CHE1CHF Labmanual 2023

CHEMISTRY 1
CHE1CHF
Laboratory Manual
(Including Lab Report Worksheets)
2023
(i)
CONTENTS
SECTION A: LABORATORY INFORMATION
1. INTRODUCTION iii
1.2 Laboratory Registration iv
1.3 Attendance iv
1.4 Prescribed Items v
1.5 Compulsory Prelab Online Exercise v
1.6 Pre-Laboratory Instructions vi
1.7 Laboratory Manual Procedures and Notation vi
1.8 Reporting of Results vii
1.9 Marks and Marking vii
1.10 Plagiarism vii
1.11 Missed Laboratory Sessions viii
1.12 Laboratory Equipment and Cleaning viii
1.13 References ix
2. SAFETY IN THE CHEMICAL LABORATORY

2.1 Laboratory Personnel ix
2.2 Dress Requirements ix
2.3 Food x
2.4 Information About the Chemicals You Use x
2.5 Risk Minimisation and Laboratory Safety xii
2.6 Laboratory Waste xii
2.7 Emergency Procedures xiii
2.8 Preparation Room xiv
2.9 Mobile Phones xiv
3. LABORATORY LAYOUT xv
SECTION B: EXPERIMENTS
Training Experiment (compulsory)…………………….................2

Training Experiment: Report Book….…....................................13
Experiment 1……………………………………………................17
Experiment 1: Report Book…………………………….....……...31
Experiment 2.……………………………………………………....35
Experiment 2: Report Book…………………………………….…45
Experiment 4. ……………………………………………………...53
Experiment 5.……………………………………………………....74
Experiment 7…………………………………………………….…86
APPENDICES
Appendix 1: Derivation of equilibrium expression (EXPT 7)…100
Appendix 2: Common Laboratory Equipment…………………104
Appendix 3. Calculation of Yields………………………………109
Periodic Table…………………………………………………….111
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SECTION A
LABORATORY INFORMATION
( iii )
1. INTRODUCTION
Chemistry an experimental science and laboratory work constitutes an important

component of the discipline. The laboratory experiments are designed to help students:
• develop chemical handling skills;

• obtain experience with the safe handling of chemicals and provide experience
with important general safety issues associated with a laboratory workplace;
• provide familiarity with common chemicals and equipment;
• foster an understanding of fundamental chemical concepts, and to appreciate
how chemical /scientific information is obtained and
• interpret experiment data, represent data graphically and hence determine
relationships between variables.
The experiments in this manual involve the preparation and properties of inorganic and
organic compounds, and measurements in analytical chemistry. Students must
perform the experiments as individuals, with submitted reports based on their own
work. Basic laboratory concepts will additionally be tested in the Workshop Tests that
run during the semester. In addition to this manual, which provides the basic
instructions for the experiments, references are given where necessary. The complete
list of references is at the end of this section.
While the experiments you undertake this semester introduce some basic techniques
and methods in chemistry, worthwhile results can only be achieved if care is taken
when doing experimental work. It is important to understand all of the techniques
involved; there is a correct way to use a dispenser and a burette, to collect a precipitate
quantitatively, to qualitatively analyse an unknown inorganic compound, or to distil a
flammable organic liquid. In case of doubt, consult one of the demonstrators. It is their
job to assist, so make use of them!
Laboratory Coordinator: Dr. Carmel Abrahams

Email: [email protected]
Technical Officer: Nuchareenat Wiratpruk

Rm 303, LIMS1
` Phone: 9479 2394
( iv )
1.2 Laboratory Registration
For the CHE1CHF laboratory, students attend a fixed day (Mon-Thurs) for the semester. An
assigned group number will be published on the laboratory notice board and on LMS in
“GRADES” in your chemistry subject (at the end of week 1).
Students must register for a lab day on:

On ALLOCATE+
https://mytimetable.latrobe.edu.au/odd/student
You can register just before semester. You are able to allocate preferences for the day.
When Allocate+ is changed to “Read Only” you will need to contact Carmel Abrahams to
see if you can have your session moved.
1.3 Attendance
Each student is required to attend the rostered 3 hours laboratory experiments. If a class is
missed for a non-medical reason the experiment may be able to be completed on another
day (subject to availability), otherwise a mark of zero will be recorded for that particular
experiment.
If a class is missed on account of illness, your Demonstrator or the First-Year Laboratory

Coordinator should be informed as soon as possible and a medical certificate presented (to
your demonstrator the next session). If it is possible to complete the experiment on another
day, it should be done. However, if this cannot be arranged, an average mark will be given
for the missed experiment as calculated from the other marks received in that semester.
Note that this does not count as an “attended” laboratory session.
IMPORTANT
If a student enrolled in CHE1CHF is absent for more than one F2F laboratory session
(including medical), the laboratory attendance HURDLE for that course will not have been
satisfied. Students who fail to meet these requirements will have their result withheld until
the laboratory component is completed in the following year. Students need contact the lab
coordinator ASAP to organise make up experiments when they miss more than one.
(v)
1.4 Prescribed Items
The following compulsory items are required for the CHE1CHF laboratory course. You
MUST also print out the Laboratory Manual and Report Book and bring this to the
laboratory session. The following items may be purchased from The School Locker in the
Agora or online.
1. One pair of SAFETY GLASSES or OVERGLASSES (regular glasses are not

sufficient).
2. One LABORATORY COAT.
3. An electronic CALCULATOR.
1.5 Compulsory Prelab Online Exercise
Students MUST undertake suitable preparation before commencing their first Workshop
session and every laboratory experiment session. This is an important occupational, health
and safety issue. You MUST read the experiment in the manual and watch the relevant H5P
video as part of your experiment preparation. Then attempt (several are allowed) the pre-lab
quiz.
Each student MUST COMPLETE the online Prelab multiple-choice exercise BEFORE their
scheduled laboratory. Students need to bring a printout of their final Prelab mark (or have it
on their phone) as proof that they have completed this task. Any student failing to do so,
WILL NOT BE ALLOWED TO COMMENCE THEIR LABORATORY SESSION.
IMPORTANT: THE RESPONSIBILITY IS YOURS to show that you have completed the
prelab exercise. This exercise should take on average 15 minutes. You can attempt the
prelab as many times as you like and for as long as you like. This score will not be included
in your final lab mark. However, you must have a score shown in your receipt (as described
below) that is >70% to make your receipt valid. Completing the Prelab will automatically give
you a full four marks out of twenty towards your report assessment.
Completing the prelab exercise provides necessary preparation for the lab, which will reduce
the time you need to complete the laboratory session and enable you to achieve the most
from each experiment.
To access the online Prelab:

• Login to LMS
• Select your chemistry subject (CHE1CHF)
• Open the Laboratory Program folder
• Watch the relevant H5P video (for your experiment)
( vi )
• Select the relevant Prelab exercise (BE CAREFUL, some weeks there are three
different experiments running – you MUST do the CORRECT Prelab!).
• Click on Begin Assessment. You have infinite attempts available.
• MAKE SURE you SAVE as you go and then click on SUBMIT ALL and FINISH.
• Print screen containing test name, date and your final score (exactly as shown
below) or show receipt on your computer Smart phone.
Note that score shown must be > than 70%.
• REMEMBER to BRING your receipt to laboratory session (on your phone is OK).
This receipt allows you into your laboratory session!
• Students will be penalized 2 marks for not having a copy of the

manual/reportbook in Week 2. After Week 2, it is a 3 mark penalty. This is
part of professional behaviours.
1.6 Pre-Laboratory Instructions

Students are expected to prepare in advance:
• read the experiment, contact SCIHUB staff about any areas they do not
understand
• watch the relevant H5P video using the lab manual as a reference
• complete the relevant online Prelab exercise (achieve at least 70%, see 1.5
above)
• bring their printout of the laboratory notes and reportbook
• understand what they are about to attempt
• identify likely risks associated with the experiment (see Risk Assessment)
• clarify any points of uncertainty with the demonstrator
At the beginning of the laboratory session, the demonstrators will give a short introduction to
explain the theory of the experiment to be carried out and to demonstrate various laboratory
techniques.
1.7 Laboratory Manual Procedures and Notation

( vii )
The procedures outlined in this manual conform to consistent notation. Underlined

instructions indicate important aspects of the procedure, for example stir slowly or weigh
accurately. Bold italicized text refers to specific safety instructions, such as do not remove
solution from the fume cupboard.
1.8 Reporting of Results
For the experiments in CHE1CHF you are not required to write detailed laboratory reports.
You must record all observations and results in the Report Book. The relevant results and
report pages for each experiment must be completed and handed to the demonstrator at
the conclusion of each laboratory session (your responsibility).
It should be emphasized that an accurate laboratory record is an essential part of good
science and so results must be recorded as they are obtained. It is important that reports are
based on your own work and are neat, clear and concise. Marks will be deducted for reports
that are not legible. Show ALL working in any calculations.
1.9 Marks and Marking
Of the total marks for the Chemistry CHE1CHF courses, 25% are allocated to laboratory
work. The marking schemes vary and depend to some extent on the type of experiments
being carried out. Each experimental report is given a mark out of 20.
Demonstrators will give further information on how student performance is assessed.

Demonstrators will provide written feedback on all graded laboratory reports. You can
access your lab marks within LMS. If you have any queries about your grades, please
contact your demonstrator or the Laboratory Coordinator.
1.10 Plagiarism
La Trobe University defines plagiarism as:
“occurs when someone uses words, ideas, or work products attributable to another
identifiable person or source:
(i) without attributing the work to the source from which it was obtained
(ii) in a situation in which there is a legitimate expectation of original authorship
(iii) in order to obtain some benefit, credit, or gain which need not be monetary”
(Fishman, T. International Center for Academic Integrity )
1. The related concept of self-plagiarism refers to the re-submission of
work as if it were original. Students must not submit their own academic
work for assessment when it has already been submitted for
assessment at another time (including at another institution), without
the express permission of the academic staff member who will assess
it.”
It is regarded as a form of academic cheating. Taken from La Trobe University (2017) Academic
policies, https://policies.latrobe.edu.au/document/view.php?id=221&version=1
La Trobe University takes plagiarism very seriously. There are serious
consequences for students caught plagiarising work.
( viii )
( ix )
1.11 Missed Laboratory Sessions
When a student is sick, they are required to bring a medical certificate to the
demonstrator or to the Laboratory Coordinator. Similarly, for a funeral of a close
relative or close friend, the student is to bring a funeral notice or a letter from a family
member. Other, “less stressful” occurrences, such as a car breakdown, athletics
meeting, work commitments and so on should be referred to the Laboratory
Coordinator. If you (the demonstrator) are unsure, refer the student to the Laboratory
Coordinator.
1.12 Laboratory Equipment and Cleaning
Students need to clean up properly

For the CHE1CHF laboratory you will be assigned to a bench place for each experiment.
The apparatus is issued in a clean, workable condition and should be checked at the
beginning of each laboratory session. Draw content lists are provided. Report any missing
or broken items immediately to your demonstrator who will inform the technician in the
Preparation Room. Under no circumstances should you remove apparatus from
another student’s bench.
You are required to keep your bench clean and tidy and, in common with all others in the
class, to assume responsibility for the laboratory as a whole.
At the end of each working period, all apparatus must be carefully cleaned and left in the
appropriate drawer. Draw content lists are provided and you are required to return your
cleaned equipment to the correct location. The bench and sink must be left clean and any
waste put in the bins provided in the benches. The fume cupboards and balance rooms
should be left in a clean and tidy condition.
Marks may be deducted for students leaving their bench place in an untidy or unclean
state.
Glassware: Detergent is provided in plastic wash bottles and should be used for cleaning
all glassware. If this is ineffective, consult the demonstrator about a special
cleaning mixture.
Reagents: Common reagents, such as acids and bases, are provided on the shelves
above each bench. Take care not to contaminate them. Solutions and reagents
for particular experiments will be put out on your benches. A few compounds
are kept in the fume cupboards. Do not take more solution than you actually
require for the experiment. Do not pour “leftovers” back into reagent bottles.
(x)
1.13 References
The following texts are referred to in certain experiments.
1. J.S. Fritz and G.H. Schenk, Quantitative Analytical Chemistry, Allyn and Bacon.
2. Peter Mahaffy; Roy Tasker; Bob Bucat; John C. Kotz; Gabriela C. Weaver; John E.
McMurry; Paul M. Treichel, Chemistry: Human Activity, Chemical Reactivity,
International Edition, 2014.
2. SAFETY IN THE CHEMICAL LABORATORY
Experimental chemistry is a vital part of your chemical training. In the laboratory you will
develop many hands-on skills and consolidate your learning of a range of chemical
principles. In order for this to happen you need to adopt a responsible and mature attitude
during your laboratory classes. Chemicals can be dangerous so it is important that you learn
and know how to handle them safely. The following section explains some of the basic code
of safe laboratory practice.
2.1 Laboratory Personnel
You will have at least one demonstrator in the laboratory with you at any time, together with
a member of the technical staff. These people have a wide knowledge of the chemicals,
equipment and procedures you are using and also appropriate emergency response
procedures. Please consult them if you are in doubt about any procedure or are involved in
an accident.
Report ALL accidents and chemical spills to YOUR DEMONSTRATOR who will inform other
laboratory personnel if further action is required.
2.2 Dress Requirements
For your safety there are several requirements that must be followed. If you are not suitably
attired you will be asked to leave the laboratory immediately.
1. SAFETY GLASSES/OVERGLASSES MUST BE WORN AT ALL TIMES. Even if

you normally wear prescription glasses you must wear safety eyewear. It is
compulsory for students wearing prescription glasses to wear Safety Over-
glasses. Sunglasses are not permitted. This also applies to demonstrators
wearing prescription glasses.
( xi )
2. Only FOOTWEAR with enclosed, solid uppers are permitted. Students with
thongs, open sandals or slipper type shoes (uncovered uppers) will not be
allowed into the laboratory.
3. LABORATORY COATS protect both clothing and person from corrosive
chemicals. Shorts and tops that leave exposed midriffs or shoulders are not
permitted.
4. Students with long hair must have it tied back before entering the laboratory.
2.3 Food
No food, drinks (including water) or chewing gum may be consumed in the laboratory for
health reasons.
Smoking is strictly forbidden in all University buildings and also constitutes a fire hazard in
the laboratory.
2.4 Information About the Chemicals You Use
Safety notes and risk assessments are included at the start of each experimental procedure
in this manual. There are two easy ways to find out more about the hazards of a chemical
you are about to use:
(i). Read the label. It should contain the following information:
• product name
• dangerous goods warnings (eg. corrosive, poison)
• chemical name(s) of the contents
• possible harmful information (risk information)
• how to use the substance safely
(ii). Material Safety Data Sheets (MSDS)
These contain more comprehensive information about the chemicals; health hazard
information, first aid procedures, and safe handling and disposal procedures.
MSDS are available on the web.

( xii )
2.4.1 Health Effects: Hazardous chemicals can adversely affect your health if you expose
yourself to them unwisely. The primary routes of exposure and ways of minimising such
exposure are:
• Respiratory (breathing in gases, vapours and particulate (dust) matter).

Work in fume cupboards when using gases and vapours.
• Contact with intact or broken skin (usually liquids or solids).
Wearing gloves and being careful can minimise this.
Always wipe up spills immediately (if necessary contact a member of staff).
• Ingestion (including accidental ingestion).
Wash your hands frequently and definitely before leaving the laboratory.
In no circumstances pipette by mouth.
2.4.2 Description of Hazard Categories and Rating Scale
There are five categories: Toxicity and Chronic, Flammability, Reactivity and Contact. Note
that some international regulations combine Toxicity and Chronic into a Health category. In
each category there is a Rating Scale, which is a number ranging from 0 (for low level of
risk) to 4 (for high level of risk).
(i) Health Category (Toxicity and Chronic) refers to the capability of the chemical to cause personal injury due
to inhalation, skin contact, eye contact, or ingestion.
Rating Risk
0 Little to no risk
1 Caution Compound can cause irritation
2 Warning May be harmful if inhaled or absorbed
3 Warning Corrosive or toxic. Avoid skin contact or inhalation.
4 Danger May be fatal on short exposure. Specialized protective equipment required
(ii) Flammability Category refers to the ability of the chemical to create or sustain a fire.
Rating Risk
0 Not combustible
1 Combustible if heated
2 Caution Combustible liquid flash point of 37.8° to 93.4° C
3 Warning Flammable liquid flash point below 37.8° C
4 Danger Flammable gases and materials rapidly vaporized under normal conditions
(iii) Reactivity Category refers to how reactive the chemical is under normal laboratory conditions.
Rating Risk
0 Very inert substance. Not reactive when mixed with water
1 May react if heated or mixed with water but not violently
2 Caution Unstable or may react violently if mixed with water
3 Warning May be explosive if shocked, heated under pressure or mixed with water
( xiii )
4 Danger Explosive material at room temperature
(iv) Contact Category refers to how dangerous physical contact with the chemical is under normal conditions.
Rating Risk
0 No unusual hazard.
1 Compound can cause irritation.
2 Caution May be harmful if inhaled or absorbed
3 Warning Corrosive or toxic. Avoid skin contact or inhalation.
4 Danger May cause severe damage with contact to skin, eyes or mucous membranes
Keep in mind, these descriptions are for general conditions and do not cover all possibilities.
For example, water has a health and contact rating of zero. However, one can kill themselves
by drowning, and boiling water or steam can be very dangerous with respect to physical
contact. Similar analogies are possible for every chemical. This just emphasizes that a
certain level of professional understanding and common sense is required when handling
chemicals.
2.5 Risk Minimization and Laboratory Safety
There are several general principles that relate to the hazard category and rating of chemical.
It should also be noted that for safety reasons, students are not allowed to enter the
preparation room.
• Regard all chemicals as hazardous until you know otherwise. Consult the MSDS. Avoid
unnecessary contact with chemicals. Read the experiment notes before entering the
laboratory. It is a responsibility of the demonstrator to highlight to students the more
hazardous aspects of experiments at the start of each laboratory session.
• Students must not leave experiments unattended.
• As a matter of safety, students should keep their work area tidy, uncluttered and clean.
• Never use force when manipulating glassware. Lubricate glass tubing with water or an
organic solvent when connecting it to rubber tubing.
• Any device that constitutes a fire hazard should not be used within the laboratory,
including cigarette lighters, matches.
2.6 Laboratory Waste
It is vital that laboratory waste is disposed of safely. If in doubt, please consult your
demonstrator.
If you break any glassware, inform your demonstrator who will arrange to have it cleaned up.
Do not attempt to pick up broken glass with your hands. Be aware that most minor
laboratory injuries are the result of cleaning up broken glass rather than the initial breakage.
( xiv )
All broken glass will be placed in the broken glass bins, not in regular paper waste bins after
being swept up with a dustpan and brush.
There are many chemicals that you should not put down the sink. In some experiments
dedicated waste containers are provided. Your demonstrator will inform you what liquid
waste can be poured down the sink and what liquid waste must be poured into the dedicated
waste containers. If the experiment produces a solid waste, this should not be thrown in the
waste-paper bins but should be placed in a dedicated solid chemical waste container. If you
are unsure always ask your demonstrator.
Do not take more of a chemical from its original container than the quantity specified in this
manual so as to minimise your chemical waste. Never return excess chemicals to their
original container, as this commonly leads to contamination.
2.7 Emergency Procedures
During the introductory session in the first-year laboratory, your demonstrator will point out
the location of emergency exits, safety showers and eye wash stations. In the event of an
emergency, you should follow the instructions of demonstrators, safety officers and
emergency personnel.
2.7.1 First Aid: All accidents must be reported to your demonstrator who will contact a first
aid officer. All technical officers are trained first aid officers. Once an injury has been attended
to, you will be asked to sign a University accident/injury form. This form protects you in the
event of any long-term consequences associated with your accident. It also helps us to
prevent similar accidents in the future.
2.7.2 Fire: First of all, do not panic. Most fires can be extinguished by covering them; thus
starving them of oxygen. Fire extinguishers are located in each laboratory with all technical
staff trained in their use (please do not use them yourself). If the fire is serious enough to set
off the fire alarms, please evacuate the building in an orderly manner and assemble in the
appropriate evacuation assembly points.
2.7.3 Evacuation: This may be necessary due to a fire, chemical spill or bomb threat in your
laboratory or elsewhere in the building. If an alarm sounds, extinguish any burners or other
heating equipment being used in your experiment, then follow the directions of your
demonstrator and exit the building swiftly through the nearest exit and make your way to the
appropriate assembly point. Follow instructions of the Fire Wardens and Technical Staff. The
nearest Assembly Point for the LIMS1 building is the behind the library next the LIMS1
building.
( xv )
2.8 Preparation Room
Students are not allowed to enter the preparation room. If unattended, ring the bell placed
on the bench next to the preparation room door and wait behind the hazard tape for
assistance.
2.9 Mobile Phones
Mobile phones need to be turned off or to silent while in the laboratory. If you need to use a
mobile phone, first make your experiment safe, inform your demonstrator, and then leave
the laboratory to make your call.
( xvi )
3. LABORATORY LAYOUT
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It is important that you are familiar with the safety features of laboratory, including:
• Emergency exits
• Fire extinguishers and fire blankets
• Emergency eye-wash station
• Emergency shower
1
SECTION B: EXPERIMENTS
TRAINING EXPERIMENT
4 marks for Prelab OH&S receipt and 16 marks for attending.
An Introduction to the First Year Chemistry Laboratory.
The Chemistry Foundations (CHE1CHF) subject at La Trobe seeks to provide

students with fundamental, essential concepts that will support each student’s
foundational science knowledge for a broad range of degrees. An important role of
this foundational chemistry subject is also the development of important generic
laboratory skills that students will likely use throughout their degree and beyond.
Throughout the laboratory program, within CHE1CHF, students will:
• learn and practice key equipment handling skills
• practice the safe handling of chemicals
• learn/develop workplace OH&S practices
• undertake various chemical reactions and observe and report the outcomes
• practice the formalism associated with describing chemical reactions
• undertake various numerical calculations associated with chemical reactions
At the start of semester, students undertake this Training Experiment in LIMS1 304.
This session provides you with a supported opportunity to practice many of the
activities you will be asked to undertake in later experiments. This compulsory, low-
stakes session will involve six activity stations that each student group will rotate
through. Within the groups students will mostly undertake these activities in pairs.
The stations will include:
• Station A: Thin layer chromatography and weighing on a top loading balance.

• Station B: Serial dilution and the use of a pipette.
• Station C: Modelling molecules.
• Station D: Key volumetric titration skills.
• Station E: Testing your knowledge
• Station I: Important OH&S talk
The activities in each of these Workshop stations are discussed in detail below.
Note: Every group will start at a different Station and rotate through the
activities! Complete the Training Experiment Report Book as you work through
the stations.
Students MUST be on time for this COMPULSORY session. Students that

are not on time will need to attend another session during Week 2. Each
station will need to finish after ~28 minutes. So, make sure you listen to your
demonstrator and prepare for the class by reading and bringing your signed
Chemistry Lab induction & Authorization form.
2
Station A: Part I: Thin layer chromatography and weighing on a top loading
balance (30 min).
With instruction from the demonstrator and working in pairs students will:
1. draw a pencil line 1 cm from the base of one TLC plate;

2. using a micropipette, spot the dye mixture onto the middle of that line;
3. place < 1 cm height of solvent (eluent) into the developing jar (if it not already
there);
4. place the TLC plate into the developing jar, close the lid (develop the
chromatogram);
Fig. 1: Developing TLC.
This Photo by Unknown Author is licensed under CC BY-

5. when the solvent reaches ~ 85% (may be lower to save time) of the height of
the plate, remove the and mark the height with a pencil and
6. using a ruler, calculate the Rf value of the red spot.
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Part II: While waiting for the solvent to move up the plate, weigh out either NaCl
(table salt, ~3.2 g) or sucrose (table sugar, ~27 g) on a top loading balance.
(i) Place an empty weighing jar on the balance.
(ii) Zero (tare) the balance.
These Photos by Unknown Author
is licensed under CC BY-SA-NC
Fig. 2: NaCl solid lattice.
Fig. 3: A top loading balance.
(iii) One student will weigh out NaCl (~3.2 g), the other will weigh out sucrose (~27
g). Note: Never add a chemical directly in the balance. Take the weighing
jar off to fill – do not re-zero!
(iv) Record the masses (g) in the Report Book to two decimal places (round up or
down).
3
Clean up
Part I
1. Leave the eluent in the jar. EXCEPT for the last group of the session for
the day, they should empty the eluent from TLC jar into hydrocarbon waste
bottle in the fume cupboard. TLC jar is to be rinsed with a small amount of
acetone, empty into hydrocarbon waste bottle, then place back on the bench
with the lid off to dry.
2. Place TLC in toxic solid waste container.
Part II
1. Place the solid (NaCl or sucrose) back in the jar.
Normally you should wash and dry the weighing jar (in this time sensitive
session it is NOT necessary.)
4
Station B: Dilution and using a pipette (30 min).
TAKE CARE WHEN USING THE PIPETTE: Follow the demonstrator’s
instructions! While attaching the pro-pipetter, hold the pipette nearest the end
of attachment.
Making up solutions of various dilutions is an important generic skill.

With instruction from the demonstrator and working in pairs, students will make a 1
in 10 dilution of a supplied ~1 M stock solution (using a 50 mL volumetric flask) by:
1. First determining 10% of 50 mL (record this in Report Book).
2. CAREFULLY, place the pro-pipetter, holding the pipette at the end you
are attaching it to, until it feels firm.
3. Pre-rinse the pipette, use the pro-pipetter by drawing up the stock solution into
the pipette by turning the wheel downwards with your thumb, and then release
the volume into a beaker. This is one of your rinsings.
4. By pipette, add the volume determined in 1. (above) of the ~1 M stock solution,
into the 50 mL volumetric flask and then
5. Using a RO (reverse osmosis) water wash bottle add RO water to just below
the graduated mark. Then carefully, using a disposable pipette add RO water
dropwise until the water meniscus sits on the graduation mark. Stopper the
flask and holding this stopper in place, invert the flask a few times to
homogeneously mix the solution. This is solution A.
If time permits, your demonstrator will then describe how a further 1 in 10

dilution of solution A might be carried out. Your demonstrator will record the UV
absorption of the three solutions (stock solution, solution A and RO water).
Fig. 4: A serial dilution, showing five 1 in 10 dilutions.
This Photo by Unknown Author is licensed under CC BY-SA-NC
5
Clean up
1. Tip the contents of the volumetric flasks into the appropriate waste container
in the fume cupboard.
2. Take flasks to the sink, wash with detergent, rinse with RO water, then place
back on the bench.
3. Dismantle pro-pipetter from pipette, at the bench. Do not remove pipettes
from bench.
6
Station C: Modelling molecules (30 min).
Polarity is an important concept that students need to understand (but not completely
today!). A molecule is polar if the distribution of electrical charge is over the
molecule, is uneven. This may arise when you have bonds between different atoms.
Since different atoms, when they share bonding electrons, have a different ability to
attract those bonding electrons towards themselves (this ability is called
electronegativity). We can compare this to a tug of war for the shared bonding
electrons between two atoms. If one atom is more electronegative than the other,
that means it is stronger at pulling the negatively charged bonding electrons towards
their nucleus, making that atom slightly negative. Most elements have different
electronegativities.
Without a great deal of knowledge, you can assess the likely polarity of a molecule
by looking at the symmetry of the molecule model. Highly symmetrical molecules
and C, H compounds we reasonably predict as non-polar. All other molecules
with reduced symmetry you can predict will be polar i.e. the molecule has a
permanently negative end and a permanently positive end.
Examples of:
i) Polar molecules
H H
H I C H C
Cl
H
Cl H C
H 3C H
Hydrogen iodide - HI
H
chloroethane - CH3CH2Cl
ii) Non-polar molecules

H H
C
N N C
H H
H H C
H H
Nitrogen - N2 H 3C
H
ethane - CH3CH3
Table: Colour guide to the molecular model atom representation in 1st year lab.
Connector Colour Atom
white hydrogen
black carbon
red oxygen
blue nitrogen
green chlorine
Note: Every single section of clear hosing in these models represents two bonding electrons.
7
Polar compounds tend to dissolve in polar liquids (solvents). Non-polar compounds
tend to dissolve in non-polar solvents. In pairs students will:
1. With your partner, assign the provided models of common solvents as polar or
non-polar by considering their symmetry or if they only contain C&H.
Example: Hexane (C6H14); C is black, H is white.
The ionic solid, AgCl, is very insoluble. When solutions of AgNO3 and NaCl are
mixed a solid forms (a precipitate) according to the following reaction (your
demonstrator will demonstrate this):
AgNO3(aq) + NaCl(aq) à AgCl(s) + NaNO3(aq)
2. Using the model kits & provided images your demonstrator will explain this
model representation of the above precipitation reaction, showing the solvation
of the Ag+, Na+, NO3- and Cl- ions when they are dissolved in solution. They will
also show the 3D lattice of solid AgCl.
When a carbon is NOT bound to four different groups of atoms) its mirror image is
superimposable (the same molecule)!
mirror
Z Z
C C
W W
Y Y
Z Z
Z
Z
The molecules above superimposed.
C
W C
W Y
Z Y
Z
I.e. Each group coming off the carbons can be placed in the same position when
these molecules are superimposed – so they are the same molecule!
When a carbon is bound to four different groups (colours) of atoms its mirror image
is non-superimposable!
8
X
C
W
Y
Z
W-Z = different types of atoms (or groups of atoms)
3. Using pre-prepared models, representing the above molecules and their

mirror images, try to superimpose the mirror image models i.e. place them on
top of each other with all the groups in the same position (ask yourself, when
can it be done?).
9
Station D: Key titration skills (30 min).
With instruction from the demonstrator and working in pairs students will:
1. Starting ASAP, practice filling a burette.
a) Take burette out of clamp.

b) Invert, close tap, add funnel.
c) Fill below eyeline (NOT to 0.00 cm3). IMPORTANT: Ensure tap is
closed!
2. Reading a burette. At this station you will be required to read the solution level
of two burettes.
Scale is in mL (cm3)
This Photo by Unknown Author is

licensed under CC BY-SA-NC
Record the heights of the solution inside the burettes (i.e. the bottom of the
meniscus) in your Report Book. The correct reading here is 30.31 mL. Note:
the direction of the numbering!
3. Which three of the following are concordant (within 0.20 mL) titres? The titre
is the volume delivered from the burette into the reaction. The reaction is
routinely repeated four times. You determine the average titre from three
concordant results.
Titration Titre (mL)
1 10.05
2 10.10
3 9.98
4 10.22
4. Your demonstrator will demonstrate a titration to you. They will show you how
an indicator is added and the changes you might observe.
5. Your demonstrator will show how to rinse/clean the burette. Leave it inverted,
with tap open.
10
Station E: Testing Your Knowledge (30 min).
Students will complete a short worksheet containing the basic scientific knowledge
that students learn at school. Students should not worry if they do not perform well in
this worksheet. Take the sheet to a SCIHUB session/s this will allow you to quickly
master the concepts/knowledge. This worksheet, will assist you with the Workshop 1
Test, it will cover:
• Prefixes, i.e. 1 microgram = µg = 1 x 10-6 g.
• Element symbols/names i.e. Cu is copper.
• Significant figures (calculations) (attend the tutorial in Week 1).
• Subatomic particles, i.e. 32𝐻 has 1 proton, 1 neutron and 1 electron.
• Logarithms
• Rearranging algebraic expressions (attend the tutorial in Week 1).
On your LMS, there is a 2023 SCIHUB subject. The list of tutors and the links to the
online ZOOM sessions are found here. There are different tutors and times, try one
that suits.
There will also be face-to-face sessions available. Attending one session before each
experiment, workshop test or getting help with OWLs will help you enormously.
Face-to-face Tutorial sessions are valuable. Students can ask questions about
assessment and what content is important and what content less so. These are
designed to be engaging sessions.
Station F: Safety talk (30 min).

Students are responsible for signing the RA/attendance (see end of Report Book) in
THIS Station! Students must also show their OH&S quiz receipt.
Have YOUR Prelab OH&S receipt ready as you walk into the Station F room!
Your demonstrator will talk through the following OH&S issues with you:
• Personal Protective Equipment (PPE) requirements
• phone rules
• fire extinguisher/blanket locations
• gloves and taps
• lab safety equipment / fire blankets / eyewash station / showers / waste
• emergency evacuation location
OHS
First Name Surname Student ID Group RA signed
quiz
1 Jane Doe Thurs_10:00_Group_1 ü (student signature)
2 John Smith Thurs_10:00_Group_1
11
12
Training Experiment – Report Book
Station A Part A - TLC

Name of eluent?
Find Rf value of red spot
Part B – Weighing the mass of NaCl and sucrose

Record the actual mass of NaCl Record the actual mass of sucrose
weighed out. (~3.20 g) weighed out. (~27.00 g)
Station B How can you readily tell if a substance absorbs visible

light?____________________
What is 10% of 10 mL? __________________
What is 10 % of 50 mL? _________________
What is the provided stock solution
concentration?_________________
What is the concentration of solution A?_________________
How does the absorbance change as the solution becomes more
dilute?
________________________________________
Station C After looking at the models assign the following solvent molecules as
polar or non-polar.
Solvent Polar or Non-polar
Water (H2O)
Hexane (C6H14)
Acetone (CH3COCH3)
Ammonia (NH3)
Ethanol (CH3CH2OH)
Chloroform (CHCl3)
Toluene (C6H5CH3)
Tetrachloromethane (CCl4)
Dimethyl ether (CH3OCH3)
Station D Burette Record burette readings
(to 2 decimal places!)
1
2
List the three concordant results
from the table.
Station E Where do you get extra help in CHE1CHF? -

_________________________
Student’s will work through a provided worksheet in this session.
Station F Students need to sign attendance sheet below (see attached) and
show your demonstrator in Station F.
13
14
After completing Station F (OH&S) in the Introductory Laboratory session students MUST complete the
checklist below, sign the declaration and hand this form to their demonstrator in Station F.
Students are ONLY allowed to commence experimental work in the teaching lab after completing
this form.
I understand that: (tick
here)
I must always wear a lab coat while in lab
I must wear safety glasses at all times in lab and ensure that long hair is tied back.
I must wear fully enclosed footwear in the labs (thongs, sandals, ballerina flats, clogs, scuffs, high
heels and other open-style shoes are PROHIBITED in labs.)
No smoking, no illicit drugs, no food (or drink) consumption (including chewing gum) can occur
within the laboratory.
I must not: sit on benches, stand on stools, kneel on the floor, run or engage in practical jokes in
the laboratory.
I have identified the location of the storage space for bags / other belongings. No items are to be
stored on floor of the teaching laboratory.
I will not use a mobile phone for any reason in the laboratory (including work-related purposes
such as a calculator or taking experiment setup photos) and, if carried in a pocket, it will be on
silent. All mobile phone use should be outside of the laboratory.
I will not wear my lab coat and gloves outside of the laboratory.
I will ask assistance before using lab equipment that I am unfamiliar with or haven’t used before.
I will turn up for lab on time, well prepared, adopt an alert attitude in the lab and will always be
conscious of potential hazards.
I will not enter prep room without permission.
OH&S is important in the lab, and I will conduct myself in a safe manner.
In an event of spill, I will immediately inform the demonstrator or the laboratory technician.
I must report any breakages, accidents or faulty equipment to the demonstrator or the laboratory
technician, immediately.
I MUST clean: apparatus, my work bench and be signed out before leaving the lab.
I understand what I need to do and where I need to go in the event of an emergency evacuation.
I have been shown: (tick

here)
the location and use of eye wash, safety shower and emergency exit
the location of gloves (contaminated gloves need to be disposed of in the solid toxic waste)
where to report incidents and near misses or breakage
where to access first aid
the solid toxic waste – white cans or buckets either placed on the benches or in fume cupboards
the liquid waste – dispose of liquid waste to appropriate waste container
Student Name: __________________________________ Subject: ____________

Signature: ______________________________________ Date:
____/____/____
Demonstrator’s Name: ____________________________
Signature: _______________________________________ Date: ____/____/____
15
16
EXPERIMENT 1
TLC & M&M©’s
AIMS OF THE EXPERIMENT

To separate components in a mixture, using the technique of Thin Layer
Chromatography (TLC). To observe the effects, resulting from the differing solvent
polarity, on the TLC separation of components in a mixture. Apply the technique of
TLC, to separate and identify food dyes used in the coating on M&M®s.
SKILLS IN FOCUS
• Preparation of a micropipette by drawing out a capillary tube heated in a flame
(see short video on LMS, NOTE: no gloves as gloves can melt).
• The safe use of a Bunsen burner.
• Developing a chromatogram using the technique of Thin Layer Chromatography
(see short video on LMS).
• Extraction of compounds using solvents of varying polarity.
• Appropriate waste disposal of organic substances.
• Appropriate use of basic lab equipment (gloves, fume cupboards, gas taps, etc.).
REMEMBER FOR WORKSHOP TEST

• A mixture is the combination of two or more substances, where each substance
retains its own physical properties.
• A mixture can be separated by utilizing difference in the physical properties of the
components (e.g. melting points, phase, solubility, etc.,).
• Examples of mixtures: sea water (water and dissolved solids); ink (different dye
compounds); etc.,
• The stationary phase in TLC is often finely divided solid alumina (or silica).
• The mobile phase in TLC is a solvent or solvent mixtures.
• Definition of analyte - a substance whose chemical constituents are being identified
and measured.
17
CHEMICAL ALERT
(Risk Assessment)
Substances: dye, water (H2O)
~25 ml solvent [ethanol (C2H5OH), butanol (C4H9OH), acetone (propanone, CH3COCH3),
chloroform (trichloromethane, CHCl3), ethyl acetate (ethyl ethanoate, CH3CO2C2H5), methanol
(CH3OH), toluene (methyl benzene, C6H5CH3), cyclohexane (C6H12)]
Hazards: Ethanol has a flammability rating of 3 and a toxicity, contact and chronic rating of 2. Butanol has
a contact rating of 3 and a flammability and toxicity rating of 2.
Acetone has a flammability rating of 3 and a toxicity, contact and chronic rating of 2.
Ethyl acetate has a flammability rating of 3 and a toxicity and contact rating of 2.
Toluene has a flammability and chronic rating of 3 and a toxicity and contact rating of 2.
Chloroform has a chronic rating of 3 and a toxicity and contact rating of 2.
Cyclohexane has a flammability rating of 3 and a toxicity, contact and chronic rating of 2.
Methanol has a flammability rating of 3 and a toxicity of 3/4, contact and chronic rating of 3/4.
RATINGS: 0 = Nil, 1 = Low, 2 = Moderate, 3 = High, 4 = Extreme
Protection: Read ALL safety warnings on coded solutions and unknown solids.
Safety glasses are required. Disposable gloves are available.
Avoid contact with all solvents and mixtures (dyes included)
INTRODUCTION
Chromatography - is a process for separating a mixture of compounds into its

individual components. This separation is achieved by passing a sample mixture
(analyte) in a moving stream of solvent (mobile phase) through a material (stationary
phase) that provides resistance by virtue of chemical interactions (not reactions)
between the components of the sample and the stationary phase (see Table 1).
TABLE 1: Common chromatographic methods and their uses

Method Stationary Phase Mobile Application
Phase
1 Column Alumina or Silica Solvent Separation of mixtures
Chromatography
2 Thin-layer Alumina or Silica Solvent Analysis
Chromatography (limited use for separation)
3 Paper Paper Solvent Analysis
Chromatography
4 Gas Chromatography Non volatile liquid Gas Analysis and separation
coated on solid support e.g. N2
Thin-Layer Chromatography (TLC)

In thin-layer chromatography (TLC) [Figure 1], the stationary phase is a layer of finely
divided solid, usually alumina or silica, deposited on a solid support. A small drop of the
sample solution to be investigated (the “analyte”) is spotted near the bottom of the plate, and
the plate is then placed in a jar (‘development tank’) with a suitable solvent at the bottom,
below the level of the sample spots. The solvent, the mobile phase, then moves up the
plate, by capillary action, carrying the components of the spot of sample with it. The
18
components in the spot interact differently with the stationary phase and therefore travel at
different rates – resulting in separation.
Here are two YouTube videos to illustrate the concept and process.
http://www.youtube.com/watch?v=Mer8RFcGDvk
https://www.youtube.com/watch?v=qdmKGskCyh8
Flask
TLC plate
Moving solvent front

Sample spots
Developing solvent
Figure 1: TLC plate in developing flask.
When the solvent front has moved up to ~85% of the height of the plate, the plate is removed
from the development tank and the position of the solvent front marked immediately.
The solvent is then allowed to evaporate from the plate. At this stage, all visible spots are
marked. There may be some colourless spots as well. There are several methods available
to make these visible (e.g. UV, etc.).
The Rf value (Retention factor), for each marked spot on the

chromatogram, can be calculated using the formula below:
distance compound moved

Rf =
distance solvent moved
The Rf value is a ratio, and is a measure of the relative

distance that a compound has moved. The Rf value is quite
characteristic and can be used for the identification of
compounds, provided conditions are constant, e.g. same
solvent.
Often in TLC the solvent (mobile phase) is non-polar, and the stationary phase is
polar. Using a more polar solvent, it is possible to increase the time spent by a polar
compound dissolved in the moving phase and hence to increase the distance moved
up the plate. The dielectric constant of a solvent can be used as a guide to its
polarity, the higher the dielectric constant the more polar the solvent. Typical
dielectric constants for several solvents are presented in Table 2 below.
19
TABLE 2: Useful solvents for TLC.
Solvent Dielectric Constant

n-hexane 1.9 Less
Cyclohexane 2.0 polar
Toluene 2.4
Diethyl ether 4.3
Chloroform 4.8
Ethyl acetate 6.0
Butanol 17.0
Propanol 20.0
Acetone 21.0
Ethanol 24.0
Methanol 33.0 More
Water 80.0 polar
Polarity – The concept of polarity is important for understanding chromatography. A

molecule is polar when it has an overall uneven distribution of electrons relative to
the protons within the nuclei. Water (H2O) is polar molecule since it has a
permanently slightly negative end (d-) and a permanently slightly positive (d+) end.
This occurs because the electronegative oxygen draws the two electrons it shares in
each O-H bond closer to the oxygen atom. rather than equally sharing those bonding
electrons. This and the fact that hydrogen atoms do not surround the oxygen atom
symmetrically results in a slightly negative (d-) end of the water (see red) and a
slightly positive (d+) end of the molecule [Figure 2]. Polar molecules will generally
dissolve polar molecules (or ionic substances).
When the electron distribution is even then the molecule is non-polar i.e. N2, Cl2,
CH4, etc..
d-
Figure 2: Water molecule polarity.
d+ d+
In this experiment a number of solvents, of varying polarity, will be used so that you can
observe the effect of solvent polarity on the separation of components of a mixture.
20
Summary
The purpose of Part A is to:
• make-up micro-pipettes
• demonstrate the concept of chromatography for separating the components of
a provided mixture,
• observe the effect of solvent polarity on mixture separation,
• interpret chromatograms, developed from different solvents, to determine how
to optimising solvents for use in TLC, and
• identify components of a mixture by comparison with reference dyes.
The techniques and approach will then be applied in Part B to identify components of
a dye mixture used in the coatings of M&Ms.
PART A - SEPARATION OF THE COMPONENTS OF A DYE MIXTURE BY TLC
The dye mixture you are provided with (Part A) contains the following three dyes:
OCH3
N
N
HO
Sudan Red G
N N
Indophenol Blue
O
Note: The exercise is not designed to fully optimise the solvent conditions, but to simply
explore the effect of solvent polarity on component separation, and to identify the key
criteria that would be used to optimise solvent conditions. To find the optimum
conditions for the separation of these dyes it would be necessary to try out a larger
number of solvents of different polarity, and to also consider mixtures of solvents. The
solvents that are considered in the experiment are sufficient to make illustrate the
concepts and make some conclusions.
21
PROCEDURE
Note: For PART A students will each prepare their own TLC plates but will work in pairs to
choose 4 solvents to develop their TLC plates in. All other work is expected to be done
individually including the Rf calculations and interpretation of the TLC plates.
Prepare micropipettes (capillary tubes) for use throughout the experiment.
1. Prepare a at least 3 (and up to 6) capillary micropipettes (for the whole expt.) by drawing
out melting point tubes. There is an instructional video on LMS and your demonstrator
will demonstrate the technique.
WARNING! Be careful to not place your fingers on the hot parts of the glass
capillary tube during this procedure. Place fingers at the ends of the tube
when heating and drawing. No gloves to be worn for the preparation of the
micropipettes. Wait a short time and allow the drawn middle section to cool
before snapping in two.
2. Each student prepares four TLC plates to trial 4 different solvents (work in pairs
when choosing the solvents and using the jars). On each TLC plate, draw a pencil
line across the plate at 1 cm from the bottom of a plate.
Apply a spot of the Part A dye mixture to each of the 4 TLC plates, as shown below.
The spot should be no larger than 2 mm in diameter. The spot should not be close
to the side of the plate.
Dye mixture
spot
3. Dry the spot with the aid of the hairdryer supplied on the side bench.
4. Develop the four chromatograms (TLC plates) by placing them separately in four
jars using one of the solvents chosen from the sequence below, in each jar. Note:
The spot must be above the level of liquid in the development tank, or the
compound will be washed into the bulk eluent.
By working in pairs, students will place each of their TLC plates in the jar at the
same time to develop simultaneously (i.e. two plates per jar). Suggested solvent
sequence is: hexane, chloroform or ethyl acetate, ethanol, acetone.
Cap the jar and let the chromatogram develop. When the solvent front nearly
reaches the top of the silica layer, remove the plate from the jar and mark the
position of the solvent front immediately, then air dry the slide and mark the
22
positions of all the visible spots. Keep all TLC plates and tape them to the Table in
your Report Book.
5. Your demonstrator will discuss with the group the results of separation using
different solvents. Consider if there is any relationship between the polarity of the
solvent and the amount of separation of each component. Which solvent is best at
separating which component of the dye mixture?
Identifying the components of this dye mixture (by comparison with reference
dyes)
Now that the effect of solvent has been considered (to optimize dye mixture
separation), we can proceed to identify the components of the dye mixture.
Note: This procedure is completed individually by you.
6. Now individually, on a fifth TLC plate, draw a pencil line 1 cm from the bottom of
the plate. On this plate you will place 4 spots evenly spaced along the pencil line:
the dye mixture (used in Part A), and the three reference dye solutions that are
provided. Dry the spots, and then develop the TLC plate (step 4 above) using
Eluent A (solvent) as supplied. Eluent A has been optimised for separation of the
dye mixture.
Reference
Dye dyes
mixture
This step enables the components of the dye mixture to be identified by comparison
with the individual reference dyes. Components of the mixture that travel the same
distance (have the save Rf value) as one of the reference dyes can be identified as
being the same as the reference dye.
NOTE: Pairs of students are issued with four (4) jars. If you need use a jar again,
discard the solvent in the appropriate solvent waste bottle in fume cupboard and
rinse jar with a small amount of the new solvent that you intend to use.
7. Students record the results from the Step (6) chromatogram in their Report Book.
Tape this TLC plate in your Report Book.
23
PART A Questions
Results and Discussion

(i) Identify the no. of observed spots after TLC in dye mixture.
(ii) Visually compare spots in the mixture with known dyes (on same plate) and
state which of these known dyes are likely to be part of the mixture.
(iii) Comment on the ability of Eluent A (solvent) to separate components of the dye
mixture.
(iv) Which of the solvents or solvent mixtures you tried gave you the best separation of the
spots from the dye mixture in Part A?
Part A General Questions

i) What is polarity when considering molecules?
ii) A mixture of a polar dye and less polar dye needs to be separated by TLC, circle which
of the following two solvents would be more suitable: acetone or hexane?
iii) What general conclusions can you make about the relationship between the Rf and
solvent polarity?
iv) Do you get more than one spot for any of the dyes in Part A – if so, why?
24
PART B. EXTRACTION AND IDENTIFICATION OF THE COLOURING
COMPOUNDS (DYES) FOUND IN BROWN M&M®S
INTRODUCTION
The colour of food is an integral part of our culture and enjoyment of life. Who would deny
the mouth-watering appeal of a deep-pink strawberry ice cream on a hot summer's day or a
cold glass of a favourite soft drink?
Even early civilizations such as the Romans recognized that people "eat with their eyes" as
well as their palates. Saffron and other spices were often used to provide a rich yellow colour
to various foods. Butter has been coloured yellow as far back as the 1300s.
Food colour additives are dyes, pigments or substances that impart colour when applied to
a food, drug, cosmetic, or the human body. The Food and Drug Administration (FDA) is
responsible for regulating all colour additives used in the United States while in Australia,
this is overseen by Food Standards Australia New Zealand (FSANZ). All colour additives
permitted for use in foods are classified as either "exempt from certification" or "certifiable".
Colour additives that are exempt from certification include pigments that are derived from
natural sources such as vegetables, minerals or animals, and man-made counterparts of
natural derivatives.
Certifiable colour additives are man-made, with each batch being tested by the manufacturer
and the FDA. This "approval" process, known as colour additive certification, assures the
safety, quality, consistency and strength of the colour additive.
There are nine certified colours approved for use in food in the United States. Five can be
found in M&M® candies; these are listed in a copy of the nutrition panel below.
25
Structures of SOME Common Food Dyes:
Green No. 3 OH
Blue No.1 SO3Na
N(C2H5)CH2 -O SO3-
3S
SO3-
C
N(C2H5)CH2
N N
SO3Na
Colour - Bright Blue

Common Food Uses - Beverages, dairy Colour - Fast Green FCF
products, powders, jellies, confections, Common Food Uses – Tinned peas,
condiments, icing. vegetables, jellies, sauces, fish, dessert.
Red No.40 OCH3 HO
NaO3S N N
SO3Na
Yellow No.5
H 3C HO
N
SO3Na NaO3S N N
Colour - Orange-red NaOOC

Common Food Uses - Gelatins, puddings, Colour - Lemon-yellow
dairy products, confections, beverages, Common Food Uses - Custards, beverages,
condiments. ice-cream, confections, preserves, cereals.
Yellow No.6 HO
NaO3S N N
SO3Na
Colour - Orange
Common Food Uses - Cereals, baked goods,
snack foods, ice-cream, beverages, dessert
powders, confections
26
CHEMICAL DETECTIVE -You are working for a rival chocolate company who want to
develop a new product, B&Bs, of brown M&M® like sweets. You are asked to
determine the dyes used to colour the brown M&M®s.
You can use thin layer chromatography (TLC) to separate the food dyes that make up
the shell coating of brown M&M®s and then by comparing your results with the Rf
values and colours of several approved food dyes, you will be able to identify the
number and types of dyes used in the brown coating. Here are several FD&C (Food,
Drug and Cosmetic) approved food dyes in common use in our foods.
Dyes supplied:
FD&C Dye Common Name

FD&C Blue No.1 Brilliant blue FCF
FD&C Red No.40 Allura red AC
FD&C Yellow No.5 Tartrazine
FD&C Yellow No.6 Sunset yellow
FD&C Green No.3 Fast green FCF
M&M®s supplied: Only brown ones… DO NOT CONSUME
27
PROCEDURE – Part B
Ensure that you have pre-prepared a sufficient number of spotting glass

capillaries.
Prepare a solution of the brown M&M ® s coating.
(1) Place four brown M&M ® s into a 50 ml beaker.
(2) Then, they add 2 ml of a 1:1 mixture of water and ethanol (supplied on shelf) to
the beaker.
(3) Swirl the solvent for approximately 1 minute until the candy coating has
dissolved. Remove the M&M ® s from the solvent well before the chocolate
centre has been exposed (the surface of the coating will start to look
mottled (marked with spots or smears).
Prepare two TLC plates.
(4) As before, you draw a horizontal line 1 cm from the bottom of two TLC plates with
a pencil (as shown below). On Plate 1 there will be 4 spots (illustrated below).
Place 4 evenly spaced pencil dots along the horizontal line to help spot the dyes.
On the second plate (Plate 2) there will be 3 spots. Place 3 evenly spaced pencil
dots along the horizontal line to help spot the dyes. Ensure that the spots are not
too close to the edge of the plate.
Plate 1 Plate 2
Key
Brown
Brown M&M Brown M&M dye spot
M&M dye spot
dye spot 5 FD&C dyes spots
(5) On both Plates 1 & 2, apply a single spot of the extracted brown dye. The brown
dye solution is not very concentrated so you will need to spot the solution several
times (repeat spotting on the same spot) to obtain a sufficiently dark spot. It is
important to dry each spot (with hair dryer) between applications of the brown
solution to maintain as small and concentrated a spot as possible. Try to keep
your spots within 2 mm in diameter.
On Plate 1 also apply three of the five FD&C dyes supplied. In brief, note (with
pencil) the number of the dye under the spot.
28
(6) On Plate 2, spot the remaining two FD&C dye solutions supplied. In brief, note
(with pencil) the number of the dye under the spot.
Dry the spots thoroughly with the hairdryer provided by your demonstrator on
the side bench.
(7) Develop the chromatograms using Eluent B (solvent) provided and record your
results on your Report Book.
Part B General Questions
i) What is the mobile phase in this experiment?

ii) What is the stationary phase in this experiment?
iii) Why was a pencil used to mark the TLC plates rather than a pen or marker?
iv) Why should we not use water as the solvent (Part B)?
CLEANUP
Place any used spotting capillaries, unwanted TLC plates and contaminated
broken glass in white solid toxic waste cans provided on each bench or into
the white solid toxic waste buckets in the fume cupboard.
Discard Eluent A, Eluent B and chloroform solvents into the Chlorinated Waste bottle
located in the fume cupboard. Discard all other solvents (toluene, ethyl acetate,
acetone, ethanol, & methanol), into the hydrocarbon liquid waste bottle located in the
fume cupboard.
TLC jars are to be rinsed with a small amount of acetone into Acetone Waste bottles
and left on the shelf, directly above YOUR bench with the lids off to dry.
Discard any clean (uncontaminated) broken glass into the dedicated broken glass
bins located in the lab
Sign the “Sign-Off” sheet when you have checked with your demonstrator and they
are satisfied with your clean up.
29
30
NAME DATE
Student No: LAB DAY+GROUP
EXPERIMENT 1: Report Book
TLC & M&M®s
PART A. Separation of Dye Mixture by TLC
Summarize your results in this Part A Table with fully labeled diagrams. Include all
spots, their colours and their retention values for each solvent system.
Part A Table Distance Travelled Rf Value of Spot TLC Plate

by Spot (cm) (taped)
Solvent 1 Red: Red:
Yellow: Yellow:
Blue: Blue:
Solvent 2 Red: Red:
Yellow: Yellow:
Blue: Blue:
Solvent 3 Red: Red:
Yellow: Yellow:
Blue: Blue:
Solvent 4 Red: Red:
Yellow: Yellow:
Blue: Blue:
31
NAME DATE
PART A Results and Discussion & Questions:
TLC of Dye Mixture in Eluent A against 3 Reference Dyes (Part A, Steps 6 & 7)
i) Identify the no. of observed spots after TLC in dye mixture. ____________
ii) Visually compare spots in the mixture with known dyes (on same plate) and state
which of these known dyes are likely to be part of the mixture.
__________________________________________________________________
__________________________________________________________________
_________________________________________________________________
iii) Comment on Eluent A’s ability to separate components.
iv) Which of the solvents or solvent mixtures, you tried, gave you the best separation of
the spots from the dye mixture in Part A?
Part A General Questions:
i) What is polarity, when considering molecules?
ii) A mixture of a polar dye and less polar dye needs to be separated by TLC, circle
which of the following two solvents would be more suitable: acetone or hexane?
iii) What general conclusions can you make about the relationship between the Rf and
solvent polarity?
iv) Do you get more than one spot for any of the dyes in Part A – if so, why?
32
NAME DATE
PART B. Extraction and Identification of Colouring Matter (dyes) found in

Brown M&M®s
Summarize your results in a fully labeled diagram. Calculate the Rf value for each
dye spot.
Distance Travelled by Spot
FD&C Colour and Number Rf Value of Spot
(cm)
TLC Plate Diagram showing colours in Brown M&M ® s
Distance
Colour of Spot Travelled by Spot Rf Value of Spot
(cm)
\ Brown M&M ® s Coating contains the following

colours:
_____________________________________________
Part B Question 2:
i) What is the mobile phase in this experiment?
ii) What is the stationary phase in this experiment?
iii) Why was a pencil used to mark the TLC plates rather than a pen or marker?
iv) Why should we not use water as the solvent (Part B)?
33
NAME DATE
34
EXPERIMENT 2
SOLUBILITY OF SALTS

To introduce students to methods for identifying ions dissolved in solution. To observe and
record any changes that occur upon the mixing of ionic solutions and to express these
observations in the form of balanced chemical equations. Use the observations of this
experiment to make general predictions about the solubility of ionic species.
SKILLS IN FOCUS
• Use observation and critical thinking skills – i.e. to draw conclusions from the
results of several reactions.
• Write and balance chemical equations that describe the result of mixing
aqueous ionic solutions.
• Understanding solubility.
• Use solubility tests and a flame test to determine the identity of three unknown
solutions (qualitative tests).
• Further practise of the safe use of a Bunsen burner.
• Familiarity with polyatomic ions.
REMEMBER FOR WORKSHOP TESTS

• How to balance equations!
• Recall the solubility rules for Ag+, Ba2+, SO42- and Cl- ions.
• Recall the names, formula and charges on the common ions (in Table 1.1 below)
• How to name ionic solids
35
CHEMICAL ALERT
(Risk Assessment)
Substances: 0.1 M Barium nitrate, Ba(NO3)2, 2.6 g per 100 ml solution
0.1 M Calcium nitrate, Ca(NO3)2•4H2O, 2.4 g per 100 ml solution
0.1 M Copper(II) nitrate, Cu(NO3)2•3H2O, 2.4 g per 100 ml solution
0.1 M Iron(III) nitrate, Fe(NO3)3•9H2O, 4.0 g per 100 ml solution
0.1 M Lead nitrate, Pb(NO3)2, 3.3 g per 100 ml solution
0.1 M Potassium nitrate, KNO3, 1.0 g per 100 ml solution
0.1 M Silver nitrate, AgNO3, 1.7 g per 100 ml solution
0.1 M Zinc nitrate, Zn(NO3)2•6H2O, 3.0 g per 100 ml solution
0.1 M Sodium carbonate, Na2CO3.H2O, 1.2 g per 100 ml solution
0.1 M Sodium chloride, NaCl, 0.6 g per 100 ml solution
0.1 M Sodium hydroxide, NaOH, 0.4 g per 100 ml solution
0.1 M Sodium phosphate, Na3PO4•H2O, 1.4 g per 100 ml solution
0.1 M Sodium sulfate, Na2SO4•10H2O, 3.2 g per 100 ml solution
0.1 M Sodium iodide, NaI, 1.4 g per 100 ml solution
0.1 M Sodium oxalate, Na2C2O4, 1.3 g per 100 ml solution
0.1 M Sodium thiosulfate, Na2S2O3•5H2O, 2.5 g per 100 ml solution
Hazards: Substance Rating

0.1M barium nitrate, Ba(NO3)2 T(2), B(2)
0.1M calcium nitrate, Ca(NO3)2•4H2O NH
0.1M copper(II) nitrate, Cu(NO3)2•3H2O B(1)
0.1M iron(III) nitrate, Fe(NO3)3•9H2O T(2), B(2)
0.1M lead nitrate, Pb(NO3)2 T(2), C(3)
0.1M potassium nitrate, KNO3 T(2), B(1)
0.1M silver nitrate, AgNO3 T(1)
0.1M zinc nitrate, Zn(NO3)2•6H2O T(2)
0.1M sodium carbonate, Na2CO3.H2O B(1)
0.1 M Sodium chloride, NaCl NH
0.1 M Sodium hydroxide, NaOH B(3)
0.1 M Sodium phosphate, Na3PO4•H2O T(2), C(2)
0.1 M Sodium sulfate, Na2SO4•10H2O NH
0.1 M Sodium iodide, NaI B(1)
0.1 M Sodium oxalate, Na2C2O4 NH
0.1 M Sodium thiosulfate, Na2S2O3•5H2O NH
10 M HCl B(3), C(2)
NH = Non Hazardous
F=Flammability; T=Toxicity; B=Body Contact; R=Reactivity; C=Chronic
Protection: Safety glasses are required.

Disposable gloves are available
1. INTRODUCTION
1.1 General
In chemistry, a chemical reaction is said to have occurred when reactants are transformed
into products. Chemical reactions are described by equations. For example, the reaction of
nitrogen (N2) with hydrogen (H2) to form ammonia (NH3) is described by the following
balanced equation:
N2(g) + 3H2(g) 2NH3(g)
36
In the following experiment you will observe a number of chemical reactions. You will record
your observations and draw conclusions regarding the chemical change that has taken
place, based on these observations. You will then express these changes in the form of
balanced chemical equations. These fundamental skills of observation, accurate recording
and interpretation are essential for the practical chemist and scientist.
1.2 Aqueous Solution Chemistry

Many chemical reactions (and nearly all biological) reactions occur among species dissolved
in water. In fact, if we are to understand the chemistry that takes place in the atmosphere,
oceans, rivers, groundwater and animals (including humans) an understanding of aqueous
chemistry is absolutely vital.
Everyone has at some time dissolved table salt (NaCl) in water. How many have ever really
considered how this occurs? If we are to understand the chemistry that occurs in water we
need to consider the species present in aqueous solution.
Solid NaCl is an ionic solid [Figure 1]. The Na+ cations (yellow) and the Cl- anions (green)
arrange themselves in a lattice (regular repeating unit). The cations and anions are held
together by the strong electrostatic attraction of the negative charges for positive charges.
Water is a polar molecule [Figure 2]. This means the molecule, as a whole, possesses a
slightly negative end (d-) and a slightly positive end (d+).
d-
d+ d+
Figure 1: Section of ionic lattice of NaCl. Figure 2: Water molecule.
It is for this reason that we say water possesses a permanent dipole (it is polar). The
reason the ionic solid NaCl appears to “disappear” when dissolved in water, is because
the water molecules are able to surround (solvate) the individual ions on the surface
of the crystalline NaCl. These individually, solvated ions are then able to be “washed”
away and move freely through the solution. This is process is known as dissolution.
The following YouTube clip illustrates dissolution of an ionic compound.
https://www.youtube.com/watch?v=xdedxfhcpWo
37
1.3 Useful definitions for solution chemistry
Solution -a homogeneous mixture of two or more substances. A solution
consists of solute(s) + solvent.
Solute - the substance dissolved in the solvent.
Solvent - the liquid that dissolves the solute (in this experiment, water).
Solubility - the maximum amount of solute that will dissolve in an amount solvent,
at a given temperature.
Precipitate - the solid material present in a solution. A solid may settle at the
bottom of a vessel or a solution may appear a little cloudy - in both
cases a precipitate is present.
Ionic solid (salt) - is a substance containing both positively charged (cations) and
negatively charged (anions) species.
Ionic solutions - ionic solids that are dissolved in a solvent (e.g. water).
Ion - a species with a positive or negative charge.
Aqueous solution - a solution where the solvent is water.
1.4 Aqueous Precipitation Reactions

In this experiment you will consider the reactions of aqueous solutions, specifically
precipitation reactions. You will be supplied with several ionic solutions. As stated above,
these contain solvated cations and anions.
When two such ionic solutions are reacted together, the resulting products reflect an
exchange of the anions and cations – called an exchange reaction (1). If one or both of the
products is insoluble in water, a solid (precipitate) will form. Equation (2), exchange reaction,
is called a precipitation reaction.
AB (aq) + CD (aq) → AD (s or aq) + CB (s or aq) (1)
AgNO3 (aq) + NaCl (aq) → AgCl (s) + NaNO3 (aq) (2)
If a precipitate forms on the mixing of two such ionic solutions this generally indicates that
the ion-ion interaction of the solid is favoured over the ion-dipole interaction of the ions with
water (i.e. the ions would prefer to exist in the solid state rather than in solution).
The following experiment is concerned with determining the solubility, in water, of common
combinations of cations and anions. The observations made from your experiments will allow
you to devise solubility rules and thus allow you to predict which ionic compounds will be
insoluble and thus form a precipitate in an appropriate exchange reaction.
38
Writing and Balancing Ionic Equations
1. Identify the ions present in a solution given the ionic formula.
Example: An 0.1 M Ba(NO3)2 solution contains Ba2+ cations and NO3- anions.
To assist you a list of common polyatomic ions is provided in the following table
(you are also expected to know the common atomic ions that form e.g. halogens:
F, Cl, Br and I (for example) form halide ions of charge -1 : F-, Cl-, Br- and I-;
hydrogen forms a H+ cation, and Group I metals form +1 cations).
2. Be able to write a chemical equation containing the correct chemical formulae for
all the reactants and products in each reaction. See what is required in Chemical
Reactions below
Example: Ba(NO3)2 + Na3PO4 Ba3(PO4)2 + NaNO3
3. Balance each of the reactants and products so that each compound is neutral,
i.e. has an overall charge of zero. Once this is complete, identify the correct
physical state of each compound and include the state in your written equations
(e.g. (g) for gas, (l) for liquid, (s) for solid, or (aq) for aqueous species)
Example: Ba(NO3)2(aq) + Na3PO4(aq) Ba3(PO4)2(s) + NaNO3(aq)
4. Be able to balance chemical equations (i.e. they should obey the Conservation
of Mass).
Example: 3 Ba(NO3)2(aq) + 2 Na3PO4(aq) Ba3(PO4)2(s) + 6 NaNO3(aq)
Table 1.1 Names and formulas of common polyatomic ions.

Name Formula Name Formula
Ammonium NH4+ Perchlorate ClO4-
Permanganate MnO4-
Acetate CH3COO- Thiocyanate SCN-
Bicarbonate (Hydrogen carbonate) HCO3-
Bisulfate (Hydrogen sulfate) HSO4- Carbonate CO32-
Bisulfite (Hydrogen sulfite) HSO3- Chromate CrO42-
Chlorate ClO3- Dichromate Cr2O72-
Chlorite ClO2- Hydrogen phosphate HPO42-
Cyanide CN- Oxalate C2O42-
Dihydrogen phosphate H2PO4- Peroxide O22-
Hydroxide OH- Sulfate SO42-
Hypochlorite ClO- Sulfite SO32-
Nitrate NO3-
Nitrite NO2- Phosphate PO43-
39
PART A - PRECIPITATION REACTIONS OF AQUEOUS SALT SOLUTIONS
PROCEDURE
All ionic solutions are available in dropper bottles, at 0.1 M concentration.
There are two copies of the data grid in the student laboratory report book. The first
is for recording observations and results, the last page should be detached to use as
a template in Step 1.
Drops of the appropriate solutions will be put into each square of the grid (onto the
plastic sheet). Students need to be careful to avoid cross-contamination. Students
should finish with an 8x8 grid of solubility results from which they can draw conclusions.
(1) Place a clean plastic sheet over the data grid (from your laboratory report book). The
data grid includes sodium salts across the top horizontal row (labelled 1-8) and a series
of nitrate salts in the vertical column (labelled A-H).
(2) To each horizontal row A (ie A1 to A8), add 1 drop of 0.1 M silver nitrate solution
(AgNO3).
Ø Put the drop in the centre of the box on the grid to avoid the risk of drops being
contaminated by other solutions.
Ø Dropper must not touch the plastic sheet or other drops.
(3) Repeat Step (2) for each row (ie B to H) by adding 1 drop of the following:
To Row B, add 0.1 M barium nitrate, Ba(NO3)2.
To Row C, add 0.1 M calcium nitrate, Ca(NO3)2.
To Row D, add 0.1 M copper(II) nitrate, Cu(NO3)2.
To Row E, add 0.1 M zinc nitrate, Zn(NO3)2.
To Row F, add 0.1 M lead(II) nitrate, Pb(NO3)2.
To Row G, add 0.1 M potassium nitrate, KNO3.
To Row H, add 0.1 M iron(III) nitrate, Fe(NO3)3.
40
You should now have a drop in each box on the grid. These are the cations
(positively charged ions) with a common anion of a nitrate. Now it is time to add
the various anions (in columns) to the existing drop of cation solution in each box
in the grid.
(4) In each box in vertical Column 1 (A1 to H1), add a drop of 0.1 M sodium
carbonate, Na2CO3. The added drop must mix with the drop of solution that was
placed in the box in Steps 2-3.
Ø The dropper must not touch the plastic sheet or other drops to avoid cross-
contamination.
(5) As in Step 4, add 2-3 drops of the solutions listed to each of the vertical columns
indicated:
To Column 2, add 0.1 M sodium chloride, NaCl.
To Column 3, add 0.1 M sodium hydroxide, NaOH.
To Column 4, add 0.1 M sodium sulfate, Na2SO4.
To Column 5, add 0.1 M sodium phosphate, Na3PO4.
To Column 6, add 0.1 M sodium oxalate, Na2C2O4.
To Column 7, add 0.1 M sodium iodide, NaI.
To Column 8, add 0.1 M sodium thiosulfate, Na2S2O3.
(6) Observe carefully (observations should be made and recorded as solutions are
combined) to determine which combinations of solutions produced precipitates. In your
data table, record each combination of ions that showed the formation of a precipitate.
Record the color, texture, and other observations for each.
It is recommended to use the following labels/notation in your observations:
NR - no reaction observed
PPT – a precipitate was observed.
colour - note the colour of any precipitate or solution colour. Eg, light blue.
Cleanup
Rinse plastic sheet with water and detergent to remove remaining spots and
wipe dry with paper towel. Place acetate sheet back on your bench.
Discard any contaminated paper towel or broken glass into the toxic solid
waste bucket located in the fume cupboards and side benches. Ensure
students wipe clean the bench before they start the analysis and questions.
41
Data Analysis
1. All of the cation solutions are nitrates. What can you conclude about the general solubility
of nitrates in water?
2. The anion solutions (Columns 1-8) were all sodium salts. What can you conclude about
the general solubility of sodium salts in water?
3. Which cation(s) formed precipitates with nearly all (7 out of 8) the anions?
4. It is known that all chlorides are soluble except silver chloride. How do your results
compare with this expectation?
5. Analyse your data with respect to the solubility of carbonates, chlorides, sulfates, and
iodides, with the aim of creating similar generalised solubility rules (5 or more similar
outcomes out of 8).
6. Repeat the analysis of your data to create a generalized rule (5 or more similar outcomes
out of 8) for the solubility of each of the metallic cations: lead(II), Pb2+; calcium, Ca2+,
copper(II), Cu2+; and zinc, Zn2+.
Chemical Reactions
7. Write a balanced chemical reaction (net ionic equations) all for precipitate forming
reactions of (i) Fe3+ and (ii) Cu2+ including the physical state of each of the reactants
and products.
Questions
8. Draw a picture of a solvated sodium ion (Na+) and a solvated chloride ion (Cl-).
9. The anion solutions (Columns 1-8) were all sodium salts. Could potassium salts be
substituted for the sodium salts? Explain your answer.
10. As an environmental chemist you want to purify water which is contaminated with lead
nitrate. Describe how you would use the general solubility rules you have derived to purify
the water. (Hint: think precipitation).
11. Use the chemical species in the following table and the solubility rules you have just
derived to answer these questions.
Ag+ S Ca2+ NO3-
SO42- K+ O2 Pb2+
C2O42- Cl- all none
(a) Which are cations?
(b) Which are not ions?
(c) Which will precipitate with 0.1 M lead(II) ions?
(d) Which will precipitate with 0.1 M potassium ions?
(e) Which will not precipitate with 0.1 M silver ions?
(f) Which will precipitate with 0.1 M sulfate ions?
(g) Which will precipitate with 0.1 M nitrate ions?
(h) Which will precipitate with 0.1 M calcium ions?
(i) Which will precipitate with 0.1 M chloride ions
42
PART B: CHEMICAL DETECTIVE - IDENTIFICATION OF UNKNOWN SALT
SOLUTIONS
INTRODUCTION
You have just started work as a chemical analyst, working for a water authority. One
of your jobs is to note down exact observations about the appearance of unknown
solutions which have been taken from waste output pipes of several factories. You
will do tests to detect certain substances, such as metals and sulfates.
Chemical analysis can be divided into two categories; qualitative analysis – what is present
and quantitative analysis – how much is present. In this investigation you will learn to apply
principles of qualitative analysis for some common metal ions (i.e. elements that typically
form cations in solution). This experiment is part of a classical analysis scheme developed
by chemists of past generations to identify unknowns. It uses solubility rules and a flame
test.
Solutions: A, B and C contain one of the following dissolved ionic solids: barium nitrate,
Ba(NO3)2, potassium nitrate, KNO3, or copper nitrate, Cu(NO3)2.
Your aim is to identify the ions present in solutions A, B and C by observing and analysing
the outcomes of the following tests:
I. The reaction of each solution with sodium hydroxide (NaOH). Observe the link to the
solubility rule: All hydroxides are insoluble except those of Na+, K+, NH4+ and Ba2+.
II. The reaction of each solution with sodium sulphate (Na2SO4). Observe the link to the
solubility rule: All sulphate salts are soluble except those of Ca2+, Ba2+ and Pb2+.
III. Flame Test - TAKE CARE. Several cations can be detected and identified by the
colour they emit when placed in a flame. Instead of doing a flame test on the unknown
solutions here you will use the solid for the flame test (brighter colour). Ideally you
would use the solution for the flame test. Observe the colour emitted when a drop of
each solution is heated in a Bunsen burner flame.
Metal Cation Flame Test Colour

lithium crimson red
sodium yellow-orange
potassium pale lilac
calcium brick red
barium yellow-green
copper emerald green
Perform the tests by following the scheme below and record your observations, equations
and conclusions in the report sheet provided.
Cleanup
Rinse clean, your plastic sheet in the sink at the end of the bench. Rinse with tap
water. Wipe your bench clean. Sign the demonstrator “sign-off” sheet before
leaving.
43
TEST SCHEME:
Solutions: A, B and C
containing nitrate salts of
Ba2+, K+ and Cu2+
On a new clean and dry acetate sheet, All hydroxides are

combine a drop of each solution with a
drop of sodium hydroxide solution insoluble except those of
Na+, K+, NH4+ and Ba2+.
Results
Solution A:
Solution B:
Solution C:
Solutions A, B and C
Ba2+, K+ and Cu2+
On your clean and dry acetate sheet, All sulphate salts are
combine a drop of each solution with a
drop of sodium sulphate solution soluble except those of
Ca2+, Ba2+ and Pb2+.
Results
Solution A:
Solution B:
Solution C:
Solutions A, B and C
Ba2+, K+ and Cu2+
Dip the wire loop into the jar labelled 10M HCl (fume cupboard), Metal Flame
rise with distilled water and place in a blue Bunsen flame until it Cation Test
glows orange-red. Allow wire to cool before each dipping. Do this a Colour
few times until the wire is clean. Dip wire into UNKNOWN solid A lithium crimson
red
and observe colour when placed in flame. Repeat this step twice sodium yellow-
more. Repeat the test procedure with UNKNOWN solid B and C orange
remembering to acid clean and flame the Nichrome wire between potassium pale lilac
each solid. calcium brick red
barium yellow-
green
copper emerald
green
Results
Solution A:
Solution B:
Solution C:
44
NAME DATE
EXPERIMENT 2: Report Sheet
Solubility
Data Analysis
1. All of the cation solutions are nitrates. What can you conclude about the general
solubility of sodium salts in water?
2. The anion solutions (columns 1-8) were all sodium salts. What can you conclude about
the general solubility of nitrates in water?
3. Which cation(s) formed precipitates with nearly all the anions?
4. It is concluded that all chlorides are soluble except silver chloride. How do your results
compare with this conclusion?
5. Use your data to derive a general solubility rule (5 or more similar outcomes out of 8)
carbonates, chlorides, sulfates, and iodides.
Carbonates:
Chlorides:
Sulfates:
Iodides:
45
NAME DATE
6. Repeat the analysis of the data to create a generalized rule for the solubility of each of
the metallic cations: lead(II), Pb2+; calcium, Ca2+, copper(II), Cu2+; and zinc, Zn2+.
Lead(II):
Calcium:
Copper(II):
Zinc:
7. Equations for the reactions where there is an insoluble product formation involving:
(i) Ferric nitrate (Fe3+)
46
NAME DATE
(ii) Copper nitrate (Cu2+)
QUESTIONS
1. Draw a picture of a solvated sodium ion and a solvated chloride ion.
2. The anion solutions (Columns 1-8) were all sodium salts. Could potassium salts be
substituted for the sodium salts? Explain your answer.
47
NAME DATE
3. As an environmental chemist you want to purify water which is contaminated with lead
nitrate. Describe how you would use the general solubility rules you have derived to purify
the water. (Hint: think precipitation).
4. Use the terms in the following table to answer these questions.

Ag+ S Ca2+ NO3-
SO42- K+ O2 Pb2+
C2O42- Cl- all none
(a) Which are cations?

(b) Which are not ions?
(c) Which will precipitate with 0.1 M lead(II) ions?
(d) Which will precipitate with 0.1 M potassium ions?
(e) Which will not precipitate with 0.1 M silver ions?
(f) Which will precipitate with 0.1 M sulfate ions?
(g) Which will precipitate with 0.1 M nitrate ions?
(h) Which will precipitate with 0.1 M calcium ions?
(i) Which will precipitate with 0.1 M chloride ions?
48
NAME DATE
Observations 49
NAME DATE
PART B: Identification of Unknown Salt Solutions
Unknown Solution A
Test Observation Equation for Any Precipitation Reaction*

Did / Did Not
Reaction with NaOH
Precipitate (circle)
Did / Did Not
Reaction with Na2SO4
Flame Colour
Conclusion: Solution A is __________________
Unknown Solution B

Did / Did Not
Reaction with NaOH
Did / Did Not

Flame Colour
Conclusion: Solution B is __________________
Unknown Solution C

Did / Did Not
Reaction with NaOH
Did / Did Not

Flame Colour
Conclusion: Solution C is __________________
* Use the Solubility Rules given to write balanced equations for selected
precipitation reaction
50
NAME DATE
51
NAME DATE
52
EXPERIMENT 4
ORGANIC FAMILIES – REACTIONS AND IDENTIFICATION OF

FUNCTIONAL GROUPS

Functional groups are groups of atoms found within molecules that are involved in, or
responsible for, the chemical reactions characteristic of those molecules. This experiment
is designed to familiarize you with several common organic functional groups, including
their representation and their chemical reactions. You will also investigate some reactions
typical of these functional groups that are also described in your organic chemistry
lectures.
SKILLS IN FOCUS
• Observation and critical thinking skills – drawing conclusions from the results of
several organic reactions.
• To provide further experience in writing and balancing reactions.
• Practise identifying and naming functional groups present in organic compounds
from their structures.
• Recognising the role functional groups play in an organic compound’s reactivity.
• Waste disposal of organic substances.

• Identify functional groups present in molecules (examinable)
• Interpret (or draw) line structures of organic compounds
• Recall selected general reactions of functional groups including electrophilic
addition
53
CHEMICAL ALERT
(Risk Assessment)
Substances: bromine water, cyclohexane, cyclohexene, Lucas Reagent (zinc chloride in conc. hydrochloric
acid), 2-methyl-2-butanol, 2-pentanol, 1-pentanol, octanal, pentanal, pentan-2-one, iso butyl
methyl ketone, 2,4-dinitrophenylhydrazine, butyraldehyde, Schiff’s Reagent, 5% acetic acid
solution, benzoic acid (C6H5COOH)
Hazards: Bromine has a toxicity and contact rating of 4, and a reactivity and chronic rating of 2.
Cyclohexane has a flammability rating of 3, a contact and toxicity rating of 2.
Cyclohexene has a flammability rating of 3, a contact and toxicity rating of 2.
Lucas Reagent has a contact rating of 4 and a toxicity rating of 4
2-Methyl-2-butanol has a flammability rating of 4 and a toxicity and contact rating of 2.
2-Pentanol has a flammability rating of 2 and a toxicity rating of 2 and contact rating of 3.
1-Pentanol has a flammability rating of 2 and a toxicity rating of 2 and contact rating of 3.
Octanal has a flammability rating of 2 and a toxicity rating of 2.
Pentanal has a flammability rating of 3 and a toxicity rating of 2.
Pentan-2-one has a flammability rating of 3 and a toxicity rating of 2.
Iso-butyl methyl ketone has a flammability rating of 3 and a toxicity rating of 2.
Benzoic acid has a toxicity, contact and chronic rating of 2.
2,4-Dintrophenylhydrazine has a flammability rating of 3 and a toxicity rating of 3 and contact
rating of 3.
Schiff’s Reagent has a toxicity rating of 3 and a contact rating of 4
Protection: Read ALL safety warnings on coded solutions and unknown solids.
Safety glasses MUST be worn.
Avoid all contact with bromine. Disposable gloves MUST be worn. Carry out all work with
bromine in a fume cupboard. Risk: C2
INTRODUCTION
We recognise our friends by their facial appearance, their characteristic voice on the phone
etc. Likewise, functional groups on organic molecules are a specific group of atoms that
characterise that molecule and undergo the same or similar chemical reactions regardless
of the size of the rest of the molecule. An example of a functional group is the alcohol group,
–OH. There are characteristic reactions of alcohols that generally most compounds
containing this group will undergo. Two different alcohols methanol and 1-propanol are
shown below.
H H H
H O H C O H
C H C C
H H H H H
methanol 1-propanol
Some functional groups participate in acid-base chemistry: amines are weak bases while
carboxylic acids and phenols are weak acids. Some functional groups participate in redox
chemistry: aldehydes and some alcohols are readily oxidised while aldehydes and ketones
are readily reduced. In substitution reactions, some functional groups act as nucleophiles
(donating electrons) while others are electrophiles (accepting electrons). Finally, multiple
bonds, as in alkenes and alkynes are required for addition reactions. See Table 1 below for
examples.
http://www.youtube.com/watch?v=nMTQKBn2Iss
54
Table 1: Some reactions of functional groups
REACTION TYPE EXAMPLE(S)
Acid/Base
Oxidation
(addition of oxygen
OR loss of hydrogen)
Reduction
(addition of hydrogen
OR loss of oxygen)
Substitution
Addition
55
This predictable reactivity allows a chemist to attempt a variety of reactions on an organic
compound and determine what functional group(s) is/are present. To use any reaction as a
test for a functional group, it is necessary for the product mixture to appear significantly
different from the reactants. This may be due to the formation of a precipitate or coloured
product, or it may be due to the consumption of a solid or coloured reactant. It is good
practice to employ positive and negative controls to ensure that each test has been
performed correctly.
In this experiment, you will perform several distinguishing tests so that you are able to
understand the specific reactivity of certain functional groups. Table 2 below lists some
common organic functional groups you will have encountered in your course work.
56
Table 1: Some Common Organic Functional Groups
Chemical Structural
Group Formula Prefix Suffix Example
Class Formula
Alkane Alkyl RH alkyl- -ane

ethane
Alkene Alkenyl R2C=CR2 alkenyl- -ene
ethylene
Alkyne Alkynyl RC≡CR' alkynyl- -yne acetylene
H3C CH3
CH3
C
Benzene Derivative Phenyl RC6H5 phenyl- -benzene HC CH
HC CH
C
H 2-phenylpropane
Haloalkane Halo RX R─X halo- alkyl halide chloroethane
Alcohol Hydroxyl ROH hydroxy- -ol

methanol
Ketone Carbonyl RCOR' keto- -one methylethyl ketone

butanone
Aldehyde Aldehyde RCHO aldo- -al

acetaldehyde
ethanal
Carboxylic Acid Carboxyl RCOOH carboxy- -oic acid

acetic acid
ethanoic acid
Ester Ester RCOOR' alkyl alkanoate

ethyl butanoate
Ether Ether ROR' alkoxy- -ether

diethyl ether
Amide Carboxamide RCONR2 carboxamido- -amide

acetamide
ethanamide
Primary Amine RNH2 amino- -amine

methylamine
Amine Secondary AmineR2NH amino- -amine

dimethylamine
Tertiary Amine R3N amino- -amine

trimethylamine
Peroxide Peroxy ROOR peroxy- alkyl peroxide di-tertbutyl peroxide
Nitro Compound Nitro RNO2 nitro- nitromethane
57
The functional groups that are studied in this experiment are:
alkanes aldehydes Before the experimental session, you must familiarise
alkenes ketones yourself with the chemical structures and names of the
alcohols carboxylic acids organic chemicals that will be used in this investigation.
esters
PROCEDURES
PART A REACTIONS OF ALKANES AND ALKENES
Most halogens (chlorine (Cl2), bromine (Br2) and iodine (I2)) react readily with carbon-carbon
multiple bonds that are not part of an aromatic ring, . The products of these reactions are
clear or colourless – just like the organic reactant.
Bromine is typically chosen as the test reagent for double bond containing alkenes and triple
bond containing alkynes because if it reacts, its rich brown/orange colour will disappear. If
the brown/orange colour persists, it is because there are no unsaturated bonds (double) for
the bromine to react with.
The general chemical formula of the halogen addition reaction is:
X
R R’’ R’’
+ X2 R
X
’R R’’’ ’R R’’’
(X = halogens, Br or Cl; R, R’, R’’ or R’’’ = hydrocarbon groups or H )
This type of reaction is labelled as halogenation and an electrophilic addition.
Here you will undertake the reaction of Br2 with:
and
cyclohexane cyclohexene
58
1. Action of Bromine Water – Test for double and triple CC bonds.
Caution: Bromine water is a solution of bromine in water and is highly toxic. It

MUST be kept in the fume cupboard at all times. If bromine water gets on your skin,
wash the affected part with water, quickly and thoroughly, and report to the lab
technician in the prep room. Wear gloves and handle with care!!
Conduct this part of the experiment in the fume cupboard.
(1) Place 5 drops of cyclohexene in a clean micro test-tube in the fume cupboard.
(2) Add 1 drop of bromine water from the dropping bottle in the fume cupboard.
Carefully swirl or shake the mixture.
(3) If the brown/orange colour fades, add more bromine water (1 drop) and shake.
If the colour keeps fading, add further drops of bromine water, one drop at a
time, shaking the test tube after each drop. Use a maximum of 5 drops only.
If too much bromine is added to a solution, a false negative result may be
generated as all the alkene is consumed before the bromine.
(4) Record your observations and equations in your Report Book.
(5) Do not bring the test tube out in the open laboratory. Dispose of the
residue in the halogenated waste container supplied in the fume
cupboard. Rinse the test tube twice with acetone and pour washings in
the same waste container.
(6) Repeat this test with cyclohexane (5 drops in another clean micro test tube).
(7) Record your observations and equations on your Report Book.
(8) Dispose of the experimental waste into the Halogenated Organic Waste
bottle in fume cupboard. Rinse the test tube several times with small
amounts of acetone. Place the rinsings in the Halogenated Organic Waste
bottle also. Leave the test tubes inverted in your rack to dry.
59
PART B DISTINGUISHING TEST FOR PRIMARY, SECONDARY AND
TERTIARY ALCOHOLS
1. Lucas Test for Alcohols
Lucas reagent is a solution of zinc chloride (ZnCl2) in concentrated aqueous HCl.

Tertiary alcohols (in which three carbon atoms are attached to the same carbon as the
–OH group) react immediately with the Lucas reagent producing a cloudy solution due
to the formation of an insoluble alkyl chloride. Secondary alcohols (in which two carbon
atoms are attached to the same carbon as the –OH group) react more slowly (approx.
5 minutes). Primary alcohols (only one carbon atom is attached to the same carbon as
the –OH group) do not react at all.
Primary
ppt. does not appear
Secondary
ppt. appears with in 5 minutes
Tertiary
ppt. appears immediately
Caution: Lucas Reagent contains concentrated hydrochloric acid (HCl). If Lucas

Reagent gets on your skin, wash the affected part with water quickly and
thoroughly, and report to the lab technician in the prep room. Wear gloves and
handle with care!!
Here you will observe the Lucas test for three alcohols: primary, secondary and tertiary.
OH
HO
HO
tert-pentanol 2-pentanol 1-pentanol
(1) Place 5 drops of tert-pentanol (2-methyl-2-butanol) in a clean micro test tube. In

a separate test tube, place 5 drops of 2-pentanol and in a third micro test tube,
place 5 drops of 1-pentanol.
(2) Add 5 drops of Lucas Reagent (ZnCl2 in HCl) to each of the three test tubes and
carefully shake each one.
(3) Record your observations and equations on your Report Book.
60
(4) Dispose of the experimental waste by tipping into Organic Waste bottle in
fume cupboard. Rinse the test tube, several times, with small amounts of
acetone. Place the rinsings in the Organic Waste bottle also. Next, rinse
test tubes with tap water in fume cupboard sink then again with a small
quantity of acetone. Leave the test tubes inverted in your rack to dry.
PART C DISTINGUISHING TESTS FOR ALDEHYDES AND KETONES
The distinguishing tests here are aimed at;

(a) distinguishing aldehydes and ketones from everything else (Eq. 1) and,
(b) distinguishing between aldehydes and ketones (Schiff’s test)
The 2,4-dinitrophenylhydrazine reaction distinguishes aldehydes and ketones from

everything else. If a bright yellow, orange or red precipitate forms, the compound
contains an aldehyde or ketone.
Equation 1: Reaction of aldehyde or ketone with 2,4-dinitrophenylhydrazine
Caution: 2,4-dinitrophenylhydrazine is an irritant. Do not allow it to contact skin

or eyes. If the hydrazine reagent gets on your skin, wash the affected part with
water, quickly and thoroughly, and report to the lab technician in the prep room.
Wear gloves and handle with care!!
61
Test for the Presence of an Aldehyde or Ketone on:
H O OH
O
pentanal pentan-3-one 2-propanol
(1) Add 4 drops of 2,4-dinitrophenylhydrazine reagent to a clean micro test tube.
(2) Add 2 drops of pentaldehyde (pentanal). If a precipitate does not form within 5
minutes, gently warm the test tube in a beaker of hot water, cool and scratch the
inside of the test tube with a glass rod or small metal spatula.
(3) Record your observations and equations on your Report Sheet.
(4) In a separate clean micro test tube, repeat the test using 4 drops of 2,4-
dinitrophenylhydrazine reagent and, this time, 2 drops of the ketone supplied,
pentan-3-one.
(5) Again, record your observations and equations on your Report Book.
(6) Now repeat the test (in a separate clean micro test tube) using 2 drops of 2-
propanol (isopropyl alcohol) to see the colour density in a solution containing an
organic that does not react with the hydrazine reagent.
(7) Again, record your observations and equations on your Report Book.
(8) Dispose of the experimental waste by tipping into Organic Waste bottle in
fume cupboard. Rinse the test tube, several times, with small amounts of
acetone. Place the rinsings in the Organic Waste bottle also. Leave the test
tubes inverted in your rack to dry.
62
2. Schiff’s Test for Aldehydes (distinguishes between aldehydes and
ketones)
Schiff’s reagent is a selective oxidising agent that will only react with aldehydes and
not ketones.
Schiff’s reagent contains an oxidised form of the bright pink dye, fuschin. In this form
the reagent is decolourised (colourless). When the Schiff’s reagent reacts with an
aldehyde, the dye is reduced back to its pink form and the solution turns pink.
Schiff’s Reagent
A Schiff’s test is undertaken on the following:
H O OH
O
pentanal butan-2-one 2-propanol (for comaprison)
(1) In three separate clean micro test tubes, place 3 drops of Schiff’s reagent from
the labelled dropping bottle.
(2) Add 3 drops of an alcohol (isopropyl alcohol) to the first test tube, 3 drops of
pentanal to the second test tube and finally 3 drops of 2-butanone to the third
test tube. Carefully shake each test tube. Let the test tubes sit for 5-10 minutes.
(3) Observe any colour changes and record your findings on your Report Sheet.
Record the chemical names and draw the chemical structures of 2-propanol
(isopropyl alcohol), pentanal and 2-butanone on your Report Book.
(4) Dispose of the experimental waste by tipping into the (Non-Halogen)

Organic Waste bottle in fume cupboard. Rinse the test tube, several times,
with small amounts of acetone. Place the rinsings in the Organic Waste
bottle also. Leave the test tubes inverted in your rack to dry.
63
PART D SODIUM HYDROGEN CARBONATE TEST FOR CARBOXYLIC
ACIDS
Carboxylic acids react with sodium hydrogen carbonate (sodium bicarbonate) to form
a salt and carbon dioxide gas.
O O
+ NaHCO3 + H2O + CO2 (gas)
R OH R O Na
Carboxylic Acid
For budding cooks - baking powder, the combination of sodium bicarbonate

and tartaric acid (a carboxylic acid) causes your baking products, such as muffins, to
rise beautifully as a result of the CO2 gas produced during the baking process.
The reaction of NaHCO3 is undertaken on the following compounds:
O
OH
OH OH
ethanoic acid ethanol
(acetic acid) benzoic acid
(1) Place 5 drops of acetic (ethanoic) acid solution (10% v/v) in a clean micro test
tube.
(2) Add 1 ml saturated sodium hydrogen carbonate (NaHCO3) solution from the
dropping bottle supplied.
(3) Observe whether the solution reacts and gives off a gas (it will produce bubbles
if it does). Record your observations and equations in your Report Book.
(4) In another micro test-tube, repeat the test by adding 1 ml of saturated sodium
hydrogen carbonate (NaHCO3) solution to a small spatula-full of benzoic acid.
Record observations and equations in your Report Book.
64
(5) Again, in a separate micro test tube, repeat the same test (in (4) above, with
using 5 drops of ethanol. Record observations and equations on your Report
Book.
(6) Dispose of the experimental waste by tipping into the Non-Halogenated

Organic Waste bottle in the fume cupboard. Rinse the test tube several
times, with small amounts of acetone. Place the rinsings in the Organic
Waste bottle also. Leave the test tubes inverted in your rack to dry.
PART E TEST FOR ESTER FORMATION - PLEASE REMIND

STUDENTS THAT SMELLING A REACTION IS
STRONGLY DISCOURAGED.
Esters have the structure of R”-COOR. These low boiling, volatile esters are known for
their "fruity" smell and flavour. They are used in artificial flavourings.
In the laboratory, esters can be made by a number of routes. One method is to react
an acid with an alcohol,
carboxylic acid + alcohol à ester + water
In the presence of an acid catalyst, alcohols react with carboxylic acids to produce an
ester and water. This is known as a condensation reaction.
O H+ O
+ ROH + H 2O
”R OH ”R OR
Carboxylic Acid Alcohol Ester
Caution: Extreme care must be used when handling concentrated acids. Please
ensure that you wear gloves and work in the fume cupboard.
The reaction of glacial (anhydrous) acetic (ethanoic) acid is undertaken on the

following compounds:
HO HO
3-methyl butan-1-ol octanol

(isopentyl alcohol)
65
(1) In a clean micro test tube, place 5 drops of isopentyl alcohol (3-methyl butan-1-
ol). In a separate clean test tube, place 5 drops of octanol.
(2) Add 1 drop of concentrated sulfuric acid (H2SO4) to each of the test tubes.
(3) With caution, add 2 drops of glacial acetic acid (CH3COOH) to each of the test
tubes and very carefully swirl the contents of the test tubes.
(4) Gently heat the test tubes by placing them in a beaker of hot water for a few
minutes
(5) Carefully smell the odour of each test tube separately. DO NOT PLACE YOUR
NOSE DIRECTLY OVER THE TEST TUBE. Carefully hand wave over the test
tube opening until you are able to detect a pleasant ester smell.
(5) Can you identify what fruits the esters smells like? Record your findings and
equations in your Report Book.
(6) Dispose of the experimental waste by tipping into the Non-Halogenated

Organic Waste bottle in the fume cupboard. Rinse the test tube, several
times, with small amounts of acetone. Place the rinsings in the Organic
Waste bottle also. Leave the test tubes inverted in your rack to dry.
PART F THE SOLUBILITY OF ALCOHOLS
“Like dissolve like” is a useful simple rule that we encountered in Experiment 1.

Alcohols are organic compounds that contain a polar –OH (hydroxyl group) attached
to a non-polar hydrocarbon chain (see 1-butanol below). The polar group will want to
dissolve in polar water while the non-polar hydrocarbon chain will be repelled by the
water. The solubility of an alcohol in water will therefore be determined by which of the
two forces are stronger.
H2 H2
C C Polar group
H3C C OH OH
H2
1-butanol
The following solubility tests will allow you to observe when the size of the hydrophobic
carbon chain starts to impact on the solubility of the alcohol in water.
66
(1) In five clean micro test tubes, place 0.5 mL of Reverse Osmosis (RO, pure) water
(in each).
(2) To each test tube then add one of the following alcohols:
• ethanol
• 2-propanol
• 1-propanol
• 1-butanol
• 1-hexanol
Predict in your own mind whether each alcohol will be soluble or not – given what you
might expect.
(3) Record these observations in your Report Book.
(4) Dispose of the experimental waste by tipping into Non-Halogenated Organic

Waste bottle on the sink. Rinse the test tube, several times, with small
amounts of acetone. Place the rinsings in the Organic Waste bottle also.
Leave the test tubes inverted in your rack to dry.
QUESTIONS
(1) Draw the structural formula for 3-octene. Write the molecular formula for 3-octene.
Is 5-octene possible? Explain.
(2) How do an alcohol and a carboxylic acid differ structurally?
(3) What feature do aldehydes and ketones have in common? Draw and name this
feature.
(4) Why are there no numbers associated with aldehyde naming?
(5) Draw the structural formula for pentanoic acid.
(6) Write a balanced equation, showing all products, for the reaction of propanol and
butanoic acid.
67
NAME DATE
EXPERIMENT 4: Report Book
Organic Families – Reactions and Identification of Functional Groups
PART A. Reactions of Alkanes and Alkenes
1. Action of Bromine Water
Organic Compound Observation
cyclohexene
cyclohexane
Equations: Write an equation for the above compounds which caused a

decolourisation of bromine (Br2) water. Name and draw all reactants and products.
PART B. Distinguishing Test for Primary, Secondary and Tertiary

Alcohols
1. Lucas Test for Alcohols

tert-pentanol
(2-methyl 2-butanol)
2-pentanol
1-pentanol
Equations: Write an equation for the above alcohols that give a precipitate upon
reaction with the Lucas Reagent. Name and draw all reactants and products.
68
NAME DATE
PART C. Distinguishing Test for Aldehydes and Ketones
1. The 2,4-dinitrophenylhydrazine (2,4-DNP) reaction

pentanal
pentanone
propan-2-ol
Equations: Write an equation for the above compounds that give a positive result
with 2,4-DNP. Draw all reactants and products for these reactions.
2. Schiff’s Test for Aldehydes
propan-2-ol (alcohol)
pentanal (aldehyde)
2-butanone (ketone)
69
NAME DATE
PART D. Sodium Hydrogen Carbonate Test for Carboxylic Acids

acetic acid
benzoic acid
ethanol
Equations: Write an equation for the above compounds that showed effervescence
with sodium hydrogen carbonate. Name and draw all reactants and products.
PART E.
Alcohol Used in Fruit Smell Detected

Esterification NOTE: SMELLING A REACTION IS ONLY ALLOWED WITH CARE IN
PART E - EXPT 4.
isopentyl alcohol
(3-methylbutan-1-ol)
octanol
Equations: Write an equation for the esterification reaction of your selected

alcohol. Name and draw all reactants and products.
70
NAME DATE
PART F.
Alcohol Used in Line Structure of Alcohol Solubility in Polar Water

Solubility Tests
ethanol
2-propanol
(iso-propyl alcohol)
1-propanol
(n-propanol)
1-butanol
1-hexanol
QUESTIONS
(1) Draw the structural formula for 3-octene. Write the molecular formula for 3-octene. Is
5-octene possible? Explain.
(2) How do an alcohol and a carboxylic acid differ structurally?
(3) What feature do aldehydes and ketones have in common? Draw and name that
feature.
(4) Why are there no numbers associated with aldehyde naming?
71
NAME DATE
(5) Draw the structural formula for pentanoic acid.
(6) Write a balanced equation for the reaction of propanol and butanoic acid.
72
NAME DATE
73
EXPERIMENT 5
TITRATION – DETERMINING THE CONCENTRATION OF ACID

AND BASE SOLUTIONS
AIM OF THE EXPERIMENT
To prepare a standard solution (a solution with a known concentration), for use in a
volumetric analysis (acid/base titration). To familiarise students with the volumetric technique
of titration and the correct use of glassware and equipment used in volumetric analysis.
SKILLS IN FOCUS
• procedure for undertaking an acid/base titration
• ability to recognize a BrØnsted-Lowry acid/base
• recognize titration end-points
• preparation of a standard solution
• recognise when dry glassware is required in a titration
• read the burette to two decimal places (interpolation)
• obtain concordant results (within a range of 0.2 mL)
• stoichiometry

• acid base reactions
• identification of BrØnsted-Lowry acids/bases
• stoichiometry / concepts such as the mole and concentration
• the use of units
CHEMICAL ALERT
(Risk Assessment)
Substances: 0.1 M NaOH solution, 0.05 M H2SO4 solution, potassium hydrogen phthalate
solution
Hazards: 0.1 M sodium hydroxide (NaOH) has a body contact rating of 3.
Protection: Read ALL safety warnings on coded solutions and unknown
solids.
Safety glasses are required.
Avoid contact with NaOH. Disposable gloves are available.
74
INTRODUCTION
Determining the concentration of species in solution, using volumetric analysis, is a

very important skill for a chemist. Volumetric analysis involves the making-up, storage
and delivery of solutions of accurately known concentrations and/or volumes.
In order to determine the concentration of a solution, there must be something to

compare it against (benchmark). This benchmark is referred to as a standard. In order
to use a standardised solution, the solution must be prepared. It is prepared by
dissolving a dried, accurately weighed amount of a specially chosen compound in a
known volume of distilled water in a volumetric flask. After preparation of the standard,
the exact concentration of the standard solution is determined by calculation (c= n/V).
Where the mass (moles, n) and the volume (L) are accurate.
Volumetric analysis is commonly undertaken by titration. A titration is a method where

a measured volume (from a burette) of a reagent (titrant) is added to a solution of
known volume (this is often the analyte, but not always as you will discover in this
experiment).
The point at which just enough titrant is added to exactly react with the analyte is
known as the equivalence point. This point is marked by an indicator added to the
analyte solution at the beginning of the titration that changes colour very near to the
equivalence point. When the indicator first changes colour this indicates the endpoint.
The closer the endpoint is to the equivalence point the more accurate the titration.
In this experiment you will:

• Make-up a standard solution,
• Use the standard solution in a titration to determine the concentration of a NaOH
solution,
• Use the NaOH solution (now known with an accurate concentration) in a titration
to determine the concentration of a H2SO4 solution.
In the titrations we make use of an acid-base reaction, equation (1). A BrØnsted-

Lowry acid is a proton (H+) donor and a BrØnsted-Lowry base is a proton acceptor.
Potassium hydrogen phthalate [Figure 1] is used as a primary standard for
standardizing bases, such as sodium hydroxide (NaOH), because it can be prepared
in a high state of purity and stored indefinitely without change in composition. It
contains one acidic proton, which is ionized and titrated with hydroxide ions.
Your first titration will require you to determine the concentration of a sodium hydroxide
(NaOH, base) solution using potassium hydrogen phthalate (a monoprotic acid),
equation (2). When the concentration of the sodium hydroxide is determined, it will
then be used as a secondary standard to determine the concentration of sulfuric acid
(H2SO4), equation (3).
75
Base + Acid à Water + Salt (1)
One acidic proton present

H O (easily removed) H O
Base
H C C H H C C
C C O C C O Na
NaOH + HOH + (2)
C C C C O
O K K
H C C H C C
H O H O
Base + Acid Water + Salt
Two acidic protons

(easily removed)
2 NaOH + H2SO4 2 HOH + 2 Na+ + SO42- (3)
C
Figure 1: OH
Potassium hydrogen phthalate
(molar mass 204.22 g mol-1) OK
C
The acid-base indicator phenolphthalein [Figure 2] is used to determine the end-point of the
NaOH / potassium phthalate titration.
HO O
O
OH
CO2-
O
Figure 2a: Phenolphthalein: Clear at pH<8.5 Figure 2b: Phenolphthalein: Pink at pH>8.5
(acidic or slightly basic) (basic or alkaline)
76
PROCEDURE
Prior to the commencement of your experimental work, your demonstrator will discuss the
steps in the preparation of the STANDARD SOLUTION, and the correct use of the
BURETTE, CALIBRATED PIPETTE and DISPENSER.
When doing titrations, it is important to obtain concordant (reproducible) results. A single

titration is never considered sufficient. Concordant or reproducible titration results,
means that three separate titration volumes are within 0.10 ml of each other. The range
of titres from highest to lowest should be no more than 0.2 ml difference.
Many students have difficulty in determining the exact end point. You should titrate to an
endpoint that corresponds to the lightest, permanent colour change.
GLASSWARE AND TECHNIQUES USED IN VOLUMETRIC ANALYSIS
As mentioned in the introduction, volumetric analysis, involves the making up, storage and
delivery of solutions of known concentrations and or/volumes. It is intrinsic to this process
that all equipment and glassware that is to be used is thoroughly cleaned and has been
rinsed with the appropriate liquid.
A burette is a vertical cylindrical piece of laboratory glassware with a

volumetric graduation on its full length and a precision tap, or stopcock
on the bottom. It is used to dispense, precise amounts of liquid reagent
in experiments. Burettes are extremely accurate - a 50 ml burette has a
tolerance of 0.05 ml. Burettes measure from the top since they are used
to measure liquids dispensed out the bottom. The difference between
starting and final volume is the amount dispensed. A burette must be
thoroughly rinsed with the solution it is to deliver.
PREPARATION OF YOUR BURETTE FOR TITRATION
(1) Sodium hydroxide (NaOH) solution (approx. 0.1 M) is supplied (see your
demonstrator before obtaining this solution). Close the tap on your burette. With
the aid of a small funnel in the top, pour in approx. 5 ml of distilled water. Remove the
burette from its stand and carefully rotate it to rinse, thoroughly, the entire inside
surface. Drain by opening the tap. Close the tap. Now rinse it with a 5 ml portion of
the NaOH solution supplied using the same technique. Repeat the rinse with another
5 ml of NaOH solution. Clamp the burette in its stand with the graduations facing you
and ensure the tap is closed.
77
(2) Carefully taking the burette out of the burette holder, using a funnel, students
will fill burette with NaOH solution below eye height. (Students should note the
approximate molarity of the NaOH and record this value on report Book). They must
then REMOVE THE FUNNEL. RETURN the burette to the burette holder, open the
burette tap and run enough solution through the tap into a waste beaker or flask to
ensure that there are NO air bubbles below the tap. (Ensure that students let the
solution run through the tip of the burette while rinsing). The solution level in the
burette should be below the 0.00 ml mark.
(3) The following diagram shows a portion of a burette. Locate the bottom of the meniscus
of the liquid in YOUR burette at eye level. Here 15.74 cm3.
(4) Record the initial burette reading to two decimal places.
Your burette is now ready for use in a titration
A volumetric flask is a piece of laboratory glassware used in volumetric analysis for the
preparation of solutions. It is made of glass and consists of a flat-bottomed base with a long
neck fitted with a stopper. The neck has a single ring graduation mark for the volume that
the flask is designed to measure. Volumetric flasks are used for making up solutions of
known volume and concentration.
78
PART A: PREPARATION OF A STANDARD SOLUTION OF POTASSIUM HYDROGEN
PHTHALATE
(1) Rinse your 250 ml volumetric flask thoroughly with distilled water, three times.
(2) Collect a sample vial, containing an accurately weighed amount of potassium hydrogen
phthalate (PHP), from your demonstrator. ON YOUR REPORT BOOK, RECORD THE
MASS OF THE PHP, AS SHOWN ON THE LABEL.
(3) Half fill (approx. 100 ml) the volumetric flask with distilled water.
(4) Transfer the potassium hydrogen phthalate (solute) into the 250 ml volumetric flask
through a small, clean and dry funnel placed in the neck of the flask.
(5) Use your distilled water wash bottle to rinse ALL traces of the PHP solid, from the
sample vial and the funnel, into the volumetric flask.
(6) Stopper the volumetric flask and shake it thoroughly to dissolve all traces of the solute.
Always keep your thumb on the stopper. This step will take some time (5-10
minutes) but you must ensure that the entire solid has dissolved.
(7) Collect approx. 100 ml of distilled water in a beaker. Fill the volumetric flask with distilled
water until the bottom of the meniscus is about one centimetre below the graduation
mark when the flask is held vertically and the mark is at eye level. Then use a plastic
pipette for smaller water additions until the bottom of the meniscus is on the
graduation mark.
(8) Stopper the flask. Mix the solution thoroughly, to ensure uniformity, by carefully
inverting and shaking the flask. Repeat three or four times. Always keep your thumb on
the stopper.
(9) Calculate the concentration (molL-1) of your PHP standard solution on your report sheet.
You have now prepared a primary standard potassium hydrogen

phthalate solution!
79
PART B. STANDARDIZATION, BY TITRATION, OF A SODIUM HYDROXIDE
SOLUTION USING POTASSIUM HYDROGEN PHTHALATE
A calibrated pipette (with Pro-pipetter) is a device for delivering a precise volume of

solution.
CHECK WITH YOUR DEMONSTRATOR IF YOU ARE UNSURE OF THE OPERATION OF

THE Pro-pipetter!!
(1) Rinse a 250 ml conical flask with a small amount of your potassium hydrogen phthalate
(PHP) solution. Transfer approx. 100 ml of your PHP into the conical flask.
(2) Collect the pipette and Pro-pipetter. Ensure that all the liquid has been fully expelled
after previous use and that the outside walls of the pipette are dry. Wipe with absorptive
tissue if necessary.
How to use Pro-pipetter

Insert the glass pipette into the pump with a slight pressure. This assures a secure fit.
NOTE: Extreme care must be taken when inserting glass pipette because of the
possibility of shattering!
1. Slide the white wheel (A) down with a thumb to fill up the solution.
2. Slide the white wheel (A) up with a thumb to empty the solution.
3. Press the side lever (B) for a quick dispensing of the solution.
4. To remove the glass pipette, just pull it out slowly.
80
(3) Using the instructions above, rinse the pipette by immersing the tip in the conical flask
containing your 100 ml of PHP solution. Expel solution fully into a waste beaker or
flask.
(4) Holding the pipette vertically and immerse the tip fully in the conical flask containing
your PHP solution. Gently raise 20 mL of the PHP solution until the PHP solution’s
meniscus sits 20 ml pipette’s graduated mark.
(5) Dispense this 20 ml of the PHP solution into a clean 250 ml conical flask.
(6) Repeat steps 4-5 to generate three further PHP titration samples in separate 250
ml conical flasks.
These samples are now your acid solutions which will be titrated with the
standardized base (NaOH solution).
(7) Take one conical flask at a time. Add two drops of phenolphthalein indicator to the
conical flask and swirl the flask gently to mix the solution. Place a white tile under the
flask.
(8) Titrate the acid solution with the 0.1 M NaOH solution. The NaOH is added, from the
burette, while constantly swirling the solution in the conical flask. If right-handed, the
left hand opens the burette tap and the right hand holds the flask by the neck, imparting
a swirling motion. Addition of NaOH solution is rapid at first. You will start to see a pink
colour form, however initially it is removed with swirling of the mixture. Continue the
titration very slowly and carefully until the addition of a single drop of NaOH solution,
added in the last stages, produces a pink colour that does not dissipate upon swirling
the solution.
(Each single drop delivers 0.05 ml of solution).
(9) Record the burette reading (to 0.01 ml, two decimal places) and calculate the volume
of the NaOH solution used.
(10) Repeat the titration until three concordant results are obtained i.e. three results which
agree to within 0.10 ml of each other. The range of titres from highest to lowest should
not exceed more than 0.2 ml difference.
(11) Calculate the concentration of NaOH in molL–1 from the average of the three
concordant results.
(12) Wash the contents of the conical flasks down the sink at the end of the bench and rinse
with tap water followed by distilled water. Shake gently to remove excess water.
81
PART C. CHEMICAL DETECTIVE - DETERMINATION OF THE CONCENTRATION
OF AN UNKNOWN SULFURIC ACID SOLUTION
You are working as an environmental/agricultural chemist and have found a jar of

sulfuric acid of unlabelled concentration. Before disposing of the acid, it is
important to determine the concentration – whether it is concentrated or dilute. This
is critical for how you deal with the unlabelled acid solution.
(1) Sulfuric acid (H2SO4) solution (approximately 0.05 M) is supplied (see the
demonstrator before obtaining solution). Using the dispenser, transfer a 20 ml
aliquot of the H2SO4 solution into a clean 250 ml conical flask.
(2) Add two drops of phenol red indicator. Phenol red will be yellow in acidic solutions
(pH<6.6) and red in basic (pH>8.0) solutions. See Note (below) for reasons why
different indicators are used.
(3) Refill the burette with NaOH solution if necessary. Record the initial burette volume to
two decimal places. Titrate the H2SO4 solution with the NaOH (base/alkali solution)
until the colour changes from yellow to red. Remember: slow the addition of NaOH
as the yellow colour starts to show signs of changing to red. Record the final burette
reading and hence find the titre value.
(4) Repeat the titration until three concordant results are obtained i.e. three results that
agree to within 0.10 ml of each other. The range of titres from highest to lowest should
not exceed a range more than 0.2 ml.
(5) Calculate the concentration of the H2SO4 solution in molL–1 from the average of the
concordant titre values.
CLEANUP
Wash the contents of the conical flasks and burette down the sink. All conical flasks,
burettes, pipettes, beakers and funnels should be rinsed well with tap water and finally
with distilled (RO) water.
Leave burettes clamped, inverted and with the tap open on your bench.
Conical flasks, funnels etc MUST be returned to YOUR drawer in a neat manner before
you sign the demonstrator “sign-off” sheet.
Glassware IS NOT to be left on the draining racks over the sinks.
82
Note: You may be wondering why different indicators are used in Parts A and B.
The explanation is connected to the fact that potassium hydrogen phthalate is a
weak acid while sulfuric acid (H2SO4) is a strong acid. When a weak acid is
titrated with a strong base, such as sodium hydroxide (NaOH), the pH at the
equivalence point is greater than 7. In Part A, we therefore require an indicator
such as phenolphthalein which changes colour at a somewhat alkaline pH (for
phenolphthalein the colour change occurs in the pH range 8 to 10). When a
strong acid is titrated against a strong base the pH at the equivalence point
is 7; phenol red, used in Part B, changes colour over the pH range 6.8
(yellow) to 8.4 (red).
PHENOL RED - INDICATOR

O
O O
O
S
S
O
O BASE
O
ACID
OH
HO
HO
YELLOW (ACIDIC) pH < 7.7 RED (BASIC) pH > 7.7
83
NAME DATE
Titration – Determining the Concentrations of Acid and Base

Solutions
PART A: Concentration of Standard Solution of Potassium Hydrogen Phthalate

(PHP)
g
Mass of PHP in sample vial
Molecular Weight of PHP g/mol
Mole of PHP in 250 ml volumetric m mol
Conc. of standard PHP molL-1
State your final answer with the CORRECT number of Significant Figures
PART B: Standardization of sodium hydroxide solution using potassium hydrogen

phthalate.
Titration reaction:
Write a balanced equation for reaction between NaOH and potassium hydrogen
phthalate.
Titration of PHP with NaOH (read burette to 2 decimal places)
Burette 1 2 3 4 5
Final reading
Initial reading
Titre (ml)
ml
84
NAME DATE
Average titre ml
mol
No. of moles of PHP in 20 ml
\ No. of moles of NaOH in average titre mol
\ Concentration of NaOH molL-1

(no. of mole in 1000 ml)
State your final answer with the correct number of Significant Figures
PART C. The determination of concentration of a sulfuric acid solution.
Write a balanced equation for the titration reaction of NaOH and H2SO4:
Titration of H2SO4 with NaOH (read burette to 2 decimal places)
Burette 1 2 3 4 5
Final reading
Initial reading
Titre (ml)
Average titre ml
\ No. of moles of NaOH used in titration. mol
\ No. of moles of H2SO4 present in 20 ml aliquot.

mol
\ Concentration of the H2SO4 solution molL–1

(no. of mole in 1000 ml)
85
EXPERIMENT 7
EQUILIBRIUM AND EQUILIBRIUM CONSTANTS

In this experiment, students will undertake a qualitative study of two equilibrium systems.
The effect of the addition of various substances on this reaction (and temperature) will be
observed and students will be asked to explain these changes in terms of Le Chatelier’s
principle. Students will then calculate the equilibrium constant, Ka, of an acid/base
indicator, bromothymol blue using absorbances as measure of concentrations.
SKILLS IN FOCUS
• Observation and critical thinking skills – drawing conclusions from the results of a
number of reactions.
• Observation of disturbing chemical equilibrium through change (Le Chatelier’s
principle)
• Writing and balancing reactions.
• Careful measurement of physical data and the use of this data to determine
equilibrium constants - reinforcing the concept of determining K.
• The use of a UV/Vis spectrophotometer.
• The use of the Beer-Lambert law – which relates concentration to absorbance.
REMEMBER FOR WORKSHOP TESTS/EXAM

• predict the effect change in conditions on equilibria using Le Chatelier’s principle
• derive an equilibrium expression, Kc, from a given equation (c = conc., general form)
• understanding what Ka refers to the acid dissociation constant, species acting as an
acid with water
• pH = -log10[H+] and understanding the relationship between pH and [H+]
• pKa = -log10Ka and understanding the relationship between pKa and acidity
86
CHEMICAL ALERT
(Risk Assessment)
Substances: 0.003% bromothymol blue
sodium phosphate monobasic
monohydrate, sodium phosphate dibasic, anhydrous
1 M hydrochloric acid
1 M sodium hydroxide
0.1 M Iron(III) nitrate, Fe(NO3)3•9H2O, 4.0 g per 100 ml solution
0.02 M Mercuric nitrate, Hg(NO3)2, 3.3 g per 100 ml solution
0.1 M Silver nitrate, AgNO3, 1.7 g per 100 ml solution
0.1 M Sodium hydroxide, NaOH, 0.4 g per 100 ml solution
0.1 M Sodium phosphate, Na3PO4•H2O, 1.4 g per 100 ml solution
0.1 M Sodium oxalate, Na2C2O4, 1.3 g per 100 ml solution
0.1 M Sodium thiosulfate, KSCN, 2.5 g per 100 ml solution
0.01M sodium fluoride, NaF, 42 mg per 100 ml solution
Hazards: Substance Rating

0.003% bromothymol blue C(3)
sodium dihydrogen phosphate T(2), B(2), C(2)
disodium hydrogen phosphate T(2), B(2)
1 M hydrochloric acid T(2), B(2), C(2)
1 M sodium hydroxide T(2), B(4), C(2)
1 M iron(III) nitrate, Fe(NO3)3•9H2O T(2), B(2)
1 M potassium thiocyanate, KSCN T(2), B(2)
0.02 M mercuric nitrate, Hg(NO3)2,
in 2% HNO3 (AVOID CONTACT!) T(2), B(2), C(2)
0.1 M silver nitrate, AgNO3 T(1)
0.1 M Sodium hydroxide, NaOH B(3)
0.1 M Sodium phosphate, Na3PO4•H2O T(2), C(2)
0.1 M Sodium iodide, NaI B(1)
0.1 M Sodium oxalate, Na2C2O4 NH
0.01M sodium fluoride, NaF T(3), B(3), C(2)
USE ONLY in the FUME CUPBOARD
NH = Non Hazardous
F=Flammability; T=Toxicity; B=Body Contact; R=Reactivity; C=Chronic
Protection: Safety glasses are required. Avoid contact with concentrated acid – any spillages or
contact should be treated with much cold water. Disposable gloves are available.
Risk: C2
Part A
INTRODUCTION
Reactions are processes where reactants collide together to form products. It is important
to note that while this is occurring products are also being converted back into reactants.
Chemical equilibrium in a reaction is reached when the rate for the forward reaction equals
the rate of the reverse reaction [Equation 1].
Rate of forward reaction = Rate of backward reaction (1)
If a reaction is at equilibrium, changes in: concentration; pressure; volume or temperature

may result in the system being disturbed from its equilibrium position and the system will
then proceed in such a way as to restore equilibrium. The rule for predicting the direction
of change is known as Le Chatelier’s principle.
87
Table 1 indicates the result of a number of changes to the Haber process:
N2(g) + 3H2(g) 2NH3(g) ΔH = -92.6 kJmol-1 (2)
Table 1: Effects on the Haber process with changes that disrupt equilibrium.
Changed imposed How this system alters to regain equilibrium
on system
Add more reactants More products are formed immediately to reduce the amount
(N2 or H2) reactants. Rate forward reaction > Rate reverse reaction
until equilibrium is achieved
Add more products More N2 and H2 are formed immediately to reduce the amount
(NH3) products. Rate forward reaction < Rate reverse reaction
Pressure is More products are formed immediately to reduce the pressure
increased (moles of gas). Rate forward reaction > Rate reverse reaction
Mixture is heated More N2 and H2 are formed (endothermic reaction). Rate
forward reaction < Rate reverse reaction until equilibrium is
achieved
It is clear from this Table 1, that any externally imposed changes on a system that disrupt
equilibrium will result in the system opposing those changes in order to get back to
equilibrium.
For the following general system:
aA + bB cC + dD - (3)
the equilibrium constant, Kc, of a system may be defined as follows:
[C]c [D]d
Kc = - (4)
[A]a [B]b
Kc has a constant numerical value for a given system at a given temperature. The
individual concentrations may change, but the ratio remains the same (at a given
temperature).
88
In Part A of this experiment, you will prepare an equilibrium system for the following reaction:
Fe3+(aq) + SCN-(aq) [FeSCN]2+(aq) - (5)
and study the response of this system to various stresses and explain these results.
Part A (half of the students will start with Part B (see demonstrator))
PROCEDURE
1. Into a clean 250 mL beaker add 120 mL of distilled water, 10 drops of 1M KSCN and
10 drops of 1 M Fe(NO3)3 solution. This will be your stock solution.
2. Label 10 clean test-tubes A-J.
3. Add 5 mL of this stock solution into each one of the clean test tubes.
4. Keep test tube A as a control.
5. Add the following reagents into test-tubes B through to I:

Test tube #
B 1 mL 1 M Fe(NO3)3
C 0.5 mL 1 M KSCN
D 0.25 mL (5 drops) 0.1 M AgNO3
E 2 mL conc. HCl
F 0.5 mL (10 drops) 0.02 M Hg(NO3)2
G 1 mL 0.1 M Na3(PO4)
H 1 mL 0.1 M Na2(C2O4)
I 1 mL 0.01 M NaF
Students add these reagents very carefully!
6. Record all your observations and carefully mix (this may not even be all that
necessary).
7. Heat test tube J in a hot water bath.
89
8. Compare the colour intensity of each of the test tubes with that of the control (test
tube A) and using the following table explain your observations.
Ag+ Hg2+ Cl- PO43- F- C2O42-

Fe3+ [FeCl4]- FePO4 [FeF6]3- [Fe(C2O4)3]3-
SCN- Ag(SCN) (s) Hg(SCN)2
CLEANUP
Students place all aqueous waste in the suitably labeled bottles in the fume cupboard,
as instructed.
Ensure they wash all glassware with detergent and hot water and rinse with distilled
water.
Dirty test tubes (brown stains, iron compound) needs to have 5M HCL (Highly
Corrosive! Place washings in Waste HCl container). Then give several rinses with
tap water and down the fume cupboard sink. Finally, rinse with RO (distilled) water.
Use brushes to clean test tubes properly.
NOTE: Place NaF solution test tube residues in the aqueous wastes container, rinse
once with water and place this in the residues. When you add acid – place these
residues in the acid wastes container.
Part B - Determination of a pKa using absorbance as measure of concentration.
INTRODUCTION
Bromothymol blue is an acid-base indicator that is yellow at pH < 6 and blue at pH > 8.
Between pH values of 6 - 8, bromothymol blue is some shade of green. Its chemical
structure is shown in Figure 1.
HO
Br OH
O Br
S
O O
Figure 1: Chemical structure of bromothymol blue (3', 3"-dibromothymolsulfonephthalein) as it

occurs under acidic conditions. Its chemical formula is HC27H27Br2O5S).
90
Like all acid-base indicators, bromothymol blue is a weak acid that reacts with water as
shown in the equilibria (Eq. 6) in which HBB represents the protonated (yellow) form of
bromothymol blue and BB- represents the blue conjugate base form.
HBB (yellow) + H2O ⇋ H3O+ + BB- (blue) - (6)

432 nm 616 nm
Absorbance spectra for the yellow and blue forms are shown in Figure 2. The blue form,
BB-, has an absorbance maximum at about 616 nm. The yellow form, HBB, has its
maximum absorbance at 432 nm. In this experiment, we will measure the absorbance of
the yellow form at 453 nm, where the absorbance is still strong and the absorbance of the
blue BB- is minimal.
Figure 2: Visible absorbance spectra of bromothymol blue at low pH (yellow, solid line) and high pH (blue,
dashed curve).
The equilibrium expression, Ka, for the HBB/BB- equilibrium (Eq. 7) is:
[$! %" ][''# ]

𝐾! = - (7)
[$'']
To calculate the equilibrium constant Eq. 7 for bromothymol blue you will use the
absorbances of three solutions of bromothymol blue, at different pH’s and different
wavelengths, to determine the concentration of the species in Eq. 7 (Eq. 19). A full
explanation of how Eq. 7 is converted to Eq. 19 is given in Appendix 1.
Equations 6, 7 and 19 are rewritten below.
[$! %" ][''# ()*+,)]

𝐾! =
!!→
HBB(yellow) + H2O ←!!! H3O+ + BB-(blue) - (6) - (7)
[$''(.,**/0)]
91
()**& -*../0
[$! %" ]1$%$&' ×1+,!&'
𝐾! = ()**& - (19)
1+,!&' ×11.2*
$%$&'
Part B
Procedure
1. 5 mL of bromothymol blue indicator is added to three test tubes (labelled: Y, G &B).
2. Use an auto dispenser to transfer 2.00 mL of the buffer solution to test tube G and stir
to mix the indicator uniformly through the solution. The solutions should appear green in
colour. This solution will be referred to as “Green.”
3. Use an auto dispenser to transfer 2.00 mL of 1.0 M HCl into test tube Y. The solution
should turn yellow. This solution will be referred to as “Yellow.”
4. Use an auto dispenser to transfer 2.00 mL of 1.0 M NaOH into test tube B. The
solution should turn blue. This solution will be referred to as “Blue.”
Note: They all contain the same final volume of solution (7.00 mL) and the same number
of total moles of bromothymol blue. This gives an equivalent total concentration of
bromothymol blue in each test tube.
5. Your demonstrator will determine the pH of the buffer solution using a pH meter pre-
calibrated with a standard buffer solution, pH 6.88. 10 mL of bromothymol blue indicator
and 4 mL of phosphate buffer is added. Record this pH value in your notebook.
6. i. Check that two spectrophotometers are set at 453 nm and two are set at 616 nm.
ii. Students are required to measure the absorbance of four solutions (blank, yellow,
green and blue) at 453 nm and repeat at 616nm.
iii. Students must carefully ¾ fill three cuvettes with their yellow, green and blue
solutions. The cuvettes are rinsed three times with distilled water and then finally
rinsed with the solution to be added (use ~2 mL). Then they refill each cell with a
different solution and wipe the clear sides of the cell with a tissue. Important to ensure
that the cell is properly wiped to remove all traces of solution and any finger marks.
Make sure the cell is held with fingers placed on the opaque sides.
iv. Students must place the three cuvettes in the cuvette holder (the blank (distilled
water) should already be present) in the spectrophotometer with its clear sides in the
direction of the light path and close the sample compartment.
v. Students will then record the absorbances for the three coloured solutions at 453
92
nm and then transfer the holder and contents to the other spectrophotometer and
record absorbances for all four samples at 616 nm (or vise versa).
vi. After recording the absorbances, students will remove the cuvettes containing the
coloured solutions from the spectrophotometer and empty each into the waste beaker.
Then they will wash the cuvettes three (3) times with distilled water from a wash bottle,
each time emptying the cell into the waste beaker.
7. Students need to record the temperature of the equilibrated buffer/indicator solution from
their demonstrator.
Part B
Data Analysis and Calculations
1. You could simply plug values from the table into the Ka expression:
9:,,7 .,**/0
[𝐻3 𝑂4 ]𝐴56578 × 𝐴;<378
𝐾! = 9:,,7
𝐴;<378 × 𝐴)*+,
56578
However, a more accurate result is obtained by subtracting the small absorbance of yellow
HBB at λ = 616 nm (where blue BB- absorbs) from absorbance of the green solution, and
similarly subtracting the small absorbance of blue BB- at λ = 453 nm (where yellow HBB
absorbs) from the absorbance value of the green solution.
[ H 3O + ]( A616nm - A616nm ) ´ ( A453nm )

green yellow yellow
Kc =
nm - A453nm ) ´ ( A616nm )
green blue blue
( A453
(19’)
Perform the calculation of Ka in your laboratory reportbook and report your pKa value
(remember pKa = -logKa) to two decimal places.
93
QUESTIONS
(1) Write the equation that describes the equilibrium reaction of Fe3+ with one mole of
SCN-.
(2) Using the equation in Q (1) write out the Kc expression for the reaction of Fe3+ with one
mole of SCN-.
(3) Based on your observations of test tube J, is the forward reaction between Fe3+ and
SCN- endothermic or exothermic. ______
(4) Write down the net ionic equations of any reactions that occur in test tubes B-J.
(5) Use the equation below to calculate the Ka for bromothymol blue.
7-))' 8)//,9 8)//,9

[𝐻4 𝑂5 ](𝐴626'0 − 𝐴626'0 ) × (𝐴:;4'0 )
𝐾& = 7-))'
(𝐴:;4'0 − 𝐴</1) </1)
:;4'0 ) × (𝐴626'0 )
(6) Calculate the pKa of bromothymol blue and comment on any differences with the
known value (7.10).
(7) The pKa for another indicator, methyl red is 5.0. Using the equation below, state the
pH when there will be equal amounts of the acidic (HA) and basic (A-) form of methyl
red in solution.
Henderson- Hasselbalch Equation
pH = pKa + log10([A-]/[HA]) (20)
94
CLEANUP
Students place all aqueous waste in the suitably labeled bottles in the fume cupboard,
as instructed.
Cuvettes should be washed with water and a small amount of detergent (DEFINITELY
NO ACETONE!!). Finally rinse with distilled (RO) water.
Ensure they wash all non-cuvette glassware with detergent and hot water and rinse
with distilled water.
Students replace all glassware and equipment in THEIR CORRECT DRAWERS.

Have them sign the “Sign Off” sheet when you are satisfied with the cleanup.
95
NAME DATE
Equilibrium Part A
Explanation
Observation
Reagent
Added
Tube
Test
G
A
H
E
J
I
96
NAME DATE
Equilibrium Part B
Quantity Measurement (demonstrator)
Temperature
pH
[H 3O + ] = 10 − pH
Use blank
Yellow Green Blue

Absorbance at 453 nm
Absorbance at 616 nm
97
NAME DATE
QUESTIONS
(1) Write the equation that describes the equilibrium reaction of Fe3+ with one mole
of SCN-.
(2) Write out Kc expression for the reaction of Fe3+ with one mole of SCN-.
(3) Based on your observations of test tube J, is the reaction between Fe3+ and SCN-
endothermic or exothermic. ____________________
(4) Write down the net ionic equations of any reactions that occur in test tubes B-I.
B__________________________________________________________________
C__________________________________________________________________
D__________________________________________________________________
E__________________________________________________________________
F__________________________________________________________________
G__________________________________________________________________
H__________________________________________________________________
I __________________________________________________________________
J__________________________________________________________________
98
NAME DATE
(5) Using the equation below to calculate the Kc for bromothymol blue.
9:,,7 .,**/0 .,**/0

[𝐻3 𝑂4 ](𝐴56578 − 𝐴56578 ) × (𝐴;<378 )
𝐾! = 9:,,7
(𝐴;<378 − 𝐴)*+, )*+,
;<378 ) × (𝐴56578 )
(6) Calculate the pKa of bromothymol blue and comment on any differences with the
known value (7.10).
(7) The pKa for another indicator, methyl red is 5.0. Using the equation below, state
the pH when there will be equal amounts of the acidic (HA) and basic (A-) form of
methyl red in solution.
Henderson- Hasselbalch Equation:
pH = pKa + log10([A-]/[HA])
99
APPENDICES
Appendix 1: Derivation of equilibrium expression (EXPT 7)
Bromothymol blue is a weak acid as shown in the following equilibrium in which HBB
represents the protonated (yellow) form of bromothymol blue and BB- represents the
blue conjugate base form.
HBB (yellow) + H2O ⇋ H3O+ + BB- (blue) - (6)

432 nm 616 nm
Absorbance spectra for the yellow and blue forms are shown in Figure 2. The blue
form, BB-, has an absorbance maximum at about 616 nm. The yellow form, HBB,
has its maximum absorbance at 432 nm. In this experiment, we will measure the
absorbance of the yellow form at 453 nm, where the absorbance is still strong and
the absorbance of the blue BB- is minimal.
Figure 2: Visible absorbance spectra of bromothymol blue at low pH (yellow, solid line) and high pH
(blue, dashed line).
The equilibrium expression, Kc, for the HBB/BB- equilibrium (Eq. 7) is:
[ H 3O + ][BB - ]
Kc =
[ HBB] - (7)
The value of Kc should be independent of all factors except a change in
temperature. At high pH, the concentration of the blue form, [BB-], is large and
[HBB] is small, and at low pH, [HBB] is large and [BB-] is small. In this experiment,
students will be working with a solution that is green in color, so that neither [HBB]
nor [BB-] is much larger than the other.
Both the yellow and blue forms of bromothymol blue have Beer’s law expressions
that relate absorbance (A) to concentration ([ ], in molarity) at their respective
wavelengths:
100
For the yellow form, HBB:
A453nm = e 453 nm ´ b ´ [ HBB ]
yellow
- (8)
and for the blue form, BB :

A616 -
nm = e blue
616 nm ´ b ´ [ BB -
] - (9)
where ε is the molar absorptivity (L mol-1cm-1) and b is the path length in cm.
Rearranging Equations 8 and 9 for [HBB] and [BB-], respectively, gives:
A453nm
[HBB] = yellow - (10)
ε 453nm ×b
A616nm
[ BB - ] =
e 616
blue
nm ´ b - (11)
These two equalities (10, 11) can be substituted into the Kc expression (Eq. 7) and
the b’s cancel:
A616nm
[ H 3O + ]
e 616
blue
nm ´ b
[ H 3O + ] A616nm ´ e 453
yellow
nm
Kc = =
A453nm A453nm ´ e 616
blue
nm
e 453 nm ´ b
yellow
- (12)
Note that it is not necessary to know the concentrations of [HBB] or [BB-] in
the green solution, only the ratio A616 nm / A453 nm.
There are five values from Eq. 12 that you must obtain to determine Kc for
bromothymol blue. These are summarized in Table 2.
Table 2: Quantities measured for the determination of Kc
Quantity How we measure it:
Use a pH meter to determine

[H 3O+ ]
the pH of the green solution
green Determine the absorbance of
A616nm the green solution at 616 nm
€ e 453
yellow
nm Discussed below
green Determine the absorbance of

A453nm the green solution at 453 nm
€
e 616
blue
nm Discussed below
€ 101
The Kc expression given above (Eq. 12) is now re-written with “green” labels
indicating that you will determine absorbance values at two wavelengths for the
green form of your bromothymol blue solution i.e. we calculate the pH of the green
solution so we must use the green solutions absorbance values):
[ H 3O + ] A616nm ´ e 453nm
green yellow
Kc =
nm ´ e 616 nm
green blue
A453
- (13)
The value for e
yellow
will be determined when the solution is completely yellow (low
453 nm
pH; ~100% HBB and negligible BB-) and the value for e 616nm will be determined when
blue
the solution is completely blue (high pH; ~100% BB-). This is because we need to
relate the ε values to concentration via the Beer’s law equation (A = ε x b x M) and
unless the equilibrium is shifted almost 100% one way or the other, we will not know
the concentration exactly.
The absorbance at 453 nm of the yellow solution is due entirely to the “yellow” form
(HBB); while the absorbance at 616 nm is due entirely to the “blue” form (BB-). We
can write a Beer’s law expression for the absorbance of each solution at each
wavelength:
nm = e 453nm ´ b ´ [ HBB ( yellow)]

yellow yellow
A453 - (14)
nm = e 616 nm ´ b ´ [ BB (blue )]
blue blue -
A616 - (15)
Since we have designed the experiment such that all HBB and BB- originates from
the same source, the concentration of bromothymol blue in the yellow solution
equals the concentration of bromothymol blue in the blue solution:
[ HBB( yellow)] = [ BB - (blue)] - (16)
which, upon substitution of Eq. 14 and 15 into Eq. 17, gives:
yellow blue
A453 A616
nm
= blue nm
e 453nm ´ b e 616nm ´ b
yellow
- (17)
The b values cancel and Eq. 14 is rearranged:
yellow
e 453
yellow
A453nm
nm
=
e 616
blue
nm
blue
A616nm - (18)
102
yellow
The labels “yellow” and “blue” on A453nm and A616 nm denote that these are the
blue
absorbance values of the yellow and blue solutions, at their respective wavelengths.
The above ratio of ε values can be substituted into the Kc expression (Eq. 13):
[ H 3O + ] A616nm ´ e 453nm [ H 3O + ] A616nm ´ A453nm

green yellow green yellow
Kc = =
nm ´ e 616 nm nm ´ A616nm
green blue green blue
A453 A453
- (19)
From Eq. 19, you should see how we can determine Kc from only absorbance values
and the [H3O+], obtained from a pH measurement on the green solution.
103
Appendix 2-104
Appendix 2: COMMON LABORATORY EQUIPMENT
A2.1 Measuring cylinders

Measuring (graduated) cylinders are used to measure the volume of liquids (and
solutions). The graduations on the side of the cylinder indicate the volume.
Typical sizes are 10ml, 50ml, 100ml, 250ml or 1000ml volumes. Measuring
cylinders should either be used dry or should be rinsed out with distilled water
and twice with 5 ml portions of the solution being used.
A2.2 Beakers
Beakers are a general-purpose item of glassware in the chemistry laboratory.
They are used as distillation receiving containers, to hold different layers in
an extraction, as reaction flasks, to heat solvent for crystallizations, as the
crystallization flask, as an ice bath, etc. Beakers must not be used for
titration.
A2.3 Watch glass

Watch glasses are small, flat, round pieces of glassware. They are mainly
used to dry and weigh solid compounds and to cover containers such as
TLC developing chambers. Watch glasses come in many sizes.
A2.4 Test tubes and Test tube rack

Test tubes are used for holding small amounts of liquids and solids.
Occasionally, reactions are carried out in test tubes. Small test tubes are
called ‘mini’ test tubes. Test tube racks are either wooden, plastic or
metal and are used for holding test tubes.
A2.5 Graduated Volumetric Flasks

These flasks are graduated to contain a fixed volume of liquid at a
given temperature (generally 20°C), so care should be taken to
ensure that solutions to be made up to the mark are at room
temperature. Flasks should only be handled by the (narrow) neck.
A2.6 Conical or Erlenmeyer Flasks

These should be used for titration work as they can be swirled
vigorously without any loss by splashing. Typical capacity is 250 ml.
Beakers must not be used for titration.
104
Appendix 2-105
A2.7 Buchner Flask (Vacuum flask)

The vacuum flask looks like a Conical (Erlenmeyer) flask with a
short arm coming out of it. The "arm" is designed to connect the
flask to a vacuum source. When sealed on the top with a stopper
or a Buchner funnel, the vacuum flask will hold a reduced
pressure. Note the heavy the walls of this flask - they are designed
to withstand reduced pressure without imploding. This design feature is the reason for the
high cost of this flask. Buchner flasks are used either for filtering solutions or for removing
solvent under reduced pressure.
A2.8 Buchner Funnel

The Buchner funnel is a white porcelein funnel. You need a grey or black
adaptor or a stopper with a hole in it to connect it to a side arm flask.
The Buchner is used exclusively for vacuum filtrations. The adaptor
forms a snug seal so that when reduced pressure is applied to the
vacuum flask, liquid poured into the Buchner is sucked into the flask
quickly.
A2.9 Hirsch Funnel

The Hirsch funnel is a white porcelein funnel. You need a grey or black
adaptor or a stopper with a hole in it to connect it to a side arm flask.
A2.10 Burette
Burettes are used for measuring (dispensing) accurate volumes of zero mark
solutions, for example in titrations.
Before use, burettes should be rinsed out with distilled water and twice with
5 ml portions of the solution being used. The burette should then be
carefully and gently clamped upright in the stand and allowed to drain
before the stopcock (tap) is closed. Fill the burette to a point just above the
zero line. Turn the stopcock to allow the solution to fill the tip of the burette
and the solution level is in the graduated portion of the tube. Burette tips
should be wiped dry before titration.
The burettes should be read to two decimal places (± 0.01 ml). Make Stopcock
certain that your eye is at the level of the liquid and read the level at the (tap)
lowest point of the meniscus, except for potassium permanganate and
iodine solutions, where you read the level at the top of the meniscus.
105
Appendix 2-106
After use, the burettes must be rinsed thoroughly with distilled water and returned to the
stand and clamped in an inverted position with the tap open.
Distillation/reflux glassware
A common experimental set up in organic
chemistry is for distillation or reflux. The
following glassware is used for these purposes.
The glassware is also referred to as ‘Quickfit’.
Distillation is one of the oldest and still most
common methods for the purification of liquids.
It is used to concentrate dilute alcoholic
beverages and to obtain perfumes from fruits
and flowers. In short, distillation consists of
heating a liquid, separating the vapours and
recondensing them to obtain a new liquid.
A2.11 Round bottom flask

The round bottoms on these flasks allow for uniform heating and/or boiling of
the liquid. They are commonly used in distillation. Always clamp the flask.
Always add boiling chips before heating to avoid super-heating.
A2.12 Pear Shaped Flask

Pear-shaped flasks are used in distillation, in particular for semi-micro
distillations. The pear-shape allows rapid distillation down to a small bulk.
A2.13 Condenser
A condenser is used to cool hot vapours or liquids. A condenser usually
consists of a large glass tube containing a smaller glass tube running its
entire length, within which the hot fluids pass. The outer glass tube usually
has two hose connections, and a coolant (usually tap water) is passed
through it. The cold water always enters through the bottom fitting, and
exits through the top fitting. Condensers are used for reflux (where the hot
solvent vapours of a liquid being heated are cooled and allowed to drip
back) and distillation (condensing the hot vapours into liquid for collection).
A2.14 Distillation head

A distillation head that connects the distillation flask to the condenser. The
distillation head holds a thermometer to allow the temperature of the vapoUrs to
be monitored during the distillation.
106
Appendix 2-107
A2.15 Receiver / Adaptor

A distillation adaptor that connects the condenser to the receiving
flask.
A2.16 Boss Head

Used to connect clamps to a retort stand.
A2.17 Clamp
Used to clamp glassware. Connected to a retort stand with a boss head.
A2.18 Bunsen Burner

Gas burner used for heating. Bunsen burners must never be
left unattended. The heat can be adjusted by changing the air
hole – the blue flame is the hottest. If not heating, leave the
burner with a yellow flame (adjust the air hole). Mainly used in
distillation and reflux. As an alternative, heating mantles may
be used.
A2.19 Separatory Funnel

A separating funnel, also known as separation funnel or separatory funnel,
is used in liquid-liquid extractions to separate the components of a mixture
between two immiscible solvent phases of different densities. To use the
funnel, the two phases and the mixture to be separated in solution are added
through the top with the stopcock at the bottom closed. The funnel is then
closed and shaken very strongly to bring the phases into close contact. The
funnel is then inverted and the tap carefully opened to release excess vapour pressure. The
separating funnel is set aside to allow for the complete separation of the phases. The top
and the bottom tap are then opened and the two phases are released by gravitation.
A2.20 Dispensers
These are designed to deliver a fixed quantity of liquid; most of those used in this course
will deliver 20.0 ml. To use a dispenser, the preset amount of liquid is drawn up into the
internal reservoir and then delivered into an appropriate flask by gently depressing the
plunger completely down. Do not use the full pressure of your palm.
107
Appendix 2-108
A2.21 Balances
Instructions in the use are to be found in the balance rooms. Also, at the beginning of this
course a demonstration on the use of the balances will be given by your demonstrator.
Always consult a demonstrator if in doubt. The balances are very delicate instruments
and must be handled with care. The following rules should be obeyed at all times:
(a) The floor of the balance, pans, and area around the balance must be kept
scrupulously clean. Use the brush supplied in the balance room.
(b) Samples should be weighed in sample weighing bottles or small beakers. It is
poor technique to use watch glasses or filter papers - except when using the TOP
LOADING BALANCES. Samples should be added to the weighing bottle OFF the
balance – do not add sample to the balance.
(c) Do not use scraps of paper for recording weighings as these are easily lost.
(d) All analytical data accumulated during an experiment must be recorded directly into
your laboratory notebook.
If a solid material is to be made up as a standard solution, dissolve the accurately weighed
solid in the weighing vessel in some distilled water. Transfer this solution to the volumetric
flask through a short-stemmed funnel. Rinse the weighing vessel with a stream of water
from the wash bottle to remove the last traces of the particles or solution and transfer
carefully to the volumetric flask. Repeat several times. Using a stream from the wash bottle,
wash the funnel and the stem thoroughly into the volumetric flask. Add distilled water to the
volumetric flask until it is about three-quarters full. Swirl to mix. Using a wash bottle, add
water to the flask until the level is about one centimetre below the mark. Using a pasteur
pipette or a wash bottle, add water to the flask until the meniscus is exactly level with the
mark. Stopper the flask and use both hands to invert the flask eight to ten times to thoroughly
mix the contents.
If a liquid is to be made up as a standard solution, transfer the liquid to the volumetric flask
using a dispenser. At this point, the procedure is the same as that above for the solid. After
filling to the mark, mix thoroughly as before.
108
Appendix 3-109
Appendix 3. Calculation of Yields
A3.1 Calculation of Yield When There is No Chemical Change (Reaction)

When there is no chemical reaction occurring, and the product is just extracted from the
original material (such as the extraction of caffeine from tea leaves), the yield is simply the
mass of product expressed as a percentage of the original material.
For example, if we extract 0.01 grams of caffeine from 2.00 grams of tea, the percentage
yield is calculated as:
% yield
If we are purifying a material, such as methylated spirits, to extract the ethanol, and we get
9.0 grams of ethanol from 10.0 grams of methylated spirits, then the percentage yield (or
percentage recovery) is calculated as:
% yield
A3.2 Calculation of Yield in a Chemical Reaction
There are two steps to the calculation of a percentage yield:
1. Calculation of theoretical yield

This is simply a stoichiometry problem. To calculate the theoretical yield in a reaction
requires a balanced chemical reaction, from which you must identify the limiting reagent.
You will need to determine the molecular weight of the reactants and products of
interest. The balanced equation provides the molar ratios, from which a calculation of
the number of moles of reactants enables the theoretical number of moles of products
to be determined.
2. Calculation of percentage yield
The percentage yield is simply ratio of the mass of your actual yield to the theoretical
yield.
% yield
This is best illustrated with an example.
109
Appendix 3-110
Example. In an experiment, 20.0 grams of sodium bicarbonate (NaHCO3) was decomposed

by heating according to the reaction,
A student recorded that 9.4 grams of sodium bicarbonate (Na2CO3) was produced.
Firstly, note that the molar ratio of sodium bicarbonate (NaHCO3) to sodium carbonate
(Na2CO3) is 2:1. That is, 2 moles of sodium bicarbonate will produce 1 mole of sodium
carbonate. The molecular weight of NaHCO3 is 23 + 1 + 12 + (3 x 16) = 84 g/mol. The
molecular weight of Na2CO3 is (2 x 23) + 12 + (3 x 16) = 106 g/mol.
Calculate the number of moles of reactant.
n(NaHCO3) = mass / MW
= 20.0 / 84
= 0.238 mol
Since 2 moles of NaHCO3 produces 1 mole of Na2CO3,
n(Na2CO3) = ½ x n(NaHCO3)
= 0.5 x 0.238
= 0.119 mol
Now calculate the mass of Na2CO3.
mass(Na2CO3) = n x MW
= 0.119 x 106
= 12.6 g
So, if the reaction went to completion, with no experimental errors (spills etc), this reaction
would produce 12.6 grams of sodium carbonate.
Now we can calculate the percentage yield.
% yield
110
Periodic Table
An Alphabetical List of the Elements and their Atomic Masses
Element Symbol Atomic Mass Element Symbol Atomic Mass
Actinium Ac (227) Mercury Hg 200.59
Aluminium Al 26.98154 Molybdenum Mo 95.94
Americium Am (243) Neodymium Nd 144.24
Antimony Sb 121.75 Neon Ne 20.1797
Argon Ar 39.948 Neptunium Np (237)
Arsenic As 74.92159 Nickel Ni 58.69
Astatine At (210) Niobium Nb 92.90638
Barium Ba 137.327 Nitrogen N 14.00674
Berkelium Bk (247) Nobelium No (259)
Beryllium Be 9.01218 Osmium Os 190.2
Bismuth Bi 208.98037 Oxygen O 15.9994
Boron B 10.811 Palladium Pd 106.42
Bromine Br 79.904 Phosphorus P 30.97376
Cadmium Cd 112.411 Platinum Pt 195.08
Calcium Ca 40.078 Plutonium Pu (244)
Californium Cf (251) Polonium Po (209)
Carbon C 12.011 Potassium K 39.0983
Cerium Ce 140.115 PraseodymiumPr 140.90765
Cesium Cs 132.90543 Promethium Pm (145)
Chlorine Cl 35.4527 Protactinium Pa 231.03588
Chromium Cr 51.9961 Radium Ra (226)
Cobalt Co 58.93320 Radon Rn (222)
Copper Cu 63.546 Rhenium Re 186.207
Curium Cm (247) Rhodium Rh 102.90550
Dysprosium Dy 162.50 Rubidium Rb 85.4678
Einsteinium Es (252) Ruthenium Ru 101.07
Erbium Er 167.26 Samarium Sm 150.36
Europium Eu 151.965 Scandium Sc 44.95591
Fermium Fm (257) Selenium Se 78.96
Fluorine F 18.99840 Silicon Si 28.0855
Francium Fr (223) Silver Ag 107.8682
Gadolinium Gd 157.25 Sodium Na 22.98977
Gallium Ga 69.723 Strontium Sr 87.62
Germanium Ge 72.61 Sulfur S 32.066
Gold Au 196.96654 Tantalum Ta 180.9479
Hafnium Hf 178.49 Technetium Tc (98)
Helium He 4.00260 Tellurium Te 127.60
Holmium Ho 164.93032 Terbium Tb 158.92534
Hydrogen H 1.00794 Thallium Tl 204.3833
Indium In 114.82 Thorium Th 232.0381
Iodine I 126.90447 Thulium Tm 168.93421
Iridium Ir 192.22 Tin Sn 118.710
Iron Fe 55.847 Titanium Ti 47.88
Krypton Kr 83.80 Tungsten W 183.85
Lanthanum La 138.9055 Uranium U 238.0289
Lawrencium Lr (260) Vanadium V 50.9415
Lead Pb 207.2 Xenon Xe 131.29
Lithium Li 6.941 Ytterbium Yb 173.04
Lutetium Lu 174.967 Yttrium Y 88.90585
Magnesium Mg 24.3050 Zinc Zn 65.39
Manganese Mn 54.93805 Zirconium Zr 91.224
Mendelevium Md (258)
Note: (a) Atomic masses are based on atomic mass of 12C = 12.00
(b) Values in brackets refer to the mass number of the most stable or best-known isotope.
111

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CHEMISTRY 1

2. SAFETY IN THE CHEMICAL LABORATORY

Training Experiment (compulsory)…………………….................2

Chemistry an experimental science and laboratory work constitutes an important

• develop chemical handling skills;

Laboratory Coordinator: Dr. Carmel Abrahams

Technical Officer: Nuchareenat Wiratpruk

1.2 Laboratory Registration

Students must register for a lab day on:

If a class is missed on account of illness, your Demonstrator or the First-Year Laboratory

1.4 Prescribed Items

1. One pair of SAFETY GLASSES or OVERGLASSES (regular glasses are not

1.5 Compulsory Prelab Online Exercise

To access the online Prelab:

• Students will be penalized 2 marks for not having a copy of the

1.6 Pre-Laboratory Instructions

1.7 Laboratory Manual Procedures and Notation

The procedures outlined in this manual conform to consistent notation. Underlined

1.8 Reporting of Results

1.9 Marks and Marking

Demonstrators will give further information on how student performance is assessed.

1.11 Missed Laboratory Sessions

1.12 Laboratory Equipment and Cleaning

Students need to clean up properly

The following texts are referred to in certain experiments.

2. SAFETY IN THE CHEMICAL LABORATORY

2.1 Laboratory Personnel

2.2 Dress Requirements

1. SAFETY GLASSES/OVERGLASSES MUST BE WORN AT ALL TIMES. Even if

2.4 Information About the Chemicals You Use

MSDS are available on the web.

• Respiratory (breathing in gases, vapours and particulate (dust) matter).

2.4.2 Description of Hazard Categories and Rating Scale

4 Danger Explosive material at room temperature

2.5 Risk Minimization and Laboratory Safety

2.6 Laboratory Waste

2.7 Emergency Procedures

2.8 Preparation Room

2.9 Mobile Phones

4 marks for Prelab OH&S receipt and 16 marks for attending.

An Introduction to the First Year Chemistry Laboratory.

The Chemistry Foundations (CHE1CHF) subject at La Trobe seeks to provide

• Station A: Thin layer chromatography and weighing on a top loading balance.

Students MUST be on time for this COMPULSORY session. Students that

1. draw a pencil line 1 cm from the base of one TLC plate;

Fig. 1: Developing TLC.

This Photo by Unknown Author is licensed under CC BY-

Fig. 2: NaCl solid lattice.

Fig. 3: A top loading balance.

Making up solutions of various dilutions is an important generic skill.

If time permits, your demonstrator will then describe how a further 1 in 10

Fig. 4: A serial dilution, showing five 1 in 10 dilutions.

This Photo by Unknown Author is licensed under CC BY-SA-NC

ii) Non-polar molecules

Example: Hexane (C6H14); C is black, H is white.

AgNO3(aq) + NaCl(aq) à AgCl(s) + NaNO3(aq)

3. Using pre-prepared models, representing the above molecules and their

1. Starting ASAP, practice filling a burette.

a) Take burette out of clamp.

Student Name: ______________________ Subject: