School of Chemistry

CHM1051 Lab Manual

Chemistry I Advanced
2020
 Introduction

Table of Contents
Student Information
(i) Introduction 2
(ii) Practical Timetable 3
(iii) Aims of the Laboratory Course 4
(iv) Structure of the Laboratory Course 4
(v) Icons Used in this lab manual 4
(vi) General Information 5
(vii) Laboratory Hours and Contact Details 5
(viii) Laboratory Rules 6
(ix) Pre-Lab Questions and Laboratory Reports 6
(x) Assessments 6
(xi) OH&S Information for Undergraduate Students 8
(xii) Hazards, Risks and Risk Assessments 10
(xiii) Useful Equations and Information 13
(xiv) Glassware Guide and Errors 15
(xv) Health and Safety – Safety Quiz 17

Practical Exercises - Skills

Techniques Exercise 1 Geometric Models: VSEPR Method 19
Skills Exercise 2 Quantitative Analysis of Vitamin C in Ribena® 25
Skills Exercise 3 Copper to Copper – The Copper Cycle 30
Skills Exercise 5 Equivalence Points and pKa via Experimental Methods 42

Practical Exercises - Inquiry

Inquiry Exercise 4 IDEA#1: UV-Vis Analysis of Water Samples 35
Inquiry Exercise 6 IDEA#1: QC – The Calorimetric Analysis of Baking Powder 49
Inquiry Exercise 7 IDEA#2: Rate Law Determination 55
Poster Exercise 8 The TEK Experiments 63

Appendix Exam Data Page 66

Periodic Table of Elements Back cover

(i) Introduction
Welcome to the CHM1051 laboratory experience. Chemistry is fundamentally an experimental
science, and it is the joy of designing and testing ideas with experiments that both explore and
impact on the world around us that has made chemistry so fascinating and innovative. This
practical course is intended to introduce you to some of the most important laboratory skills and
techniques used in chemistry, skills that should be useful to you even if chemistry doesn't become
your major! However, we hope that this lab course will do more than just give you good technique.
As practicing chartered chemists, we would like you to see how some of the theoretical principles
of chemistry were uncovered, and how chemistry is applied on a day-to-day basis all over the
world. Above all, we hope that you will enjoy the course, make new friends, and acquire some of
the interest and fascination for chemistry that your lecturers and demonstrators have.
Dr. Cheow Yuen Lin, Unit Coordinator, 2020

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 Introduction

ii Chemistry CHM1051 Practical Timetable 2020

GROUPS Thursday 9am to 1pm and 2pm to 6pm,Lab 3705 and 37062
Report Due1
Week Date2 Laboratory Exercises

5/3 O-Week
Bye week - No Lab This Week
1 12/3

Introduction (Health and Safety)

2 19/3 Skills Ex 1 – Geometric Models: VSEPR Method 7 days
3
Individual Online Assignment Due

3 26/3 Skills Ex 2 – Quantitative Analysis of Vitamin C in Ribena® 7 days

4 2/4 Skills Ex 3 – From Copper to Copper 7 days

5 9/4 Inquiry Ex 4 – UV-Vis Analysis of Water Samples 7 days

16/4 Mid-semester break (one week)

7 days
6 23/4 Skills Ex 5 – Equivalence Points and pKa

7 30/4 Inquiry Ex 6 - IDEA#1 Quality Control - Analysis of Baking Powder 7 days

8 7/5 Bye week - No Lab This Week

Wesak Day

9 14/5 Inquiry Ex 7 - IDEA#2 Rate Law Determination 7 days

10 21/5 Poster Ex 8 - The TEK Demonstrations

Library Workshop- Presentation Skills (10.30 am and 3.30pm)

11 28/5 Poster Ex 8 – The TEK Experiment Presentation

12 4/6 Bye Week – No Lab This Week

1
Reports are due at the time of the start of your normal laboratory session,9:00 am or 2:00 pm, on the given
number of days after completion of the experiment (including weekend and public holiday days).
2
Week commencing. Check your timetable to confirm the dates of your scheduled lab sessions.
3
The online assignment is due on Monday 23 March 11.00 PM for all students

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 Introduction

(iii) Aims of the Laboratory Course

The laboratory course has five main aims.
 Understanding scientific method.
Scientific method is important across all the sciences. It develops critical thinking and analysis. You
will be shown the basis of scientific inquiry or how to pose questions, find evidence and formulate
answers (and do it again if you still need evidence).
 Illustrating theoretical principles.
Laboratory work serves to illustrate many of the somewhat abstract theoretical principles that you
are taught in lectorials and to demonstrate their practical application.
 Gaining experience in the practice of chemistry.
This is an important skill for anyone involved in the field of chemistry as well as the wider fields of
science.
 Developing manual skills.
There are many skills involved in handling laboratory instruments and equipment, in carrying out
chemical transformations, and in making chemical measurements. These skills can only be learned
by practice. As you become more skilled, you gain confidence both in what you do and in chemistry
as a subject. As you gain confidence, your ability to study and to master new topics improves.
 Enhancing teamwork, time management skills and broader communication skills – both to peers
and the general public.
These skills are important for you to be able to use and make the most of scientific skills and
knowledge that you accrue doing your academic study.
(iv) Structure of the Laboratory Course
The class is divided into groups, so that during any laboratory session each group may be carrying
out a different exercise. You should carefully check your program so that you know which exercise
you will be doing and you should thoroughly read the exercise and perform all associated pre-lab
activities before the session. This will usually include a pre-lab video and quiz which will be found on
Moodle. It might require you to consider your aim, draw out your method or look something up. All
of these pre-lab activities are designed to help you complete the lab faster and are a hurdle
requirement. During the semester, you will undertake nine weeks of practical work.
(v) Icons Used in this Manual
Work on your Good scientific Something to
own practice think about

Work in a pair Use the Standard Hazard exists

Operating
Procedure

Work in a group Hot. Take care Corrosive

of three

Work in a group Harmful Clean and put

of four away all
glassware used

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 Introduction

(vi) General Information

Materials Required
During your lab session, you will have access to all glassware, equipment and
chemicals that you will need. You will also need the following:
 This laboratory manual.
 A dedicated laboratory notebook (stapled A4; see example to
the left), ruler, calculator and pen.
 Protective clothing (laboratory coat) to protect you and your
ordinary clothing from damage by chemicals or fire.
 Fully enclosed shoes with firm soles are required at all times
when in the laboratory. Note: You will be asked to leave the laboratory
if you wear open-toe or other inappropriate footwear (including
thongs, sandals, ballet shoes and slippers!) during your lab session.
 Laboratory safety glasses which must be worn at all times
during lab. Students who wear contact lenses should purchase
special wrap-around safety goggles.

(vii) Laboratory Hours and Contact Details

Laboratory classes Thursday Morning 9pm to 1pm Afternoons 2 pm to 6 pm
Doors close 9.15 am and 2:15 pm
The contact e-mail for CHM1051 Unit Coordinator is cheow.yuen.lin@monash.edu

You must not start work until your TA is present in the laboratory.

(viii) Laboratory Rules

Attendance: The laboratory component is a hurdle requirement for this unit. If you
arrive late you will miss the safety briefing, and will not be permitted to commence the
class. The doors to the lab will close 15 minutes after the labs commence and
attendance will not be permitted after this time. The pre-lab exercise must be
completed and passed in order to undertake the laboratory exercise prior to laboratory
entry
It is your responsibility to ensure that the work spaces used are thoroughly cleaned and dried, and
that all equipment is put away before you leave.
Note: The School of Chemistry takes your well-being and safety, and that of everyone in
the laboratory, very seriously. As such you can be asked to leave the laboratory for the
following reasons (see Safety Rules and Safety Precautions):
 Aggressive, offensive, or intimidating behaviour
 Behaviour which is deemed to be hazardous to yourself and/or class mates
 Wearing inappropriate footwear
 Not wearing appropriate safety equipment
 Using mobile phones in the laboratory

You may be allowed to continue the laboratory course but only after consultation with the first year
coordinator.

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 Introduction

Absences: If you are unavoidably absent from any session you should inform the lab staff as soon
as possible. If you are absent due to illness, you should provide a copy of your medical certificate
and a completed in-semester special consideration form to the front counter of the first year
laboratory no more than 2 days after the due date or the date of the practical. These MUST be
supplied if applying for a reschedule or an exemption. If you are absent due to exceptional
circumstances beyond your control, provide a completed in-semester special consideration form
along with supporting documentation to the front counter of the first year laboratory as soon as
possible. If there are exceptional circumstances beyond your control that mean you may miss a
laboratory session and you know in advance, provide a completed in-semester special consideration
form along with supporting documentation to the front counter of the first year laboratory as early as
possible. You may also be eligible for special consideration if you can show your obligation to military
service, jury service, emergency services such as the Country Fire Authority or Monash Sport's
athlete support program if you are participating in a key event.
Where possible, arrangements will be made to reschedule the missed exercise. As per faculty policy,
students are eligible for only one laboratory exemption per semester and then only upon approval of
a special consideration application.
If you have serious difficulties of any kind throughout the year, you should also notify the Faculty of
Science Office in writing and talk to the unit coordinator, Dr Cheow Yuen Lin. For more information,
please refer to the CHM1051 Unit Outline.

(ix) Pre-Lab Questions and Laboratory Reports/Proformas

In this unit, your pre-lab questions must be completed online, via Moodle, before each laboratory
session. The pre-lab exercises close 30 minutes prior to the beginning of that practical session and
must to be submitted before this time. The pre-lab questions are a hurdle and must be passed in
order to be allowed to complete the practical exercise. If a pass mark has not been obtained for the
pre-lab questions, then you will not be able to do the practical exercise or reschedule. Please note
that no exemptions are given for the pre-lab exercises.
Your lab report will be completed on Moodle, as an online laboratory report, but will also include your
laboratory notebook pages, and may also include things like graphs plotted on graphing paper or an
instrument printout.
Your laboratory reports must be completed on Moodle by the due dates. These are found
in the laboratory timetable and on Moodle. For the techniques exercise, the due date
for submission is three days following completion of the exercise; for all other
exercises, the report is due in one week (seven days). These include weekends and
public holidays. Reports are due at the start time of your normal laboratory session (9:00
am or 2:00 pm). Note that submission for the Online Laboratory Reports will close at
these times, and late submission will not possible.
Please note that all results must be written in pen (not pencil), as per industry standards. This
standard protects you by showing your work is original and has not been altered. It also ensures that
your documents will scan properly for Moodle. Laboratory notes written in pencil will not be accepted.
Graphs can be plotted in pencil.

(x) Assessment
The laboratory assessment component constitutes 35% of the total mark for CHM1051.
To pass this subject you must pass the laboratory component of the course (i.e. 50% minimum).
Your assessment will be based on:
a) Your pre-lab exercises (7 x 0.40 %)
b) The way in which you work in the laboratory (participation, experimental techniques),
the results that you achieve, your analysis and your reports (7 x 3.60 %)
c) Your TEK poster and oral presentation (4.00 %)
d) The results of your OLA (online assignment) (3.00 %)

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 Introduction

Each practical session is marked out of 45. Each pre-lab quiz is marked out of 5 and passing this is
a hurdle requirement to complete that practical exercise. The group poster presentations are each
marked out of 50. Marking schemes are given on Moodle for each exercise. You can keep track of
your lab marks via Moodle.
Absences: See above under
“Laboratory Rules”
Laboratory Notebook: For most
practical sessions, 10 of the 45 marks
will come from your laboratory notes
recorded during the class.
All experimental records must be
recorded in a laboratory notebook.
This should be a bound (preferably
stapled), A4 notebook. Recording
results on the practical manual, pieces
of paper towel, scrap paper and loose
notepaper is strictly forbidden!
A typical lab notebook entry (see
example to the right) MUST be written
in pen, and should include:
 Your name, student ID and
names of any partners
 Title of experiment
 Date commenced (and finished
if applicable)
 Details of any changes you
made to the method, or details
of any experimental method that
you designed yourself
 All experimental observations
and calculations
 All experimental data
 A signature from your TA
Preparing tables beforehand will save you time in the lab. It is also helpful to make notes of any
unusual events or outcomes (e.g. unexpected results) and possible explanations discussed with
your demonstrator. This makes writing your discussion section of your report much easier.
The typical mark breakdown for your laboratory notes may be:
Name and student ID (& partner if
1 All results, data and observations recorded 1
applicable)
Punctuality - showed up to the lab on time
Experiment title and date recorded 1 1
(10.00 am or 2.00 pm)
Correct style of laboratory note book 1 Good attitude and participation during class 1
Good housekeeping (all lab glassware,
Notes written in pen 1 1
reagents and apparatus cleaned up)
Method referenced (including changes if
1 Laboratory notes signed by TA 1
applicable)

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 Introduction

Learning Skills - Online Assessment

The Online Assessment (OLA) is designed to give you practice at writing Aims, Discussions and
Conclusions, and to give you feedback on your writing. You will complete the OLA using results given
to you (via Moodle) from an experiment. The Online Assessment is completed via Moodle, under the
Laboratory tab.

The assessment will require you to submit the following:

Discussion - max 300 words (10 marks)

Conclusion - max 50 works (5 marks)

You can submit these via Moodle, as a single pdf or word document.

The Online Assessment will be available via Moodle from Monday 9 March and is due by Monday
23 March 11.00 PM.

(xi) OH&S Information for Undergraduate Students

Safety Rules
 Shoes covering the whole foot must be worn. Thongs, sandals and ballet flats are never
allowed.
 Full length lab coats must be worn at all times.
 Safety glasses must be worn at all times in the proper manner (OH&S Regulations).
 No eating, drinking, or smoking.
 Long hair must be tied back.
 Any injury must be reported to the demonstrator and to the preparation room
staff.
 No visitors to the lab are allowed.
 Do not run in any part of the chemistry department.
 All accidents must be reported to your demonstrator.
 Any intoxicated student will be required to leave the laboratory immediately.
 No mobile phone use in the laboratory at any time.

Safety Precautions
Notify your demonstrator or the laboratory staff of any incident, hazard, or equipment fault that you
become aware of.
1. Fire must be avoided. Most volatile organic compounds are inflammable and must never be
used near a naked flame. Check with your demonstrator before working with solvents.
2. Fire on the bench can often be extinguished by smothering with a fire blanket or damp rag. Fire
extinguishers are provided for use by trained personnel i.e. your demonstrator or laboratory staff.
3. Clothing on fire. Get the person on the floor as quickly as possible and roll them to smother the
fire. (Damage to respiratory passages and eyes may be caused if the person remains standing.)
Fire extinguishers must not be used to extinguish burning clothing. A safety shower or fire
blanket should be used.
4. Chemicals may constitute a hazard because of toxic or corrosive action as well as from fire. In
many instances use of a dispenser will be recommended.
5. Chemicals on the skin or in the eyes should be removed immediately by washing with plenty of
water. Safety shower and eye wash facilities are located throughout the labs.
6. If a chemical is spilt on the bench or floor consult your demonstrator about safe ways of cleaning
it up. Ensure anything contaminated with the chemical is not placed in the general rubbish bins!

8
 Introduction

7. Chemicals with toxic or irritating vapours will be placed in the fume hoods and must be kept
there. Some chemicals that need special care in handling are:
• strong acids and alkali (bases) • toxic chlorinated solvents such as dichloromethane
• bromine, phenols, cyanides, sulphides • highly inflammable solvents such as acetone

Your Roles and Responsibilities

Like all other members of Australian society, you have the right to a healthy and safe environment
in which to work and study. Monash University has an extensive network of Occupational Health &
Safety staff & facilities, whose purpose is to ensure that this goal is achieved.
 As a student at Monash University you also have certain roles and responsibilities in relation to
Occupational Health and Safety, in order to help ensure your own health and safety and that of
other students, staff, visitors to the University and the general public. These are summarised
below.
 A wide range of OHS resources are available to you, some of which are listed below, but you are
also encouraged to seek out further information in this area. If you have any questions or
concerns about any of this, or about any other OHS issues, please discuss them with any of the
contact people listed below.
General
 You must read and understand this information sheet before undertaking practical classes.
 The School’s academic and technical staff will give you specific information relating to the location
of OHS facilities in your lecture theatre or laboratory, and details of practical classes in which you
are involved. You must listen to this information and comply with any health and safety
instructions.
 If you are ever unsure of the correct and safe procedure to be followed, ask one of the technical
or academic staff. Do not rely on information from other students.
Evacuations
 You should ensure you are aware of the location of fire exits, extinguishers and other emergency
facilities in your laboratory or lecture theatre, and also of the point at which you should assemble
after an evacuation. This information is available from the academic or technical staff in the area,
and is also clearly signposted.
 You should also ensure that you are aware of the meaning of the different tones produced by the
alarm system. Drills will be held regularly to assist with this.
 You also have a responsibility to ensure that if an alarm sounds you behave sensibly & do not
panic. This includes heeding the alarms tones, listening carefully to all voice announcements,
complying with instructions from Wardens, and if necessary evacuating in a calm & orderly fashion
and proceeding directly to the nominated assembly point.
First Aid
 You should not provide first aid or emergency medical assistance to any person unless you have
received formal First Aid training.
 However, you should be aware that most of the technical staff in your laboratory have been
formally trained in First Aid, Asthma Management, etc.
 You should also make sure that you are aware of the location of all emergency facilities in your
laboratory (eye-washers, safety showers, etc). The technical staff will give you this information
at your first laboratory session and facilities are also clearly signposted.
Incident Reporting
 In the past, some people have been reluctant to report incidents because they feel they might get
someone else into trouble. However, the reporting process is not intended for that purpose! We
would prefer you to think of it as a way of letting us know about an issue so we can
make sure it is resolved before anyone gets into trouble.

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 Introduction

 So, if you witness or are involved in an incident which you feel may have safety or security
implications, whether or not anyone was hurt, please report it as soon as practical to one of the
contact people listed below.

Key OHS Contact People

 Any of the School’s technical staff.

(xii) Hazards, Risks and Risk Assessments

Hazard
The potential to do harm, due to the inherent nature of the object or situation.
Eg. The blade of a sharp knife
The volatility, flammability and dense vapour of diethyl ether
An electric hotplate which has been turned on
Water running from a tap
The corrosive properties of a concentrated hydrochloric acid solution

You need to be able to IDENTIFY hazards so that you can consider possible risks.
When you have identified the hazards, find out more about them as necessary.

Risk
The probability that a harm may actually happen. E.g.
 There is a risk of cutting yourself if a sharp knife is used incorrectly
 There is a risk that diethyl ether will catch fire if it is used in the proximity of a source of ignition
 There is a risk of burning yourself if you happen to touch the top of an electric hotplate which has
been left on
 There is a risk of causing a flood in a laboratory if the running water from the tap is not directed
down a suitable drain
 There is a risk of incurring a skin burn from hydrochloric acid if it is spilt on the skin when
transferring some of the acid and you do not either wash it off quickly or use protective gloves

There actually has to be a potential for exposure to the hazard. E.g.

 There is no risk of fire from diethyl ether if the container is closed and it is stored safely and there
is no source of ignition

Risk Assessments
The process used to minimise harm:
 Identify the hazard
 Determine the risk (see Table 1.2 on following page)
 Categorise the risk based on the likelihood of exposure and the consequence of exposure
 Decide on appropriate / suitable means of controlling and minimising any risk, and disposing of
any waste produced
 Implement these measures and proceed
There are risks we assess every day on the road (e.g. travelling through an intersection when the
lights are changing!)
Risk assessments MUST be carried out before proceeding with any practical work. For most of the
exercises you undertake this semester, the risk assessment is provided for you. However, for
Exercises 3 and 6, you will need to complete your own risk assessments before undertaking any
practical work in the laboratory.

To complete your risk assessment you will need to know the possible risks of each chemical or
situation (e.g. broken glassware, use of electrical appliances). MSDS (Material Safety Data Sheets)

10
 Introduction

or SDS (Safety Data Sheets) will need to be consulted for each chemical. When you consult the
MSDS sheet look under HAZARDS IDENTIFICATION to help you determine the risk. Look under
ACCIDENTAL RELEASE MEASURES to help you complete controlling the risk. A sample risk
assessment is reproduced on the following page. If there are not enough boxes on the Hazard
Identification and Risk Assessment sheet then continue on a separate sheet of paper OR divide
each row into two rows.

When working with chemicals it is very important that you understand what you are working with,
what you are doing, and why. To write a Risk Assessment you need to list your materials and read
all relevant notes about a chemicals behaviour in the MSDS or SDS. Categorise the risk and discuss
with demonstrator if you have any questions. Lists the control measures that are relevant for the
chemical you are using e.g. use of fumehood; wear safety glasses and lab coat.
See http://www.monash.edu/__data/assets/pdf_file/0004/189517/risk-management-chemical.pdf
for further information on performing a chemical risk assessment.

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 Introduction

Table 1.1: Laboratory Exercise Partial Risk Assessment

Identify the HAZARD – Determine the RISK – CONTROL the Risk – DISPOSAL of
The POTENTIAL to do The PROBABILITY that PREVENTING an incident WASTE
harm harm may result (i.e. how do you minimise
(i.e. the chemical or (i.e. what could occur, and the risk, and therefore
situation) the Risk rating associated prevent it from happening)
with it)
dichloromethane Limited evidence of a Wear safety glasses, lab Halogenated
carcinogenic effect. coat, gloves (PPE). Avoid waste carboy in
Medium Risk breathing vapours, mist or fume cupboard
gas. Work in fume hood.
sodium bicarbonate Non-hazardous. Wear safety glasses, lab Corrosive waste
Low Risk coat, gloves (PPE). Avoid carboy in fume
breathing dust formation. cupboard
sucrose Non-hazardous. Wear safety glasses, lab Solid waste
Low Risk coat, gloves (PPE). Avoid container
breathing dust formation.
aspirin Harmful if swallowed. Wear safety glasses, lab Solid waste
Irritating to eyes, respiratory coat, gloves (PPE). Avoid container
system and skin. breathing dust formation.
Medium Risk
electrical appliances Possible risk of electrocution Take care with use. Ensure N/A
if in contact with water. appliances are tested
Low Risk annually. Minimise
interaction with water.
broken glassware Sharp when broken Take care with use of Broken glass /
Cuts and stab wounds from glassware. Do not handle contaminated
sharp edges possible. broken glass – use dust pan glass bin
Medium Risk and brush to collect.

Table 1.2: Risks can be categorised as Low, Medium, High or Extreme.

Consequences
First aid Medical Admission Fatality/permanent
No Injury
treatment treatment to hospital disabling injury
Insignificant Minor Moderate Major Catastrophic
Almost Certain Medium High High Extreme Extreme
Likely Medium Medium High High Extreme
Likelihood

Possible Low Medium Medium High High

Unlikely Low Low Medium Medium High
Rare Low Low Low Medium Medium

Note: Extreme risks are not to be undertaken by undergraduates.

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 Example Equations and Calculations

(xiii) Useful Equations and Information (Not Provided in Exam)

Tips: Always include your units!!! You will lose marks if your units ( mol, g, M, L, etc.) are not
included in your workings and in your final answer.

Always round your final answer to the correct number of significant figures! Ask your
demonstrator if you are not sure what this means, and see examples on next page.

Equations

m=nM (or equivalently n = m / M)

where: n = number of moles (mol)
m = mass in grams (g)
M = molecular mass, in g mol-1 (can also be written as Mw, Mr and MW)

 To calculate moles, concentration or volume (for solutions):

n=cv
where: n = number of moles (mol)
c = concentration in M (aka molarity, mol L-1 or mol dm-3)
v = volume in litres (L or dm3)

 To calculate concentration or volume when performing a dilution:

c1  v1 = c2  v2
where c1 = concentration of initial solution v1 = volume of initial solution
c2 = concentration of final solution v2 = volume of final solution
Note: Units for concentration and volume must remain consistent e.g. if using litres (L) for v1 you
must also use litres for v2.

Conversion

Volume: Mass:
1 litre (L) = 1000 millilitres (mL) 1 gram (g) = 1000 milligrams (mg)
1 millilitre (mL) = 1000 microliters (μL) 1 milligram (mg) = 1000 micrograms (μg)

Moles:
1 mole (mol) = 1000 millimoles (mmol)

Scientific Notation:
100 = 1 x 102 1000 = 1 x 103 10000 = 1 x 104 etc.
0.1 = 1 x 10-1 0.01 = 1 x 10-2 0.001 = 1 x 10-3 etc.

Units of Concentration:
M = molarity = mol/L = mol L-1 = mol dm-3
ppm = parts per million (10-6) = mg L-1; μg mL-1; μL L-1; μg g-1 = mg/L; μg/mL; μL/L; μg/g

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 Example Equations and Calculations

Moles and Masses Calculation Examples

Q1. How many moles of sulfuric acid are there in 250 mL of 0.200 M H 2SO4?
A. n=cv
= 0.200 mol L-1 x 0.250 L
= 0.0500 mol
= 5.00 x 10-2 mol

Q2. What is the molecular mass of H2SO4? (See Periodic Table on back cover and work to 3
decimal places)
A. M(H2SO4) = 2 x M(H) + M(S) + 4 x M(O)
= 2 x 1.008 + 32.066 + 4 x 15.999
= 98.078 g mol-1

Q3. What is the mass (in grams) of H2SO4 in Q1 above?

A. m=nM
m = 5.00 x 10-2 mol x 98.077 g mol-1
= 4.90 g (retaining 3 significant figures in the result, consistent with the data given).

Q4. 50.0 mL of a hydrochloric acid solution reacts exactly with 20.5 mL of 0.212 M NaOH
(sodium hydroxide). Calculate the molarity (M) of the hydrochloric acid solution.
A. We require the amount (in mole) of HCl per litre of solution.
We know the reaction is NaOH(aq) + HCl(aq) → NaCl(aq) + H2O(l)
Molar ratio = 1 : 1
So 50 mL of hydrochloric acid solution contains the same number of moles of HCl as 20.5
mL of 0.212 M sodium hydroxide solution contains moles of NaOH
i.e. n = c  v, so
nNaOH = 0.212 mol L-1 x 0.0205 L
= 0.004346 mol
= 4.35 x 10-3 mol
= nHCl
Therefore the concentration of HCl is:
c=n/v
= 4.346 x 10-3 mol / 0.0500 L
= 0.08692 mol L-1
= 8.69 x 10-2 mol/L or 8.69 x 10-2 mol L-1 or 8.69 x 10-2 M (retaining 3 significant figures)

14
 Glassware Guide

(xiv) Laboratory Glassware Guide: Identification and Errors

Beaker Erlenmeyer/ Side-arm Filter Buchner Funnel Schott Bottle

Conical Flask Flask

Short stemmed Glass Funnel Watch Glass Hirsch Funnel Micro Test Tube
Funnel

Graduated/ Graduated Pipette Volumetric/ Burette Standard/

Measuring Cylinder Errors: Bulb Pipette Error: Volumetric Flask
Errors: 2 mL ± 0.02 mL Errors: 25 mL ± 0.05 mL Errors:
10 mL ± 0.2 mL 5 mL ± 0.04 mL 5 mL ± 0.015 mL 25 mL ± 0.04 mL
25 mL ± 0.5 mL 10 mL ± 0.10 mL 10 mL ± 0.020 mL 50 mL ± 0.05 mL
100 mL ± 0.75 mL 25 mL ± 0.050 mL 100 mL ± 0.08 mL

15
 Glassware Guide

Weighing vial Auto pipetter Bulb for glass Plastic cuvette

pipetter

16
(xv) Health and Safety Quiz

Before attending your first laboratory practical session you need to attend the introductory session
designed to re-introduce you to the First Year Laboratories, to acquaint you with the laboratory safety
features and rules, and watch the safety video. Once you have viewed this video you should
complete the safety quiz below.

Please let the laboratory supervisor know if you have any medical condition or special
circumstances that could affect your ability to participate in the laboratory program.

Safety Quiz

Name Demonstrator

It is important to familiarise yourself with the layout and facilities of the First Year laboratories. Read
carefully through the Introduction to this Manual. Enter the following information into your
laboratory manual. Have this copy signed off by your demonstrator.

1. Identify and locate the following (tick when located):

Fire Hose Reel (Water) Safety showers

CO2 Fire Extinguisher Emergency exits
Fire blanket Eye-wash equipment

2. In which direction/s are the emergency exits? NORTH / EAST / SOUTH / WEST

3. Where are the evacuation assembly areas for the First Year Chemistry laboratories?

4. How many eye-wash/safety shower stations are located throughout the lab? _______

5. For which types of fires should water NOT be used?

17
6. What safe lab practises should be observed before commencing any work in the laboratory?

a. b.

c. d.

e. f.

7. In the event of glassware breakages:

Whom should you inform?

How should the broken glassware be
collected?
Where should the broken glassware be
disposed?

8. In the event of a burn or chemical spill on your skin, what procedure should be followed?

9. Name six things not to do in the laboratory.

a. b.

c. d.

e. f.

10. Where is the Learning Centre located?

11. What constitutes plagiarism in the laboratory? What is the penalty?

Your Signature: ____________________________ Date: _____________

Have your demonstrator check your answers and sign off on your quiz before completing your first
practical exercise:

Demonstrators Signature: _______________________ Date: ____________

18
Techniques Exercise 1: Geometric Models - Valence-Shell Electron-Pair Repulsion
(VSEPR) Method
Learning Outcomes:

1. Construct models using a model kit to build and aid visualisation of chemical structures.
2. Manipulate common diagram types and their conventions to represent a range of
inorganic molecules.
3. Visualise molecules in three dimensions to enhance understanding of shapes and
stereochemistry.
4. Generate molecular geometries, based on bond numbers and angles.

Prepare for this exercise by drawing 10 (blank) copies of Table 1.1 into your laboratory
notebook.

Reading: Blackman et al., Chemistry (2016), Chapter 5;.

NOTE: This exercise covers examinable material, which will not be covered in the
workshops.

1. Introduction

Lewis structures are schematic drawings that show how the atoms in a molecule are connected.
Unpaired electrons are shared with neighbouring atoms to form single, double or even triple bonds.
However, although Lewis structures can show the valence electron distribution, they do not
accurately depict three-dimensional structures.
Historically, a number of models have been proposed for the purpose of describing molecular shapes
and structure. One of the easiest to apply of these is the Valence-Shell Electron-Pair Repulsion
(VSEPR) model. The basis of the VSEPR model is the consideration of the repulsive forces between
pairs of valence electrons, and it is assumed that only the electrons in the valence shell influence
the molecular geometry.

Consider the two systems in Figure 3.1. The figure on the left represents the centre atom in a small
molecule with two regions of negative charge (electron domains) surrounding it. VSEPR theory
predicts these two regions of negative charge will adopt a position that minimises the repulsion, that
is, maximises the distance between them. The figure on the right represents a similar case with
three electron domains. These configurations ultimately determine the geometry of the molecule.

Figure 1.1. VSEPR models with two and three

electron domains about a spherical centre.

2. Exercise

In the following exercise you will be presented with a molecular model set which you can use to
predict and analyse the shapes adopted by different small molecules. Your demonstrator will provide

19
you with a list of molecules and your task is to construct these examples and complete a description
of their structural properties.

Table 1.1: Example of the tables found in the proforma. Each of these criterion (2.1 – 2.8) are
addressed below with respect to the example of the phosphite ion, PO 33-.

2.1. Lewis Structures (Blackman et al., Chemistry (2019), Chapter 5.3)

Follow the five steps below to construct a Lewis structure for a molecule or ion.
i. Determine the total number of valence electrons in the molecule or ion.
ii. Arrange the atoms to show how they are connected – atoms are grouped around a central
atom, which is usually the least electronegative (atom furthest away from fluorine on the
periodic table, although never hydrogen! Why not?). Place a bonding pair of electrons
between each pair of adjacent atoms to give a single bond.
iii. Begin with the terminal atoms and add enough electrons to each atom to give all of the
terminal atoms an octet (except for hydrogen! Why?).
iv. Place any electrons left over on the central atom.
v. Minimise the formal charges; if the central atom has fewer electrons than an octet, use lone
pairs from terminal atoms to form multiple bonds to the central atom in order to achieve an
octet (but be aware of exceptions to this rule; e.g. Be and B!).
The formal charge for each atom:
 depends on the difference between the number of valence electrons in the free
atom and the number assigned to it in the Lewis structure,
 is a way of computing the charge distribution within a Lewis structure; the sum of
the formal charges on the atoms within a molecule or ion must equal the overall
charge on the molecule or ion,
 does not represent a true charge on an atom; it is simply used to predict the most

20
 likely structure when a compound has more than one possible Lewis structure.
Formal Charge = # Valence Electrons – (# Non-bonding Electrons + ½ # Bonding Electrons)
Using the phosphite ion as an example:

21
2.2. Number of Atoms Bonded to the Central Atom

The phosphite ion has three atoms bonded to the central atom.

2.3. Number of Non-bonding Electron Pairs on the Central Atom

The phosphite ion has one electron pair on the central atom.

2.4. Parent Geometry (Blackman et al., Chemistry (2019), Chapter 5.4)

The parent geometry corresponds to the number of 'electron domains' about the central atom. An
electron domain may be a single bond, double bond, triple bond or a lone pair. The fundamental
principle governing geometries in VSEPR theory is that electron domains render positions such that
they are as far away from each other as possible due to the electrostatic repulsion. Names for the
different parent geometries are given Table 1.2. For example, in the phosphite ion example there is
a total of 4 electron domains (3 single bonds and one electron pair). Therefore, phosphite will
possess a tetrahedral parent geometry.

2.5. Molecular geometry with ideal bond angles

The molecular geometry is dependent on the number of atoms bonded to the central atom AND the
parent geometry. The molecular geometry may be different to the parent geometry! E.g. In the PO33-
ion example there are a total of 3 atoms bonded to the central atom, while the parent geometry is
tetrahedral. Therefore, the molecular geometry is trigonal pyramidal.

2.6. Molecular simulation

To aid in visualising the shapes of molecules, next we will use the PhET Simulation for Molecule
Shapes. On a laptop or tablet go to https://phet.colorado.edu/sims/html/molecule-
shapes/latest/molecule-shapes_en.html to access the simulation. On the landing page of the
simulation, choose "Model". This section allows you to see the 3D molecular shape of a molecule
according to a prediction made based on the number of bonding pairs and non-bonding (lone)
pairs. The expected bond angles are also shown. Explore this section and use the information that
you get from the simulations to complete Table 1.2.
Take note of the following features:
• Bonding: allows you to choose the type and number of bonding electron pairs

• Lone pair: allows you to put the desired number of nonbonding electron pairs

• Options: tick “Show Bond Angle” to see the predicted bond angle

• Name: tick “Molecular Geometry” to see the name of the shape that is formed by the
molecule and "Electron Geometry" for the parent shape

22
2.7. Perspective Drawing

The 3-D models will serve as a visual guide to help you with your perspective structures. Use the
following guidelines to draw them correctly:

Consider the molecule such that the center atom and at least one terminal atom are in the plane of
a piece of paper.

(a) Bonds lying in the plane of the paper are represented by a solid line.

(b) Bonds projecting 'into' the paper away from you are represented with a
hatched wedge-shaped line.

(c) Bonds projecting 'out of' the paper towards you are represented with a solid wedge-shaped line.

3. Report

Complete your laboratory report online, via Moodle. Ensure you have completed all sections.

Your online report must be finalised within 7 days of the completion of your class.

Table 1.2: Shape and geometry of model molecules

# Bonding e- # of Lone Pairs VSEPR Molecular Predicted bond

pairs e- notation Geometry angles

2 single bonds 0 AX2 Linear` 180

2 single bonds 0

1 double bond

3 single bonds 1

2 single bonds 1

1 double bond

1 double bond 2

1 triple bond 1

2 single bonds 2

4 single bonds 2

23
24
Skills Exercise 2: Quantitative Analysis of Vitamin C in Ribena®
Learning Outcomes:

1. Learn to competently use a burette and perform a titration in triplicate.

2. Work out reaction stoichiometry from a reaction equation.
3. Back calculate to determine concentration of an unknown acid or base.
4. Understand the role of an indicator, and distinguish between the end point and the equivalence
point of an acid/base titration.

Personal safety: It is essential that safety glasses are worn at all times in the
laboratory. Students should always wash their hands before leaving the building.
Despite only dilute solutions of acids being used, they are still corrosive and caution
should be taken during handling.

Hazard Identification and Risk Assessment

Identify the Hazard Determine the Risk Control the Risk Disposal of waste
(the potential to do harm) (the probability that (preventing an incident)
harm may result)
Ascorbic Acid (solid) Low Handle with care. Wash skin Acidic residue
Irritating to eyes, respiratory immediately with water if spill carboy in fume
system and skin. occurs. cupboard
N-Bromosuccinimide Compound is in Handle with care. Wash skin Acidic residue
Toxic if ingested or inhaled solution and is dilute. immediately with water if spill carboy in fume
(solid) Low risk occurs. cupboard
Potassium Iodide (4%) Solution is dilute. Handle with care. Rinse Acidic residue
Irritating to eyes. Low risk quickly with water if spilt on carboy in fume
Will stain skin. Will still stain skin at skin to avoid staining. cupboard
this concentration
Acetic Acid (1M) Relatively weak acid Wash skin immediately with Acidic residue
Harmful to eyes. and low water if spill occurs. carboy in fume
Corrosive concentration. cupboard
Low risk.
General glassware Medium Handle with care, dispose of Labelled broken
Cuts chipped/ cracked glassware, glass bin
collect broken glass using
dustpan and brush.
If cut occurs, see your
demonstrator, seek first aid.

1. Introduction

Ascorbic acid (molecule 1 in Figure 1.1) is commonly known as vitamin C. It was one of the first
vitamins that played a role in establishing the relationship between disease and its prevention by
proper diet. That disease was scurvy, and was prone to sailors and explorers as far back as the
16th century. The prevention of scurvy was as simple as eating fresh vegetables and fruit (which
contain ascorbic acid). It is a powerful biological antioxidant (reducing agent). Vitamin C keeps the
iron in the enzyme, prolyl hydroxylase, in the reduced form thereby maintaining its enzyme activity.
This enzyme is essential for the synthesis of normal collagen. In scurvy, the abnormal collagen
causes skin lesions and broken blood vessels. Vitamin C cannot be produced in the human body
and must be obtained from the diet (citrus fruits, tomatoes, etc.) or by taking synthetic vitamin C.
In this experiment, the amount of vitamin C is determined quantitatively by titrating the test solutions
(Ribena® and fruit juices) with N-bromosuccinimide (NBS) (2). Vitamin C is oxidised to the diketone
(3) by NBS according to the following chemical reaction (see Figure 1.1):

(1) (2) (3)

Figure 1.1: The oxidation of ascorbic acid via NBS.

What is the correct stoichiometry for this reaction?

It is important to know that although vitamin C is very stable when dry, it is readily oxidised by air
when left in solution. Therefore, the method you are about to use has been developed because it
works in the presence of a variety of other oxidisable substances with one important exception. It
will not work in the presence of sulfur dioxide or sulphite (both of which are commonly used as
preservatives of fruit juices) because they also react with NBS. Hence, only fruit juices free from
artificial preservatives will give reliable results.

In this experiment, a solution of vitamin C is acidified and mixed with a strong solution of potassium
iodide (KI). A solution of an oxidising agent (NBS) is then added slowly. Once
the vitamin C is oxidised, the I- begins to oxidise to iodine, I2, which in turn
combines with other I- ions to form the I3- ion. The indicator in this reaction uses
the I3- ion with starch, which form a dark-blue complex, thus indicating the
oxidation of the ascorbic acid is complete.

1.1 The Auto-Pipette

In this lab you will use a fixed volume auto-pipette. An auto-pipette is an

excellent way to deliver a very precise amount of water or an aqueous solution.
Auto-pipettes often do not work well with solvents other than water due to the
low surface tension of solvent (the liquid will drip out of the tip before you can
deliberately release it).

Use the SOP (standard operating procedure) “fixed volume auto-

pipettor” and practice using the pipette a few times before you
use it to transfer your sample.

1.2 The Volumetric (or Standard) Flask

A volumetric (or standard) flask is a precision instrument for making up a

Figure 1.2: Fixed
measured mass or volume of sample to an accurately determined volume of volume auto-pipette

26
solution. The volumetric flask must be clean but need not be dry. Measure into it, by pipette, the
volume to be diluted or if adding a solid to be dissolved, using a short-stemmed funnel. When making
the level finally up to the mark, use a dropping (Pasteur) pipette for accurate control. Mix the partially
diluted solution thoroughly, by inverting and shaking, before making up to mark - then mix again.
The stopper must be fitted carefully and the contents mixed thoroughly.

2. Experimental Procedure

Work individually and record all experimental data immediately in your laboratory notebook.

Practical skills tests: There are steps in this lab class where your skills will be checked by the YA
so you can be advised where your technique can improve. These are called practical skills tests and
will be checked off by your demonstrator. If your TA is busy when you get up to a certain step, do
not stop and wait. The demonstrator can test you later with water or other glassware; thus, it is
always best to get started rather than wait.
Copy Table 2.1 into your laboratory notebook, and have your TA observe you complete each task.
Table 2.1: Practical skills test table

Practical Skill Satisfactory? Comments from TA

Correctly fill a burette
Accurately read a burette to 2 decimal
places (as confirmed by your TA)
Use auto-pipette correctly
2.1 Determination of Error in Auto-Pipette

Table 2.2: Determining the error in an auto-pipette (copy this table into your laboratory notebook)

Pipette ID Number: Group

Pipette Make and Volume:
Number
Aliquot Number: Weight (g) Volume (μL)
1
2
3
4
5
Mean Mean ± sd

It is important to practice your skills with the auto-pipette to ensure accurate delivery of solution
volume. To determine the error in your volume, after practising using the auto-pipette a few times:

i. Weigh the mass of water in an aliquot from the auto-pipette using the top-loading balance.

ii. Repeat this measurement so that you have a total of five replicates.

iii. The density of water at 22 C is 997.77 kg m-3. Calculate the mean aliquot and standard
deviation of the measurements. Remember to comment on the accuracy of measurement
compared to, for example burettes and pipettes, in your report.

27
2.2 Stock Solution of Ascorbic Acid
i. Using the top-loading laboratory balance, weigh about 0.1 g of ascorbic acid (M = 176.1
g mol-1) into a weighing vial. Cap the vial.
ii. Weigh the vial and contents accurately in the analytical balance room.
iii. Weigh the vial accurately again after tipping the contents into a short stemmed glass funnel
that has been placed in the neck of a 100 mL standard volumetric flask.
iv. Calculate the difference in weight to check that the accurate mass of ascorbic acid delivered
is between 0.08 and 0.12 g.
v. Add 1 M acetic acid through the funnel, to help carry the powder into the flask, until the flask
is approximately ¾ full, and mix the solution. Add the lid and invert several times while holding
the lid on to ensure proper mixing. Your demonstrator can demonstrate the right technique.
vi. When the solution is well mixed (all the solid is dissolved), wait until drips from the stem of
the flask fall below the mark. If there are drops above the mark, they will add
to the volume after it is made up.
vii. Make the solution up to the mark with 1 M acetic acid, and thoroughly mix the
solution again.
viii. Calculate the expected concentration of stock ascorbic acid solution in mol L-1 and label the
flask.

2.3 Burette set up

i Set up the burette as per the diagram (Figure 2.3, right).

ii Rinse your burette with 2 x 5 mL x water, then 1 x 5 mL

NBS solution. Fill the burette with the NBS solution.
Allow enough solution to run out in order to remove any
air in the tip and bring the top level into the range of the
scale.

Why doesn’t the level need to be adjusted to zero?

iii. Read and record the level of the bottom of the

meniscus by estimation to within 0.05 mL.

28
2.4 Standardisation of NBS

i. Using an auto-pipette, accurately pipette 1000 μL (1.000 mL) of the diluted ascorbic acid
solution into a conical flask.

ii. Add 5 mL of 4% KI solution and 10 drops of starch solution.

iii. Titrate with the stock NBS solution until a permanent mauve colour just appears and record
the volumes, reading the burette to ±0.05 mL.

iv. Perform titrations until you have three concordant titres. Results are concordant if they are
within ±0.1 mL of each other. Ideally, they will be within ±0.05 mL from the average. Continue
until you have three concordant results. See your demonstrator if you cannot achieve
concordant results.
v. Record your titration results directly into your laboratory book in a table of the form shown in
Table 3.3.
vi. Calculate the concentration of NBS (mol L-1)
Table 2.3: Example titration results

Titration number: Rough 1 2 3 4 error

Final burette reading (mL) 12.65 21.80 9.85 18.90 ±0.05 mL
Initial burette reading (mL) 1.75 12.65 0.85 9.85 ±0.05 mL
Titre (mL) 10.90 9.15 9.00 9.05 ±0.10 mL

2.5 Method for determining Quantity of Vitamin C (Ascorbic Acid) in Fruit Juice

i. Using an auto-pipette, deliver 2000 μL of your fruit juice sample into a conical flask.

ii. Pour in 5 mL of 4% KI solution, add 10 drops of starch solution and titrate quickly with
standard NBS solution until a permanent blue/purple colour just appears.
iii. Record your titration results directly into your laboratory book in a second table of the form
shown in Table 1.1.
iv. Repeat until three concordant results are obtained. See your demonstrator if you are having
trouble.

v. Repeat method 2.5 for all samples of fruit juice/Ribena ®

vi. CLEAN ALL LABORATORY EQUIPMENT USED,
vii. Calculate the amount in mol of ascorbic acid in each of the 2.000 mL samples
of Ribena and fruit juice.
viii. Calculate the mass of ascorbic acid in each 2.000 mL sample.
ix. Calculate the concentration of ascorbic acid in the fruit juices as mg ascorbic acid per 100
mL of juice.

3. Report

Complete your laboratory report online, via Moodle. Ensure you have performed all necessary
calculations, completed all sections and uploaded your graphs and laboratory notes to Moodle. Your
online report must be finalised within 7 days of the completion of your class.

29
Skills Exercise 3: Copper to Copper – The Copper Cycle
Learning Outcomes:

1. Perform a separation by filtration.

2. Perform simple calculations involving molarities and stoichiometry.
3. Appreciate that solubility rules can simplify the task of converting one compound to another.
4. Understand the difference between a physical and chemical change.

Personal safety: It is essential that safety glasses are worn at all times in the laboratory. Students
should always wash their hands before leaving the building.
Hazard Identification and Risk Assessment
Identify the Hazard Determine Control the Risk Disposal of
(the potential to do harm) the Risk (Preventing an incident) waste
Sodium Hydroxide (4 M) Low risk Avoid contact with skin and wash Acidic residue
CORROSIVE,causes burns, immediately with water if spill occurs. container in fume
damaging to eyes cupboard
Nitric Acid (6 M) Medium – Use in fumehood. Handle with care. Acidic residue
CORROSIVE HIGH risk Use gloves if necessary. Wash skin container in fume
Causes burns, damaging to immediately under water if spill occurs. cupboard
eyes, stains skin.
Sulfuric Acid (6 M) Medium Use in fumehood. Handle with care. Acidic residue
CORROSIVE, causes risk Wash skin immediately under water if container in fume
burns, damaging to eyes. spill occurs. cupboard
Hydrochloric Acid (5.5 M) Medium Use in fumehood. Handle with care. Acidic residue
CORROSIVE, causes risk Wash skin immediately under water if container in fume
burns, damaging to eyes. spill occurs. cupboard
Copper II Chloride Low risk Avoid contact with skin and wash with Residue container
Damaging to eyes, can water immediately if spill occurs. in fume cupboard
irritate skin. Harmful if
ingested or inhaled
Zinc Powder Low Avoid inhalation of solid and spilling onto Put filter paper
Irritating to eyes and skin. Wash skin with water if it comes with zinc residue
respiratory system into contact. in the rubbish bin
Hotplate Low Do not place hands directly over N/A
Burns hotplate or directly on hot surface. Use
wooden peg to remove hot objects.
General glassware Medium Handle with care, dispose of chipped/ Labelled broken
Cuts cracked glassware, collect broken glass glass bin
using dustpan and brush. If cut occurs,
see your demonstrator & seek 1st aid.
Reading: Blackman et al., Chemistry (2019), Chapter 3; CHM1051 Workbook Week 0.

1. Introduction
In chemistry it is very important to be able to manipulate the state of the metal salt or metal. This is
especially important in mining, where the ore that is mined is always in a different form from what we
need for use in manufacturing. For example, Cu 2S ore is heated with air to react it with oxygen to
isolate copper metal. Sulphur dioxde is the by-product (Cu2S(l) + O2(g)  2 Cu(l) + SO2(g)).

In this laboratory exercise, you will take copper through different forms to finally reach
copper metal (Figure 2.1). As you do this, you will gain experience observing and
recording your scientific observations. A very important scientific skill.

30
You will start with copper metal, and at the end, you will have copper metal again. In a five step
process you will explore a number of different chemical transformations and experimental
techniques. You will also need to be conscious of some important safety elements of the exercise,
including the use of concentrated acids and bases. The copper cycle that you will be following is
shown in the flow diagram below.

Cu(s) Cu2+(aq) Cu(OH)2(s) CuO(s) Cu2+(aq) Cu(s)

Figure 2.1: Copper transformations
Decantation
n
1.1 Recording Results and Observations

When recording observations for experiments, it is important to be unambiguous with your wording,
and as specific as possible. Recording accurate observations makes it much easier to work out what
(if any) reaction has occurred – the properties of the reactants and the products (i.e. colour, state,
physical appearance etc.) inform us when it comes to writing the chemical equations. The language
you use to describe your observations is important. For example, ‘clear’ may be an ambiguous word
– is it colourless or transparent? Observations for reactions should cover at least three key points:

What are you starting with? What are you doing? What did you end up with?
(state, colour, bubbles, (chemical addition, heating, (state, colour, bubbles,
sediment) diluting etc.) sediment, temperature)

For example: The aqueous copper chloride solution started out as transparent and bright blue. Upon
addition of 4 M sodium hydroxide a precipitate formed. The solution became opaque (due to the
suspended precipitate) and the colour changed to a very light blue.

1.2 Writing Chemical Equations

In chemistry, chemical equations are written to assist with explaining observations. Today you will
be writing three forms of equations: full equations, ionic equations and net ionic equations. It is
important to remember that the chemical equations you write must match your observations! For
example, if you observed the formation of a solid, the corresponding equation should have a solid
as one of the products. When writing equations always balance the equations and always include
states, that is (s) for solid, (l) for liquid, (g) for gas and (aq) for aqueous (dissolved in water).

Start the process by writing out the reactants on the left hand side (LHS) of the reaction arrow, and
the products on the right hand side (RHS) (1). Next, balance the LHS and the RHS – there should
be exactly the same number of each type of atom on both sides (2). Finally, add in the states (3) –
use your observations to guide you if you are not sure.

Zn + HCl  ZnCl2 + H2 (1) Here the LHS & RHS are not balanced

31
Zn + 2 HCl  ZnCl2 + H2 (2) x 2 the HCl on the LHS to balance the Cl & H atoms

Zn(s) + 2 HCl(aq)  ZnCl2(aq) + H2(g) (3) Add in states

Notice that the HCl and ZnCl2 are depicted as ‘aqueous’. When performing a reaction using water
as the solvent, acids, bases and salts will usually be dissolved in the water, and will thus be present
in their ionic (charged) forms. These ions (charged atoms or molecules) will not be bonded together
when in solution, as they will be surrounded by water molecules. This can be represented by writing
an ionic equation (4). The HCl and ZnCl2 are now represented as dissociated ions:

Zn(s) + 2H+(aq) + 2Cl-(aq)  Zn2+(aq) + 2Cl-(aq) + H2(g) (4)

From the ionic equation we can now determine which atoms/ions have undergone a physical change,
and which are spectator ions. When writing the net ionic equation we omit the spectator ions, as they
do not play a part in the actual chemical reaction. In this example, the chloride ions (Cl-) do not
undergo a change in state (i.e. they remain aqueous) and are thus omitted from the net ionic equation
(5):

Zn(s) + 2H+(aq)  Zn2+(aq) + H2(g) (5)

2. Equipment

2.1 Apparatus
Balance Small beakers pH beaker Pasteur pipettes Spatula
Hotplate Filter paper Glass Rod Wooden peg Wooden peg
Long stemmed filter funnel

2.2 Chemicals

Metallic copper Zinc dust

6 M H2SO4 (sulfuric acid) 6 M HNO3 (nitric acid) (KEEP IN FUMEHOOD!!!)

4 M NaOH (sodium hydroxide) 5.5 M HCl (hydrochloric acid) (KEEP IN FUMEHOOD!!!)

2.3 Safety aspects

Nitric acid, sulfuric acid, hydrochloric acid, and sodium hydroxide are corrosive and
may be dangerous if splashed into the eyes or onto skin. Use the pipettes already in
the acid and base bottles to deliver the volumes you need. Do not pour these liquids into measuring
cylinders. The pasture pipettes will deliver approximately 1mL of liquid. If contact occurs flush
immediately with water and in the case of contact with eyes, seek medical advice. Spills
can be diluted with water and mopped up with an absorbent cloth, which should be
rinsed with water and disposed of in the normal rubbish bin.

32
The reaction of nitric acid with copper metal produces a toxic NO2 gas, which must be kept in the
fumehood! Repeat, this reaction must only be done in the fumehood.

Residues can be safely discarded into the corrosives waste carboy in the fume hood.

3. Experimental Procedure
Work in pairs and record all experimental data into your proforma.

3.1 Part A: Cu2+ from solid copper

Place a clean, dry 100-mL beaker on an analytical balance. Tare the balance, and
then place a strip of copper wire in the beaker. Record the actual mass of copper
added.
In THE FUMEHOOD, add about 10mL of 6M HNO3 to the copper wire (use the
pasture pipette in the HNO3 bottle to do this. The pasture pipettes will deliver
approximately 1mL of liquid. Heat the contents of the beaker on the hotplate until
the copper has fully dissolved and the brown NO 2 gas that is formed has dispersed.
Note: The NO2 gas produced by this reaction is TOXIC! This reaction must be performed in the
fumehood!

3.2 Part B: Cu(OH)2 from Cu2+

IN THE FUMEHOOD, add 4 M NaOH in 1 mL portions to the dissolved copper solution,

with stirring, until a permanent precipitate forms. Test the solution pH by touching your
stirring rod to a piece of pH paper. Continue adding 1mL portions of NaOH until the solution
reaches a pH greater than 9.

3.3 Part C: CuO from Cu(OH) 2

Place the beaker with your solution back onto the steam bath for approximately 10 – 15 minutes
until the solution turns black, the colour change is due to the formation of CuO.

While the solution is on the steam bath set up a suction filtration system with a Buchner funnel that
requires a 4.25cm piece of filter paper. When the beaker containing the CuO has cooled enough to
be handled, start the suction on the filtration system and slowly pour the contents of the beaker into
the funnel. Use a wash bottle of distilled water to make sure all of the solid is transferred, then
wash the solid with two 10mL portions of distilled water.

When there is no more liquid in the funnel, stop the suction and remove the funnel. Place the
funnel in a safe place, being careful not to spill any solid. Pour the filtrate (the liquid that was
collected) from the filter flask into the corrosive wastes container. Rinse the filter flask several
times with water.

3.4 Part D: Cu2+ from CuO

Set up the suction filtration system again and re-attach your Buchner funnel. Before applying the
suction, add approximately 5mL of 6M H2SO4 to the funnel followed by distilled water. You

33
 should begin to see the CuO dissolve. Wait 1 minute, then start the suction to suck the liquid
into the flask. Stop the suction and add another 1-2 mL of 6M H2SO4 followed by distilled
water. Wait 1 minute, then suck the liquid into the flask. Repeat this process until most of the
CuO has dissolved. Finally, pour two 10mL portions of water through the funnel to wash any
excess dissolved copper into the filter flask.

Remove the funnel from the filtration system. Carefully pour the contents of the filter flask into a clean
400-mL beaker. Wash the excess copper solution from the flask into the beaker with a few
small portions of distilled water. You should now have a nice blue solution, indicative of
dissolved Cu2+.

3.5 Part E: Solid copper from Cu2+

IN THE FUMEHOOD, use a small spatula to measure out approximately a pin head’s worth • of
zinc powder. (DANGER: Flammable hydrogen gas is evolved.) Let the reaction continue until
little or no hydrogen gas is evolved. If any blue is still visible in the solution after the bubbling has
stopped, add the Zinc powder in very small portions, and again wait for the bubbling to stop.
Repeat this process until all the blue colour has been removed from the solution. You should
now have solid copper at the bottom of the beaker. Add a few drops of concentrated hydrochloric
acid (HCl) to the Cu2+ solution. Record your observations. You may or may not observe a reaction
here. If you do, write the equation and the net ionic equation. If you do not, explain why HCl was
added to the solid.

Place a new piece of filter paper in your filtration system and use suction to filter the liquid away
from the solid copper. Wash the copper several times with distilled water, and let it air dry in the
funnel for a few minutes. Then stop the suction, remove the funnel, and pour your filtrate into the
corrosives container in the fume hood.

Scrape the copper onto a watch glass (but not before recording the mass of the watch glass).

3.6 Part F: Calculation of Percentage Yield and XRF analysis

i. Use the analytical balance to weigh out a clean and dry weighing vial to the nearest 0.0001 g.
Record the mass. Quantitatively transfer the solid copper into the pre-weighed, clean, dry
weighing vial. Using the analytical balance, weigh the capped vial plus copper sample and
record the mass. Complete the calculations on the results sheet. Submit your copper sample
on a piece of paper towel to your demonstrator who will use a hand held X-ray fluorescence
(XRF) instrument to determine if you really have recovered copper from copper and what the
purity is!

4. Report

Complete your laboratory report online, via Moodle. Ensure you have performed all necessary
calculations, completed all sections and uploaded your graphs and laboratory notes to Moodle.

Your online report must be finalised within 7 days of the completion of your class.

34
Inquiry Exercise 4: Determination of the Contaminant in Regional Lakes
Using UV-visible Spectroscopy
Learning Outcomes
1. Understand the Beer-Lambert Law and its application in absorbance spectroscopy.
2. Qualitative and quantitative analysis of a series of water samples.
3. Constructing and utilising calibration curves to determine unknown concentrations.
4. Collaboration with team members and the demonstrator to successfully complete an
investigative analysis and submit a comprehensive report.

The IDEA Experiments you will come across in units such as CHM1051, BIO1011 and PHS1011
are a little different to some of the lab exercises you will have already done in your Science degree.
These exercises will not come with a procedure mapped out for you, which means that the whole
procedure is NOT written in the lab manual. For some parts of this exercise, you will have to
design and perform your own experiment.

You will be working in a group of 4 students. You need to assign roles within your group and
delegate the work that has to be done over the four hours.

Do not forget that at the end of the four hour session, you need to have finalised all experimental
work, plotted all graphs and planned your discussion section with your group.

"IDEA" stands for Inquiry-Design-Explore-Answer, and that’s exactly what working scientists do in
their professional life.
1. Inquiry: A sound scientific approach to
answering questions and solving problems
always commences with the process of asking
deep questions. What is the quickest way to
perform this experiment? The most ethical?
The least expensive? The ‘greenest’? Are you
able to foresee roadblocks along the way?
2. Design: Once you have considered the
limitations, challenges and practicalities of the
experiment, you can start to design your
experiment. Weigh up what expertise and
techniques you have at your disposal. Ask
questions of each other, your demonstrator,
and the literature, and come up with a flow chart
for how the experiment will proceed.
3. Explore: When you are ready to commence,
delegate different jobs amongst your team, and
start to gather data! You may find along the way
that your design needs to be changed!
4. Answer: Once you have gathered the best data you can, see if you are able to form some
conclusions. Discuss the results of your experiments amongst yourselves and determine
whether the original problem has been solved.

35
Safety comments: It is essential that safety glasses and laboratory coat are worn at all times in the
laboratory. Glasses to be put on at entrance (sliding door) and taken off at entrance as you are
leaving. Wash hands before leaving the building. Gloves should be used when handling chromium
nitrate solution.
Hazard Identification and Risk Assessment
Identify the Hazard Determine the Risk Control the Risk Disposal of
(the potential to do harm) (the probability that (preventing an incident) waste
harm may result)
Copper sulphate Compound is in Handle with care. Wash skin Heavy metal
pentahydrate solution and is immediately with water if spill occurs. residue carboy
Cu(SO4).5H2O (solution) dilute. in fume
Irritating to eyes, & skin. Low risk cupboard
Cobalt sulphate Compound is in Handle with care. Wash skin Heavy metal
heptahydrate solution and is immediately with water if spill occurs. residue carboy
Co(SO4).7H2O (solution) dilute. in fume
Irritating to eyes, Low risk cupboard
respiratory system & skin.
Nickel sulphate Solution is dilute. Handle with care. Rinse quickly with Heavy metal
hexahydrate Low risk water if spilt on skin to avoid staining. residue carboy
Ni(SO4).6H2O (solution) in fume
Irritating to eyes & skin. cupboard
Chromium nitrate Solution is dilute. Wash skin immediately with water if Heavy metal
nonahydrate Medium risk spill occurs. residue carboy
Cr(NO3)3.9H2O in fume
(solution) cupboard
General glassware Medium Handle with care, dispose of chipped/ Labelled
Cuts cracked glassware, collect broken broken glass
glass using dustpan and brush. bin
If cut occurs, see your demonstrator,
seek first aid.

You will be performing this experiment in groups of 3-4, and submitting the final report as a group.
In order to be able to do that, you will need to go onto Moodle and select your group.

Lab Group Selection (BEFORE the lab!)

 Go onto Moodle, to the Laboratory Information workbook, Exercise 4.
 Group sizes should be 4 (or 3) students.
 Make sure you choose a group from your usual lab session
eg. if you attend a Thursday morning/afternoon session, select a "AM/PM 3705/3706"
group.
 You can organise with your friends to make sure you choose the same group.

1. Introduction

Recently, farmers in Western Australia have reported unusual colours in some of the lakes located
near the local mining areas. Following this phenomenon, a federal task force was appointed to
investigate this environmental issue, and specimens have been sent to the Water Science Research
Group here at Monash University. Given the time restraints placed on the research group, the
analysts have asked that the Advanced Chemistry students assist them in analysing the samples
and submitting a report based on their findings.

Today, the Cary 60 UV-Vis spectrophotometers will be used for two purposes:

36
  Comparing the absorbance spectra of known transition metal samples to your authentic
sample, so as to qualitatively determine the contaminants of the water samples

 Constructing a calibration curve using standards of known concentrations and plotting graphs
of concentration vs. absorbance, so as to quantitatively determine the concentrations of
contaminants in the water samples

1.1 Electromagnetic Radiation and Colour

UV-visible (UV-vis) spectroscopy is based on the selective absorption of electromagnetic radiation

(Figure 4.1) by atoms and molecules in the wavelength range of 180-780 nm.

Figure 4.1: Electromagnetic radiation and UV-Visible spectrum

UV-visible radiation has enough energy to cause transitions in bonding electrons. These transitions
are the main reason for the colour of the material. In the case of transition metals, the electron
transitions normally occur in d-orbitals; these are known as d - d electron transitions. Not all electronic
transitions occur at wavelengths within the visible range; however, many of those associated with
aromatic molecules and transition metal complexes fall in this range.

The observed colour of a material corresponds to the wavelength of visible light which is transmitted
by the sample, NOT the wavelength that is predominantly absorbed by the compound. Table 4.1
summarises the relationship between these 'complimentary colours' and the colour actually
absorbed.

Table 4.1: Absorbed colours and their complementary colours in the visible region
Colour observed
Colour absorbed (complementary colour) Absorbed wavelength (nm)
Red Green 720
Red-orange Blue-green 680
Orange Blue 610
Yellow Indigo 580
Yellow-green Violet 560
Green Purple 530

37
 Blue-green Red 500
Blue Orange 480
Indigo Yellow 430

1.2 UV-Visible Spectroscopy

The UV-Vis spectrophotometer consists of a light source, a sample compartment, a detector and a
data acquisition computer. The sample compartment is between the light source and the detector.
The spectrophotometer measures the amount of ultraviolet and visible light transmitted by the
sample in the sample compartment. UV-Vis is typically used for liquid samples contained in a
transparent “cell” or “cuvette”.

The absorbance, A, of a sample is defined according to the relationship shown in equation (1). Note
that this is a logarithmic relationship!
𝐼
𝐴 = −𝑙𝑜𝑔 𝐼 (1)
0

Here, I0 is the intensity of the light incident on the sample, and I is the intensity of the transmitted
light.

According to the Beer-Lambert Law (2) absorbance of a sample (A) will be proportional to the number
of absorbing molecules (the molar concentration, c) in the spectrophotometer light beam (in the
sample cell). It is necessary to correct the absorbance value as well as other operational factors if
the spectra of different compounds are to be compared in a meaningful way. The corrected
absorption value is called “molar absorptivity”, and is particularly useful when comparing the spectra
of different compounds and determining the relative strength of light absorbing function.

A=cl (2)

Here A = absorbance,  = molar absorptivity, l = length of the cell in cm and c = sample concentration
in moles per litre (mol L-1). The length of the cuvettes used in this lab is 1 cm. As there is a linear
relationship between absorbance and concentration, calibration curves can be made allowing the
determination of the concentration in unknown samples based on their recorded absorbance.

2. The Experiment

This report will be completed in groups of 3-4. One report will be submitted per group. Ensure all
points are covered (see Section 3.1 for the report structure), all observations are included, and all
graphs and tables are labeled. Hand-written graphs and spectra can be scanned or a photo taken
and pasted to the appendix of the report.

This investigation will consist of both qualitative and quantitative analysis. You will be provided with
the specimens from the contaminated lakes and a number of known transition metal standards.
Initially, you will be required to determine the potential contaminants of the water samples. Having

38
determined the identity of the contaminating species you will then use the provided stock solutions
to determine the concentration of each contaminant in the samples.

2.1 Use of the UV-Vis Spectrophotometer

i. Fill your cuvettes to ¾ capacity with the solution to be measured

ii. Wipe the outside of the cuvette with a lint-free paper towel before placing inside the
spectrophotometer

iii. Use a cuvette of your solvent (in this case distilled water) to zero or provide a baseline for
the instrument

iv. Use the Scan program to record the absorbance spectrum for your solution

v. Use the Concentration program to record the absorbance of your solutions at a particular
wavelength and plot a calibration curve

vi. Print out any absorbance spectra; record any data generated from taking absorbance
measurements.

You may be required to dilute your solutions! When the absorbance is greater than 1, >
90% of the incident light is absorbed by the sample. This doesn’t leave much light to
detect and the sensitivity of the instrument is very low causing errors and non-linearities
between the ‘apparent’ absorption and concentration. What might happen when the
absorbance is very low, less than 0.1, to the accuracy of your measurements?

2.2 Qualitative determination

How will you determine the identity of the contaminants in your samples? In your groups of 3 – 4
students, take down some of your initial observations, of both your sample solutions and your
standard solutions. What do you notice? Are there any initial tests you could perform to deduce or
exclude the potential components? How will you conclusively determine the identity of the
contaminants in your sample?

The absorbance spectra for transition metals can be quite distinctive!

Come back to your group and discuss with your peers your observations and ideas for qualitative
testing. When given the ok by your demonstrator, perform any tests required to determine the identity
of the metal contaminants in your water samples. Remember to record all results and observations
in your laboratory book. Don’t forget to label any tables and/or graphs produced!

39
2.3 Quantitative determination

Now that you know what is in your samples, how will you determine how much there is? In your
groups of 3 – 4 discuss how you can quantitatively determine the concentration of the contaminants
within your samples. Write down your method/s for your quantitative analysis. Be sure to include any
dilutions you need to perform, and how you will perform them. Include any glassware or
instrumentation you will use. Some points to remember/consider:

 The known transition metal standards you were provided with have their concentrations
written on the reagent bottles, or can be provided by the lab staff
 When constructing a calibration curve, your unknown should fall in the middle of the curve
(i.e. there should be at least one standard measurement below and above your sample)
 Each calibration curve should have at least 3 points of reference, in addition to a blank
measurement
 Absorbance measurements should always be less than 1! (Why?)
 How will you determine the wavelength at which measurements for your respective
standards and samples should be determined?
 You have been provided with 25 mL volumetric flasks. Use them! (in preference to 100 mL
flasks). This exercise centres on an environmental issue, and where possible we also try
and minimise our environmental impact here in the lab. If you can minimise the waste
produced – do it!

When your demonstrator has approved your method/s, complete your quantitative analysis of the
water samples from the lake.

3. Report

Use your experimental results to plot your calibration curves, determine the concentration of the
contaminants within your water samples, and finalise your reports. Remember to take any dilution
factors into account when performing your calculations, and to fully label any graphs and/or tables
you produce!

Be sure to attach all results (observations/absorbance spectra/calibration curves etc.) so that they
can be easily referred to by our research group here at Monash.

3.1 Report Structure for Exercise 4

Write up and submit your report as a group, using the following report structure.

1. OBJECTIVE: What is the purpose of undertaking this investigation and completing this report?

2. QUALITATIVE ANALYSIS

2.1 Initial Observations

Report the sample number and observations for each sample.

Report the concentration and observations for each standard solution.

2.2 Method Detail the procedure/s you used to qualitatively determine the contaminant/s within your
samples. Did you have to perform any dilutions?
40
2.3 Results Record all results for the qualitative analysis. Be sure to include details such as the
wavelengths of maximum absorbance (λ max) determined for each solution. If applicable, label and
attach any extra sheets to the end of the report.

2.4 Qualitative Analysis – Conclusions What conclusions did you draw from the qualitative
analysis of you samples? How many components were present in each of your samples? What was
the identity of the contaminant/s within the samples? How do you justify your conclusions?

3. QUANTITATIVE ANALYSIS

3.1 Method Detail the procedure/s you used to quantitatively determine the concentrations of
contaminant/s within your samples. Ensure you include any dilutions you may have had to perform,
both on your samples and on the standard solutions. Include any wavelengths you used in the
construction of calibration curves.

3.2 Calculations and Results Tabulate your data and report all results for the quantitative analysis.

4. DISCUSSION (Max. 500 words) Discuss the results you obtained for the water samples you
analysed. Include any sources of error you may have encountered. Consider the environmental
impact of the types and concentrations of the metals you have discovered to be present in the lake
samples. How would they affect the local fauna and flora? Do some research to find out any extra
information regarding these contaminants (don’t forget to reference your sources though- and don’t
copy information word-for-word; that’s plagiarism!).

4.1 Question

In the CHM1051 workshops, we discussed the interconversion between wavelength, frequency and
energy. Use the lambda max values from your four UV-VIS spectra to determine the energy of the
electronic transitions measured for each metal-containing solution.

5. CONCLUSION Finish your report with a short statement commenting on what you achieved, and
what your final numerical result/s were.

6. REFERENCES (If applicable).

7. APPENDIX Attach all graphs, laboratory notes and calculations as part of the appendix. Ensure
your laboratory notes have been signed, and follow the requirements as listed on page 7. Also, make
sure that all pages you submit are labelled!

Complete your laboratory report as a group, and submit it online, via Moodle. Ensure you have
recorded all observations, completed all sections and calculations, and uploaded your laboratory
notes to Moodle.

Your online report must be finalised within 7 days of the completion of your class.

41
 Ex. 5: Equivalence point and pKa

Skills Exercise 5: Equivalence Points and pKas via Experimental Means

Learning Outcomes
1. Construct and interpret an acid-base titration curve.
2. Experiment with a standard pH meter and acid/base indicators.
3. Distinguish weak and strong acids/bases, and mono- and polyprotic acids/bases
4. Distinguish between the end point and the equivalence point of an acid/base titration

Personal safety: It is essential that safety glasses and laboratory coat are worn at all
times in the laboratory.. Wash hands before leaving the building. Despite only dilute
solutions of strong acid and strong bases being used, both are still quite corrosive and
particular caution should be taken during handling.
Hazard Identification and Risk Assessment
Identify the Hazard Determine the Risk Control the Risk Disposal of waste
(the potential to do harm) (the probability that (preventing an incident)
harm may result)
Hydrochloric Acid (0.1 M) Solution is dilute. Handle with care. Wash Neutralise and dispose
CORROSIVE Low risk. skin immediately under of down the sink with
Causes burns, damaging to water if spill occurs. copious amounts of
eyes. water.
Sodium Hydroxide (0.1 M) Solution is dilute. Handle with care. Wash Neutralise and dispose
CORROSIVE, Causes Low risk. skin immediately under of down the sink with
burns, damaging to eyes. water if spill occurs. copious amounts of
water.
Sodium Carbonate Solution is dilute. Wash skin immediately Neutralise and dispose
(Na2CO3) (0.1 M) Low risk. under water if spill occurs. of down the sink with
Harmful if swallowed copious amounts of
Irritating to eyes and skin water.
General glassware Medium Handle with care, dispose Labelled broken glass
Cuts of chipped/ cracked bin
glassware, collect broken
glass using dustpan and
brush. If cut occurs, see
your demonstrator, seek
first aid.
Reading: Blackman, Chemistry. John Wiley & Sons 2016, Chapter 9 and 11 and Weeks 9 &
10 Workbooks.

1. Introduction

Acids and bases are central to the science and chemistry of water. They are also used extensively
throughout industry and are important in nature and food science. The Brønsted-Lowry definition of
acids and bases considers an acid-base reaction as a proton transfer from an acid to a base. Thus,
within the Brønsted-Lowry definition, an acid is a proton donor and a base is a proton acceptor. In
this practical exercise we investigate some of the properties of acids and bases using acid-base
titrations.

42
 Ex. 5: Equivalence point and pKa

1.1 The definition of pH

The acidity of an aqueous solution is related to the “activity” of hydronium ions in the solution (aH2O),
however in the laboratory we use the more easily measured "concentration", [H 3O+], as an
approximation for the activity. Because of the wide range of values of [H3O+] commonly encountered,
(1 to 10-14 M), the acidity is usually measured using a log scale, this is the pH scale. The pH of a
solution is calculated by:

pH  -log10[H3O+] (1)

Exact calculations use activities instead of concentrations, but not always practical. Water always
participates in a self-dissociation equilibrium:

H2O + H2O ⇌ H3O+ + OH- (2)

described by the well-known self-dissociation equilibrium constant:

[H3O+][OH-]  Kw = 1 x 10-14 at 25oC. (3)

In a neutral aqueous solution [H3O+] = [OH–] and at 25oC the pH of a neutral solution is 7.00. Acidic
solutions have lower values of pH (high values of [H 3O+]), whereas basic solutions have higher
values of pH (low values of [H3O+]).

1.2 Strong Acids and Bases

Acids that strongly dissociate completely into H3O+ ions when dissolved in water are strong acids.
Hydrochloric acid is a strong acid. This can be expressed as a general strong acid equation:

HA + H2O  H3O+ + A- (4)

Note the use of the one way arrow implying that the reaction goes all the way and is not reversible.
+ –
An example of a strong acid would be hydrochloric acid: HCl(aq) + H2O(l)  H3O (aq) + Cl (aq)

A strong base is one that completely dissociates in water. The generalised equation for a strong
base is:

B(aq) + H2O(l)  BH+(aq) + OH-(aq) (5)

+ –
Sodium hydroxide is an example of a strong base: NaOH(aq)  Na (aq) + OH (aq)

Other examples of strong acids include nitric acid (HNO 3), and sulfuric acid (H2SO4) (in its first
dissociation). Strong base include potassium hydroxide (KOH).

1.3 Weak Acids and Bases

A weak acid is one that coexists at equilibrium with its corresponding (or “conjugate”) base, as for
example, with acetic acid (HOAc):

HOAc(aq) + H2O(l) ⇌ OAc–(aq) + H3O+(aq) (6)

43
 Ex. 5: Equivalence point and pKa

To express weak acids and bases we use a reversible arrow as shown above in Equation 6. The
acidity constant, Ka (an equilibrium constant for an acid), can be determined from the concentrations
of acid and base in solution using the following equation:

+ -
Ka = [H3O ][OAc ]
[HOAc] (7)

The “p” notation (as used in pH) is based on the definition, pX = – log
[X], where p is an abbreviation for power. Using this definition, we
can write:

pKa = -log10 Ka (8)

If we combine these two equations, pH can be determined by any

concentration of the weak acid, HA, with its conjugate base, A –

[A-]
pH = pKa + log10
[HA] (9)
Figure 5.1: Table
A weak base is correspondingly a base that does not fully dissociate. vinegar or acetic acid, a
weak base ready for use.
B(aq) + H2O(l) ⇌ BH+(aq) + OH-(aq) (10)

Basicity constants, Kb, are also able to be defined.

1.4 Measuring pH with a pH Meter.

pH can be measured using a glass electrode and a

suitable reference electrode. Frequently, the glass
electrode and the reference electrode are housed in
the same casing as a combination electrode (see
Figure 5.3). The electrical
potential of the glass
electrode is sensitive to
changes in pH, whilst the
reference electrode
remains at a fixed
potential. The two
electrodes, together with the solution between them form an electrical cell,
and a voltmeter measures the difference between the two electrodes and
can be calibrated to display the result in pH units (see Figure 5.2). Your
demonstrator will explain the use of the pH meter. Note: The combination
pH electrode is fragile, so raise and lower it with care and do not use it to
stir the solution. The electrode must not be allowed to dry out, so keep it
immersed in distilled water between readings.

Figure 5.2 (Above right): The pH meter – your demonstrator will explain how to use it.
Figure 5.3 (Above left): Combination pH electrode

44
 Ex. 5: Equivalence point and pKa

The readings of a pH meter are only valid if the meter has been calibrated with a buffer of known pH
appropriate to the range of measurement. Additionally, temperature has a significant effect on pH
measurements, so temperature should always be reported along with pH.

1.5 Measuring pH with Indicators.

Indicators have been developed to find ‘end-points’ that correspond to equivalence points more or
less accurately. The end-point of a reactions is the actual point at which an indicator changes and
the volume of reactant added is recorded (thus endpoint = equivalence point + indicator error).

Today we will use both a pH meter and a number of indicators to follow an acid-base titration. We
will place an acid-filled burette over a beaker containing the pH electrode and a solution of base. As
acid is titrated into the base, the pH decreases, slowly at first and then more quickly until after the
equivalence point when the rate of decrease begins to slow down again. The equivalence point is
the number of moles of standard is equivalent (in stoichiometric ratio) to the number of moles of
unknown. The equivalence point can be determined from a graph of pH against volume of acid
added by finding the point of maximum slope, which is the point at which the curve changes from
convex to concave (see Figure 5.4). The end-point can be determined via the colour change of the
indicator, and the equivalence point and end-point can thus be compared.

Figure 5.4: The titration curve above represents the titration of a weak acid with a strong base.
Notice the following points: (a) initially, pH ~ 3, (b) the equivalence point is considered to be the point
where the slope of the curve is greatest, (c) the volume corresponding to half of the volume added
at the equivalence indicates a point on the curve where pH = pK a.

45
 Ex. 5: Equivalence point and pKa

1.5 Bulb pipette usage

The pipette is a precision instrument for convenient delivery of an accurately determined volume of
liquid (an aliquot). You should never hold a pipette by the glass bulb because the heat of your hand
can cause a significant change in the volume it will deliver. Always hold it by the upper
stem.

Rinse the pipette twice with the solution to be used in the measurements, then draw the
liquid by suction to just above the mark and adjust until the bottom of the meniscus just
touches the mark. Using the first finger to seal the top allows greater flexibility than
using the thumb and is especially helpful when using graduated pipettes. Slowly rotate
the pipette to allow accurate control of the level.

The standard procedure for draining a pipette is to hold it vertical with its tip in contact
with the side of the vessel for 15 seconds after the continuous discharge has ceased
(see Figure 5.5). At the end of 15 seconds remove the pipette from the vessel.
Disregard any liquid remaining in the pipette tip. Always use a pipette filler!

Figure 5.5:
2. Experimental Procedure Draining a pipette
into a conical flask.
Note: Graph paper is available from your demonstrator. When completed,
these graphs should be signed off by your demonstrator, and pasted into your laboratory
book. When performing each experiment, plot at least 20 data points per graph. When
plotting each graph, remember to include:
 Appropriate title
 Axis labels (including units)
 Temperature at which the titration was performed
 Equivalence point/s and pKas (where appropriate)

2.1 Calibration of pH meter

Calibrate your pH meter according to the SOP (standard operating procedure)
provided.

2.2 Titration of ~0.l M NaOH with ~0.l M HCl

i. Pipette 10 mL of NaOH into a 100 mL beaker and add 20 mL (measuring cylinder) of distilled
water so that the electrodes are immersed. Add 2-3 drops of Bromothymol Blue indicator.
Measure the pH and the temperature.
ii. Fill the burette with 0.1 M HCl (record the exact concentration of the acid) and take an initial
reading to ±0.05 mL (there is no need to start exactly at 0.00).
iii. Arrange the burette, beaker, electrodes and pH meter so that titration can be conducted while
the electrodes remain in place (see Figure 5.6).
iv. Add approximately 1 mL of acid from the burette. (Record the burette readings to ±0.05 mL).
Swirl the solution thoroughly and measure the pH. Do not remove the electrodes or STIR
with them!

46
 Ex. 5: Equivalence point and pKa

v. Plot the amount of acid added against the resulting pH. The reading should be plotted as
soon as it is measured. The graph scales should be pH 0 - 14 (y-axis), volume of acid 0 - 20
mL (x-axis).
vi. Repeat steps iv and v. As the pH begins to fall more steeply, the volume of acid per addition
should be reduced to about 0.1 mL. If you overshoot at this stage, repeat the titration. You
do not need to add small portions slowly from the burette right from the start. Instead add an
amount just less than the amount required to overshoot, and then add small amounts to
precisely detect the end-point. Note any colour changes observed.

Figure 5.6: burette set up with pH meter.

vii. Once you are well past the equivalence point (steepest point on the graph), use 1 mL aliquots
again.
viii. Mark the equivalence point on your graph. Read the pH of the solution at the equivalence
point (taken at the mid-point of the steepest part of the curve). Record the volume of HCl
required for equivalence.
ix. Using the accurate concentration of HCl listed on the bottle, calculate the concentration of
NaOH used in the experiment.

2.3 Titration of ~0.1 M Na2CO3 with ~0.1 M HCl

The procedure is similar to that of the titration of NaOH with HCl. However, there are two equivalence
points, one after addition of approximately 10 mL of HCl, the other after addition of about 20 mL of
HCl. A total of 25 mL of HCl should be added altogether.
i. Make up a standard solution of ~0.1 M sodium carbonate. To do this, weigh out 0.53 g of
Na2CO3(s), and make up to 50 mL (in a volumetric flask) with water. Refer to Exercise 2 for
notes on making up a standard solution using a powdered reagent and a volumetric flask.

47
 Ex. 5: Equivalence point and pKa

ii. Pipette 10 mL of sodium carbonate solution into a clean beaker. Add 20 mL (measuring
cylinder) of distilled water so that the electrodes are immersed. Add 2-3 drops of
Phenolphthalein indicator. Measure the pH and the temperature.

iii. Titrate by addition of HCl from the burette (in a similar manner to Section 2.2). Remember
there are two equivalence points in this titration. Plot the titration curve as you proceed.
The graph scales should be pH 0 - 14 (y-axis), volume of acid 0 - 30 mL (x-axis).

iv. When you have reached the first end point, add 2-3 drops of Methyl orange indicator to your
beaker.

v. Mark the two equivalence points on your graph.

vi. Use the graph to determine the initial pH (solution of Na 2CO3) and the pH of a solution of
sodium hydrogen carbonate (NaHCO 3) at the first equivalence point.

vii. Use the graph to determine the pH of a saturated solution of carbon dioxide (the 2nd
equivalence the point).

viii. The first part of the titration can be described approximately by Equation 11 and the graph
follows Equation 12 where pKa2= -log10 (acid dissociation constant of HCO3-).

CO32–(aq) + H3O+(aq)  HCO3– (aq) + H2O(l) (11)

[CO32-]
pH = pKa + log10 [HCO3-] (12)

ix. Find the value of pH at the point where [HCO 3-] = [CO32-], and hence determine an
approximate value of pKa for the hydrogen carbonate ion (pKa1 for carbonic acid.).

x. Between the first and second equivalence points the reaction can be described approximately
by Equation 13 and the graph follows Equation 14 where

xi. pKa1 = -log10Ka1 (acid dissociation constant of H2CO3).

HCO3– + H3O+  H2CO3 + H2O (13)

[HCO3-]
pH = pKa + log10
[H2CO3] (14)

xii. Find the value of pH at the second halfway point (where [H 2CO3] = [HCO3-]) and hence
determine an approximate value of pKa for carbonic acid (pKa1).

xiii. Compare the calculated mean of pKa1 and pKa2 with the observed pH at the first equivalence
point.

Clean-up: Thoroughly clean all your glassware with warm water. Make sure the pH electrode is
thoroughly rinsed and stored in a container of fresh deionised water.
Report: Complete your laboratory report online, via Moodle. Ensure you have performed all
necessary calculations, completed all sections and uploaded your graphs and laboratory notes to
Moodle. Your online report must be finalised within 7 days of the completion of your class.

48
Inquiry Exercise 6: Calorimetric Analysis of Baking Powder
Learning Outcomes
1. Distinguish between exothermic and endothermic reactions.
2. Use calorimetry to determine the enthalpy of a chemical reaction.
3. Devise a method using calorimetry to analyse a powder with an unknown composition.
4. Manipulate data and determine unknown compositions using a calibration curve.

The IDEA Experiments you will come across in units such as CHM1051, BIO1011 and PHS1011
are a little different to some of the lab exercises you will have already done in your Science
degree. These exercises will not come with a procedure mapped out for you, which means that the
whole procedure is NOT written in the lab manual. For some parts of this exercise, you will have to
design and perform your own experiment.

You will be working in a group of 4 students. You need to assign roles within your group and
delegate the work that has to be done over the four hours.

Do not forget that at the end of the four hour session, you need to have finalised all experimental
work, plotted all graphs and planned your discussion section with your group.

"IDEA" stands for Inquiry-Design-Explore-Answer, and that’s exactly what working scientists do in
their professional life.
5. Inquiry: A sound scientific approach to answering questions and solving problems always
commences with the process of asking deep questions. What is the quickest way to perform this
experiment? The most ethical? The least
expensive? The ‘greenest’? Are you able to
foresee roadblocks along the way?
6. Design: Once you have considered the
limitations, challenges and practicalities of the
experiment, you can start to design your
experiment. Weigh up what expertise and
techniques you have at your disposal. Ask
questions of each other, your demonstrator,
and the literature, and come up with a flow
chart for how the experiment will proceed.
7. Explore: When you are ready to commence,
delegate different jobs amongst your team,
and start to gather data! You may find along
the way that your design needs to be changed!
8. Answer: Once you have gathered the best
data you can, see if you are able to form some
conclusions. Discuss the results of your
experiments amongst yourselves and determine whether the original problem has been solved.
 Ex. 6: Baking powder analysis

Safety comments: It is essential that safety glasses and laboratory coat are worn at all times in
the laboratory. Glasses to be put on at entrance (sliding door) and taken off at entrance as you are
leaving. Wash hands before leaving the building.
Hazard Identification and Risk Assessment
Identify the Hazard Determine Control the Risk Disposal of waste
(the potential to do the Risk (preventing an incident)
harm)
Citric Acid Low Wash with water if in contact with the skin Down the sink with
Irritating to eyes, skin plenty of water
Sodium Carbonate Low Wash skin immediately under water if spill Down the sink with
May cause eye burns occurs. plenty of water
Harmful if swallowed.
Irritating to skin
General glassware Medium Handle with care, dispose of chipped Place broken glass in
Cuts /cracked glassware, collect broken glass the labelled broken
using dustpan & brush. If cut occurs, see glass bin
your demonstrator, seek first aid
Reading: Blackman et al., Chemistry. (2019), Chapter 8; CHM1051 Workbooks Week 7 & 8.

1. Introduction

Baking powder or baking soda are common ingredients used for cakes
and other baked goods. Baking soda is pure sodium bicarbonate
(NaHCO3) whereas baking powder consists of baking soda and one or
more acid salts. These salts are usually classified into two categories:
the low-temperature acid salts (see Figure 6.1) such as potassium
tartrate or calcium dihydrogen phosphate and the high-temperature acid
salts such as sodium aluminium sulfate or sodium aluminium
phosphate. If the baking soda is used, then an acidic ingredient, such
as lemon juice (which contains citric acid) or vinegar (which contains
acetic acid) must be added to the batter so that a chemical reaction
occurs.

In this practical a mixture of Citric Acid (CA) and Figure 6.1: Chemical
structure of molecules.
Sodium Bicarbonate (SB) will be used. Citric
Acid is a triacid (pKa1 = 3.1, pKa2 = 4.7 and pKa3 = 6.4). Sodium
bicarbonate (NaHCO3) is an amphoteric species: it can act as an acid and
as a base (pKa (HCO3-/CO32-) = 10.4 and pKa (H2CO3/HCO3-) = 6.4).

Your goal is to determine the exact composition of Monash University’s new

Baking Powder.

2. Calorimetry Background

Calorimetry is used to quantify the heat released or absorbed by a chemical

reaction or a physical process, for example dissolution or phase transition.
Chemical reactions that raise the temperature (release thermal energy) are called exothermic
reactions. Chemical reactions that lower the temperature (absorb thermal energy) are called

50
 Ex. 6: Baking powder analysis

endothermic reactions. Change in temperature due to chemical reactions is measured as enthalpy

(H). The enthalpy H of a chemical species describes its internal energy.

If a reaction is exothermic, then the chemical species lose internal energy to its surroundings (raising
the temperature), and so H is negative. Conversely, if a reaction is endothermic, the chemical
species absorb energy from its surroundings (lowering the temperature), and so H is positive. We
will be investigating the thermodynamics of the chemical reaction between citric acid and sodium
bicarbonate.

The change in enthalpy (H) of a chemical reaction is related to the change in temperature (T):

H = - m C T
where m is the total mass of solution (g) and C is the heat capacity (J K-1 g-1).

Recording the evolution of the temperature of the system gives information about the change in
enthalpy of the system.

3. The Experiment

After instructions from your demonstrator, record all observations and determine the chemical
reaction that occurs. Be sure to explain the observations in your laboratory notebook. As you conduct
your experiments, some useful things to consider about might be:

 What is the balanced chemical equation?

 What type of reaction is it?
 Can you explain your observations based on the chemical reaction?
 Is the reaction exothermic or endothermic?
 What would the energy diagram (to illustrate the relative H) for this reaction look like?
 How will you measure ΔT and why will you measure it like that?
 How much solid will you be using for each experiment?
 What mixture compositions will you use, and why?
 What calculations will you need to perform?
 What method will you use to determine the composition of Monash University’s Baking Powder?
What glassware and equipment will you use?
 What composition of the baking powder would you suggest that Monash University produces to
give rise to the best cake (if we were to assume that the more gas produced, the more the cake
will rise)? Can you explain your answer using experimental results and the chemical equation?
 Is the the dissolution of solid citric acid and dissolution of solid sodium bicarbonate in water
exothermic or endothermic? What is the ΔT of these two reactions?
 Using your experimental results, can you calculate (or perhaps approximate) the change in
enthalpy of the chemical reaction?

51
 Ex. 6: Baking powder analysis

4. Calibration Curve

In order to determine the composition of a mixture, scientists perform calibration curves using
mixtures of known compositions. They then measure and plot the change in the “significant
parameter” (y axis) versus the composition (x axis) as is done in Figure 6.2. The choice of the
experimental data is very important as the scientist has to cover the whole range of expected
compositions. Finally, the scientists perform the same experiment with the mixture of unknown
composition and using the calibration curve they deduce the composition of the mixture.

In the following example, the change in temperature ( T) is plotted against the mass percentage of
solid A. Six mixtures are prepared within the range 0-50%. The unknown mixture has a T of 5.0°C.
Using the line of best fit (line that matches most of the experimental data – see Figure 6.2), the mass
percentage of solid A can be deduced and found as 25%.

Data Points

Mass %
of solid A

Figure 6.2: Example of a calibration curve.

In your groups of 3-4, consider the following:

 You will be performing calorimetry experiments; therefore, what will the ‘significant parameter’
be?
 What will your ‘significant parameter’ be plotted against when you draw your calibration
curve/s? You will be measuring mixtures of sodium bicarbonate and citric acid. How will these
mixtures be expressed on your graph/s and in your table? It can be useful to express (and
graph) the compositions of these mixtures in different ways. Why? What are some different
ways they could be expressed? Why might this be useful?
 In order to plot a calibration curve, one parameter is varied whilst keeping all other
parameters constant. Why is this? Why is it not useful to vary more than one parameter at a
time?
 For this calibration curve, which parameter will you be varying? And by extension, which
parameters must therefore be kept constant? Refer to 4.1: Experimental procedure, below.
 You will be dissolving your solid in 30mL of water. How much solid will you be using?

Come back to your group of 16 and discuss your answers with your peers. When you have the ok
from your demonstrator, begin your experimental analysis.

52
 Ex. 6: Baking powder analysis

Table 6.1: Calorimetry data table. Copy this table into your laboratory notebook, to make it easier to
record your data for the calibration curve.

sodium total total

citric acid (CA) _____ _____ _____
bicarbonate (SB) mass moles
mTOT (g) nTOT _____ _____ _____ ΔT (°C)
m (g) n (mol) m (g) n (mol)
(mol)

4.1 Experimental Procedure

Remembering the video:

i. Nest two foam cups inside each other and place in 400 mL
beaker.

ii. Add 30 mL of water into the cup and place a lid on it. The
water should be brought to room temperature prior to
beginning the experiment. Why?

iii. Clean, dry and label 3 weighing bottles (Citric Acid,

NaHCO3, Mixture).

iv. Weigh out in the first container labelled “Citric acid”

roughly the desired amount of citric acid. Record the exact
mass.

v. Weigh out in the second container labelled “NaHCO 3”

roughly the desired amount of sodium bicarbonate.
Record the exact mass.
Figure 6.3: Experimental setup
vi. Transfer both powders into the third container labelled
“mixture”. Be sure to transfer all powder (you can tap the
vial to avoid powder sticking at the bottom). Reweigh empty containers.

53
 Ex. 6: Baking powder analysis

vii. Insert the Pasco temperature sensor through a small hole in the lid of the cup. Do not touch
this when running an experiment. Why?

viii. When everything is ready, click on the “Record” button on the program to begin data
recording. The temperature should be constant. If not, click on the “Stop” button, wait for a
minute and click again on the “Start” button.

ix. After about 15 seconds have elapsed, lift the lid of the cup and quickly add the mixture to the
water. Ensure the lid is adequately put back on the cup (avoid gaps). Swirl the beaker for 10-
15 seconds. Make sure the temperature sensor is on the edge of the cup while stirring so the
temperature can be recorded at any time.

x. After overall 30 seconds have elapsed, leave the cup on the bench with the temperature
sensor in it. Let the computer record the temperature for 5 minutes for the first experiment
(for your subsequent experiments you can stop the experiment when you want).

xi. Click on the “Stop” button to end data recording.

xii. Dispose of the reaction products in the sink. Rinse the cup with distilled water for use in the
next experiment.
xiii. Repeat from step (ii) with different compositions (at least 8 compositions) of citric acid and
sodium bicarbonate.

xiv. On the graph paper provided, plot graphs of the ‘significant parameter’ (y-axis) versus the
different mixture compositions (however you have chosen to express them) (x-axis).
Determine the line of best fit for all graphs.

5. Determination of the Composition of the Monash Baking Powder

In your laboratory book, provide the method you plan to perform in order to determine the
composition of the Monash Baking Powder. The demonstrator must check this before you can
go on. They will provide you with feedback to help improve your experiment design if needed.

Then perform the experiment and determine the composition of the Monash Baking Powder. If
necessary, you can perform further tests in order to get the composition. You will have to explain
these tests in your report. Once you have recorded all the information needed in your
laboratory book, go to ‘Experiment’ on the program and select ‘Delete All Data Runs’
from the list.

6. Report
Complete your laboratory report online, via Moodle. Ensure you have performed all necessary
calculations, completed all sections, and uploaded your laboratory notes to Moodle.

Your online report must be finalised within 7 days of the completion of your class.

54
 Ex. 6: Baking powder analysis

Inquiry Exercise 7: Rate Law Determination-Timing the Iodine Clock

Learning Outcomes
1. Explore the idea of “rate order”.
2. Design a simple experiment to determine the overall rate order of a chemical
reaction.
3. Understand the effects of experimental conditions on rate, such as concentration and
temperature.
4. Work in teams, delegate tasks, and optimise your time management and efficiency.

The IDEA Experiments you will come across in units such as CHM1051, BIO1011 and PHS1011
are a little different to some of the lab exercises you will have already done in your Science
degree. These exercises will not come with a procedure mapped out for you, which means that the
whole procedure is NOT written in the lab manual. For some parts of this exercise, you will have to
design and perform your own experiment.

You will be working in a group of 4 students. You need to assign roles within your group and
delegate the work that has to be done over the four hours.

Do not forget that at the end of the four hour session, you need to have finalised all experimental
work, plotted all graphs and planned your discussion section with your group.

"IDEA" stands for Inquiry-Design-Explore-Answer, and that’s exactly what working scientists do in
their professional life.
1. Inquiry: A sound scientific approach to
answering questions and solving problems
always commences with the process of
asking deep questions. What is the quickest
way to perform this experiment? The most
ethical? The least expensive? The
‘greenest’? Are you able to foresee
roadblocks along the way?
2. Design: Once you have considered the
limitations, challenges and practicalities of the
experiment, you can start to design your
experiment. Weigh up what expertise and
techniques you have at your disposal. Ask
questions of each other, your demonstrator, and
the literature, and come up with a flow chart for
how the experiment will proceed.
3. Explore: When you are ready to commence,
delegate different jobs amongst your team, and
start to gather data! You may find along the way that your design needs to be changed!

55
 Ex. 6: Baking powder analysis

4. Answer: Once you have gathered the best data you can, see if you are able to form some
conclusions. Discuss the results of your experiments amongst yourselves and determine
whether the original problem has been solved.

Personal safety: It is essential that safety glasses and laboratory coat are worn at all times in the
laboratory. Glasses to be put on at entrance (sliding door) and taken off at entrance as you are
leaving. Wash hands before leaving the building.
Hazard Identification and Risk Assessment
Identify the Hazard Determine the Risk Control the Risk Disposal of waste
(the potential to do harm) (the probability that (preventing an incident)
harm may result)
Sulfuric acid (0. 36M) Solution is dilute. Handle with care. Wash skin Corrosives residue
CORROSIVE, causes Low risk. immediately under water if spill carboy in fume
burns, damaging to eyes occurs. cupboard
Potassium Iodide (0.025 Solution is dilute. Handle with care. Rinse quickly Corrosives residue
M) Low risk with water if spilt on skin to carboy in fume
Irritating to eyes Will still stain skin at avoid staining. cupboard
Can stain skin this concentration
Thiosulfate (0.0025 M) Low Avoid contact with skin, wash Corrosives residue
Irritating to eyes, & skin immediately with water if spill carboy in fume
occurs. cupboard
Hydrogen Peroxide (0.8 Low Avoid contact with skin as it Corrosives residue
M) can have a bleaching effect, carboy in fume
Harmful if swallowed wash immediately with water if cupboard
Irritating to eyes and skin spill occurs.
General glassware Medium Handle with care, dispose of Labelled broken
Cuts chipped/ cracked glassware, glass bin
collect broken glass using
dustpan and brush. If cut
occurs, see your demonstrator,
seek first aid.
Reading: Blackman et al., Chemistry. (2019), Chapter 15 and CHM1051 Workbooks Weeks 11
& 12.

1. Introduction

Kinetics is the study of how quickly chemical reactions occur. Some chemical reactions occur very
quickly – for example explosions, while others proceed very slowly. Understanding the kinetics of a
reaction gives information about the mechanism of that reaction.

1.1 Determining the Rate Order:

The rate of a reaction is the increase in concentration of products over time, at a particular instant in
time. Alternatively, it can be defined as the decrease in concentration of reactants over a period of
time, at a particular instant in time.

During today’s experiment, the aim is to determine the rate order of the chemical reaction. That is,
how the rate of the reaction changes as the concentration of reactants changes. This is not covered
in lectures until week 11, so today we will keep this pretty simple. More reading can be found in your
textbook, Blackman, 2016 p. 640-648 and Weeks 11 & 12 Workbooks.

56
 Ex. 6: Baking powder analysis

 Zero Order Kinetics occurs when the concentration of a reagent [A] is increased, and the rate
of the reaction doesn’t change!  Rate ~ [A]0

 First Order Kinetics occurs when the rate of the reaction increases proportionally with
concentration.  Rate ~ [A]1. That is, if the concentration of one reagent is doubled, the rate of
the reaction doubles. If the concentration is tripled, the rate triples, and so on.

 Second Order Kinetics occurs when the rate of the reaction increases proportionally with
concentration.  Rate ~ [A]2. That is, if the concentration of one reagent is doubled, the rate of
the reaction quadruples (2 2). If the concentration is tripled, the rate increases by a factor of nine
(32), and so on.

A general expression for the rate of reaction is written:

𝑅𝑎𝑡𝑒 = 𝑘[𝐴]𝑥 [𝐵]𝑦

In this general rate equation, A and B might be reactants (for example), while x and y are the order
of the reaction with respect to reactant A and B respectively. The constant, k, is known as the rate
constant.

1.2 The Iodine Clock Reaction

The following chemical equation describes the so-called “Iodine Clock Reaction”.

H2O2(aq) + 2 I-(aq) + 2H3O+(aq)  I2(aq) + 4 H2O(l) (1)

Practically, hydrogen peroxide is added to a mixture of

potassium iodide and sulfuric acid. This process
occurs faster or slower depending on the
concentration of each reactant. Using the rate of
formation of iodine you will determine the rate law of
the reaction.

1.3 Measuring the Rate

This is done by means of the well-known reaction Figure 7.1: The iodine clock reaction gives
between iodine (I2) and a (relatively) small amount of a sudden, obvious colour change that can
thiosulfate ion (S2O32-) to form the tetrathionate ion be used to determine the kinetics of the
(S4O62-) (2). reaction.

I2(aq) + 2 S2O32-(aq)  S4O62- (aq) + 2 I-(aq) (2)

When hydrogen peroxide is added to the mixture, the iodine formed by reaction (1) reacts instantly
with thiosulfate by reaction (2), until all the thiosulfate is used up. The ‘excess’ iodine then begins to
accumulate in solution and (in the presence of starch) the colourless solution suddenly turns blue.
(Iodine forms a complex with starch and this complex has a brilliant blue colour). This kind of reaction
is widely known as a 'clock reaction'.

57
 Ex. 6: Baking powder analysis

2. Experimental Procedure

2.1 The Aim: The aim of today’s experiment to determine the rate law for the iodine clock
experiment. Based on the four reagents in this process, the rate law has the general form:

rate = [S2O32-]w[H2O2]x[I–]y[H3O+]z (3)

 You will need to determine w, x, y and z. Note that the success of the experiment depends
on there being a large excess of the reactants H 2O2, I- and H3O+ for reaction (1), relative to
the thiosulfate used for reaction (2).

Some of the questions you should consider might be:

 How does the rate change as [H2O2], [I-], and [H3O+] are increased? Can you test these
simultaneously, or do you have to change only one concentration at a time?
 How does the rate change as [S2O32-] is increased?
 How does the rate change as temperature changes?

2.2 The Demonstration

Your demonstrator is going to show you an example of how this experiment works. Watch closely -
you are going to have to design the rest of this experiment yourself. Here is a basic description of
the procedure your demonstrator is following:
The following materials are added to a 250 mL conical flask, in the order shown:
i. 35 mL 0.36 M H2SO4 (measuring cylinder)
ii. 43 mL distilled water (measuring cylinder)
iii. 10 mL 0.025 M KI (pipette)
iv. 10 mL 0.0025 M thiosulfate (pipette)
v. 1 mL starch solution (measuring cylinder)
At this point, a stop-watch or timer should be ready!
vi. 1 mL of 0.8 M hydrogen peroxide (fumehood using the 2 mL pipette provided).
Time is measured from the moment the peroxide is added, and the mixture is swirled gently 3 or 4
times. The solution is left to stand until a blue colour appears, due to an I3--starch complex. Determine
the time elapsed (in seconds). There are a few important points you should consider.
 Is temperature important? If so, can you measure it?
 When performing the first experiment (initially performed by your demonstrator) you
should completed it yourself at least three times to verify the timing.
 When following the instructions above, what is the total volume of the mixture? Do you
think this is important?

2.3 Inquiry  Design  Explore  Answer

Once your demonstrator has completed the demonstration, you will complete the experiment in your
group. It is time to consider how you might design an experiment to determine the overall rate order
for the experiment.
 In your laboratory book, provide the method you plan to perform in order to determine the
rate law for the iodine clock experiment. The demonstrator must check this before you
can go on. They will provide you with feedback to help improve your experimental
design if needed.

58
 Ex. 6: Baking powder analysis

 Complete this experiment, recording all data in your laboratory notebook. Use Section 3.
‘Hints and Tips’ to guide you.
 The marking scheme can be found on Moodle.
 There is a lot to do, so delegate your jobs accordingly!

59
 Table 7.1: Iodine clock data table. Copy this into your laboratory notebook, and for each row, indicate the reagent you are focusing on for that test.
Time Measured
Volume H2O [H3O+]1 & [I-]1 & [H2O2]1 & [S2O32-]1 & # mol S2O32- # mol I2 reacted Reaction Rate
T °C (s) (Colour
added (cm3) Vol (cm3) Vol (cm3) Vol (cm3) Vol (cm3) reacted in (2) with S2O32- in (2) (I2) (mol/s)
Change)

1
Concentration in the flask, not concentration of the original solution!

60
3. Hints and Tips
3.1 Results
Tabulating your data:
 Copy Table 7.1 into your laboratory notebook to tabulate your data.
 Provide a title for the table
 Complete the first row using the values determined in the pre-lab questions.
 Calculate the # of moles used/produced, based on your 100 mL volume.
 Note the time taken for the colour change to appear.
 Finally, divide the # mol I2 reacted in Eq. (2) by the time, to determine the reaction rate.
 Ensure you reproduce the same clock reaction as your demonstrator for comparison.

Graphing your data:

 For each of the variables you have
investigated, you should produce a graph of
reaction rate vs concentration (or
temperature).
 Each graph will need to be plotted in excel
and uploaded to Moodle.
 Don’t assume there will be a straight line, or
even a gradient! This will depend on whether
you have zero, first or second order kinetics.
 Ensure you use the appropriate scale for each
graph! Figure 7.2: An example of a graph of
reaction rate vs concentration.

Understanding your results:

 Use the appearance of your graphs to determine the rate order with respect to [H 2O2], [I-],
[H3O+] and [S2O32-].
 Therefore, what is the rate law for this reaction?
 How does the rate change with respect to ΔT?

3.2 Group Results:

As a class, plot your results on the graphs that your demonstrator has available. Discuss these
results as a class, and compare them to your group results. How do they compare? If they are
different to your group results, consider why. Does having a larger data set help in the evaluation
and interpretation of the results? Does having multiple people perform the experiment make a
difference? Why/why not?
 Ex. 7: Iodine Clock

3.3 Understanding the Reaction

Below are the reactions performed today:

H2O2(aq) + 2I-(aq) + 2H3O+(aq)  I2(aq) + 4H2O(l) (1)

I2(aq) + 2S2O32-(aq)  S4O62- (aq) + 2I-(aq) (2)

I2(aq) + I-(aq) + Starch (aq)  (I3- -Starch)complex (aq) (3)

During your practical today you are detemining the rate law for Reaction 1. In your group, discuss
the purpose of reactions 2 and 3. With respect to hypothetical scenarios #1 and #2, discuss what
would you observe:
 At the macro level
 At the sub-micro level
Scenario #1: No thiosulfate (S2O32-) is added to the flask
Scenario #2: Neither thiosulfate nor starch is added to the flask

Consider the following:

What is meant by the terms ‘limiting reagent’, and ‘in excess’?

Consider the reaction between carbon, C, and oxygen, O 2, to form carbon dioxide.
C + O2  CO2
We can see that the stoichiometry is a 1:1 ratio for C and O 2.
Now consider what would happen if 3 moles of C was allowed to react with 4 moles of O 2?
 3 moles of C would react with 3 moles of O 2 to form 3 moles of CO2.
 There would also be 1 mole of unreacted O2.
We say that the carbon was the “limiting reagent”, and that oxygen was “in excess”.

As a class, calculate the initial concentrations of reagents present in the flask (ignoring the starch).
Then determine the empicial ratios for each reagent, based on the first reaction as written in your
lab manual.
 Based on what you have calculated, do you think hydrogen peroxide (H2O2) is the limiting
reagent, or in excess? Why?

Now consider the moment when the blue colour change is about to occur (i.e. when there is no
more thiosulfate remaining in solution).
Based on the initial experiment and initial concentrations of reagents, calculate the concentrations
of the reagents present in the flask at the moment just before the blue colour change begins (you
can ignore the starch, and the S4O62- which is formed as the other byproduct in this reaction).
 Does Reaction 1 continue beyond this point? Why or why not?
 Based on what you have calculated, which reagent in Reaction 1 is the limiting reagent?

4. Report
Complete your laboratory report online, via Moodle. Ensure you have performed all necessary
calculations, completed all sections, and uploaded your laboratory notes to Moodle.
Your online report must be finalised within 7 days of the completion of your class.
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Poster Exercise 8: The TEK Experiments
Learning Outcomes
1. Explore a number of interesting but simple chemical experiments.
2. Research the underlying elements of thermodynamics/equilibria/kinetics in order to explain the
observed chemistry.
3. Use a multimedia presentation (digital poster or vodcast) to explain the chemistry to your peers.

1. Introduction
This week’s activity is a little different. Our demonstrators are going to give you an opportunity to sit
back and focus on using your observation skills, although there will be some opportunity to
participate.
We have organised a ‘round-robin’ collection of short demonstrations for you to observe – simple
chemical experiments with some interesting underlying thermodynamics, equilibria or kinetics, and
in some cases all of the above.
Make sure you make note of the reagents used in the different reactions you will observe in this
week’s activities. Ask the demonstrator to clarify anything along the way if you are unsure of the
chemicals or equipment being used to demonstrate a reaction.

Reading: Blackman et al., Chemistry (2019). Chapters 8-12 &15; CHM1051 Workbooks, Week
7-12.

2. The Demonstrations
Here is the shortlist of some of the activities – have a think about which subtopic each one explores.
You will be require a notepad and pen to take notes throughout the experiments. At the end of the
show, there will be a chance to break away into groups of 2 or 3 to start planning.

Experiment 1: Elephants Toothpaste Experiment 4: The Rainbow Clock

Experiment 2: Fire without Matches Experiment 5: Colourful Cobalt
Experiment 3: The Blue Fountain Experiment 6: Sugar Snake

Some questions to consider:

 What did you observe (use all of your senses where appropriate)?
 What is the chemical reaction?
 What principles are being explored with this specific reaction?
 What chemicals are involved?
 What factors affect the rate of the reaction?
 Is there a significant change in energy content of the products versus reactants?
 Can we speed up/slow down the reaction?
 Why do these chemicals react the way they do?
 What are the components of the equilibrium/oscillation reaction?
 Ex. 8: TEK Experiments

3. Presentations

Instead of the usual lab report this week, you will prepare either a digital poster (easy) or a vodcast
(more challenging) to present in Week 12. You will have access to the big screens so come prepared
with your presentation USB key. Do not use links to youtube clips, but feel to embed footage you
have recorded yourself in the lab. Do not print out your poster. Poster presentations should be
accompanied by a 5 minute oral presentation. Be prepared to answer questions from your
classmates and tutors.

If you chose to do a Powerpoint presentation, it should contain only a single slide with the relevant
information on it. Every individual will need to present some aspect of the chemical reaction being
discussed. You will be assessed on the slide presentation as a group so make sure everyone
understands the chemical reaction discussed, and presents part of the slide as well as being able to
answer questions relating to the reactions on the slide.

Take Photos and Record Footage! Don’t be afraid to use a camera during the show so that you
can add to the visual appeal of your presentation! Make it interesting so that others want to read your
poster and learn the material you have learnt. Remember, it is not important to only learn interesting
things but also make interesting the things that are to be learnt.

The Assessment: Of course this exercise is all about exploring the chemistry, so your presentation
will be assessed with this in mind. Your demonstrator will be marking your posters. You will also be
judged by your peers.
Prizes! Every presentation will also be judged by your classmates. A prize will be given out to the
popular favourite!
Group work: Since you are working in groups, make sure you have swapped details (email, phone
number) so that you can collaborate over the following week. Everyone is expected to know the
material presented by their group.

Poster Template: We have created a Powerpoint template for you to download from MOODLE.
Make sure you use this template, as it has to right font size pre-set to look good via our projector
system in the First Year Labs. The poster should explain the topic in a clear, coherent and correct
way with text and graphics. They key idea of a poster is to communicate information visually to other
people even if you are not present to talk about it. However, you should be able to discuss specific
aspects covered in more detail if requested.

Oral Presentation: Presentations are a good way of communicating your research to a large group
of people quickly. You have 4-5 minutes as a group to present the reaction you have observed.
Giving a presentation gives you the opportunity to receive instant feedback from your demonstrator
and peers. Your presentation can include models, demonstrations, samples or anything that will help
communicate the key points to the audience (but no hyperlinks to online material). The questions at
the end of the presentation (from your peers or demonstrator) may be directed at any member of the
group so ensure you understand the chemistry behind not only what you prepared, but also the
information prepared and presented by any member of your group.

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 Ex. 8: TEK Experiments

Presentation Marking scheme (/50)

65
 Appendix

Appendices

Data Page (as per exam)

Useful equations Physical constants
Wave equation: c =  c = 2.998 x 108 ms-1
Einstein equation: E = h
h = 6.626 x 10-34 J.s
1 1 1
Rydberg equation: = 𝑅(𝑛2 − 𝑛2 )
𝜆 𝑎 𝑏
R = 1.097 x 107 m-1
1 1
Balmer equation: 𝜈 = 3.29 × 1015 (𝑛2 − 𝑛2 )
𝑎 𝑏
NA = 6.022  1023
Bond order = 1 (# bonding electrons - # anti-bonding electrons)
2 R = 8.314 J/K/mol
Gases = 0.08206 atm·L/mol·K
Ideal 
Gas Equation: pV = nRT
1 atm = 1.013 x 105 Pa
𝑛 2𝑎
Non-Ideal Gas Equation: (𝑝 + )(𝑉 − 𝑛𝑏) = nRT
𝑉2
1 bar = 1.0 x 105 Pa
Total Pressure =  Partial Pressures of Component Gases
 Kw at 25 oC = 1.0 x 10-14
Thermodynamics
ΔU = q + w G = H – TS 0 oC = 273.15 K
w = -pV Go = -RTlnK

q = mcT G = G + RT ln Q

Equilibria
[base]
Henderson-Hasselbach: pH = pKa + log
[acid]
E°cell = E° red - E°ox

Kinetics
Zero-order reaction: [A]t = [A]o - kt
First-order reaction: [A]t = [A]oexp(-kt)
1 1
Second-order reaction (only one reactant A): − [𝐴] = 𝑘𝑡
[𝐴]𝑡 0

Half-life: t1/2 = 0.693/k

Arrhenius equation: k = Ae-Ea/RT
𝑘2 −𝐸𝑎 1 1
ln ( )= ( − )
𝑘1 𝑅 𝑇2 𝑇1

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