions thoroughly. Decolorization of bromine is a positive test for the presence
of double bond or triple bond.

V. Report Sheet :

Saturated or Unsaturated
Compound Tested Observations Hydrocarbon

34
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _________________ ID No. ______________

Experiment No. 4
PROPERTIES OF ARENES or AROMATIC COMPOUNDS (BENZENE)

I. Introduction:

Benzene is the first and principal member of the series of aromatic hydrocarbons. It
has a pleasant odor and colorless at room temperature. It is insoluble in water but soluble in
most non-polar inorganic solvents.

Benzene is an organic chemical compound. It is composed of 6 carbon atoms in a

ring, with 1 hydrogen atom attached to each carbon atom, with the molecular formula of C6H6.

It is an aromatic hydrocarbon, a cyclic hydrocarbon with a continuous pi-bond. It is

colorless and highly flammable liquid with a sweet smell. To test one of its chemical properties
is by burning. When burned, it produces a yellow flame with black smoke and black soot.

II. Objective:

Test the solubility of benzene in different solvents.

III. Materials :

Benzene propanone (acetone) methanol

Water 3 test tubes test tube rack (small)

35
IV. Procedure :

1. Place 1 ml of benzene into each of the three test tubes.

2. Add 1 ml of water in the first test tube.

3. Shake the mixture thoroughly and set it aside in a test tube rack.

4. Do the same to the rest of the compounds (acetone and methanol) to the 2nd and 3rd test
tubes respectively.

5. After 5 minutes, observe each mixture. If the substance is insoluble, a cloudy mixture or two
separate layers are formed. If it is soluble, a clear (transparent) solution with no layering is
observed.

V. Report Sheet:

Compound Tested
Miscible or Immiscible

Water + benzene

Acetone + benzene

Methanol + benzene

36
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical
Department of Chemistry Chemistry Practical

Name
Name :: _____________________________________
_____________________________________
Class
Class :: _________________ IDNo.
________________ ID No._______________
_____________

Experiment No. 5
CLASSIFYING ALCOHOLS AS 1o, 2o, OR 3o BY LUCAS TEST

I. Introduction :

The Lucas reagent is a mixture of ZnCl2 in concentrated hydrochloric acid, HCl. It is used
to determine whether an alcohol is primary (1o), secondary (2o), or tertiary (3o).

The Lucas reagent will convert a soluble alcohol to an insoluble alkyl chloride according to
the reaction:
ZnCl2

R OH + H Cl R Cl + H2O

The appearance of a milky suspension in the reaction mixture indicates the reaction has taken
place. Tertiary alcohols react immediately. Secondary alcohols take time to react. Primary
alcohols will show no reactivity with Lucas reagent.

II. Objective:
Classify alcohol as to primary or tertiary based on the reaction with Lucas reagent.

III. Materials :

ethanol 2 test tubes

tert. butanol plastic dropper
Lucas reagent

37
IV. Procedure :

Caution ! Lucas reagent contains concentrated

hydrochloric acid (HCl). It is toxic and
corrosive. Handle it with care.

1. Put 1 ml of alcohol into each of the two test tubes. Using a dropper, add about 1 ml of Lucas
reagent drop wise/ slowly.

2. Record your observations for each alcohol in the Report Sheet. Then classify the alcohol as to
primary or tertiary alcohol.

V. Report Sheet :

Alcohol Observations Primary or Tertiary Alcohol

Alcohol No. 1

Alcohol No. 2

38
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _________________ ID No. _____________

Experiment No. 6
CLASSIFYING ALCOHOLS BY USING ACIDIFIED POTASSIUM DICHROMATE

I. Introduction :

Alcohols can be oxidized by strong oxidants, such as K2Cr2O7 in H2SO4, but differs
depending on the degree of alcohol

ll

RCH2OH + K2Cr2O7 C + Cr+3

R H

a primary alcohol orange aldehyde green/blue

ll

CH3CH2OH + Cr+6 Cr+3 + C

CH3 H

a primary alcohol orange green/blue an aldehyde

further oxidation

ll

C
CH3 OH

carboxylic acid

39
As the alcohol is oxidized, the Cr+6 is reduced to Cr+3, which turns the orange color of the
solution to blue-to-green color. The appearance of the blue-to-green color within one minute is
considered a positive test for a primary or a secondary alcohol.

OH O

l ll

CH3 - C CH3 + Cr+6 Cr+3 + CH3 C CH3

a secondary alcohol orange green/blue a ketone

no further oxidation

OH

CH3 - C CH3 + Cr+6 no reaction (still orange)

CH3

a tertiary alcohol orange

II. Objective:

Classify alcohol as to primary or tertiary using acidified dichromate (VI) solution.

40
III. Materials :

ethanol 2 test tubes

tert. butanol plastic dropper

acidified K2Cr2O7

IV. Procedures :

1. Put 1 ml of alcohol A into test tube A, and 1 ml of alcohol B into test tube B.

2. Add 2 ml of acidified K2Cr2O7 solution into each of the previously labeled test tubes.

3. Place the two test tubes in a warm water bath.

4. After 5 minutes, note any color change and record your observations on the report
sheet.

V. Report Sheet :

Alcohol Observations Alcohol Classification

(1oor 3o)

41
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _________________ ID No. ______________

Experiment No. 7
PHYSICAL PROPERTIES OF ALDEHYDES AND KETONES

I. Introduction :

In general, aldehydes and ketones with fewer than five carbon atoms will be completely
soluble in water, but as the number of carbon atoms increases, the solubility decreases. The
reason for this lies in the fact that only the carbonyl group can be accommodated by water
through hydrogen bonding and dipole-dipole interactions. If the carbon chains are not large, the
interaction of the carbonyl group with water is sufficient to keep the entire molecule in solution.
But as the number of carbon atoms increases, the water-repelling character of the carbon chain
overwhelms the water-loving nature of the carbonyl group and it is difficult for the organic
molecule to stay in the solution.

II. Objective:

Test the solubility of aldehydes and ketones in water.

III. Materials :

formaldehyde 3 test tubes

propanone (acetone) test tube rack (small)

pentanone

42
IV. Procedure :

1. Label the three test tubes as A, B and C

2. Place 2 ml of distilled water into each of the three previously labeled test tubes.
3. Add 2 ml of each compound to be tested into the appropriate test tube.
4. Shake each mixture thoroughly and set it aside in a test tube rack.

5. After 5 minutes, observe each mixture. If the substance is insoluble in water, a cloudy
mixture or two separate layers are formed. If it is soluble, a clear (transparent) solution with no
layering is observed.

V. Report Sheet :

Compound Tested Miscible or Immiscible

Note :

miscible - clear solution with no layering

immiscible - cloudy mixture or two separate layers

43
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _______________ ID No. _______________

Experiment No. 8
TOLLENS TEST FOR ALDEHYDES

I. Introduction :

Aldehydes can be distinguished from ketones by the Tollens test, because aldehydes are
easily oxidized to carboxylic acids, while ketones are not. Tollens reagent is a solution of silver
nitrate in aqueous ammonia. Silver ion is the oxidizing agent and is reduced to silver metal as
the aldehyde is oxidized to carboxylic acid. The positive Tollens test is the appearance of a
mirror of silver metal on the wall of the test tube, or a dark gray to black precipitate of silver
metal.

RCHO + 2 [Ag(NH3)2] + 2OH- -- RCOO -, NH4+ + 2 Ag + H2O + 3NH3

Aldehyde Tollens reagent soluble salt silver

of the acid mirror

II. Objective:

Distinguish aldehydes from ketones using the Tollens silver mirror test.

III. Materials :

test tubes Tollens reagent

test tube rack acetaldehyde

medicine dropper acetone

44
IV. Procedure :

1. Put 2ml of 5% AgNO3 solution in each test tube. Then add 2 drops of 5% NaOH.

2. Add 1ml of 1M NH4OH solution (aqueous ammonia) until the initial precipitate just dissolves.

3. Add 4 drops of compound A into the first test tube and 4 drops of compound B into the
second test tube

4. Mix each well and warm the test tubes in a water bath for 3 up to 5 minutes. If the test tube
is clean, a silver mirror on the glass surface constitutes a positive test; otherwise, a gray or
gray-black precipitate of silver metal is the positive test.

V. Report Sheet :

Indicate whether you observed a positive reaction (+) or negative reaction (-) in each of the
following compounds using the Tollens test. Write down your observations. Then classify the
compound as to aldehyde or ketone.

Positive or Negative Aldehyde

Reaction with
Compound Tollens Test Observations or
Tested
Ketone

Compound A

Compound B

45
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _______________ ID No. _______________

Experiment No. 9
FEHLINGS TEST FOR ALDEHYDES

I. Introduction :

Aldehydes can be distinguished from ketones by the Fehlings test. Aldehydes are easily
oxidized to carboxylic acids because a hydrogen atom is attached to the carbonyl, while ketones
are not.

acetaldehyde (an aldehyde) acetone (a ketone)

Aldehydes can be oxidized by a mild oxidizing agent like Cu+2 in alkaline solution used in
Fehlings test. Fehlings reagent is a deep blue Cu+2 solution that forms a brick red precipitate
of Cu2O in the presence of aldehydes.

II. Objective:

Distinguish aldehydes from ketones using Fehlings test.

III. Materials :

Fehlings solution (A and B) 2 test tubes

acetaldehyde test tube rack (small)
acetone medicine dropper
100-ml beaker (1) hot plate

46
IV. Procedure :

1. Mix 1 ml of Fehlings solution A with 1 ml of Fehlings solution B in each of the two test
tubes.
2. Then add 1 ml of compound A into the first tube and 1 ml of compound B into the second
tube.
3. Make sure of the tubes with compound A and compound B, before placing them in the water
bath.
4. Heat the mixture for 3 5 minutes in a water bath and take note of any changes in color or
formation of precipitate.

V. Report Sheet :

Aldehyde

Compound Tested Positive Reaction or Observations or

Negative Reaction with
Fehlings Test Ketone

Compound A

Compound B

47
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Experiment No. 7
Name : _____________________________________

Class : _______________ ID No. ________________

IODOFORM TEST FOR METHYL KETONES

Experiment No. 10
IODOFORM TEST FOR METHYL KETONES

I. Introduction :

The iodoform test or reaction is a reaction where iodoform (CHI3) is produced by the
multiple halogenation of a methyl ketone ( a molecule containing the R- CO CH3 group ) in
the presence of a base. It is a chemical test used for the detection of ketones and aldehydes
carrying a methyl group. The reagents are iodine and sodium hydroxide.

Iodine solution is added to a small amount of aldehyde or ketone, followed by just

enough sodium hydroxide solution to remove the color of the iodine.

A positive result is the appearance of a very pale yellow precipitate of triiodomethane

(previously known as iodoform) CHI3. It is given by an aldehyde or ketone containing the
grouping:

O
CH3 C
R
R can be a hydrogen or a hydrocarbon group (for example, an alkyl group).

If R is a hydrogen, then you have an aldehyde ethanal, CH3CHO.

Ethanal is the only aldehyde to give the triiodomethane (iodoform ) reaction.

If R is a hydrocarbon group, then you have a ketone. Those ketones that do have a
methyl group on one side of the carbon-oxygen double bond will give this reaction.

48
II. Objective:

Identify the presence of a CH3CO group in aldehydes and ketones using the iodoform
reaction.

III. Materials :

acetaldehyde acetic acid iodine solution

benzaldehyde butanone 5 test tubes
acetone 0.1N NaOH solution droppers

IV. Procedure :

1. Put 1 ml of acetaldehyde into the first test tube, 1 ml of benzaldehyde into the second
test tube, 1 ml of acetone into the third, 1 ml of butanone into the fourth and 1 ml of acetic
acid into the fifth.

2. Add 3 4 drops of iodine solution into each of the test tubes.

3. Add 0.1N NaOH solution drop wise into each of the test tubes until the light yellow
precipitate appears.

4. Record your observations on the report sheet.

49
V. Report Sheet :

Compound Observations

acetaldehyde

benzaldehyde

acetone

butanone

acetic acid

Question:

Which of the following compounds give positive result and why?

____________________________________________________________________________

____________________________________________________________________________

50
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Experiment No. 5
Name : _____________________________________

Class : _________________ ID No. ______________

Experiment No. 11
OXIDATION OF CARBONYL COMPOUNDS USING ACIDIFIED POTASSIUM (VI)
DICHROMATE

I. Introduction :

The carbonyl group is common to both aldehydes and ketones. In aldehydes, the
carbonyl group always has a hydrogen bonded to it. Because the aldehyde group must include
at least one hydrogen atom with the carbonyl, the aldehyde function will always appear at the
end of a carbon chain.

(the aldehyde functional group)

The aldehyde functional group can be condensed to CHO, and the general formula for an
aldehyde can be written as R-CHO. Note that the H comes before the O in the aldehyde
formula , but after the O in alcohols.

In ketones, the carbonyl group is always bonded to two other carbon atoms, never directly to a
hydrogen atom.

(the ketone functional group)

The ketone functional group can be condensed to RCOR, in which R is either an alkyl or aryl
(aromatic) group.

51
II. Objective :
Compare the oxidation of aldehyde and ketone using acidified potassium dichromate
(VI).

III. Materials :

ethanal (acetaldehyde) 2 test tubes

propanone (acetone) test tube rack (small)

acidified potassium dichromate (VI) solution plastic droppers

IV. Procedure :

1. Put 1 ml of acidified potassium dichromate (VI) solution into each of the two test tubes.

2. Then add 5 drops of acetaldehyde into the first tube and 5 drops of acetone into the second
tube.

3. Observe which of the two compounds will react with acidified K2Cr2O7.Then write down your
observations on the report sheet.

V. Report Sheet :

Positive Reaction or
Negative Reaction with
Compound Tested Acidified Potassium Observations
Dichromate (VI)

Acetaldehyde

Acetone

52
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _________________ ID No. ______________

Experiment No. 12
OXIDATION OF CARBONYL COMPOUNDS BY FEHLINGS SOLUTION

I. Introduction :

Sugar is a sweet-tasting soluble naturally occurring carbonyl compound. Sugars such as

glucose show many properties that are typical of carbonyl compounds.

Fehlings test has been used to detect sugar in the urine of people suffering from
diabetes. The pancreas of these patients produces insufficient insulin to cope with the sugar in
their diet. This means that the sugar accumulates in the blood and, when it reaches a certain
concentration, it is excreted by the kidney, and appears in the urine. Depending on the
concentration of glucose, the solution may simply turn green, produce a fine yellow precipitate
or give a dark red precipitate.

II. Objective :

Show the oxidation of a carbonyl compound using Fehlings solution.

III. Materials :

Fehlings solution 2 test tubes

glucose test tube rack (small)
spatula hot plate
water beaker, 250 ml

53
IV. Procedure :

1. Put 2 ml of distilled water in one of the test tubes. Then dissolve one spatula of
glucose. Keep it aside in the test tube rack.
2. In another tube, prepare Fehlings solution by mixing together 3 ml of Fehling A with 3
ml of Fehling B.
3. Then add the Fehlings solution into the glucose-water mixture.
5. Boil the mixture gently. Write down your observation in the Report Sheet.

V. Report Sheet :

Describe and explain what happens when Fehlings solution is added to glucose-water mixture.
__________________________________________________________________________
__________________________________________________________________________

54
 Batterjee Medical College for Science and Technology
Department of Chemistry Chemistry Practical

Name : _____________________________________

Class : _______________ ID No. ________________

\

Experiment No.13
FEHLINGS TEST FOR CARBOHYDRATES

I. Introduction :

A carbohydrate is an organic compound that consists only of carbon, hydrogen, and

oxygen.

The term is most common in Biochemistry, where it is a synonym of saccharide. The

carbohydrates (saccharides) are divided into three chemical groupings.

1. Monosaccharide

2. Disaccharide

3. Polysaccharide

Monosaccharide - general formula (CH2O)n

If the carbonyl group is an aldehyde, the monosaccharide is an aldose; if the carbonyl

group is a ketone, the monosaccharide is a ketose.

Examples : glucose, fructose and glyceraldehydes

Disaccharide - two joined monosaccharide and these are the simplest polysaccharides

Disaccharides can be classified into two types.

1) reducing disaccharides or biose - if the functional group is present in bonding with

another sugar unit (open-structure)

2) Non-reducing disaccharides - if the functional group is cannot bond with another sugar
unit (closed-structure)

Examples include sucrose and lactose.

55
Polysaccharides are long carbohydrate molecules of repeated monomer units. General
formula of Cx(H2O)y

Types of Polysaccharide:

1. homopolysaccharide or homoglycan - when all the monosaccharides in a polysaccharide

are the same type

2. heteropolysaccharides or heteroglycans - when more than one type of monosaccharide

Examples : starch and glycogen

II. Objective :

Determine the carbohydrate by using Fehlings Test.

III. Materials:

Fehling A solution Fehling B solution

Sucrose test tubes (3)

Fructose test tube rack

Glucose Pasteurs pipette

Hot plate beaker

IV. Procedure :

1. Mix 1 ml of Fehlings solution A with 1 ml of Fehlings solution B in each of the three test
tubes.

2. Then add 1 ml of compound A into the first tube, and 1 ml of compound B into the
second tube, and 1 ml of compound C into the third tube.

3. Make sure of the tubes with compounds A, B and C, before placing them in the water
bath.

4. Heat the mixture for 3 5 minutes in a water bath and take note of any changes in
color or formation of precipitate.

56
V. Report Sheet :

Fehlings Test used to determine the carbohydrate. A positive result will show a
brick-red precipitate.

Carbohydrate Positive / Negative

Glucose

Sucrose

Fructose

Question:

What sugar/s gave a positive result with Fehlings Test ? Why?

_____________________________________________________________

_______________________________________________________________________

57