CHEM 1010 Lab Manual F23

CHEM 1010U Laboratory Manual
Fall 2023
Senior Laboratory Instructor:
Richard Bartholomew
UA 3071
richard.bartholomew@uoit.ca
Table of Contents
DEDICATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii
LABORATORY CALENDAR. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
INTRODUCTION. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
LABORATORY ATTENDANCE AND REPORT SUBMISSION POLICIES . . . . . . . . . . . . . . 3
WHMIS AND LABORATORY SAFETY TRAINING. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6
SAFETY RULES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
SAFETY PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
GOOD LABORATORY PRACTICE. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17
SAFETY ACKNOWLEDGEMENT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21
LABORATORY REPORTS. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
SIGNIFICANT FIGURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
LABORATORY REPORT RECEIPT SHEET . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36
MISSED EXPERIMENTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
ANALYTICAL CHEMISTRY TECHNIQUES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

Weighing Techniques . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
Volumetric Techniques. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
Preparation of a Standard Solution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 53
Suction Filtration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
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Genesys20 Spectrophotometer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
Seven-Easy pH Meter . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
MICROSOFT EXCEL - AN INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61
LOCKER EQUIPMENT LIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78
1. LABORATORY SAFETY AND ORIENTATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
2. DETERMINATION OF STOICHIOMETRY BY TITRATION . . . . . . . . . . . . . . . . . . . . . . . 94
3. ANALYSIS OF AN ALKALI METAL CARBONATE BY BACK TITRATION OF

HYDROCHLORIC ACID . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
4. SYNTHESIS OF MALEIC ACID AND CONVERSION TO FUMARIC ACID.. . . . . . . . . 122
5. MEASUREMENT OF THE IDEAL GAS CONSTANT, ‘R’ . . . . . . . . . . . . . . . . . . . . . . . . 139
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DEDICATION
The CHEM 1010 laboratory manual is dedicated to the first UOIT (as it was then!) honours
chemistry graduates, who completed their degrees in May, 2007. They took a leap of faith and
travelled a long and sometimes bumpy road.
Tara Andrusiak
Laura Beckford
Laura Benninger
Katey Jakins
Aliaksei Shkarupin
And for those honours chemistry graduates who followed:
Class of 2008 Class of 2010 Class of 2011 Class of 2012

Lori Van Belle Jesse Allan John Austria Laura Duffin
Patrick Edge Chris Branco Chris McKim
Class of 2009 Matt Feeney Jillian Fischer Stuart McNelles
Faine Briscoe Wei Gong Nick Fougere Bhumika Modi
Jennie Eastcott Ken Johnson Giti Gunarajah Allan Nixon
Gurpaul Kochhar Shumail Kamal Shannon Hill Emily Palmer
Stephanie Mavilla Nadine Long Xuyen Hoang
Amanda Northcott Brad Marquardt Fazil Momand
Allen Pauric Kathryn Navarro Maya Saikali
Holly Wrathall Olga Palazhchenko Ashley Yabut
Andrew Pedersen Kaitlyn Yarrow
Melissa Stogran
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Class of 2013 Nadia Laschuk Nawid Safi Class of 2018
Matthew Baxter Michelle Pacheco Noor Ul-Huda Renata Barichello
Heather Cornwell Aayushi Patel Matthew Visentin Emily Barsanti
Neil Grenade Krishentus Arden Ward Yonas Berhane
Pathinather
Areeba Naheed Jessica Pauze Alyssa White Neelam Brahmbhatt
O’Rian Reid Gregory Ramsaroop Class of 2017 Clarissa Chau
Denise Rowsell Blake Roberts Jesse Campbell Rachel Comia
Cassandra Scott Sara Tucker Dion Chang Ryan Dwyer
Cassandra Taylor Fahima Umarwadia Adam Cook Maryam Ferhad
Nick-Hugh Wisdom Shontelle Van Maajida Darsot Dana Frackelton
Norman
Class of 2014 Class of 2016 Jacquelyn Egan Allison Jones
Bryce Cochrane Simarpreet Aashat Holly Fruehwald Manpreet Kaur
Tanya Fernandes Ramla Ali Heather Geoffrey Sin On Lai
Kayla Fisher William Asomaning Scott Gillis Carter Lapointe
Waleed Nusrat Valerie Bartlett Dylan Harris Krysta Mowers
Thiviya Veronica Cavallari Lucas Hynes Chase Murdoch
Pathmanathan
Gobishankar Stephanie Dagg Michael Leschinsky Jade Poisson
Sooriyakumar
Gurinder Virdi Yash Desai Brittany Loxton Robert Potter
Class of 2015 Davin Florent Aamir Navivala Donna Riel
Jocelyn Anderson Golnaz Ghoncheh Jonell Pearson Anna Starzyk
Megan Cearns Haitham Mohamed Michaela Phillips Jun Zhang
Sydney Cobourn Ifedi Orizu David Raveenthrajan
Kalaina Johnson Stefan Ramkissoon Samantha Thomas
Charmy Kantawala Zhiying Ren Inas Yusuf
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Class 2019 Class of 2020 Class of 2021
Rana Ahmad Muna Abdulaziz Dalia Alaboudi
Paola Canas Hind Al-Shamali Xin Chen
Alexandra Deckert Mona Almaghrabi Marco Chiu
Sabrina Ebenreth Bilal Bhatti Connor Clark
Fatma Faiez Keenan Black-Araujo Sarah Davenport
Charlene Fernandez Saranie Elamurukan Earl Dela Cruz
Ifrodet Giorgees Laura Gaitan Rojas Isabelle Allensy Erasquin
Samantha Herbert Nada Hassan Rony Gantous
Kamisha Hinds Andrew Hynes Mackenzie Gfroerer-Priede
Kevin Mariscal Asim Khalid Megan Hutton
PJ Mazzonna Mahnaz Khan Roxana Irimus
Jil Patel Farhan Mohamed Sujani Kaneshamoorthy
Nora Rayappoo Adaobi Obua Stephen Kerr
James Regush Omik Patel George Lagos
Mursal Sadat Nigel Pereira Mary-Kate Marren
Nargas Sadat Raquel Simpson Peter Melino
Pragash Senathirajah Cathy-Colette Tanya Thien Nguyen
Liam Stocks Ashaleni Tharmarajah Mopinsun Sivapalasingam
Mason Sullivan Nandalall Tularam Ashaleni Tharmarajah
Sulaiman Torakhel Ali Usaid Dimitrios Vernezos
Kayla Treflik Mansi Vyas Jireh-Eirene Viera
Michael Ziarno Yuwei Wang
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Class of 2022 Class of 2023
Rashad Adem Mackenzie Bell
Ahmad Alhendi Adam Blair
David Goh Arsala Butt
Vineththa Jeyanesan Jessica Cleghorn
Fanqi Kong Thinuri De Silva
Emily Laird Vittoria-Ann Di Palo
Huiwan Liu Sandy El Badaoui
Yueshudeng Luo Gobe Ele
Chyna Mercer Maria Garcia
Katherine Nguyen Stephanie Gunpat
Samuel Payne Wasee Intemas
Joshua Pereira Kyle La Salle
Brian Persaud Sabrina Lukes
Connor Pettigrew Jaiden Panchal
Raymond Sarju
Hira Shoaib
Guanxin Zuo
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LABORATORY CALENDAR
Fall 2023
Laboratories begin the week of September 12. The exact dates of your laboratory periods
depend on the CRN in which you are registered. These dates can be found on your MyOntariotech
schedule or on the preview of available courses on MyOntariotech:
View Available Courses (click “Search for Courses” and make the appropriate selections).
Dates Experiment
September 12 - 22 1 - Laboratory Safety and Orientation
September 26 - October 6 2 - Determination of Stoichiometry by Titration
October 10 - 13 Reading Week - no experiments. No reports due.
October 17 - 27 3 - Analysis of an Alkali Metal Carbonate by Back Titration of
Hydrochloric Acid.
October 31 - November 1 4 -Synthesis of Maleic Acid and Conversion to Fumaric Acid.
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November 14 - 24 5 - Measurement of the Ideal Gas Constant, “R”
Experiments are performed in UA 3420 or UA 3480. The room depends on the CRN in
which you are registered.
Note: the report for experiment 5 is due at the end of the laboratory period.
Be sure you use the current version of the laboratory manual for all aspects of preparation
for experiments and writing your reports. The laboratory manual changes from year to year
sometimes in small, but significant ways.
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INTRODUCTION
CHEM 1010U and CHEM 1020U are two general chemistry courses that cover chemistry
in very broad strokes (there is much more to learn!) giving students exposure to almost all the major
sub-disciplines of chemistry: physical and analytical chemistry and organic and inorganic chemistry.
The experiments in the laboratory portions of the two courses reflect this broad approach.
At its very heart chemistry is an experimental science. No theory can really be said to be
“true” until its validity had been tested by experiment. Progress in chemistry relies on good
laboratory work. Clever experimental design and execution, good technique, and careful observation
are required. These skills are developed by doing experiments and your journey to laboratory
proficiency begins in the first-year laboratories!
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Ontario Tech University Chemistry, F23; Policies - 8.9
LABORATORY ATTENDANCE AND REPORT SUBMISSION

POLICIES
Attendance at laboratory periods and submission of laboratory reports are compulsory.

Failure to attend a laboratory period or to submit a report for the experiment may result in a grade
of zero for the work. A student who fails to attend more than TWO (2) laboratory periods or fails
to submit more than TWO (2) laboratory reports will not receive credit for the laboratory portion
of the course. This may result in failure of the course. If you miss a laboratory period for any
reason, please read the “Missed Experiments” section of the laboratory manual and follow the
instructions there.
The date of the first experiment is given in the “Laboratory Calendar” and in announcements
made on Canvas. Do not assume the start date for experiments in this chemistry course is the same
as the start date in any other course at the university. Courses operate completely independently of
each other.
Students must arrive on time at the start of the laboratory period to receive instructions about
safe conduct of the experiments. Students who arrive more than 10 minutes late will not be allowed
to perform the experiment at that time. Students arriving less than 10 minutes late to a laboratory
period will be admitted at the discretion of the teaching assistant. If you are forbidden from
performing an experiment because of lateness, please read the “Missed Experiments” section of the
laboratory manual and follow the instructions there.
Details about laboratory reports (format, deadlines, etc.) are given in the “Laboratory
Reports” section of this manual. Please read that section carefully. Note: even if you work with a
partner (or in a group), you must still submit your own, distinct report. There are no “group” reports.
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When you submit your laboratory report be sure to have the teaching assistant (or whomever
receives your report) sign your “Laboratory Report Receipt Sheet”; it is your proof that you
submitted your report and if the report is lost, you can use the receipt sheet to demonstrate that you
submitted the report. In circumstances in which the report is lost and the Laboratory Report Receipt
Sheet has been signed, the final laboratory grade will be calculated based on the marks for the
remaining laboratory reports. If the Laboratory Report Receipt Sheet has not been signed and the
report is lost, a mark of zero will be recorded. It is your responsibility to have the receipt sheet
signed. If you are submitting reports on-line, you are responsible for ensuring the complete file is
submitted. Be aware that some mechanisms of electronic submission (e.g. Google Classroom) may
involve two steps (e.g. “upload” and “submit”) to complete the submission; you are responsible for
completing all steps and ensuring your report has been submitted. You are not required to submit
reports electronically - you may always submit them on paper.
In CHEM 1010U, 1020U, 1800U, 2030U and 2130U your marked laboratory report will
normally be returned to you by the start of the laboratory period following the submission of the
report. If your report is not returned to you at this time, confirm with your teaching assistant that TA
has it. This is particularly important if you submitted your report to someone other than your
teaching assistant. If you suspect your report is missing, you must alert the senior laboratory
instructor no more than three (3) working days after the laboratory period in which the report should
have been returned to you. Failure to inform the senior laboratory instructor of the missing report
by this deadline may result in a grade of zero for the laboratory report. You will be given access
(through a link posted on Canvas) to a Google sheet that reports your current grades. You should
review this document regularly for errors or omissions. If you find an error or omission in your
grades, you should alert the senior laboratory instructor immediately.
For CHEM 2040U, 3040U, 3530U, 3540U and 4040U, you will be given access to a Google
Sheet (through your ontariotechu.net account) that will report your current grades and whether a
report has been received but not yet marked. You should review this document regularly for errors.
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If you suspect your report is missing, you must alert the senior laboratory instructor no more than
three (3) working days after submission. Failure to inform the senior laboratory instructor of the
missing report by this deadline may result in a grade of zero for the laboratory report.
If you have suffered exceptional extenuating circumstances (e.g., grave personal misfortune,
acute mental health problems) which may prevent you from submitting a laboratory report on time,
you must contact the senior laboratory instructor no more than five (5) working days after the due
date for the laboratory report in order to be considered for a special accommodation. Documentation
may be required. All applications for such accommodations MUST be made by e-mail to the senior
laboratory instructor. No accommodations will be granted for late applications.
The percentage of the final mark of the course assigned to the laboratory component will be
decided by the professor teaching the course.
For the purposes of applying policies, procedures and deadlines / time-lines in this laboratory
manual a “working day” is defined as any day Ontario Tech University conducts normal business.
The days constituting “reading week” (in any semester) are considered “working days” with the
exception of the days listed below. The following days are not “working days”: all Saturdays and
Sundays, Family Day, Good Friday, Victoria Day, Canada Day, Civic Holiday in August, Labour
Day, Thanksgiving, the days of the Christmas closure and other days the University may declare as
university holidays.
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Ontario Tech University Chemistry, F23; Safety Training - 7.7
WHMIS AND LABORATORY SAFETY TRAINING
WHMIS
“WHMIS” (workplace hazardous materials index system) is a system for assessing and
reporting the risks associated with dangerous materials. It also sets standards for labelling such
materials. Familiarity with WHMIS is a first step in chemical laboratory safety training.
All students working in chemistry laboratories should have completed on-line WHMIS
training before their first laboratory period. Currently, you can access the training through this
website:
WHMIS Training
You login by providing your Banner ID (or student number) and your network password. The
training will take about 30 minutes. To obtain your certificate return to the website, scroll down and
follow the link “Check here to view training record” – you will have to enter your login credentials
again – and you should see a list of all the university training you have completed. Click on your
WHMIS certificate and print a copy of it. Bring it to your first laboratory period to show to your
teaching assistant. Alternatively, you may create an electronic copy and email it to your TA. You
will be required to present this certificate at the first laboratory period for all subsequent chemistry
courses. You only need to complete the training once and it may be acceptable proof of WHMIS
training if you land a job with the University in the future.
Laboratory Safety Training (for students in CHEM 2040, third-year courses and CHEM 4040)
In addition to WHMIS training upper year chemistry students must complete the on-line
Laboratory Safety Training Module provided by the Ontario Tech University Joint Health and Safety
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Ontario Tech University Chemistry, F23; Safety Training - 7.7
Committee (JHSC) on the s2Learning.com platform. If you have already completed the training (in
another CHEM course), you do not have to repeat it. Simply bring your certificate as proof of
completion and show it to your instructor.
To complete the training, you must first register for it. To register go to:
Laboratory Safety Training
provide the required information, then click “Register”. You only register for the laboratory safety
training course once. Note your user name and password because you will need them if you need
to login to the safety training again.
After you register (or login to the system), select “My Learning” at the top of the screen, then
select “My Courses.” Click on “UOIT Lab Safety”, select the CURIE Lab Safety module, then click
the “Launch” button to begin the training.
To complete the training, you must pass the final quiz with a score of at least 90%. When
you have completed the training, click “Print Your Certificate” (at the lower left) to print or save
your certificate. Keep your certificate because you will be required to show it in future chemistry
courses. You only need to complete the training once.
If you need to return to the course, go to

https://s2universitysafety.com
and login by entering your username (or email address) and password to re-enter the system.
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Ontario Tech University Chemistry, F23; Safety -21.37
SAFETY RULES
Safety in the laboratory is of the utmost importance to your instructors and it must be to you
as well. Everybody’s safety depends on each student adhering to the safety rules and procedures
outlined in this manual. For first-year students, an introductory safety video is available on Canvas
for you to watch. The video may be a useful reminder to upper year students!
The following rules must be obeyed and will be rigorously enforced.
1. ALL students must wear safety goggles. For people with eyeglasses they must be worn over
regular glasses. This rule will be vigorously enforced.
2. Contact lenses should not be worn in the chemistry laboratory.
3. All students must wear a lab coat. Lab coats protect skin and clothing from chemicals. The
front of the lab coat must be buttoned while working in the laboratory. Cotton generally
provides better protection from fire than synthetic fibres; cotton / polyester blends may
provide greater protection from spills.
4. Open shoes or sandals are forbidden. They expose your feet to spilled chemicals. Footwear
must completely enclose the foot from ankle to toe.
5. Loose or bulky clothing presents a hazard and must not be worn in the laboratory.
6. Clothing that exposes large areas of the body (e.g. shorts, tank tops) must not be worn in the
laboratory.
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7. Long hair must be tied back. The simple rule: if it can be tied back, it must be tied back!
8. Aisles must be kept clear of boots, coats, knapsacks, etc.
9. Students must know the locations of:
a) fire extinguishers
b) eye wash stations
c) emergency showers
d) emergency exits
e) fire blanket
f) fire alarms
10. The eyewash stations, shower, fire blanket and fire extinguishers must not be obstructed.
11. Smoking, vaping, eating, gum-chewing, and drinking are all strictly forbidden in the
laboratory. Neither food nor drink may be brought into the laboratory. This includes water
bottles or canteens. These must be left outside the laboratory. Food and drink brought into
a laboratory may be inadvertently contaminated by toxic materials.
12. No experiment may be started without an instructor present and no student may enter the
laboratory without an instructor present. Unauthorized experiments are strictly forbidden.
Experiments must not be left unattended.
13. Never put broken glass in the regular garbage. To do so presents risks to cleaning staff.
Broken glass should be swept up with a dust pan and brush and disposed in the receptacle
for broken glass. ONLY broken glass should be placed in this container.
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14. When diluting acid be sure to add the acid to the water. Add the acid slowly and with plenty
of stirring. Diluting acids generates huge amounts of heat (it is a very exothermic process).
Keeping the water in excess allows this heat to be more effectively dissipated. If the heat is
not adequately dissipated, the rapid heating may cause the solution to be ejected from the
beaker, injuring the experimenter. If the acid is added to the water, the ejected solution will
be comparatively dilute and therefore less dangerous.
15. Organic solvents and inflammable or pyrophoric (igniting spontaneously when exposed to
air) reagents require special handling. They must be used in a fume hood.
16. NEVER, EVER pipette by mouth. Safety bulbs are provided for pipetting. When pipetting
by mouth, it is very easy to lift the tip of the pipette above the level of the liquid being
pipetted. As a result, solution will enter the mouth which may lead to poisoning or other
injury.
17. Never point the mouth of a test tube at yourself or others. This is especially true if the test
tube is being heated.
18. NEVER taste chemicals or solutions. Should you get any chemicals in your mouth, do not
swallow. Rinse your mouth thoroughly then consult an instructor.
19. If you must smell a chemical, waft the vapours toward your face with your hand. Do not
place the container directly under your nose - you may be overcome by the gas.
NOTE: Students who arrive for laboratories inappropriately dressed, who do not have a lab coat or
who do not have safety goggles may be forbidden from performing the experiment.
Students who violate the safety rules may be dismissed from the laboratory period. In such
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cases the student will be given a grade of zero for the laboratory report.
Safety Goggles
All students must wear safety goggles in the chemistry laboratories. This is in response to
accidents that have occurred because of the inadequacies of safety glasses.
Students often complain that safety goggles are uncomfortable and that they fog. These
problems can be alleviated (somewhat) by the way the goggles are worn. You should wear the
goggles with the strap near the top of the head (just behind the crown), so that they are not held too
tightly against the face. Many people wear safety goggles like swimming goggles with the strap
around the back of the head, behind the ears. The goggles then form a tight seal against the face
which is uncomfortable and increases fogging.
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SAFETY PROCEDURES
Fire
Fire is one of the most serious problems that may be faced in the chemistry laboratory. For
no other safety issue is the adage “an ounce of prevention is worth a pound of cure” more applicable.
For all fires, if time permits, turn off all services (burners, hot plates, water, etc.).
In the event of a small fire, use the fire extinguisher. Remove the pin by twisting and pulling
it out. Direct the nozzle of the extinguisher at the base of the fire, squeeze the trigger and sweep
back and forth across the base of the fire. Ensure that at all times you are between the fire and your
escape route. Small fires can rapidly and easily become large fires. If the fire cannot be safely
extinguished in 30 s, leave the room and activate the fire alarm. If in doubt, leave the room and
activate the fire alarm.
For large fires leave the room and activate the fire alarm. If in doubt, leave the room and
activate the fire alarm. The more time people have to escape the building the more likely they will
be successful. The last person out of the room must close the door – this is the single most effective
way to slow the spread of fire. Leave the building by the nearest exit and move well away from the
building. The teaching assistant should alert Security or a Fire Warden.
Clothing on Fire
DO NOT RUN! Wrap the victim in the fire blanket or use a cotton lab coat to smother the
flames. “Drop and Roll” is effective. The emergency shower can be used. Have someone call
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Security (x-2400) to get medical assistance.
Fire Alarm / Building Evacuation
Ontario Tech University uses a “two stage” fire alarm system. The first stage is a warning
that there may be an emergency in the building. In the first stage the fire alarm rings at a rate of ~30
rings per minute. At the first stage of the alarm, stop all your experiments when it is safe and
convenient to do so and prepare to leave the building. Await further instructions. If the fire alarm
progresses to the second stage (louder, more frequent alarm), immediately stop all experiments.
Note: the fire alarm may not have a stage one; it may sound immediately at stage two. Turn off all
services (gas, electricity, water, etc.). Before leaving the laboratory make sure the hallway is free
of smoke and fire. If it is, leave the laboratory and exit the building by the quickest route (see
below). Close the door to the laboratory. Once outside, move away from the building and assemble
at the meeting points given below. The meeting point in UB is the western end of the first floor
atrium. If UB is closed, meet in the car park immediately to the east of UA (Founders 1). Your TA
will do a headcount to ensure everyone is out. Do NOT wander away without telling your TA!
Under no circumstances should you return to the building until told by the fire department that it is
safe.
If you are unable to leave the laboratory because of smoke in the hallway, you should close
the door and line the bottom of the door with lab coats that have been soaked with water. This will
reduce the amount of smoke entering the room. Call Security (x - 2400) to let them know where you
are and that you are trapped.
University authorities may order the evacuation of university buildings for reasons other than
for fire. Under such circumstances you should follow the instructions from Security without delay.
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Evacuation Routes from Laboratories
In the event of fire, do not use the elevators. People who are unable to use the stairs should
wait at the designated safety zones (indicated with red carpet or red tape) for assistance. The
designated safety zones are near the stairwells.
Room Primary Escape Secondary Escape

Instrument Turn right, descend staircase at Turn left, descend staircase at the northeast
Room, UA southeast corner of building. Exit corner of the building. Exit by the north
3402 building by southeast entrance. doors. Assemble in UB atrium.
Assemble in Founders 1 car park.
UA 3420 Turn left, descend staircase at Turn right, then left along southern
northwest corner of atrium. Exit corridor. Descend staircase at southeast
building by north doors. corner of building. Exit building by doors
Assemble in UB atrium. at southeast corner. Assemble in Founders
1 car park.
UA 3480 Turn left, descend staircase at Go straight along southern corridor.
northwest corner of atrium. Exit Descend staircase at southeast corner of
building by north doors. building. Exit building by doors at
Assemble in UB atrium. southeast corner. Assemble in Founders 1
car park.
UA 3520 Turn right, descend staircase at Turn left, then right along western
southeast corner of building. Exit corridor. Descend staircase at northwest
building by southeast entrance. corner of atrium. Exit building by north
Assemble in Founders 1 car park. doors. Assemble in UB atrium.
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Room Primary Escape Secondary Escape

UA 3680 Turn right, descend staircase at the Turn left, descend staircase at southeast
northeast corner of the building. corner of building. Exit building by
Exit by the north doors. Assemble southeast entrance. Assemble in Founders
in UB atrium. 1 car park.
Medical Situations
Ontario Tech University maintains a service called the Campus Emergency Response Team
(CERT). CERT is staffed by volunteers who have had extensive first aid training. If CERT
assistance is required, call Security (x-2400); they will dispatch a team.
Pregnancy
If you are, think you may be or are planning to become pregnant, you should be aware that
the risks to a mother and a developing foetus from the chemicals used in these laboratories are
generally unknown. You may wish to consider deferring this course until after your baby has been
born. If you decide to take this course, consultation with your family doctor is strongly encouraged.
If you would like the Safety Data Sheets for the chemicals in this course, they will be provided.
Fainting
If at any time you feel light-headed, dizzy or that you may faint, immediately sit down on the
floor. Fainting itself is rarely harmful; falling because of it may cause injury. Call for medical
assistance. If someone should faint, try to assess whether they have been injured by the fall. Make
them as comfortable as possible and call for medical assistance.
15
Cuts
Minor cuts should be treated with plenty of cool water. Ensure no foreign objects are present
(such as glass) and apply an appropriate dressing. Seek medical attention at the campus health clinic.
For more serious cuts the victim should sit or lie down and keep the cut elevated. Bleeding
should be kept to a minimum by applying direct pressure (assuming no foreign objects are present
in the wound). Call for Security (x - 2400) for emergency medical assistance.
Burns
Burns can be either thermal (caused by heat) or chemical. In both cases the first step is to
apply plenty of cool water. If the chemical reacts with water, remove it by brushing it from the skin.
If necessary, seek medical attention.
Allergies and Other Pre-existing Conditions
If you suffer from severe allergies or other pre-existing medical conditions such as epilepsy,
diabetes, etc, it may be helpful, but not required, to alert your instructor(s) and to advise them of any
necessary precautions or first-aid treatment.
16
GOOD LABORATORY PRACTICE
1. Use clean equipment. Dirty apparatus can lead to poor results (and poor grades!) or to
unexpected and potentially dangerous reactions. Beakers and flasks can be cleaned with soap
and water followed by thorough rinsing with tap water and deionized water. Soap should be
avoided when cleaning volumetric glassware such as pipettes, burettes and volumetric flasks
because it can be difficult to remove completely.
2. Once a chemical or reagent has been removed from its original container it must NEVER
be returned to the container. To do so risks contaminating the entire stock and thereby
ruining the experiments of others. If you have excess, it is cheaper to throw it away
(appropriately) or share it with another student, than to risk contaminating the stock.
3. Chemicals are expensive and solutions can be time consuming to prepare. DO NOT
WASTE CHEMICALS. Read the manual very carefully and take only what you need.
4. Carefully read the labels of reagent bottles to ensure you are getting the right chemicals. Be
sure to properly label apparatus containing chemicals or solutions. Accidents may result
from the erroneous mixing of chemicals.
5. Remember to re-cap reagent bottles immediately after use. This prevents the waste of
chemicals by contamination and spillage. Do not allow caps to become contaminated
through contact with the bench top or with other chemicals.
6. Do not remove reagent bottles to your benches. This unnecessarily frustrates and delays
other students.
17
7. Certain chemicals used in these laboratories are hazardous or present an environmental risk.
Dispose of these chemicals in the appropriate waste containers.
8. Set up apparatus so that it is well back from the edge of the bench. All services (gas taps,
water taps, electrical outlets, etc.) should be readily accessible.
9. Keep your work area clean, tidy and well-organized. Cluttered work areas can lead to
accidents. Clean up all spills quickly. At the end of the laboratory period clean your work
area.
10. Do not dispose of solid or insoluble materials in the sinks. Doing so inevitably leads to clogs
of the plumbing and to floods.
11. Large spills of acids and bases can be treated with the appropriate spill kit. Afterwards the
bench should be washed with plenty of cold water.
12. Mercury spills should be cleaned up immediately. The vapour from mercury is quite toxic.
Mercury spills are often treated with powdered sulphur which reacts with the mercury to
form mercury sulphide. The resulting solid is collected and treated as chemical waste.
13. Do not wander aimlessly in the laboratory.
14. Never interfere with the work of other students unless that work presents an immediate
danger to yourself or to others.
15. At the end of the laboratory period clean all equipment and return it to its appropriate place.
16. If solutions or samples must be stored, they must be properly labelled. At a minimum the
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label must include: i) all the chemical species present and their concentrations; ii) the solvent
(when applicable); iii) the date the material was stored and iv) your name. Additional
information that should be on the label is: v) the course; vi) the experiment; vii) sample code
(when applicable).
Handling Glassware
1. Apparatus that can roll (such as thermometers, etc). should be placed on the bench at right
angles to the edge of the bench to prevent it rolling onto the floor.
2. Suction flasks (or Büchner flasks) may collapse violently under vacuum if cracked or
otherwise weakened. Inspect suction flasks before using. Do not strike or tap a suction flask
while it is under vacuum.
3. Chipped, broken or cracked glassware should be discarded. Heating cracked glassware is

very dangerous - the glassware may shatter. Inspect glassware before using.
4. Remember - hot glassware looks identical to cool glassware! Be careful when handling hot
glassware.
5. When inserting glass tubing into a stopper match the tubing to the size of the hole.
Sometimes the tube can be lubricated with water or glycerol. To protect hands from being
cut, wrap tube in a towel before inserting into the stopper. Apply force to the tube length-
wise while slowly twisting the tube. Hold the tube near the stopper.
6. To break glass tubing, use a triangular file to scratch the tubing at the point of the break.
Moisten the scratch and wrap the tube with a towel. Place thumbs against the glass tubing
19
on the opposite side of the scratch. Press against the tube while pulling hands apart. Fire
polish the ends of the tubing before using.
20
SAFETY ACKNOWLEDGEMENT
Carefully read the following and print and sign your name on the form. You must sign this
form and present it to your laboratory instructor at the beginning of your first laboratory period.
I have read the safety rules and good laboratory practices outlined at the beginning of this
laboratory manual and agree to abide by these rules and practices. I acknowledge that failure to follow
these rules may result in dismissal from the laboratory period, a mark of zero for the experiment and no
opportunity to repeat the experiment. I accept that persistent failure to abide by the safety rules and good
laboratory practices will result in dismissal from the laboratory portion of the course.
I have read the guidelines on laboratory reports. I acknowledge that failure to abide by these
instructions may lead to loss of marks.
I have read the instructions on the use of laboratory equipment and agree to use the equipment in
accordance with those instructions. I acknowledge that using the equipment in such a way that is dangerous
or that is potentially damaging to the equipment may result in dismissal from the laboratory period, a mark
of zero for the experiment and no opportunity to repeat the experiment. I accept that persistent abuse of
equipment will result in dismissal from the laboratory portion of the course.
Name: _______________________________________________________
Signature: _______________________________________________________
Student Number: _______________________________________________________
Date: _______________________________________________________
Laboratory Period: _______________________________________________________
21
Ontario Tech University First-year Chemistry, F23; Reports 21.42
LABORATORY REPORTS
Be sure you use the current version of the laboratory manual for all aspects of writing your
reports. The laboratory manual changes from year to year sometimes in small, but significant, ways.
If you need help with preparing your laboratory reports, you may attend the office hours of
any of the CHEM 1010 laboratory teaching assistants. Alternatively, you may email:
Chem1010lab@ontariotechu.ca
If you use this email address, please include your name, the name of your laboratory teaching
assistant and your laboratory CRN. Any reply that you receive will be copied to your laboratory
teaching assistant. All the teaching assistants, the senior laboratory instructor and the CHEM 1010
laboratory technician have access to this email address, so the answers to your questions may come
from any one of them. Please note: this is a “communal” email address - your email can be read by
any of the instructors. DO NOT send private, confidential or sensitive information (or information
that you wish to keep private or confidential) to this email address.
Format for First-Year Chemistry Laboratory Reports
Laboratory reports in first-year chemistry are not “formal” reports. That is, you do not need
to submit reports with “Introduction”, “Method”, “Results and Discussion” sections. You need to
submit the signed data sheet(s), your sample calculations (including graphs) and the answers to any
questions posed in the laboratory manual.
Experiments (or parts of experiments) may be performed with a partner (or in groups), but
each student must submit their own, distinct report. There are no “group” reports for first-year
chemistry courses.
22
Guidelines for Reports
1. Deadlines for submission of reports are:
CHEM 1010U:
The laboratory reports for experiments 1 - 4 are due at the beginning of your next
laboratory period. The reports for experiment 5 is due at the end of the laboratory
period in which the experiment is performed.
CHEM 1020U and CHEM 1800U:

The laboratory reports for experiments 1 - 4 are due at the beginning of your next
regularly scheduled laboratory period. The reports for experiment 5 is due at the end
of the laboratory period in which the experiment is performed.
2. If you have been exempted from an experiment (see Missed Experiments), the deadline for
submitting any laboratory report that was due in the missed laboratory period will be three
(3) working days after the last date on which the experiment was performed (see the
Laboratory Calendar). The report may be submitted to the senior laboratory instructor or to
your laboratory teaching assistant.
3. Marks will be deducted from late laboratory reports at a rate of two (2) marks per “working”
day. No report will be accepted if it is more than four (4) working days late. A “working
day” is defined in the Laboratory Policies section.
4. The laboratory report must be typewritten or written using indelible ink - the choice is yours.
Two (2) marks will be deducted if the report (or any part of the report) is not typewritten and
not written in indelible ink (e.g. pencil must not be used for reports or to record data).
23
5. All original experimental data must be recorded with indelible ink. Before leaving the
laboratory have your data signed by an instructor. The signed, original data must be
submitted with the laboratory report. If no signed data are submitted with the report or if
data are not recorded in ink, two (2) marks will be deducted. Note: signed data sheets will
be used to track attendance at laboratories. If you do not submit a signed and dated data
sheet, you will be recorded as “absent”.
6. Any errors in recorded data should be corrected by drawing a single line through the
erroneous data and writing the corrected data close by. The original data should remain
legible.
7. White-out, correction fluid, correction tape or any similar product must never be used on
laboratory reports. Two (2) marks will be deducted for using these products.
8. Laboratory reports should be legible and well-organized. The grammar, style, and spelling
in laboratory reports will be considered when laboratory reports are graded. Persistently
poor spelling or grammar will be penalized.
9. Sample calculations must always be shown. In some cases the same calculation will be
repeated (in titrations, for example) - it is not necessary to show every individual calculation.
All steps should be shown so the marker can understand how the calculation was done and
locate any errors in the method or arithmetic. Failure to show sample calculations will
result in substantial loss of marks even if the final answers are correct.
10. Academic misconduct is a serious offence and will be punished. Academic misconduct
includes, but is not limited to: plagiarism (copying) of laboratory reports or allowing others
to copy your work, acquiring answers to questions from third-party, “homework” websites
or from other third parties, posting completed or partially completed reports on “homework”
24
sites (or allowing third parties to post your laboratory reports), submitting false data,
misrepresenting data, using data from other students without the permission of the instructor
or submitting one’s own laboratory report (or any part of a report) from a previous attempt
at the course. Details about academic integrity, misconduct, punishments and appeals
procedures can be found at:
Academic Integrity at Ontario Tech.
Reading and understanding these regulations are your responsibilities.
Note: if you share your report with another student and they use it to commit academic
misconduct, you may also be found guilty of academic misconduct.
11. Reports should be submitted directly to your laboratory teaching assistant (TA). Your TA
will provide instructions about how to submit your reports. Different TA’s may use different
methods for submission, so follow the instructions from your TA.
12. The student is responsible for ensuring that all required parts of the report are submitted (e.g.
that the correct file has been submitted). Students will not be permitted to re-submit a report
once the TA has marked the report (or the reports of the class) and returned it (them).
13. You MUST submit the cover sheet provided for each experiment. Two (2) marks will be
deducted if the cover sheet is not submitted.
Graphs for First Year Laboratories
Graphs may be drawn by hand or generated by computer - the choice is yours. If doing by
hand, you must use graph paper that uses at least ten divisions per centimetre and each data point
should be circled.
25
Whether drawn by hand or generated by computer follow these guidelines:
1. Unless instructed otherwise, the independent variable should be on the x-axis (the
“abscissa”) and the dependent variable should be on the y-axis (the “ordinate”).
2. Use appropriate scales for the axes. Scales should be chosen so the data fill the available
space. When plotting by hand, the scale should also be chosen to allow easy plotting and
reading of values; a scale in which 10 divisions represents 2/3 of a unit is not convenient!
The intersection of the axes does not have to take place at the origin (0, 0). Default scaling
in computer software is not always the best choice.
3. The axes must be labelled. The name of the quantity and the units in which it is measured
should be written beside the axis, e.g.: “temperature / 0C” or “concentration / mol L-1".
4. Major divisions on the axes should be labelled.
5. A title must be added to each graph. Enough information must be in the title to make it clear
what the data represent and why the graph has been constructed. For example:
Experiment 5: Determination of the Order of Reaction for the Reaction between

Hydrochloric Acid and Thiosulphate Ion (2HCl(aq) + Na2S2O3(aq) ÿ S(s) + SO2(aq) +
H2O(l)) at 200C.
The title should not merely state what the graph is - “Concentration vs. Time”, for example,
is not an adequate title.
6. Do not play “connect-a-dot” with the data. When appropriate, draw a smooth curve to “best
fit” the points. In many cases the curve may be a line. When using a computer, the equation
26
of the line or curve may be calculated by regression analysis. If this is the case, the function
used for the regression should be shown with the graph. The values of the adjustable
parameters (e.g., the slope and intercept) should also be included. If the equation of the line
has been calculated by a regression analysis, the correlation coefficient (r2) should be
included.
7. DO NOT use data points to calculate the slope of the line. If the slope is calculated “by
hand”, the points used for the calculation must be clearly indicated on the graph. Clearly
label the points with ‘x’ and ‘y’ co-ordinates.
Marking Schemes
A “performance evaluation” is part of your evaluation in the laboratory and is an assessment

by the teaching assistant of your conduct in the laboratory. Preparation, organization, general
attitude and safety will all be considered. An “average” student typically receives a grade of 3.5 /
5.
The allocation of marks for the laboratory component of the course is:
Laboratory Reports 25 marks total

Performance Evaluation 5 marks
Final Laboratory Grade 30 marks total
The percentage of the final mark of the course assigned to the laboratory will be decided by
the professor teaching the course.
27
Adjustments to Laboratory Grades
Teaching assistants are provided with uniform marking schemes for all the experiments.
However, within the context of these marking schemes teaching assistants will execute their own
judgement. At the end of the semester laboratory grades may be adjusted to account for variation
between individual teaching assistants. This may result in an increase or a decrease in your
laboratory grade. For semesters in which there is more than one teaching assistant, an overall class
average for the laboratory marks will be calculated and the marks for each individual teaching
assistant will be scaled to this value. No correction will be applied if the correction would be less
than 2 marks in 30 of the final laboratory grade.
28
SIGNIFICANT FIGURES
No measurement in science can be considered absolutely exact; that is, without error. All
measurements will include some uncertainty. Significant figures are used to reflect the degree of
uncertainty in a measurement. In general, more significant figures implies greater confidence in the
value. Proper understanding and use of significant figures is an essential aspect of scientific
communication.
As an example, consider the measurement of a piece of string with a ruler. Let us assume
the smallest division on the ruler is 0.1 cm. The end of the string will quite likely lie between two
divisions of the ruler (say, between 11.5 and 11.6 cm). Hence, you must estimate another digit to
get a better idea of the length of the string. One person might estimate the length as 11.52 cm while
another might estimate the length as 11.53 cm. It is commonly accepted that the last digit reported
is estimated. However, this last digit is still recorded as a “significant figure”.
The number of significant figures allows scientists to distinguish between more and less
precise measurements. The mass of a coin measured on an analytical balance (which measured to
±0.0001 g) might be recorded as 7.0164 g (five significant figures), but if the same coin were
weighed on an open-pan balance (which measured to ±0.01 g) the recorded mass would be 7.02 g
(three significant figures). It would be incorrect to record the mass from the open pan balance as
7.020 g because this implies, falsely, that the open pan balance weighs to ±0.001 g.
Rules for Counting Significant Figures
1. All non-zero figures are significant.
29
11.82: 4 significant figures

2. All zeros between non-zero figures are significant

3. If a decimal point is present, all zeros to the right of a non-zero figure are significant

2500.: 4 significant figures
If a decimal point is absent, the “significance” of the zeros is ambiguous. For a number such
as 101 000 the number of significant figures is unclear. Such numbers are usually written
in scientific notation so that the number of significant figures can be assessed. Thus, 101 000
might be written as:
1.01×105: 3 significant figures

1.010×105: 4 significant figures
4. Zeros to the left of a non-zero figure (but not between significant figures) are not significant.
30
0.0007: 1 significant figure
Significant Figures in Calculations
Rules for Rounding off Numbers
When rounding off numbers follow these rules:
1. If the digit following the last digit to be kept is greater than 5 increase the last digit kept by
one.
2. If the digit following the last digit to be kept is less than 5, leave the last digit kept
unchanged.
3. If the digit following the last digit to be kept is equal to 5 and any of the digits following the
5 is greater than zero, increase the last digit kept by one.
4. If the digit following the last digit to be kept is equal to 5 and all the digits following the five
are zero, round the last digit to be retained to the nearest even number.
Multiplication and Division
For multiplication and division the final result should be reported with the same number of
significant figures as the number with the fewest significant figures used in the operation. Examples:
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2.12 3 significant figures

× 3.025 4 significant figures
6.413
Reported as: 6.41 (3 significant figures)
12.053 5 significant figures

÷ 6.2 2 significant figures
1.94403
Addition and Subtraction
For addition and subtraction the number of significant figures to the right of the decimal point
in the final result must equal the number of significant figures to the right of the decimal in the
number with the fewest significant figures to the right of the decimal. For example:
8.102 3 significant figures to the right of the decimal

+ 10.11 2 significant figures to the right of the decimal
+ 111.1 1 significant figure to the right of the decimal
229.312
Reported as: 229.3 (1 significant figure to the right of the decimal place; four significant figures
total)
32
Be careful when adding numbers written in scientific notation. When adding or subtracting,
ensure all the numbers are written with a common exponent before adding them.
8.139×10-5 0.08139×10-3
+ 2.16×10-4 Y + 0.216×10-3
+ 1.218×10-2 + 12.18×10-3
12.47739 × 10-3
Reported as: 12.48×10-3 or 1.248×10-2
Logarithms and Exponentials
When taking the logarithm of a number, the number of decimal places in the result equals
the number of significant figures in the original number. For example:
log10 (1.35×10-2) = 1.86967
Reported as: 1.870 (the original number has 3 significant figures so this number is reported to 3
decimal places).
ln (2.5) = 0.91629
Reported as: 0.92
Only the digits after the decimal point are considered significant. The numbers to the left of the
decimal point locate the decimal point.
For raising numbers to powers the rules are “reversed”. The number of significant figures
33
in the result must equal the number of significant figures after the decimal point in the original
number.
e3.140 = 23.10387
100.31 = 2.0417
“Exact” Numbers:
Some numbers in science are considered to be “exact”. Exact numbers can be considered
to have an “infinite” number of significant figures. A number is “exact” when the objects can be
counted individually. For example, 112 jellybeans in a jar, 21 students in a laboratory, 43 apples in
a basket. The coefficients and subscripts in chemical equations are “exact”:
Zn(s) + 2HCl(aq) ÿ ZnCl2(aq) + H2(g)
All the numbers in this equation are considered exact. Numbers that are defined are considered
exact. This occurs most commonly for conversion from one unit to another (for example from
inches to centimetres or from kilograms to grams):
1 inch = 2.54 cm, exactly

1 kg = 1 000 g, exactly
So, to convert 12.12 inches (four significant figures) to centimetres:
12.12 inches × 2.54 cm / inch = 30.7848 cm
Reported as: 30.78 cm (four significant figures)
34
In a sequence of calculations, at each step you should report the value with the correct
number of significant figures. However, to avoid “rounding errors”, which may become
considerable if there are many steps, all the figures provided by the calculator should be carried
through the calculation until the end. At the end, the number should be rounded off to give the
correct number of significant figures.
35
LABORATORY REPORT RECEIPT SHEET
This sheet can be used as proof that you have submitted a laboratory report. Whenever you
hand in a report, have an instructor sign and date this sheet. Keep the sheet in safe place (e.g., staple
it into your laboratory notebook). If an instructor loses a report, this sheet will act as proof that you
handed in the report.
Name (print): __________________________________________________
Student Number: __________________________________________________
Course: _________________________ Semester: _________________________
Experiment Instructor Signature Date

1
2
3
4
5
Check out
At the end of the semester you must “check-out” your locker equipment. Ensure that all of the
equipment is present, clean, and in good repair. Have the teaching assistant check it. Failure to
“check-out” may result in the withholding of your laboratory marks.
36
Ontario Tech University Chemistry, F23; Missed Experiments 9.15
MISSED EXPERIMENTS
All students must attend at least three (3) laboratory periods (of five) in order to receive
credit for the laboratory portion of the course.
A student who misses an experiment (for any reason) must complete the “Record of Missed
Experiment” posted on the Laboratories page of the course Canvas site. If you have missed your
laboratory period, you may: i) attend an alternative laboratory period; ii) be given an accommodation
for the missed experiment or iii) be exempted from the experiment. Exemptions will not often be
granted.
If you do not perform an experiment or do not submit a laboratory report for the experiment
and have not been granted an exemption, you will receive a grade of zero for the missed experiment.
If requested, documentation for missed experiments should be submitted electronically to the

senior laboratory instructor. You may either photograph or scan the documentation and email it to
the senior laboratory instructor:
richard.bartholomew@ontariotechu.ca
Include all pages and ensure the documentation is legible. If you submit a hard copy of your
documentation, or if a hard copy is requested, be sure to make and keep a copy of the documentation
for your own records.
Attending an Alternative (“Make-up”) Laboratory Period
You may attend any alternative laboratory period in which space is available. You may check
up-to-date enrollments in laboratory periods at the preview of available courses:
Search for Available Courses
37
The opportunity to attend an alternative laboratory period is made available on a first-come, first-
served basis. Just because the laboratory CRN has available seats, does not mean you will be able
to do your experiment at that time. Students who are registered in a given CRN have priority; space
will be allocated to these students first. Even if you are initially admitted to a laboratory period, you
may have to surrender your space if a registered student shows up no later than 10 minutes after the
start of the laboratory period.
Before attending an alternative laboratory period, you must complete the “Re-scheduled
Experiment” form posted on the laboratories page on the course Canvas site. Bring the completed
form with you to your alternative laboratory period. At the end of the laboratory period, you MUST
ensure the teaching assistant has signed this form and your data sheets. The signed form acts as
proof to your regular TA that you performed the experiment. Without this proof, your report will
not be marked and you will receive a grade of zero for the report.
When you arrive at the laboratory room, you should line up at the designated place to wait
to see if a space will be available for you.
The report that should have been submitted in your missed laboratory period may be
submitted to the TA of the alternative laboratory period. Be sure to indicate on your report the CRN
and TA name for your regularly scheduled laboratory period.
The report for the experiment performed in the “make-up” laboratory period will be due at
the beginning of your next regularly scheduled laboratory period. If you attend an alternative
laboratory period for the experiment 5 (the final experiment), the report will be due at the end of the
laboratory period.
38
Accommodations if an Alternative Laboratory Period is Unavailable
If, by the end of the offering of a given experiment (each experiment is offered for two weeks
of classes), you have not been able to perform the experiment, you must contact the senior laboratory
instructor to arrange an accommodation for the missed experiment. The senior laboratory instructor
may request documentation to explain your absence or require you to complete and submit a “request
for academic consideration”. If you do not contact the senior laboratory instructor within three (3)
working days of the end of the offering of an experiment, no accommodation will be granted and you
will receive a grade of zero for the report for the missed experiment. To be eligible for an
accommodation, you must have completed the “Record of Missed Experiment”.
Exemptions
A student may only be exempted from an experiment for “acceptable reasons”. The
acceptable reasons for missing an experiment are: medical / health reasons, bereavement, religious
observance, or court appearance. You may be asked to submit appropriate documentation to the
senior laboratory instructor. Exemptions will rarely be granted. Please note: exemptions for missed
experiments will NOT be granted to accommodate other academic requirements or commitments
(e.g. midterms, assignments, etc.).
If you are exempted from a laboratory period for an acceptable reason, the deadline for
submitting any report that was due in the missed laboratory period will be extended by three (3)
working days from the end of the experiment cycle. Longer extensions may be granted at the
discretion of the senior laboratory instructor.
The maximum number of accommodations plus laboratory exemptions for a course in a given
semester is two (2). In other words, you must attend at least three (3) laboratory periods to receive
credit for the laboratory portion of the course.
39
Ontario Tech University Analytical Chemistry Techniques, F23; 20.35
ANALYTICAL CHEMISTRY TECHNIQUES
In all the sub-disciplines of chemistry good technique is crucial to obtaining good results and
this is particularly true for quantitative aspects of chemistry. To be successful you must master the
standard techniques (described below) of analytical chemistry. For many of the techniques links to
videos of the techniques are provided.
Weighing Techniques
The accurate measurement of mass is fundamental to all aspects of chemistry. Because of

advances in technology, mass can be one of the most accurately known quantities in any experiment.
For greatest efficiency the proper balance must be chosen and the proper procedure must be
followed. In chemistry two types of balances (along with specialized variations) are commonly used:
the “open-pan” balance and the “analytical” balance.
Open-pan Balance (open-pan balance)
Open-pan balances are used when i) a mass with less accuracy is required; ii) the mass is
heavier than can be accommodated on an analytical balance; iii) an approximate mass of a substance
must be transferred from one container to another.
Operating an open-pan balance is very simple. Press the “tare” button to “zero” the balance,
place the object on the balance pan and record the mass. To measure an approximate mass of
substance into a receiving vessel, place the receiving vessel on the balance pan and press the “tare”
button. This will re-zero the balance. Essentially, the mass of the receiving vessel has been
subtracted. As a substance is added to the receiving vessel, the balance displays the mass of added
40
material. Using an open-pan balance avoids transferring chemicals on the analytical balance which
may cause damage to the analytical balance if the chemicals are spilled.
The Analytical Balance (analytical balance)
The Mettler-Toledo analytical balance used in chemistry laboratories at Ontario Tech

University is designed to weigh relatively small masses (less than 120 g) with very great precision
(to ±0.000 1 g). These balances are remarkably easy to use but are very delicate and must be handled
with great care.
1. To ensure the greatest accuracy the balance should be level. This can be confirmed by
observing the “level indicator” on the balance (which functions exactly like a carpenter’s
spirit level). The bubble should be exactly in the middle of the circle. If not, consult the
teaching assistant.
2. Ensure all the doors are closed. If it is not on already, turn on the balance. The balance will
run through a series of checks and eventually should display 0.0000 g (or a value very close
to zero). Note: the balance can use different units so make sure the display shows the units
required for your measurement - typically, grams.
3. Press the “tare” button. This will set the mass reading to zero.
4. Gently slide open one of the doors and place the item to be weighed on the pan. The item
must not touch the sides of the balance or the outer ring of the pan.
5. Close all the doors of the balance. Air currents affect the measured mass.
6. Wait until the balance indicates the reading has stabilized then record the mass.
41
7. Remove the object and close all the doors.
8. Chemicals must NEVER be placed directly on the balance pan because they may react with
it and damage the balance. They must be held in or on some suitable container. Preferably,
it is a closed container.
9. If chemicals are spilled in or on the balance, they must be cleaned up immediately. Consult
a teaching assistant.
10. Special care must be taken when measuring the mass of liquids or solutions If they are
weighed on an analytical balance, they MUST be in closed containers.
11. To avoid spilling chemicals (and subsequent damage to the balance), chemicals must not be
transferred to a weighing container on (or in) the analytical balance. The transfer should be
done using an open-pan balance.
12. Objects which are hot should not be weighed on the analytical balance. The air currents
caused by the hot object will cause erroneous readings of the mass.
13. Make sure no one is leaning on the balance table when the measurement is being made
because this will adversely affect the measurement.
14. When using the balance for a sequence of measurements on the same object (as, for example,
when performing a “weight-by-difference”), it is good practice to use the same balance. This
will minimize error because any (constant) error in the balance will be cancelled or partially
cancelled in the difference when the difference in mass is calculated.
15. The analytical balance is a very accurate and sensitive instrument. Handling glassware
42
leaves fingerprints and the analytical balance may detect this difference in mass. For greatest
accuracy, the weighing vessel should be handled with tongs, while wearing gloves or with
a piece of paper towel wrapped around the vessel.
16. Substances which are not dry can be difficult to weigh on the analytical balance because the
evaporation of water makes it difficult to obtain a stable mass. Similarly, substances which
are hygroscopic (water absorbing) are hard to weigh because of the absorption of water
which leads to ever increasing mass.
17. DO NOT move the analytical balances.
Weight-by-Difference (weight by difference)
This technique allows very accurate measurement of a relatively small mass transferred to
a receiving vessel (e.g., a flask or a beaker). Usually an analytical balance is used, but an open-pan
balance may also be used if the masses involved are comparatively large.
1. Using an open-pan balance weigh the approximate amount of the substance required into a
weighing vial. A small beaker may also be used, but a weighing vial is preferable.
2. Weigh the vial plus contents on the analytical balance and record the mass.
3. Pour the contents of the vial into the receiving vessel.
4. Re-weigh the now (mostly) empty vial on the same analytical balance (see above for the
reason why) and record the mass.
The mass transferred to the receiving vessel is simply the difference between the two masses.
43
It does not matter if the weighing vial is completely emptied into the receiving vessel because any
sample remaining in the weighing vial is included in the mass of the “empty” vial. However, none
of the substance may be spilled; all of it must be in either the weighing vial or the receiving vessel.
If it is spilled, the spilled mass is not taken into account when calculating the mass transferred and
the calculated mass transferred will not be correct
Weight-by-difference can also be done in “reverse”. First, the mass of an empty weighing
vial is recorded. Then the weighing vial is filled and the mass of the filled vial is recorded. The
mass of the substance in the vial is the difference between the two recorded masses.
An accurate weight-by-difference is best achieved by ensuring the mass of the vial (or
beaker) is not too large compared to the mass of the substance in the vial (or beaker). In other words,
the difference between the two masses should not be small compared to the two masses that have
been measured. For example, consider trying to determine the mass of a feather by weighing the
feather in a cast iron frying pan, then weighing the empty frying pan!
Volumetric Techniques
Volumetric techniques are probably just as important as weighing technique. In CHEM 2030
/ 2130 volumetric analysis is used extensively. Good volumetric technique is necessary to obtain
good results.
In analytical chemistry several important and accurate types of volumetric glassware are
commonly used: the pipette (in various forms), the burette and the volumetric flask. Other useful,
but not as accurate, pieces of glassware include the graduated cylinder and the Erlenmeyer flask. In
the vast majority of analyses, the glassware does not need to be dry to start the analysis. When
necessary, any residual water, or other solvent, is removed (“exchanged”) by systematic rinsing with
44
the solution that will be used in the glassware. This replaces the water (or solvent) with the solution
and ensures the solution is not diluted. NEVER attempt to “dry” glassware by shaking out excess
liquid. This is an excellent way to break glassware, particularly burettes and pipettes which have
delicate tips. Do NOT invert glassware (e.g., graduated cylinders, Erlenmeyer flasks, and volumetric
flasks) on the bench top in an attempt to drain excess liquid; glassware in this position is easily
knocked over and broken.
Volumetric glassware is normally designated as either “TC” (to contain) or “TD” (to deliver)
at an indicated temperature. “TC” means the glassware will contain the designated volume; if the
liquid is drained or poured out, less than this volume will be transferred. “TD”, on the other hand,
means that if the glassware is drained (or emptied), the designated volume will be transferred to the
receiving vessel. The difference between “TC” and “TD” is an important one and should be
considered when selecting glassware for an experiment or procedure.
The Meniscus (the meniscus)
To properly use volumetric glassware it is important to understand how to read a “meniscus”.

When most liquids (including water) are confined to a vessel, they will form a concave surface; the
liquid will be higher at the edges than at the centre. This curvature is called the “meniscus” and is
caused by the interaction of the molecules of the liquid with the molecules of the vessel. A meniscus
is more pronounced for narrower vessels. Generally, the meniscus should be read at its lowest point.
In some unusual cases (e.g. reading mercury in a barometer) reading the top of the meniscus is
required. To avoid parallax error, position your eye at the same level as the bottom of the meniscus.
The bottom of the meniscus can sometimes be more easily read by placing a white card with a dark
stripe behind the glass tube with the top edge of the dark stripe level with the bottom edge of the
meniscus. The bottom of the meniscus will be sharper and easier to see.
45
Transfer Pipette (transfer pipettes)
The transfer pipette is one of the fundamental tools of analytical chemistry. It is accurately
calibrated “to deliver” (designated as “TD”) the prescribed volume to the receiving vessel. When
used properly, the error in volume transferred is probably less than 0.2%. The trick is to use it
properly! For beginners some practice will be required.
To prepare a pipette for use it should be rinsed with tap water, then with deionized water, and
finally with the solution / liquid that is to be transferred. The rinsings should be performed three
times. Squeeze the pipette bulb and place it over the thick end of the pipette. NEVER use your
mouth!! Place the thin end (the tip) in the liquid. Slowly release your grip on the bulb to draw liquid
into the pipette. Fill the pipette about half full. Remove the bulb and quickly place your finger over
the end. Hold the pipette nearly horizontal and rotate it so the liquid inside coats the entire inner
surface. Drain the liquid through the tip into a waste beaker. Do not pour the liquid out the top of
the pipette. Rinse the pipette twice more.. A clean pipette should drain smoothly and leave no
droplets on the inner surface of the pipette. If droplets do form, the pipette needs more “vigorous”
cleaning. Consult an instructor.
Unless absolutely necessary, do not use soap to clean a pipette. Soap can be difficult to rinse
completely from a pipette and may leave a contaminating film.
Once the pipette has been properly cleaned and rinsed, a very precise volume can be
transferred with the pipette. Use the bulb (NEVER use your mouth!!) to draw the liquid into the
pipette until the liquid level is well above the graduation mark. For large volume pipettes you may
have to squeeze and use the bulb a second (or third!) time. If so, when you remove the bulb quickly
place your first finger over the top of the pipette. During the swap you may find it helpful to gently
rest the bottom of the pipette on the bottom of the beaker. While filling the pipette, do not lift the
bottom of the pipette above the level of the liquid. If you do, liquid will squirt into the bulb. This
46
is a very bad thing! It can lead to cross contamination of solutions. See below for instructions on
cleaning a contaminated pipette bulb. Once the level of the liquid is above the graduation mark,
remove the bulb and quickly cover the end of the pipette with your first finger. Do NOT use your
thumb!!
Lift the tip of the pipette out of the solution. Using a kimwipe or piece of paper towel, wipe
excess liquid from the tip. While touching the tip of the pipette to the side of the beaker slowly
release the pressure of your finger on the top of the pipette to lower the level of the liquid. Keep the
pipette vertical while doing this. Keep your eye level with the graduation mark. Lower the level of
the liquid in the pipette until the bottom of the meniscus is exactly at the mark.
To transfer the liquid to the receiving flask vessel, place the tip of pipette against the side of
the receiving vessel. Keep the pipette vertical. If necessary, angle the receiving vessel. Remove
your finger and allow the pipette to drain. Once the pipette is empty wait ~10 s (to ensure complete
and consistent draining) and touch the tip to the side of the receiving flask. Do NOT blow out the
small amount of liquid in the tip - the pipette is calibrated for the small amount that remains in the
tip.
Mohr Pipette (Mohr pipette)
Unlike a transfer pipette (which delivers a fixed volume) a Mohr pipette can be used to
deliver variable volumes. The level of accuracy of a Mohr pipette is slightly lower than for a transfer
pipette. The technique for using a Mohr pipette is very similar to using a transfer pipette. However,
two differences must be kept in mind. First, for a Mohr pipette the volume delivered is determined
by the difference between graduations. If the meniscus is lowered from the graduation at 1.00 mL
to the graduation at 4.20 mL, the volume delivered to the receiving vessel is 3.20 mL. Second, a
Mohr pipette is NOT calibrated for the liquid that remains in the tip. If you fill a Mohr pipette and
then drain it, you will transfer more solution than you think!
47
When using a Mohr pipette, it is a good idea to avoid draining to the last graduation on the
pipette. If, for some reason, you drain too much from the pipette, you will not be able to determine
how much liquid was transferred, so the analysis will be useless.
A Mohr pipette is very useful when multiple transfers (i.e., to different receiving vessels)
must be made. As long as the sum of the volumes to be transferred is less than the total volume of
the Mohr pipette, all of the transfers can be completed with a single fill of the pipette.
Serological Pipette
These types of pipettes are not used extensively in chemistry, but do find wide application
in biology and biochemistry. Like a Mohr pipette, they are capable of delivering a variable volume.
Unlike a Mohr pipette, they do not operate “by difference”. If filled to the 7.00 mL mark, for
example, and drained, the pipette delivers 7.00 mL to the receiving vessel. Some serological pipettes
require “blow out” of the liquid in the tip; some do not. If you use a serological pipette, you must
check to see which type you are using. In this course serological pipettes will not be used.
“Eppendorf”(or micro-) Pipette
Micropipettes are often used in biology and chemistry to transfer small (< 1 mL) volumes.
They sometimes have high relative systematic error and variation in volume delivered (from one
pipette to another) can be significant. Proper calibration of the pipette is necessary if they are to be
used for accurate volumetric work. They must also be re-calibrated periodically as their mechanisms
wear over time. Eppendorf pipettes are frequently used improperly leading to significant error. In
general, for accurate analytical work a transfer or Mohr pipette is preferred.
Using the pipette is straightforward. Attach an appropriate tip (the tips are often colour coded
to the pipette) and depress the button on the top until the “stop” is reached. Hold the pipette vertical
48
and immerse the end of the tip in the solution. Slowly release the button to fill the tip. Place the tip
of the pipette against the side of the receiving vessel and push the button all the way to the bottom
(past the “stop”) to fully discharge the contents. To dispose of the tip press down on the button on
the front of the Eppendorf. The pipette should be kept vertical at all times during the transfer. As
a general rule: if there is a tip attached, the pipette should be kept vertical. Tipping it on its side can
allow the contents of the tip to enter the mechanism of the pipette and damage the mechanism.
Cleaning a Pipette Bulb
If solution enters the pipette bulb, the bulb must be cleaned to avoid contaminating
subsequent solutions. Remove the white taper from the end of the bulb and rinse it thoroughly with
deionized water. Rinse the inside of the bulb three times with deionized water and squeeze the bulb
repeatedly after each rinsing to expel the water in the bulb. Store the bulb with the open end down
to allow any water to drain from the bulb.
Burette / Titration (using a burette, titrating)
A titration is an analytical chemistry technique in which one reagent (the titrant, in a burette)
is carefully added to another reagent (the analyte, in a flask or beaker) until the reaction is
“complete” (i.e., all of the analyte has been converted to products). A titration is used to determine
the accurate concentration of either the titrant or the analyte. Ideally, a titration seeks to measure the
“equivalence point”. The equivalence point is the volume of titrant required to deliver a
stoichiometric number of moles of titrant; that is, the volume at which the number of moles of
analyte and the number of moles of titrant added to the flask are in their stoichiometric ratio. In
practice, the volume of titrant required to reach the “end point” is measured. The end point is simply
the point at which the titration is stopped. This is determined with an “indicator” which is a species
added to the titration flask that changes a physical property at (or very near) the equivalence point.
The most common change is colour.
49
A burette allows variable, but accurately measured, volumes to be added to a receiving

vessel. The volume delivered is determined from the difference between a final and an initial
volume reading. A 50 mL burette is typically graduated in 0.1 mL intervals; the volume should be
recorded to 0.01 mL by estimating between graduation marks.
A burette is cleaned in a similar way to a pipette. It should be rinsed at least three times with
small portions of tap water, followed by three times with deionized water and finally with three times
with the solution that will be used to fill the burette. As with the pipette, hold the burette
horizontally and rotate it so that the liquid covers the entire inner surface of the burette. Drain the
some of the liquid through the stopcock into a waste beaker (ensure the tip remains full). Extra
liquid can be poured out the top of the burette. Before rinsing with the solution, ensure the burette
is working properly by draining some deionized water through the tip. Ensure no bubbles are in the
tip. Once the tip is bubble-free, ensure the tip is always full by draining a small amount of the
solution through the tip with each rinsing of the burette.
Using a funnel and a beaker, fill the burette with solution to just above the ‘0' graduation.
While filling the burette, ensure that the funnel is below eye level. This reduces the risk of spilling
chemical on the face and in the eyes. If you spill any solution on the outside of the burette, wipe the
outside of the burette with paper towel and wash your hand afterwards. Remove the funnel and open
the stopcock and drain some of solution through the burette tip into a waste beaker. Ensure no
bubbles are in the tip. Touch the tip of the burette to the side of the waste beaker to remove the last
drop. The level of the liquid must be below ‘0'.
Before starting the titration, record ther “initial volume”. When reading the volume, the
burette must be vertical and the meniscus should be at eye level. Read the volume at the bottom of
the meniscus. You should be able to estimate the volume to 1/10 of a graduation (typically this
means to 0.01 mL). You may find it useful to use a “burette card” (a white card with a black stripe.
The card is placed behind the burette with the top of the black strip at the level of the meniscus) to
50
help read the meniscus. On a burette the volume increases as you read down the burette and
indicates the volume that has been dispensed from the burette not the volume remaining in the
burette. Therefore, you do not need to do any arithmetic before recording the volume; simply record
the volume on the burette.
The directions here are for a right handed person; “lefties” should reverse all directions. The
burette is set up with the stopcock facing right. The stopcock is controlled with the left hand - the
palm of the hand is behind the burette and the stopcock is controlled by the thumb and first finger.
Initially, this will feel quite awkward but with practice will become more comfortable. The right
hand is used to swirl the receiving vessel (normally, a flask). Swirling promotes the mixing of
reagents and is crucial to obtaining accurate results. Keep the tip of the burette below the rim of the
receiving vessel to ensure all the liquid dispensed from the burette is added to the receiving vessel.
Before beginning the titration, ensure sufficient titrant is in the burette to complete the
titration (i.e, to reach the end point). This is particularly true if you start a titration without a full
burette. If the burette is drained below the last graduation, the volume dispensed cannot be
accurately known and the analysis is pointless. Initially, the titrant (the solution in the burette) may
be added quickly. As the end point is approached, the additions should be smaller. Very close to
the end point titrant should be added drop-wise (or even ½ drop-wise!). To add titrant drop-wise,
allow a drop to form slowly on the tip of the burette and then touch the tip to the side of the receiving
vessel. Wash the side of the vessel with a little deionized water from a wash bottle. Near the end
point rinse down the sides of the flask to ensure all of the titrant dispensed from the burette has
reacted with the solution in the flask.
Once the end point is reached wait a few seconds for the burette to drain properly then read
the final volume. Read the meniscus in exactly the same way as when the initial volume was read.
The volume dispensed to the receiving vessel is the difference between the final volume and the
initial volume.
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To clean the burette after the experiment is finished, drain any remaining solution into a
waste beaker. Rinse several times with tap water then with deionized water. Store the burettes
upside down (tips facing upwards) and with the stopcocks open.
Graduated Cylinder
A graduated cylinder measures volumes with moderate accuracy; it is better than a beaker,
but not as accurate as a pipette. Care should be taken to note whether the cylinder is calibrated “to
deliver” (TD) or “to contain” (TC).
Larger graduated cylinders often have a plastic collar. This collar should be positioned near
the top of the graduated cylinder - it prevents breakage if the graduated cylinder is knocked over.
Volumetric Flask
A volumetric flask is used to prepare solutions of very accurately known concentration.

These solutions can be made by dissolving solids (see Preparation of a Standard Solution) or by
diluting other solutions (or liquids). Normally, when the solution is prepared by dilution, the transfer
of the solution (or liquid) being diluted is accomplished with a transfer pipette of appropriate volume
(see transfer pipette).
Prior to preparing a solution, the volumetric flask should be rinsed several times with
deionized water (or the solvent used to prepare the solution).
Once the dissolved solid or solution to be diluted has been transferred to the flask, fill the
flask ~3/4 full with solvent and swirl the mixture to ensure good mixing. Continue filling the flask
until the meniscus is ~1 cm below the graduation. Complete the filling by adding water (or solvent)
drop-wise until the bottom of the meniscus is exactly on the graduation mark. Be very careful. If
52
the meniscus is above the graduation (by even a little bit), you must start again. Once the meniscus
is on the graduation, stopper the flask and invert it (“bubble up, bubble down”) 20 - 25 times to
ensure good mixing. This is a crucial step - improper mixing of solutions is a large source of error
in undergraduate experiments. While inverting the flask, hold the stopper in place.
Note: it is not necessary to measure or calculate the amount of solvent to add to the flask to
dilute the solution to volume. Volumes are frequently non-additive (especially when dealing with
non-aqueous solvents), so the required volume may be more or less than calculated. Filling the
volumetric flask to the mark avoids this problem.
Volumetric flasks are calibrated “to contain” (TC) their designated volume at their designated
temperature.
Never put hot or cold solutions in a volumetric flask. Never expose the volumetric flask to
extremes of temperature. The resulting expansion and / or contraction of the glass may ruin the
calibration of the volumetric flask.
Preparation of a Standard Solution (preparing a standard solution)
A solution whose concentration is accurately known is a “standard” solution. In many cases

a standard solution may be prepared directly from the solid and the solid is referred to as a “primary
standard”. A primary standard should have the following properties: i) it should be available in high
purity ($99.9%); ii) it should not absorb moisture from the air (i.e., must not be hygroscopic); iii)
it should be thermally stable so that it can be dried; iv) it should have high molecular weight to
reduce relative weighing errors because a “large” mass of the solid must be weighed out to get a
given number of moles; v) it should be stable in air. If a substance does not qualify as a primary
standard, it can often be “standardized” by titrating it with a solution of a primary standard.
53
The following is the procedure for preparing an aqueous primary standard solution (see, also,
instructions for using a volumetric flask).
1. The solid should be dried to constant mass. This ensures the solid contains no moisture and
gives a very accurate mass for the solid. Drying to constant mass means drying the solid at
> 1000C, cooling it, weighing it and repeating this process until the mass is constant.
2. Place a clean, dry weighing vial (or small beaker) on an open-pan balance and tare the
balance. Add the required mass of solid to the vial. You do not need to record this mass.
Make sure the cap is on the vial and re-weigh it on the analytical balance. Record the mass
to ±0.000 1 g.
3. Pour the solid into a clean beaker of roughly the same volume as the final volume of
solution. Do not spill any solid. If you do, you must start again. Do not worry about getting
all the solid from the vial into the beaker; not spilling any solid is more important.
4. Record the mass (±0.000 1 g) of the now (mostly) empty vial using the same analytical
balance, again to . The difference between this mass and that recorded in step 2 gives the
exact mass of solid transferred to the beaker.
5. Add deionized water, using approximately ½ the final solution volume, to the beaker.
6. Stir the solution without spattering until all the solid has dissolved. If you remove the
stirring rod at any point, be sure to rinse the stirring rod with deionized water in such a way
that the rinsings flow into the beaker. In this way, you will not lose any solid on the stirring
rod.
7. You are now ready to begin the quantitative transfer of your solution to the volumetric flask.
54
It is vital that you transfer all the solution - therefore, all the weighed solid - to the
volumetric flask.
8. Place a funnel in the neck of the volumetric flask. Using the stirring rod as a guide, carefully
pour the solution so that it runs down the rod through the funnel into the flask. If the liquid
stops flowing through the funnel, try lifting the funnel slightly out of the neck of the flask.
9. Using your wash bottle, thoroughly wash the inside wall of the beaker. Transfer the
washings to the volumetric flask using the stirring rod and funnel just as you did in step 8.
Repeat the washing and transfer twice more (for a total of 3 times). Be careful not to use too
much water in this and all rinsings.
10. Rinse the end of stirring rod using your wash bottle such that the rinsings flow through the
funnel into the volumetric flask.
11. Finally, using the wash bottle, rinse the inner surface of the funnel.
If steps 8 - 11 have been performed correctly, you will have successfully transferred all the
solid to the volumetric flask.
12. Now for the crucial step! Carefully fill the volumetric flask so that the bottom of the
meniscus lies exactly on the graduation. It can be neither above nor below the mark. If the
meniscus is above, you will have to start again!! The last little bit of water should be added
drop-wise using a medicine dropper or Pasteur pipette to ensure the flask is not overfilled.
13. After you have filled the flask, invert it (“bubble up, bubble down”) 20 - 25 times, while
holding the stopper in place, to ensure thorough mixing of the solution.
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Suction Filtration (suction filtration)
Suction filtration is an efficient method to separate a precipitate from a solution (the

“supernatant”). It can be used when either the precipitate or the supernatant is required. The
technique employs a partial vacuum in a flask to draw the supernatant through a filtering device.
Suction filtration is often used to quantitatively separate the precipitate from the solution.
Always inspect the suction flask for damage or cracks before use. A damaged flask can
implode violently when placed under vacuum and cause serious injury. When using a suction flask,
secure it with a ring clamp or an adjustable clamp. Otherwise, it will probably topple over.
For the recovery of small amounts of product, a Hirsch funnel or a sintered glass crucible is
used and for larger quantities a Büchner funnel is used. The sintered glass crucible requires no filter
paper and is often used when the precipitate must be dried by heating in an oven. Sintered glass
crucibles use special holders to attach them to the suction flask. For the Hirsch and Büchner filters,
a one hole stopper is put on the top of the filter flask and the appropriate funnel inserted into the
hole. A thick walled rubber tube connects the side arm of the suction flask to an aspirator which
generates the vacuum in the flask.
When using a Büchner or Hirsch funnel, place a filter paper sufficiently large to cover all the
holes in the funnel. Moisten the paper with a small amount of the solvent to ensure the filter paper
adheres well to the bottom of the funnel. Turn on the aspirator. A moderate vacuum is created in
the flask that will draw the supernatant solution through the filter paper.
To recover the solid, decant the supernatant solution onto the filter paper using a stirring rod
as a guide and allow the solution to pass through the filter paper. Next, transfer as much as possible
of the solid from the beaker onto the filter paper by scraping it out with a “rubber policemen”. Small
portions of cold solvent can be used to wash out the solid and to rinse off the stirring rod and rubber
56
policeman. Do not use too much solvent or the solid may re-dissolve. Get the crystals as dry as
possible with the suction filtration. Break the vacuum by lifting the funnel out of the hole or by
removing the tube from the side arm of the flask. Be careful - the side arm is fragile. Wash the solid
with the small amount of cold solvent and then re-establish the vacuum. Apply the suction until the
solid is once again dry. To facilitate better drying of the solid, it can be pressed with the blunt end
of a scoopula to squeeze out any solvent. Large “clumps” of solid can also be broken apart but take
care not to tear the filter paper. Repeat the washings 2 - 3 times, breaking the suction before each
washing. Several washings with small amounts of solvent are better than one washing with a large
amount of solvent. Once the solid is dry, break the suction then turn off the aspirator. It is important
to break the suction first. Otherwise, water from the aspirator line may be sucked back into the
suction flask contaminating the filtrate. Carefully remove the solid from the filter paper onto a watch
glass or into a sample vial. Be careful not to tear the filter paper.
When the supernatant is to be kept, it is a good idea to employ a trap between the aspirator
and the suction flask. The trap is a second flask with a two hole stopper and two glass rods in the
holes. One glass rod is connected to the aspirator and the other is connected to the side arm of the
suction flask. Any water sucked in from the aspirator will be caught in the trap and not contaminate
the filtrate. The trap flask must be able to withstand a vacuum - an ordinary Erlenmeyer flask will
not do.
Genesys20 Spectrophotometer
The Genesys20 spectrophotometer is remarkably easy to use but is a sensitive and delicate
piece of equipment and should be treated accordingly. If, during the course of the experiment, you
spill anything on (or in!) the spectrophotometer, immediately clean it up.
1. The lamp in the instrument must warm up prior to use to get the best results. Turn the
57
instrument on roughly 15 minutes before taking measurements. The power switch is at the
back of the instrument next to the power cord.
2. The current mode of operation appears in the display. Press the “A/T/C” button to select the
desired mode of operation. Unless you are explicitly told otherwise, you will use the
“absorbance” (“A”) mode for chemistry experiments.
3. Select the wavelength appropriate for the experiment you are conducting (normally given in
the experiment procedure). Press either the nm> or the nm? key to choose the wavelength.
If you hold down the key, the wavelength will change more quickly.
4. Open the sample compartment and insert a cuvette containing the “blank” into the cell
holder. A “blank” is a solution containing everything but the species of interest). Note that
the light path is from top to bottom (as opposed to left to right). Make sure the cuvette is
positioned so that the light is passing through the clear walls of the cuvette. Do not touch
the clear walls of the cuvette as this will leave fingerprints and cause erroneous results.
Close the sample compartment door.
5. Press the “0 ABS / 100% T” key to set the blank absorbance to 0 (or, equivalently, %
transmittance to 100%). This subtracts any absorbance arising from the blank. Periodically,
you should repeat steps 4 and 5 to counter any problem arising from “drift” in instrument
response.
6. Remove the blank and insert the cuvette containing the sample into the cell holder. Close
the sample compartment door and record the absorbance shown on the LCD display.
7. If you must re-use the cuvette with more than one solution, be sure to rinse it thoroughly
three times with small portions of the new solution. Start with the most dilute solution and
58
work toward the most concentrated.
Seven-Easy pH Meter
1. Turn the pH meter on.
2. A manual temperature correction must be used to obtain the correct pH. Record the room
temperature using the thermometer in your locker. Press the thermometer button (at lower
left) and use the up and down arrows until the display reads the correct temperature. Once
the temperature is set, press the “Read” button twic.
3. The electrode should be left in pH 4 buffer when not in use. To ready the electrode for use,
twist the purple, plastic ring near the top of the electrode to expose a little hole near the top
of the electrode.
4. A 3 point calibration will normally be performed. To begin, remove the electrode from the
buffer. Using a wash bottle, rinse the electrode with de-ionized water. Gently BLOT excess
water from the electrode using a kimwipe. Do NOT wipe or rub the electrode.
5. To calibrate the meter immerse the electrode in pH 7.0 buffer and press the “Cal” button.
When the calibration has finished, the pH meter will display pH = 7.0.
6. Remove and rinse the electrode and place it in the second buffer (in this case pH 4.0). Press
the “Cal” button. Again, when the calibration is finished, the meter will display the correct
value (pH = 4.0). Each time you move the electrode from one solution to another you should
rinse the electrode and blot it dry. If you are performing only a two point calibration, go to
step 8.
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7. Repeat step 6 with the third buffer (pH 10.0). At this point the meter will also display the
slope and the offset. The slope should be between 95-105%. The offset should be between
±15 mV. If either of these is outside the limits, repeat steps 4 - 7. If it fails a second time,
inform an instructor.
8. Once again, rinse the electrode with de-ionized water, dry it by blotting with a kimwipe, and
place it in the solution to be tested. Press the “Read” button to record the pH. If an “A” is
present on the right side of the display, hold the “Read” button for 2 seconds until the “A”
disappears. IMPORTANT: ensure the “A” has disappeared before you begin.
9. At the end of the experiment rinse the electrode thoroughly with deionized water, blot it dry
with a kimwipe and return the electrode to the pH 4.0 buffer.
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Ontario Tech University Chemistry, F23; Excel 11.14
MICROSOFT EXCEL - AN INTRODUCTION
This guide was originally written for Excel 2013, but the differences between Excel 2013 and
the current version should be minor so these instructions should still be, generally, applicable.
Excel (as well as other spreadsheet programmes) is a powerful computational tool with wide
application in all areas of science, in chemistry and in analytical and physical chemistry in particular.
Calculations on large quantities of data with Excel are quicker and far easier than on a calculator.
Because Excel will re-calculate results “instantly” if one of the input variables is changed, it can be
easily used to examine the effect(s) of changing variables. Likewise, if an error has been made
entering one of the input variables, the correction can be made simply by entering the new value and
all the subsequent calculations will be automatically corrected; much easier than re-doing all the
calculations by hand!
In junior courses Excel is used primarily for stoichiometric and titration calculations, for
statistical functions (such as AVERAGE and STDEV.S), for graphing experimental data and for
linear regression. In upper-year courses, more sophisticated calculations will have to be done. This
guide will provide very basic instruction on how to use Excel that will allow you to get started if you
are unfamiliar with it. There is much more to learn and whole books have been written on it (e.g.
“Excel for Chemists - A Comprehensive Guide”, 3rd Edition, E. Joseph Billo, Wiley, 2011). To
become truly proficient, you will have to explore, experiment and play with the programme (and use
the on-line help!). The introductory material that follows will be far more useful if you read it while
using Excel.
Navigation and Orientation
When Excel starts you are presented with a blank “worksheet” consisting of numbered rows
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(vertically) and labelled (with letters) columns (horizontally). Each intersection of a column and a
row is a “cell” which is designated using the column letter and the row number: for example, A1,
C4, F7. The individual cells hold data: numbers, mathematical formulae, text, etc.
At the top of the spreadsheet is the “Ribbon”. The Ribbon has several tabs (“File”, “Home”,
“Insert”, etc.). Clicking on each tab gives a set of related tools or operations. For example, clicking
on the “File” tab allows you to save your spreadsheet, open existing spreadsheets, print spreadsheets,
etc.
Beneath the Ribbon and to the right is the “formula bar” which shows the formula used to
calculate the value in the currently selected cell or, if no formula has been used, the contents of the
cell.
An Excel file can be organized into several “worksheets”. Normally, the data in a given
worksheet are related in some way. The different worksheets have different “tabs” at the bottom of
the spreadsheet. By default the tabs are labelled as “sheet 1", “sheet 2", “sheet 3" and so on. Each
tab can be given a more descriptive (and more useful) title by right-clicking on the tab, selecting
“Rename” and entering the new name. Collectively, the worksheets form a “workbook” and when
the file is saved all the worksheets are saved together in a single file or workbook. New worksheets
can be added to a workbook by clicking the “Insert Worksheet” button (immediately to the right of
the last worksheet tab), designated with a plus sign. Alternatively, you can right-click on a tab and
select “Insert”. Worksheets can be deleted by right-clicking on the tab and choosing “Delete”.
Worksheets can be moved (either within the workbook or to another workbook) by right-clicking
on the appropriate tab and choosing “Move or Copy...”.
Navigating around a worksheet is accomplished either by using the mouse or by using a

series of key strokes. You can go to a particular cell using the mouse simply by clicking on the cell
or by entering the cell address in the box immediately to the left of the formula bar. You can scroll
62
through the worksheet (vertically or horizontally) by clicking on the arrows in the scroll bars (at the
bottom and on the right of the worksheet) or by dragging the scroll bar in the appropriate direction.
Navigation with keystrokes is accomplished by:
Arrow Keys Move left, right, up or down by one cell

Ctrl + arrow key Moves to the last of the continuously
occupied cells in the chosen direction
Enter Move down one cell
Tab Move right one cell
Shift + Tab Move left one cell
Home Move to the beginning of a row
Ctrl + Home Move to cell A1
Page Up Move to the top of the window
Page Down Move to the bottom of the window
Alt + Page Up Move to the left of a window
Alt + Page Down Move to the right of a window
Ctrl + End Move to the last occupied cell (bottom right
hand corner)
Entering and Editing Data in a Worksheet
The data in cells can be either numbers, text, or formulae. As the data are entered into the
cell they appear in both the cell and in the formula bar. The entry of data in a cell is completed by
either pressing Enter (the cursor will move to the cell immediately below the active cell) or by
clicking the T on the formula bar. In the latter case the cursor remains on the active cell. To cancel
an entry (and restore the previous entry) click X on the formula bar.
Any data that contain text characters (any character other than the digits 0 - 9, decimal point,
63
or *, +, -, ^, $, %) are recognized by Excel as a “text” entry. By default, text entries are left-aligned
in a cell while numbers are right-aligned (alignment of data in cells can be changed by formatting
the cells). All data that are prefaced with a single quote are recognized as text by Excel. This is
useful if you want to enter numerals as text.
An equation (called a formula in Excel) can be entered in a cell. The cell will display the
value calculated by the formula while the formula itself will be shown in the formula bar at the top
of the worksheet. Formulae usually make use of values (or contents) in other cells (or ranges of
cells) by using cell references (e.g. A2 or C1:C8). A huge advantage of using Excel (or other
spreadsheets) is that if the value in a cell reference is changed the value calculated by the formula
in the cell is automatically updated. Formulae can contain numbers, cell references, arithmetic
operations (addition, subtraction, multiplication, division), parenthesis and Excel’s worksheet
functions (see below).
Some important points about entering formulae:

C A formula must begin with the equals sign (=).
C The arithmetic operations are: addition (represented with “+”), subtraction (-), multiplication
(*), division (/) and exponentiation (^).
C Other functions and operations can be represented using Excel’s built-in functions (see
below).
C The normal hierarchy of arithmetic operations applies. Parentheses can be used to override
the normal order of operations.
Consider the following examples in which the value for ‘x’ is in cell A1:
Mathematical Function Excel Formula

=2*A1+3
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Mathematical Function Excel Formula

=(2*A1^2+4*A1+1)/(A1+2)
=4.75+log10((1-A1)/(1+A1))
Formulae (or parts of formulae) can be copied from one cell to another by copying the formula from
the formula bar.
Pressing F2 allows editing of the data in the current cell. Data can be deleted, copied, etc.
from the formula bar.
Excel has over 300 built in worksheet functions. In Excel the worksheet function consists
of two parts: the name of the function and the argument of the function. The argument is the number
(or formula) to which the function is applied. In Excel, the argument is contained within a set of
parentheses. Within the set of parentheses the data (or cell references) can be separated by commas
(for individual data) or by colons (to indicate a range of cells). In this course the most important
functions are for mathematics and statistics (the argument is bolded):
Function Result
LN(number) Calculates the natural logarithm of a number
LOG10(number) Calculates the base-10 (common) logarithm
of a number
EXP(number) Calculates the value of ‘e’ raised to the power
of a number
SQRT(number) Calculates the square root of a number
AVERAGE(number1, number2,...) or Calculates the average value of the numbers

AVERAGE(cell reference 1:cell reference 2) given or of the specified range.
65
Function Result
STDEV.S(number1, number2,...) or Calculates the sample standard deviation of
STDEV.S(cell reference 1:cell reference 2) the numbers given or of the specified range.
T.INV.2T(probability, degrees of freedom) Returns the two-tailed inverse of the
Student’s t-distribution (see experiment 1,
CHEM 2030 / 2130)
F.INV.RT(probability, degrees of freedom Returns the inverse of the right-tailed F
[1], degree of freedom [2]) probability distribution (see experiment 1,
CHEM 2030/2130)
LINEST(known_ ys, known_xs, Returns an array of linear regression
const_logical, stat_logical) parameters (see below and Harris,
Quantitative Chemical Analysis)
SLOPE(known_ys, known_xs) Calculates the slope of the regression line y =
mx + b
INTERCEPT(known_ys, known_xs) Calculates the intercept of the regresson line y
= mx + b
Note: for LN( ), LOG10( ), EXP( ) and SQRT( ), “number” can also be a cell reference or a formula.
In the latter case Excel will apply the function to the result of the formula.
File Management
The commands needed for managing files are found under the File tab in the Ribbon.
The “Open” command can be used to locate and open existing files (workbooks). The “New”
command can be used to create a new workbook (by clicking “Blank workbook”). If you click on
“Recent”, a list of workbooks (Excel files) that have been worked on recently will appear. Clicking
on one of these file names will open the workbook.
66
A workbook currently being used can be saved by choosing “Save” from the File menu. This
will save the workbook with its current name. The same thing can be achieved by pressing Ctrl +
S. If you want to change the file name (or the folder in which it is stored), choose “Save As” and
choose the new folder and enter the new file name.
Editing a Worksheet
Often the first step in editing a worksheet is selecting cells. Selecting cells (or ranges of
cells) is accomplished in one of several ways:
• Click on the cell in one corner of the range and, while pressing the left mouse button drag
the cursor to the opposite corner of the selection
• Click on the cell in one corner of the range and hold down the Shift key and click a second
cell. All the cells between the row and column of the first cell and the row and column of
the second cell will be highlighted.
• A complete row (or column) can be selected by clicking on the number (letter) associated
with that row (column).
• If the desired range of cells is bounded by empty cells, the range of cells can be selected by
using Ctrl + Shift + arrow key to choose in the appropriate direction.
To choose more than one non-adjacent range, hold down the Ctrl key while choosing each separate
range. Once a range of cells has been chosen they will be highlighted and the cells can be copied,
deleted, or moved (see Editing a Worksheet below).
To insert a new column in a workbook, click a column letter to highlight the entire column.
Then, right click on the mouse and choose “Insert”. The new column will be placed to the left of
the highlighted column. To insert more than one column, highlight more than one column. All the
new columns will be inserted to the left of the first highlighted column. Rows can be inserted in
exactly the same way by clicking on and highlighting the row. New rows are inserted above the
highlighted row. Alternatively, rows and columns and can be inserted by clicking on the “Insert”
67
button on the “Home” tab. This will insert one row (above) or one column (to the left) at a time.
Deleting columns or rows is accomplished by highlighting the columns or rows, right

clicking the mouse and choosing “Delete”. Columns to the right of the deleted columns are shifted
to the left; rows below the deleted rows are shifted up. As with insertion the “Delete” button on the
Home tab can also be used.
Individual cells can be inserted by highlighting the cells, right-clicking on the mouse and
choosing “Insert”. You will be asked whether the existing cells should be shifted down or to the
right. You can also insert columns or rows in this way. Deleting individual cells works in a similar
way. Right-click the mouse and choose “Delete”. Now you will be asked whether existing cells
should be shifted up or to the left. Again, columns or rows can be deleted with this method.
Data in cells, ranges of cells, entire rows or entire columns can be copied to other locations
in the worksheet, to different worksheets in the same workbook or even to other workbooks. First,
select (highlight) the cell or range to be copied. Next, press Ctrl + C (or select “Copy” in the
Clipboard group on the Home tab). A dashed line will appear around the cells being copied. Select
the destination and press Ctrl + V (or select “Paste” from the Clipboard group). When performing
the Paste operation it is best to simply select the cell that will be in the upper left hand corner of the
destination range and then press Ctrl + V. If you wish to move data, then instead of using Ctrl + C,
use Ctrl + X (“Cut” from the Clipboard group).
When data are pasted into a new range, they are pasted with all the attributes (formatting,
formulae, etc.) of the original data. This may not always be desirable (e.g. you may wish to paste
the results of a formula as opposed to the formula itself). In such circumstances, choose “Paste
Special” from the Clipboard group and choose which attributes you wish to include.
If the data that are copied contain numbers or text, the values are duplicated in the new cell.
68
If, however, the copied cell(s) contain formulae, the formulae will be changed because (unless
specified otherwise) Excel uses relative cell referencing when formulae are copied. This concept
is probably best illustrated with an example. Suppose the formula in cell B1 is:
(5.1)
If this formula were copied into cells B2, B3, B4...., the formulae would be:
(5.2)
(5.3)
(5.4)
etc.
If it were copied into cell C1, the formula would be:
(5.5)
Relative cell referencing allows formulae to give the same results if columns or rows are inserted
or deleted or if the cell contents are moved. So, if a column were inserted between columns A and
B, the formula in cell C1 would be:
(5.6)
If the contents of A1 were moved to C3, the formula in B1 would be changed to:
(5.7)
Sometimes using relative cell references is not desirable; when a formula is copied or moved,
you may want a reference in the formula to remain fixed to one particular cell. This is done with
absolute cell referencing. To use an absolute cell reference preface the column letter and the row
number with a dollar sign (e.g. $A$1). If the formula in cell B1 is:
(5.8)
and it is copied to the cells B2, B3, B4..etc., each cell will have the same formula:
(5.9)
The referred cell in the formula does not change.
69
A mixed reference is a reference such as $A1 or A$1. In the former case the column
reference remains fixed, but the row reference will change. In the latter case, the column reference
can change while the row reference will be fixed.
Formatting Worksheets
Column width or row height can be changed by clicking on the Format button in the Cells
group of the Home tab of the Ribbon. Select “Column Width” or “Row Height” and enter the value
for the width or height. Alternatively (and probably easier), position the cursor over the separator
bar between two columns (on the right-hand side of the column whose width you want to change).
The cursor will change to a double-headed arrow: »º. Click the left mouse button and drag to the
right or left to increase or decrease the width. An analogous method can be used to change row
heights.
In order to make worksheets more readable it is sometimes desirable to “Hide” columns (or
rows). Click on the column label to highlight the column, right-click on the mouse and choose Hide.
The column will no longer be visible, but all the data and any cell references will be preserved. To
reveal a hidden column, highlight the columns on either side of the hidden column, right-click on
the mouse an choose “Unhide”. In a similar fashion, rows can be hidden and revealed.
Formatting of cells is accomplished by selecting the desired cells then right-clicking on the
mouse and choosing “Format Cells...”. Several tabs will then be presented:
Number: sets the format for numbers in the cell. This can be scientific notation, number of
decimal places etc.
Alignment: sets position of the data within the cell. “Wrap Text” ensures that all text in a
cell is visible within the width of the cell (the height of the cell will change as necessary).
“Merge Cells” will combine all the selected cells into a single cell.
70
Font: Allows you to set the font and font attributes (type, size, colour, bold, etc.).
Border: Allows you to set up the borders around the cell.
Fill: Allows you to set the colour of the background (not the data) in the cell.
Printing
Printing functions are found under the “File” tab in the Ribbon. You can choose to print a
selected worksheet, a selection of a worksheet or the entire workbook. You can also choose the
paper size and whether the print-out will be scaled (e.g., to allow it to fit on a single page).
Worksheets (and graphs) can be printed either in portrait or in landscape orientation.
Graphs (or Charts)
Graphs (or charts as Excel calls them) are one of the more important functions in Excel for
chemists1. Excel offers 11 standard chart types, most of which are of little or no use to chemists;
most chart types are useful for displaying financial information (and probably why they are called
“charts” as opposed to “graphs”). For chemistry students the most important chart type is the XY
(Scatter).
The first step in creating a chart is to select the data (a column of x data and a column of y
data) that will be plotted. You may have more than one set of y data for a given set of x data. Each
set of y data is a “series”. If the x data and y data are not adjacent, hold down the Ctrl key while
selecting the separate ranges.
1
Using Excel to create graphs for courses in chemistry is perfectly acceptable, but SigmaPlot may be a
better option, offering greater flexibility and wider regression options.
71
Once the data are selected, click on the “Insert” tab of the Ribbon and choose “ scatter (X,
Y) or bubble chart” from the “Charts” group. There are five types of scatter plot. Generally, the type
to choose is “Scatter” (the names of the types will appear if the cursor hovers over each icon). When
you choose one of the types, the chart will be created immediately as an “embedded chart” in the
active worksheet.
Alternatively, the graph may be created by choosing (ensure no data are selected or
highlighted) “Insert scatter (X, Y) or bubble chart” and choosing “scatter”. Click “select data” and
“Add” under “Legend Entries (Series).” You can give the series a name and then choose the X
values. Next, choose the corresponding Y values. Click “OK”.
The chart will appear with a light grey border around it to indicate the chart is “active”.
Three “Chart Tools” tabs will appear in the Ribbon at the top of the worksheet. These tabs are
“Design”, “Layout” and “Format”.
The “Design” tab allows you change the general appearance of the chart, to change the data
that are used for the plot and to move the chart to its own sheet (or to another worksheet). All graphs
in chemistry must have the following basic elements: a title and axis labels. This corresponds to
“layout 1" in Excel (the use of a legend is optional and can be deleted after the graph is created). To
change the layout of an existing chart, click on the chart to “activate” it (the light grey border will
form around it and the Chart Tools tabs will appear in the Ribbon), click the Design tab and make
the changes that you want. The chart will be automatically changed.
The “Layout” tab allows you to change the appearance of the graph in more detail. For
example, you can change the scales on the axes, change the appearance of the axes (e.g. axis title
position, tick-marks, gridlines, etc.), change the appearance of the plot area (e.g., borders, colour,
etc.), add a trendline and add error bars. The title of the graph can be changed by clicking on the title
of the graph (a solid outline box will form around the title) and typing the new title in the formula
72
bar. Likewise, the axis titles can be changed by clicking on the axis title and typing the new title in
the formula bar. Changes to the axis format can be made by clicking on “Axes” and choosing either
the vertical or the horizontal axis and then choosing “More Axis Options”. This will allow you to
change various aspects of the appearance of the axes. Under “Axis Options” you can set the
maximum and minimum values for the values of the axis (i.e. you can set the scale of the axis). You
can also set the interval between tick-marks (major and minor). In creating a graph, it is important
that the horizontal (‘x’) and vertical (‘y’) axis scales are chosen in such a way that the plotted data
fill the available space. Excel’s default choices for the scales of the axes will not necessarily ensure
this is the case. The “Layout” tab also allows you to add a “trendline” which is useful if the
experiment requires a regression analysis. The trendline option allows you to add the function of
best fit (along with the equation and regression coefficient, if desired) to the graph.
The “Format” tab contains “Shape” and “WordArt” options. The most useful option in this
tab is the “Size” group which (as the name implies!) allows you to change the size of the chart. The
size of the graph can also be changed by clicking on the chart (to activate it), positioning the cursor
over one of the sets of three dots in the chart border and clicking and dragging the cursor. If a set
of dots in the corner of the chart border is chosen, the chart is enlarged in both the horizontal and
vertical directions such that the ratio of height to width (the aspect ratio) remains constant.
LINEST and Linear Regression
The objective of a linear regression in a scientific analysis is to find the equation of the “line
of best fit” to the data. The general equation of a line is:
(5.10)
where ‘m’ is the slope of the line and ‘b’ is the intercept of the line. A regression analysis finds the
values of ‘m’ and ‘b’ of the line that best fits the data.
The LINEST function is the preferred method for performing linear regression in Excel.
73
Harris, Quantitative Chemical Analysis, has a very good example of how to use LINEST for linear
regression and that example is the basis for the description that follows.
To perform a linear regression with LINEST, you must first select (or highlight) a 3 row x
2 column block of cells (an array or matrix) in the worksheet. This array will contain the output of
the LINEST function. With the 3 x 2 array highlighted enter =LINEST in the formula bar. Excel
will first prompt you to choose the y-values. Choose these by clicking and dragging over the y-data
(the chosen range of data will appear in the formula bar). Enter a comma and Excel will prompt you
for the x-values. As with the y-data, click and drag over the x-data; again, the chosen range of the
data will appear in the formula bar. For both the x- and y-data the ranges may be entered directly
by entering the cell references in the formula bar. Enter another comma and Excel will ask you if
you wish to perform the fit with or without a constant (i.e., you can choose to set b = 02). If you wish
to force b to be zero, then enter “FALSE”. Otherwise, enter “TRUE”. Enter a final comma and
choose whether to output “STATS”. Entering “TRUE at this point will cause Excel to print out the
slope, intercept, regression coefficient and standard errors in the slope and intercept (in general, you
will want to have these data). To get the results of the linear regression (the line of best fit), press
Ctrl+Shift+Enter (simultaneously). The output from LINEST will be given in the 3x2 array you
previously highlighted as:
slope (m) intercept (b)

standard error of slope (sm) standard error of intercept (sb)
the coefficient of regression (R2) standard deviation of y estimate (sY.X)
From these results a confidence interval (CI) can be calculated for ‘b’ and ‘m’. The confidence
interval is a statement of the range in which the true value is expected to lie (at a given confidence
level, commonly 95%). It indicates that there is a 95% (for example) chance the true value lies
within the stated interval. The size of the range depends on the confidence level, the standard error
2
From the point of view of rigorous statistical theory, a regression analysis in which b is forced to zero
does not make sense. Statistical theory assumes that the relationship between X and Y is not deterministic, but
defining Y = 0 when X =0 (i.e. forcing b = 0) is deterministic and violates the assumptions of the theory.
74
and the ‘t’ value. The confidence intervals (CI) on ‘b’ and ‘m’ are given by:
(for the intercept) (5.11)
(for the slope) (5.12)
where tá, df is the two-tailed ‘t’ value. It can be found in Excel using the T.INV.2T(á,df) function.
‘á’ is given by:
(5.13)
where CL is the confidence level (most often 95%). ‘df’ is the degrees of freedom, given by:
(5.14)
where ‘n’ is the number of measurements (data points).
When calculating a “prediction” value for a given value X, the prediction interval on
is given by:
(5.15)
where:
(5.16)
= the average of all the X values of the data points

Xi = the X value of the ith data point
n = the number of data points.
75
One of the more common uses of the regression line is to calculate a predicted from an
observed Y value. The confidence interval on (for Y=mX + b, but not for Y = mX) is given by:
(5.17)
where
(5.18)
k = the number of replicate measurements of Y. k is most commonly 1

n = the number of data points
= the mean value of Y for the data points.
The coefficient of regression (R2) is “the fraction of the variance in the dependent variable
(Y) explained by the relationship with the independent variable” 3. If the R2 value is close to one,
a large proportion of the variance is ascribed to the relationship (i.e., the variables are highly
correlated). In many applications in chemistry (particularly in calibration), the model describing the
relationship between X and Y is normally very good, so we expect X and Y to be highly correlated
and the R2 value to be high. We expect the coefficient of regression to be close to one because our
(valid) model predicts the relationship. Consequently, the R2 value is not always the best assessment
of the quality of the fit or the data; other measures should be considered.
First, the relative errors in the slope and in the intercept should be examined. A linear
3
“Data Analysis for Chemistry: An Introductory Guide for Students and Laboratory Scientists”, p. 154, D.
Bryan Hibbert and J. Justin Gooding, Oxford University Press, 2006.
76
regression may have a very good R2 value but have high relative error in the slope and intercept,
especially if the number of data points is small. High relative errors in the slope and intercept imply
greater relative errors in any quantities predicted by the regression equation.
Second, a “residuals” plot can be constructed. This is a plot of vs. Xi where Yi is
the observed value at Xi and is the value predicted by the regression line at Xi. The plot should
show a random distribution of residuals about . If not, a linear fit to the data might
not be appropriate or the data might be suspect.
An alternative (although less desirable) to the LINEST function for linear regression is to use
the two Excel functions SLOPE and INTERCEPT. These functions will calculate the slope and
intercept of the line of best fit, but will not provide any of the statistics that are provided by LINEST.
The syntax for the SLOPE function is:
=SLOPE(known_ys, known_xs)
The data ranges can be entered either by clicking and dragging over the cells to select them or by
entering the cell references directly in the formula bar. The set of known ys and the set of known
xs is separated by a comma. The syntax for the INTERCEPT function is:
=INTERCEPT(known_ys, known_xs)
and its use is directly analogous to the SLOPE function.
The foregoing is not meant to be an exhaustive description of Excel. The best way to become
proficient using Excel is to practise.
77
Ontario Tech University Chemistry, F23; Equipment - 21.31
LOCKER EQUIPMENT LIST
Item Number
50 mL beaker 2
150 mL beaker 2
250 mL beaker 2
400 mL beaker 1
600 mL beaker 1
50 mL Erlenmeyer flask 1
10 mL graduated cylinder 1
Gas lighter 1
Crucible tongs 1
Thermometer, alcohol 1
Tweezers 1
Funnel, short stem, plastic 2

Watchglass, 100 mm 2
Medicine dropper 2
Scoopula 1
Stirring rod 1
Stirring rod with rubber policeman 1
Test tube brush, large 1

Test tube bush, small 1
Test tube rack 1
Test tube holder 1
Test tube, 20 mm x 150 mm 12
Wash bottle, 500 mL 1

Plastic bottle, 500 mL 1
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Ontario Tech University Chemistry, F23; Equipment - 21.31
Beakers Erlenmeyer Flasks Graduated Cylinders
Gas Lighter Thermometer Tweezers
Plastic Funnel Watchglass Medicine dropper
Scoopula Stirring Rods Test Tube Brushes
Test Tube Holder 20 x 150 mm Test Wash Bottle (l) and

Tubes and Rack Plastic Bottle (r)
Equipment photographs courtesy of Kaitlyn Yarrow
79
Ontario Tech University CHEM 1010, F23; Exp. 1-17.28
1. LABORATORY SAFETY AND ORIENTATION
Objectives
1) To become familiar with the safety equipment and procedures in the laboratory; 2) to recognize
the glassware and equipment in the lockers; 3) to prepare a standard solution of sodium chloride; 4)
CHEM 1010 - to practise using a pipette and to assess the variability of the volume delivered.
Introduction
This experiment is divided into three distinct “parts”: i) general laboratory safety and
orientation; ii) preparation of a standard solution; iii) pipetting practice (for CHEM 1010).
Everyone’s safety and security in a chemistry laboratory depend on each student knowing and
obeying the safety rules and working safely. The introductory pages of the manual and the First-Year
Laboratory Safety Video outline the safety rules and procedures. You should thoroughly familiarize
yourself with the safety rules and procedures of the laboratory in order to ensure your own safety and
the safety of others. The rules discussed here are applicable to all undergraduate chemistry
laboratories. Be aware that failure to comply with the safety rules may result in your dismissal from
a laboratory.
Two very important roles of the teaching assistant are to ensure all students are informed of
the safety rules of the laboratory and to ensure they are followed. At the beginning of this laboratory
period the teaching assistant will spend some time explaining the safety aspects of the laboratory,
pointing out safety equipment, and describing procedures.
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At the beginning of the semester, the technicians ensure that all the equipment on the locker
equipment list is in each locker and in good repair. After the safety talk, please check your locker.
If you discover anything is missing or broken, ask the teaching assistant or the technician for a
replacement. At the end of each laboratory period, make sure all the equipment that is supposed to
be in the locker (no more, no less!) is there and that your bench top has been wiped clean with a
damp sponge. The first-year chemistry technician or your TA may do inspections of lockers and
benches and if the workspace is dirty or equipment is missing, marks will be deducted from the last
student who used the locker (2.5 marks from the laboratory report).
In the second part of the experiment, students will prepare a “standard” solution - a solution
of accurately known concentration - of sodium chloride, NaCl. Many solutions in chemistry need
to have accurately known concentrations and are made by dissolving a known mass of a solid (the
solute) in a known volume of liquid (the solvent). These solutions are called primary standards and
are used to determine the concentrations of compounds in other solutions. Therefore, the primary
standard solutions must be made with great care and great accuracy. Preparing a standard solution
is a fundamental skill in chemistry. The calculation of the concentration of the chemical species in
the primary standard solution is straightforward. The number of moles of the compound is given by:
(1.1)
where:
mcompound = mass of the compound (in g)
Mcompound = molar mass of the compound (in g mol-1)
The concentration (in mol L-1) is given by:
(1.2)
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where:
Vsolution = volume of the solution (in L)
Concentration is an “intensive” property which means it does not change as the amount of solution
changes. In other words, the concentration of solute in 10.0 mL of the solution is the same as the
concentration in 20.0 mL of the same solution. An “extensive” property does change with the
amount of material. The number of moles of a compound is an extensive property: 2 g of NaCl
contain more moles of NaCl than 1 g of NaCl.
In this experiment a solution of ~0.1 mol L-1 NaCl will be prepared. Sodium chloride is not
commonly used as a primary standard, but the technique used to prepare the sodium chloride solution
is the same as would be used for making a primary standard.
Finally, in this laboratory period CHEM 1010 students will practise using a pipette. A
transfer pipette is used to transfer an accurate volume of liquid from one vessel to another. This is
a crucial aspect of performing a volumetric analysis and a technique that is employed extensively
in subsequent experiments in CHEM 1010 and in analytical chemistry.
All pipettes will have some systematic error associated with them. A 25.00 mL pipette, even
when used properly, will probably not deliver exactly 25.00 mL. It may deliver a volume that is
slightly higher or slightly lower. This “systematic error” can be measured by pipetting several
portions (“aliquots”) of a liquid of known density and measuring the mass transferred. The volume
transferred is calculated from the mass transferred using the density. Theoretically, if the pipette is
used exactly reproducibly, the volume, therefore the mass, transferred will be the same for each
aliquot. The difference between the volume actually transferred and the volume given on the pipette
is the systematic error and it can be taken into account in subsequent calculations (a process known
as “calibration”). In practice, variations in technique lead to variations in volume transferred. The
“variability” of the amount transferred (or “random error”) will be small if good technique is
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employed and high if poor technique is used. Good technique should lead to good agreement
amongst the volumes (or masses) transferred and poor technique leads to poor agreement. In this
experiment several aliquots will be pipetted to practise and assess technique. Good pipetting skills
are important in many aspects of analytical chemistry.
Procedure
The techniques used in this experiment are: open-pan balance, analytical balance, weight-by-
difference, pipetting, and preparing a standard solution.
In chemistry laboratories preparation of aqueous (“of, or in, water”) solutions requires

deionized water. It is provided in large carboys at the end of each laboratory bench.
Part I: Safety Orientation
You should watch the laboratory safety video posted on Canvas and review the safety rules
and procedures outlined at the beginning of the laboratory manual. In the first part of the laboratory
period the teaching assistant will briefly review the safety protocols and procedures that are outlined
in the introduction of this manual. You should answer and submit questions 1 - 8 on p. 92.
Part II: Locker Equipment Check
In the introductory pages of the laboratory manual is a list of equipment (p. 78) that should
be in each locker. Pictures are provided in the introduction to help you identify the equipment.
Review this list and ensure that all the equipment on the list is in your locker kit. If you do not
recognize a piece of equipment, ask the teaching assistant. If a piece of equipment is missing, ask
the teaching assistant or technician for a replacement.
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During the semester the technicians and teaching assistants may perform random checks of
the lockers to ensure all the equipment that should be in the lockers has been returned. If equipment
is missing, damaged or if there is extra equipment, you will have marks deducted from your report.
Likewise, if your work area is not cleaned after the experiment, you will lose marks.
Part III: Preparation of a Standard Solution of NaCl
For this part of the experiment you should watch the following videos: open-pan balance,
analytical balance, weight by difference, the meniscus, the volumetric flask, and preparing a standard
solution.
The volumetric flasks for preparing the NaCl solution will be provided in the laboratory. The
TA will point them out.
1. Place a 50 mL beaker on the open-pan balance and “tare” (zero) the balance. Add ~1.5 g of
NaCl to the 50 mL beaker.
2. Weigh the 50 mL beaker + NaCl on the analytical balance. The analytical balance will give
a mass to four decimal places. Write down all these numbers.
3. Pour the NaCl into a clean 250 mL beaker. Be careful not to spill any of the NaCl. It is more
important not to spill any of the NaCl than to get it all out of the 50 mL beaker.
4. Re-weigh the now (mostly) empty 50 mL beaker on the same analytical balance. Again,
write down all the numbers. The difference between this number and the number recorded
in step two is the mass of NaCl transferred. This technique to determine a mass is “weight-
by-difference”.
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5. Add ~125 mL of deionized water to the 250 mL beaker (this volume does not have to be
measured accurately).
6. Using a glass stirring rod, carefully stir the solution until all the NaCl dissolves. Do not
splatter the solution. If, at any point, you remove the stirring rod from the beaker, rinse it
with deionized water from a wash bottle so that the rinsings flow into the beaker. This
ensures no NaCl is lost from the beaker.
7. Obtain a 250.0 mL volumetric flask and rinse it thoroughly three times with small portions
of deionized water.
8. Now the quantitative transfer of the NaCl solution in the beaker must be performed. You
need to transfer all the dissolved NaCl to the flask.
9. Place a funnel in the neck of the volumetric flask and, using the stirring rod as a guide,
carefully pour the NaCl solution so that it runs down the rod through the funnel and into the
flask. Do not place the stirring rod on the bench once you have completed this step; put it
in the beaker.
10. Using a wash bottle carefully wash the inside walls of the beaker with deionized water.
Using the stirring rod as you did in step 9, transfer the washings to the volumetric flask.
Repeat the washings twice more. Do not use too much deionized water at this stage - the
total volume added to the flask must be less that 250 mL!
11. Rinse the end of the stirring rod so that the rinsings go through the funnel into the flask.
12. Finally, rinse the inside surface of the funnel with deionized water.
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If steps 9 - 12 have been performed properly, all the NaCl transferred to the 250 mL beaker
(step 3) should have been transferred to the flask.
13. Carefully fill the flask with deionized water so that the bottom of the meniscus is exactly on
the mark. If this is done properly, there will be 250.0 mL of solution in the flask (within the
systematic error in the flask). The bottom of the meniscus cannot be above nor below the
mark. Be very careful as the solution nears the mark. The last few millilitres should be
added with a medicine dropper. If the flask is overfilled, the procedure should be started
again. If you overfill the flask, consult with a TA before proceeding.
14. Once the solution is prepared, stopper it and have the teaching assistant check your work.
The stopper needs to fit snugly but should not be put in with excessive force. To do so, risks
injury or jamming the stopper in the neck of the flask.
15. Invert the flask 20 - 25 times (while holding the stopper in place with your hand) to ensure
thorough mixing.
Part IV: Use of the Transfer Pipette (CHEM 1010 only)
For this part of the experiment you should watch the video on transfer pipettes.
25.00 mL pipettes will be provided in the laboratory. The teaching assistant will point them
out.
1. Obtain a 25.00 mL transfer pipette and rinse it three times with tap water. The pipette is
rinsed by using the bulb to half fill the pipette, holding the pipette horizontally and rotating
it to allow the liquid inside to contact the inner surface of the pipette. Allow the liquid to
drain through the tip of the pipette. Do NOT pour the liquid out the top of the pipette or
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allow liquid to enter the bulb.
2. Collect ~150 mL of deionized water in a 250 mL beaker. Rinse the pipette once with
deionized water.
3. Weigh an empty 250 mL Erlenmeyer flask on a tared (zeroed) open-pan balance (two
decimal places) and record the mass.
4. Pipette 25.00 mL of deionized water into the flask. Tare an open-pan balance and weigh the
flask + water.
5. Repeat step 4 four more times (for a total of 5 transfers). Good pipetting technique should
give nearly identical masses for each transfer.
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Experiment 1 - Laboratory Safety and Orientation
Name: _______________________
Course: _______________________
Day: _______________________
Time: _______________________
TA Name: _______________________
You must submit this sheet with your report.
88
Ontario Tech University CHEM 1800U, F23; Exp. 1-17.28
89
Ontario Tech University CHEM 1800U, F23; Exp. 1-17.28
90
DATA SHEET - Laboratory Safety and Orientation
If you are submitting your lab report electronically, you must scan or photograph all the data sheets
with your data as recorded in the laboratory period, signed and dated by the teaching assistant, and
submit them with your report.
Student Name: _____________________________

Student Number: _____________________________
Date: _____________________________
TA Signature: _____________________________
Part III - Preparation of Standard Solution
mass of 50 mL beaker + NaCl / g: ____________________________________

mass of “empty” 50 mL beaker / g: ____________________________________
mass of NaCl used / g: ____________________________________
Final volume of solution / L: ____________________________________
Checked by the TA (TA initials): ____________________________________
Part IV - Pipette Practice (CHEM 1010 only)
First Aliquot Second Third Fourth Fifth Aliquot

Aliquot Aliquot Aliquot
Mass before
transfer / g
Mass after
transfer / g
Mass
transferred / g
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Calculations and Questions
Part I - Safety Orientation
1. Using the laboratory template provided (see pp. 89 - 90) for your room, indicate the
location(s) of:
a. The fire extinguisher(s)
b. The eyewash stations
c. The first aid kit
d. The fire blanket
e. The spill kits
2. List five (5) restrictions and / or requirements for clothing in a chemistry laboratory.
3. Students must never pipette by mouth. Why not?
4. Sadio is a student working in a first-year chemistry laboratory. When making a solution of

sodium carbonate, he weighs out too much. What should he do with the excess sodium
carbonate? Why?
5. Kaitlyn needs to store a solution in her laboratory locker for a week. What information must
be on the label? What other information should be on the label?
6. What is the proper way to dispose of broken glass?
7. What steps should you take if the fire alarm sounds?
8. What are the appropriate treatments for i) cuts and ii) minor burns?
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Part III - Preparation of Standard Solution
1. Calculate the concentration of the NaCl solution in mol L-1 and with the correct number of
significant digits.
2. Why is it desirable to use the same analytical balance to weigh the weighing vial + NaCl and
to weigh the “empty” weighing vial?
3. Avoiding spilling the NaCl in the weighing vial is more important than getting all of the
NaCl out of the vial. Why?
4. When transferring the dissolved NaCl from the beaker to the volumetric flask, all the
glassware (beaker, stirring rod, funnel) are thoroughly rinsed with deionized water. Why?
Part IV - Pipette Practice (CHEM 1010 only)
1. Calculate the average mass of water transferred with the pipette.
2. Assuming the density of water is 1.00 g mL-1, calculate the average volume of water
transferred.
3. Calculate the percent error between the average volume transferred and the volume stated
on the pipette (25.00 mL).
4. Describe at least three flaws in your technique that may have led to variability in the volume
of water transferred.
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2. DETERMINATION OF STOICHIOMETRY BY TITRATION
Objectives
1) To practise using the pipette and the burette, two essential pieces of volumetric glassware; 2) to
practise stoichiometry calculations; 3) to determine the stoichiometric coefficients for the reaction
between potassium iodate, potassium iodide and hydrochloric acid.
Introduction
The “titration” is a very common method of analysis in chemistry to determine the

concentration of a reactant in a solution. In a titration a solution of a reactant in a burette is slowly
added to an accurately known volume of a solution of a second reactant in a flask. The concentration
of one of the reactants must be accurately known. The reactant of unknown concentration is called
the “analyte”. The solution in the burette is called the “titrant”. Once the analyte is completely
consumed (the reaction is “complete”), the addition of the titrant is stopped and the volume of added
titrant is determined. Because the concentration and volume of one of the reactants and the volume
of the other reactant are all accurately known, the concentration of the analyte can be calculated
using the stoichiometry of the reaction.
To know when the reaction is complete - when to stop adding titrant - a small amount of
“indicator” is added to the flask. An indicator is a substance which changes some physical property,
most often its colour, when the reactant in the flask is completely consumed. At the “end point” the
indicator changes its property and titrant is no longer added - the titration is “ended”. The
“equivalence point”, however, is what the analyst really wants to know; it is the point at which the
two reactants are present in their stoichiometric ratio. The “end point” and the “equivalence point”
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are not, to be completely rigorous, the same thing. If the indicator is properly chosen, the difference
is very small and in first-year experiments the equivalence point and the end point are assumed to
be the same. A more detailed examination of this question is undertaken in advanced analytical
chemistry courses.
In this experiment, titration is used to determine the coefficients of a chemical equation for
the reaction between potassium iodate (KIO3), potassium iodide (KI) and hydrochloric acid (HCl).
When these three species are mixed, iodine is produced and the solution turns dark brown. The
unbalanced net ionic equation is:
IO3-(aq) + I-(aq) + H+(aq) ÿ I2(aq) + H2O(l) (2.1)
An accurately known number of moles of IO3- (as potassium iodate) is mixed with an excess of I- (as
potassium iodide) and H+ (as hydrochloric acid). The IO3- is the limiting reagent and it is completely
consumed. Therefore, the number of moles of IO3- consumed by the reaction is the same as the
number of moles of IO3- added.
The iodine atoms produced in reaction (2.1) come from both the iodate and the iodide. In
each species (the iodate or the iodide) the number of moles of iodine atoms equals the number of
moles of the species because the mole ratio of I to IO3- is 1:1 and the mole ratio of I to I- is 1:1.
Therefore, the total number of moles of iodine atoms is given by:
(2.2)
We find from the total number of moles of molecular iodine ( ) produced in reaction
(2.1). is found by titration (see below). The number of moles of iodate consumed in reaction
(2.1), , is the same as the number of moles of iodate added because iodate is the limiting
reagent. Therefore, the number of moles of iodide ( ) that reacted can be calculated. Having the
numbers of moles of IO3-, I- and I2 allows the calculation of the mole ratio IO3-: I- : I. Finally, the
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coefficients for H+ and H2O in reaction (2.1) are found by inspection.
The number of moles of molecular iodine, , produced by reaction (2.1) is determined by
titration. Iodine reacts with thiosulphate according to:

I2(aq) + 2S2O32-(aq) ÿ S4O62-(aq) + 2I-(aq) (2.3)
S2O32-(aq), S4O62-(aq) and I-(aq) are all colourless while I2(aq) is dark brown. At the end point the
colour disappears because all of the I2(aq) has been consumed. As the thiosulphate is added to the
iodine solution, the colour fades from dark brown to light yellow because the amount of iodine
decreases. Unfortunately, the disappearance of the colour is gradual, therefore the end point is hard
to see. To solve this problem a small amount of starch is added once the solution is pale yellow.
Starch and iodine form an intensely blue complex. Once all the iodine is consumed (the end of the
reaction) the complex no longer exists and the colour disappears. The change from blue to
colourless is very sudden (or “sharp”), so the end point is very easy to detect. The sharpness of the
end point makes this a popular titration in analytical chemistry. The starch must not be added too
early because the colour change is then no longer sharp and the end point is difficult to see.
Apparatus and Materials
1) 50 mL burette; 2) funnel; 3) 250 mL beaker; 4) 400 mL beaker; 5) 5.00 mL pipette; 6) pipette

bulb; 7) 150 mL beaker; 8) 50 mL beaker; 9) 3 x 250 mL Erlenmeyer flasks; 10) wash bottle; 11)
~0.2 mol L-1 Na2S2O3; 12) ~0.12 mol L-1 KIO3; 13) 0.5 mol L-1 KI; 14) 1.0 mol L-1 HCl; 15) starch
indicator.
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Safety
• Most of the solutions used here are quite dilute, therefore not particularly dangerous.
• HCl spills should be neutralized with a small amount of sodium bicarbonate and then
cleaned up with a sponge.
• Small spills can be cleaned up with a sponge. Wear gloves. Rinse the sponge afterwards
with plenty of tap water. Wipe down the bench top. Clean hands thoroughly.
• In the event of eye exposure - rinse thoroughly with running water for 15 minutes (30
minutes for HCl) and seek medical attention immediately. Notify teaching assistant /
technician / senior laboratory instructor as soon as possible. Other students should stop
their experiments.
• In the event of skin exposure - rinse thoroughly with cool running water for 15 minutes. If
irritation develops, seek medical attention.
• Accidental mixing of HCl and S2O32- will precipitate sulphur and release SO2 gas. The
solution will turn cloudy and release a foul smell (from the SO2). Such solutions should be
disposed of in the fume hood in the waste bucket provided (with the thiosulphate waste)
immediately.
• KIO3 is an oxidizing agent. Waste KIO3 solutions should be collected separately from the
other solutions in the waste vessels provided. Waste HCl can be flushed down the sink with
plenty of water. Waste thiosulphate should be collected in the waste vessels provided. The
waste solutions from the titration should be collected in the waste vessels provided.
Thiosulphate and titration waste can be collected together.
97
Procedure
You should review the techniques used in this experiment: pipetting, the burette and titrating
which are described in the introductory pages of the laboratory manual; Videos: transfer pipettes,
titrating.
1. Obtain a 50 mL burette and rinse it three times with small amounts (~10 mL) of tap water.
To rinse the burette, ensure the stopcock is closed, add the water (from a beaker), hold the
burette almost horizontally and rotate the burette so that the entire inner surface is rinsed.
Allow some water to drain through the stopcock so that there are no bubbles in the tip. Close
the stopcock and pour the rest of the water out the top of the burette.
Be careful not to knock the tip against the bench - it is fragile and it may break.
2. In a similar fashion, rinse the burette three times with deionized water.
3. Collect ~100 mL of the standard Na2S2O3 solution in a clean, dry beaker. The beaker must
be dry otherwise the Na2S2O3 solution will be diluted, changing its concentration. Record
the concentration of the Na2S2O3 solution. Do not take more than 100 mL without the
permission of an instructor.
4. Using a small amount of the Na2S2O3 solution rinse the inner surface of a funnel (rinsing into
a waste beaker). Use this funnel to add Na2S2O3 your burette.
5. Rinse the burette three times with small portions of the Na2S2O3 solution in the same manner
you rinsed the burette with deionized water. Drain a portion of the Na2S2O3 solution through
the stopcock into a waste beaker. With the stopcock closed, pour the remainder out the top
of the burette into a waste beaker.
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6. Fill the burette with your Na2S2O3 solution. While doing so, make sure the top of the burette
is below eye-level. If the top of the burette is above eye-level, solution may be spilled on the
face. Fill the burette to just above the zero mark. Remove the funnel and drain some
Na2S2O3 through the stopcock. Ensure no bubbles are in the tip of the burette. If the level
of the Na2S2O3 is below the zero mark, this does not matter. The level of the Na2S2O3 must
not be above the zero mark. If you spill any Na2S2O3 on the outside of the burette, be sure
to clean it off with some paper towel.
7. Record the volume on the burette to two decimal places. This will require you to estimate
the position of the meniscus between two graduations on the burette (failure to record the
volume to two decimal places will result in the loss of marks). This reading is the “initial”
volume reading of the Na2S2O3 solution. Remember, the scale reads from 0 at the top to
50.00 mL at the bottom and represents the volume dispensed from the burette, NOT the
volume remaining in the burette. You do not have to do any arithmetic; simply record this
initial volume.
8. Obtain a 5.00 mL pipette. Rinse it three times with tap water followed by three rinsings with
deionized water. To rinse the pipette use the bulb to draw enough liquid into the pipette to
half fill, roughly, the wide part of the pipette. Ensure the tip of the pipette remains
submerged otherwise liquid will be sucked into the pipette bulb. Remove the bulb, place
your finger over the end and hold the pipette horizontally. Remove your finger and rotate
the pipette to thoroughly rinse the inner surfaces of the pipette. Allow the liquid to drain
through the tip of the pipette. Do NOT pour the liquid out the top of the pipette or allow
liquid to enter the bulb.
9. 30 mL aliquots of standard KIO3 solution (of accurately known concentration) will have been
dispensed into test tubes. Obtain one of these test tubes and pour the solution into a clean,
dry 150 mL beaker. It is important that the beaker be dry so the KIO3 is not diluted. Record
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the exact concentration of the KIO3 solution. You will not be able to get more KIO3 so do
not waste it.
10. Pour ~10 mL of the KIO3 solution into a clean, dry 50 mL beaker. Do not use a larger
beaker otherwise it will be difficult to ensure the pipette tip is submerged while drawing
liquid into the pipette. Using this portion of the KIO3 solution, rinse the 5.00 pipette three
times (as in step 8). Throw away any extra KIO3 solution in the 50 mL beaker.
11. From the 150 mL beaker pipette exactly 5.00 mL of the KIO3 solution into a clean 250 mL
Erlenmeyer flask. The flask does not need to be dry.
12. Add 10 mL of 0.5 mol L-1 KI and 10 mL of 1.0 mol L-1 HCl to the Erlenmeyer flask. Be sure
to add the acid last. Swirl to mix well. I2 should be produced immediately turning the
solution a deep, reddish brown.
13. Immediately place the flask underneath the burette and titrate the solution with the Na2S2O3.
The tip of the burette should be just below the top of the flask. This ensures all the titrant
run out of the burette ends up in the flask. Open the stopcock to allow Na2S2O3 to flow into
the flask. As the Na2S2O3 flows into the flask, the flask should be continuously swirled to
promote good mixing.
14. Initially, the Na2S2O3 can be added quite quickly. As the Na2S2O3 solution is added the
brown colour will lighten becoming, eventually, a pale yellow. At this point add 2 - 3 drops
of starch indicator. The solution should turn a deep blue. If the starch is added a bit too early
the solution may turn “mucky” green. The titration can still be done, but this is not ideal.
Do NOT add the starch at the beginning of the titration!
15. The end point is very “sharp” - the colour will change suddenly - and indicated by the
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complete discharge of the colour (blue to colourless). As you approach the end point you
should slow down your additions of Na2S2O3. Close to the end point you should add Na2S2O3
drop-wise or even (if you are skilled!) half drops at a time. At this point touch the tip of the
burette to the side of the flask and use the wash bottle to wash down the sides of the flask.
This ensures any Na2S2O3 dispensed from the burette reacts with the I2.
16. Once the end point has been reached, stop adding Na2S2O3. Wait a few moments and record
the final volume of Na2S2O3 (again, to 0.01 mL). The volume of Na2S2O3 added to the flask
is the difference between the final and initial volumes.
17. First titrations are often not as accurate as subsequent ones. The first titration should give
you a reasonable idea about the volume of Na2S2O3 that will be used in subsequent titrations.
Do at least three titrations (starting from step 11). Continue the titrations until two titration
volumes agree within ±0.1 mL, but do not do any more than five titrations. The number of
titrations you can perform is limited by the KIO3 that you have - do not waste it!
18. Before each titration ensure the amount of Na2S2O3 remaining in the burette is sufficient for
the titration. If you have any doubt about whether there is sufficient Na2S2O3, fill the burette.
19. If you must do more than three titrations, empty the flasks, rinse well with tap water followed
by deionized water and use the flasks again. The flasks do not need to be dry. Do not take
more KIO3 solution without the instructor’s permission.
20. Average all the titration volumes (titres) that are within 0.1 mL and use the average volume
in the calculations.
21. When you have finished, drain the burette and rinse it 3 times with tap water followed by 3
rinsings with deionized water. Leave the stopcock open and clamp the burette upside down
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in the stand.
22. Rinse the pipette and flasks 3 times with tap water followed by 3 times with deionized water.
102
Experiment 2 - Stoichiometry by Titration
Name: ____________________________
Day ____________________________
Time: ____________________________
TA Name ____________________________
103
DATA SHEET - Stoichiometry by Titration
Student Name: _____________________________

Student Number: _____________________________
Date: _____________________________
TA Signature: _____________________________
Volume of 0.5 mol L-1 KI / mL: _____________________________
Volume of 1.0 mol L-1 HCl / mL: _____________________________
Concentration of KIO3 / mol L-1: _____________________________
Volume of KIO3 per titration / mL: _____________________________
Concentration of Na2S2O3 / mol L-1: _____________________________
Indicator: _____________________________
Colour change at end point: _____________________________
Volumes of Na2S2O3
I II III IV
Final Volume / mL
Initial Volume / mL
Volume of Na2S2O3 / mL
Average Volume of Na2S2O3 (average of volumes within ±0.1 mL):_______________________
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1. Calculate the number of moles of Na2S2O3 in the average volume of Na2S2O3. Using
equation (2.3) calculate the number of moles of molecular iodine. This is the same as the
number of moles of molecular iodine produced by reaction (2.1).
2. All of the iodine produced by reaction (2.1) is in the form of I2 (molecular iodine). Calculate
the number of moles of atomic iodine (I) produced by reaction (2.1).
3. Calculate the number of moles of KIO3 consumed by reaction (2.1). Remember, it is the
limiting reagent.
4. Calculate the number of moles of I- consumed by reaction (2.1).
5. Determine the ratio for IO3- : I- : I2 for reaction (2.1). Express this as a ratio of integers.
6. Using the results for question 5 complete the balancing of:

____IO3-(aq) + ____I-(aq) + ____H+(aq) ÿ ____I2(aq) + ____H2O(l)
7. In this experiment you were given a precise concentration for the KIO3 solution but not for
the KI solution. Explain why it is not necessary to know precisely the number of moles of
KI added.
8. A funnel is often used to fill the burette with titrant, but is removed before the titration is
begun. Why must the funnel be removed?
9. Volumetric glassware (pipettes, burettes, volumetric flasks, etc.) is usually designated as “TC
at 200C” or “TD at 200C”. What do “TC” and “TD” indicate? What is the difference?
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3. ANALYSIS OF AN ALKALI METAL CARBONATE BY BACK

TITRATION OF HYDROCHLORIC ACID
Objectives
1) To further practise the techniques of volumetric analysis;; 2) to become familiar with the
technique of “back-titration”; 3) to determine the unknown alkali metal in a carbonate salt.
Introduction
In the “Stoichiometry by Titration” experiment the “titration” was introduced. That titration
was a “direct titration” - the titrant (thiosulphate) was added directly to the analyte (iodine) until the
end point was reached. In a “back titration” the amount of the analyte is found indirectly. At the
start an excess and accurately known amount of a reagent is added to the analyte. Some of the
reagent reacts with the analyte according to a known reaction and the analyte is completely
consumed. Some of the reagent is left over - the excess. Next, titrant is added to the excess amount
of the reagent to determine how much of it remains. Knowing how many moles of the reagent were
added originally (nadded) and how many moles remain (the excess, nexcess), yields the moles that reacted
with the analyte (nreacted):
(3.1)
Once nreacted is known the moles of analyte can be calculated. The back titration determines nexcess.
Back titrations are useful when the end point of the back titration is easier to see than the end point
of the direct titration or when an excess of reagent is required to drive the reaction with the analyte
to completion.
In this experiment the identity of an alkali metal (lithium, sodium, or potassium) carbonate
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will be determined by calculating its molar mass. This analysis could be done by a direct titration
because the reaction between hydrochloric acid (HCl) and the alkali metal carbonate (M2CO3):
M2CO3(s) + 2HCl(aq) ÿ 2MCl(aq) + CO2(g) + H2O(l) (3.2)
is rapid and goes to completion with a stoichiometric amount of HCl. In fact, this reaction (with M
= Na) is often used to standardize HCl solutions. However, methyl orange is the indicator and the
colour change - from yellow to orange - is difficult to see for an inexperienced titrator (and even for
some experienced ones!). Therefore, the analysis is ideally suited to a back titration.
In this experiment an accurately known, excess number of moles of HCl is added to a known
mass of the alkali metal carbonate. Some of the HCl reacts with the alkali metal carbonate
(according to equation (3.2)) and some of the HCl is left over. The resulting solution is transferred
to a 250.0 mL volumetric flask and diluted with water to give precisely 250.0 mL of solution. This
solution contains all the excess HCl from the reaction with the alkali metal carbonate. 25.00 mL
aliquots (portions) of this solution are titrated with aqueous sodium hydroxide of accurately known
concentration. Hydrochloric acid reacts with sodium hydroxide (NaOH) according to:
HCl(aq) + NaOH(aq) ÿ NaCl(aq) + H2O(l) (3.3)
The indicator for the titration reaction is bromothymol blue which changes from yellow to green at
the end point.
The concentration of the HCl in the 25.00 mL aliquot is determined from the titration results
(reaction (3.3)) and this concentration is the same as the concentration of HCl in the 250.0 mL
volumetric flask. The volume of the flask is precisely known (250.0 mL), so the number of moles
of hydrochloric acid in the flask can be calculated. This value is the number moles of hydrochloric
acid remaining after the reaction with the alkali metal carbonate. In other words it is the excess
number of moles of HCl (nexcess). Because the number of moles of HCl originally added to the alkali
metal carbonate is known and the number of moles of HCl remaining (the excess) is known, the
number of moles of HCl that must have reacted with the alkali metal carbonate can be calculated:
(3.4)
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The HCl is in excess, so the alkali metal carbonate is the limiting reagent in reaction (3.2).
Therefore, the number of moles of the alkali metal carbonate can be calculated from the number of
moles of HCl that reacted with the alkali metal carbonate. Once the number of moles of alkali
metal carbonate is known, the molar mass of M2CO3 can be calculated using the known mass of
metal carbonate:
(3.5)
From this molar mass, the alkali metal can be identified.
Apparatus
1) 50 mL beaker; 2) 250 mL beaker; 3) stirring rod; 4) wash bottle; 5) 150 mL beaker; 6) 10.00 mL
pipette; 7) pipette bulb; 8) plastic funnel; 9) 250.0 mL volumetric flask; 10) eyedropper; 11) 25.00
mL pipette; 12) 250 mL (or 125 mL) Erlenmeyer flasks; 13) 50 mL burette; 14) unknown alkali
metal carbonate (M2CO3); 15) 1.0 mol L-1 hydrochloric acid; 16) bromothymol blue indicator; 17)
0.05 mol L sodium hydroxide
Safety
The chemicals and concentrations used in this experiment are, for the most part, fairly
innocuous.
Unknown carbonate
• Spills can be cleaned up with a dust pan and brush and disposed in the regular garbage.
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Wipe down the area with damp paper towel and wash hands thoroughly afterwards.
• Skin exposure: remove solid from skin. Wash area thoroughly with water.
• Eye exposure: immediately flush area with copious quantities of running water for at least
15 minutes. Seek medical attention. Notify teaching assistant, technician or senior
laboratory instructor.
1.0 M HCl
• Spills should be treated with a small amount of sodium bicarbonate to neutralize the acid.
Wear gloves and wipe up the spill with paper towel. Rinse area with water. Wash hands
with soap and water.
• Skin exposure: immediately flush skin with cool running water. Continue for 15 minutes.
Wash area thoroughly with soap and water. If irritation develops, seek medical attention.
• Eye exposure: Immediately flush with running water for at least 30 minutes. Seek medical
attention. Notify teaching assistant, technician or senior laboratory instructor. Other
students should stop working.
0.05 M NaOH
• Spills should be treated with a small amount of acetic acid to neutralize the base. Wear
gloves and wipe up the spill with paper towel. Rinse area with water. Thoroughly was
hands with soap and water.
• Skin exposure: immediately flush skin with cool running water. Continue for 15 minutes.
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Wash area thoroughly with soap and water. If irritation develops, seek medical attention.
• Eye exposure: Immediately flush with running water for at least 30 minutes. Seek medical
attention. Notify teaching assistant, technician or senior laboratory instructor. Other
students should stop experiment.
Waste
• The waste from this experiment is almost completely innocuous.
• The solution resulting from the reactions should be an almost neutral solution of MCl. It can
be put down the sink with plenty of water.
• Extra HCl and NaOH can be mixed together (to partially neutralize) and then put down the
sink with plenty of running water.
Procedure
Techniques used in this experiment are: the open-pan balance, the analytical balance, weight
by difference, transfer pipette, burette and titrating. Videos of the techniques are: open-pan balance,
analytical balance, weight by difference, transfer pipettes, titrating.
Part I: Reaction of Alkali Metal Carbonate with Excess Hydrochloric Acid.
1. Obtain a clean, dry 50 mL beaker and place it on the open-pan balance. Tare the balance and
transfer ~0.5 g of your unknown alkali metal carbonate (M2CO3) into the 50 mL beaker.
Note the code number of the unknown.
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2. Weigh the 50 mL beaker + solid on the analytical balance and record the mass. Be sure to
write down all the numbers!
3. Pour the solid into a 250 mL beaker - be careful not to spill any - and re-weigh the now
(mostly) empty 50 mL beaker on the same analytical balance used in step 2. It does not
matter if all the solid gets into the 250 mL beaker; it is more important not to spill any. The
difference between the masses recorded in step 2 and step 3 gives the mass of alkali metal
transferred to the 250 mL beaker (“weight-by-difference”).
4. Add ~100 mL of deionized water to the beaker. The solid may or may not dissolve easily
depending on which alkali metal carbonate it is. A stirring rod can be used to facilitate
dissolution, but if it is removed at any point, it must be rinsed so that no sample is lost from
the beaker. Avoid getting solid on the sides of the beaker. Solid on the sides can be rinsed
down with a little deionized water. Any undissolved solid will dissolve when the HCl is
added (see below).
5. Using a clean, dry 150 mL beaker obtain ~60 mL of standardized ~1 mol L-1 hydrochloric
acid (HCl). The beaker must be dry to avoid diluting the HCl and changing its concentration.
Record the exact concentration of the hydrochloric acid.
6. Obtain a 10.00 mL pipette. Rinse it once with tap water followed by three rinsings with
deionized water. To rinse the pipette use the bulb to draw enough liquid into the pipette
(from a small beaker) to half fill (roughly) the wide part of the pipette. Remove the bulb,
place your finger over the end and hold the pipette on its side. Remove your finger and rotate
the pipette to thoroughly rinse the inner surfaces of the pipette. Allow the liquid to drain
through the tip of the pipette. Do NOT pour the liquid out the top of the pipette or allow
liquid to enter the bulb.
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7. Decant (pour) ~20 mL of the HCl solution into a clean, dry 50 mL beaker. If you use a
larger beaker, it may be difficult to pipette the HCl from it. Rinse the 10.00 mL pipette three
times with ~5 mL portions of the HCl solution. After rinsing the pipette dispose of the
remaining HCl in the 50 mL beaker and rinse the 50 mL beaker three times with small
portions of the standardized HCl (in the 150 mL beaker). Discard the rinsings. Pour ~25 mL
of the HCl in the 150 mL beaker into the 50 mL beaker.
8. Pipette 20.00 mL (10.00 mL, twice) of the ~1 mol L-1 HCl into the beaker containing the
metal carbonate solution. The exact volume of added HCl must be known. The solution will
effervesce gently as the carbonate reacts with the acid to form CO2.
9. Once the HCl has been added, stir the solution gently with a glass stirring rod to expel any
CO2. None of the solution can be lost, so if you remove the stirring rod, be sure to rinse it
into the beaker with deionized water.
10. Obtain a 250.0 mL volumetric flask and rinse it three times with deionized water. The flask
does not need to be dry.
11. You are now ready to begin the quantitative transfer of your solution to the 250.0 mL
volumetric flask.
12. Place a clean (rinse with deionized water) funnel in the neck of the volumetric flask. Using
the stirring rod as a guide, carefully pour the solution so that it runs down the rod through the
funnel into the flask. Do not, at any point, place the stirring rod on the bench; it should be
returned to the beaker.
13. Using your wash bottle, thoroughly wash the inside wall of the beaker. Transfer the
washings to the volumetric flask using the stirring rod and funnel (just as you did in step 12).
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Repeat the washing and transfer twice more (for a total of 3 times). Be careful not to use too
much water in this and all rinsings. The total volume transferred to the flask must be less
than 250 mL!
14. Rinse the end of stirring rod using your wash bottle such that the rinsings flow through the
funnel into the volumetric flask.
15. Finally, using the wash bottle, rinse the inner surface of the funnel.
If steps 12 - 15 have been performed correctly, you will have successfully transferred all the
solution to the volumetric flask.
16. Now for the crucial step! Carefully fill the volumetric flask so that the bottom of the
meniscus lies exactly on the graduation. It must not be above or below the mark. If the
meniscus is above, you may have to start again!! The last little bit of water should be added
drop-wise using a medicine dropper to ensure the flask is not overfilled. After you have
filled the flask, stopper it and have a teaching assistant check your work. If you have
overfilled the volumetric flask, consult with the TA before proceeding. The TA may instruct
you to continue with the experiment.
17. After you have filled the flask and had it checked by a teaching assistant, invert the flask 20 -
25 times (while holding the stopper in place) to ensure thorough mixing of the solution:
“bubble up, bubble down”. Good mixing is crucial when preparing a solution in a
volumetric flask.
Part II : Titration of Excess Hydrochloric Acid
1. Obtain a clean 25.00 mL pipette and rinse it once with tap water followed by three times with
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deionized water.
2. Pour a small amount (50 mL or less) of your solution from part I into a clean, dry 150 mL
beaker. Rinse your 25.00 mL pipette three times with small portions of this solution. Throw
away any solution that remains in the beaker. Pour a fresh portion of the solution into the
beaker.
3. Using the pipette transfer 25.00 mL aliquots of the solution to each of three 250 mL
Erlenmeyer flasks (125 mL flasks can also be used). Add 2 - 3 drops of bromothymol blue
indicator to each flask. The solution should be yellow.
4. Collect ~120 mL of standardized 0.05 mol L-1 NaOH in a clean, dry beaker. Note the exact
concentration of the NaOH solution. Obtain a 50 mL burette from the storage rack at the
front of the laboratory and properly clean and properly rinse it (see burette and titrating and
“Stoichiometry by Titration”). Ensure the top of the burette is below eye-level and, using a
funnel, fill the burette to just above the zero mark with the NaOH. Fill the burette to just
above the zero mark. Remove the funnel and drain some NaOH through the stopcock.
Ensure there are no bubbles in the tip of the burette. The level of the NaOH may be below
the zero mark, but this does not matter. The level of the NaOH must not be above the zero
mark. If you spill any NaOH on the outside of the burette, be sure to clean it with some
paper towel.
5. Record the volume on the burette to two decimal places. This is the initial volume reading
of the NaOH solution. Failure to record the volume to two decimal places will result in loss
of marks. Remember: the scale on the burette represents the volume dispensed from the
burette, not the volume in the burette.
6. Place one of the flasks underneath the burette and add the NaOH from the burette. The tip
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of the burette should be just below the top of the flask to ensure all the NaOH dispensed from
the burette is added to the flask. Open the stopcock to allow NaOH to flow into the flask.
As the NaOH flows into the flask, swirl the flask continuously to promote good mixing.
Initially, add the NaOH quite quickly.
7. The end point is indicated by the colour change from yellow to green. As you add NaOH,
the solution may turn green (or blue), briefly, with the colour returning to yellow as the
solution is swirled (placing a white sheet underneath the flask can make the colour change
easier to see). As you get closer to the end point the solution will remain green (blue) longer
and longer and you should slow down your additions of NaOH. Close to the end point you
should add NaOH drop-wise or even (if you are skilled!) half drops at a time. At this point
touch the tip of the burette to the side of the flask and use the wash bottle to wash down the
sides of the flask. This ensures all NaOH dispensed from the burette reacts with the HCl in
the flask.
8. Once the colour change is “permanent” you have reached the end point; stop the titration.
Wait a few moments and record the final volume of NaOH (again, to 0.01 mL). The volume
of NaOH added to the flask is the difference between the final and initial volumes.
If the solution turns a persistent blue, you have added too much NaOH. However, record this
volume as you may have overshot the end point by only a drop or so.
9. First titrations are often not as accurate as subsequent ones because you will not know where
the end point is. The first titration will give you an approximate volume of NaOH that will
be needed for subsequent titrations. With subsequent titrations you can initially add the
NaOH quite quickly. Do at least three titrations. Continue the titrations until two titration
volumes agree within ±0.1 mL, but do not do any more than five titrations.
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10. If you must do more than three titrations, empty the flasks, rinse once with tap water
followed by three times with deionized water and use the flasks again. They do not need to
be dry. Do not take more NaOH solution without the instructor’s permission.
11. Before each titration ensure the amount of NaOH in the burette is sufficient. If you have any
doubt about whether the volume of NaOH is sufficient for the next titration, fill the burette.
12. When you have finished, drain the burette and rinse it 3 times with tap water followed by 3
rinsings with deionized water.
13. Rinse the pipettes and flasks 3 times with tap water followed by 3 times with deionized
water.
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Experiment 3: Analysis of an Alkali Metal Carbonate by

Back-Titration of Hydrochloric Acid
Name:
Day:
Time:
TA Name:
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DATA SHEET - Analysis of an Alkali Metal Carbonate by Back Titration of

Hydrochloric Acid
Student Name: _____________________________

Student Number: _____________________________
Date: _____________________________
TA Signature: _____________________________
Code number of unknown alkali metal carbonate: _____________________________
Mass of 50 mL beaker + M2CO3 / g: ________________________

Mass of “Empty” 50 mL beaker / g: ________________________
Mass of M2CO3 transferred / g: ________________________
Volume of 1 mol L-1 HCl added to alkali metal carbonate / mL: ________________________
Exact Concentration of HCl / mol L-1: ________________________
Alkali metal solution checked by TA (initialled): ________________________
Volume of alkali metal solution per titration / mL: ________________________

Concentration of NaOH Solution / mol L-1: ________________________
Indicator: ________________________
Colour change at end point: ________________________
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Volumes of NaOH
I II III IV V
Final Volume / mL
Initial Volume / mL
Volume of NaOH / mL
Average Volume of NaOH / mL: ________________________
Average all the volumes (titres) that are within 0.1 mL and use the average volume in the
calculations.
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1. Calculate the concentration of HCl in the 250.0 mL volumetric flask. From this calculate the
excess number of moles of HCl added to the alkali metal carbonate (see the introduction).
2. Calculate the total number of moles of HCl added to the alkali metal carbonate in Part I.
From the total number of moles of HCl added and knowing the excess number of moles,
calculate the moles of HCl that reacted with M2CO3.
3. Calculate the number of moles of M2CO3 in your original ~0.5 g sample.
4. From the exact mass of M2CO3 used in the experiment, calculate the molar mass of M2CO3.
5. Identify the alkali metal, M. Justify your assertion.
6. In Part I the solution of M2CO3 + HCl is transferred to volumetric flask and diluted to
precisely 250.0 mL. Why must this be done? In other words, why is it not possible to titrate
aliquots taken directly from the beaker?
7. In part II a small amount of the HCl solution is decanted into a beaker and used to rinse the
25.00 mL pipette. Any extra solution is thrown away and new solution poured into the
beaker for pipetting. Why is the extra solution thrown away?
8. In general the alkaline earth carbonates (MCO3; M = Mg2+, Ca2+, Sr2+, Ba2+ ) are insoluble in
water. Would the method used in this experiment work for determining the molar mass of
the alkaline earth? Why or why not? How would the calculations have to be changed?
9. Three students, Eduardo, Joshua and Zahra, are each assigned a different alkali metal
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carbonate from Li2CO3, Na2CO3 and K2CO3. By a remarkable (possibly suspect!)

coincidence they all use exactly the same mass of alkali metal carbonate. If Joshua uses the
largest volume of NaOH for the back titration and Zahra uses the smallest volume, which
student has which alkali metal carbonate? Explain how you make the assignments.
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4. SYNTHESIS OF MALEIC ACID AND CONVERSION TO

FUMARIC ACID.
Objectives
1) To prepare maleic acid from maleic anhydride; 2) to convert the maleic acid to its geometric
isomer, fumaric acid; 3) to compare solubilities and melting points of the two products.
Introduction
Carbon can form single, double and triple bonds and this ability contributes to the diversity
and complexity of organic chemistry. Carbon is able to form so many types of bonds because of its
electron configuration: 1s2 2s2 2px1 2py1 2pz0; 4 valence electrons.
In all cases a given carbon atom forms a total of four bonds (no more, no less!); carbon is
“tetravalent”. The four bonds can be a combination of four single bonds, one single + one triple, two
singles + one double, etc. However, the electronic configuration for a ground state carbon suggests
only two unpaired electrons (2px1 and 2py1) in the valence shell are available for bonding which
implies the formation of only two bonds. Valence Bond Theory attempts to explain the bonding of
carbon by invoking the concept of “orbital hybridization”. In order to form the 4 singly occupied
orbitals needed to form four bonds, the carbon atom mixes (hybridizes) the valence orbitals (2s, 2px,
2py, 2pz) that it has. After mixing the four valence orbitals, the total number of hybrid orbitals plus
non-hybridized orbitals must equal four. The bonding of carbon and resulting molecular geometry
are explained using three types of hybridization.
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sp3 Hybridization
In sp3 hybridized carbon the 2s orbital is mixed with the three 2p orbitals to form four
equivalent sp3 orbitals, each with one unpaired electron. The four sp3 orbitals are distributed
symmetrically about the carbon atom to minimize electron - electron repulsion. Consequently, they
form a “tetrahedron” - a four-sided, hence “tetra”, shape - around the central carbon with angles
between the hybrid orbitals of (ideally) 109.50. The sp3 orbitals overlap with the orbitals of other
atoms to form four single, “sigma” bonds. The carbon atom in chloroform (trichloromethane,
CHCl3) has this type of hybridization and has tetrahedral geometry:
sp2 Hybridization
When a carbon atom is sp2 hybridized, the 2s orbital is mixed with two of the 2p orbitals to
form three sp2 orbitals and one non-hybridized 2p orbital is left over. Three sigma bonds form from
the three sp2 orbitals. The non-hybridized 2p orbital forms a “ð-bond”. When a ð-bond and a sigma
bond occur between two atoms, a “double” bond exists between the atoms. The three sp2 orbitals
are distributed around the carbon atom so they form a triangle with angles between the hybrid
orbitals of 1200. The three sp2 orbitals lie in the same plane and the remaining 2p orbital is
perpendicular to the plane. The carbon atoms in ethene (C2H4) exhibit this type of hybridization and
ethene has trigonal planar geometry:
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sp Hybridization
For an sp hybridized carbon atom the 2s orbital is mixed with one of the 2p orbitals to give
two sp orbitals and two non-hybridized 2p orbitals. The two sp orbitals form two sigma (single)
bonds while the 2p orbitals form two ð-bonds. When a sigma bond and two ð-bonds are formed
between two atoms, a “triple” bond exists between the two atoms. The two sp orbitals are at 1800
to one another and the two 2p orbitals are at 900 to each other and to the sp orbitals. The carbon
atoms in ethyne (C2H2) show sp hybridization and ethyne is linear:
Hybridization in other Atoms
Valence Bond Theory can also explain bonding and geometry for atoms other than carbon.
Oxygen, for example, can have four sp3 hybridized orbitals. Oxygen has six valence electrons. When
these electrons are distributed amongst the four sp3 hybrid orbitals, two orbitals are “filled” (two
electrons) and two are half full (one electron each). The filled orbitals “contain” the two lone pairs
on an oxygen atom. The two half-filled orbitals form two sigma bonds to other atoms (e.g. H2O).
Oxygen can also be sp2 hybridized which allows it to form one sigma bond and one ð-bond. When
oxygen is double bonded to another atom, it is sp2 hybridized.
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Cis - Trans Isomerism
Hydrocarbons (compounds containing only carbon and hydrogen) that contain only carbon-
carbon single bonds (C-C) are “alkanes”. A hydrocarbon with a double bond (C=C) is an “alkene”
and a hydrocarbon with a triple bond (C/C) is an “alkyne”. Double bonds are stronger than single
bonds, but, perhaps counter-intuitively, alkenes are generally more reactive than alkanes: the
increased electron density around the double bond makes it more vulnerable to attack by
“electrophiles” which are chemical species that are attracted to electron-rich regions of other
molecules.
Rotation around the axis of a double bond requires breaking a ð-bond, so “spontaneous”
rotation at a double bond is not possible. Because of this rigidity, different arrangements of atoms
or groups of atoms around the double bond are possible. This leads to geometric isomerism:
different compounds with the same chemical formula, but different arrangements of atoms around
a double bond. As an example, consider 2-butene. The two methyl (CH3) groups can be on the same
side of the double bond (the ‘cis’ isomer) or on opposite sides of the double bond (‘trans’ isomer):
These two compounds have the same chemical formula but they have different physical properties:
Melting Point / 0C Boiling Point / 0C

trans-2 butene -105.5 0.9
cis-2 butene -138.9 3.7
Generally, cis alkenes are less stable than the trans isomer because of “steric hindrance”. In cis-2
butene the hydrogen atoms of the two methyl groups are fairly close to one another causing
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repulsions (steric hindrance) between the two methyl groups. In the trans isomer the methyl groups
are well separated so the repulsion (and steric hindrance) is smaller. Therefore, the trans isomer is
more stable.
In this experiment you will prepare maleic acid:
by hydrolyzing maleic anhydride:
Fumaric acid is the trans isomer of maleic acid and it will be prepared by adding 6 mol L-1
HCl to aqueous maleic acid and boiling the solution. The HCl catalyses the conversion of maleic
acid to fumaric acid:
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The mechanism (the detailed, step-by-step chemical process) of the conversion is beyond the scope
of this course, but is given in the appendix. Reaction mechanisms are discussed in upper-level
organic chemistry courses.
Apparatus
1) 50 mL beaker; 2) 150 mL beaker; 3) Büchner flask and funnel; 4) filter paper; 5) retort stand; 6)
two finger-clamps; 7) heating mantle and controller; 8) 250 mL round bottom flask; 9) reflux
condenser; 10) rubber tubing; 11) capillary tubes; 12) Mel-Temp; 13) tweezers; 14) boiling stones;
15) maleic anhydride; 16) 6 mol L-1 HCl.
Safety
• Maleic anhydride will cause chemical burns if you get it on your skin. If you spill it on your
skin, immediately brush the solid from your skin and promptly flush the area with copious
amounts of cool, running water.
• The 6 mol L-1 HCl should be used only in the fume hood. Spills should be neutralized with
baking soda (until fizzing stops) and the neutralized solution cleaned up with dampened
paper towel (wear gloves). Rinse area with water and wash hands thoroughly.
• If HCl is spilled on the skin, rinse thoroughly with cool running water.
• If either maleic anhydride or HCl are splashed in the eye, rinse the eye for at least 30
minutes at the eye-wash station. Seek medical attention. Other students should stop their
experiments.
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• If dissolved maleic acid is spilled, the spill can be treated with sand and the sand collected
and disposed of as hazardous waste. Consult with a technician.
• Make sure to add boiling stones to the round bottom flask when performing part II.
Procedure
Useful videos for this experiment: open pan balance, weight by difference, and suction
filtration.
Text descriptions available at: open-pan balance, weight by difference and suction filtration.
You will work with a partner for this experiment.
Part I - Preparation of Maleic Acid
1. Using an open-pan balance, weigh ~8 g of maleic anhydride into a 50 mL beaker. Record

the mass of the beaker plus maleic anhydride.
2. On a hotplate heat 15 mL of deionized water (add 1 - 2 boiling stones) in a 150 mL beaker

until the water starts to boil.
3. Once the water has started boiling remove the beaker from the hotplate. CAREFUL - the
beaker will be hot. Handle the beaker near the top. Add the maleic anhydride. .
4. Return the beaker to the hotplate. After all the maleic anhydride has dissolved and there are
no further signs of reaction, remove the beaker from the hotplate and allow the solution to
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cool to room temperature.
5. Record the mass of the (now empty) 50 mL beaker used to weigh the maleic anhydride in
step 1.
6. Once the beaker has cooled, put the maleic acid solution on ice for 1 to 2 minutes to allow
as much of the maleic acid as possible to precipitate.
7. Collect the solid maleic acid using suction filtration and a Büchner funnel (suction filtration).
Note: you must collect both the filtrate (the liquid) and the crystals, so make sure the suction
flask is clean before you start.
8. When rinsing out your beaker, only use small amounts of water.
9. On an open-pan balance, weigh a clean, dry beaker. Transfer the filtered crystals of maleic
acid to the beaker and re-weigh the beaker. Calculate the mass of the crystals collected.
Part II: Conversion of Maleic Acid to Fumaric Acid
1. Transfer the filtrate from part I to the round bottom flask.
2. At the fume hood, add 20 mL of 6 mol L-1 HCl and 3 - 4 boiling stones. Swirl the solution
a couple of times to ensure good mixing.
3. Set up your equipment as shown in Figure 4.1. Attach the heating mantle to the rod of the
retort stand. The round bottom flask should sit at the bottom of the heating mantle (despite
how it appears in the photograph!) to ensure efficient transfer of heat to the solution.
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Figure 4.1: Reflux Apparatus for Conversion of Maleic Acid to Fumaric Acid
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Make sure the flask is securely clamped (to ensure stability). The condenser need only be
loosely clamped to allow easy raising and lowering of the assembly.
4. Ensure there is a good seal between the condenser and the flask. Start the water running
through the condenser; make sure the water enters at the bottom of the condenser and exits
from the top and that the water is draining into a sink. The latex tubing should not touch any
part of the heating mantle. Turn on the heating mantle (to a setting of ~7) and allow the
solution to come to the boil.
5. Once the solution is boiling, reduce the heating mantle setting to about 5 and allow the
solution to reflux gently for ~10 minutes. Do not allow the solution to boil dry.
6. After 10 minutes, raise the flask (and assembly). Do not touch the flask itself as it will be
hot. Allow the flask to cool to approximately room temperature. Tighten the clamp on the
condenser. Remove the flask and place it in an ice bath to complete the precipitation of the
fumaric acid.
7. Collect the fumaric acid using suction filtration (suction filtration). The round bottom flask
can be rinsed with a small amount of cold water to remove as much of the fumaric acid as
possible. Remove the boiling stones using tweezers and allow the crystals to air dry.
8. Once the crystals have dried, weigh them on an open-pan balance using the weight by
difference technique.
Part III - Solubility and Melting Points of the Products
1. Place 0.5 g (roughly a scoopula tip) of each of the maleic acid and the fumaric acid in two
different test tubes. Half fill each test tube with deionized water and shake the test tube.
131
Note whether the solid dissolves or not.
2. Using the Mel-Temp apparatus (see instructions below), record the melting points for each
of maleic acid and fumaric acid. You may find that the compounds do not melt “cleanly”;
they may sublime or decompose. If so, record the temperature at which this occurs. Initially,
heat at a setting of 5 until reaching 1000C, then reduce the setting to 4.
Using the “Mel-Temp” Melting Point Apparatus
A Mel-Temp apparatus allows the rapid and accurate determination of melting points to
roughly 5250C.
1. Use a thoroughly dry sample that has been finely ground. This ensures uniform distribution
of any impurities. The sample can be ground on the watch glass using a stirring rod or the
end of a scoopula.
2. Put sufficient solid in the capillary tube to fill the capillary tube ~ 3 - 4 mm deep. This can
be tricky, but the easiest method is probably to dip the open end of the capillary into some
of the solid then gently tap the closed end on the bench to pack the solid into the tube.
3. Place the thermometer into the well of the Mel-Temp. Be very careful - these are mercury
thermometers. Report any breakage or mercury spill to your instructor immediately. If the
Mel-Temp apparatus has been set up for you, do not handle the thermometer.
4. Plug in the unit and turn it on.
5. Put the capillary tube(s) into the holder. The Mel-Temp can accommodate up to 3 capillaries
132
at one time.
6. Initially you may heat the samples rapidly (at a setting of 5 or 6). Once the temperature
reaches ~1000C reduce the setting to about 4.
7. Observe the samples with your eye about 6" (15 cm) from the eye-piece.
8. Record the temperature at the first sign of the formation of liquid.
9. Record the temperature once the last bit of solid turns to liquid. The temperature recorded
in step 8 and this temperature represent the melting point range for your sample.
10. Once the melting point has been measured turn off the Mel-Temp and allow it to cool. To
do a second determination you will have to allow the apparatus to cool below the expected
melting range.
133
Experiment 4 - Synthesis and Conversion of Maleic Acid
Name: ____________________________
Partner: ____________________________
Day: ____________________________
Time: ____________________________
TA Name: ____________________________
134
DATA SHEET - Synthesis and Conversion of Maleic Acid
Student Name: _____________________________

Student Number: _____________________________
Date: _____________________________
TA Signature: _____________________________
Part I:
Mass of beaker + maleic anhydride / g: _______________________

Mass of empty beaker / g: _______________________
Mass of maleic anhydride / g: _______________________
Mass of beaker / g: _______________________

Mass of beaker + maleic acid / g: _______________________
Mass of maleic acid / g: _______________________
Part II:
Mass of beaker / g: _______________________

Mass of beaker + fumaric acid / g: _______________________
135
Mass of fumaric acid / g: _______________________
Part III:
Melting Point of Maleic Acid / 0C: _______________________

Melting Point of Fumaric Acid / 0C: _______________________
136
1. Calculate the theoretical yield and the percent yield of maleic acid in part I. Your percent
yield of maleic acid was almost certainly much less than 100%. Why?
2. In this experiment the maleic acid was separated from the supernatant by suction filtration.
The tube was removed from the suction flask before the pump was switched off. Why is this
important?
3. Draw the structure for fumaric acid and for each atom other than hydrogen indicate the
hybridization.
4. For each of the following molecules deduce the hybridization of the central atom. Explain
your reasoning.
a. BeH2 - linear, 2 sigma bonds
b. BF3 - trigonal planar, 3 sigma bonds
5. Explain the difference in water solubility between maleic acid and fumaric acid. Which of
the two would you expect to be more soluble in carbon tetrachloride?
6. According to the CRC Handbook the melting point of maleic acid is 1390C and the melting
point of fumaric acid is 2990C (in a sealed tube; fumaric acid sublimes). However, maleic
acid is more polar. Explain this difference.
137
Appendix: Proposed Mechanism for the Conversion of Maleic Acid to Fumaric Acid.
Free rotation then occurs at the carbocation:
138
Ontario Tech University CHEM 1010, F23; Exp. 5 - 21.37
5. MEASUREMENT OF THE IDEAL GAS CONSTANT, ‘R’
The report for this experiment is due at the end of the laboratory period.
Objectives
1) To apply Dalton’s Law of Partial Pressures to a mixture of gases (water vapour and hydrogen);
2) to measure the ideal gas constant and compare the measured value with the accepted value (8.314
L kPa mol-1 K-1).
Introduction
The behaviour of gases as the pressure, volume, temperature and amount of gas (i.e., the
number of moles of gas) are changed was one of the earliest things studied systematically in science.
Over 300 years ago Boyle observed that, to a very good approximation, the volume of a fixed
amount of gas was inversely proportional to the pressure of the gas at a constant temperature:
(5.1)
Charles expanded (no pun intended!) on this and reported that at constant pressure the volume of a
constant amount of gas was directly proportional to its temperature:
(5.2)
Charles’s results showed that when the V vs. T data were extrapolated to a volume of 0 L the
corresponding temperature was ~ -2730C which was defined as “absolute” zero. The Kelvin scale
measures temperatures relative to absolute zero. At roughly the same time Gay-Lussac showed (not
surprisingly!) that for a fixed volume and amount of gas the pressure of a gas was proportional to
139
its temperature:
(5.3)
The volume of a gas depends on how much of it - the number of moles - is present at fixed
temperature and pressure:
. (5.4)
This was first stated in a slightly different way by Avogadro.
These four laws are combined into a single statement:
(5.5)
(5.6)
so:
(5.7)
where ‘b’ is a proportionality constant more commonly called ‘R’, the ideal gas constant. Equation
(5.7) is written in its more recognizable form as:
(5.8)
and is known as the ideal gas law. Note: equation (5.8) applies in the “ideal” case. For real gases
equation (5.8) is an approximation and better models are needed for more advanced applications of
physical chemistry and chemical engineering. However, the ideal gas law is a very good
approximation for many gases, including hydrogen, at moderate pressures and temperatures. The
failures of the ideal gas law are examined in higher level physical chemistry courses.
Dalton’s Law of Partial Pressures is also very important in the study of gases. It states that
each gas in a mixture exerts a pressure proportional to its concentration (or mole fraction). The total
pressure is the sum of the individual “partial” pressures:
(5.9)
140
(5.10)
(5.11)
(5.12)
In this experiment you will react an accurately known mass of magnesium with an excess of
hydrochloric acid to generate hydrogen:
Mg(s) + 2HCl(aq) ÿ MgCl2(aq) + H2(g) (5.13)
From the stoichiometry of the reaction the number of moles of hydrogen gas produced can be
accurately calculated if the mass of magnesium used is accurately known and magnesium is the
limiting reagent. You will use a gas burette to measure the volume of H2(g). If the temperature is
known and the pressure of the hydrogen gas can be determined, the value of the gas constant ‘R’ can
be calculated from the ideal gas equation:
(5.14)
Measuring the pressure of the hydrogen is non-trivial but straightforward. The gas in the
burette is collected over water, so it is a mixture of hydrogen gas and water vapour. The total
pressure of gases (Pgases) in the burette is given by Dalton’s Law:
(5.15)
(5.16)
where is the pressure of the hydrogen gas and is the pressure of the water vapour (the
vapour pressure). The vapour pressure of water as a function of temperature is well-known and
given in the table at the end of the experiment. The experimental challenge, then, is to measure Pgases.
141
How is the total pressure in the gas burette measured? Initially, the gas burette is completely
filled with water. The open end of the burette is plugged with a one hole stopper and submerged in
a 600 mL beaker filled with water. As the reaction proceeds, the generated hydrogen displaces the
water. After the reaction between the magnesium and the hydrochloric acid is complete the burette
will be partially filled with water; more accurately, a dilute solution of HCl. At the top of the burette
will be a mixture of only two gases: hydrogen and water vapour. If the pressure of the gases in the
burette, which push down on the column of water, were equal to the atmospheric pressure, which
pushes the column of water up, the level of the water in the burette would be the same as the liquid
level in the 600 mL beaker. However, the water level in the burette will be higher than the level in
the beaker, so the pressure of the gases in the burette (Pgases) must be less than atmospheric pressure:
(5.17)
(5.18)
Plevel difference is found by measuring the difference between the water levels in the burette and in the
beaker (i.e, the height of the column of water in the gas burette). The atmospheric pressure will be
provided, so to calculate Pgases, we need to find Plevel difference (in Pa).
The downward forces on the water column in the burette are the weight of the water plus the
force exerted by the gases in the burette. The upward force on the water column is the pressure
exerted by the atmosphere (Pascal’s Principle4). The column of water is not moving so the forces
on the water column must be balanced. Therefore:
(5.19)
(5.20)
(5.21)
h = height of the water column in m
4
Pascal’s Principle: pressure applied to a confined fluid is transmitted throughout the fluid and acts in all
directions equally. In this situation the atmosphere applies the pressure to the surface of the water in the beaker.
142
A = cross sectional area of the water column (hA = volume of water in the column), in
m2 .
ñ = density of water, which we shall assume is 1 000 kg m-3. Note the density of water
varies with its temperature. For more accurate work, the density should be found at
the temperature of the water in the experiment.
g = acceleration due to gravity, 9.81 m s-2
Dividing by A and noting that P = F / A:
(5.22)
(5.23)
Comparison of equations (5.23) and (5.18) shows that:

(5.24)
Therefore, if the height of water in the column (h) is measured in metres and Patmosphere is reported in
Pascals, Pgases (in Pa) can be calculated. The atmospheric pressure (in mm Hg) will be reported in the
laboratory. Note: 1 mm Hg = 133.32 Pa.
Once Pgases is known can be found from equation (5.16) and ‘R’ can be calculated from
equation (5.14).
Apparatus
1) 600 mL beaker; 2) copper wire; 3) 00 one hole stopper; 4) gas burette; 5) retort stand; 6) burette
clamp; 7) metric ruler; 8) magnesium ribbon; 9) 6 mol L-1 hydrochloric acid (HCl).
143
Safety
Magnesium
• Magnesium is a combustible metal that will burn with an intensely white light that is
damaging to the eyes. Do not look at the burning metal. The chances of ignition in this
laboratory are extremely remote. If magnesium does ignite, the fire can be smothered with
sand from the bucket in the laboratory.
6 M HCl
• Spills should be treated with a small amount of sodium bicarbonate to neutralize the acid
(the effervescence will stop). Wear gloves and wipe up the spill with a damp sponge or
paper towel. Thoroughly rinse the sponge and wash hands with soap and water.
• Skin exposure: immediately flush skin with cool running water. Continue for 20 - 30
minutes. Wash area thoroughly with soap and water. If irritation develops, seek medical
attention.
• Eye exposure: immediately flush with running water for at least 30 minutes. Notify teaching
assistant, technician or senior laboratory instructor. Other students should stop their
experiments. Seek medical attention.
Waste
• The waste from this experiment is fairly innocuous: a dilute solution of magnesium chloride
in ~0.3 mol L-1 HCl. It can be disposed of in the sinks with plenty of water.
144
Procedure
Useful videos for this experiment are found here: analytical balance, weight by difference;
text descriptions at: the analytical balance, weight by difference.
Part I: Calibration of Gas Burette
At the top of the gas burette is small volume which may or may not be calibrated (the “dead
volume”). In order to get an accurate value for the gas constant, this dead volume needs to be
determined.
1. Put roughly 9 mL of water in a 10.0 mL graduated cylinder and record the volume in the
cylinder.
2. Using a dropping pipette transfer water to the gas burette until the level of the water is at the
first graduation on the burette.
3. Record the volume remaining in the graduated cylinder. The difference between the volume
recorded in step 1 and this volume is the “dead” volume of the gas burette.
4. Record the value of the first graduation on the gas burette. This volume and the “dead
volume” should be very similar (if not the same).
Part II Determination of the Ideal Gas Constant
1. Half fill the 600 mL beaker with deionized water.
2. Rinse the gas burette with tap water followed by deionized water. Add the water to the
145
burette using a beaker.
3. Obtain a strip of magnesium ribbon roughly 2 - 3 cm long. Using a small beaker, weigh the
magnesium ribbon using the analytical balance (weight-by-difference).
4. Obtain a 25 cm length of copper wire and twist roughly 20 cm around the end of a stirring
rod to make a coil. Leave the remaining 5 cm straight to use as a “handle”. The copper coils
may be provided.
5. Put the magnesium in the copper coil so that the copper wire forms a “cage” around the
magnesium. The magnesium must be held securely so that the magnesium does not come
free. Do not flex the magnesium strip too much or it may break.
6. Thread the straight portion of the copper wire through the hole of the 00 stopper.
7. Ensure the gas burette is empty then carefully pour ~15 mL of 6 mol L-1 hydrochloric acid
into the gas burette. 6 mol L-1 hydrochloric acid is corrosive. If you spill any on your skin,
immediately rinse with plenty of cold water and wash your hands thoroughly with soap and
water.
8. Fill the gas burette with deionized water. Be careful not to cause undue mixing of the acid
and the water. This may be easier if the water is gently poured down the side of the burette.
Be sure to completely fill the burette - there must not be any air remaining in the burette!
9. Put the stopper in the burette and position the coil so that the magnesium is about 4 cm into
the burette; it must not block the hole. It will be held in place by the copper cage / wire.
Again, make sure there is no air left in the burette.
146
10. Cover the stopper hole with your finger and invert the burette. Quickly submerge the
stoppered end of the burette in the water in the 600 mL beaker and remove your finger. Do
not remove your finger until the end of the burette is submerged. Clamp the burette in place.
Do not allow the end of the burette to rise above the level of the water in the beaker.
11. The acid is more dense than the water, so it quickly falls towards the bottom of the burette.
Once the acid reaches the magnesium the reaction will begin and proceed rapidly, producing
hydrogen gas.
12. Once the reaction appears to have finished, ensure no magnesium is on the sides of the
burette or trapped in the copper coil.
13. Free any hydrogen gas adhering to the copper coil or to the sides of the burette by gently
tapping the burette with a pencil.
14. The reaction is exothermic. Wait about 5 minutes then record the room temperature to the
nearest 0.10C. At this point it is reasonable to assume the temperature of the gases in the
burette is equal to the room temperature.
15. Record the volume of gas in the burette to the nearest 0.1 mL.
16. Finally, measure the difference in water level between the water in the beaker and the water
in the burette. Measure this in millimetres using a ruler. Convert the height to metres to use
in equation (5.23). Note the atmospheric pressure, Patmosphere. It will be written on the board
for you. You must convert this pressure from mm Hg to Pa. 1 mm Hg = 133.32 Pa.
17. Drain the gas burette completely and rinse several times with tap water, followed by
deionized water. Flush the contents of the beaker down the drain using lots of running water
147
and clean the beaker with plenty of tap water followed by deionized water.
148
Experiment 5 - Measurement of R
The report for this experiment is due at the end of the laboratory period.
Name: ________________________
Course: ________________________
Day: ________________________
Time: ________________________
TA Name: ________________________
149
DATA SHEET - Measurement of the Ideal Gas Constant, R
Student Name: _____________________________

Student Number: _____________________________
Date: _____________________________
TA Signature: _____________________________
Initial volume in the 10.0 mL graduated cylinder / mL: ______________________

Final volume in the 10.0 mL graduated cylinder / mL: ______________________
“Dead” volume of the gas burette / mL: ______________________
Mass of beaker + magnesium strip / g: ______________________

Mass of beaker / g: ______________________
Mass of magnesium strip / g: ______________________
Volume reading from the burette / mL: ______________________

Volume reading of the first graduation / mL: - ______________________
Correction for “dead” volume / mL: + ______________________
Volume of gases in the burette / mL: = ______________________
Height of the water column / mm: ______________________

Height of the water column / m: ______________________
Temperature / 0C: ______________________
150
Atmospheric pressure / mm Hg: ______________________
Atmospheric pressure / Pa: ______________________
151
Show all calculations:
1. From the measured height of the water column, calculate Pgases in kPa (equation (5.23)). Be
careful with units.
2. Calculate the pressure of the water vapour in the gas burette, . Use the table below.
You may have to use a linear interpolation between points in the table (see explanation after
the table).
3. Calculate the pressure of hydrogen in the gas burette ( )
4. Convert your measured temperature from the Celsius to the Kelvin scale.
5. Based on the chemical equation for the reaction between magnesium and hydrochloric acid
(equation (5.13)), calculate the number of moles of hydrogen gas that was produced in the
reaction. Assume the magnesium is the limiting reagent.
6. From the experimental data and the ideal gas equation, calculate an experimental value for
the gas constant in L kPa mol-1 K-1.
7. Given the accepted value for ‘R’ is 8.314 L kPa mol-1 K-1, determine the percentage error in
this experiment:
(5.25)
152
8. Once the reaction is complete, you must wait for a few minutes before taking the
measurements. Why?
9. In the reaction between magnesium and hydrochloric acid (HCl), the HCl was in huge
excess. Why was this necessary?
10. At the start of the experiment (before the HCl reacts with the magnesium) the burette, the gas
burette must be completely filled with liquid (water + 6 mol L-1). Why is this necessary?
11. Imagine a new solvent, aquaforte, has been synthesized that has many of the same properties
as water (in other words, magnesium and HCl will react in aquaforte in just the same way
as they do in water). If the density of aquaforte is 1.137 g mL-1 and you repeat the
experiment with aquaforte in the beaker and in the gas burette, how high will the column of
aquaforte be?
153
THE VAPOUR PRESSURE OF WATER
Temperature / T/K Pressure / kPa

0
C
15 288.15 1.71
16 289.15 1.81
17 290.15 1.93
18 291.15 2.07
19 292.15 2.20
20 293.15 2.33
21 294.15 2.49
22 295.15 2.64
23 296.15 2.81
24 297.15 2.99
25 298.15 3.17
26 299.15 3.36
27 300.15 3.56
28 301.15 3.77
29 302.15 4.00
30 303.15 4.24
Linear Interpolation
It is very likely that the temperature you record for this experiment will lie somewhere between the
values given in this table. To estimate the vapour pressure a “linear interpolation” will be used. This
method assumes that between two values in the table the dependent variable (here, vapour pressure)
154
depends linearly on the independent variable (temperature). The following equation can then be
used:
(T2,P2) and (T1,P1) represent the two known pairs of data from the table and (Tinterp, Pinterp) is the
interpolated point. So:
As an example, if Tinterp = 17.60C (the measured temperature), T1 = 170C, T2 = 180C, P1 = 1.93 kPa
and P2 = 2.07 kPa and Pinterp = 2.01 kPa (the interpolated water vapour pressure).
The astute reader will notice from the data in the table that the vapour pressure is not a linear
function of temperature. Therefore a linear interpolation is not strictly valid. However, when the
‘x’ and ‘y’ intervals are “small” it is a reasonable approximation.
155

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CHEM 1010U Laboratory Manual

LABORATORY ATTENDANCE AND REPORT SUBMISSION POLICIES . . . . . . . . . . . . . . 3

WHMIS AND LABORATORY SAFETY TRAINING. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

GOOD LABORATORY PRACTICE. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17

LABORATORY REPORT RECEIPT SHEET . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 36

ANALYTICAL CHEMISTRY TECHNIQUES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40

MICROSOFT EXCEL - AN INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61

LOCKER EQUIPMENT LIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 78

1. LABORATORY SAFETY AND ORIENTATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80

2. DETERMINATION OF STOICHIOMETRY BY TITRATION . . . . . . . . . . . . . . . . . . . . . . . 94

3. ANALYSIS OF AN ALKALI METAL CARBONATE BY BACK TITRATION OF

4. SYNTHESIS OF MALEIC ACID AND CONVERSION TO FUMARIC ACID.. . . . . . . . . 122

5. MEASUREMENT OF THE IDEAL GAS CONSTANT, ‘R’ . . . . . . . . . . . . . . . . . . . . . . . . 139

And for those honours chemistry graduates who followed:

Class of 2008 Class of 2010 Class of 2011 Class of 2012

LABORATORY ATTENDANCE AND REPORT SUBMISSION

Attendance at laboratory periods and submission of laboratory reports are compulsory.

WHMIS AND LABORATORY SAFETY TRAINING

If you need to return to the course, go to

The following rules must be obeyed and will be rigorously enforced.

2. Contact lenses should not be worn in the chemistry laboratory.

8. Aisles must be kept clear of boots, coats, knapsacks, etc.

9. Students must know the locations of:

Security (x-2400) to get medical assistance.

Fire Alarm / Building Evacuation

Evacuation Routes from Laboratories

Room Primary Escape Secondary Escape

Room Primary Escape Secondary Escape

Allergies and Other Pre-existing Conditions

GOOD LABORATORY PRACTICE

13. Do not wander aimlessly in the laboratory.

3. Chipped, broken or cracked glassware should be discarded. Heating cracked glassware is

Format for First-Year Chemistry Laboratory Reports

Guidelines for Reports

1. Deadlines for submission of reports are:

CHEM 1020U and CHEM 1800U:

Graphs for First Year Laboratories

Whether drawn by hand or generated by computer follow these guidelines:

4. Major divisions on the axes should be labelled.

Experiment 5: Determination of the Order of Reaction for the Reaction between

A “performance evaluation” is part of your evaluation in the laboratory and is an assessment

Laboratory Reports 25 marks total

Adjustments to Laboratory Grades

Rules for Counting Significant Figures

1. All non-zero figures are significant.

11.82: 4 significant figures

2. All zeros between non-zero figures are significant

410.58: 5 significant figures

211.00: 5 significant figures

1.01×105: 3 significant figures

0.0806: 3 significant figures

0.0007: 1 significant figure

Significant Figures in Calculations

Rules for Rounding off Numbers

When rounding off numbers follow these rules:

Multiplication and Division

2.12 3 significant figures

Reported as: 6.41 (3 significant figures)

12.053 5 significant figures

Reported as: 1.9 (2 significant figures)

Addition and Subtraction

8.102 3 significant figures to the right of the decimal

Reported as: 12.48×10-3 or 1.248×10-2

Logarithms and Exponentials

Course: _ Semester: _