BROCK UNIVERSITY

CHEM 1P91
LAB MANUAL

FALL
2016
This manual belongs to: _______________________________________________

Email: _____________________________________________________________

Lab Section/Day/Time: _______________________________________________

If found, please return to MC H 302

Demonstrator’s Name: ________________________________________________

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 TABLE OF CONTENTS
Disclaimer............................................................................................................................... 4
...

Introduction............................................................................................................................. 5
...

To Users of Contact 6
Lenses.......................................................................................................

Laboratory Rules and 7

Safety......................................................................................................

CHEM 1P91 Procedures and 13

Reports........................................................................................

Experiment 1: Determining 17
Density..........................................................................................

Experiment 2: Illustrating Chemical 20

Reactions.........................................................................

Experiment 3: Synthesis of 29
Alum..............................................................................................

Experiment 4: Determining the Formula of a 32

Hydrate..............................................................

Experiment 5: Determining Vitamin Tablet 35

Composition.........................................................

Appendix A: Significant 38
Figures...............................................................................................

Appendix B: 39
Filtration...............................................................................................................

Appendix C: Volumetric 42
Apparatuses.......................................................................................

Appendix D: 45
Graphing...............................................................................................................

Fundamental Constants and Conversion Factors 46

Errors and Accuracy 47

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DISCLAIMER
The experiments in this CHEM 1P91 Lab Manual have been used by this department for a
number of years. To the best of my knowledge, they are either original experiments, or are
extensively modified and rewritten versions of standard experiments that commonly appear in
typical lab manuals. To the best of my knowledge, none are copies of copyrighted work.

Georgii Nikonov
Chair, Department of Chemistry
Brock University

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 INTRODUCTION

For our small span,

the sun has fuel, the moon lifts the lulling sea,
the highway shudders with stolen hydrocarbons.

-from John Updike’s Ode to Entropy

Welcome to CHEM 1P91!

The experiments held within these pages are meant to give you a concrete demonstration of
some of the abstract concepts covered in your lectures and textbook. When you step into the
laboratory, you become a chemist. You will (hopefully) model real scientific processes, master
advanced techniques for chemical analysis and synthesis, and develop solid laboratory habits that
will serve you for years to come. Just as inspiration for new and innovative research ideas can
come from everyday life, you will perform experiments in this course that have been developed as
solutions to everyday problems.

Tips for Getting the Most Out of Your Laboratory Experience

1. Read all of the introductory sections of this manual. They are there for your safety!

2. Pay attention to points written in bold or italics or things surrounded by boxes

3. Make good use of the appendices at the back of the manual.

4. Never be afraid to ask questions to your laboratory demonstrators or your peers.

APPLY! CONCEPTUALIZE!
These questions have to do with the Visualization is a useful tool for problem
practical applications of an experiment. Use solving and the purpose of these boxes is to
creativity to imagine how different aspects get some of your thought processes down on
of the lab might influence other situations. paper.

NOTICE! HYPOTHESIZE!
These boxes are meant to draw your Use your own knowledge and any other
attention to some important detail in the resources at your disposal to make an
experiment. It may be a key concept, or a educated guess at the questions in these
vital part of the procedure or equipment. boxes.

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 TO USERS OF CONTACT LENSES
The use of contact lenses in place of traditional eyeglasses leads to a situation in a chemical
laboratory which is potentially dangerous.1 In the event of splashing of a liquid or solution of a
chemical into the eye, both hard and soft contact lenses can act to trap the material in contact with
the eye, and so prevent its removal by irrigation. In addition, soft contact lenses are porous to many
chemicals, and can accumulate material from the atmosphere, bringing it into immediate contact
with the eye. In view of these and other hazards outlined in ref. 1, the Department of Chemistry
recommends the following policy to users of contact lenses:

1. that contact lenses not be worn in the laboratory unless there is no alternative, and in this
event, then

2. that the lenses used should preferably be of the hard type, and that all users of contact lenses
in a laboratory should wear safety goggles, and not safety glasses. The former provide more
complete protection from splashing liquids.

Georgii Nikonov
Chair, Department of Chemistry
Brock University

1. Chem. & Eng. News, 57, (47), 4 (1979).

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 LABORATORY RULES AND SAFETY
APPROPRIATE CLOTHING

□ Always wear your lab coat with the buttons secured!

□ Never wear sandals or any type of open-toe shoe in the lab!

□ Always tie back loose or long hair! You don’t want to dip it into a beaker of acid or a
burning flame!

□ Always wear long pants, rather than shorts or skirts! Covered legs have an extra barrier
against potentially harmful spills!

You must wear safety glasses or goggles

approved by the Department of Chemistry
while in the lab at all times!

SAFETY EQUIPMENT

Before beginning work in any laboratory environment, you should make yourself aware of
the location of all the following safety equipment:

Chemical Shower: Use this when corrosive liquid has spilled over a large area of your clothing
or skin. Remove all clothes immediately and rinse affected areas thoroughly. Remember: safety
before modesty!

Eye-Wash Fountain: Located at sink by main entrance to lab, use this when any chemical has
been splashed into your eyes. Hold your eyelids open wide and have someone else help you flush
them with water for at least 15 minutes.

First Aid Kit: This kit has typical first aid materials (like Band-Aids) as well as solutions for
chemical burns.

Chemical burns often do not become serious if the affected area is washed promptly.
If you spill a corrosive chemical onto your skin,
immediately rinse with lots of water from the sink!
Be sure to inform your demonstrator if an accident does occur.

Spill Kit: Use this kit for large surface spills of solvents, acids, or bases.

Fire Extinguisher: The lab is equipped with a number of carbon dioxide (CO 2) extinguishers
spread out around the room, which are effective against larger fires involving organic liquids and
electrical wiring (B & C class fires).

Small fires in beakers or flasks can be smothered by covering them with your manual!

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Fire Blanket: Located in a red metal box beside main entrance to the lab is a pleated fire blanket.
These can be used to cover an individual whose clothing catches on fire.

If your clothing catches on fire, the rule is still to

Stop, Drop, and Roll!
Try to avoid any hazards that might be on the floor near you.
Someone else will retrieve the fire blanket.

Fire Alarm: Fire alarm pull stations are located in every hallway on campus. Use them only if a
serious fire starts. When the fire alarm rings, everyone must evacuate the building.

Gas Cut-Offs: If there is an accident while using a Bunsen burner, shut the valve providing fuel
to the problem if it is safe to do so. If you might be harmed while attempting to shut the closest
valve, cut off the main gas line located beside the door to the lab.

Telephone: Emergency phone numbers and procedures are located next to the telephone in the
balance room.

Material Safety Data Sheets (MSDS): These pages provide a summary of hazards associated
with any of the chemicals present in the lab. Specific chemical hazards are listed at the beginning
of each experiment in this manual, but you may consult the MSDS at any time if you are interested
in more detailed information on the safety and handling of a particular compound.
You can also access a number of MSDS online for free at
http://msds.chem.ox.ac.uk/ and http://www.msdsxchange.com

LABORATORY CONDUCT

1. Be sure to follow the experimental procedures carefully. Make changes only if your
instructor specifically tells you to. When in doubt, ask.

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2. Read labels carefully. Pay special attention to dilute and concentrated labels on acids and
bases.

3. Should an accident occur, call loudly for help.

4. Do not eat, drink, or smoke in the lab – ever.

Many instances of chemical poisoning can be traced to violation of this important rule.

5. Consider all chemicals to be dangerous and potentially lethal unless you find out otherwise
(e.g. by looking up their properties in the MSDS binder). If you are instructed to smell a
gas, waft the vapours towards your nose cautiously.

Our goal is to respect, but not fear, chemicals.

6. If you spill a corrosive chemical on yourself (particularly if you get something in your
eyes) wash it off immediately! Use the chemical shower if the spill is over a large area of
your body. Use the eye-wash fountain to rinse chemicals from your eyes (for a minimum
of 15 minutes).

If you splash something in your eye, yell for help and start rinsing your eyes immediately!
Arrangements will be made to transport you to the hospital for professional evaluation
and treatment once the initial first-aid is completed.
Most eye contact will be minimized by the lab glasses or goggles that you are wearing.

7. Wash your hands before leaving the lab, especially before eating or using the washroom!

8. Keep all work areas clean and tidy, including the common areas where reagents are stored,
as well as the balance room. Clean up broken glassware immediately with a dustpan and
broom, by placing pieces into the proper receptacle (not directly into the garbage). If you
spill a chemical, ask your demonstrator how to clean it up.

9. Dispose of all chemicals properly. Do not pour chemicals directly down the sink, unless
your demonstrator gives you permission. Each chemical has its own waste container. Be
sure to read the colour-coded labels.

Red: non-halogenated organic liquid

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 Green: halogenated organic liquid
White: solid organic waste
Blue: inorganic liquid bases
Yellow: inorganic liquid acids

10. Always pour concentrated acids into water, never water into acid! Pouring a small
volume of water into a larger volume of concentrated acid may release enough heat to cause
the acid to splatter. Hot, concentrated acids are extremely corrosive! Furthermore, never
mix a concentrated acid with a concentrated base – the reaction will be violent!

To help you remember:

Acid into Water = Awwwww…
Water into Acid = Waaaaaah!

acid

water

11. Never work alone in the laboratory.

12. Don’t panic when an accident occurs! For example, if a beaker of solvent catches fire, you
can easily put it out by placing a watch glass, larger beaker, clipboard, book, etc., over it
to smother the flames, provided you stay calm.

13. If the fire alarm goes off, take a few seconds to turn off your Bunsen burner and any nearby
electrical equipment. Then leave the building by the nearest safe exit.

14. Backpacks, handbags, etc., are to be placed in the designated area near the blackboard. Do
not leave things in the aisles where people may trip over them.

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PREVENTING COMMON LABORATORY ACCIDENTS

A. Fires and Explosions

□ Keep flammable materials away from flames. Common flammable materials you may
encounter in these labs include: organic liquids, including alcohols, esters and ketones,
magnesium, powdered iron and hydrogen gas.

□ Pay careful attention when working around open flames. Extinguish all flames when not
in use.

□ Use an electric heater or water bath when heating flammable liquids; never heat them in a
container directly over a flame.

□ When gases are generated by heat or chemical reaction, be sure that they have a way to
escape from the container. Pressure build-up can cause an explosion.

□ Always follow directions when mixing chemicals. Do not use larger amounts than the
experiment calls for. Mix chemicals in the order specified.

□ Be careful of disposing of reactive chemicals. More than one explosion has been caused
by a student dumping something down the sink or into the wrong waste container.

B. Cuts

□ Throw away broken or chipped glassware into the broken glass container.

□ Protect your hands with a cloth when handling glass with sharp edges, or use a dustpan and
broom.

□ When inserting glass tubing into a hole in a rubber stopper or cork, always grasp the
tubing near the point of insertion to minimize strain on the glass. Most cuts in the lab
are due to violation of this rule. If the tubing is difficult to insert, lubricate it with a little
glycerine.

C. Chemical and Physical Burns

□ Most burns in the lab are due to spilling concentrated acid or base on the skin. You have a
few seconds to rinse off these chemicals before serious burning begins. If the spill is on
your hands, wash them immediately with water from the sink. If the spill is over a larger
area of your body, get to the chemical shower and immediately remove all clothing and
turn the water on.

□ Use a cork or rubber stopper to seal all test tubes or flasks which must be shaken. Do not
use your thumb or finger as a stopper.

□ When diluting concentrated acid, add the acid slowly to the water. Never the other way
around.

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 □ When boiling liquids or carrying out reactions in test tubes, keep the mouth of the test tube
pointed away from yourself and your neighbours.

D. Poisoning

□ Some chemicals may cause acute or lethal poisoning very quickly, while others may have
effects that appear more slowly or less obviously. In order to avoid both short and long-
term poisoning, observe all laboratory rules at all times. Many were designed with poison
prevention in mind.

□ Keep toxic or irritating fumes in the fume hood at all times.

PENALTY FOR REPEATED VIOLATION OF SAFETY RULES

Common sense tells you that you will be much safer in the lab if you and your neighbours
do your best to follow the rules above. The rules don’t cover every possible situation, so exercise
due caution and judgment in your work.

The Chemistry Department does reserve the right to impose one or both of the following
penalties on a student who repeatedly violates safety rules, thus becoming a hazard to self and
others:

i. The student may be required to write an essay on some aspect of lab safety (topic to be
assigned by instructor) before being allowed to continue work in the labs.

ii. The student may not be allowed to work in the lab at all.

These penalties are rarely invoked; however, when they are, any labs missed are counted
as zeroes (unexcused, no make-up allowed). Remember that you are only allowed to miss one lab
in order to pass the course, regardless of what your final average is. A student could still fail the
course even with an average of 80 after the lab work was incomplete.

Best wishes for a safe, accident-free, lab experience!

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 CHEM 1P91 PROCEDURES AND REPORTS
All measurements and observations are to be recorded in pen in a student lab notebook
with permanent binding and special carbonless sheets. These are available at the Brock Bookstore.
Please bring your notebook, lab manual, and calculator to every lab.

BEFORE COMING TO LAB EACH WEEK

□ Read the experiment! Try to answer any pre-lab questions that are asked.

□ On a separate sheet of lined paper, list the main steps of the procedure and note any
questions you have.

□ In your lab notebook, write the following information at the top of the page: your name,
your demonstrator’s name, your lab section (day and time), the date, the experiment
number, and the title of the experiment.

When you first obtain your student lab notebook, make sure you tear out the periodic table
found on the second page and reinsert it after the first carbonless sheet.
This ensures that what you write on the top sheet only gets duplicated on a second sheet
(the one that says COPY) and not on several other copy sheets underneath.

□ Write a purpose: one or two complete sentences in your own words telling why the
experiment is being done and what techniques are being used.

□ Consult the hazard table provided for the experiment into your notebook to make yourself
aware of the possible hazards of each chemical you will be working with.

□ Prepare a blank data table and leave enough space to write in quantitative measurements
as well as qualitative observations.

□ Do not use a title page or do any calculations at this point.

IN THE LAB

□ Store any additional books, bags, and coats in the designated area near the blackboard.

□ Wear your lab coat and safety glasses at all times!

□ Have your demonstrator initial your neatly prepared data tables and procedure notes before
starting the experiment. You will be asked to leave if you are not prepared.

□ Write down any changes to the procedure or other announcements that are written on the
blackboard.

□ Never write anything during the lab session on a scrap of paper! Record all quantitative
measurements (including units!) directly into your data tables in ink. Bring your notebook

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 with you into the balance room when weighing samples. Make sure that you are making a
legible copy onto the second sheet of your notebook.

If you make an error, neatly cross out the incorrect word or number with a single stroke
and write the corrected value above or below the mistake.
This is why you left yourself plenty of space
in the data tables you prepared before coming to lab.

□ Record the appearance of all starting materials as well as any changes that occur during
the experiment. Observations may be written in point-form, but be specific and write as
many observations as possible! When you think you’ve written enough, write some more.

Sample Observations:
The solution turned from colourless to dark blue…
The mixture got warm and bubbled strongly…
A foggy white precipitate formed but then disappeared as more acid was added…
The solution remained clear and colourless…

You may abbreviate “clear and colourless” as “c and c”, if you desire.
Try to limit other abbreviations.

□ Before you leave the lab, you may want to do a rough calculation on a separate sheet of
paper to see if you need to do another trial before cleaning up. Do not carry out
calculations on the same page as your experimental data.

□ Make sure your demonstrator initials the bottom of every sheet of paper you write on
in the lab! Remember to hand in the carbonless COPY sheet before leaving. If you did
not complete an experiment during your regular lab time, submit your COPY sheet by
placing it in your regular demonstrator’s drop-box immediately after completing the
experiment. If you fail to give a copy of your data to your demonstrator, your lab will
not be marked!

No changes to observations or measurements are to be made to your original data sheet

after handing in the COPY sheet.

□ Clean your work area! Wash off the counter and all glassware used, put equipment back
in its proper place, and double-check that the gas jets near you are completely turned off –
even if you weren’t using them!
If you do not clean up after yourself, your demonstrator will not initial your data sheets
and your lab will not be marked!

□ Wash your hands before leaving the lab, especially before eating or using the washroom!
THE LABORATORY REPORT

You will be required to write a short lab report for the experiments. All reports are due by
5 p.m. on the second day after the lab work is performed. Lab reports will be uploaded to
Crowdmark. Talk to your demonstrator about accommodating special circumstances.

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In the order in which they appear, your lab reports should consist of the following sections:

1. Original Data Sheets: Take a clear image of your original data sheets and use them as the
first page(s) of your report. Do not copy out the data tables onto another sheet of paper.
If you really feel that the tables are too messy to read legibly, you may re-write the tables,
but place them after the original data sheets. You do not need a title page.

2. Sakai Sheets: Download and fill-out the report sheets from Sakai.

3. Additional Calculation Sheets (if necessary): Calculations may be done either in pencil
or pen, as long as they are neat, legible, and labelled! Show all calculations! This is the
only way you can get credit for your work! You may choose to show every step, or you
may write out the formula on one line and show only the answer; whichever is easier for
you.

Tips for calculations:

□ Consider fully completing the calculations for one trial before starting the next trial.

□ Show a unit beside every number you write down!

□ Keep one extra rounding digit for all intermediate values and round only the final average
to the number of significant figures allowed by the measurements.

Review Appendix A for rules regarding significant figures!

□ When more than one trial has been done, you must calculate the precision of the
measurements. See the Handy Sheets at the back of this lab manual.

If your lab report is handed in on time,

it should be marked and returned during your next lab period!

Be safe, and have a great year!

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 DEPARTMENTAL POLICY ON LABORATORIES

1. Students are required to wear lab coats and safety glasses in the lab at all times and will
not be permitted to perform an experiment without them.

2. Due to COVID restrictions, a face mask, covering the mouth and nose, must be worn at
all times.

3. Whenever possible, students should try to make up a missed experiment in another lab
section during the same week. Permission from the senior demonstrator is required.

4. Medical excuses, signed by a doctor, are to be given to the senior demonstrator.

5. Labs missed for reasons other than medical may also be made up with the permission of
the senior demonstrator, but some documentation for the reason must again be given.

6. All but one experiment must be completed for each course and reports handed in to
receive a course credit. Note however that any uncompleted experiment receives a mark
of zero.

7. Data tables will be checked in class each week. Reports are due two days after the
experiment is performed and should be uploaded to Crowdmark. Late reports will lose
10% each late day unless granted an extension by the senior demonstrator.

8. Students will never use another student’s experimental data unless approved by the senior
demonstrator. As well, students will never represent another student’s work as his/her
own.

9. Students who copy reports, or allow their reports to be copied, will be severely penalized.

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 EXPERIMENT 1
Determining Density

Pre-Lab Readings:
Appendix A: Significant Figures
Appendix C: Volumetric Apparatuses
Appendix D: Graphing

Introduction If you make a graph of the data in Table 1,

you can compare the density of your unknown
For this experiment, you are given a solution to the curve of the graph and interpolate
solution of ethanol in water, but you are not the weight % (the composition). You then know
told just how much ethanol is in the solution. the amount of ethanol present in your solution
How do you find out? Why do you even want and it is no longer unknown!
to know?
So why do we want to know the
To answer the first question: what if you concentration of an ethanol solution anyway?
have an analytical balance and a buret? You Ethanol and water may not be an exciting
can measure out a volume of liquid to the combination, but what about other chemical
nearest 0.01 mL and then weigh the liquid to solutions?
four decimal places. When you know the
mass and volume of a sample, you can APPLY! Why might it be important for a
calculate the density! chemist to determine an unknown
concentration?
Density is defined as the mass of a _______________________________
substance per unit volume, at a given _______________________________
temperature. Chemists that have come before
you have gone to great lengths to determine
the density of various concentrations of Of course, this isn’t the only way to
ethanol in water at room temperature, and determine the concentration of a given solution.
their results are given in Table 1 below. This is merely one physical method among
many other physical and chemical methods for
Table 1: Density of Aqueous Ethanol determining the composition of a sample.
Solutions as a Function of the Weight %
Concentration NOTICE! As you dissolve more ethanol into
Wt. % Density at 20°C (g/mL) water, the density of solution (circle one):
Ethanol
0.00 0.9982 increases / decreases
15.00 0.9751
30.00 0.9538 Refer to Table 1.
45.00 0.9247
60.00 0.8911
75.00 08556
90.00 0.8180

17
 Method
You have now completed trial 1 and have
Accurately weigh a clean, dry, 50 mL recorded the initial/final weights of your flask
Erlenmeyer flask on an analytical balance and and the initial/final buret readings. The first
record the initial weight to four decimal column of your data table may be completed.
places.
Rather than wasting time and emptying the
You will be assigned solution of unknown flask between trials, pretend that your flask is
ethanol concentration in a labelled buret. now empty and use the final weight of the flask
in trial 1 as the initial weight of the flask for trial
Record the letter label of your unknown 2.
solution in your lab notebook!
This is the only way you can receive a mark Add another 10-12 mL of the same unknown
for accuracy! solution to your flask, being careful to
accurately record the initial and final buret
Before you take an initial buret reading, readings. Record the new final weight of your
make sure that there are no air bubbles in the flask for trial 2.
tip of the buret! If there are, allow a tiny
amount of liquid to pass through the tip and On a separate sheet of paper, calculate the
into a waste flask until there are no more air density of each of your trials, the average
bubbles. density, and the % precision (refer to the Errors
and Accuracy section on page 72 of this
Record the initial buret reading manual).
and all further buret readings
to two decimal places! If your precision is greater than 1%, do more
(e.g. 0.01 mL) trials until at least two densities are within a 1%
range of each other. You may then pour your
Quickly add approximately 10-12 mL of unknown solutions into the waste containers
unknown ethanol solution to your flask. Don’t provided in the fumehoods..
waste time trying to get an exact number!

Wait about 15 seconds to allow the liquid

to settle inside the buret before recording the
final buret reading to the nearest 0.01 mL.
Record the final weight of the flask
(containing your unknown solution) to four
decimal places.

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SAMPLE DATA TABLE (Leave yourself lots of space when you copy this into your notebook!)
Unknown Letter: __________

Trial 1 Trial 2 Trial 3 Trial 4

Final weight of flask: ___________ g ___________ g ___________ g ___________ g
Initial weight of flask: ___________ g ___________ g ___________ g ___________ g
Weight of liquid: ___________ g ___________ g ___________ g ___________ g
Final buret reading: _________ mL _________ mL _________ mL _________ mL
Initial buret reading: _________ mL _________ mL _________ mL _________ mL
Volume of liquid: _________ mL _________ mL _________ mL _________ mL

Observations: i.e. colour, clarity, odour, and anything else that relates to sample appearance

19
 EXPERIMENT 2
Illustrating Chemical Reactions

Pre-Lab Readings: None. This is a highly qualitative experiment.

Hazard Table
NaCl – sodium chloride May cause irritation.
NaBr – sodium bromide Irritant. May affect central nervous system.
KI – potassium iodide Harmful if swallowed. May cause skin or eye irritation.
Na2SO4 – sodium sulfate Irritant.
Na2CO3 – sodium carbonate Irritant. May be harmful if swallowed.
NaOH – sodium hydroxide Irritant. Corrosive.
AgNO3 – silver nitrate Corrosive. May be harmful if swallowed.
Mg(NO3)2 – magnesium nitrate Oxidizer. Eye, skin, and respiratory irritant. May be harmful
if swallowed.
Ba(NO3)2 – barium nitrate Irritant. Strong oxidizer. May be fatal if swallowed. Chronic
exposure may lead to damage of the central nervous system,
liver, spleen, kidney, or bone marrow.
Cu(NO3)2 – copper (II) nitrate Irritant. May be harmful if swallowed. May cause liver or
kidney damage.
Fe(NO3)3 – iron (III) nitrate Irritant. Oxidizer.
Co(NO3)2 – cobalt (II) nitrate Irritant. Oxidizer. May be harmful if swallowed.
HCl – hydrochloric acid Corrosive. Irritant. Harmful or fatal if inhaled or swallowed.
HNO3 – nitric acid Corrosive. Harmful if inhaled or swallowed.
H2SO4 – sulfuric acid Corrosive. Harmful by ingestion or skin contact.
CH3COOH – acetic acid Concentrated solutions are corrosive.
NH3 – ammonia Corrosive. Harmful if inhaled or swallowed.
phenolphthalein in methanol Irritant. May be harmful if swallowed. Possible cancer
hazard.
CH3COOH – acetic acid Concentrated solutions are corrosive.
Mg – magnesium metal turnings Irritant. Flammable solid. Harmful if swallowed.
FeCl3 – iron (III) chloride Irritant. May be harmful if swallowed.
H2O2 – hydrogen peroxide Irritant. Oxidizer. May be harmful if swallowed.
Na2SO3 – sodium sulfite Irritant. May be harmful if swallowed. May cause allergic
reactions.
NH4Cl – ammonium chloride Irritant. May be harmful if swallowed.
CuCl2 – copper (II) chloride Irritant. Harmful if swallowed.
aluminum foil May cause skin or eye irritation.
powdered iron metal Flammable solid. Irritant. May be harmful if swallowed.
[NH4]2[Fe][SO4]2 – iron (II) Irritant. May cause liver damage.
ammonium sulfate
NH4SCN – ammonium Irritant. Harmful if swallowed. Contact with acids releases
thiocyanate toxic gas.
K3[Fe(CN)6] – potassium iron Harmful if swallowed. Contact with acid liberates hydrogen
(III) cyanide cyanide, a very toxic gas.

20
 Introduction Part A: Precipitates

This experiment is divided into 10 A solution is a clear, homogeneous mixture.

procedures to illustrate 10 different common It can be any colour as long as it does not
chemical reactions. A chemical reaction is a contain any particles (all components are
process that transforms one or more chemical dissolved). When two solutions are mixed, a
species (reactants) into new substance(s) precipitate may form which makes the mixture
(products). cloudy or foggy. The particles of solid are
often visible and eventually settle at the bottom
In general, a chemical reaction will occur if of the container.
one or more of the following conditions are
met: You can predict when a reaction will occur
by noting whether an insoluble compound is
□ One reactant can act as an acid and the formed. To do this, you need to know which
other as a base. compounds are soluble in water and which are
not. Solubility rules for various classes of
□ An insoluble compound might be compounds are given in most first-year
produced. chemistry textbooks, but two are shown below
as examples.
□ A gas will be formed.
All chlorides are soluble in water except
□ One reactant is an oxidizing agent and those of silver, lead (II), and mercury (I).
the other is a reducing agent.
All hydroxides are insoluble in water
There are five kinds of observations you except those of sodium, potassium,
can make that indicate a chemical reaction has rubidium, and cesium.
occurred. Barium hydroxide is slightly soluble in
water.
1. An insoluble solid (precipitate) makes Hydroxides that are insoluble in water
the mixture cloudy or settles to the will dissolve in acids.
bottom of the container.
Many insoluble compounds are important
2. A definite colour change is visible. to life as we know it. Calcium carbonate is a
mineral found in the human ear and forms the
3. The change in concentration of H3O+ escarpment on which Brock sits. Calcium
cations (pH) is detected using pH paper phosphates make up bones and teeth. Silicates
or a chemical indicator. form the shells of some microorganisms and
are also a major constituent of most igneous
4. Heat is released or absorbed and a rocks.
change in temperature is detected.

5. Bubbles or fizzing indicates that a gas

is produced, which can be collected
and tested to determine its identity.

21
Procedure 1: Solubility of Silver Salts 0.1 M silver nitrate AgNO3
0.1 M copper (II) nitrate Cu(NO3)2
Place two drops of each of the following 0.1 M iron (III) nitrate Fe(NO3)3
solutions into separate depressions of a 0.1 M cobalt (II) nitrate Co(NO3)2
wellplate: Add a drop of 0.1 M sodium hydroxide
0.1 M sodium chloride NaCl NaOH to each well. Record detailed
0.1 M sodium bromide NaBr observations.
0.1 M potassium iodide KI
0.1 M sodium sulfate Na2SO4 To each depression that contains a
0.1 M sodium carbonate Na2CO3 precipitate, add two drops of 3.0 M nitric acid
0.1 M sodium hydroxide NaOH HNO3. Record detailed observations.
Add a drop of 0.1 M silver nitrate AgNO3
to each well. Record detailed observations.

Carefully rinse and dry your wellplate Mg(NO3)2 Ba(NO3)2 AgNO3

after each procedure!

Cu(NO3)2 Fe(NO3)3 Co(NO3)2

NaCl NaBr KI

Na2SO4 Na2CO3 NaOH

Figure 2: Wellplate setup for Procedure 3

Part B: Acids and Bases

Many common reactions between acids and

Figure 1: Wellplate setup for Procedure 1 bases take place without a colour change and
without forming a precipitate or generating a
Procedure 2: Anions in Tap Water gas. If the reaction is on a large enough scale,
or uses concentrated conditions, you can
Add one drop of 0.1 M silver nitrate AgNO3 occasionally detect a reaction by the amount of
to about 25 mL of tap water in a clean, dry heat generated. Most of the time, however,
beaker. Stir with a clean, dry glass rod. chemists use pH paper or a chemical indicator
Repeat the procedure with about 25 mL of to determine whether the H3O+ or OH-
distilled water. Make detailed observations. concentrations have changed when solutions
of acids and bases are mixed. Remember that
Procedure 3: Solubility of Hydroxides pH is defined according to E1:

Place two drops of each of the following E1: pH   log H   

solutions into separate depressions of a where [H+] is the concentration of H3O+ in
wellplate: units of mol/L
0.1 M magnesium nitrate Mg(NO3)2
0.1 M barium nitrate Ba(NO3)2

22
Procedure 4: Detection of Acidity or Basicity Procedure 5: Neutralization

Place two drops of each of the following Arrange three clean, dry test tubes in a rack.
solutions into separate depressions of a
wellplate: To the first test tube, add:
0.1 M hydrochloric acid HCl 1 dropper full of 3.0 M sulfuric acid
0.1 M nitric acid HNO3 1 drop of phenolphthalein indicator
0.1 M sulfuric acid H2SO4 2 droppers full of 3.0 M sodium
0.1 M acetic acid CH3COOH hydroxide
0.1 M sodium hydroxide NaOH Touch the side of the test tube. Note any
0.1 M ammonia NH3 temperature or colour change.

Dip a clean, dry glass rod into one of the To the second test tube, add:
solutions and place a drop onto half a piece of 1 dropper full of 0.1 M sulfuric acid
pH paper. Match the colour of the paper to the 1 drop of phenolphthalein indicator
pH legend provided. Record the colour change 2 droppers full of 0.1 M sodium
and the numerical value given for pH. Rinse hydroxide
the glass rod and repeat the test with each Touch the side of the test tube. Note any
solution. temperature or colour change.

Add a drop of phenolphthalein indicator to To the third test tube, add:

each depression and record any colour changes 1 dropper full of 0.1 M sulfuric acid
you observe. (no phenolphthalein indicator)
2 droppers full of 0.1 M sodium
hydroxide
Touch the side of the test tube. Note any
HCl HNO3 H2SO4 temperature or colour change.

Part C: Gases
CH3CO2H NaOH NH3 There are five classes of reactions that
generate gasses.

1. Active metals can react with acids to

produce hydrogen gas. i.e.

E2: 2 Al(s) + 6 HCl(aq) → 2 AlCl3(aq) + 3 H2(g)

Figure 3: Wellplate setup for Procedure 4
2. Metals dissolve in nitric acid to
produce nitrogen dioxide gas. i.e.

E3: Cu(s) + 4 HNO3(aq) → Cu(NO3)2(aq)

+ 2 NO2(g) + H2O(l)

23
 3. Carbonates, sulfites, and sulfides smells like rotten eggs, and NH3 is described
dissolve in acid to generate carbon as “ammoniacal”. NO2 is yellow-brown and
dioxide, sulfur dioxide, or hydrogen acrid. Cl2 is a poisonous, yellow-green gas
sulfide respectively. i.e. which has a choking, irritating scent.

E4: CaCO3(s) + 2 HNO3(aq) → Ca(NO3)2(aq) CO2 and SO2 are acid anhydrides. These
+ CO2(g) + H2O(l) gases give an acidic reaction with moist pH
paper. NH3 dissolves in water to give a basic
E5: Na2SO3(s) + H2SO4(aq) → Na2SO4(aq) solution and a basic reaction with moist pH
+ SO2(g) + H2O(l) paper.

E6: ZnS(s) + 2 HCl(aq) → ZnCl2(aq) + H2S(g) Procedure 6: Acids and Metals

4. Hydrogen peroxide or metal peroxides Arrange three clean, dry test tubes in a rack.
can decompose to liberate oxygen gas. To the first test tube, add one dropper full
i.e. of 3.0 M hydrochloric acid.
To the second test tube, add one dropper
E7: 2 H2O2(aq) → O2(g) + 2 H2O(l) full of 3.0 M nitric acid.
To the third test tube, add one dropper full
(Glass bottles containing hydrogen peroxide of 3.0 M sulfuric acid.
can explode from pressure build up
over a period of a few months Add a small piece of magnesium metal to
if not cared for properly!) the first test tube and immediately cover the
hole with your thumb to trap any gases inside.
5. Ammonium salts react with strong
bases (such as sodium hydroxide) to After about 30 seconds, test the
produce ammonia gas. i.e. flammability of the gas by inserting a burning
splint into the top of the test tube. Record
E8: NH4NO3(aq) + NaOH(aq) → NH3(g) detailed observations about the reaction after
+ NaNO3(aq) + H2O(l) the splint test. Repeat the above procedure for
each test tube.
Gases have a number of characteristic
properties that make them possible to identify. Procedure 7: Generating Oxygen
For example, if you insert a burning splint into
a small container of hydrogen gas, a “popping” Place 5 drops of 0.4 M iron (III) chloride
sound may be heard. If you insert the same FeCl3 in a clean, dry test tube, then add two
burning splint into a small container of oxygen droppers full of 6% hydrogen peroxide
gas, the splint may burn more brightly. If the solution and immediately cover the hole with
flame is extinguished, however, the gas is not your thumb to trap any gases inside. After
of a flammable variety. about 30 seconds, test the flammability of the
gas by inserting a burning splint into the top of
Some gases have a particular colour or the test tube. Record detailed observations
odour associated with them. H2, N2, O2, CO2, about the reaction after the splint test.
and N2O are colourless and odourless. SO2,
H2S, and NH3 are colourless but each has a
distinctive scent: SO2 is acid and irritating, H2S

24
Procedure 8: Other Gas-Producing Reactions as combustion and corrosion. You will use a
couple of different metal reactants to examine
Into separate corner depressions of a displacement reactions and redox reactions
wellplate, place two drops of the following with acids.
solutions:
1.5 M sodium carbonate Na2CO3 An example of a displacement reaction is
1.5 M sodium sulfite Na2SO3 the “silver tree” reaction. A drop of liquid
1.5 M ammonium chloride NH4Cl mercury is added to an aqueous silver nitrate
solution.
Carefully lay a moistened piece of pH paper
across the top of each depression, being careful E9: 2 AgNO3(aq) + Hg(l) → 2 Ag(s)
not to touch the solution. Extra-carefully add + Hg(NO3)2(aq)
one drop of 1.0 M sulfuric acid down the side
of each depression, being extra-careful not to In this reaction, metallic mercury (0) is
touch the paper. Record detailed observations. oxidized to mercury (II) and silver (I) is
reduced to silver metal (0). The mercury is said
You may carefully sniff the depressions to to displace the silver from silver nitrate,
see if you can detect the odours of the gases forming beautiful needle-shaped crystals of
evolved, if you like. The volumes being used silver that give the reaction its name.
and produced are small enough that you should
be safe. In Part C, you saw that metals can react with
acids to generate hydrogen gas, but what
Repeat the procedure for all three wellplate happens to the oxidation state of the metal?
depressions using 1.0 M sodium hydroxide What about when you digest breads or cereals
instead of 1.0 M sulfuric acid. containing reduced iron using your own
stomach acid? Reduced iron is metallic Fe0 and
stomach acid is HCl. You know that common
oxidation states of iron are iron (II) and iron
Na2CO3 Na2SO3 (III), but iron must be in the +2 oxidation state
to be absorbed by the body and used. In the
final procedure, you will find out what happens
when iron is ingested, and if it is actually
beneficial to buy and eat iron-fortified foods.

Procedure 9: Redox Displacement

NH4Cl Place two droppers full of 0.1 M copper (II)

chloride CuCl2 solution in a clean, dry 50 mL
beaker. Add five or six 1 cm squares of
Figure 4: Wellplate setup for Procedure 8
aluminum foil to the beaker, pushing the metal
down into the solution with a glass stirring rod
Part D: Redox Reactions
if necessary. Record detailed observations.
Redox reactions occur when the oxidation
states of the reactants are different than the
oxidations states of the products. There are
many different types of redox reactions, such

25
 Procedure 10: Iron in Stomach Acid (HCl) To the first column (spots, 1, 3, and 5), add
one drop of 0.1 M ammonium thiocyanate
Place two shakes of powdered iron from the NH4SCN. To the second column (spots 2, 4,
plastic shaker into a clean, dry 50 mL beaker. and 6), add one drop of saturated potassium
Add two droppers full of 1.0 M hydrochloric iron (III) cyanide K3[Fe(CN)6].
acid and set the beaker aside while you prepare
your wellplate. Swirl the beaker containing powdered iron
and hydrochloric acid. To the third row (spots
SCN- [Fe(CN)6]3- 5 and 6), add two drops of this beaker solution.
↓ ↓ Record detailed observations.

The goal here is to compare the colour of the

Fe2+ → 1 2 bottom two depressions (spots 5 and 6) to the
two other spots in the column above them. This
will let you see which oxidation state (+2 or
+3) the iron is in when it is dissolved in
Fe3+ → 3 4 hydrochloric acid. You do two tests (i.e. one
with SCN- and one with [Fe(CN)6]3- to get a
more reliable answer, since matching these
colours is sometimes a challenge.
Fe/HCl → 5 6
Dispose of all waste
in the containers provided!
Figure 5: Wellplate setup for Procedure 10
Do not pour anything down the sink!
To the first row (spots 1 and 2), add two
drops of 0.01 M iron (II) ammonium sulfate
[NH4]2[Fe][SO4]2. To the second row (spots 3
and 4), add two drops of 0.01 M iron (III)
nitrate Fe(NO3)3.

SAMPLE DATA TABLE (Leave yourself lots of space when you copy this into your notebook!)

These tables will take 3-4 pages. Keep the following points in mind when making observations
throughout the experiment.

Observations:
i.e. colour, clarity, odour, and anything else that relates to sample appearance
Make separate observations of each starting material before beginning the experiment.
Make separate observations after each step of the procedure.
Make a final observation of the product(s) of any reaction(s).
Note any appearances, disappearances, or changes in colour, clarity, odour, etc,
as you observe them!

“Clear” and “colourless” do not describe the same thing!

You may abbreviate “clear and colourless” as “c & c”, if you desire!

26
Part A: Precipitates

Procedure 1: Solubility of Silver Salts

Reaction with AgNO3 (Don’t forget to describe this reagent as well!)
NaCl
NaBr Leave 2 lines between each reagent
KI to describe initial appearances
Na2SO4 and final products!
Na2CO3
NaOH

Procedure 2: Anions in Tap Water

Tap water
Distilled water Leave 2 lines between each reagent

Procedure 3: Solubility of Hydroxides

Mg(NO3)2
Ba(NO3)2 Leave 3 lines between each reagent
AgNO3 to describe reaction with NaOH
Fe(NO3)3 and any precipitate reactions
Co(NO3)2 with HNO3 (Describe these reagents as well!)
Cu(NO3)2

Part B: Acids and Bases

Procedure 4: Detection of Acidity or Basicity

pH paper colour pH paper value phenolphthalein

HCl _____________ _____________ _____________ Leave 1 line between
HNO3 _____________ _____________ _____________ each reagent
H2SO4 _____________ _____________ _____________
CH3COOH _____________ _____________ _____________
NaOH _____________ _____________ _____________
NH3 _____________ _____________ _____________

Procedure 5: Neutralization
3 M H2SO4 + 1 drop phenolphthalein + 3 M NaOH
0.1 M H2SO4 + 1 drop phenolphthalein + 0.1 M NaOH Leave 2 lines between each
0.1 M H2SO4 + 0.1 M NaOH

Part C: Gases

Procedure 6: Acids and Metals

HCl + Mg metal
HNO3 + Mg metal Leave 4 lines between each
H2SO4 + Mg metal
Procedure 7: Generating Oxygen
FeCl3 + H2O2 Leave 4 lines of space

27
Procedure 8: Other Gas-Producing Reactions

H2SO4 NaOH
Na2CO3 Leave 3 lines between
Na2SO3 each reagent
NH4Cl

Part D: Redox Reactions

Procedure 9: Redox Displacement

CuCl2 + Al metal Leave 4 lines of space
Procedure 10: Iron in Stomach Acid (HCl)

NH4SCN K3[Fe(CN)6]
[NH4]2[Fe][SO4]2 Leave 1 line
Fe(NO3)3 between formulas
Fe metal in HCl

28
 EXPERIMENT 3
Synthesis of Alum: KAl(SO4)2·12H2O

Pre-Lab Readings:
Appendix A: Significant Figures
Appendix B: Filtration

Hazard Table
aluminum foil May cause skin or eye irritation.
KOH – potassium hydroxide Corrosive. Harmful if swallowed.
H2SO4 – sulfuric acid Corrosive. May be fatal if ingested or inhaled. Possible
carcinogen if fumes or spray inhaled.
C2H5OH – ethanol Flammable. Irritant. Long-term exposure may cause liver,
kidney, or heart damage

Introduction The alum you will be preparing in this

experiment has the formula KAl(SO4)2·12H2O
Aluminum is the third most abundant and is commonly used in pickling, leather
element on the surface of the Earth and the tanning, and water purification.
single most abundant metal. Sir Humphrey
Davy, a British chemist and physicist, The key to preparing alum from aluminum
discovered the element in 1807. Though he foil is that you can take advantage of the
was unable to isolate it himself, he was first to amphoteric nature of one of the aluminum
dub it “alumium” after the Latin name salts. Remember that this means one of the
“alumen” for a substance drawn from a mineral salts produced in an intermediate step of the
of ancient times. reaction pathway will be able to behave as
either an acid or a base.
Five years later, he changed the element’s
official name to “aluminum” and later still, CONCEPTUALIZE! Write balanced equations
under encouragement from the Royal for the following steps of the reaction to
Chemical Society, to “aluminium” in order to synthesize alum:
keep with the traditional nomenclature of other
metals. Aluminium is now the preferred 1. Aluminum metal reacts with water to
spelling among many international chemical produce hydrogen gas and aluminum
societies, though its common spelling in North hydroxide, which is a white, insoluble
America lacks the second “i”. salt. It may appear grey if the
aluminum foil contains black
Alum is the name given to a family of impurities.
chemicals that share a similar “double salt”
formula. Whereas traditional salts contain one
cation and one anion, a double salt has more
than one type of either charged species in its
formula.

5th floor of Brock Library (Call # TN 775 C65) Cowles, A. The True Story of Aluminum; Henry Regnery
Company: Chicago, IL, 1958; pp 1-13.

29
 2. Aluminum hydroxide reacts with beaker with a watch glass to prevent fumes
potassium hydroxide to produce from filling the room. The aluminum should
soluble potassium ions and aluminate dissolve in about 30 minutes with periodic
ions Al(OH)4-. stirring with a glass rod. Filter off any black
impurities using gravity filtration.

The solution now contains K+, Al(OH)4-,

and excess OH-. Once it is cool enough to
touch the side of the beaker, slowly and
3. Aluminate ions combine with sulfuric carefully add 30.0 mL of 6.0 M H2SO4 while
acid to produce aluminum hydroxide stirring. Solid Al(OH)3 should appear, then
again, soluble SO42- ions, and water. It dissolve once more as the sulfuric acid is
should look like a white precipitate at added. Gently boil the solution until you are
this point. left with a volume of approximately 50 mL.

Let the solution sit at room temperature for

15 minutes before placing it on ice for a further
15 minutes. Add approximately 30 mL of
ethanol to a separate flask and place it on ice
4. As more sulfuric acid is added, as well.
aluminum hydroxide further reacts to
produce soluble Al3+ and SO42- ions Crystallization is perhaps as much an art
and water. as it is a science. Little disturbance and lots
of time will produce the largest and purest
crystals. Alum crystallizes easily as well-
formed octahedral crystals.

Filter the crystals using a Buchner funnel

5. Alum KAl(SO4)2·12H2O crystallizes and wash with two 10 mL portions of the
out when water is cooled enough to cooled alcohol. Draw air through the filter
cause the soluble ions (of which alum paper for 15 minutes to dry the crystals before
is made) to coalesce and precipitate out spreading them out on a paper towel to be
of solution. graded (for crystal size and dryness) while you
clean up.

Record the final weight of the alum crystals

to four decimal places. Hand in your crystals to
the demonstrator for grading.
Method
mass of alum
E1: % yield   100%
Weigh approximately 1.00 g of aluminum theoretical yield
foil on a top-loading balance and record the
weight to two decimal places. Quickly tear the
foil into pieces (no smaller than the tip of your
thumb) and place the foil in a 250 mL beaker.
Add 50.0 mL of 1.5 M KOH and cover the

30
SAMPLE DATA TABLE (Leave yourself lots of space when you copy this into your notebook!)

Wt. of aluminum foil _____________ g

Wt. of dry alum _____________ g

Observations:
i.e. colour, clarity, odour, and anything else that relates to sample appearance
Make separate observations of each starting material before beginning the experiment.
Make separate observations after each step of the procedure.
Make a final observation of the product(s) of any reaction(s).
Note any appearances, disappearances, or changes in colour, clarity, odour, etc,
as you observe them!

31
 EXPERIMENT 4
Determining the Formula of a Hydrate

Pre-Lab Readings:
Appendix A: Significant Figures

Hazard Table
There is no hazard table required for this experiment because you are only heating relatively
stable, solid materials.

Introduction The pentahydrate is stable to about 110°C,

at which point it decomposes to the
A hydrate is a chemical compound which monohydrate. Beyond 200°C the species is
consists of an ionic salt and some number of anhydrous, which loses SO3 and decomposes
water molecules. This is different from an ionic to CuO at 700°C.
salt dissolved in solution because the water
molecules in a hydrate are either bonded To write the formula of a hydrate, the
directly to a metal centre or have been convention is to show the number of water
incorporated into the solid crystal structure. molecules associated with one anhydrate
Water molecules in solution form (and are formula unit. The dot between the anhydrate
continuously reforming) hydrogen bonds and salt and the water molecules of the formula
dipole interactions with the ions they surround. denotes that the water is actually bonded to the
anhydrate.
Hydrates of different ionic salts can have
great variation in their composition and Many hydrates have an integral number of
stability. Some effloresce, or lose their water water molecules associated per molecule of
spontaneously to the atmosphere under ionic salt. This means that the number of water
standard conditions, and must be handled molecules is usually a small, whole number,
carefully to retain their structure. Others must like that of CuSO4·5H2O. There are, of course,
be strongly heated in order to liberate the water exceptions to this trend, as some hydrates have
molecules. Figure 1 shows the behaviour of stable forms consisting of some fraction of
copper (II) sulphate pentahydrate upon heating water molecules.
as an example.
If you are given a sample of hydrate, there
3.00 is no way of telling how much water is bonded
CuSO4·5H2O
2.50
to the salt by observation alone, since the solid
does not appear to be wet. By carefully heating
CuSO4·H2O
2.00
CuSO4 the sample at the correct temperature,
1.50
CuO however, most hydrates will lose their water
1.00 molecules and can be completely converted to
0.50
the anhydrous compound. This will result in a
loss of mass and the difference in the initial
0.00
0 200 400 600 800 1000
and final weights of the sample can be used to
determine the original formula for the hydrate.
Figure 1: Weight loss (g) of CuSO4·5H2O as
a function of temperature (°C)

32
 Method crucible to gently warm the hydrate.

Never touch the crucible with your Observe whether the solid dissolves in its
fingers after it has been heated! own water of hydration by peeking through the
Use tongs! partly open lid. If you do notice this
observation, you will need to continue heating
The crucible and lid are made of very your sample very gently (to avoid splattering
porous material that will absorb water from your sample all over the place) and place the
your skin and cause major error in your crucible in a dessicator to cool (to avoid
calculations. absorbing too much moisture from the air). If
your hydrate does not dissolve, increase heat
Following the setup shown in Figure 2, heat moderately until the bottom of the crucible
a crucible for 15 minutes using a Fisher burner glows a slight red.
with the lid slightly ajar. Turn off the flame,
close the lid, and allow the crucible to cool for Heat the solid for 15 minutes (or 20
10 minutes. Record the weight of the cooled minutes if the salt partly dissolved), replace
crucible and lid to four decimal places. the lid, and allow the solid to cool for 10
minutes on a ceramic pad (or in a dessicator if
NOTICE! This has dried the crucible so that the salt partly dissolved). Make sure you
any water loss during future heating comes close the lid while cooling! Most dehydrated
only from the unknown hydrate sample. The compounds will deliquesce, or absorb water
lid must be left open slightly so that moisture from the atmosphere. Record the new weight
on the inside can escape. of the cooled crucible, lid, and now anhydrous
sample.
A: tongs
How do you know that you have removed
A
B: crucible all of the water in the original hydrate? If you
B with lid heat the sample again, no further water should
slightly ajar be lost and the weight should remain constant
after a second heating. Repeat the heating-
C: ring cooling cycle until two weights are within
C clamp 0.5% precision.
D
supporting
ceramic If you are having trouble obtaining a
Figure 2: Crucible setup precise weight, try cooling your sample in the
triangle
D: Fisher burner placement dessicator in case the crucible or sample is
(Bunsen burner shown) absorbing water from the atmosphere. If this
fails, you may not be allowing the sample to
Using an analytical balance, add cool for a long enough period of time. When
approximately 1.0 g of your unknown hydrate the crucible is warmer than the analytical
to the crucible and record the new weight of balance, the metal parts of the balance will
your crucible, lid, and hydrate to four decimal expand or tiny air currents in the chamber will
places. Replace the crucible (with lid slightly cause the weight to fluctuate.
ajar) on the heating apparatus and sweep the
flame back and forth across the bottom of the Solid material goes into waste containers!

33
 Obtain the correct anhydrate formula from your demonstrator before leaving the lab!
This is the only way you can receive a mark for accuracy!

SAMPLE DATA TABLE (Leave yourself lots of space when you copy this into your notebook!)

Unknown Letter: __________

First Heating Second Heating Third Heating

Wt. of crucible + lid + hydrate ___________ g
Wt. of crucible + lid ___________ g
Wt. of hydrate ___________ g
Wt. of crucible + lid + anhydrate ___________ g ___________ g
Wt. of crucible + lid ___________ g ___________ g
Wt. of anhydrate ___________ g ___________ g

Formula of Anhydrate: _______________

Observations:
i.e. colour, clarity, odour, and anything else that relates to sample appearance
Make a separate observation of your starting material before beginning the experiment.
Make a final observation of the product.
Note any appearances, disappearances, or changes in colour, clarity, odour, etc,
as you observe them!

34
 EXPERIMENT 5
Determining Vitamin Tablet Composition

Pre-Lab Readings:
Appendix A: Significant Figures
Appendix C: Volumetric Apparatuses

Hazard Table
KIO3 – potassium iodate Irritant. May cause skin or eye irritation. May be harmful if
swallowed.
KI – potassium iodide Irritant.
HCl – hydrochloric acid Corrosive. Harmful or fatal if inhaled or swallowed.
starch Low risk.

Introduction antioxidant, and as an enzyme cofactor in the

synthesis of many important biological
Long before it was chemically identified, chemicals, but it must be obtained through diet.
vitamin C played an important historical role. The majority of other animals and plants can
The disease known as scurvy caused manufacture their own vitamin C using
immobility, bleeding from the mucous glucose as a starting point.
membranes, and loss of teeth for centuries;
common among people who were unable to O

include vegetables or fruit in their diets. Sailors O

OH
and soldiers gone for long periods of isolation
often died of this disease. HO OH

In the 18th century, it was recognized that HO

the consumption of citrus fruits prevented Figure 1: Chemical structure of L-ascorbate
scurvy. Thus, when British sailors began to
carry limes on board their ships, scurvy was Some people take vitamin supplements in
eliminated, and the term “limey” was born order to ensure that they are getting the
(which refers to a British sailor). essential nutrients that they require. In this lab,
you will analyze a vitamin tablet to find out the
In 1937, Hungarian physiologist Albert exact amount of vitamin C it contains.
Szent-Györgyi was awarded the Nobel prize in Wouldn’t you want to know that you were
medicine for first isolating and characterizing getting all that was paid for?
vitamin C. Its chemical name is L-ascorbate
but it is more commonly referred to as ascorbic The key to this experiment is a redox
acid and the chemical structure is shown in reaction between vitamin C and iodine. It is
Figure 1. difficult, however, to make aqueous iodine
solutions with reliable concentrations. The
Vitamin C is probably one of the most well- iodine required for this redox will be supplied
known essential nutrients; a substance which is by another reaction between iodate (IO3-),
needed for the proper functioning of an iodide, and acid as shown in E1:
organism, but cannot be manufactured by that
organism. In humans, vitamin C is used as an E1: IO3- + 5 I- + 6 H+ → 3I2 + 3 H2O

35
 In your reaction flask, you will have a Never leave the flask open
dissolved vitamin tablet, potassium iodide, and for long periods of time!
hydrochloric acid, as well as a starch indicator. Vitamin C is oxidized by oxygen
This solution will be carefully titrated with (as well as by iodine).
iodate. According to E1, iodine will be
produced but will immediately react with the Obtain approximately 100 mL of KIO3
vitamin C by E2: solution provided.
O O Write down the exact concentration
O
OH
O
O in your notebook!
+ -
E2: HO + I2 → HO +2H +2I Rinse out a clean buret with two 10 mL
OH O
volumes of KIO3 before filling the buret with
HO HO
the same solution. Allow a tiny bit of solution
When all of the vitamin C has reacted, the to drain out the tip and force out any air
iodine that is generated no longer gets used up bubbles that are trapped. Take an initial buret
by the redox reaction and instead forms a dark reading.
blue complex with the starch.
Pipette 5.00 mL of vitamin C solution from
Method the volumetric flask into a 250 mL Erlenmeyer
flask. To this sample, add
Weigh a vitamin tablet to four decimal 5.0 mL of 0.6 M KI solution
places. Place the tablet in a 250 mL beaker and 5.0 mL of 1.0 M HCl
add approximately 50 mL of distilled water. 1.0 mL of starch indicator
Let the tablet sit for a few minutes to soften, using a graduated cylinder and swirl to mix.
then use a glass stirring rod to break up the
tablet and stir the solution until no visible Use proper technique to titrate the sample
chunks of tablet remain. The solution may still with KIO3. The endpoint is the first permanent
be cloudy. trace of blue colour that remains after 20
seconds of swirling. Repeat the procedure until
Use a funnel to quantitatively transfer the at least two trials are within 1.0% precision or
solution into a 100 mL volumetric flask. Rinse less.
the empty beaker with a small amount of water
from a wash bottle and add this liquid to the Discard of all solutions in the appropriate
flask. Slowly and carefully fill the volumetric waste containers. Do not pour anything down
flask to the calibration mark. Stopper the flask the sink!
and invert several times to uniformly mix the
vitamin C solution.

36
SAMPLE DATA TABLE (Leave yourself lots of space when you copy this into your notebook!)

Weight of vitamin C tablet: _________ g

Trial #1 Trial #2 Trial #3 Trial #4 Trial #5

Final buret reading _______ _______ _______ _______ _______
mL mL mL mL mL
Initial buret _______ _______ _______ _______ _______
reading mL mL mL mL mL
Volume of KIO3 _______ _______ _______ _______ _______
mL mL mL mL mL

Observations:
i.e. colour, clarity, odour, and anything else that relates to sample appearance
Make separate observations of each starting material before beginning the experiment.
Make a final observation of the product(s) of any reaction(s).
Note any appearances, disappearances, or changes in colour, clarity, odour, etc,
as you observe them!

37
 APPENDIX A
Significant Figures
No measuring instrument is perfectly Addition and Subtraction
accurate, and every measured quantity reflects
some degree of uncertainty. If you use several Addition or subtraction calculations are
measurements in a single calculation, you can limited by the number of decimal places in the
only be as accurate as your least reliable given set of values.
measurement. Do not try to be more accurate e.g.
than your experimental data allows by simply 37.25 mL 4 s.f.
adding more decimal places! + 3.5 mL 2 s.f.
40.8 mL 3 s.f.
If a volume is recorded as 23.15 mL, this
implies that the 2, 3, and 1 are known with Multiplication and Division
certainty, and that the 5 is doubtful. The exact
volume actually lies somewhere in between Multiplication or division calculations are
23.14 mL and 23.16 mL. The last digit of any limited by the number of significant figures in the
measurement is always assumed to be given set of values.
estimated and uncertain! e.g.
2.024 mol/L 4 s.f.
Zero  2.50 L 3 s.f.
5.06 mol 3 s.f.
The zero is used both to represent a quantity
and to fix a decimal point. Rounding Rules

Examples to fix a decimal point: If the digit to be dropped is above 5, round the
0.1 mL 1 significant figure previous digit up.
0.002 mL 1 sig. fig. (e.g. 0.149 rounded to 2 s.f. becomes 0.15)
0.00501 mL 3 s.f.
0.005010 mL 4 s.f. If the digit to be dropped is below 5, leave the
previous digit as it is.
Examples to represent quantity: (e.g. 0.142 rounded to 2 s.f. becomes 0.14)
1600 mL 2 s.f.
1600.0 mL 5 s.f. If the digit to be dropped is 5, and there are
digits that follow, round the previous digit up.
Examples using scientific notation: (e.g. 0.1453 rounded to 2 s.f. becomes 0.15)
1.6  103 mL 2 s.f.
1.600  103 mL 4 s.f. If the digit to be dropped is 5, and there are no
Scientific notation is an extremely useful digits that follow, and the previous digit is even,
tool to avoid ambiguity! leave the previous digit as it is.
(e.g. 0.145 rounded to 2 s.f. becomes 0.14)
Conversion factors are exact numbers:
100 cm If the digit to be dropped is 5, and there are no
e.g.
1m digits that follow, and the previous digit is odd,
and should be ignored when considering the round the previous digit up.
following rules for calculations. (e.g. 0.155 rounded to 2 s.f. becomes 0.16)

38
 APPENDIX B
Filtration

Simple Filter Paper for Gravity Filtration

1. Take one dry piece of filter 2. Fold the filter paper in half. 3. Fold the filter paper in half
paper. again to form a circle quarter.

Note: Try not to crease any

filter paper folds too sharply
(for either method) as this
may cause tears or rips during
filtration.

4. Hold three of the four loose

edges together and pull the
fourth edge open to form a
cone. Place the cone into a
funnel.

Fluted Filter Paper for Gravity Filtration

1. Take one dry piece of filter 2. Fold the filter paper in half. 3. Unfold the filter paper and
paper. fold in half again to make a
crosshair pattern.

39
4. Fold one of the circle 5. Repeat the same type of 6. Hold one of the four newly
quarters in half so that the new fold with each of the formed peaks and gently
crease points in the opposite remaining three quarters of squash it flat against the rest
direction of each other fold. the filter paper. of the filter paper.

Note: While this method

may seem complicated, the
increased surface area
provided by fluting the filter
paper significantly speeds up
the amount of time required
for gravity filtration.

7. Point the two new peaks 8. Complete fluting by

away from the rest of the filter repeating steps 6 and 7 on the
paper. One quarter of this remaining three quarters of
piece of filter paper is now the filter paper.
properly fluted.

Notes on Gravity Filtration □ Place the dry, folded filter paper in a

glass funnel and moisten it with the
solvent you will be using to rinse with.

□ You may want to pour all solutions

down a glass rod to avoid spilling and
losing your product.

□ Make sure the end of the funnel is well

below the opening of the flask or
beaker that is catching the liquid
portion as it flows through the filter
paper.

□ Use a rubber policeman to scrape any

solids into the funnel for rinsing.

□ It is always better to rinse with several

smaller volumes than one larger
volume.
Notes on Suction Filtration □ Place a small round circle of filter
paper inside the Buchner funnel and

40
 moisten it with the solvent you will be
using to rinse with.

□ Turn on the faucet as far as it will go

A to receive maximum suction.
B
□ All of the notes on gravity filtration
apply to suction filtration as well.

The following experimental errors can arise

C even when you do a filtration as carefully and
correctly as possible:
A: rubber hose connected to aspirator on sink
1. Precipitates may be left on the sides of
B: Buchner funnel with rubber adapter glassware, stirring rods, and filter
paper.
C: filtration flask with sidearm
2. Solvent may remain on the precipitate
and filter paper.

3. Some product is lost because of its

solubility in the solvent.

41
 APPENDIX C
Volumetric Apparatuses

As a chemist, you have at your disposal a dissolve the solute without over-filling the flask.
wide variety of glassware to use when Swirl the solution until it is mixed completely,
measuring volumes of liquid. Some are more then slowly add solvent until the meniscus is close
accurate than others and it is up to you to decide to the calibration mark. Add the last bit of solvent
the degree of accuracy required by your one drop at a time to ensure that the bottom of the
measurement. If you have to measure 500 mL meniscus lies exactly on the line.
of solution, using a beaker to transfer the
volume all at once (with a poor accuracy of If the solution sits for any length of time before
±5%) might be more appealing than making use, it should be re-mixed by securing the stopper
many more measurements using a 50 mL and inverting the flask several times.
graduated cylinder (with a higher accuracy of
±0.1 mL). Pipettes

Volumetric Flasks

Pipettes are calibrated to deliver an exact,

known volume. The ones shown here have a single
Volumetric flasks are calibrated to hold an calibration line at 50, 10, and 5 mL respectively,
exact, known volume. The one shown here has which means that when the pipette is filled up to
a single calibration line at 100 mL, which that line, it contains 50 mL (±0.05 mL), 10 mL
means that when the flask is filled up to that (±0.02 mL), or 5 mL (±0.01 mL) of solution. To
line, you have made 100 mL (±0.08 mL) of ensure an accurate delivery, follow these steps
solution. when using a pipette:

To make a solution using a volumetric flask, 1. Use a pipette bulb. Squeeze as much
first transfer quantitatively the desired solute to
your clean, dry glassware. Then add just
enough solvent to the flask to completely

42
 air out of the bulb as you are able. Just
barely slip the bulb onto the blunt end
of the pipette so it will be easy to
remove quickly. Insert the tip of the
pipette into the desired liquid and □ Always thoroughly rinse the buret with tap
gradually release your grip on the bulb. water, then distilled water, and two rinses
with the solution to be delivered by the
2. When the liquid rises above the buret. Make sure each rinse comes in
calibration mark, slip the bulb off and contact with all of the inner surfaces of the
quickly cover the opening of the pipette buret by holding it horizontally and
with your thumb or finger before the rotating the glassware with your fingertips
liquid level drops below the line. before it is passed through the buret tip
into a waste container.
3. Remove the pipette from the liquid and
touch the tip against the wall of a □ With the stopcock closed, fill the buret
beaker. Very carefully allow the liquid with solution, using a clean, dry funnel if
level to fall just until the bottom of the necessary. Pass a tiny bit of solution
meniscus is level with the calibration through the tip of the buret and eliminate
mark. any air bubbles in the stem by flicking the
glass gently. Top up the liquid level in the
4. Allow the pipette to drain by gravity buret until it is just below zero.
into your desired container. Touch the
tip of the pipette to the side of the □ Allow the buret contents to settle for 15
container but DO NOT try to blow out seconds before taking a reading. Make all
the last drop from the pipette! The measurements to the nearest 0.01 mL. Be
pipettes you use are calibrated TD (to sure that the meniscus (the curved surface
deliver) and takes this leftover liquid of the solution in the buret) is at eye-level
into account already. to avoid reading error due to parallax. Use
a meniscus reader (a dark line drawn on a
Try not to draw any liquid into the bulb. If piece of paper) to avoid incorrectly
this should happen, rinse the bulb carefully judging the bottom of the meniscus.
with tap water, then distilled water, and allow
it to drain for several minutes.

Burets

Burets are calibrated to deliver an exact,

known volume up to a maximum of 50 mL
(±0.06 mL) and the volume delivered can vary
from measurement to measurement. While the
lines marked on the buret are for every 0.1 mL,
the volume should be read to the nearest 0.01
mL using your own interpolation. Keep the 14.92 mL *** 14.98 mL ***
following points in mind while working with a
buret:

To use a meniscus reader, make sure that between the initial and final volumes of the
you are eye-level with the surface of the buret.
solution. Hold the meniscus reader behind the
43
buret and well below the meniscus. Slowly □ Always do at least three sample titrations
raise the dark line until you notice the very and do the first titration quickly to get a
bottom of the meniscus turn dark and visible. rough idea of how much titrant solution it
The lowest part that you can get highlighted is will take (since you will likely over-shoot
the very bottom of the meniscus. the first endpoint anyway). If you titrate
the smallest sample first, it will give you
Always remember that burets are read an idea about how much titrant you will
from 0.00 mL at the need for the other samples. If, after three
top to 50.00 mL at the bottom! samples, your precision is still too poor, do
more samples until you have at least two
□ Keep the tip of the buret well below the that are within an acceptable range.
top of the flask containing your sample
to be titrated. Do not dispense the titrant The following experimental errors can arise
solution from the buret too quickly or even when you do a titration as carefully and
you will over-shoot your endpoint. correctly as possible:
Place a piece of white paper underneath
the flask to make detecting a colour 1. Error in each volume measurement arises
change easier. Control the rate of flow from the estimation of the last digit and
with your off-hand (use your left to hold from the accuracy of the buret calibration
the stopcock if you are right-handed, during manufacturing.
use your right if you are left-handed)
and swirl your flask constantly with 2. Appearance of a coloured endpoint means
your free hand. a slight excess of one of the reactants.
Estimation of this endpoint introduces
some uncertainty in the results.

3. Non-qualitative transfer of reactants into

the flask can be minimized but not
eliminated.

□ As the endpoint draws nearer, the

colour change in the flask will persist
for a longer period of time. Stop the
addition of titrant and rinse down the
walls of the flask and the tip of the buret
with distilled water from a wash bottle.
Add titrant solution one drop at a time
with thorough mixing until the colour
persists for more than 20 seconds. This
is your endpoint. Calculate the total
amount of solution required for the
titration as a difference

44
 APPENDIX D
Graphing

A graph is a useful tool to visualize an 4. Label the axes with the name of the
average trend in data measurements, since each variable as well as the units used.
individual measurement taken during an i.e. volume of water (mL)
experiment has some error associated with it
and there is no way to tell which measurement 5. Draw a line of best fit (Only if it is a
is the most accurate in the series. linear relationship)
6. using a ruler so that roughly equal
One of the most common ways to convert numbers of data points are above and
data into a graph is to measure how one below the line, and the distances from
variable (y) is dependent on another (x) to form the data points to the line are as small
a series of ordered pairs (x,y). When this as possible.
relationship is linear, it is easy to average the i.e. it does not matter how many
data using the familiar linear equation points the line actually passes through.
y  mx  b
where m is the slope, and b is the intercept 7. If one of your variables is time, always
(both of these values often have important start at t = 0 on that axis.
physical implications)
8. Show a table of all the values used to
In this course, you will use the following construct a graph somewhere in your
rules for constructing graphs: report.

1. Take up as much of the page with data 9. Draw all scales, points, lines, and labels
points as possible, so choose an neatly and legibly with a sharp pencil
appropriate scale to do so. or fine-tipped pen.
i.e. if all of your data is between 12
and 18 on one scale, start numbering at 10 and
choose a scale unit which allows you to use up
lots of space and end at 20

2. Plot the independent variable on the x-

axis and the dependent variable on the
y-axis.
i.e. mark the x-axis horizontally and
the y-axis vertically

3. Give your graph a title.

i.e. “y as a function of x” or “y vs. x”

45
 HANDY SHEET

Fundamental Constants

Avogadro’s Number NA 6.022  10 23

Velocity of Light in a Vacuum c 2.9979  108 m / s
Atomic Mass Unit amu 1.6606  10 24 g
Gas Constant R 0.08206 L  atm / mol  K
8.3145 J / mol  K
Absolute Zero To  273.15 K
Standard Temperature T 0 C 273.15 K 
Standard Pressure P 1 atm
Pi π 3.1416
Base for Natural Logarithms e 2.7183

Commonly Used Conversion Factors

Length 1 Angstrom Å   10 8 cm Volume 1 L  1000 mL

1 micron    10 4 cm 1 mL  1 cm 3

Mass 1 kg  1000 g Energy 1 cal  4.184 J

1 g  1000 mg 1 L  atm  0.103 kJ

Pressure 1 atm  760 mmHg Other lnx   2.303 logx 

1 atm  1.01325  105 Pa K 
K  C  273.15 C  
1 torr  1 mmHg  C 

Prefixes Used with SI Units

Tera Giga Mega Kilo Deci Centi Milli Micro Nano Pico
(T) (G) (M) (K) (d) (c) (m) (μ) (n) (p)
1 2 3 6 9
10 12
10 9
10 6
10 3
10 10 10 10 10 10 12

46
 Systematic vs. Gross Sources of Error
Or “Why Didn’t I get 100% Yield?”

actual yield
% yield   100%
theoretical yield

Systematic Errors Gross Errors

These errors are inherent in the techniques. These errors are an indication of sloppy lab
They can be minimized, but never completely work. They can be completely eliminated by
eliminated. Techniques and measurements are carrying out techniques and measurements in a
as accurate as the experiment and instruments careful manner. If you are asked to list
can be. sources of error, never include gross errors!

Examples Examples

□ Product left on filter paper □ Product spilled on countertop

□ Product slightly soluble in solution □ Use of dirty glassware
□ Uncertainty in last digit of a □ Incorrect reading of measurements
measurement DO NOT CITE THESE ERRORS!

Precision vs. Accuracy

Precision: How well do your trial results

agree with each other? If you do not
change any of the variables between the % precision 
high value  low value   100%
trials, do you get similar results? Use this average of all values
equation to determine just how precise
your technique is.

Accuracy: Does your experimental value

match the one popularly accepted in the
literature? How closely can you replicate average value  true value
% accuracy   100%
the results of the classical chemistry true value
masters? Use this equation to determine
just how accurate your technique is.

47
 PERIODIC TABLE

1A 8A
1 18
1 2
H 2A 3A 4A 5A 6A 7A He
1.0079 2 13 14 15 16 17 4.0026
3 4 5 6 7 8 9 10
Li Be B C N O F Ne
6.941 9.0122 10.811 12.011 14.0067 15.9994 18.9984 20.1797
11 12 13 14 15 16 17 18
Na Mg 3B 4B 5B 6B 7B 8B 8B 8B 1B 2B Al Si P S Cl Ar
22.9898 24.3050 3 4 5 6 7 8 9 10 11 12 26.9815 28.0855 30.9738 32.066 35.4527 39.948
19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35 36
K Ca Sc Ti V Cr Mn Fe Co Ni Cu Zn Ga Ge As Se Br Kr
39.0983 40.078 44.9559 47.88 50.9415 51.9961 54.9380 55.847 58.9332 58.69 63.546 65.39 69.723 72.61 74.9216 78.96 79.904 83.80
37 38 39 40 41 42 43 44 45 46 47 48 49 50 51 52 53 54
Rb Sr Y Zr Nb Mo Tc Ru Rh Pd Ag Cd In Sn Sb Te I Xe
85.4678 87.62 88.9059 91.224 92.9064 95.94 (98) 101.07 102.905 106.42 107.868 112.411 114.82 118.710 121.75 127.60 126.904 131.29
55 56 57 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86
Cs Ba La* Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn
132.905 137.327 138.905 178.49 180.948 183.85 186.207 190.2 192.22 195.08 196.966 200.59 204.383 207.2 208.980 (209) (210) 222
87 88 89
Fr Ra Ac**
(223) (226) (227)

58 59 60 61 62 63 64 65 66 67 68 69 70 71
* Lanthanide Series Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu
140.115 140.908 144.24 (145) 150.36 151.965 157.25 158.925 162.50 164.930 167.26 168.934 173.04 174.967
90 91 92 93 94 95 96 97 98 99 100 101 102 103
**Actinide Series Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr
232.038 231.036 238.029 (237) (244) (243) (247) (247) (251) (252) (257) (258) (259) (260)

48