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001 Lab Manual-Winter 2024
001 Lab Manual-Winter 2024
1. Do not enter the laboratory unless the instructor is present. Inform the instructor if you have to leave the lab area.
2. Safety glasses and buttoned lab coats must be worn at all times while in the laboratory. Long pants and closed stable shoes are
recommended. Long hair must be tied back, and loose or hanging jewellery must be removed before experiments are carried out.
3. Eating and drinking is forbidden in the laboratory. Do not taste, touch or smell chemicals.
5. Coats and backpacks must be kept away from the working area, and from the floor space between the benches.
7. Know the location of fire extinguishers, fire blanket, safety shower, eyewash fountain and first aid kit in the laboratory.
8. Read the labels of chemicals very carefully. Be careful in handling and mixing chemicals. You should be familiar with the system
of codes used to indicate safety hazards.
9. All accidents, regardless of how minor they may seem, must be reported immediately to your instructor.
10. If a chemical spills onto your skin or clothing, wash it off immediately with plenty of cold water and notify your instructor.
11. If a chemical gets into your eyes or on your face, wash immediately in the eyewash fountain with plenty of water. Notify your
instructor.
12. If a chemical spills onto the bench or the floor, notify the instructor immediately and take appropriate action to clean it up.
13. Make sure that apparatus is stable and securely fastened. Never leave an “experiment in progress” unattended. Turn off all
equipment when it is not in use.
14. Never aim the opening of test tubes or flasks at yourself or anyone else.
15. Use fume hoods, as instructed, whenever toxic or irritating fumes may be evolved.
16. Never place flammable material near an open flame or hot plate.
17. Never use mouth suction for filling pipettes. Use a suction bulb.
18. When diluting acid with water, always add the acid to the water.
19. Do not force glass tubing or thermometers into rubber stoppers. Use water or grease to lubricate the tubing and keep your hands
close together during insertion.
21. The disposal of chemicals must be carried out in accordance with instructions given in the lab manual or by the instructor.
22. At the end of the experiment, wipe your bench space clean with damp paper towel.
24. The removal of chemicals or equipment from the laboratory is strictly forbidden.
I have read the above safety regulations and agree to abide by them during all laboratory sessions for this course.
i
TABLE OF CONTENTS
Page
EXPERIMENTS
GRAPH PAPER
COURSE OBJECTIVES
Revised W22
v
SAFETY REGULATIONS
1. Do not enter the laboratory unless the instructor is present. Inform the instructor if you have to leave the lab area.
2. Safety glasses and buttoned lab coats must be worn at all times while in the laboratory. Long pants and closed
stable shoes are recommended. Long hair must be tied back, and loose or hanging jewellery must be removed before
experiments are carried out.
3. Eating and drinking is forbidden in the laboratory. Do not taste, touch or smell chemicals.
5. Coats and backpacks must be kept away from the working area, and from the floor space between the benches.
7. Know the location of fire extinguishers, fire blanket, safety shower, eyewash fountain and first aid kit in the
laboratory.
8. Read the labels of chemicals very carefully. Be careful in handling and mixing chemicals. You should be familiar
with the system of codes used to indicate safety hazards.
9. All accidents, regardless of how minor they may seem, must be reported immediately to your instructor.
10. If a chemical spills onto your skin or clothing, wash it off immediately with plenty of cold water and notify the
instructor.
11. If a chemical gets into your eyes or on your face, wash immediately in the eyewash fountain with plenty of water.
Notify your instructor.
12. If a chemical spills onto the bench or the floor, notify the instructor immediately and take appropriate action to clean it
up.
13. Make sure that apparatus is stable and securely fastened. Never leave an “experiment in progress” unattended. Turn
off all equipment when it is not in use.
14. Never aim the opening of test tubes or flasks at yourself or anyone else.
15. Use fume hoods, as instructed, whenever toxic or irritating fumes may be evolved.
16. Never place flammable material near an open flame or hot plate.
17. Never use mouth suction for filling pipettes. Use a suction bulb.
18. When diluting acid with water, always add the acid to the water.
19. Do not force glass tubing or thermometers into rubber stoppers. Use water or grease to lubricate the tubing and keep
your hands close together during insertion.
21. The disposal of chemicals must be carried out in accordance with instructions given in the lab manual or by the
instructor.
22. At the end of the experiment, wipe your bench space clean with damp paper towel.
24. The removal of chemicals or equipment from the laboratory is strictly forbidden.
vi
vii
viii
CHEMISTRY 001 INFORMATION SHEET H11
The following data have been taken from the CRC Handbook. Some of the values may be different from those in the textbook.
For atomic masses, use the Periodic Table.
General Information:
ix
Dissociation Constants (at 25oC):
x
LABORATORY NOTES
I. LAB REPORTS
(The following procedures may be modified. Please consult with your instructor.)
Data must be recorded in ink, with no erasures. Show a sample of each calculation done in the
lab. Express your results to the maximum precision possible. Add a discussion to your lab report:
this will be a brief summary of what the lab accomplished and how this was done; also, comment
on the relative accuracy of your results. State which instrument(s) limited the accuracy of your
measurements, and describe the specific problems that you encountered in the lab that may have
led to errors. If possible, make a comparison between your results and the results obtained by
other students or those values given in the chemical literature (for example, handbooks or texts).
The instruments used in a chemical laboratory are graduated by lines corresponding to units or
parts of units. To read an instrument, line up the variable marker (the needle or the bottom of the
meniscus, for example) with the eye and the scale to avoid parallax error:
Mentally subdivide the small space between the graduation lines to obtain a reading that is one
decimal place more precise than the graduations. When you record this reading, the last digit (that
you estimated) is the first digit of which you are unsure (the “last significant figure”). Most
instrument scales are designed so that a reading made this way indicates the probable precision of
the measurement: the last significant figure is the first digit that is uncertain.
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III. PRECISION OF GLASSWARE
Graduated beakers are used to measure volumes roughly; they are containers with a precision of
±5%.
Graduated cylinders are used to measure volumes approximately; they are usually calibrated to
contain volumes with the following precisions:
10 mL: ± 0.1 mL 25 mL: ± 0.1 mL
50 mL: ± 0.2 mL 100 mL: ± 0.2 mL
Pipettes and burettes are used to determine volumes accurately; they are calibrated to deliver
certain volumes and have a precision of:
1 mL pipette: ± 0.01 mL
5 mL pipette: ± 0.01 mL
10 mL pipette: ± 0.02 mL 50 mL burette : ± 0.02 mL
20 mL pipette: ± 0.03 mL
25 mL pipette: ± 0.03 mL
A volumetric flask contains an accurately known volume of solution at a given temperature (often
20oC); it has a precision of :
100 mL volumetric flask: ± 0.2 mL
250 mL volumetric flask: ± 0.1 mL
xii
3. Transfer the cool solution quantitatively to the volumetric flask in the following way: use
a funnel for the main bulk of the solution; wash out the beaker and transfer the washing to
the flask. Using a squeeze bottle, wash the neck of the flask, the stirring rod and funnel,
allowing the water to go into the flask. This ensures the quantitative transfer of all solute
to the flask.
4. Fill up the flask to just below the mark. Stopper it and invert it quickly a few times.
Remove the stopper, wait 30 seconds, and add water, drop wise, to bring the bottom of the
meniscus to the mark. Invert again.
5. Transfer a portion of the solution to a clean beaker in order to use it. To make sure that the
concentration is not changed by this procedure, rinse the clean beaker twice with small
quantities (3 mL portions) of the solution.
B. Pipette
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8. Remove the hanging drop by touching a glass surface gently.
9. Allow the contents to run into the reaction vessel. Hold the pipette vertical for 15 seconds
after emptying.
10. Complete the deliver by touching the pipette tip to the liquid surface.
11. A small amount of liquid remains in the pipette and should not be blown or shaken out.
The pipette is calibrated to deliver the printed volume while retaining the last little bit.
12. Wipe the outside of the pipette dry before pipetting the next sample.
13. Clean the pipette after use.
C. Burette
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D. Titration Technique
The solution to be titrated should be pipette into a beaker, or preferably, an Erlenmeyer (conical)
flask. The latter reduces the risk of loss by splashing. If any solution does splash on the sides,
wash it back into the solution with a wash bottle, since this does not change the amount of
reagents present in the flask. When titrating, operate the stopcock with the left hand while the
right hand is free for swirling the flask.
The first titration is often “rough” in that the “end-point” may be passed. The “end-point” is the first
permanent color change of the indicator. The first rough titration is used as a guide to the approximate
volume required. During the second and third titrations, the solution can be urn in rapidly from the
burette to within 1 mL of this approximate value. Thereafter, add the solution drop wise. Touch the flask
gently to the tip of the burette to remove a hanging drop, and wash it into the solution. The last two
titrations should be within 0.10 mL of each other.
xv
EXPERIMENT 1
Objective
- To understand density in terms of mass and volume, and to see this relationship graphically.
Introduction
The density (d) of a substance is defined as the ratio of the mass of an object (m) to the volume it occupies
(V)
d=m/V
Density is a property of a substance which does not depend on the quantity of substance being examined.
This can be seen graphically, by drawing a graph of mass vs volume for several different masses and
volumes of a substance.
The mass of a substance can be determined by weighing it on a balance. The volume of a liquid can be
measured with a graduated cylinder, while the volume of a solid object can be determined by measuring
the volume of the liquid that is displaced when the object is placed in the liquid in a graduated cylinder.
To determine the density of a liquid, the mass of several different portions of the liquid can be plotted
against the volume occupied by those portions. Likewise, the density of a solid can be determined by
plotting the mass of several pieces of the solid against the volume that those pieces occupy.
The slope of the graph has the units of g/mL or g/cm3, and is equal to the density of the substance being
studied. If the density of a substance is constant, the slope remains constant as the mass or volume is
changed.
16
In this experiment, the slopes of different graphs of mass vs volume will be used to determine first, the
density of water, second, the density of an unknown liquid and third the density of a solid. If the density
of each substance is constant, then a straight line will fit the data points for each different substance
reasonably well.
Procedure
Weigh a 50 mL graduated cylinder that is dry and empty (Mass 1). Volume 1 is zero since the cylinder
does not contain any water. Add about 10 mL of water with a wash bottle, and record the precise volume
which is the level of water in the graduated cylinder (Volume 2). Weigh the cylinder and water (Mass 2).
Add about 15 mL more water to the graduated cylinder with a wash bottle, and again record the volume
(Volume 3). Weigh the cylinder and water (Mass 3). Add another 15 mL of water with a wash bottle and
record the total volume in the graduated cylinder (Volume 4). Weigh the cylinder and water (Mass 4).
For each of the Masses 1 to 4, determine the mass of water (Mass n – Mass 1), where n is 1 to 4. Using
suitable scales, plot a graph of the mass of water vs the volume of water, with the mass of water on the y-
axis and the volume of water on the x-axis. Draw the best straight line through the data points and
determine the slope of the line, which is equal to the experimental value of the density of water.
Repeat the procedure of Part A using an unknown liquid and determine its density.
17
Part C: Determination of the density of a solid through liquid displacement
Add about 25 mL of water to a 50 mL graduated cylinder. Record Volume 1, the level of water in the
graduated cylinder, and Mass 1, the mass of the cylinder and water. Carefully add a piece of metal to the
graduated cylinder by tipping it and lettering the piece slide in gently. Try not to splash the water as this
is done. Record Volume 2, the level of the liquid and Mass 2, the mass of the graduated cylinder and
contents. Repeat this procedure twice more, each time adding another piece of metal, and recording the
water level (Volume 3, 4) and the mass of the graduated cylinder and its contents (Mass 3, 4).
For each data point, determine the mass of the solid and volume it occupies. Make a graph of solid added
(y-axis) vs volume of solid (x-axis). Draw the best straight line through the points and determine the
density of the solid from the slope of the line.
18
19
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 1: DATA SHEET Partner’s Name: _________________________________
Part A
Data Calculated
Calculate the density of water from the graph showing all calculations.
The slope of a line is equal to the tangent, and is given by the formula:
Choose any two well-separated points on the straight line (excluding the measured data points), and
calculate ∆y and ∆x.
20
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 1: DATA SHEET Partner’s Name: _________________________________
Part B
Data Calculated
Part C
Data Calculated
21
EXPERIMENT 4
Objectives
Introduction
Chemical reactions involve interactions between atoms, molecules or ions to form new substances. The
new substances formed (products) have completely different properties than the reactants which were
mixed together at the start.
There are several different kinds of reactions and they are usually classified according to the types of
substances which are allowed to react. Among the most important are:
1. Combination Reactions
In these reactions, two substances, either elements or compounds, react together to form a single
product.
2. Decomposition Reactions
These reactions occur when a single compound breaks down or decomposes into two or more
different substances.
22
3. Reactions of Acids
Acids are compounds which release hydrogen ions (H+) when they are dissolved in water.
The hydrogen ion is a reactive species and is responsible for giving the acid its characteristic
properties. Two types of acid reactions are:
(a) Reactions of metals with dilute acids: In these reactions, some metals, not all, react
with a dilute acid to form a metal salt and hydrogen as which is given off.
(b) Neutralization reactions: These reactions occur when an acid reacts with a base, for
example, a metal hydroxide, to form a salt and water.
4. Redox Reactions
These reactions involve the oxidation of one of the substances and the reduction of another
substance in order to form the products. Such redox reactions are characterized by changes in
oxidation numbers, that is, by the loss or gain of electrons. Usually an atom in one of the
substances is oxidized and loses electrons as its oxidation number increases, while an atom in the
other substance is reduced and gains electrons as its oxidation number decreases.
Ion combination reactions take place in solution and occur when suitable ions, which have been
separated by dissolving, combine together to form an insoluble precipitate.
-
e.g.: Ag+(aq) + Cl (aq) → AgCl(s)
23
During this lab you will study the following six reactions which are characteristic of the types outlined
above, and then use the knowledge gained to identify an unknown substance.
1. Combination Reactions
2. Decomposition Reactions
Ammonium carbonate can be decomposed by heating into ammonia gas, water and carbon
dioxide.
3. Reactions of Acids
4. Redox Reactions
Hydrogen peroxide solution oxidizes sodium iodide solution to liberate elemental iodine.
24
5. Ion Combination Reactions
Iron(III) chloride solution reacts with sodium hydroxide solution to form a gelatinous brown
precipitate of iron(III) hydroxide. Sodium chloride is left in solution.
Procedure
Part A
1. Combination Reactions
Add about 1 mL of 6.0 mol/L ammonia solution to a clean test tube. To a second test tube add
1 mL of 6.0 mL/mol hydrochloric acid solution. Hold these tubes together so that the open ends
touch each other and watch carefully. Record the results on the data sheet.
2. Decomposition Reactions
In a clean, dry test tube, place a small quantity (enough to just cover the tip of a spatula) of solid
powdered ammonium carbonate. Warm the tube gently on a hot plate and watch what happens.
Carefully wave the gas coming from the tube toward your nose and cautiously smell it. Take
another clean test tube and add about 1 mL of 6.0 mol/L hydrochloric acid to it. Hold the open
end of this tube closely to the open end of the first tube (which contains the ammonium
carbonate). Watch what happens and record all observations.
3. Reactions of Acids
25
(b) Reactions of Acids with Bases (neutralization)
Add about 1 mL of 6.0 mol/L hydrochloric acid to a clean test tube. Add about 1 mL of
6.0 mol/L sodium hydroxide solution and feel the bottom of the test tube with your hands.
Look carefully inside the tube to see if anything is visible.
4. Redox Reactions
Add about 1 mL of 0.1 mol/L sodium iodide solution to a clean test tube. Add 1 mL of hydrogen
peroxide solution and swirl for one minute. Watch what happens and record all observations.
Add about 1 mL of 1.0 mol/L iron(III) chloride solution to a clean test tube. Add several drops of
6.0 mol/L sodium hydroxide solution. Record all observations.
The unknown solution assigned to you will be one of the following substances:
ammonia, hydrochloric acid, sodium hydroxide, hydrogen peroxide or sodium iodide
Using any of the reactions you have carried out in this lab, conduct several tests in order to identify your
unknown. Describe each test you conduct and record all observations.
26
27
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 4: DATA SHEET Partner’s Name: _________________________________
TYPES OF REACTIONS
Part A
1. Combination Reactions
i) Observations:
ii) Explain your observations by writing a word description of the reaction which occurred.
2. Decomposition Reactions
i) Observations:
ii) What happened when the tube containing hydrochloric acid was held near the first test tube?
iii) Explain your observations by writing a word description of the reactions which occurred.
iv) Write the chemical equations for the reactions which occurred.
28
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 4: DATA SHEET Partner’s Name: _________________________________
3. Reactions of Acids
a) Reactions of Acids with Metals
i) Observations:
ii) Explain your observations by writing a word description of the reaction which occurred.
ii) Explain your observations by writing a word description of the reaction which occurred.
29
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 4: DATA SHEET Partner’s Name: _________________________________
4. Redox Reactions
i) Observations:
iii) Explain your observations by writing a word description of the reaction which occurred.
i) Observations:
ii) Explain these observations by writing a word description of the reaction which occurred.
30
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 4: DATA SHEET Partner’s Name: _________________________________
Test 1
i) Describe the test.
iii) Can you identify your unknown by this test? If so, what is it ?
31
EXPERIMENT 5
Objectives:
- to analyze for the presence of certain anions in aqueous solution by means of simple qualitative tests.
Introduction:
In qualitative analysis, the identity of substance present in a mixture is the information to be determined
by the experimenter. Qualitative analysis is based on the fact that no two ions behave identically in all
their chemical reactions. Those reactions which will identify the ions in the fewest possible steps have
been chosen for this experiment.
Procedure:
Clean 6 test tubes and rinse each twice with distilled water (5 mL of distilled water is sufficient to rinse a
test tube). It will be necessary to identify these test tubes, either with labels or by position in the test tube
rack. The order will be: NaCl, NaBr, NaI, Na2SO4, and Na2CO3 as well as one labelled as the unknown.
Obtain an unknown solution and record the number on the data sheet.
Into each of the first 5 test tubes, put a few drops (5 or 6) of the appropriate known solution
(i.e. 0.1 mol/L NaCl in the first tube, 0.1 mol/L NaBr in the second, and so on), and a few drops of the
unknown into the sixth test tube. (Save the remainder of the unknown solution for other tests).
1. Add a few drops of 0.1 mol/L silver nitrate solution to all 6 test tubes. Record your observations (i.e.
formation and colour of precipitate, gas evolution, etc.). If a reaction occurs in a given test tube,
write the overall chemical equation for the reaction.
32
2. Now add about 10-15 drops of 1 mol/L nitric acid to each test tube. Mix the solution thoroughly with
a stirring rod. Record your observations (i.e. dissolution of precipitate, no change, etc.). Again, write
the overall, total ionic, and net ionic equations for any reactions that occur.
Part B: Barium Chloride Test
Wash all 6 test tubes and rinse each tube with distilled water. Put a few drops of the specified known
solutions into each of the 5 test tubes and the unknown into the 6th test tube.
1. Add a few drops of 0.1 mol/L barium chloride solution to all 6 test tubes. Record your observations.
If a reaction occurs, write the overall chemical equation for the reaction.
2. Now add 10-15 drops of 1 mol/L hydrochloric acid to each test tube, mix the solution with a stirring
rod. Record your observations. If a reaction occurs, write the equation for it.
Again wash and rinse all 6 test tubes. Put a few drops of the specified solutions into each of the 6 test
tubes. Add a few drops (1 or 2) of 1 mol/L nitric acid and a few drops (3 or 4) of chlorine aqueous to
each test tube. Now add 5 or 6 drops of hexane and shake vigorously. Because hexane and water are
immiscible, the two liquids form separate layers. Note the colour of the hexane upper layer in each test
tube. Write the overall equation for any reaction which occurs.
33
CHEMISTRY 001 Name: _________________________________
1. Solution Observations
NaCl
NaBr
NaI
Na2SO4
Na2CO3
Unknown
Equations:
34
001: DATA SHEET 5 Name: ________________________________
2. Solution Observations
NaCl
NaBr
NaI
Na2SO4
Na2CO3
Unknown
Equations:
35
001: DATA SHEET 5 Name: ________________________________
Partner's Name: _________________________
1. Solution Observations
NaCl
NaBr
NaI
Na2SO4
Na2CO3
Unknown
Equations:
36
001 DATA SHEET 5 Name: ________________________________
2. Solution Observations
NaCl
NaBr
NaI
Na2SO4
Na2CO3
Unknown
Equations:
37
001: DATA SHEET 5 Name: ________________________________
1. Solution Observations
NaCl
NaBr
NaI
Na2SO4
Na2CO3
Unknown
Equations:
38
39
EXPERIMENT 7
Objectives
- To study the ideal gas law
- To verify the constant value for “R”
Introduction
The modern formulation of the ideal gas law is the result of many experiments carried out by scientists
before the middle of the 19th century. The quantitative studies of gases by Robert Boyle, Jacques Charles,
Amadeo Avogadro and John Dalton lead to the generalization.
In the century that this generalization has been used by scientists, it has been found that many gases
deviate from this “ideal gas equation” under some conditions of temperature and pressure. In this
experiment you will determine the value of the constant “R” for hydrogen near room temperature and at
atmosphere pressure. By comparing your experimental value of “R” with the value of “R” for an “ideal”
gas, you can see if hydrogen deviates from “ideal” behaviour.
Procedure
DISCARD ALL WASTE IN THE WASTE CONTAINER PROVIDED
Weigh a 4 cm strip of magnesium ribbon on the analytical balance. Roll the strip into a loose ball and tie
a length of thread securely around and through it. Fill a 600 mL beaker about two-thirds full of tap water.
Pour 15 mL of a 6 mol/L hydrochloric acid solution into a gas measure tube and carefully fill the rest of
the tube to the very top with distilled water, preventing the acid and water layers from mixing as much as
possible.
40
Submerge the magnesium sample to a depth of five centimetres in the gas measuring tube and insert a
one-holed stopper to hold the thread in place. Make sure that no air is trapped beneath the stopper. With
your thumb covering the hole in the stopper, quickly invert the tube and put the opening under the surface
of the water in the beaker. Remove thumb and clamp the tube in an upright position. The more dense
hydrochloric acid will now fall down around the magnesium sample and hydrogen will be evolved.
Following the completion of reaction, the volume of H2 and its partial pressure are determined in the
following manner. Stopper the gas measuring tube with your thumb and transfer it to the large jar of
water available in the lab, keeping the stoppered end down. In this jar, the gas tube may be moved up or
down so that the level of water in the tube can be matched with the level of the water outside the tube. In
this position, the pressure inside the tube (water vapour plus hydrogen) will be equal to the pressure
outside the tube (the atmospheric pressure in the lab). In this position, carefully read the volume of the
gas in the tube. Record the temperature of the water bath used. Use Dalton’s Law to calculate the partial
pressure of H2.
Vapour pressure of H2O + Partial pressure of H2 = Barometric pressure
41
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 7: DATA SHEET Partner’s Name: _________________________________
TRIAL 1 TRIAL 2
Assuming that an experimental error of ± 5% is not unreasonable, according to your experiment, does
hydrogen behave like an ideal gas at ordinary temperature and pressure? Explain.
42
43
EXPERIMENT 8
Introduction
One of the characteristics of chemical changes is that they are often accompanied by energy changes
which become evident through temperature changes, sound generated, light emitted. What we will be
exploring in this experiment is the change in heat as the reaction proceeds.
When heat is given off by the reaction, the reaction is termed as Exothermic and this is shown by a
negative sign in front of the quantity of heat; if heat is absorbed, the reaction is Endothermic, and this is
indicated by a positive sign in front of the quantity of heat. The quantity of heat exchanged in a chemical
change obviously depends on the amount of substance reacted. To standardize, we therefore calculate the
heat change for one mole of substance.
To determine heat changes for a given reaction, we need to know three things: (i) the mass of the
solution; (ii) the specific heat of the solution; and (iii) the temperature for the reaction. The mass
of the solution can be easily determined on the balance. The specific heat of the solution is more of a
problem, but to simplify our calculations, and to get a very good estimate, we note that the solutions that
we are working with are more than ninety percent water. We can therefore use the specific heat of water
which is 4.184 J/g C. The measurement of the temperature can be approximated by measuring the
temperature of the mixed solution over a period of about 2 minutes. The highest temperature measured
during that period of time will represent the final temperature. The initial temperature will be the room
temperature. The temperature difference, ∆T = final temperature – initial temperature
The quantity of heat released (or taken in) is given by the following expression: quantity of heat =
temperature change x specific heat x mass of solution. This quantity must be converted to determine
how much heat would be evolved (or absorbed) per mole of reactant and is represented by the symbol ∆H.
44
Procedure
Measure out 50.0 mL of 1.00 M HCl in a graduated cylinder and add this to a pre-weighed styrofoam
cup. In a clean and dry graduated cylinder, measure out 30.0 mL of 2.00 M NaOH. Record the
temperature of the HCl and the NaOH. They should be within 0.5 degrees of each other. If they are not,
adjust the temperatures so that they are both at the same temperature.
Then, quickly and carefully, add the NaOH, completely, to the HCl in the Styrofoam cup, stir once with
the thermometer and start to record the temperature every 10 seconds for a period of two minutes.
Once you have finished measuring the temperature, weigh the reaction mixture on a balance and record
the weight. Discard the solution, get another clean, dry styrofoam cup and repeat the experiment, but this
time, use 45.0 mL of 1.00 M HCl and 20.0 mL of 2.00 M NaOH.
Calculate the heat evolved (absorbed) in each trial (make sure that you determine the limiting reagent).
Then covert this to a molar quantity representing the heat, ∆H, and average this value out (make sure that
you use the proper algebraic sign.). Compare this to the value of ∆H, calculated from ∆H°f values listed
below and determine the percent error and comment on possible sources of error.
45
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 8: DATA SHEET Partner’s Name: _________________________________
10 50
90
20
60 100
30
70 110
40
80 120
TRIAL 1 TRIAL 2
Percent error
46
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 8: DATA SHEET Partner’s Name: _________________________________
Sample Calculations
47
EXPERIMENT 9
RATE OF REACTION
Objectives:
Introduction
Chemical kinetics is the study of the rates and order of chemical reactions, as well as the influence of
experimental factors on these rates. Chemical reactions take place as atoms, molecules or ions collide
with each other to form a variety of products. Chemists also study the kinetics of a reaction so that the
reaction mechanism or pathway can be determined. The mechanism shows which species collide, how
many collide simultaneously, and the sequence in which collisions occur as reactants are converted into
products.
Not all collisions are successful. For a reaction to occur, two requirements must be met. First, the
colliding species must be properly oriented. Second, there must be enough energy to overcome repulsive
forces so that existing bonds can be broken and new bonds can be formed to give different substances.
Every chemical reaction occurs at a definite rate, or speed, depending on the experimental conditions.
The most important of these are: the concentrations of the reactants, the temperature, the pressure and the
presence of catalysts. At a given temperature, some reactions take place rapidly, while others are slow.
For example, at room temperature the neutralization of a base by an acid is very rapid, whereas the
combination of hydrogen with nitrogen to form ammonia is extremely slow. Between these two
extremes, there are many inorganic and organic reactions that take place at speeds that are measureable,
and at temperatures that are accessible in the laboratory.
From the above, it is clear that the more molecules (atoms or ions) there are in the reaction mixture, the
greater the change of collision and the faster the reaction. Thus, an increase in concentration should result
in an increase in reaction rate.
48
Likewise, decreasing the temperature decreases the energy content of the molecules and means that fewer
molecules will have the necessary energy for reaction. This minimum energy, which is required for the
reaction to occur, is called the Activation Energy. A decrease in temperature should result in a decrease
in reaction rate.
The effect of changing concentration and changing temperature on the rate of the reaction will also be
observed. The rate of reaction is determined by measuring the time required for a given amount of
magnesium (Mg) metal to be consumed by hydrochloric acid (HCl) solutions of varying concentrations.
In this experiment, the amount of magnesium is kept constant whereas the hydrogen ion concentration,
[H+], is varied, so that the rate of reaction is influenced only by the varying [H+]. The reaction rate is
equal to the rate of appearance of magnesium ion, Mg2+ (aq), in the solution.
Therefore: Rate =
Since the mole ration of Mg(s) to Mg2+ is 1:1 in the chemical equation:
then ∆ [Mg2+] =
and Rate =
49
Procedure
DISCARD ALL WASTE IN THE WASTE CONTAINER PROVIDED
1. Clean a 24 cm length of magnesium ribbon by rubbing the metal lightly with a small piece of
sandpaper to remove the surface oxide layer. Cut the ribbon into six equal pieces of 4 cm length
with the aid of a ruler. Weigh the six pieces together and determine the mass of one piece
assuming all six pieces are the same.
2. Make up 30 mL of each of the following give solutions of hydrochloric acid: 2.0 M, 1.5 M,
1.0 M, 0.50 M and 0.25 M. To do this, calculate the volumes of 3.0 mol L–1 stock hydrochloric
acid solution and water that must be mixed using the dilution equation:
(number mL stock HCl solution) x [HCl] 3.0 M = (30.0 mL diluted solution) x [HCl] diluted
Measure the calculated volume of stock hydrochloric acid solution using a 10 mL graduated
cylinder. Pour this acid into a 50-mL graduated cylinder and then dilute to the 30-mL mark
by carefully adding water from a water bottle. Make up the other four solutions in a similar
way. Pour each diluted solution into a 50-mL beaker. Record the temperature of each of
these solutions.
3. Drop a piece of magnesium into the 2.0 mol L–1 acid solution and start timing the reaction. Stir
gently at first to make sure the metal does not stick to the sides of the beaker. Measure the time
elapsed when the reaction stops. Repeat the procedure with the other four acid solutions.
4. Prepare another 30 mL sample of 2.0 mol L-1 hydrochloric acid solution. Pour the solution into a
50 mL beaker as before and suspend the beaker carefully in an ice water bath contained in a
250-mL beaker. Check the temperature of the hydrochloric acid solution, and when the
temperature has fallen below 10oC, measure it. Then drop the last piece of magnesium into the
cold hydrochloric acid solution and time the reaction.
5. Plot a full-page graph of rate of reaction vs the concentration of the hydrochloric acid solution,
with rate of reaction on the vertical axis and concentration of hydrogen ion on the horizontal axis.
50
51
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 9: DATA SHEET Partner’s Name: _________________________________
RATE OF REACTION
1 2.0
2 1.5
3 1.0
4 0.50
5 0.25
6 2.0
Plot a graph of the rate of the reaction vs hydrogen ion concentration (excluding the low temperature
solution data point) on green millimetric graph paper provided.
52
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 9: DATA SHEET Partner’s Name: _________________________________
3. In which reaction (Trial) is the number of collisions between magnesium and the hydrogen ions
the highest per second?
53
EXPERIMENT 10
Objective:
Introduction:
In many chemical reactions the reactants are not to totally converted to the products because of a reverse
reactions; that is, because the products react to form the original reactants. Such reactions are said to be
reversible and are indicated in the equation by a double arrow (⇌). The reaction proceeding to the right is
called the forward reaction; to the left, the reverse reaction. Both reactions occur simultaneously.
Every chemical reaction proceeds at a certain rate or speed. The rate of a reaction is variable and depends
on the concentration of the reactants and the conditions under which the reaction is conducted. When the
rate of the forward reaction is equal to the rate of the reverse reaction, a condition of chemical equilibrium
exists. At equilibrium the products react at the same rate they are produced. Thus, the concentrations of
substances in equilibrium do not change, but both reactions, forward and reverse, are still occurring.
The principle of Le Chatelier applies to systems in equilibrium and states that when the conditions of a
system in equilibrium are changed the system reacts to counteract the change. Experimentally we will
observe the effect of changing the concentration of one or more substances in a chemical equilibrium.
Consider the hypothetical equilibrium system:
A +B ⇌ C + D
When the concentration of any one of the species in this equilibrium is changed, the equilibrium is
disturbed. Changes in the concentrations of all the other substances will occur to establish a new position
of equilibrium.
54
For example, when the concentration of B is increased, the rate of the forward reaction increases, the
concentration of A decreases, and the concentrations of C and D increase. After a period of time the two
rates will become equal and the system will again be in equilibrium. The following statements indicate
how the equilibrium will shift when the concentration of A, B, C and D are changed.
An increase in the concentration of A or B will cause the equilibrium to shift to the right.
An increase in the concentration of C or D will cause the equilibrium to shift to the left.
A decrease in the concentration of A or B will cause the equilibrium to shift to the left.
A decrease in the concentration of C or D will cause the equilibrium to shift to the right.
Evidence of a shift in equilibrium by a change in concentration can easily be identified by the formation
of a precipitate or by observing any changes in colour that occur.
4. Ammonia Solution
The following reactions occur in solution:
55
phenolphthalein phenolphthalein
NH3 (aq) + H2O (ℓ) ⇌ NH4+ (aq) + OH⁻ (aq)
colourless pink
H2O
NH4Cl (solid) ⇌ NH4+ (aq) + Cl⁻ (aq)
Procedure:
DISCARD ALL WASTE IN THE WASTE CONTAINER PROVIDED
Prepare a stock solution to be tested by adding 1 mL each of iron(III) chloride and potassium thiocyanate
solutions to 50 mL of distilled water. Pour about 5 mL of the stock solution into each of four test tubes.
Use the first tube as a control for comparison.
Add about 1 mL of iron(III) chloride solution to the second tube and observe the colour change. Add
about 1 mL of potassium thiocyanate solution to the third tube and observe the colour change.
Add 0.1 mol/L silver nitrate solution drop-wise (less than 1 mL) to the fourth tube until almost all the
colour has disappeared. The white precipitate formed consists of both silver chloride and silver
thiocyanate (AgSCN). Pour about half the contents (including the precipitate) into another tube. Add
iron(III) chloride solution dropwise (1 to 2 mL) to one tube and observe the result, using the other tube as
a comparison.
Pour about 2 to 3 mL of potassium chromate solution into a test tube. Add 2 drops of 6 mol/L nitric acid
and note the colour change. Now add 2 mol/L sodium hydroxide dropwise to the tube until the original
colour is restored.
Part C: Cobalt(II) Chloride Solution
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Place about 2 mL (no more) of cobalt chloride solution into each of two test tubes. In order to obtain the
desired equilibrium reaction, add about 3 mL of concentrated hydrochloric acid (12 mol/L) dropwise to
one of these test tubes. Note the result. To this freshly prepared equilibrium system, add water slowly,
using the squeeze bottle until the reverse reaction is evident. (Make sure the water mixes properly but
DO NOT CAP THE TUBE WITH YOUR FINGERS WHEN MIXING.)
Prepare a stock solution for testing by adding 2 drops of concentrated ammonia solution and 2 drops of
phenolphthalein solution to 50 mL of tap water. Phenolphthalein is an indicator which turns pink in the
presence of hydroxide ions.
Dissolve a very small amount of solid ammonium chloride in about 5 mL of stock solution and observe
the result.
Take 8.0 mL of distilled water in a test tube and add 1.0 g of solid ammonium chloride. Use the top-
loading balance to weight out the solid. Stopper the tube and shake vigorously for 3 to 4 minutes, or until
the salt has completely dissolved. Continue the process of ammonium chloride addition (in 1.0 g
amounts) and shaking until no more salt dissolves and there is an excess of the solid salt in the test tube
after the shaking period. Place the test tube on a rack and allow the undissolved solid to settle to the
bottom. Withdraw approximately two mL of the saturated solution from the top of the test tube using a
clean, dry dropping pipette, and place it in a clean, dry test tube. Take care not to transfer any solid
ammonium chloride with the dropping pipette.
Perform the following test in the fume hood. Add several drops of concentrated hydrochloric acid
solution to the 2 mL sample of the saturated solution. Observe any changes that occur.
57
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 10: DATA SHEET Partner’s Name: _________________________________
What is the evidence for a shift in equilibrium when iron(III) chloride is added to the stock solution?
What is the evidence for a shift in equilibrium when potassium thiocyanate is added to the stock solution?
What is the evidence for a shift in equilibrium when silver nitrate is added to the stock solution? (The
formation of a precipitate is not the evidence since the precipitate is not one of the substances in the
equilibrium.)
The change in concentration of which ion in the equilibrium equation caused this equilibrium shift when
silver nitrate was added to the stock solution?
Write a net ionic equation to illustrate how the addition of silver ion caused this concentration change.
When the mixture was divided and further tested, what evidence showed that the mixture still contained
SCN⁻ ions in solution?
58
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 10: DATA SHEET Partner’s Name: _________________________________
What is the evidence for a shift in equilibrium when the nitric acid was added?
Explain how sodium hydroxide caused the equilibrium to shift back again.
Describe what you observed when concentrated hydrochloric acid was added to the cobalt(II) chloride
solution.
Describe what you observed when water was added to the equilibrium system.
State whether the amount of each of the following substances was increased, decreased or unaffected
when water was added to the equilibrium reaction.
2-
Co(H2O)62+ (aq) _______________, Cl⁻ (aq) _______________, CoCl4 (aq) _______________
59
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 10: DATA SHEET Partner’s Name: _________________________________
Explain, in terms of the equilibrium, the results observed when ammonium chloride was added to the
stock solution. Write a net ionic equation to describe this reaction.
In which direction would the equilibrium shift if sodium hydroxide were added to the original
equilibrium.
Would boiling the ammonia solution so that ammonia (NH3) gas is expelled have any effect on the
original equilibrium? Explain your answer.
What is the evidence for a shift in equilibrium when hydrochloric acid was added to the saturated
solution?
over →
60
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 10: DATA SHEET Partner’s Name: _________________________________
What ion caused the equilibrium to shift? Write the net ionic equation that describes the shift in
equilibrium.
61
EXPERIMENT 13
ACID-BASE TITRATION
Objectives
Introduction
One of the most rapid and convenient methods for quantitative analysis is volumetric analysis – the
determination of the volume of a solution of known concentration that is just required to react with a
solution of unknown concentration. The solution of known concentration (the “standard” solution) is
carefully added from a burette until the reaction with the other solution is complete (the “theoretical end-
point” or “equivalence point”). As a rule, the end-point is visualized by addition of an indicator that
changes colour at, or near, the theoretical end-point. The exact volume of standard solution required is
recorded and the balanced chemical equation is used to calculate the amount of reactant present in the
unknown solution.
In this experiment, a standard solution of sodium hydroxide is used to determine the concentration of a
dilute solution of acetic acid in water (which is sold as “vinegar”). Vinegar is produced by oxidation of a
solution of alcohol, and may be diluted by the manufacturer for reasons of taste or economy.
You are asked to determine the acetic acid content of a certain brand of vinegar. The reaction used in the
titration is:
HC2H3O2 (aq) + OH⁻ (aq) → H2O (ℓ) + C2H3O2⁻ (aq)
(acetic acid) (hydroxide ion) (acetate ion)
62
The indicator used is phenolphthalein, and this turns pink in the presence of a small concentration of
hydroxide ions. The first pink colour throughout the solution signals that sufficient hydroxide ions have
been added to the vinegar to react with all the acetic acid present.
Procedure
Clean a burette well and rinse it will distilled water. Drain. Pick up 75 mL of standard sodium hydroxide
solution in a clean dry beaker. Add 5 mL to the burette and rinse it well. Discard the rinse by running it
through the stopcock of the burette. Repeat with two more 5 mL portions of the standard solution, then
fill the burette to about one mL above the zero. Run some standard solution out through the stopcock to
remove the air bubble, and to bring the liquid level somewhere below the zero, where it can be read.
Weigh a clean 125 mL Erlenmeyer flask on the top loading balance and record the mass. Add
approximately 2.5 g of the vinegar assigned to you and record the mass of the vinegar.
Add some distilled water and 3 drops of phenolphthalein solution to the flask containing the vinegar.
Record the initial reading of the burette. Titrate by adding the standard solution from the burette to the
flask, first rapidly, then more carefully, and finally drop-wise as the end-point approaches. The solution
should be swirled continuously. Near the end-point, the walls of the flask should be rinsed down with
distilled water. Finally, one drop of the standard solution will give a permanent pink colour in the flask
where there was no colour before. Record the final burette reading at this point. Complete the
calculations, showing your method.
Refill the burette with standard solution. Wash and rinse the flask and repeat the whole determination on
another 2.5 g sample of vinegar.
63
CHEMISTRY 001 Name: _________________________________________
EXPERIMENT 13: DATA SHEET Partner’s Name: _________________________________
ACID-BASE TITRATIONS
TRIAL 1 TRIAL 2
Equation (neutralization)
64
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