Experiment 1

HEAT EFFECTS AND CALORIMETRY1

Heat is a form of energy, sometimes called thermal energy, that can pass spontaneously from an object at a high
temperature to an object at a lower temperature. If the two objects are in contact, the hotter object cools down and
the colder object warms up. Given sufficient time, both objects reach the same temperature which is between the two
starting temperatures.
Heat flow is ordinarily measured in a calorimeter. A calorimeter is simply a container with insulating walls, so
that no heat is exchanged between the contents of the calorimeter and the surroundings. Heat flow to and from
anything contained in the calorimeter is confined within the calorimeter, so that

qtot = 0

However the calorimeter itself, and whatever is placed in it exchanges heat so that

qtot = 0 = qcalorimeter + q1 + q2 + …

where q1, q2, … are the heat absorbed or evolved by the items in the calorimeter. The heat flow is calculated from
temperature changes and the object’s specific heat or heat capacity. In this experiment, you will observe the heat
changes (1) when a hot metal is placed in water, (2) when a solute is dissolved in water, and (3) when a reaction takes
place in aqueous solution. To simplify the experiment, we will assume that the calorimeter itself will not absorb or lose
heat, qcalorimeter = 0, leaving us with the following equations for the three heat changes:

(1) qmetal + qwater = 0

qmetal = -qwater
mmetal × cmetal × (tf, metal – ti, metal) = -[mwater × cwater × (tf, water – ti, water)]
(2) qsolution + qwater = 0
qsolution = -qwater
qsolution = -[mwater × cwater × (tf, water – ti, water)]
(3) qreaction + qwater = 0
qreaction = -qwater
qreaction = -[mwater × cwater × (tf, water – ti, water)]

In the first part, you will calculate the specific heat, c, of an unindentified metal. The specific heat of an elemental metal
is related to its molar mass by the Dulong and Petit Law:

25
𝑀𝑀 =
𝐽
𝑐( ° )
𝑔𝐶

where MM is the molar mass of the metal. The Dulong and Petit law shows that about 25 joules is required to raise the
temperature of one mole of many metal by 1°C. Once the specific heat of the metal is known, the approximate molar
mass can be calculated. The specific heat of water is 4.18 J/g°C.

1
From Slowinski, E.J., Wolsey, W.C. and Rossi, R.C. 2014. Chemistry Laboratory Manual for Science Majors, Philippine edition.
Cengage Learning.
 In the second part, you will calculate the molar heat change or enthalpy of the dissolution of a salt in water.
Because the solution process involves replacing solute-solute and solvent-solvent interactions with solute-solvent
interactions, energy change usually accompany the process as the nature of interactions and distances between
attracting bodies are changed.
Finally, in the last part of the experiment, you will measure the molar enthalpy of reaction between an acid and
a base. Chemical reactions involve the breaking and formation of bonds, processes that respectively absorb and evolve
energy. When the bonds formed are generally stronger than the bonds that were broken, there will be a net evolution
of heat and the reaction will be exothermic. This is manifested by a rise in the temperature of the surroundings. When
the bonds broken are stronger than the bonds formed, there will be a net absorption of heat and the reaction is
endothermic. The temperature of the surroundings drop when endothermic reactions occur. Because the reactions are
happening between molecules and ions, the immediate surroundings in aqueous reactions is the water medium in
which the substances are dissolved.

Procedure:
A. Specific Heat
Obtain a calorimeter, a sensitive thermometer, and a sample of metal in a large stoppered tube. The calorimeter
consists of two nested polystyrene foam cups with a foam cover. There are two holes in the cover: one for a
thermometer and the other for a stirring rod.
Fill a 400-ml beaker two thirds full of water and begin heating it to boiling. While the water is heating, weigh
your sample of unknown metal in the stoppered tube. Remove the metal from the tube, and weigh the empty tube
and stopper. Return the metal in the tube, and with the stopper loosely covering the tube, put the tube in the hot
water in the beaker. The metal should be below the surface of the water level in the beaker. Continue heating the
metal in the boiling water for at least 10 minutes.
While the water in the beaker is boiling, weigh the calorimeter. Place 40 mL of water in the calorimeter and
weigh it again. Insert the stirrer and thermometer into the cover and put it on the calorimeter. Make sure that the
bulb of the thermometer is completely immersed in the water. Read the initial temperature of the water in the
calorimeter. Take the tube out of the boiling water and quickly dry the test tube. Open the tube and drop the metal
into the water in the calorimeter. Cover and stir the water in the calorimeter. Take care that no water from the
calorimeter splashes out of the calorimeter. Record the maximum temperature reached by the water. Repeat the
experiment using 50 mL of water. Be sure to dry the metal before reusing it.

B. Heat of Solution
Place about 50 mL of distilled water in the calorimeter and weigh as the previous procedure. Measure the
temperature of the water. In a small beaker weigh out about 5 g of the salt assigned to you. Add the compound to
the calorimeter. Stir continuously and occasionally swirl the calorimeter. Determine the maximum or minimum
temperature reached as the solid dissolves. Check to make sure that all the solid is dissolved.

C. Heat of Reaction
Rinse out your calorimeter with distilled water, pouring the rinse into the sink. In a graduated cylinder, measure
out 25 mL of 2.00 M HCl; pour this into the calorimeter. Rinse out the cylinder with distilled water and measure
out 25 mL of 2.00 M NaOH. Measure the temperature of the acid and of the base, making sure to rinse and dry
the thermometer before dipping it into the solutions. Put the thermometer back into the calorimeter cover.
Pour the NaOH solution into the HCl solution and cover the calorimeter. Stir the reaction mixture, and record
the maximum temperature that is reached by the neutralized solution.
Calculate the enthalpy of neutralization. Since the masses of the solutions were not determined, use a
value of 1.02 g/mL average density for both solutions in this experiment to calculate the mass of the solutions.
Use 4.18 J/g°C for the specific heat of the solutions.
Group No. _______________ Names: ___________________________
Section: ________________ ___________________________
___________________________

DATA SHEET
Heat Effects and Calorimetry

A. Specific Heat
Mass of stoppered test tube plus metal
Mass of test tube and stopper
Mass of calorimeter
Mass of calorimeter and water
Mass of water
Mass of metal
Initial temperature of water in calorimeter
Initial temperature of metal
Equilibrium temperature of metal and water in
calorimeter
twater
metal
qwater
Specific heat of the metal
Approximate molar mass of metal
B. Heat of Solution
Mass of calorimeter plus water
Mass of beaker
Mass of beaker plus solid
Mass of water
Mass of solid
Initial temperature
Final temperature
qwater for the dissolution
H for the dissolution
H for the dissolution /g salt
H for the dissolution /mol salt
C. Heat of reaction
Initial temperature of HCl solution
Initial temperature of NaOH solution
Final temperature of the neutralized mixture
t
qwater
H for the reaction
H for the reaction/per mole of H+ and OH-
reacting
 Experiment 2

COMBUSTION AND AIR QUALITY

OBJECTIVE: By the end of the activity, the student will be able to

1. Understand the nature of combustion

2. Appreciate desirable combustion characteristics of fuels

MATERIALS: matches, small candle, Bunsen burner (optional), alcohol burner, hexane, toluene, naphthalene
balls, blue and red litmus paper

PROCEDURE:

1. Light a match and place a moist blue litmus paper over the flame (hold the litmus paper with tongs).
Maintain enough distance between the flame and the paper so that it does not burn. The idea is to allow
the gaseous products of combustion to react with the moisture and the litmus dye. Note the color of the
litmus paper. Repeat the procedure using red litmus paper. Do the same with the other flame sources
(candle, Bunsen burner, alcohol burner). Write your observations.
2. CAUTION: The following must be done inside a fume hood. Place about 5 mL of hexane in an evaporating
dish and carefully ignite it with a lighted match or better yet an. Observe the color and general
appearance of the flame. Hold a second evaporating dish with tongs over the flame, allowing the flame
to come in contact with the bottom. Observe soot formation (if any). Do the same, separately, for
toluene and naphthalene. Compare with the flame of the alcohol lamp. Hold an evaporating dish over
the alcohol lamp flame. Note your observations.
Group No. _______________ Names: ___________________________
Section: ________________ ___________________________
___________________________

DATA SHEET
Combustion and Air Quality

Draw the Lewis molecular structures of the combustible materials tested, and the products of their complete
combustion, water and carbon dioxide.

Hexane Toluene

Naphthalene Ethanol

Water Carbon dioxide

Based on your observations, what generalization can you make about the products of combustion?

Write the balanced chemical equations for the complete combustion of the four combustible substances.

1.

2.

3.

4.

Look up the values for the heat of formation of the combustible materials tested and water and CO2. Also, find
the bond dissociation energies of the bonds in the combustion reactants and products.

Hf° Hexane _______________________ Bond dissociation energy C-C _________________

Hf° Toluene _______________________ Bond dissociation energy C=C _________________

Hf° Naphthalene _____________________ Bond dissociation energy C-H _________________

Hf° Ethanol _______________________ Bond dissociation energy O=O _________________

Hf° Carbon dioxide ___________________ Bond dissociation energy C=O _________________

Hf° water _______________________ Bond dissociation energy O-H _________________

Cite the sources of your thermochemical data:

1.
2.
3.
4.
Calculate the heats of reaction for the complete combustion of the four substances by Hess’s Law using (a)
heats of formation and (b) bond dissociation energies. Look up the heats of combustion of the four substances
and fill in the table below.

Heat of reaction
Heat of reaction
calculated from
Heat of combustion calculated from heat
Fuel Flame appearance bond dissociation
H in kJ/mol of formations
energies
H in kJ/mol
H in kJ/mol
Hexane

Toluene

Naphthalene

Ethanol

Comment on the discrepancy or agreement of the calculated heats of reaction with tabulated heats of
combustion.

From the structures of the four substances used in this experiment and your observations, what possible
correlations of combustion properties with molecular structure exist?
 Experiment 3

SMOKING, HEALTH and POLLUTION

Reading assignment:
Onor, I. O., Stirling, D. L., Williams, S. R., Bediako, D., Borghol, A., Harris, M. B., Darensburg, T. B., Clay, S. D., Okpechi,
S. C., … Sarpong, D. F. (2017). Clinical Effects of Cigarette Smoking: Epidemiologic Impact and Review of
Pharmacotherapy Options. International journal of environmental research and public health, 14(10), 1147.
doi:10.3390/ijerph14101147

West R. (2017). Tobacco smoking: Health impact, prevalence, correlates and interventions. Psychology & health, 32(8),
1018-1036.

Saha, S. P., Bhalla, D. K., Whayne, T. F., & Gairola, C. (2007). Cigarette smoke and adverse health effects: An overview
of research trends and future needs. The International journal of angiology : official publication of the International College
of Angiology, Inc, 16(3), 77-83.

The health issues associated with cigarette smoking has long established smoking as a strong risk factor for
many cardiovascular and respiratory diseases. The identification of the specific causative chemicals found in cigarette
smoke could allow better safety measures that would limit exposure to the more noxious compounds. In this
experiment you are assigned to find out the experimental processes that would identify the chemical components of
cigarette smoke. This will involve trapping smoke and extracting chemical constituents of smoke, isolation of the
different compounds, and then finally identification of the components. The isolation and identification usually involve
instrumental methods and is assigned to the students for submission at the end of the term. However, for the
experiment during the lab period, the students will perform the extraction of the smoke into a liquid solution using a
procedure that they will adopt from literature. Class time can be spent in selecting the best method to employ from the
students’ findings or alternatively, the different groups can perform their experiments and the class can compare results
to determine which method gives the best outcomes.

OBJECTIVES: In this activity, the students

1. Will look up procedures that will determine the chemicals that are present in cigarette smoke
2. Will perform their procedure up to the extraction part converting the smoke into a liquid mixture, using
materials that they will bring on their own and chemicals that they have verified are available in the laboratory
3. Will submit the methodology for the separation and identification part are to be submitted as a research paper
at the end of the term.
 Experiment 4

DETERMINATION OF DISSOLVED OXYGEN IN A WATER SAMPLE

(WINKLER METHOD)

Chemicals: 1. Manganese(II) sulfate solution (MnSO4) ; (4 cm3)

[prepared by dissolving 48 g of MnSO44H2O in water to give 100 cm3 solution]
2. Alkaline potassium iodide solution; (4 cm3)
[prepared by dissolving 15 g of KI in about 25 cm3 of water, adding 66 cm3 of 50% NaOH, and diluting to
100 cm3]
3. Concentrated sulfuric(VI) acid; (4 cm3)
4. 0.0125 M sodium thiosulfate solution; (100 cm3)
5. Freshly prepared starch solution.

Introduction:
The amount of dissolved oxygen is an indicator of the cleanliness of water. A high level of dissolved oxygen in a water
sample shows that the water is clean and unpolluted. In this experiment, Winkler method is used to determine the
amount of dissolved oxygen in water.
In an alkaline solution, dissolved oxygen will oxidize manganese(II) to the trivalent state.

8OH-(aq) + 4Mn2+(aq) + O2(aq) + 2H2O(l)  4Mn(OH)3(s)

The analysis is completed by titrating the iodine produced from potassium iodide by manganese(III) hydroxide.
2Mn(OH)3(s) + 2I-(aq) + 6H+(aq)  2Mn2+(aq) + I2(aq) + 6H2O(l)
Sodium thiosulphate is used as the titrant.

2S2O32-(aq) + I2  S4O62-(aq) + 2I-(aq)

Success of the method is critically dependent upon the manner in which the sample is manipulated. At all stages, every
method must be made to assure that oxygen is neither introduced to nor lost from the sample. Furthermore, the sample
must be free of any solutes that will oxidize iodide or reduce iodine.
Procedure
1. Use a 250 cm3 volumetric flask to collect a water sample. Fill the flask completely with water without trapping
any air bubbles.
2. Add 1.0 cm3 of manganese(II) sulphate solution to the sample using a pipette. Discharge the solution well below
the surface (some overflow will occur).
3. Similarly introduce 1.0 cm3 of alkaline potassium iodide solution. Be sure that no air becomes entrapped. Invert
the bottle to distribute the precipitate uniformly. [Hazard Warning: Care should be taken to avoid exposure to
any overflow, as the solution is quite alkaline.]
4. When the precipitate has settled at least 3 cm below the stopper, introduce 1 cm3 of concentrated sulphuric(VI)
acid well below the surface. Replace the stopper and carefully mix until the precipitate disappears. A magnetic
stirrer is helpful here.
5. Allow the mixture to stand for 5 minutes and then withdraw 100 cm3 of the acidified sample into a 250 cm3
conical flask.
6. Titrate with 0.0125 M sodium thiosulphate until the iodine colour becomes faint. Then add 1 cm3 of starch
solution, and continue adding the thiosulphate solution until the blue colour disappears.
7. Record the volume of thiosulphate solution used and calculate the dissolved oxygen content in the sample in mg
dm-3.
 Experiment 6

A SILLY POLYMER

In the course of performing this experiment the student will

• learn to cross-link a polymer and observe the changes in physical properties as a result of this cross-
linking
• observe the changes in a cross-linked polymer at varying temperatures
• learn concepts of molecular motion and intermolecular bond strength

Principles:

If a substance springs back to its original shape after being twisted, pulled or compressed, it is most likely a
polymer called an elastomer. The elastomer has elastic properties (i.e., it will recover its original size and shape after
being deformed).

Examples of elastomers are rubber bands and car tires.

The liquid latex (Elmer’s glue) which you will use in this experiment is a solution consisting of the polymer
named polyvinyl acetate (PVA). The silly putty is formed by joining the globules of PVA using sodium borate (a cross-
linker). This cross-linking causes the mixture to undergo an irreversible gelation reaction. The silly putty is held together
by weak intermolecular bonds that provide flexibility and rotation about the chain of the cross-linked polymer.

Materials:

(L): 55% Elmer’s glue solution in water, 4% borax solution, food colors

(S): Styrofoam cups, plastic bags

Safety Precautions:

• Borax (as solid or solution) can burn your eyes; it is absolutely necessary to wear safety goggles and lab
aprons at all times.
• Wash hands thoroughly after handling the silly putty.

Procedure:

1. Pour 20 mL of Elmer’s glue emulsion into a Styrofoam cup and add enough food color to your preferred shade
(optional).
2. Add 8.5 mL of the cross-linker (borax solution) to the glue emulsion.
3. Immediately begin stirring the mixture together using a wooden stick.
4. When the mixture starts to come off the sides of the cup, the silly putty may be taken out and kneaded in the
hands. Continue to knead to a desired consistency then shape into a ball.
5. Drop the ball from a height of 30 centimeter. Measure (using a ruler) the height to which the ball rebounds.
 6. Stretch the silly putty slowly from each side.
7. Compress the silly putty back into a ball.
8. Pull the silly putty quickly from each side and compare the results.
9. Place the silly putty on regular newsprint paper and press down firmly.
10. Remove the silly putty from the newsprint and make observations.
11. Place the silly putty in a bag and keep in the refrigerator for 10 minutes.
12. Repeat step 5 and compare results.
13. Return the putty to the Styrofoam cup and and add more borax solution incrementally. Mix and observe changes
on the putty.

Questions:

1. How do the physical properties of the glue-water mixture change as a result of adding sodium borate?
2. What would be the effect of increasing the concentration of sodium borate in the mixture?
3. In this experiment, how did you measure the elasticity of the polymer you prepared?
 Experiment 7

SURFACTANTS and WATER HARDNESS

OBJECTIVE: In this experiment, you will explore the behavior of surfactants and the effects of certain ions on it.
Observations made will allow you to devise a procedure and perform tests to answer the following questions:

1. What properties of water are affected by surfactants like soap or detergent?

2. What is the effect of surfactants on a mixture of oil and water?
3. How does soap differentiate between hard water and soft water?
4. Is our tap water at home hard or soft?
5. Which ions cause water hardness?

MATERIALS: 400 ppm hard water, MgCl2, NaCl, Na2SO4, CaSO4, Na2CO3, test tubes, stoppers, beakers, distilled water,
piece of cardboard, (bath soap, shampoo, detergent, and water samples to be brought by students from their homes)

PROCEDURE:

1. Mix some soap with distilled water in a small beaker. Put some water in a second beaker. Simultaneously dip a
finger of one hand into the soapy water, and a finger of your other hand into the water. Transfer about the same
amount of the liquids by touching both fingers on a piece of cardboard. Ensure that the two liquids DO NOT
touch or mix on the cardboard. Observe the behavior of the two liquids on the cardboard. Repeat if necessary,
but always transfer the liquids onto dry spots on the cardboard. Do the comparison again but this time touch a
nonabsorbent surface like the laboratory bench (tile or resin).
2. Half fill two 50 mL beakers with distilled water, then add enough oil to cover the surface of the water. Without
stirring, add soapy water dropwise at the center of the oil layer in one beaker. Add water with liquid detergent
to the other beaker. Record your observations. Repeat the procedure using hard water in the place of distilled
water.
3. Add 5 mL of distilled water and 10 drops of oil to each of 2 test tubes. Shake one test tube vigorously and
observe. Stand the test tube and note what happens as the liquid settles. Now add 2 mL soapy water to one
tube and 2 mL water with detergent to the other. Shake each tube again and observe what happens when the
mixture settles. Repeat the procedure using hard water instead of distilled water.
4. Using your observations on the effect of hard water on the surfactants, determine whether your water sample
from home is hard or soft.
5. Prepare 5 test tubes by adding 5 mL of distilled water and a small amount of bar soap. To one test tube add a
pinch of MgCl2; to another, NaCl; to a third, Na2SO4; to a fourth, CaSO4, and to the last, Na2CO3. Shake vigorously
and observe.