CHEM 1010U Laboratory Manual

Fall 2019
Senior Laboratory Instructor:
Richard Bartholomew
UA 3071
[email protected]

Table of Contents

DEDICATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii

LABORATORY CALENDAR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1

INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2

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

LABORATORY CARRY-FORWARDS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6

WHMIS TRAINING . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7

SAFETY RULES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8

SAFETY PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12

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

SAFETY ACKNOWLEDGEMENT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20

MISSED EXPERIMENTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21

LABORATORY REPORTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 24

SIGNIFICANT FIGURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29

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

ANALYTICAL CHEMISTRY TECHNIQUES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37

i
MICROSOFT EXCEL - AN INTRODUCTION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57

LOCKER EQUIPMENT LIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 73

1. LABORATORY SAFETY AND ORIENTATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75

2. DETERMINATION OF STOICHIOMETRY BY TITRATION . . . . . . . . . . . . . . . . . . . . . . 89

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

HYDROCHLORIC ACID . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 102

4. QUANTITATIVE TITRATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117

5. MEASUREMENT OF THE IDEAL GAS CONSTANT, ‘R’ . . . . . . . . . . . . . . . . . . . . . . . . 129

ii
 DEDICATION

The CHEM 1010 laboratory manual is dedicated to the first UOIT 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

iii
 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
Rana Ahmad
Paola Canas
Alexandra Deckert
Sabrina Ebenreth
Fatma Faiez
Charlene Fernandez
Ifrodet Giorgees
Samantha Herbert
Kamisha Hinds
Kevin Mariscal
PJ Mazzonna
Jil Patel
Nora Rayappoo
James Regush
Mursal Sadat
Nargas Sadat
Pragash Senathirajah
Liam Stocks
Mason Sullivan
Sulaiman Torakhel
Kayla Treflik

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 LABORATORY CALENDAR

Fall 2019

Laboratories begin the week of September 9, 2019. The exact dates of your laboratories
depend on the CRN in which you are registered. These dates can be found on your schedule or on
the preview of available courses on MyCampus: www.uoit.ca/mycampus/avail_courses.html.

Dates Experiment
September 9 - 20 1 - Laboratory Safety and Orientation
September 23 - October 4 2 - Determination of Stoichiometry by Titration
October 7 - 11 3 - Analysis of Alkali Metal Carbonate by Back Titration of
Hydrochloric Acid
October 14 - 18 Reading Week - no experiments
October 21 - 25 3 - Analysis of Alkali Metal Carbonate by Back Titration of
Hydrochloric Acid
October 28 - November 8 4 - Quantitative Titration
November 11 - 22 5 - Measurement of the Ideal Gas Constant, “R”

1
 INTRODUCTION

Welcome to Chemistry at OntarioTech University!

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. The
experiments in CHEM 1010U emphasize proper laboratory technique and the quantitative aspects
of laboratory chemistry. The experiments in CHEM 1020U are designed to illustrate, concretely,
principles presented in the lectures.

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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 OntarioTech University Chemistry, F19; Policies - 4.5

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 the report may result in a grade of zero. A student
who 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 Blackboard. You should not assume the start date for experiments in chemistry courses 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. 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 the this manual. Please 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.

When you submit your laboratory report be sure to have the teaching assistant (or whomever

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 OntarioTech University Chemistry, F19; Policies - 4.5

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.

In CHEM 1010U, 1020U, 1800U, 2030U and 2130U your marked laboratory report will
normally be returned to you in 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 (s)he 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.

For CHEM 2040U, 3040U, 3530U, 3540U and 4040U, you will be given access to a Google
Sheet (through your uoit.net account) that will report your current grades and whether a report has
been received but not yet marked. Periodically, your current grades will be posted (as an Excel file)
on Blackboard. If you suspect your report is missing, you must alert the senior laboratory instructor
no more than three (3) working days after the publication of the inventory. 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

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 OntarioTech University Chemistry, F19; Policies - 4.5

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.

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 OntarioTech University Chemistry, F19; Policies - 4.5

LABORATORY CARRY-FORWARDS

Students who have previously taken CHEM 1010U or CHEM 1020U and passed the
laboratory portion of the course may be eligible for a “laboratory carry-forward” which allows them
to use their laboratory grade from a previous attempt at the course as credit for their current attempt.
Students who are granted a laboratory-carry forward are not permitted to perform experiments and
are not required to submit laboratory reports. Details about qualifications, application and granting
of laboratory carry-forwards are found on the Faculty of Science Advising page:
https://science.uoit.ca/undergraduate/academic-advising/academic-policies.php
If you apply for laboratory carry-forward, you should continue to attend laboratories and submit
reports until your application is approved.

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 OntarioTech University Chemistry, F19; WHMIS - 3.3

WHMIS TRAINING

“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 must have completed on-line WHMIS training
before their first laboratory period. You can access the training through this website:

http://healthandsafety.uoit.ca/training/whmis.php

You login by providing your Banner ID and the postal code that you have provided to OntarioTech
University (i.e., the postal code in the mailing address that the University has on file for you). The
training will take about 1 hour and you will receive a certificate once you have completed it. You
should print a copy of this certificate and bring it to your first laboratory period to show to your
teaching assistant. 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.

If you are an international student from a country that does not have postal codes or you do
not have a “valid” postal code, contact the senior laboratory instructor for instructions on accessing
the training.

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 OntarioTech University Chemistry, F19; Safety - 17.33

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, a YouTube video is available for you to watch:
Laboratory Safety Video (which 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 eye protection. For people with eyeglasses it must be worn over
regular glasses. This rule will be vigorously enforced. First-year students MUST wear
safety goggles.

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.

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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 OntarioTech University Chemistry, F19; Safety - 17.33

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 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.

12. No laboratory may be started 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.

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).

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 OntarioTech University Chemistry, F19; Safety - 17.33

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 only 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.

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 glasses may be forbidden from performing the experiment. Students who
violate the safety rules may be dismissed from the laboratory period. In such cases the student will
be given a grade of zero for the laboratory report.

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 OntarioTech University Chemistry, F19; Safety - 17.33

Safety Goggles

Beginning in the Fall 2019 semester all first-year 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 causes fogging.

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 OntarioTech University Chemistry, F19; Safety - 17.33

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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 OntarioTech University Chemistry, F19; Safety - 17.33

Security and get medical assistance.

Fire Alarm / Building Evacuation

OntarioTech 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 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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 OntarioTech University Chemistry, F19; Safety - 17.33

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 southeast corner of building. Exit corner of the building. Exit by the north
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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 OntarioTech University Chemistry, F19; Safety - 17.33

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

OntarioTech 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.

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 OntarioTech University Chemistry, F19; Safety - 17.33

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 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 (although not required) to alert your instructor(s) and to advise them
of any necessary precautions or first-aid treatment.

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 OntarioTech University Chemistry, F19; Safety - 17.33

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) 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 causes frustration and unnecessary
delay for other students.

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 OntarioTech University Chemistry, F19; Safety - 17.33

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
hazard 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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 OntarioTech University Chemistry, F19; Safety - 17.33

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. 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.

5. 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
on the opposite side of the scratch. Press against the tube while pulling hands apart. Fire
polish the ends of the tubing before using.

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 OntarioTech University Chemistry, F19; Safety - 17.33

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: _______________________________________________________

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 OntarioTech University Chemistry, F19; Missed Experiments 5.9

MISSED EXPERIMENTS

If you miss an experiment, you must contact the senior laboratory instructor within five (5)
working days of having missed the experiment. Failure to notify the senior laboratory instructor
within five days will result in a grade of zero for the laboratory report.

Students who miss an experiment (for whatever reason) may be eligible to re-schedule the
experiment. The process to request a re-scheduled experiment is given below. Where re-scheduling
is not possible, a student may be excused from an experiment for “acceptable reasons” after
providing appropriate documentation to the senior laboratory instructor. The acceptable reasons for
missing an experiment are: illness (or other medical reasons), bereavement, religious observance,
varsity athletics or court appearance. You may be excused for other reasons at the discretion of the
senior laboratory instructor who may require documentation for your absence. Remedies other than
re-scheduling such as quizzes or assignments in lieu of laboratory reports may also be used (but not
necessarily). Please note: exemptions or re-scheduling of experiments will NOT be granted to
accommodate other academic requirements or commitments (e.g. midterms, assignments, etc.).

In the case of foreseeable circumstances (e.g., varsity athletics, religious observance),

requests for re-scheduling and/or being excused from an experiment MUST be made at least seven
(7) working days in advance.

Documentation for missed experiments should be submitted electronically to the senior

laboratory instructor. You may either photograph or scan the documentation (include all pages and
ensure the documentation is legible) and email it to the senior laboratory instructor. 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. Any documentation for missed experiments MUST be
submitted no more than five (5) working days after the missed experiment.

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 OntarioTech University Chemistry, F19; Missed Experiments 5.9

If you have missed a laboratory period for an acceptable and documented reason, the deadline
for submitting any report that was due in the missed laboratory period will be extended by the
number of days covered by your documentation. If no duration is specified in the documentation,
the deadline will be extended by one day. The report may be submitted to the senior laboratory
instructor.

Re-scheduling Experiments

You are permitted to re-schedule only ONE (1) experiment without supporting
documentation.

You should complete the “Request for a Re-Scheduled Experiment” form available in the
“Laboratories” section of the Blackboard site for the course. To complete the form, you must
suggest an alternative laboratory period during which to perform the missed experiment.

It is solely your responsibility to find a laboratory period when you can attend. A list of
scheduled laboratory periods is available on the “Preview of Available Courses” at MyCampus:
http://www.uoit.ca/mycampus/avail_courses.html
There must be sufficient space in the laboratory period. In other words, the number of students
enrolled in the section must be less than the maximum number of students allowed in the section.
Note, re-scheduling is done on a first-come, first-served basis; a laboratory period may be full
because of re-scheduling even if MyCampus indicates a vacancy.

Once completed, the form (in MS Word format) must be submitted via e-mail to the senior
laboratory instructor for the course for approval. Requests submitted on paper or in person will not
be considered. Your request MUST be submitted no more than three (3) working days after the
missed laboratory period and should be submitted at least three days in advance of the laboratory

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 OntarioTech University Chemistry, F19; Missed Experiments 5.9

period you wish to attend. You should use the following subject line in your e-mail:

<CHEM XXXX> - request for lab re-schedule, <your name>

If your request is approved, the senior laboratory instructor will sign and return the form to you by
e-mail. Approval is solely at the discretion of the senior laboratory instructor and not all requests
will necessarily be approved. If your request is approved, you must present the signed (by the senior
laboratory instructor) form to the teaching assistant when you arrive at your re-scheduled laboratory;
it is your permission to attend the period. At the end of the period have the teaching assistant sign
the form and any relevant data sheets, laboratory notebooks, etc. When you submit your laboratory
report to your regular teaching assistant, attach the completed form with all relevant signatures.
Failure to do so will result in a grade of zero for the laboratory report. Unless otherwise stated, the
report for the re-scheduled experiment will be due at the beginning of your next regularly scheduled
laboratory period.

Unless otherwise stated, any laboratory reports that are submitted late as a result of missing
a laboratory period will have late days / penalties assessed at the usual rate.

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

LABORATORY REPORTS

Be sure you use the current version of the laboratory manual for all aspects of preparation
and writing your reports. The laboratory manual changes from year to year sometimes in small, but
significant ways.

1. With the exception of the last experiment, laboratory reports are due at the beginning of your
next laboratory period. The report for the last experiment is due at the end of the last
laboratory period. If you have missed a laboratory period for an acceptable and documented
reason, the deadline for submitting any laboratory report that was due in the missed
laboratory period will be extended by the number of days covered by your documentation.
If no duration is specified in the documentation, the deadline will be extended by one day.
The report may be submitted to the senior laboratory instructor.

2. 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.

3. Marks will be deducted from late laboratory reports at a rate of two (2) marks per “business”
day. No report will be accepted if it is more than four (4) business days late. Any day the
university is open (whether classes take place or not) is a business day.

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 ink.

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

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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.

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
will be assessed. 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, 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
misconduct, punishments and appeals procedures are given in the university calendar. It is
the student’s responsibility to read and understand these regulations.

11. You MUST submit the cover sheet provided for each experiment. Two (2) marks will be

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

deducted if the cover sheet is not submitted.

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.

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 for the course.

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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.

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).

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

6. Do not play “connect-a-dot” with the data. When appropriate, draw a smooth curve to “best

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

fit” the points. In many cases the curve may be a line. When using a computer, 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.

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 your original data (signed by the TA), your sample calculations (including graphs) and the
answers to any questions posed in the laboratory manual.

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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.

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

11.82: 4 significant figures

3.75: 3 significant figures

2. All zeros between non-zero figures are significant

410.58: 5 significant figures

256.032: 6 significant figures

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

211.00: 5 significant figures

40.0: 3 significant figures
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 x 105: 3 significant figures

1.010 x 105: 4 significant figures

4. Zeros to the left of a non-zero figure (but not between significant figures) are not significant.

0.0806: 3 significant figures

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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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 OntarioTech University First-year Chemistry, F19; Reports 17.34

2.12 3 significant figures

x 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

Reported as: 1.9 (2 significant figures)

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)

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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 x 10-5 0.08139 x 10-3

+ 2.16 x 10-4 Y + 0.216 x 10-3
+ 1.218 x 10-2 + 12.18 x 10-3
12.47739 x 10-3

Reported as: 12.48 x 10-3 or 1.248 x 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 x 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

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

in the result must equal the number of significant figures after the decimal point in the original
number.

e3.140 = 23.10387
Reported as: 23.1 (3 significant figures)

100.31 = 2.0417
Reported as: 2.0 (2 significant figures)

“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) 6 ZnCl (aq) + H (g)

2 2

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 = 1000 g, exactly

So, to convert 12.12 inches (four significant figures) to centimetres:

12.12 inches x 2.54 cm / inch = 30.7848 cm

Reported as: 30.78 cm (four significant figures)

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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.

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 OntarioTech University First-year Chemistry, F19; Reports 17.34

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 __________________________________________________

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.

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 OntarioTech University Analytical Chemistry Techniques, F19; 16.30

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. Links are provided here to videos
of the techniques.

Weighing Techniques

Good weighing technique is vital to success in all aspects of chemistry and the measurement
of mass is fundamental in 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

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 OntarioTech University Analytical Chemistry Techniques, F19; 16.30

subtracted. As a substance is added to the receiving vessel, the balance displays the mass of added
material. Using an open-pan balance avoids transferring chemicals on the analytical balance.

The Analytical Balance (analytical balance)

The Mettler-Toledo analytical balance used in chemistry laboratories at OntarioTech

University is designed to weigh relatively small masses (less than 120 g) with very great precision
(to ±0.0001 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.

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 OntarioTech University Analytical Chemistry Techniques, F19; 16.30

7. Remove the object and close all the doors.

8. Chemicals must NEVER be placed 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 as
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

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 OntarioTech University Analytical Chemistry Techniques, F19; 16.30

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.

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 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.
It does not matter if the weighing vial is completely emptied into the receiving vessel. However,

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 OntarioTech University Analytical Chemistry Techniques, F19; 16.30

none of the substance may be spilled; all of it must be in either the weighing vial or the receiving
vessel.

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 of 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.

Volumetric Techniques

Volumetric techniques are probably just as important as weighing technique (in CHEM
2030/2130 volumetric analysis will be used extensively). Good volumetric technique is necessary
to obtain good results.

In analytical chemistry there are several important (and accurate) types of volumetric
glassware: the pipette (in various forms), the burette and the volumetric flask. Additionally, there
are other useful (but not as accurate) pieces of glassware: 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 the solution that will be used in the glassware. This replaces the water with the solution
and ensures the solution is not diluted. NEVER attempt to “dry” glassware by shaking out excess
water. 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 water; glassware in this position

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 OntarioTech University Analytical Chemistry Techniques, F19; 16.30

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. The meniscus should be read at its lowest point (although
in some unusual cases 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.

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 may be required.

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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 rinsings (through the tip) into a waste beaker. Repeat the rinsings
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
is a very bad thing (see below for instructions on cleaning a contaminated pipette bulb)! It can lead
to cross contamination of solutions. 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

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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!

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.

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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 good (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
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.

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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 volume of titrant required to deliver a stoichiometric number of moles of
titrant; that is, the volume at which the moles of analyte and moles of titrant are present 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.

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

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with the solution that will be used to fill 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. 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. Repeat the rinsings at least twice more.

Using a funnel and a beaker, fill the burette with solution to just above the ‘0' graduation.
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'. Record this “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. 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 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 burette is set up with the stopcock facing right (the directions here are for a right handed
person; “lefties” should reverse all directions). 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.

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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.

To clean the burette after the experiment is finished, drain any remaining solution into a
waste beaker. Rinse several times with tap water and 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).

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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
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 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.

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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.

The following is the procedure for preparing a 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 ±0.0001 g.

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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. It is more important not to spill any.

4. Record the mass (±0.0001 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 to the beaker (approximately ½ the final solution volume).

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.
It is vital that you transfer all the solution (therefore, all the 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.

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.

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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.

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. For the Hirsch and
Büchner filters, a one hole stopper is put on the top of the filter flask and the appropriate funnel

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inserted into the hole. Sintered glass crucibles use special holders. 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 (using a stirring rod as a guide) the supernatant solution onto the
filter paper and allow it 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
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
(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 and 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

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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
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” (a solution
containing everything but the species of interest) into the cell holder. 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

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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 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 and use the
up and down arrows until the display reads the correct temperature.

3. The electrode should be left in pH 4 buffer when not in use. To ready the electrode for use,
lower the rubber safe-lock device (located near the top of the electrode) 2 cm to expose the
refilling port (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

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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 7.00 buffer and press the “Cal” button.
When the calibration has finished, the pH meter will display pH = 7.00.

6. Remove and rinse the electrode and place it in the second buffer (in this case pH 4.00). Press
the “Cal” button. Again, when the calibration is finished, the meter will display the correct
value (pH = 4.00). 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.

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. Hold the
“Read” button for 2 seconds until the “A” on the right side of the display 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 4.00 buffer.

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 OntarioTech University Chemistry, F19;Excel 7.12

MICROSOFT EXCEL - AN INTRODUCTION

This guide was originally written for Excel 2013, but the differences between Excel 2013 and
Excel 2016 are minor and should not affect these instructions.

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

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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,

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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.

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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.

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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”

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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.

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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:
=2*A1+3
If this formula were copied into cells B2, B3, B4...., the formula would be:
=2*A2+3
=2*A3+3
=2*A4+3
etc.
If it were copied into cell C1, the formula would be:
=2*B1+3
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:
=2*A1+3
If the contents of A1 were moved to C3, the formula in B1 would be changed to:
=2*C3+3.

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$1). If the formula in cell B1 is:
=4*$A$1+6
and it is copied to the cells B2, B3, B4..etc., each cell will have the same formula:
=4*$A$1+6
The referred cell in the formula does not change.

A mixed reference is a reference such as $A1 or A$1. In the former case the column

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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: »šº. 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.

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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.

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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” (without markers). 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

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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:

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.

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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 = 0). 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)
square of the regression coefficient (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
and the ‘t’ value. The confidence intervals (CI) on ‘b’ and ‘m’ are given by:

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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:

where CL is the confidence level (most often 95%). ‘df’ is the degrees of freedom, given by:

where ‘n’ is the number of measurements (points on the line).

When calculating a “prediction” value of Y0 for a given value X0, the prediction interval on
Y0 is given by:

where:

= the average of all the X values in the domain

Xi = the X value of the ith measurement
n = the number of calibration points on the line.

One of the more common uses of the regression line is to calculate an X0 value from an observed Y0
value. The confidence interval on X0 (for Y=mX + b, but not for Y = mX) is given by:

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where

k = the number of replicate measurements of Y0 (most commonly this is 1)

n = the number of points on the calibration line

= the mean value of Y for the points on the calibration line

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.

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 OntarioTech University Chemistry, F19; Equipment - 17.31

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
125 mL Erlenmeyer flask 2
250 mL Erlenmeyer flask 3

10 mL graduated cylinder 1
25 mL graduated cylinder 1
100 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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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

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 OntarioTech University CHEM 1010 / 1800, F19; Exp. 1-13.24

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)
to practise using a pipette (CHEM 1010).

Introduction

Two very important roles of the teaching assistant are to ensure all students are informed of
the safety rules of the laboratory and to enforce the rules. Everyone’s safety and security in the
laboratory depends on each student knowing and obeying the rules and working safely. At the
beginning of this laboratory period the teaching assistant will spend some time explaining the safety
rules of the laboratory, pointing out safety equipment, and describing procedures. The introductory
pages of the manual and this video - First-Year Laboratory Safety Video - also 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. Be aware
that failure to comply with the safety rules may result in your dismissal from the laboratory.

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

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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).

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)

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 10.0 mL of a solution is the same as the concentration
of 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.

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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.

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 will be employed extensively in
CHEM 1010 experiments later this semester.

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 (or 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 (and 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
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 several experiments in CHEM 1010 later this semester (and in subsequent chemistry
courses).

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 OntarioTech University CHEM 1010 / 1800, F19; Exp. 1-13.24

Procedure

The techniques used in this experiment are: open-pan balance, analytical balance, weight-by-
difference, pipetting, and preparing a standard solution. Videos of the techniques are available at:
open-pan balance, analytical balance, weight by difference, the meniscus, the volumetric flask,
preparing a standard solution, and transfer pipettes.

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

In the first part of the laboratory period the teaching assistant will explain the safety protocols
and procedures that are outlined in the introduction of this manual. Once the teaching assistant has
completed the introduction you must submit answers the following questions. You should answer
questions 2 - 5 on a separate sheet.

1. Using the laboratory template provided (see pp. 84 - 85) , 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. What is the proper way to dispose of broken glass?

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4. What steps should you take if the fire alarm sounds?

5. What are the appropriate treatments for i) cuts and ii) minor burns?

Part II: Locker Equipment Check

In the introductory pages of the laboratory manual is a list of equipment (p. 73) 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.

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

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.

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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 all of it 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”.

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 (do not splatter the solution) until all the
NaCl dissolves. 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.

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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. If steps 9 - 12 have been
performed properly, all the NaCl transferred to the 250 mL beaker (step 3) should be
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 must be started again.
If you overfill the flask, empty it, rinse three times with deionized water and start again from
the beginning.

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)

25.00 mL pipettes will be provided in the laboratory. The teaching assistant will point them

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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
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, dry, stoppered 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 and stopper the flask. Tare an open-pan
balance and weigh the stoppered 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.

6. When you have finished, empty the flask, place it in the oven to dry and replace the flask in
your locker with a cooled one.

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Experiment 1 - Laboratory Safety and Orientation

Name: ____________________________

Course ____________________________

Day ____________________________

Time: ____________________________

TA Name ____________________________

You must submit this sheet with your report.

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Results and Questions

Part I - Safety Orientation

On a separate piece of paper answer the questions posed in the procedure (on p. 78). Include
the completed laboratory template (p. 84 or 85) showing the locations of the safety equipment.

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) ____________________________________

Calculate the concentration of the NaCl solution (in mol L-1 and with the correct number of
significant digits).

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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

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 percentage difference between the average volume transferred and the volume
stated on the pipette.

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4. On a separate sheet describe any 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 iodate, iodide and acid.

Introduction

The “titration” is a very common method of analysis in chemistry. 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 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”
are not, to be completely rigorous, the same thing. If the indicator is properly chosen, the difference

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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 iodate (IO3-), iodide (I-) and acid (H+). 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; the limiting reagent) 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. The number of moles of iodide ( ) that reacted can now be calculated. Having the

numbers of moles of IO3-, I- and I2 allows the calculation of the mole ratio IO3-: I- : I. Finally, the
coefficients for H+ and H2O in reaction (2.1) are found by inspection.

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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. Once the solution is a pale yellow a small amount of starch indicator is added. 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. Without the starch the colour change at the end point
is not sudden, so it is much harder to detect. However, the starch must not be added too early
because then the colour change is 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

Safety

• Most of the solutions used here are quite dilute, therefore not particularly dangerous.

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• 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. Other students should stop their
experiments. Notify teaching assistant / technician / senior laboratory instructor as soon as
possible.

• 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.

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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, 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. 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, it 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.

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. 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
the exact concentration of the KIO3 solution. You will not be able to get more KIO3 so do
not waste it.

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10. Pour ~10 mL of the KIO3 solution into a clean, dry 50 mL beaker. 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 and indicated by the 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

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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 will give you
some 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
in the stand.

22. Rinse the pipette and flasks 3 times with tap water followed by 3 times with deionized water.

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Experiment 2 - Stoichiometry by Titration

Name: ____________________________

Day ____________________________

Time: ____________________________

TA Name ____________________________

You must submit this sheet with your report.

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Results, Calculations and Questions

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.

Note on the Calculations

This is the first experiment (of three) that will involve titrations. The calculations for
titrations (regardless of the specific reaction) are usually very similar. The objective is to calculate
the concentration (or amount) of an analyte (the reagent in the flask) based on the concentration and
volume of the titrant (the reagent in the burette). The known quantities are usually: 1) the volume

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of the analyte solution; 2) the volume of the titrant (this is what is measured); 3) the concentration
of the titrant and 4) the stoichiometric ratio between titrant and analyte (from the balanced chemical
reaction).

Because the calculations are so similar, you might find it beneficial to construct an Excel
spreadsheet to perform them. In the spreadsheet, you would enter the values for the variables above
and the spreadsheet would calculate the final concentration of the analyte (see below). As an
example, consider a titration between oxalic acid (the analyte) and permanganate (the titrant):

5C2O4H2(aq) [oxalic acid] + 2MnO4(aq) [permanganate] + 6H+(aq)

ÿ 10CO2(g) + 2Mn2+(aq) + 8H2O(l)

in which 10.00 mL of oxalic solution are titrated with 8.794 x 10-4 mol L-1 permanganate solution.
In this reaction the stoichiometric ratio is given by:

The calculations for one titration are identical (but with different values) to any other, so a
spreadsheet is easily set up to do the calculations. An example is given below. If the spreadsheet
is set up correctly, it is a template for almost all titration calculations. Remember, if you use this
option, you should always provide sample calculations.

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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 previous 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 (which is completely consumed) according to a known reaction and some is left over (the
excess). Next, titrant is added to the excess amount of the reagent to determine how much is left
over. Knowing how many moles of the reagent were added originally (nadded) and how many moles
are left over (the excess, nexcess), yields the moles that reacted with the analyte (nreacted):
(3.1)

Once this is known the moles of analyte can be calculated. 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
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):

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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
and 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 (the excess number
of moles of HCl) after the reaction with the alkali metal carbonate. 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)

The HCl is in excess so the alkali metal carbonate is the limiting reagent in reaction (3.2). Therefore,

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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.
Wipe down the area with a damp sponge and wash hands thoroughly afterwards.

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• 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 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 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 experiment.

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 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 15 minutes.
Wash area thoroughly with soap and water. If irritation develops, seek medical attention.

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• 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: the open-pan balance, the analytical balance, weight by
difference, transfer pipette, burette and titrating. Videos of the techniques: 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.

2. Weigh the 50 mL beaker + solid on the analytical balance and record the mass. Be sure to

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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.

7. Decant (pour) ~20 mL of the HCl solution into a clean, dry 50 mL beaker. If you use a

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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 two times) 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
fizz 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).
Repeat the washing and transfer twice more (for a total of 3 times). Be careful not to use too

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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.
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
deionized water.

2. Pour a small amount (50 mL or less) of your solution from part I into a clean, dry 150 mL

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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. Clean and properly rinse a 50 mL burette (see burette
and titrating and “Stoichiometry by Titration”) and fill it 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.

6. Place one of the flasks underneath the burette and add the NaOH from the burette. The tip
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,

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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. The
volumes marked on the burette indicate the volume dispensed from the burette not the
volume in the burette.

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.

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.

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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. Open the stopcock and clamp the burette upside down in the
burette stand.

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 ____________________________

You must submit this sheet with your report.

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Results, Calculations and Questions

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 ________________________

Volume of alkali metal solution per titration / mL ________________________

Concentration of NaOH Solution / mol L-1 ________________________

Indicator: ________________________
Colour change at end point: ________________________

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
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

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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. QUANTITATIVE TITRATION

Objectives

1) To gain further experience with standard glassware of volumetric analysis (the pipette and the
burette) and with performing titrations; 2) to determine the concentration of a solution of acetic acid.

Introduction

Volumetric analysis is very important in all aspects of chemistry but especially in analytical
chemistry. Volumetric analysis, as the name implies, involves measuring the quantity of some
chemical or reagent by measuring volumes. The common pieces of equipment for doing this are the
pipette, the burette, and the volumetric flask. Titrations are, perhaps, the most common form of
volumetric analysis.

The success of a titration in a volumetric analysis depends on accurately knowing the

concentration of one of the reactants. A solution whose concentration is accurately known is called
a “standard” solution. In many cases a standard solution can be prepared directly from a solid.
When this is possible, the solid is called a “primary standard”. Primary standards should have the
following properties: i) they should be available in high purity ($99.9%); ii) they should not absorb
moisture from the air (i.e., must not be hygroscopic); iii) they should be thermally stable so they can
be dried; iv) they should have high molar mass to reduce weighing errors; v) they should be stable
in air. A substance that is not a primary standard can often be “standardized” (i.e., its concentration
accurately determined) by titration with a primary standard.

In this experiment sodium hydroxide is the titrant in the determination of the concentration

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of acetic acid. Sodium hydroxide is a very common titrant for determining the concentrations of
weak acids. However, sodium hydroxide cannot be used as a primary standard for several reasons.
First, it is hygroscopic so it is impossible to weigh accurately. Second, it is unstable in air, reacting
with carbon dioxide (CO2) to form carbonates. Third, it has a relatively low molar mass - the relative
error in the number of moles will be larger compared to using a high molar mass compound.
Because sodium hydroxide is not a primary standard, a sodium hydroxide solution must standardized
before it is used in a volumetric analysis.

In this experiment the sodium hydroxide solution is standardized by titrating it with a

hydrochloric acid solution (HCl) of accurately known concentration. The reaction between NaOH
and HCl is:
NaOH(aq) + HCl(aq) ÿ NaCl(aq) + H2O(l) (4.1)
The stoichiometric ratio between NaOH and HCl is 1:1. Knowing the end point volume and the
concentration of the HCl allows the calculation of the number of moles of HCl required to reach the
equivalence point. From this, the number of moles of NaOH can be found and, knowing the volume
of NaOH used in the titration, the accurate concentration of the NaOH can be determined.

Once the sodium hydroxide is standardized the concentration of the acetic acid is found based
on the following reaction:
NaOH(aq) + CH3COOH(aq) ÿ NaCH3COO(aq) + H2O(l) (4.2)
The stoichiometric ratio between sodium hydroxide and acetic acid is 1:1. The principles of the
calculation of the acetic acid concentration are the same as for the calculation of the sodium
hydroxide concentration.

Apparatus and Materials

1) 400 mL beaker; 2) 250 mL beaker; 3) 150 mL beaker; 4) 50 mL burette; 5) 25.00 mL pipette; 6)

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10.00 mL pipette; 7) 3 x 250 mL Erlenmeyer flasks; 8) wash bottle; 9) ~0.1 mol L-1 sodium
hydroxide (NaOH) solution; 10) standardized hydrochloric acid solution (~0.1 mol L-1); 11)
phenolphthalein indicator; 12) bromothymol blue indicator; 13) unknown concentration acetic acid
solution (~0.25 mol L-1).

Safety

• In case of eye exposure, rinse eye thoroughly at the eye-wash station (minimum of 30
minutes); seek medical attention. Other students should stop experiment. Notify TA, senior
laboratory instructor or technician.

• In case of skin exposure, rinse thoroughly with cool, running tap water. If skin irritation
develops, seek medical attention.

• Spills of NaOH can be treated with a small amount of vinegar and mopped up with a sponge.
Rinse the sponge with tap water. Wash hands thoroughly.

• Spills of acetic acid or HCl can be treated with sodium bicarbonate (until evolution of CO2
stops) then cleaned as with NaOH spills.

• Waste can be put down the sinks with plenty water to rinse. Any excess HCl can be mixed
with excess NaOH to neutralize it then put down the drain with plenty of water.

Procedure

The techniques used in this experiment are: pipetting, the burette and titrating. Videos:

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transfer pipettes, titrating.

In this experiment marks will be assigned for both accuracy (how close your results are to
the true value; 6/25) and precision (how reproducible your results are; 3/25).

Part I: Standardization of Sodium Hydroxide Solution

In this and subsequent parts of the experiment you may find it convenient to discard rinsings
into a large beaker (400 mL or 600 mL).

1. Rinse the burette once with tap water then three times with deionized water. Use only about
10 mL each time. To rinse the burette, add water and hold the burette almost horizontally.
Rotate the burette so all of the inner surface of the burette is rinsed. Drain a portion of the
water through the stopcock into a waste beaker, close the stopcock and pour the remainder
out through the top.

2. Collect ~200 mL of NaOH in a clean beaker. The beaker need not be dry. If the beaker is
not dry, mix the NaOH in the beaker well. Cover the beaker with a watch glass.

3. Using a small amount of the NaOH solution, rinse the inner surface of a funnel. Use this
funnel to add NaOH to your burette (ensure the funnel is below eye-level when adding NaOH
to the burette).

4. Rinse the burette three times with the NaOH solution in the same manner you rinsed the
burette with deionized water. Again, drain a portion of the NaOH through the stopcock into
a waste beaker. Ensure no bubbles are in the tip of the burette. Empty the remaining NaOH
through the top of the burette.

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5. Fill the burette with your NaOH solution. 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.

6. Obtain a clean, dry 250 mL beaker and collect ~150 mL of the standardized HCl solution.
It is important that the beaker be dry. Note the exact concentration of the HCl (written on
the bottle). Pour ~50 mL of the HCl solution into a clean, dry 150 mL beaker.

7. Read the section on using a pipette at the beginning of this manual and following those
instructions, rinse a 25.00 mL pipette with tap water (once), deionized water (three times)
then with the HCl solution in the 150 mL beaker (three times). The pipette must be properly
rinsed to ensure that when it is used to transfer the solution, the solution is not diluted by the
small amount of residual water in the pipette. Do not use more than ~13 mL (the wide part
of the pipette should not be more than ½ full) for each rinsing.

8. Because it may have been diluted with water from the pipette, throw away any HCl solution
in the 150 mL beaker. Rinse the 150 mL beaker with small portions (3 times) of the HCl
solution. This is to prevent dilution of the HCl solution by any residual water in the beaker.
Do not use too much HCl in the rinsings or you risk running out of standard solution. Pour
~100 mL of the HCl solution into the now clean and rinsed beaker.

9. Using the 25.00 mL pipette transfer 25.00 mL of HCl solution into each of 3 clean (but not
necessarily dry) 250 mL Erlenmeyer flasks. Add 3 drops of bromothymol blue indicator to
each flask. Two different indicators will be used in this experiment - read the bottle carefully
and make sure you add the correct one! After addition of the correct indicator the solution
should be light yellow.

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10. Record the initial volume of NaOH. You should record this to 0.01 mL (i.e., 1/10 of a
graduation).

11. Place one of the flasks underneath the burette and begin the titration. The tip 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.

12. 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 help make the colour
change easier to see). As you get closer to the end point the solution will remain green (or
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 any NaOH dispensed from the burette reacts with
the HCl.

13. 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. The
volumes marked on the burette indicate the volume dispensed from the burette, not the
volume in the burette.

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.

14. First titrations are often not as accurate as subsequent ones (because you will not know where

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the end point is). The first titration will give you an approximate volume of NaOH that will
be needed for subsequent titrations. Do at least three titrations. Continue the titrations until
two titration volumes agree within ±0.1 mL, but do not do any more than four titrations. An
experienced analyst can usually get 3-4 titrations within 0.05 mL!

15. If you must do more than three titrations, empty the flasks, rinse once with tap water
followed by three times with deionized water. You do not need to dry the flasks. You may
find it necessary to add more HCl solution to the beaker from which you have been pipetting.

16. 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.

Part II: Determination of the Concentration of Acetic Acid Solution

Note: it is not necessary to know the concentration of the sodium hydroxide solution before
beginning these titrations. However, the concentration of sodium hydroxide is necessary to calculate
the concentration of the acetic acid (the objective of the experiment!).

1. Clean out the flasks from part I by thoroughly rinsing them with tap water (once) followed
by deionized water (three times). The flasks do not need to be dry to begin the titrations.

2. Collect roughly 70 mL of the acetic acid of unknown concentration in a clean, DRY (it is
important that the beaker be both clean and dry) 150 mL beaker.

3. Rinse a second, clean 150 mL beaker three times with small portions of the acetic acid. Pour
~20 mL of acetic acid into the 150 mL beaker.

4. Rinse a 10.00 mL pipette once with tap water, three times with small amounts of deionized

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water (~5 mL) then three times with small portions of the acetic acid solution. Discard the
rinsings and the contents of the second 150 mL beaker.

5. Again, rinse the second 150 mL beaker three times with small portions of the acetic acid.
Pour ~40 mL of acetic acid into the beaker.

6. Transfer 10.00 mL of the acetic acid from the second 150 mL beaker into each of three clean
250 mL Erlenmeyer flasks. Add ~25 - 30 mL of deionized water and 2 - 3 drops of
phenolphthalein indicator. The solution should be colourless.

7. Just as with the HCl solution, titrate the acetic acid solution with the NaOH. The end point
is marked by the colour change of colourless to pink (the fainter the pink, the better). Do at
least three titrations. Continue the titrations until two titration volumes agree within ±0.1
mL. Do not do any more than four titrations.

8. When you have finished, drain the burette and rinse it 3 times with tap water followed by 3
rinsings with deionized water. Open the stopcock and clamp the burette upside down in the
burette stand.

9. Rinse the pipettes and flasks 3 times with tap water followed by 3 times with deionized
water.

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Experiment 4: Quantitative Titration

Name: ____________________________

Day ____________________________

Time: ____________________________

TA Name ____________________________

You must submit this sheet with your report.

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Results, Discussion and Questions

Part I: Standardization of Sodium Hydroxide Solution:

Concentration of HCl Standard Solution / mol L-1 _______________________

Volume of HCl Solution / mL ________________________

Indicator: ________________________

I II III IV
Final Volume / mL
Initial Volume / mL
Volume of NaOH used / mL

Average all the volumes (titres) that are within 0.1 mL. Use the average volume to calculate the
concentration of the NaOH.

Average Volume of NaOH / mL ________________________

Concentration of NaOH (show calculations) / mol L-1 ________________________

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Part II - Determination of the Concentration of Acetic Acid

Volume of Acetic Acid Solution / mL ________________________

Indicator: ________________________

I II III IV
Final Volume / mL
Initial Volume / mL
Volume of NaOH used / mL

Average all the titres (volumes) of NaOH that agree within 0.1 mL. Use this volume and your
standardized concentration of NaOH to calculate the concentration of acetic acid.

Average Volume of NaOH / mL ________________________

Concentration of Acetic Acid (show calculations) / mol L-1 ________________________

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1. Why must the funnel be removed from the top of the burette during the titration?

2. 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?

3. For convenience the procedure directs you to use clean and dry beakers to collect the
hydrochloric acid and acetic acid. Why? How would you change the procedure so that the
beakers did not have to be dry?

4. The beaker used to collect the NaOH in part I only needs to be clean. Why is it unnecessary
for the NaOH beaker to be dry?

5. Fatima has been asked to prepare a solution of Mg(ClO4)2 with an accurately known
concentration. However, she discovers that each time she tries to weigh the Mg(ClO4)2 the
mass is slightly greater. Explain this observation.

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

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
its temperature:
(5.3)
The volume of a gas depends on how much of it (the number of moles) is present at fixed

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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 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. The total pressure is the
sum of the individual “partial” pressures:
(5.9)

(5.10)

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(5.11)

(5.12)

In this experiment you will react an accurately known mass of magnesium (measured using
the analytical balance) with an excess of hydrochloric acid:
Mg(s) + 2HCl(aq) ÿ MgCl2(aq) + H2(g) (5.13)
From the stoichiometry of the reaction the number of moles of hydrogen gas can be calculated
(assuming all the magnesium reacts). 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.

How is the total pressure in the gas burette measured? Initially, the gas burette is filled with
water. The open end (actually the end with the one hole stopper) of the burette is submerged in a
600 mL beaker filled with water. As the reaction proceeds, the generated hydrogen displaces the

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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). If the pressure of the
gases in the burette were equal to the atmospheric pressure, 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 in the water levels (in millimetres) between 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 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 Principle2). 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

A = cross sectional area of the water column (hA = volume of water in the column), in
m2 .
ñ = density of water, 1 000 kg m-3
g = acceleration due to gravity, 9.80 m s-2

2
Pascal’s Principle: pressure applied to a confined fluid is transmitted throughout the fluid and acts in all
directions. In this situation the atmosphere applies the pressure to the surface of the water in the beaker.

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Dividing by A (and noting that P = F / A):

(5.22)

(5.23)

If Pgases = 0 (i.e., a vacuum at the top of the burette so no force pushing down on the column
of water), and the height of the water column would be given by:

(5.24)

If Patmosphere = 101 325 Pa (101.325 kPa), then h = 10 339 mm (assuming ñ(H2O) = 1000 kg m-3).
Therefore,
(5.25)

From equations (5.23) and (5.24) (with Pgases = 0):

(5.27)

Dividing equation (5.27) by equation (5.25) gives:

(5.28)

(5.29)

Substituting equation (5.29) into equation (5.23):

(5.30)

Therefore, if the height of water in the column (h) is measured in millimetres and Patmosphere is

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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).

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 fizzing 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.

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• 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.

Procedure

Note: Students must submit the laboratory report for this experiment at the end of the laboratory
period.

Useful videos for this experiment: 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 is uncalibrated (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

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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. Record the volume on the burette corresponding to the first
graduation.

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.

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
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. Form the magnesium strip into a coil.

5. 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.

6. 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.

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7. Thread the straight portion of the copper wire through the hole of the 00 stopper.

8. 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.

9. 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!

10. 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.

11. 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.

12. 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.

13. Once the reaction appears to have finished, ensure no magnesium is on the sides of the
burette or trapped in the copper coil.

14. Free any hydrogen gas adhering to the copper coil or to the sides of the burette by gently
tapping the burette with a pencil.

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15. 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.

16. Record the volume of gas in the burette to the nearest 0.01 mL. Add the “dead” volume to
this volume to account for the uncalibrated volume at the top of the burette.

17. Finally, measure the difference in water level between the water in the beaker and the water
in the burette. Measure this in millimetres. Note the atmospheric pressure, Patmosphere. It will
be written on the board. You will have to convert this pressure from mm Hg to Pa. 1 mm
Hg = 133.32 Pa.

18. 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
and clean the beaker with plenty of tap water followed by deionized water.

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Experiment 5 - Measurement of R

Name: ____________________________

Course: ____________________________

Day ____________________________

Time: ____________________________

TA Name ____________________________

You must submit this sheet with your report.

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Results, Discussion and Questions

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 of the first graduation / mL - _______________________
Correction for “dead” volume / mL +_______________________
Volume of gases in the burette / mL =_______________________

Height of the water column / mm _______________________

Temperature / 0C _______________________

Atmospheric pressure / mm Hg _______________________

Atmospheric pressure / Pa _______________________

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Show all calculations:

1. From the measured height of the water column, calculate Pgases in kPa. (Equation (5.30))

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:

(5.31)

8. Why must you wait after the end of the reaction before taking your measurements?

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9. If you did not measure and take into account the “dead volume” in the burette, would your
measured value of ‘R’ be higher or lower? Explain.

10. In the reaction between magnesium and hydrochloric acid (HCl), the HCl was in huge
excess. Why was this necessary?

11. In this experiment the fluid used in the gas burette was water (primarily for convenience and
safety). However, any fluid could be used and most measurements of pressure using this
type of apparatus are done using mercury, hence the mm of Hg as units of pressure. If the
gas burette and beaker had been filled with mercury, how high would the column of mercury
have been for your experiment? The density of mercury is 13.5 g mL-1.

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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)

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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.

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