PChem Manual Ed 2023

Practical Manual
Year: I
PHYSICAL CHEMISTRY FOR PHARMACY
Lab Technologists: Klaudia T. Angula, Mr Jonathan M. Ortmann & Iyaloo Matheus
Compiler This Ed: JM. Ortmann & KT Angula (PhD)
Year: 2023
School of Pharmacy
Contents
MANUAL 1: PRACTICAL ADDITIONAL INFORMATION, DATA RECORDING SHEETS AND EXERCISES 18
Introduction .................................................................................................................................................... 18
Laboratory etiquette ............................................................................................Error! Bookmark not defined.
Weighing technique ......................................................................................................................................... 27
Pipette technique ............................................................................................................................................. 28
Practical 1: Introductory Practical; Accuracy in Weighing, Measuring Volumes and Calibration of a Pipette . 28
Practical 2: Colligative Properties Molecular Weight Determination by Freezing Point Depression ............... 18
Practical 3: Acid-Base Titration ......................................................................................................................... 23
Practical 4: Heat of a Reaction ........................................................................................................................ 33
Practical 5: Determination of Vapour Pressure and Enthalpy of vaporization ................................................. 42
Practical 6: Solubility Rules ............................................................................................................................... 44
Practical 7: The Standard Free Energy of Formation of the Complex between Salicylic Acid and Ferric Ions . 46
Practical 8: Determination of the Dissociation Constant (Ka), of a weak acid using pH Measurement ........... 47
Practical 9: Chemical Kinetics; Hydrolysis of Methyl Acetate ................................................................... 49
Practical 10: Redox Chemistry ................................................................................................................ 50
MANUAL 2: PRACTICAL BACKGROUND INFORMATION AND EXPERIMENTAL PROCEDURES ........... 55
Practical 1: Introductory Practical; Accuracy in Weighing, Measuring Volumes and Calibration of a Pipette . 55
Practical 2: Colligative Properties Molecular Weight Determination by Freezing Point Depression ............... 19
Practical 3: Acid-Base Titration ......................................................................................................................... 23
Practical 4: Heat of a Reaction ........................................................................................................................ 34
Practical 5: Determination of Vapour Pressure and Enthalpy of vaporization ................................................. 42
Practical 6: Solubility Rules ............................................................................................................................... 46
Practical 7: The Standard Free Energy of Formation of the Complex between Salicylic Acid and Ferric Ions . 49
Practical 8: Determination of the Dissociation Constant (Ka), of a weak acid using pH Measurement. .......... 54
Practical 9: Chemical Kinetics; Hydrolysis of Methyl Acetate ................................................................... 56
Practical 10: Redox Chemistry ................................................................................................................ 65
Appendix 1: t-distribution table ....................................................................................................................... 69
Appendix 2: Periodic Table of Elements ........................................................................................................... 70
17
MANUAL 1: PRACTICAL ADDITIONAL INFORMATION,
DATA RECORDING SHEETS AND EXERCISES
Introduction
WELCOME!
Welcome to the world of physical chemistry! The practical manual aims to help you prepare each week for
either a tutorial or a practical session covering a topic more or less corresponding to the lectures you have
been exposed to.
PRACTICALS
Practicals are concerned with the actual doing rather than with theory. However, good understanding of
the theory is essential for the success of your experiments. Therefore, each session begins with the
background information. It is your responsibility to familiarise yourself with the background information
provided, as well as the practical procedures before you come to the practical. You are less likely to make
mistakes, and waste both time and resources, when you come prepared. When reading through the
procedures, try to understand what you will be doing in each step and why. Make a simple flow diagram of
the steps you will be taking to guide you during the practical. It is easier to follow a flow diagram (with
drawings if you can) than a written procedure. See what you would prefer from the example below:
“Obtain a clean, dry 150 ml beaker and carefully weigh to the nearest 0.001 g; record this weight for beaker 1
on the Report Sheet. Obtain from your instructor a sample of the unknown mixture; use a mortar and pestle
to grind the mixture into a fine powder. With the beaker still on the balance, carefully transfer approximately
2 g of the unknown mixture into the beaker. Record the weight of the beaker with the contents to the nearest
0.001 g. Calculate the exact sample weight by subtraction.”
1. Weigh 150mL 2. Grind unknown 3. Put ±2g of 4. Calculate

beaker; record mixture powder to beaker & sample weight
weigh together
Each practical experiment will be conducted in groups. Split the tasks evenly among your group members
so that everyone participates in some way.. With some practicals the last 30 minutes will be reserved for
assessment, while in others you will be required to write a lab report to be handed in before the next
session.
Presentation of a formal report
There are two types of reports which are acceptable depending on the time available and the purpose of
the exercise. In the first type, the partial report, the laboratory record contains all the essential details
without going into the theory, experimental details or comparison with other methods etc.; these are left
to the second type, the formal report. The main purpose of writing a report is to let other people know the
significance of the experiment. Therefore, it is important that the report be written comprehensively. Many
experiments in Physical Chemistry require formal reports and these must be written individually, even
when the experiment is carried out with a partner or in a group.
Given the experimental results, the discussion can bear personality, or in extreme cases different
conclusions can be drawn. Much time is saved if graphs are plotted as the experiment progresses, since
18
this permits a rapid assessment of the quality and acceptability of the measurements. Reports should be as
short as possible yet contain everything necessary for any other Chemist to be able to understand them
without reference to the instruction sheets. In addition, skill in writing is a worthwhile achievement and a
valuable aid in the industry, medicine, commerce and academic life.
Main features to concentrate on in report writing are:

1. A clear statement of the objective(s) of the experiment
2. A brief description of the method and apparatus
3. Working out the results
4. Presenting the essential conclusions of the theory, the results and calculations in a clear and
systematic manner.
GENERAL FORMAT
NB: The format of the report given below is just a guide and attempts to improve the general presentation
bearing in mind the four features stated above can be made. Under no circumstances is it claimed to be a
perfect model.
FULL REPORT
Title page:
• Your name and student number

• Experiment number and title
• Due date of the report
Introduction:
• Give theoretical background information on the practical (from the theoretical point of view –
principles of the measurement, the theoretical background, what is expected from this experiment
and why).
• If performing a chemical reaction, give the balanced equation.
• When applicable, include structure of the compound being synthesised.
Aim:
• In ONE sentence, give the aim of the experiment (what were you trying to achieve). <E.g. “This
experiment was aimed at calibrating volumetric glassware” or “The aim of this experiment was
to…”>
Methods:
• In a PARAGRAPH, briefly narrate how the experiment was performed. <E.g. “An empty 50 mL
beaker was weighed on a top loading balance. Using a 25 mL pipette, 25 mL of tap water was added
to the pre-weighed 50 mL beaker and the weight was recorded. This was repeated 50 times…”>
• DO NOT WRITE IN POINT FORM!
• You do not need to list the equipment and reagents used.
• Although you are using the lab manual to write the report, rewrite it in your own words; do not
copy word by word from the manual.
• Any additional information not written in the procedure of the manual or any corrections to it
should be noted in this section.
• Methods should always be written in past tense and passive manner (avoid using words like “I”
“me” and “we”). <E.g. Instead of “I/we weighed 0.5 g of NaCl” rather write “NaCl (0.5 g) was
weighed” or “ 0.5 g of NaCl was weighed”>
19
Results:
• Numerical data should be tabulated and supplemented, where necessary, by a summary of other
data necessary for calculations.
• The rows and columns of the table must be clearly and adequately labelled, and units of
measurement must be given.
• Where certain calculations are performed repeatedly, just give the formula used in the calculation
and give one example of how the formula is used and say that the rest of the calculations were done
that way.
• The axis of graphs should be clearly labelled.
• Graphs and tables should also have descriptive heading of what is being shown.
Discussion:
• Interpret the results, do not merely restate the results – what is the significance of the results, how
does it compare with literature etc. (bearing in mind the aim of your experiment)
• It is important to make a point of argument clear and logic consistent. Remember that no results
can be absolutely correct
• Identify sources of errors and suggest ways to improve the result
Conclusion:
Recite briefly the important conclusions of the theory, the results and calculations in a clear and
systematic manner. The precise form is at the student’s discretion, but it might refer to the following:
• Summarize your report in a paragraph

• Did it succeed in demonstrating any particular principles?
• What was the most serious source of inaccuracy?
• How could the experiment be improved in general and with respect to accuracy?
<E.g. “The experiment succeeded in demonstrating the use of two methods in determining the
endpoint of a titration reaction. Although a pH meter may be challenging to use and requires
tremendous skills, it is more accurate in determining the endpoint compared to the use of visual
indicators...” OR “The aim of this experiment which was to determine the endpoint of a titration of HCl
with NaOH using a pH meter and bromothymol blue indicator was achieved. The use of the pH meter
was found to be more accurate in determining the end point and consequently, the equivalence point
as compared to the use of an indicator, except that more skills are required to effectively use the pH
meter(1)”>
References:
• Reference sources should be used mainly for your introduction and discussion of your report. It is
the law to reference both in-text (citing) and at the end of the report. References used in-
text must appear on the reference list.
• Use at least TWO other sources in addition to the lab manual.
• Please reference properly using the the Vancouver referencing style.
➢ www.physicalchemistrylabs
PARTIAL REPORT
The partial report should contain the following:
• Title page
• Aim
• Results
20
• Discussion
• Conclusion
• References
Please note:
• Practical assessments are a significant component of your continuous assessment. Please take time
in compiling your reports – they do count.
• It is your responsibility to sign the attendance register when you come to the practical. Failure to
sign the attendance register leads to an assumption that you were not in class which in turn lead to
you being given a zero for that practical (even if you submit a report). NO PRACTICAL ATTENDANCE,
NO MARK.
• Submit your report at the beginning of the following practical. It is your responsibility to make sure
you have a printed copy ready before the start of the practical session.
21
Laboratory Safety & Equipment
Learning Objectives
• To learn and adhere to the proper conduct, proper protective clothing, and safety rules when in
the laboratory.
• To be familiar with the proper handling of common laboratory equipment.
• To be able to interpret warning labels and safety signs.
• To know how to prevent accidents and learn the first aid steps in case of an accident.
PROPER CONDUCT IN THE LABORATORY
1. Be PUNCTUAL to all 3. Pranks, fooling around,

laboratory sessions. Late- running around or any other
comers without a valid excuse unprofessional behaviour
will not be allowed in. will NOT be tolerated.
4. Pay attention to all
2. Be RESPECTFUL toward the
information presented
authority of the lab technician
throughout the practical and
facilitating the practical.
FOCUS on the experiment.
PROTECTIVE CLOTHING
Laboratory Coat
➥ Wear your lab coats at all times in any lab setting.
➥ Button up to ensure maximum protection.
➥ Long-sleeved lab coat is mandatory in any chemical or biological lab setting.
Eye Protection
➥ Wear protective eyewear at all times in a chemical lab setting.
➥ Take note that harmful substances can be drawn behind contact lenses by
capillary action, making it hard to wash out the eyes.
➥ If you wear glasses, place the lab goggles over them to ensure maximum safety.
Closed Shoes
➥ Always wear closed shoes in any laboratory setting.
➥ This means no high heels, open-toed shoes, or any shoes that pose a risk to
tripping or exposure to chemicals.
Gloves
➥ Always wear gloves where the practical requires it.
➥ If you are allergic to latex, notify the laboratory technician so that you can be
accommodated.
22
LAB SAFETY RULES
✓ DOs  DON’Ts
1. Adhere to ALL safety rules
communicated to you either in 1. NO eating, drinking and
writing, verbally or by means applying make-up!
of appropriate signage.
2. Familiarize yourself with the
2. NO electronic devices such
practical procedure BEFORE
as laptops, mobile phones or
the practical & be aware of any
tablets!
necessary safety precautions.
3. Know where the eyebaths, fire
3. NO unauthorized
extinguishers, fire-blankets,
experiments may be
emergency showers and first
conducted.
aid kits are located.
4. Report any personal injury, 4. NO loose long hair or
chemical spills, or equipment clothing. Tie your hair back
breakages to the lab neatly and tuck away any
technician. loose clothing.
5. Clean the working area and all

5. NEVER leave an experiment
the equipment used before
unattended.
leaving the laboratory.
6. NEVER pour chemicals

6. Wash hands thoroughly before down the drain unless
leaving the laboratory. permitted to do so by the lab
technician.
6. Adhere to the proper waste

disposal of any material used
in the laboratory.
23
LAB SAFETY SIGNS
NATIONAL FIRE PROTECTION ASSOCIATION HAZARD LABELS
The National Fire Protection Association has developed a visual guide for a number of chemicals that offer
a quick review of the health hazard, flammability, reactivity and special hazards a chemical may present.
The diamond shaped design is broken into four sections (blue, red, yellow and white). The symbols and
numbers in the four sections indicate the degree of hazard associated with a particular chemical or material.
24
25
ACCIDENT PREVENTION & FIRST AID
➥ Always wear protective eyewear.

➥ Any chemical should be poured slowly.
➥ Never point a pipette into your face.
➥ If chemicals enter the eye wash out immediately at the nearest tap or eyebath.
➥ Washing should continue for at least 10 minutes
➥ Never wash an acid splash out with a base or vice versa.
➥ After the eyes have been thoroughly rinsed seek professional medical attention.
➥ Never grab equipment without checking its temperature (especially glass).

➥ Always use tongs or forceps to move heated objects.
➥ Never leave flames or other heating sources unattended.
➥ Cool at once under running water.

➥ Do not cover burns with cloths and oily or greasy ointments.
➥ Do not puncture blisters
➥ Seek medical attention
➥ Most cuts occur when handling glass.

➥ Always handle glass with care. Where necessary use a cloth to manipulate glass through
stoppers etc.
➥ Small cuts should be allowed to bleed, then disinfect and bandage.

➥ Large cuts need to have their bleeding stopped and be bandaged. Seek medical
attention immediately.
➥ Stop bleeding by raising the affected limb.
➥ If bleeding persists apply pressure to appropriate pressure point or directly to the
wound using a large dressing.
➥ Never taste or ingest any chemical.

➥ Perform all experiments producing noxious gases in a fume hood.
➥ Seek medical attention immediately.

➥ Take with sample or be able to identify the poisonous agent.
➥ In case of gaseous poisoning remove affected individuals from area and seek medical
attention immediately.
26
Weighing technique
The following procedures should be used when weighing on an analytical balance:
1. The balance must be placed on a heavy table e.g. marble table to minimize the effect
of vibrations on the reading.
2. At the point of use, check that the balance is level. The air bubble should be centred
within the circle of the level indicator. If not call a technologist to help (level the
balance using the levelling feet).
3. Note the maximum capacity of the balance. The analytical balance has a maximum
capacity of 220 g and the top loader has a maximum capacity of 600 g. If the weighing
vessel or the weighing vessel plus the sample is heavier than the maximum capacity
the weigh display will show “H”.
4. Note the readability of the balance. The analytical balance has a readability of 0.1 mg
(0.0001 g) while the top loader has 0.01 g. These balances should thus be used for
accurate weighing only; namely where the weight must be accurate within 0.1 mg or
0.01 g etc.
5. Press the ON/OFF button to switch the balance on or off.
6. Press “T” (the yellow bar) before weighing if the weight does not read 0.0000g.
7. Open one of the sliding doors of the balance and carefully place the clean weighing
vessel on the balance pan. The mass of the empty vessel is called the tare. By pressing
“T” again the tare reading will reset to zero. NB! To prevent mass change do not handle
the tared vessel too much.
8. Remove the vessel from the pan. The weighing display will show the mass of the empty
vessel again but with a minus sign in front. The mass of the empty vessel has thus been
subtracted automatically. Now add the sample to be weight to the vessel, place it back
onto the pan and record the mass of the sample.
9. Chemicals should never be placed directly onto the pan. This precaution protects
the balance from corrosion and allows you to recover the entire chemical being weighed.
10. An alternative procedure called “weighing by difference” is necessary for hygroscopic
reagents which rapidly absorbs moisture from the air. First weigh a capped bottle
containing the dry reagent. Then pour some reagent from the weighing bottle into a
receiver, cap the weighing bottle and weigh it again. The difference equals the mass of
reagent delivered to the receiving vessel.
Preventing weighing errors
27
1. Do not lean, press or write on the balance bench. Be careful not to bump the balance.
2. Samples should be at ambient temperature, namely the temperature of the surroundings
before weighing to avoid errors due to convective air currents. A sample that has been
dried in an oven usually takes about 30 minutes to cool to room temperature.
3. The glass doors of the analytical balance must be closed during weighing to prevent air
currents from affecting the reading.
4. Make sure your weighing vessel is clean and dry on the outside before placing it on the
balance pan.
5. Make sure the balance pan is clean and dry.
Pipette technique
(a) Make sure the pipette is clean. Rinse the pipette with water and then twice with the
sample solution to replace the water.
(b) Make sure you know how to use the pipette filler pump/bulb!
(c) Suck the solution into the pipette using a pipette filler pump (not your mouth) until it is
well above the graduation mark. Do not suck it into the pipette filler pump!! Insert only
the tip of the pipette onto the liquid that is being sucked up. Make sure the tip of the
pipette is below the surface of the solution. Remove the pipette from the solution.
(d) Wipe away any liquid adhering to the outer side of the pipette stem. Adjust the level of
the meniscus, keeping the pipette vertical and the graduation mark to eye level. The
bottom of the meniscus should be brought in line with the graduation mark. The excess
liquid can be dropped back into the bulk of the solution. The tip of the pipette is
‘touched off’ onto the side of the container to remove any adhering droplets.
(e) Bring the pipette tip slowly over the receiving vessel and drain the contents completely.
(f) The pipette must be held vertically during deliver and drainage. Touch the wall of the
receiving vessel when draining the pipette, do not drain the pipette with the tip below
the surface of the liquid in the container and take care to avoid any splashing. Remove
the last drop by resting the tip against the wall of the container for about 15 seconds.
Don’t blow out the remaining liquid. The pipettes used in this and most other
laboratories are calibrated for this kind of discharge.
Practical 1: Introductory Practical; Accuracy in Weighing, Statistical

Calculations, Measuring Volumes and Calibration of a Pipette
28
EXPERIMENTAL
PART 1: Measuring the density of Antifreeze
Data Recording Sheet: Weighing: Density of antifreeze
Temperature of antifreeze: __________________oC
Trial 1 Trial 2 Trial 3

Mass of flask +
antifreeze
Mass of empty flask
Density of antifreeze
Show calculations
1. Use the measured mass and volume to calculate the density of the antifreeze for each
measurement.
2. Using the three values for the density, calculate:
(a) The mean density(𝑥),
(b) The average deviation (s) from the mean from your determinations and
(c) Estimate the error in measurements using the t-test at 95% confidence interval (CI).
The t-distributions table is in appendix A.
𝑡𝑠
𝜇 = 𝑥̅ ±
√𝑛
= 𝑥 ± 𝐶𝐼
3. Complete the data sheet and answer questions.
Questions
1. What is the maximum capacity of the analytical balances in our laboratory?

2. Why must you press ‘T’ before weighing?
3. Why must you be careful not to bump or lean on the balance bench?
4. What must you do if after zeroing the balance, while you are busy weighing out a
chemical powder and by accident spill some on the balance pan?
5. What will happen to the readings if you try to weigh a sample that is still wet?
6. Why is it more correct to refer to the mass of a body rather than to its weight?
PART 2: Calibration of a pipette
Temperature and density are some of the factors that affect the accuracy of pipetting. Table 1
below shows the standard density (g/ml) of water at specific room temperatures.
29
Table 1: Density (g/ml) of water
Temp (oC) Density Temp (oC) Density Temp (oC) Density
10 0.9997026 18 0.9985986 26 0.996787
11 0.9996084 19 0.9984082 27 0.996516
12 0.9995004 20 0.9982071 28 0.996237
13 0.9993801 21 0.9979955 29 0.995948
14 0.9992474 22 0.9977735 30 0.995650
15 0.9991026 23 0.9975415
16 0.9989460 24 0.9972995
17 0.9987779 25 0.9970479
30
Part 2A: Data Recording Sheet
Temperature of water used to calibrate the pipette
Temperature of water before calibration: ___________℃

Average Temperature: ________℃
Temperature of water after calibration: ___________℃
Part 2A
Stated volume of pipette = ________ mL
Trial 1 Trial 2 Trial 3 Trial 4
Mass of Erlenmeyer plus

1
25mL H2O (g)
2 Mass of Erlenmeyer (g)
Mass of 25 mL H2O
3
(1 - 2) (g)
Volume delivered by the

4 pipette
(show calculations)
___________mL ___________mL ___________mL ___________mL
Mean volume of water delivered by the pipette (show calculation):
Average Volume delivered: ___________ mL
Trial 1 Trial 2 Trial 3 Trial 4
Deviation of the
delivered volume
from the mean
(show calculation)
Average deviation from the mean (show calculation below)
Average deviation from mean: _____________mL
Volume delivered by your 25-mL pipette _______________mL ± _______________mL
31
Calculations
• By subtraction, calculate the mass of water delivered by the pipette on each occasion.
Calculate the mean temperature, the mean mass and the deviation of these masses from
the mean and calculate the standard deviation.
• Use the examples below as a guide:
EXAMPLE 1
The following volumes were obtained for the calibration of a 10-mL pipette: 10.15 mL, 10.12
mL and 10.00 mL. Calculate the mean and average deviation from the mean.
SOLUTION:
(10.15 + 10.12 + 10.00)
𝑀𝑒𝑎𝑛 (𝑥̅ ) = = 𝟏𝟎. 𝟎𝟗 𝒎𝑳
3
Deviation from the mean is given by: deviation from mean = |value - mean|
Thus, for the three measurements, their deviation (Dev.) from the mean is given by:
Dev. Measurement 1 = |10.15 – 10.09| = 0.06 mL
Hence the standard deviation (s) is:
∑(𝑥 − 𝑥̅ )2
𝑠=√
𝑛−1
(0.06)2 + (0.03)2 + (0.09)2

𝑠 =√ = 𝟎. 𝟎𝟖 𝒎𝑳
3−1
The reported value is therefore;
𝑥̅ ± s
∴ 10.09 ± 0.08 mL
32
Part 2B: Data Recording Sheet –Calibration of a Pipette
Temperature of water used to calibrate the pipette
Temperature of water before calibration: ___________℃

Average Temperature: ________℃
Temperature of water after calibration: ___________℃
Volume transferred with the pipette = _________mL
Mass of beaker Mass of beaker + 8mL water Mass of 8mL water Temp. of water
(g) (˚C)
(g) (g)
(1)
(2)
(3)
(4)
Calculation
• By subtraction, calculate the mass of water delivered by the pipette on each occasion.
• Calculate the mean temperature, the mean mass of the water, the standard deviation and
the standard error of the mean (SE) (deviation of these masses from the mean).
𝒔
𝑺𝑬 =
√𝒏
𝑥̅ ± 𝑺𝑬
Calculate the volume of water delivered or contained in the vessel and the discrepancy between
the theoretical volume (8.00mL) and the volume calculated
(a) Mean mass of water:

(b) Mean temp. of water:
(c) Deviation of these masses from mean:
(d) Standard deviation:
(e) Mean volume of water delivered by pipette:
(f) Discrepancy between stated volume and mean volume:
(g) Volume delivered by your 10 mL pipette:………..mL ( =…….
Part 2B: Questions to be answered
Questions
1. Explain why the pipette must be rinsed with the sample solution?
2. Why must the pipette be vertical and level with the eye when adjusting?
3. What is meant by the term aliquot?
4. Why is not necessary to dry the inside of the beaker before beginning the repeat of the
procedure.
33
Practical 2: Colligative Properties Molecular Weight Determination by
Freezing Point Depression
MOLAR MASS CALCULATIONS
The molecular mass (molar mass) of a solute can be determined by changes in the freezing
point or boiling point. The freezing point method is more practical because of the greater
temperature interval involved. It also can be more accurately measured since the boiling point
is more sensitive to atmospheric pressure changes than the freezing point.
In this experiment, you will use glacial acetic acid, HC2H3O2, as the solvent. Glacial acetic acid
has a freezing point of 16.7 0C and a Kf value of 3.9 0C/m. Since the measured freezing point
of a substance depends upon its purity, the atmospheric pressure, and the calibration of the
thermometer, you must first determine the freezing point of your sample of pure glacial acetic
acid under the conditions of this experiment. Then, after adding a measured quantity of an
unknown solute to the solvent, you will measure the freezing point of the solution.
You can calculate the molecular weight (MW) of the solute from these relationships:
1. Freezing point lowering, ∆𝑇𝑓 = 𝑇𝑓0 − 𝑇𝑓 = 𝐾𝑓 × 𝑚 × 𝑛, where Tf 0 is the freezing

point of the pure solvent, Tf is the freezing point of the solution, m is the molality with
respect to the solute, and n is the number of solute particles formed in solution (for
example, n = 2 for NaCl).
(𝑔𝑟𝑎𝑚𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒)
2. Moles of solute = = g / MW
𝑀𝑊 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒
3. Kg of solvent = (𝑔𝑟𝑎𝑚𝑠 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡) / (1000 𝑔. 𝐾𝑔−1 )
4. Molality of the solution, m = (𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒) / (𝑘𝑔 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡)
By substitution, we can derive the following equation for simple determination of molar mass
by using freezing point depression:
(𝑲𝒇 )(𝒈𝒔𝒐𝒍𝒖𝒕𝒆 )(𝒏)

𝐌𝐖𝐬𝐨𝐥𝐮𝐭𝐞 =
(∆𝑻𝒇 )(𝒌𝒈𝒔𝒐𝒍𝒗𝒆𝒏𝒕 )
where n is the number of moles of solute particle(s) per mole of solute.
Example 2:
Calculate the freezing point of a solution containing 3.60 g of glucose, C6H12O6 , in 50.0 g of
water. The molecular mass of glucose is 180.0 g/mol, the normal freezing point of pure water,
Tf 0, is 0.00 0C, and Kf for water is 1.86 0C/m.
18
Answer:
• First calculate the molality of the solution:
𝐌𝐚𝐬𝐬 𝟑. 𝟔𝟎 𝐠
𝐌𝐨𝐥𝐚𝐥𝐢𝐭𝐲 = = = 𝟎. 𝟒𝟎𝟎 𝐦
𝐌𝐨𝐥𝐞𝐜𝐮𝐥𝐚𝐫 𝐦𝐚𝐬𝐬 𝟏𝟖𝟎. 𝟎 𝐠/𝐦𝐨𝐥
• Then calculate ∆Tf:
∆𝑻𝒇 = 𝑲𝒇 × 𝒎 × 𝒏 = (𝟏. 𝟖𝟔 ℃/𝐦)(𝟎. 𝟒𝟎𝟎 𝐦)(𝟏) = 𝟎. 𝟕𝟒𝟒 ℃
• The freezing point of the solution is lowered by 0.744 0C. To determine the freezing point of the
solution, subtract the change in the freezing point from 0.00 0C (the freezing point of pure water):
∆𝑻𝒇 = 𝑻𝒇 ° − 𝑻𝒇 ⟹ 𝑻𝒇 = 𝑻𝒇 ° − ∆𝑻𝒇 = 𝟎. 𝟎𝟎 ℃ − 𝟎. 𝟕𝟒𝟒 ℃ = −𝟎. 𝟕𝟒𝟒 ℃
• Therefore, the freezing point of the solution is −0.744 ℃.
Example 3:
What is the molecular mass of an organic compound if a solution of 3.25 g of the compound in
125.0 g of water has a freezing point of − 0.930 0C?
Answer:
• First calculate the freezing point change, ∆Tf :
∆𝑻𝒇 = 𝑻𝒇 ° − 𝑻𝒇 = 𝟎. 𝟎𝟎 ℃− (−𝟎. 𝟗𝟑𝟎 ℃) = 𝟎. 𝟗𝟑𝟎 ℃
• For non-ionic organic compounds, n=1. Therefore:
(𝑲𝒇 )(𝒈𝒔𝒐𝒍𝒖𝒕𝒆 )(𝒏) (𝟏. 𝟖𝟔 ℃/𝒎)(𝟑. 𝟐𝟓 𝒈)(𝟏)

𝐌𝐖𝐬𝐨𝐥𝐮𝐭𝐞 = = = 𝟓𝟐. 𝟎 𝐠/𝐦𝐨𝐥
(∆𝑻𝒇 )(𝒌𝒈𝒔𝒐𝒍𝒗𝒆𝒏𝒕 ) (𝟎. 𝟗𝟑𝟎 ℃)(𝟎. 𝟏𝟐𝟓𝟎 𝒌𝒈)
• Verify that the proper units of molecular weight, g/mol, do indeed result from the calculation.
Figure 1. Freezing curve for a pure solvent and solution.
19
PRACTICAL 2: Review Questions and Exercises
Due before lab begins (to be handed in). Answer on a separate sheet of paper and attach to this page.
1. Define the following terms:

a. Solute
b. Solvent
c. Solution
2. What safety rules must be observed during this experiment?
3. Why is a molality concentration scale used in the context of colligative properties and not the more
common concentration scale molarity?
4. Assume that you have a solution of an unknown solute in cyclohexane. If the solution has a freezing
point depression of 9.50 0C, what is the molality of this solution? (The freezing point depression
constant for cyclohexane (Kf) is 20.4 0C/m).
5. Cyclohexanol, C6H11OH, is sometimes used as the solvent in molecular weight determination by
freezing point depression. If 0.253 g of benzoic acid, C 6H5COOH, dissolved in 12.45 g of cyclohexanol,
lowered the freezing point of pure cyclohexanol by 6.55 0C, what is the molal freezing point constant
(Kf) of this solvent?
6. Calculate the freezing point of 0.1 m aqueous solutions of a) NaCl b) Glacial acetic acid
7. Calculate the boiling point of 0.1 m aqueous solutions of a) BaCl2 b) sucrose
8. What is supercooling? How can it be minimized?
9. Distinguish between non-volatile and volatile substances. Give two examples of each.
10. When 0.49 g of a molecular compound was dissolved in 20.00 g of cyclohexane, the freezing point of
the solution was lowered by 3.9 0C. Determine the molecular mass of this compound.
(Kf = 20.4 0C/m)
20
PRACTICAL 2: Data Recording Sheet
Surname, Initials:_____________________ Course:________ Date:________
Student Number:_____________________ Group:________ Table:________

Calculate the following and show your calculation (to be handed in with lab report):
1. Volume of glacial acetic acid ___________ mL
2. Mass of glacial acetic acid (show calculation) ___________ g ___________ kg
3. Freezing point of pure glacial acetic acid (Tf 0) from graph __________ 0C
4. Mass of unknown used ___________ g
5. Freezing point of the solution (Tf) from graph ___________ 0C
6. ∆Tf (#3 - #5) ___________ 0C
7. Molecular weight of unknown ___________ g/mol
21
Data – Temperature vs. Time
Glacial Acetic Acid
Time (sec) 0 30 60 90 120 150 180 210 240 270 300
Temperature
(oC)
Solution (Glacial Acetic Acid +Unknown)
Time (sec) 0 30 60 90 120 150 180 210 240 270 300
Temperature
(oC)
PRACTICAL 2: Post-Laboratory Questions & Exercises
Due after completing lab (to be handed in with lab report). Answer on a separate sheet of paper and
attach to this page.
1. Define the following terms:
a) Molality
b) Colligative properties
c) Freezing point depression
2. What was the objective of this experiment and how was it achieved?
3. If 0.2436 g sample of an unknown substance was dissolved in 20.0 ml cyclohexane. The density of
cyclohexane is 0.779 g/ml. The freezing point depression (∆Tf) was 2.5 0C. Calculate the molar mass
of the unknown substance.
4. How many moles of solute particles are there in one mole of the following substances? (n = ?):
a) sodium sulfate, Na2SO4
b) naphthalene, C10H8
c) sodium phosphate, Na3PO4
5. How many grams of ethylene glycol, C2H5(OH)2, must be dissolved in 200.0 g of water to lower the
freezing point to –29.75 0C?
22
Practical 3: Acid-Base Titration
Data Recording Sheet
Record your results in a table below (to be handed in with lab report).
Table 1:
Trial 1 Trial 2 Average
Average
pH
Volume Volume volume
Burette pH Burette pH (pH 1+pH
added added (V1+V2)
reading (pH 1) reading (pH 2) 2)
(V1) (V2) 2
2
Table 2:
Change in Change in
Volume of NaOH Average
volume pH (∆𝑝𝐻) ∆𝐩𝐇
added (actual burette pH volume
(∆𝑉) = pH 2 – pH ∆𝐕
reading in mL) (V2+V1)/2
= V2 – V1 1
1.11
0.00 (V1)
(pH 1)
1.23
3.00 (V2) 3.00 0.12 =(3.00+0.00)/2
(pH 2)
6.30 3.30
23
Post-Laboratory Questions & Exercises
Due after completing lab (to be handed in with lab report):
1. Draw a titration curve (pH vs Vol. of NaOH added). The appearance of the graph will be
graded.
2. Make a table of changes in pH and in volume. Take the successive pairs of readings: pH1
and pH2 and V1 and V2. Also work out the change in pH per change in volume and the
average volume.
∆𝑝𝐻
3. Plot a graph of vs average volume. This is a first derivative plot for the titration curve.
∆𝑉
∆𝑝𝐻
4. From the graph of vs average volume, estimate the volume of NaOH added (to 2
∆𝑉
decimal places) at the equivalence point. The equivalence point should appear as a peak
on this graph. Use this volume to estimate the pH at the equivalence point from your
titration curve.
5. Compare the appearance of the three titration curves (SA-SB, WA-SB and SA-WB).
6. Compare the pH at the equivalence point for the three titrations.
32
Practical 4: Heat of a Reaction
Example (Heat of Solution):
In an experiment, 1.2g of sodium hydroxide pellets, NaOH(s), were dissolved in 100mL of

water at 25oC. The temperature of the water rose to 27.5oC. Calculate the enthalpy change
(heat of solution) for the reaction.
Answer:
• Calculate the heat released, in J, by the reaction:
−𝐪 = 𝐦 × 𝐂 × ∆𝐓 = 𝟏𝟎𝟎𝐠 × 𝟒. 𝟏𝟖𝟒 𝐉. 𝐊 −𝟏 . 𝐠 −𝟏 × (𝟐𝟕. 𝟓 𝐊 − 𝟐𝟓 𝐊) = 𝟏𝟎𝟒𝟔 𝐉
• Calculate the moles of solute (NaOH(s)):
𝐦 𝟏. 𝟐 𝐠
𝐧= = = 𝟎. 𝟎𝟑𝟎 𝐦𝐨𝐥
𝐌𝐑 (𝟐𝟐. 𝟗𝟗 + 𝟏𝟔. 𝟎𝟎 + 𝟏. 𝟎𝟎𝟖)𝐠/𝐦𝐨𝐥
• Calculate the enthalpy change, ∆H, in kJ/mol of solute:
−𝐪 −𝟏𝟎𝟒𝟔 𝐉
∆𝐇 = ÷ 𝒏𝒔𝒐𝒍𝒖𝒕𝒆 = ÷ 𝟎. 𝟎𝟑𝟎 𝐦𝐨𝐥 = −𝟑𝟓 𝐤𝐉/𝐦𝐨𝐥
𝟏𝟎𝟎𝟎 𝟏𝟎𝟎𝟎
∆H is negative because the reaction is exothermic (energy is released).
For more examples, visit http://www.ausetute.com.au/heatreact.html
33
Practical 4: Data Recording Sheet
Hydration of Concentrated Sulfuric Acid:
Temperature of water
Temperature of water after adding
acid
Temperature change
1. Is this an endothermic or exothermic

reaction? ………………………………………………………………………………
2. In this reaction, what is the major change, in terms of bonds made or broken, that causes the heat
effect? ………………………………………………………………………………………………………………………………………
3. If you had used dilute sulfuric acid rather than concentrated sulfuric acid, would you expect the
temperature change to be greater or less? Why?
………………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………………
………………………………………………………………………………………………………………………………………………………………
Dissolving of Ammonium Chloride:
Temperature of water
Temperature of water after adding
salt
Temperature change
1. Is this an endothermic or exothermic

reaction? …………………………………………………………………….…………
2. If you had used 40 mL of water and 6 g of ammonium chloride, rather than the 20 mL and 3 g in
the experiment, would you expect to get a larger, smaller, or identical temperature change? Why?
………………………………………………………………………………………………………………………………………………………………
……………………………………………………………………………………………………………………………………………….
40
Neutralization reactions:
Neutralization 1:
Temperature of acid and

water
Temperature of
neutralization
Temperature change
Neutralization 2:

water
Temperature of
neutralization
Temperature change
Neutralization 3:

water
Temperature of
neutralization
Temperature change
Neutralization 4:

water
Temperature of
neutralization
Temperature change
Neutralization 5:

water
Temperature of
neutralization
Temperature change
Treatment of Data
For each of the above reactions:
1. Calculate the heat released.

2. Calculate the heat (enthalpy) of reaction.
3. Compare the heat of reaction for the neutralization steps.
41
Practical 5: Determination of Vapour Pressure and Enthalpy of vaporization
TREATMENT OF DATA
1. Correct all volume readings by subtracting 0.2 ml to compensate for the inverted
meniscus. Using the measured values for the volume and temperature from step 7 and the
atmospheric pressure, calculate the number of moles of the trapped air. Assume that the
vapour pressure of the water is negligible compared to atmospheric pressure at the low
temperature.
2. For each temperature, calculate the partial pressure of air in the gas mixture as follows:
Pair = pressure of air
𝒏𝒂𝒊𝒓 𝑹𝑻 nair = number of moles of air
𝑷𝒂𝒊𝒓 = V = volume (m3)
𝑽
R = universal gas constant (Joule/mol K)
T = temperature (K)
3. Calculate the vapour pressure of water at each temperature i.e.
𝑷𝒘𝒂𝒕𝒆𝒓 = 𝑷𝒂𝒕𝒎 − 𝑷𝒂𝒊𝒓 Patm = atmospheric pressure
Ask the demonstrator for this value. (An optional, small correction may be made by
correcting for the effect of the difference in water levels).
1
4. Plot lnPwater versus and draw the best straight line through the points. Determine the
𝑇
slope and using the Clausius-Clapeyron equation, calculate ∆Hvapour. Find the value of
vapour pressure at 65 °C using the graph.
42
Record your results in a table below (to be handed in with lab report).
Atmospheric pressure is 1 atm.

• 1 atm = 101.3 kiloPascal (kPa) = 760 mmHg = 760 torr.
• 1 bar = 100 kPa
• R =0.08214 K mol.atm.L-1 = 8.314 K.mol.J
Volume of air Moles of air Partial Partial pressure of

Temp Temp Volume of air
trapped trapped pressure of air water
oC (K) trapped (ml)
(L) (n) (Pair) (Pwater)
≤5
Room
temp.
50
55
60
65
70
75
80
1/T (K-1) lnP water
43
Practical 6: Solubility Rules

PART A:
1. Summarize your findings in the table below (fill in the rest as shown):
Cation Anion
Name Symbol Cl- NO3- SO42-
Potassium K+ ✓ ✓ ✓
Sodium Na+
Ammonium NH4+
2. Use the information contained in your table to complete the following general “rules” on the
solubility of various types of salts in aqueous solution:
• All nitrates are [soluble/insoluble] in aqueous solution.
• All chlorides are [soluble/insoluble] in aqueous solution, except ______________________________________
• All sulphates are [soluble/insoluble] in aqueous solution, except _____________________________________
3. You could possibly also draw the following conclusion from your observations: “All sodium, potassium
and ammonium compounds are ____________________________________________________________”
4. How reliable do you think this conclusion would be, and why?
____________________________________________________________________________________________________________________
____________________________________________________________________________________________________________________
____________________________________________________________________________________________________________________
____________________________________________________________________________________________________________________
44
PART B:
1. Record your results in the table below.
Cation Carbonate Hydroxide

Addition of Addition of
Name Symbol CO32- Acid (2M OH- Acid (2M
HNO3) HNO3)
Potassium K+
Sodium Na+
Ammonium NH4+
Indicate with a tick (✓) in the table. If no precipitate forms, there is no need to test with HNO 3.
2. As in Part A, use the information in your table to complete the following solubility rules:
• All carbonates are [soluble/insoluble] in water, except _________________________________________________
• All hydroxides are [soluble/insoluble] in water, except ________________________________________________
3. What can you conclude about the solubility of carbonates in acid and of hydroxides in acid?
____________________________________________________________________________________________________________________
____________________________________________________________________________________________________________________
____________________________________________________________________________________________________________________
4. From your observations, extend your rules to describe the effect of adding:
• Acid to a carbonate _________________________________________________________________________________________
• Acid to a hydroxide _________________________________________________________________________________________
PART C:
Identification of bottles:
A _____________________________________________
B _____________________________________________
C _____________________________________________
D _____________________________________________
45
Practical 7: The Standard Free Energy of Formation of the Complex
between Salicylic Acid and Ferric Ions
Treatment of results (to be handed in with lab report).

1. Plot a graph of absorbance against mole fraction of ferric for the mixtures made from the
equimolar solutions. The maximum in the curve gives the empirical formula of the
complex.
2. Plot the absorbance values for the second part of the experiment against concentration of
ferric ions. If the Beer-Lambert Law holds, the graph should be a straight line through the
origin. Draw the best straight line through the points and from the slope of the graph
calculate the molar extinction coefficient of the complex.
3. Use the value of the molar extinction coefficient to find the concentration of the complex
in the 5:5 reaction mixture. Since the formula of the complex has been found, it is now
possible to calculate by difference the concentration of uncombined Salicylic Acid and
Fe3+ present in the mixture and hence Kc for the reaction.
4. Using the Kc value, calculate the standard free energy of formation of the complex from
the expression: ∆G° ≈ - RT lnKc = -2.203 RT log10 Kc (R = 8.314 JK-1mol-1)
5. What extra information would be needed to predict the effect of altering the temperature
on Kc?
46
Practical 8: Determination of the Dissociation Constant (Ka), of a weak
acid using pH Measurement.

PART A:
Table 2: Experimental data
Burette Reading Volume of Burette Reading Volume

(CH₃COOH) CH₃COOH (NaOH) of NaOH pH of
Trail (mL) (mL)
added added mixture
Final Initial (mL) Final Initial (mL)
Table 3: Calculation Results
[CH₃COOH]
[CH₃COOˉ] in mixture log [CH₃COOˉ]
Trail pH of mixture (undissociated) in
(mol/L) [CH₃COOH]
mixture (mol/L)
1
Calculations:
1. Show a sample calculation for each of the following using the mixture from Trail 1 only
and complete Table 3 for all the mixtures.
a. [CH₃COOˉ] in equilibrium mixture
b. [CH₃COOH] (undissociated) in equilibrium mixture
[CH COO− ]
c. log [CH 3COOH]
3
47
2. Answer the following:
[CH COO− ]
a. Use the above result to make a plot of pH (y axis) versus log [CH 3COOH] on a graph
3
paper.
b. Determine the pKₐ from the graph (indicate on the graph) and calculate Kₐ.
PART B:
Table 4: Titration Data

1st Titration 2nd Titration
Burette reading CH₃COOH NaOH CH₃COOH NaOH
Final reading (mL)
Initial reading (mL)
Volume added (mL)
Average volume of NaOH added = _______________________________
Table 5: pH of mixture with half average volume of NaOH
Burette reading CH₃COOH NaOH pH of mixture

Final reading (mL)
Initial reading (mL)
Volume of CH₃COOH
x
added (mL)
Volume of NaOH
x
added (mL)
Post-lab questions:
1. What is the significance of the pH value that you have found in Part B. Explain your
answer.
2. State at least two possible sources of error in this experiment and its influence on the
value of the Kₐ determined by you.
48
Practical 9: Chemical Kinetics; Hydrolysis of Methyl Acetate
Calculations
The difference (V∞ – Vt) is proportional to the concentration of ester left (unhydrolysed) at
time t, where Vt is the volume of NaOH required in titration (for the mixture that had reacted
in time t) and V∞ is the volume of NaOH required for the mixture that completed the reaction
(boiled). A plot of ln(V∞ – Vt) versus t will give a straight line with a gradient of -k.
49
Practical 10: Redox Chemistry

Record your results below (to be handed in with lab report).
Part A: Colours of Halogens in cyclohexane
Cl2: __________________________
Br2: __________________________
I2: ____________________________
Part B: Reactions of Halogens with the Halides
Cl− Br− I−
Cl2 3. 5.
Br2 1. 6.
I2 2. 4.
Part C: Reactions of Other Common Oxidizing Agents in Acidic Solution
Br− I−
Upper layer 7. 8.
MnO4−
Bottom layer
Upper layer 10. 9.
Fe3+
Bottom layer
Part D: Reaction of MnO4– with I– in basic solution
I–
Upper layer 11.
MnO4–
Bottom layer
50
QUESTIONS:
A. You have made 11 observations. Each one has been numbered. Consider the first 10 observations.
Indicate those cases in which no reaction occurred as such. If a reaction occurred, write a balanced
equation that is in accord with your observations.
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
51
B. Consider the 11th observation:
i. The ultimate product that results from the oxidation of I − in this reaction is IO3−. Although your
observation will not prove that this colourless ion was formed, show that your results indicate that
I2 was not formed.
ii. The colour of the aqueous layer will enable you to deduce the unambiguous product from the
reduction of MnO4−. What is that product?
iii. Write a balanced reaction equation for the reaction.
iv. How do the reactions in acidic and basic solutions differ?
C. Answer the following:

i. Rank the oxidizing strengths of the halogens according to your results. Explain.
ii. Rank the reducing strengths of the halides. Explain.
iii. Rank the oxidizing strengths of MnO4– and Fe3+. Explain.
52
Exercise 2: Redox reaction
Summary of Steps for balancing redox in acidic medium:
1. Split the equation into two half reactions.
2. Balance any atom other than O or H first.
3. Balance O's using H2O. Add as many waters as needed to balance the oxygens on the side deficient in
oxygen.
4. Balance H's using H+. Add as many H+ ions as needed to the side deficient in H.
5. The mass should now be balanced. To balance the charge, determine the charge on each side of the
reaction, and add as many electrons to the more positive side as needed to make the charge the same
on both sides.
6. Repeat steps 1 through 4 for both half reactions.
7. If the number of electrons lost does not equal the number of electrons gained, find the common
multiple and multiply each half reaction by the necessary factor.
8. Sum both half reactions to obtain the balanced, net ionic reaction. In many cases, look for H + ions and
H2O molecules to cancel.
9. Check the final equation for mass and charge balance.
Summary of Steps for balancing redox reactions in basic medium:

1. Divide the equation into two half reactions.
2. Balance any atom other than O or H first.
3. Balance O using H 2O. Add as many H2O's as necessary to the side deficient in O.
4. As if with acid solution, balance the H's by adding H+ to the side deficient in H.
5. Switch over to base by adding the same number of OH- as there are H+ to both sides of the half reaction.
6. One side of the half reaction will contain H+ and OH-. Convert the n H+ and n OH- to n H2O's.
7. Cancel H2O molecules where possible.
8. Balance the charge by adding electrons to the more positive side to equal the less positive side.
9. Repeat these steps for the second half reaction.
10. If the number of electrons lost does not equal the number of electrons gained, find the least common
multiple and multiply each half reaction by the factor necessary to obtain the least common multiple.
11. Add the two half reactions together, cancelling the electrons, and any OH - and/or H2O where possible.
12. Check the final equation for mass and charge balance.
Exercises:
1. Determine the oxidation number of all atoms in the following compounds.
a. FeO
b. CuCl2
c. AlF3
d. H2SO4
e. NO2-
f. SO42-
1. Cr2O72- (aq) + NO2-(aq) → 2 Cr3+(aq) + NO3-(aq)

a. What is the oxidation number of Cr in Cr2O72-?
b. What is the oxidation number of N in NO2-?
c. What is the oxidizing agent in the reaction?
d. What is being reduced in the reaction?
53
2. Specify which of the following are redox reactions, and identify the oxidizing agent, the reducing agent,
the substance being oxidized and the substance being reduced.
a. CH4(g) + 2 O2(g) → CO2(g) + 2 H2O(g)
b. Zn(s) + 2 HCl(aq) → ZnCl2(aq) + H2(g)
c. Cr2O72-(aq) + 2 OH-(aq) → 2 CrO42-(aq) + H2O(l)
d. O3(g) + NO(g) → O2(g) + NO2(g)
3. For each of the following reactions, balance the reaction using half reactions
a. 2 CuCl(aq) → CuCl2(aq) + Cu(s)
b. Cu(s) + 2 Ag+(aq) → 2 Ag(s) + Cu2+(aq)
c. SiCl4(l) + 2 H2O(l) → 4 HCl(aq) + SiO2(s)
4. Balance the following oxidation-reduction reactions that occur in acidic solution using the half-
reaction method.
a. Cu(s) + NO3-(aq) → Cu2+(aq) + NO(g)
b. Cr2O72-(aq) + Cl-(aq) → Cr3+ + Cl2(g)
c. Pb(s) + PbO2(s) + H2SO4(aq) → PbSO4(s)
5. Balance the following oxidation-reduction reactions that occur in basic solution using the half-reaction
method.
a. Al(s) + MnO4- → MnO2(s) + Al(OH)4-(aq)
b. Cl2(g) → Cl-(aq) + OCl-(aq)
c. NO2-(aq) + Al(s) → NH3(g) + AlO2-(aq)
54
MANUAL 2: PRACTICAL BACKGROUND INFORMATION
AND EXPERIMENTAL PROCEDURES
Practical 1: Introductory Practical; Accuracy in Weighing, Measuring

Volumes and Calibration of a Pipette
Learning Objectives
• To overview the metric and SI units of mass and volume measurements.

• To introduce the laboratory techniques used for pipetting and weighing.
• To introduce the concepts of precision and accuracy.
• To introduce other properties such as, temperature and density.
Lab Entry Before coming to this lab session, read through your lab manual.
Checklist INTRODUCTION
Weighing is the most accurate of analytical techniques if it is done

properly. But it is perhaps easier to make careless mistakes in weighing
than in volumetric operations. Also, it is easier to damage the very precise
analytical balances if the proper procedure is not followed.
A laboratory balance is used to obtain the mass of various objects. There

are several varieties of balances, with various limits on their accuracy. Two
common kinds of balances are depicted in Figure 1. These singled-pan
balances are found in most modern laboratories. Generally they are simple
to use, but they are very delicate and expensive. The amount of material to
be weighed and accuracy required determine which balance you should
use.
A
B
Figure 1: Digital electronic balances. (A) Analytical balance (B) Top loader.
Pipettes and graduated measuring cylinders are calibrated to measure volumes of liquids. Some
volumetric apparatus are calibrated to contain a specific volume (e.g. measuring cylinders)
while other apparatus deliver a specific amount (e.g. pipettes).
55
When greatest accuracy is desired, it is necessary to calibrate volumetric glassware by
measuring the mass of water delivered or contained in the vessel, and using the density of water
to convert mass to volume. Through this method you can determine, for example, that your
particular 25 mL pipette delivers 25.016 mL, and not 25.000 mL.
Accuracy is the agreement between the measured quantity and the accepted value.
Typical Laboratory Equipment Accuracy
Equipment Accuracy
Analytical balance ±0.0001 g (± 0.1 mg)
Top-loading balance ±0.001 g (±mg)
Meterstick ±0.1 cm (±1mm)
Graduated cylinder ±0.01 mL
Pipette ±0.02 mL
Burette ±0.02 mL
Thermometer ±0.2 oC
EXPERIMENTAL
PART 1: Measuring the density of Antifreeze
1. Weigh a dry 50 mL Erlenmeyer flask to the nearest 0.1mg (0.0001g).

2. Using your pipette, measure a 10 mL sample of antifreeze into the 50 mL flask.
3. Weigh the flask and its contents, and record this mass.
4. Repeat these measurements two times to give you an indication of the precision of your
measurements.
PART 2: Calibration of a pipette
NB: Make sure you are familiar with the notes on pipette technique before you begin the
experimental work. Several weighing’s are required in the following procedure; the balance
must be vacated after each determination so that someone else has a turn. All pipetting must
be done at your bench.
MATERIALS
• 25 mL bulb pipette; 250 mL Erlenmeyer flask; Thermometer; 10 mL graduated

pipette;100 mL beaker
METHODS
Part 2A
(a) Fill the Erlenmeyer flask with tap water and allow it to reach room temperature for
about 15min.
(b) Record the temperature of the water at the beginning and at the end of the calibration
exercise. Ensure that the pipette is clean.
(c) Accurately determine the weight of a clean weighing beaker to 0.0001g.
56
(d) From the Erlenmeyer flask pipette 25 mL deionized (distilled) water into it using a bulb
(volumetric) pipette.
(e) Weigh the beaker plus water.
(f) Ensure that the outside of the beaker is dry before continuing the experiment. Be careful
not to wet/spill water on any part of the balance!
(g) Weigh the beaker again, pipette 25 mL aliquot into it and reweigh. Repeat this
procedure three times.
Part 2B
(a) Fill the Erlenmeyer flask with tap water and allow it to reach room temperature.
(b) Ensure that the pipette is clean.
(c) Accurately determine the weight of a clean weighing beaker to 0.0001g.
(d) From the Erlenmeyer flask pipette 8 mL tap water into it using a graduated pipette.
(e) Weigh the beaker plus water.
(f) Then record the temperature of the water in the weighing vessel before discarding
it.
(g) Ensure that the outside of the vessel is dry before continuing the experiment. Be careful
not to we/spill water on any part of the balance!
(h) Weigh the vessel again, pipette 8 mL aliquot into it and reweigh, Repeat this procedure
four times, recording the water temperature after each repetition.
18
Practical 2: Colligative Properties Molecular Weight Determination by
Freezing Point Depression
Learning Objectives
• To be familiar with colligative properties.
• To be able to determine the freezing point depression.
• To be able to determine the molecular weight of an unknown compound.
BACKGROUND
A solution is a homogeneous mixture (has a constant composition throughout) which consists

of a dissolved substance, the solute, and a dissolving medium, the solvent.
A solute need not to be a solid – it can be a gas, such as carbon dioxide (CO2) or a liquid, such
as ethylene glycol (antifreeze in car's cooling system). If the solution contains two liquids, the
liquid that is in the greater amount is called the solvent. The most common solvent is water.
Knowing the actual strength of a solution is more useful than knowing if it is, in general terms,
dilute or concentrated. The concentration of solutions can be described quantitatively in many
ways, such as molarity, molality, and mole fraction.
Some properties of a solution depend on the concentration of particles, such as molecules or

ions in the solution, rather than on particular characteristics of the molecular or ionic substance.
These properties are called colligative properties. The number of particles in a solvent can
affect the freezing or boiling point of solvent. To express the effect of concentration on freezing
point or boiling point, molality is used in place of molarity. Molality (m) is the number of
moles of solute per 1 kilogram (or 1000 grams) of solvent. For example, a two molal (2 m)
solution contains two moles of solute dissolved in 1 kilogram of solvent.
Example 1:
Calculate the molality of a solution prepared by dissolving 36.0 g of glucose, C6H12O6, in 400.0
g of water.
Answer:
• Convert grams of glucose to moles of glucose. The molecular mass of glucose is 180.0 g.
𝐌𝐚𝐬𝐬 𝟑𝟔. 𝟎 𝐠
𝐌𝐨𝐥𝐞𝐬 = = = 𝟎. 𝟐𝟎𝟎 𝐦𝐨𝐥 𝐠𝐥𝐮𝐜𝐨𝐬𝐞
𝐌𝐨𝐥𝐞𝐜𝐮𝐥𝐚𝐫 𝐦𝐚𝐬𝐬 𝟏𝟖𝟎. 𝟎 𝐠/𝐦𝐨𝐥
• The molality expression gives the number of moles of solute (glucose) per one kilogram of solvent
(water).
𝐦𝐨𝐥𝐞𝐬 𝐨𝐟 𝐬𝐨𝐥𝐮𝐭𝐞 𝟎. 𝟐𝟎𝟎 𝐦𝐨𝐥

𝐌𝐨𝐥𝐚𝐥𝐢𝐭𝐲 = = = 𝟎. 𝟓𝟎𝟎 𝐦
𝐤𝐠 𝐨𝐟 𝐬𝐨𝐥𝐯𝐞𝐧𝐭 𝟎. 𝟒𝟎𝟎 𝐤𝐠
When a solute is dissolved in a solvent, the vapour pressure of the solvent is reduced. The
amount of the reduction depends upon the number of solute particles in a given amount of
solvent. Since both the freezing point and the boiling point of a liquid depend on its vapour
19
pressure, introduction of a solute in a solvent will change the solvent's freezing and boiling
points. The freezing point of the liquid is lowered (freezing point depression or lowering) by
the addition of a solute. In contrast, the addition of a solute increases the boiling point of a
liquid. The change in freezing point and boiling point is directly proportional to the
concentration of the solute particles.
One mole or 6.02 x 1023 particles of a molecular solute (non-ionic) dissolved in 1000 grams of
water (making 1 molal solution) lowers the freezing point of water by 1.86 0C. This temperature
interval (1.86 0C) is the molal freezing point depression constant for water, expressed as Kf
= 1.86 0C/m. If the solute is an ionic compound total number of ions released per formula of
the solute will determine the “effective molality”. For example, one mole of the ionic solute,
NaCl, contains 2 moles of solute particles (1 mole of Na+ and 1 mole of Cl− ions). The effective
molality of a solution prepared by dissolving 1 mole of NaCl in 1 kg solvent is 2 m. In this
solution, the freezing point of water is lowered by 2 x 1.86 0C.
Similarly one mole of a molecular solute dissolved in 1000 grams of water (making molal
solution) raises the boiling point of water by 0.512 0C. This temperature interval (0.512 0C) is
the molal boiling point elevation constant for water, expressed as Kb = 0.512 0C/m. One
mole of the ionic solute, BaCl2, contains 3 moles of solute particles (1 mole of Ba2+ and 2 moles
of Cl− ions). Therefore, the boiling point of water that contains 1 mole of BaCl2 per 1 kg of
water is raised by 3 x 0.512 0C.
Boiling point and freezing point constants for water can be used to calculate:
• the freezing point of the solution

• the boiling point of the solution
• the molecular mass of the solute from the freezing point or the boiling point
MOLAR MASS CALCULATIONS
The molecular mass (molar mass) of a solute can be determined by changes in the freezing
point or boiling point. The freezing point method is more practical because of the greater
temperature interval involved. It also can be more accurately measured since the boiling point
is more sensitive to atmospheric pressure changes than the freezing point.
In this experiment, you will use glacial acetic acid, HC2H3O2, as the solvent. Glacial acetic acid
has a freezing point of 16.7 0C and a Kf value of 3.9 0C/m. Since the measured freezing point
of a substance depends upon its purity, the atmospheric pressure, and the calibration of the
thermometer, you must first determine the freezing point of your sample of pure glacial acetic
acid under the conditions of this experiment. Then, after adding a measured quantity of an
unknown solute to the solvent, you will measure the freezing point of the solution.
20
Figure 1. Freezing curve for a pure solvent and solution.
PROCEDURE
Part A: Determination of the Freezing Point of Glacial Acetic Acid
1. Prepare an ice bath by filling a Styrofoam coffee cup 2/3 full with crushed ice and a
small amount of water. You can use two cups, one inserted inside the other, for better
insulation, and you may want to place the cups in a beaker (400 or 600 mL) for better
support.
2. Obtain an empty, dry, large test tube (20 x 150 mm) and add 10.0 ml (density = 1.049
g/mL) of glacial acetic acid using a 10 mL pipet. Place a thermometer in the test tube
and record the temperature under time = 0 seconds on the data sheet.
3. Insert the test tube deep into the ice bath, carefully stirring the solution continuously
with the thermometer, and record the temperature every 30 seconds on the data sheet.
Note the initial temperature at which solid first appears in the glacial acetic acid. If you
need to repeat the process, you may warm up the glacial acetic acid in a water bath and
go to step 3. After recording the temperature for 300 seconds (5 minutes), warm the
test tube back to room temperature with a water bath and save for Part B.
21
Part B: Determination of the Molecular Weight of an Unknown Compound
1. Obtain a sample of unknown solid from your laboratory instructor and record its
identification number on the report form. The unknown is a molecular organic
compound (not ionic) so we know that n = 1. Weigh about 0.500 g of the unknown on
a weighing paper and record its weight on the report sheet.
2. Carefully add it to the test tube containing the glacial acetic acid (re-warmed back to
room temperature) from Part A. Stir the mixture until the entire unknown has dissolved.
Replace the thermometer and record the temperature (time = 0) on the data sheet.
3. Insert the test tube deep into the ice-water mixture, stirring the mixture continuously,
and record the temperature every 30 seconds on the data sheet as before. Mark the
initial temperature at which solid first appears in the mixture. To repeat the process
you may warm up the mixture in a water bath back to room temperature and start at
step 3.
NOTE:
Some supercooling may occur before freezing. Supercooling results when a solution cools
below its normal freezing point without freezing. To prevent supercooling, steady stirring of
the liquid is required. Once solid begins to form, further crystallization usually occurs rapidly
without supercooling.
22
Practical 3: Acid-Base Titration
Learning Objectives
• To study the titration curve of a strong base-strong acid, strong base-weak acid and
weak acid-strong base titrations.
BACKGROUND
Acid-base titrations are based on the neutralization reaction between the analyte and an
acidic or basic titrant. When an acid and a base are present in a stoichiometric amount, e.g. 1
mole HCl added to 1 mole NaOH, this means that the equivalence point or endpoint has
been reached in an acid-base system. The point at which all molecules of the analyte is
neutralised is known as the endpoint of an acid-base titration, and can be detected by the use
of a pH indicator, a pH meter, or a conductance meter.
The use of a pH meter to quantitatively determine the endpoint of a titration reaction is

preferred to the use of visual pH indicator. This is because the pH meter monitors the change
in pH at the equivalence point rather than just observing the colour change in the visual
indicator, and this eliminates the indicator blank errors. The use of a pH indicator is often
regarded as tedious as compared to using visual indicators. However, knowing the expected
endpoint makes the work much easier as one only has to concern themselves with dropwise
addition towards the expected endpoint. A graph of pH versus volume of analyte added is used
in determining the endpoint of the titration, which appears as a sudden change in pH.
In the titration of a strong acid with a strong base e.g. HCl with NaOH, the pH of the
hydrochloric acid will change with the increasing amount of NaOH. At the end point the
solution will become neutral with a pH of 7. This is only true for strong acid-strong base
titrations. For strong acid-weak base, weak acid-strong base and weak acid-weak base, the
conjugate salt formed may undergo hydrolysis and act as a buffer solution shifting the pH at
the end point away from 7. This is clearly visible when graphs of pH vs volume, or titration
curves are drawn.
CHEMICALS AND EQUIPMENT
• 2 x 250 mL beaker; Stirrer and stir bar; pH meter and combination electrode; 100 mL
burette; 25 mL measuring cylinder; 0.1 M NaOH; 0.1 M HCl; 0.1 M CH3COOH; 0.1 M
NH3OH; pH buffers (4, 7, and 9
PROCEDURE
Calibration of the pH meter:
• calibrate according to the pH instrument instruction.
23
Part A: Strong acid-strong base
1. Pipette 25 mL of 0.1 M HCl into a clean dry 250 mL beaker. Add 25 mL of distilled water.
2. Rinse the 100 mL burette with water first, and then with about 10 mL of 0.1 M NaOH
solution.
3. Carefully add a magnetic bar to the beaker with HCl solution. Put the beaker with HCl on
a stirrer and carefully adjust the speed.
4. Dip the electrode of the pH meter into the beaker with HCl deep enough so that the
electrode is immensed in the HCl solution but there is room for the rotating magnetic bar
not to hit the electrode.
5. Record the initial burette reading and the initial pH reading of the HCl solution.
6. Start your titration adding the titrant in 3 mL portions until about 21 mL of the titrant is
delivered, recording the pH of the HCl-NaOH solution and the exact burette reading to 2
decimal places after each addition.
7. Now, reduce the amount of titrant delivered, adding only 0.5 mL portions of NaOH and
record the pH after each addition until you reach the equivalence point. The equivalence
point is marked by a sudden increase in the pH.
8. Once the equivalence point is reached, continue adding 3 mL portions and take at least
three (3) more readings after the equivalence point.
9. Discard your titrated solution in the appropriate bottle, careful not to discard the the
magnetic bar.
10. Repeat the experiment one (1) more time.
Part B: Weak acid-strong base
1. Pipette 25 mL of 0.1 M CH3COOH into a clean dry 250 mL beaker. Add 25 mL of distilled
water.
2. Rinse the 100 mL burette with water first, and then with about 10 mL of 0.1 M NaOH
solution.
3. Record the initial burette reading and the initial pH reading of the HCl solution.
delivered, recording the pH of the CH3COOH-NaOH solution and the exact burette
reading to 2 decimal places after each addition.
5. Now, reduce the amount of titrant delivered, adding only 0.5 mL portions of NaOH and
7. Discard your titrated solution in the appropriate bottle, careful not to discard the the
magnetic bar.
32
Part C: Strong acid-weak base
1. Pipette 25 mL of 0.1 M NH4OH into a clean dry 250 mL beaker. Add 25 mL of distilled
water.
2. Rinse the 100 mL burette with water first, and then with about 10 mL of 0.1 M HCl
solution.
3. Record the initial burette reading and the initial pH reading of the NH3OH solution.
delivered, recording the pH of the NH3OH-HCl solution and the exact burette reading to
2 decimal places after each addition.
5. Now, reduce the amount of titrant delivered, adding only 0.5 mL portions of HCl and
7. Discard your titrated solution in the appropriate bottle, careful not to discard the magnetic
bar.
33
Practical 4: Heat of a Reaction
Learning Objectives
• To demonstrate the enthalpy of the hydration of concentration sulphuric acid, the
dissolution of ammonium chloride and neutralization reaction.
BACKGROUND
Heat of reaction is the heat liberated or absorbed when a chemical reaction takes place. All
chemical reactions involve a heat effect. If the reaction liberates heat, it is called an
exothermic reaction. If the reaction consumes heat, it is called an endothermic reaction. These
heat effects are the result of the formation or breaking of chemical bonds. Energy is required
to break bonds, and energy is liberated in the formation of chemical bonds. The heat of
reaction is the net heat effect for the reaction and is often the combination of several effects.
If a reaction is performed in an insulated container open to the atmosphere (thus, held at

constant pressure) and the temperature change is measured, the amount of heat absorbed or
released by the reaction can be determined. Thus, the heat (enthalpy) of reaction (∆Hrxn) can
be determined. Heat of reaction is measured in kJ mol-1 for a specified reactant or product.
Depending on the reaction performed, different names are used to refer to the heat of a
reaction. The heat of reaction for a neutralization reaction is known as the heat of
neutralization. The heat of reaction for a solute dissolving in a solvent is known as the heat of
solution. The heat of reaction for a precipitation reaction is known as the heat of
precipitation.
Measuring Heat of Reaction Experimentally
Heat of a reaction can be measured experimentally with the following procedure:
1. A known quantity of reactant is placed in a well-insulated vessel (e.g. a Styrofoam

cup)
2. The initial temperature of this reactant is recorded, Ti.
3. A known quantity of the second reactant is added, the

vessel is sealed with a lid and the reaction mixture stirred.
4. The final temperature of the reaction mixture is recorded,

Tf.
5. The heat released or absorbed, in joules, for the reaction is

calculated:
m = mass
C = specific heat capacity
−𝐪 = 𝐦 × 𝐂 × ∆𝐓
∆T= temperature change (i.e. Tf - Ti)
34
6. The enthalpy change in kJ per mole of a given reactant for the reaction is calculated:
𝐪 ΔH is negative for exothermic reactions
∆𝐇 = ÷ 𝐧𝐫𝐞𝐚𝐜𝐭𝐚𝐧𝐭
𝟏𝟎𝟎𝟎 and positive endothermic reactions.
The following assumptions are made for reaction mixtures in aqueous solutions:
a) The density of aqueous solution is the same as for water i.e. 1g/mL (e.g. 100mL
of solution is said to have a mass of 100g).
b) The volume of reactants are additive (e.g. 100mL of reactant A + 200mL of

reactant B = 300mL of reaction mixture).
c) The specific heat capacity (C) of the reaction mixture is the same as for water,
i.e. C = 4.184 JK-1g-1
d) No heat is lost to the surroundings.
This experiment will investigate the heat of reaction for three types of reactions: (1) the
hydration of a liquid, (2) the dissolving of a solid, and (3) neutralization (the reaction of an
acid with a base).
Hydration of Concentrated Sulfuric Acid
A strong heat effect is observed when concentrated sulfuric acid is added to water. This reaction
is so exothermic that it can lead to dangerous spattering. The general rule “add the acid to the
water" will help avoid the danger. The reaction involved is the hydration of sulfuric acid
molecules to form H2SO4∙H2O and H2SO4∙2H2O. The formation of the bonds between the
acid and the water is the primary cause of the heat liberated. The usual commercial concentrated
sulfuric acid contains less than 5 percent water, so some of the acid molecules are already
hydrated.
Dissolving of Ammonium Chloride
When a salt dissolves there are two major competing heat effects. The energy required to
break the ionic bonds of the crystal lattice is called the lattice energy. As the ions are freed
from the crystal lattice they become hydrated and release energy. This energy is known as
the hydration energy. If the lattice energy is greater than the hydration energy, the reaction
will be endothermic. If the hydration energy is greater than the lattice energy, the reaction
will be exothermic.
35
Neutralization Reactions
When hydrochloric acid is added to sodium hydroxide solution, heat is evolved. Since the
reaction of an acid with a base is called neutralization, this heat is called the heat of
neutralization. The molecular equation for this reaction is:
𝐇𝐂𝐈 (𝐚𝐪) + 𝐍𝐚𝐎𝐇 (𝐚𝐪) → 𝐇𝟐 𝐎 (𝐥) + 𝐍𝐚𝐂𝐥 (𝐚𝐪) + 𝐇𝐞𝐚𝐭
Since all the substances are soluble, and all of them except water are strong electrolytes, the
total ionic equation is:
𝐇 + + 𝐂𝐥− + 𝐍𝐚+ + 𝐎𝐇 − → 𝐇𝟐 𝐎 + 𝐍𝐚+ + 𝐂𝐥− + 𝐇𝐞𝐚𝐭
Therefore, the net ionic equation is:
𝐇 + (𝐚𝐪) + 𝐎𝐇 − (𝐚𝐪) → 𝐇𝟐 𝐎 (𝐥) + 𝐇𝐞𝐚𝐭
According to the net ionic equation, a neutralization reaction between a strong acid and a strong
base is the reaction of the hydrogen ions (H+) and the hydroxide ions (OH-) to form water.
Since this reaction is common to all strong acids and bases, and since a definite amount of heat
is liberated for each mole of reacting hydrogen ion and hydroxide ion, it should be possible to
use different strong acids with a fixed amount of base and obtain the same quantity of heat
for each acid neutralized. This experiment will investigate this hypothesis.
Each neutralization reaction will involve the same total volume of liquid. Thus if the same
quantity of heat actually is produced, the temperature increase should be the same for each
neutralization. This assumes a constant heat capacity for the various solutions used, which is
not precisely true, but is satisfactory for the purpose of this experiment. Duplicate runs are
made for each acid used. Because of experimental errors, variations occur in the temperature
increases obtained in duplicate runs with the same acid. Thus the variations in temperature
changes with different acids should be of the same order of magnitude, if our hypothesis of
identical reactions is correct. It is necessary to use dilute acids and bases to minimize heats of
hydration. In all the experimental trials the moles of hydroxide ion will be the limiting
reactant. Thus there will always be more moles of hydrogen ion available than of hydroxide
ion. The excess moles of hydrogen ion will remain unreacted
CHEMICALS AND EQUIPMENTS
Styrofoam cup; Measuring cylinder; Thermometer; Erlenmeyer flask; Conc. sulphuric acid;
Ammonium chloride; 1.25 M NaOH; 2.55 M HCl; 2.66 M HNO
36
PROCEDURE
NB! Wear protective glasses.

Record all temperatures to the nearest 0.1oC.
Collect all your waste solutions in a large plastic beaker and give it in to your instructor for
disposal.
Part A: Hydration of Concentrated Sulfuric Acid
NB! Concentrated sulfuric acid is an extremely corrosive, oxidizing acid and a strong
dehydrating agent. Wash immediately if you spill any on your skin or clothing.
Rinse off any acid that runs down the side of the bottle with a wash bottle and rinse the
graduated cylinder used.
1. Pour 44 mL of tap water into a Styrofoam cup. Read and record the temperature of the
water.
2. Measure 4.0 mL of concentrated sulfuric acid in a 10 mL measuring cylinder and pour

it into the water in the Styrofoam cup.
3. Stir with the thermometer and record the maximum temperature reached. Rinse off
any acid that runs down the side of the cup and rinse out the measuring cylinder.
4. Pour this dilute sulfuric acid solution from the Styrofoam cup into an Erlenmeyer
flask and save for Part C.
Part B: Dissolving of Ammonium Chloride
1. Rinse the Styrofoam cup and pour 20 mL of tap water into it. Read and record the
temperature of the water.
2. Weigh approximately 3 g of ammonium chloride crystals and pour then into the
Styrofoam cup. Stir with the thermometer and record the minimum temperature
reached.
Part C: Neutralization Reactions
You will be provided with the following solutions:

• 1.25 M NaOH stock solution; 2.55 M HCI stock solution; 2.66 M HNO stock
solution; H2SO4 stock solution: H2SO4 solution prepared in Part A.
Using the six step procedure outlined below, measure the temperature change for the
following five (5) neutralization reactions:
1. Pour the measured volumes of acid and water into the Styrofoam cup.
2. Measure out the sodium hydroxide solution.
40
3. Read and record the temperature of the water-acid mixture.
4. Add the base, stir with the thermometer, and record the maximum temperature
reached.
5. Calculate the temperature change.
6. Empty the Styrofoam cup; rinse the cup and the measuring cylinder with water.
Acid H2 O NaOH
Neutralization 1 10 mL HCl 20 mL 10 mL
Neutralization 2 10 mL HNO 20 mL 10 mL
Neutralization 3 10 mL H2SO4 20 mL 10 mL
References:
• AUS-e-TUTE n.d. Chemistry Tutorial: Heat (enthalpy) of Reaction. Retrieved 10

September 2013, http://www.ausetute.com.au/heatreact.html
• Experiment 25. n.d. Heat of a reaction. Retrieved from 10 September 2013,

http://www.sanjuan.edu/webpages/pmontbriand/files/Heat%20of%20Reaction.pdf
41
Practical 5: Determination of Vapour Pressure and Enthalpy of vaporization
Learning Objectives
• To demonstrate how to determine the vapour pressure of water in a specific range.
BACKGROUND
The Clausius-Clapeyron equation in Physical Chemistry courses is introduced as a means of
describing the variation of the vapour pressure with temperature and for determining the
enthalpy of vaporisation.
𝒅 𝐥𝐧 𝐏 𝚫𝐇𝐨𝐯𝐚𝐩
=
𝒅𝐓 𝐑𝐓𝟐
If ∆Hvap is independent of temperature then,
∆𝐇𝐨𝐯𝐚𝐩
𝐥𝐧 𝐏 = + 𝐜𝐨𝐧𝐬𝐭𝐚𝐧𝐭
𝐑𝐓
This experiment demonstrates how one can determine the vapour pressure of water in the range
of 50 °C to 80 °C using the simplest of laboratory equipment, i.e. a tall beaker, a graduated
cylinder and a thermometer.
Method: A sample of air is trapped in an inverted 10 mL graduated cylinder immersed in a

beaker of water. The water is heated to about 80 °C, and the trapped gas becomes saturated
with water vapour rapidly at this temperature. The temperature of the water bath and the volume
of the gas are recorded. The bath is then cooled and the readings of temperature and gas volume
are taken at intervals of 5 °C or less. The number of moles of water in the gas phase changes
with temperature but the amount of air is constant. With knowledge of the moles of air in the
gas sample, the partial pressure of air can be calculated at each temperature, and the vapour
pressure of the water can be obtained by determining the difference from the barometric
pressure. The number of moles of air in the mixture can be found from the measurements of
volume, temperature and pressure at the temperature near 0 °C, where water content of the gas
is less than 1 % and is neglected.
The enthalpy of vaporization is calculated through the Clausius-Clapeyron equation from a plot
of the algorithm of the vapour pressure versus 1/T. There is a small systematic error resulting
from the use of inverted graduated cylinders because the meniscus at the water interface is
reversed (see the figure). It has been estimated, by introducing known volumes of air into a
completely filled inverted cylinder, that the error involved with the use of 10 ml graduated
cylinders is 0.2 mL. Then, this value is subtracted as a correction to each volume reading.
42
• Heater and stirrer; Magnetic stirring bar; 600 mL beaker; Vial; 10 mL graduated cylinder;
Thermometer; Glass rod
PROCEDURE
1. Fill 10 mL graduated cylinder about 9 mL with distilled water.

2. Fill the vial with water and quickly invert the cylinder into the vial. An air sample of 4 to
4.5 mL should be trapped within the cylinder.
3. Lower the above setup into a 600 mL beaker filled with water. Carefully, add a magnetic
stirrer to the beaker. Add more water if necessary to the beaker to ensure that the trapped
air is surrounded by water.
4. Record the temperature of the water and the volume of air trapped.
5. Place the setup on a heater/stirrer and carefully adjust the speed so that the magnet stirs
the water to evenly distribute the heat without knocking down the vial.
6. Heat the beaker to 50 °C and record the volume of air trapped.
7. Continue heating and taking the reading at 5 °C interval until a temperature of 80°C is
reached.
8. Cool the water to less than 5 °C and record the temperature and the amount of air trapped.
Ice blocks could be added to aid the cooling.
9. Obtain a reading of the atmospheric pressure.
45
Practical 6: Solubility Rules
Learning Objectives
Part A: Chlorides, Nitrates and Sulphates
• Observe the result of the mixing of aqueous solutions of various cations with each of the following
anions: NO3-, Cl-, SO42-.
• From these observations, deduce general solubility rules for chlorides, nitrates and sulfates in aqueous
solution.
Part B: Hydroxides and Carbonates
• Observe the result of mixing of aqueous solutions of various cations with each of the following anions:
OH- or CO32-.
• From these observations, deduce general solubility rules for hydroxides and carbonates in aqueous
solutions.
Part C: Mixed Bottles – A Chemical Puzzle
• Use knowledge of solubility and other properties of solutions of compounds to confirm identity of
solutions of compounds.
PART A: Solubility of Chlorides, Nitrates and Sulphates in Aqueous Solution
INTRODUCTION
You are going to test the solubility of about 10 cations with three anions (NO3-, Cl-, SO42-), i.e.
51 salts altogether. Although this may sound like a daunting task, it can be done very efficiently
and quickly by the use of small test tubes or, even better, a “spotting tray”. Whichever you use,
the important thing is to work systematically. As you now realise no doubt, the best way of
summarising all your observations is to record them in an appropriate table. (This also helps
you to work more systematically). So devise a table similar to that given on the data recording
sheet.

• Test tubes; Pasteur pipettes; NaCl solution; NaNO3 solution; Na2SO4 solution; Na2CO3
solution; 2 M HNO3
PROCEDURE (Part: A)
Use small test tubes or a spotting tray and Pasteur pipettes (droppers) to mix together a small
volume of each of the cation solutions to be tested with an equal volume of NaCl solution.
Observe carefully. Where the compounds formed are completely soluble (no visible precipitate
forms) then indicate with a tick (✓) in the appropriate space in your table; this is illustrated for
potassium for which the chloride, nitrate and sulphate are all soluble in aqueous solution. When
a precipitate does form, its colour and nature (e.g. gelatinous, crystalline etc.) should be
recorded in the appropriate space in your table together with the relevant chemical equation.
Repeat the procedure using firstly NaNO3 solution and, secondly, Na2SO4 solution recording
your results in your table.
46
PART B: Solubility of Carbonates and Hydroxides
PROCEDURE (Part: B)
Use the same procedure for studying the solubility of the 10 cations with carbonate and
hydroxide ions as you used in Part A. Again record your data in a table (see below) indicating
soluble compounds with a tick (✓). However, also determine the effect of adding acid (2M
HNO3) to any precipitates formed. To do this, proceed as follows:
1. To any insoluble carbonates* formed add drop wise a similar volume of dilute nitric acid.
Look carefully to observe any effervescence (evolution of gas) and dissolution of the
precipitate. Describe with equations any reactions you observe.
2. To any insoluble hydroxide* formed repeat as in 1. Observe carefully and describe any
reactions that occur with equations.
* Obviously if no precipitate forms, there is no need to test with HNO3
PART C: Mixed Bottles – A Chemical Puzzle
The knowledge of solubility and other properties of compounds can often be used to identify a
compound. For example the identity of a bottle containing a solution of some chloride can be
confirmed by adding a solution containing Ag+ ions. The formation of a precipitate of insoluble
AgCl, would confirm the presence of Cl- ions in the solution.
PROCEDURE (Part: C)
You are provided with a set of bottles. These bottles contain solutions as stated below, but the
list does not tell you which solution is in which bottle.
• Sodium chloride; Sodium nitrate; Sodium sulphate; Sodium carbonate

Using only the given solutions of silver nitrate, barium chloride and dilute nitric acid, identify
the contents of as many bottles as you can.
48
Practical 7: The Standard Free Energy of Formation of the Complex
between Salicylic Acid and Ferric Ions
Learning Objectives
•
To observe the free energy of formation of a complex between salicylic acid and
ferric ions.
BACKGROUND
Ferric ions in aqueous solutions at pH 2.6 – 2.8 form a strongly coloured complex with salicylic
acid (orthohydroxybenzoic acid):
𝑭𝒆𝟑+ + 𝒙(𝒔𝒂𝒍) ↔ 𝑭𝒆(𝒔𝒂𝒍)𝒙 𝟑+
Where sal stands for salicylic acid. By measuring the intensity of the colour produced on
mixing different proportions of the reactants, the stoichiometry of the complex can be found.
In addition, if the extinction coefficient of the complex is known, its concentration in a
particular mixture can be found and hence the apparent equilibrium can be deduced from:
[𝒄𝒐𝒎𝒑𝒍𝒆𝒙]
𝑲𝒄 =
[𝑭𝒆𝟑+ ] [𝒔𝒂𝒍] 𝒙
However, the state of equilibrium is governed rigorously by the thermodynamic equilibrium

constant defined by:
𝜶𝒄𝒐𝒎𝒑𝒍𝒆𝒙
𝑲𝑻𝒉 =
𝜶𝒙𝒔𝒂𝒍 𝜶𝑭𝒆𝟑+
Where the α are the equilibrium thermodynamic activities. The two expressions are related by:
𝜸𝒄𝒐𝒎𝒑𝒍𝒆𝒙
𝑲𝑻𝒉 = ( ) 𝑲𝒄
𝜸𝑭𝒆𝟑+ 𝜸𝒙𝒔𝒂𝒍
Where, the γ terms, called activity coefficients, have the property that they approach unity as
the concentrations approach zero. In the present experiment the concentrations used are such
that γsal ≈1. Although the activity coefficients of the charged species cannot be taken to be
approximately unity, we may assume that γsal ≈ Kc so that they almost cancel out in the above
expression leaving:
𝑲𝑻𝒉 ≈ 𝑲𝒄
In general, the change in Gibbs free energy for a reaction
𝐀 + 𝐁 → 𝐂 + 𝐃
Where A, B, C and D are present with activities αA, αB, αC and αD is given by the equation:
∆𝑮 = ∆𝑮° + 𝑹𝑻 𝒍𝒏 (𝜶𝑪 × 𝜶𝑫 / 𝜶𝑨 × 𝜶𝑩 )
If all the substances are present in their standard states (i.e. all activities are unity) then ∆G
=∆G°, which is the standard free energy change of the reaction. For solutes in solution, the
49
standard state is a hypothetical one in which it is present at a concentration of 1 moldm-3 and a
pressure of 1 atm but behaves ideally, i.e. obeys Henry’s law.
The standard free energy change is related to the thermodynamic equilibrium constant by the
van’t Hoff isotherm:
∆𝑮° = − 𝑹𝑻 𝒍𝒏 𝑲𝑻𝒉
Like heats of reaction, the standard free energy change is an additive property and therefore
∆G° (and hence KTh) can be determined for the reactions which may be difficult, if not
impossible to study directly, from other reactions of known ∆G°.
Theory: Job’s method of continuous variations employs equimolar solutions of two reactants
mixed in various proportions. This method suggests that the maximum amount of equilibrium
product is formed when the proportions of the reactants correspond to the empirical formula of
the product. For example, if the reaction can be represented by:
𝒂𝑨 + 𝒃𝑩 = 𝑨𝒂𝑩𝒃
Then, the greatest amount of product is present when a parts of A are mixed with b parts of an
equimolar solution B. In the present experiment, the concentration of the ferric complex is
monitored by its absorbance of light. The Beer-Lambert Law states that the fractional
reduction in the intensity of a beam of light as it passes through an absorbing medium is
proportional to the number of absorbing molecules in the light path. This can be expressed
mathematically in the following way:
A = absorbance/optical intensity
I0 = initial intensity
I = transmitted intensity
𝐈𝟎
𝐀 = 𝐥𝐨𝐠 𝟏𝟎 ( ) = 𝜺𝒄𝒍 ε = molar absorptivity/molar extinction coefficient of solute
𝐈
being measured
c = concentration (mold/m3)
l = path length (cm)
• Spectrophotometer; Cuvette (1cm); Burette; Burette clamp; Retort stand; Small funnel ;
Thermometer; 50 cm3 beaker; 250 cm3 volumetric flask; 100 cm3 volumetric flask;
Spatula; Wash bottle; Filter paper; 0.0020 M HCl stock solution; 0.0010 M Salicylic
acid; Ferric Nitrate
50
PROCEDURE
Part A:
1. The optimum pH for the complex is about 2.6 - 2.8, which can be obtained sufficiently
nearly by working throughout with solutions of the substances of approximately 0.0020 M
HCl.
2. Prepare 0.0010 M solution of Ferric Nitrate by dissolving 0.1010 g in 250 cm3 of 0.0020
M HCl solution. (N.B. This solution hydrolyses on standing and must be used immediately
after preparation).
3. By means of two burettes, prepare 10 cm3 mixtures of 0.0010 M Ferric Nitrate and 0.0010
M Salicylic Acid in HCl in the ratios 1:9, 2:8, 3:7, …7:3, 8:2, 9:1. Record the temperature
of the mixtures.
4. Determine the absorbance of each solution using the spectrophotometer provided at
wavelength = 527 nm. Use deionised water as blank.
Part B:
5. Prepare a series of ferric solutions having strengths of 0.0010, 0.0020, 0.0040, and 0.0050
M in 100 cm3 volumetric flasks and make up to the mark with deionised water respectively.
6. Pour about 10 cm3 of each of these solutions into small beakers respectively.
7. Add excess solid Salicylic Acid (half a spatula) to small beakers respectively in order to
convert the ferric salt wholly into the complex form.
8. Filter off undissolved solid.
9. Determine the absorbance of the four resulting solutions using the corresponding ferric
solution without adding Salicylic Acid to the blank at the same wavelength.
Practical 8: Determination of the Dissociation Constant (Ka), of a weak

acid using pH Measurement.
Learning Objectives
• To determine the dissociation constant of acetic acid.
PROCEDURE
Part A:
1. You will require two burettes. Fill one with 0.1M NaOH solution and the other with
0.1M CH₃COOH.
2. Add 22.50 mL of CH₃COOH and 2.50mL of NaOH into the 100mL beaker and measure
the pH of the resultant mixture. Record the pH in Table 2 in the report sheet
3. Repeat the same procedure with the other mixtures (for Trail 2-4) as given in Table 1
below.
54
Table 1: Volumes of the reagents for each trail
Volume of CH₃COOH
Trail Volume of NaOH (mL)
(mL)
1 22.50 2.50
2 20.00 5.00
3 17.50 7.50
4 15.00 10.00
Part B:
1. Use the burette to measure 30.00 mL of the ethanoic acid from Part A into a titration flask
(conical flask). Titrate with NaOH solution from the second burette using phenolphthalein
as the indicator. Note the volume of NaOH required for complete neutralization. Record
your results in Table 4.
2. Repeat the procedure for a 2nd time and determine the average volume of NaOH required
for complete neutralization of acetic acid.
3. In a 100 mL beaker, mix 30.00mL of the acid (ethanoic acid) and half the mean titre
volume of NaOH, from step 2, and measure the pH of the mixture. Record your result in
Table 5.
55
Practical 9: Chemical Kinetics; Hydrolysis of Methyl Acetate
Learning Objectives
• To determine the rate constant of the hydrolysis of methyl acetate.
BACKGROUND
Chemical kinetics is concerned with the quantitative study of chemical rates of reaction as
well as explaining the steps or mechanism of reactions. The rate of a chemical reaction
generally depends on the concentration of species/reactants, temperature and catalyst. Rate of
reaction can be measured as the rate of the disappearance of reactants or the rate of formation
of products in a chemical reaction. Rate of reaction is generally defined as dc/dt (differentiation
of concentration with respect to time).
The overall order of a reaction is defined to be the sum of the individual orders of reaction in
each of the species involved. Thus, a reaction whose rate is proportional to the concentration
of only one of the reactants or products of the reaction (i.e., the reaction is first order in that
species) is termed a first order reaction. In this experiment, you will study a reaction that, under
the experimental conditions you will employ, corresponds to such a case. Rates of reaction can
be determined experimentally. The differential equation for the rate law of a first order reaction
whose rate depends only on the concentration of one reactant can be written (in the case of unit
stoichiometry) as:
c = concentration of reactant on which the rate depends
𝒅𝒄
Eq. 1 − = 𝒌𝒄 t = time
𝒅𝒕 k = rate of constant/specific rate constant
A → B
Time = 0 a
Time = t (a – x) x
In an experiment, it is generally more useful to write equation (1) in the form of equation (2):
𝒅𝒄 a = initial concentration of reactant
Eq. 2 − = 𝒌(𝒂 − 𝒙) (a – x) = concentration of reactant present at time t
𝒅𝒕
Integrating equation (2) produces equation (3):

𝒂
Eq. 3 𝐥𝐧 = 𝒌𝒕
𝒂−𝒙
Rearranging equation (3) gives equation (4):
ln (a-x) = -kt + ln a
Eq. 4
kt = ln a – ln (a-x)
Therefore, for a first order reaction, a graph of ln(a – x) versus t is a straight line with gradient,
-k. Quantities that are proportional to concentration can be used instead as replacement for
56
concentration in the above equations. In 1889 Arrhenius found that the values of rate constants
increase exponentially with temperature. The relationship between rate constant and
temperature is given by the Arrhenius equation:
−𝑬𝒂 A = pre-exponential factor
Eq. 5 𝒌 = 𝑨𝐞𝐱𝐩 ( ) Ea = activation energy of reaction
𝑹𝑻
For more precise rate data, experiment can be repeated with careful temperature control.
Determination of the rate constant of hydrolysis of methyl acetate with HCl 0.5 M as
catalyst
Theory: When esters such as methyl acetate react with water, some are converted to alcohol
and acid, and the reaction can be explained as;
Eq. 𝐂𝐇𝟑 𝐂𝐎𝐎𝐂𝐇𝟑 + 𝐇𝟐 𝐎

6 ⇌ 𝐂𝐇𝟑 𝐂𝐎𝐎𝐇 + 𝐂𝐇𝟑 𝐎𝐇
This is a reversible reaction, but with the presence of excess water, this reaction can be
considered as a complete reaction. Hydrolysis occurs slowly in pure water, with acid as catalyst.
If this reaction is conducted in a dilute solution with the presence of a known concentration of
strong acid, the rate and order of the reaction depends only on the concentration of methyl
acetate. This is thought to be due to the concentration of water which is considered to be
constant throughout the experiment and the concentration of acid does not change. The rate of
reaction, however, is proportional to the concentration of acid.

• Conical flask; Burette; Pipette; Stopwatch; Water bath
• Methyl acetate; 0.5 M of HCl; 0.1 M of NaOH; Phenolphthalein indicator
PROCEDURE
1. Transfer 100 mL of 0.5 M HCl into a conical flask with a stopper and place the flask in
the water bath.
2. Place another conical flask or bottle that contains methyl acetate in the same water bath.
3. While the temperature of these chemicals equilibrates, prepare a burette filled with 0.1 M
NaOH solution.
4. Record the temperature of the water bath at an interval of 15 minutes.
5. When the temperature of the chemicals is in equilibrium with the temperatures of the
water bath (after ≈ 10 minutes), pipette 5 ml of methyl acetate into the conical flask that
contains the acid. Record the time of mixing as the initial time for the reaction (to) in
measuring the reaction time (t). Shake the conical flask well and do not remove it from
the water bath.
57
6. Use a pipette to immediately transfer 5 mL of the mixture into a 250 mL conical flask that
contains 25 mL of icy water. Record the time as the time of reaction, t. In this case, t is
equal to 0 minutes.
7. The acid/methyl acetate solution (in which reaction has been stopped) is then quickly
titrated with 0.1 M NaOH using phenolphthalein as the indicator. (Make sure the solution
is cold during titration).
8. Take titre readings for consecutive 5 mL solution mixtures that have reacted in the
following time intervals: 10, 20, 30, 45, 60 and 80 minutes. Follow the same procedures
as above (steps 6 and 7).
9. Make sure the time the reaction is stopped is recorded for every consecutive 5 mL mixture
taken from the source mixture.
10. Finally, heat the remaining mixture for about 10 minutes until it boils to complete the
reaction. Cool it down and titrate the solution twice.
References
1. Mahan, B.H. (1987). University Chemistry, 4th edn. Addison-Wesley.
2. Finlay, A. (1954). Practical Physical Chemistry, 8th edn. Longmans
64
Practical 10: Redox Chemistry
Learning Objectives
• To determine the oxidizing strength of provided halogens.
• To determine the reducing strength of provided halides.
• To observe the product obtained from an oxidation-reduction reaction in acid solution and basic
solution.
BACKGROUND
We encounter oxidation-reduction reactions every day. Examples include the combustion of coal,
natural gas, oil, and gasoline; the operation of automobile’s battery; the formation of an image on
photographic film, and the removal of stains by bleach.
Although oxidation-reduction reactions are diverse, when you compare a number of these reactions,
you can find some common features. Each reaction consists of a simultaneous oxidation and
reduction. Moreover, the reactants must include an oxidizing and a reducing agent. Electrons are
always lost by the reducing agent and gained by the oxidising agent.
You will be supplied with solutions of three halogens: Cl2, Br2 and I2. They have been prepared in
solution from stoichiometric quantities of certain oxidising and reducing agents. By observing the
effects of these halogens on the corresponding halides (Cl−, Br−, I–), you will be able to rank the
halogens according to their oxidizing strengths and the halides according to their reducing
strengths. Your subsequent observations on the reactions of two halides (Br– and I–) with two
common oxidising agents will enable you to rank the latter according to their oxidizing strengths.
You will also observe that the products obtained from an oxidation-reduction reaction in an acidic
solution can differ markedly from those obtained in a basic solution. Finally, and most importantly,
you will write a balanced equation for each of reaction that you have observed.
HALOGENS & HALIDES
You will deal with halogens and halides in each part of this experiment. A brief description, outlined
below, of some of their properties will allow you to understand some of your observations more
easily. If you want to learn more about these substances, consult the prescribed textbook (Chang,
Chapter 21).
The elemental form of halogens are diatomic (Cl2, Br2, I2 and At2), and each of them is an oxidizing
agent. This experiment only uses Cl2, Br2 and I2. However, F2 is not used because it is a very strong
oxidizing agent and requires special conditions for its study. Astatine is not used because it is
radioactive and can only be used in laboratories certified to handle radioactive material.
Aqueous solutions of Cl2, Br2 and I2 can be prepared either by dissolving these elements in water or
by generating them in solution as products of certain oxidation-reduction reactions. Aqueous
solutions of Cl2, Br2 and I2 are called chlorine water, bromine water and iodine water, respectively.
Each solution has its own characteristic colour, depending on the concentration and thickness of the
solution. Chlorine water is colourless to yellow; bromine water is yellow to red; and iodine water
is red-brown to brown.
These halogens are soluble in cyclohexane (C6H12), a substance that is itself insoluble in water. When
cyclohexane is added to an aqueous solution of a halogen, two layers are formed. The upper layer is
65
the cyclohexane layer (also referred to as the organic layer) since cyclohexane is insoluble and less
dense than water. The bottom layer is the aqueous layer. When cyclohexane is added to an aqueous
solution of a halogen, a portion of the halogen passes from the aqueous layer to the upper cyclohexane
layer (a process called extraction). A characteristic colour is then imparted to the upper cyclohexane
layer. The colour of a halogen in the upper cyclohexane layer will differ somewhat from its colour in
an aqueous solution, as you will discover during the experiment.
The reduction of a halogen (X2) yields a halide (X–) according to the half-reaction:
𝐗 𝟐 + 𝟐𝐞− → 𝟐 𝐗 −
Halogens are oxidizing agents, and the halides are reducing agents. Compounds of halides are
colourless if the positive ion (the cation) belongs to either Group 1 or Group 2, for example NaI or
CaCl2. Compounds of these types are ionic and hence insoluble in cyclohexane.
REDUCTION OF OTHER COMMON OXIDISING AGENTS
You will also encounter two other oxidizing agents in this experiment. These are potassium
permanganate (KMnO4) and Iron (III) chloride (FeCl3).
Reduction of the purple permanganate ion (MnO4–) can either give a green manganate ion (MnO42–) or
a brown-black solid in form of manganese oxide (MnO2) or manganese (II) cation (Mn2+), an ion that
is pink but will be virtually colourless at the concentrations used in this experiment.
The reduction of iron (III) cation (Fe3+) will give iron (II) cation (Fe2+), a pale green ion that will be
virtually colourless at the concentration found in this experiment.
CONCEPTS OF THE EXPERIMENT
You will mix aqueous solutions of potential oxidizing agents in each part of this experiment. However,
do not expect a reaction to occur in every mixture that you prepare. If a reaction occurs, there will be
tell-tale signals. The formation or the disappearance of the characteristic colour of one of the halogens
in the upper cyclohexane layer is usually a signal of a reaction in the aqueous layer. In some instances,
colour changes to the aqueous layer will also indicate that a reaction has occurred.
PREPARATION OF CHLORINE WATER
You will prepare your own chlorine water. To do this, obtain a clean dry Test Tube and add:
• 50 drops of distilled water
• 50 drops of household bleach
• Carefully add 1M HCl drop-wise until bubbles start forming.
Your solution is then ready for use.
66
• 3x Large test tubes with stoppers, 3x Small test tubes, Chlorine water, Bromine water, Iodine
water, Cyclohexane, 0.2 M NaCl, 0.2 M NaBr, 0.4 M NaI, 0.1 M KMnO4, FeCl3, 3 M H2SO4
PROCEDURE
Part A:
1. Obtain 3 large test tubes with stoppers, and three small test tubes.
2. Label the large test tubes so that you will know which halogen each contains.
3. Place 15 drops of the chlorine water in one of the small test tubes, 15 drops of bromine water
in the second test tube and 15 drops of iodine water in the third test tube. Add approximately
1 mL of cyclohexane to each test tube and shake or swirl very gently. No stopper should be
required. The colour of the halogen should appear in the upper layer. View this against a
white background and record the colour of each halogen.
Part B: Reactions of Halogens with Halides
1. Wash and dry the small test tubes.
2. Place 10 drops of 0.2 M NaCl in each of the two test tubes.
3. Add 10 drops of bromine water to the first test tube and 10 drops of iodine water to the
second test tube.
4. Add approximately 1 mL of cyclohexane to each of these test tubes, shake or swirl gently and
record your observations. NOTE: if no reaction occurs, only the colour of the halogen that
you added will appear in the upper cyclohexane layer.
5. Wash and dry the test tubes.
6. In an identical fashion, test 10 drops of 0.2 M NaBr with chlorine water and iodine water.
Record your observations
7. Finally, after washing and drying, test 5 drops of 0.4 M NaI with chlorine water and bromine
water. Record your observations.
Part C: Reactions with Other Common Oxidizing Agents
1. Wash and dry the small test tubes.
2. Place 15 drops of 0.2 M NaBr in each of the 2 test tubes.
3. Add 1 drop of 0.1 M KMnO4 solution to the first test tube and 5 drops of FeCl3 solution to the
second test tube.
4. Add 5 drops of 3 M H2SO4 to each test tube.
67
5. Add approximately 1 mL of cyclohexane to each of these test tubes, shake or swirl the test
tubes very gently and record your observations.
6. Repeat Step 1 through to Step 5, this time using 8 drops of 0.4 M NaI instead of 15 drops of
0.2 M NaBr.
Part D:
1. Wash and dry one of the test tubes.
2. Add 8 drops of 0.4 M NaI, 5 drops of 6 M NaOH, 1 drop of 0.1 M KMnO4, and add
approximately 1 mL of cyclohexane. Shake or swirl the test tube very gently and record your
observations for both layers.
3. Clean all the glassware you used and leave it to dry.
<<<<<<<<<END>>>>>>>>>
68
Appendix 1: t-distribution table
69
Appendix 2: Periodic Table of Elements
70

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Practical Manual

PHYSICAL CHEMISTRY FOR PHARMACY

Lab Technologists: Klaudia T. Angula, Mr Jonathan M. Ortmann & Iyaloo Matheus

Compiler This Ed: JM. Ortmann & KT Angula (PhD)

1. Weigh 150mL 2. Grind unknown 3. Put ±2g of 4. Calculate

Presentation of a formal report

Main features to concentrate on in report writing are:

• Your name and student number

• Summarize your report in a paragraph

PROPER CONDUCT IN THE LABORATORY

1. Be PUNCTUAL to all 3. Pranks, fooling around,

5. Clean the working area and all

6. NEVER pour chemicals

6. Adhere to the proper waste

NATIONAL FIRE PROTECTION ASSOCIATION HAZARD LABELS

➥ Always wear protective eyewear.

➥ Never grab equipment without checking its temperature (especially glass).

➥ Cool at once under running water.

➥ Most cuts occur when handling glass.

➥ Small cuts should be allowed to bleed, then disinfect and bandage.

➥ Never taste or ingest any chemical.

➥ Seek medical attention immediately.

Preventing weighing errors

Practical 1: Introductory Practical; Accuracy in Weighing, Statistical

PART 1: Measuring the density of Antifreeze

Data Recording Sheet: Weighing: Density of antifreeze

Temperature of antifreeze: __________________oC

Trial 1 Trial 2 Trial 3

1. What is the maximum capacity of the analytical balances in our laboratory?

PART 2: Calibration of a pipette

Temperature of water used to calibrate the pipette

Temperature of water before calibration: ___________℃

Stated volume of pipette = ________ mL

Trial 1 Trial 2 Trial 3 Trial 4

Mass of Erlenmeyer plus

2 Mass of Erlenmeyer (g)

Volume delivered by the

___________mL ___________mL ___________mL ___________mL

Mean volume of water delivered by the pipette (show calculation):

Average Volume delivered: ___________ mL

Trial 1 Trial 2 Trial 3 Trial 4

Average deviation from the mean (show calculation below)

Average deviation from mean: _____________mL

Volume delivered by your 25-mL pipette _______________mL ± _______________mL

(0.06)2 + (0.03)2 + (0.09)2

The reported value is therefore;

Temperature of water before calibration: ___________℃

Volume transferred with the pipette = _________mL

(a) Mean mass of water:

Part 2B: Questions to be answered

MOLAR MASS CALCULATIONS

1. Freezing point lowering, ∆𝑇𝑓 = 𝑇𝑓0 − 𝑇𝑓 = 𝐾𝑓 × 𝑚 × 𝑛, where Tf 0 is the freezing

3. Kg of solvent = (𝑔𝑟𝑎𝑚𝑠 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡) / (1000 𝑔. 𝐾𝑔−1 )

4. Molality of the solution, m = (𝑚𝑜𝑙𝑒𝑠 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒) / (𝑘𝑔 𝑜𝑓 𝑠𝑜𝑙𝑣𝑒𝑛𝑡)

(𝑲𝒇 )(𝒈𝒔𝒐𝒍𝒖𝒕𝒆 )(𝒏)

where n is the number of moles of solute particle(s) per mole of solute.

• First calculate the molality of the solution:

• Then calculate ∆Tf:

∆𝑻𝒇 = 𝑲𝒇 × 𝒎 × 𝒏 = (𝟏. 𝟖𝟔 ℃/𝐦)(𝟎. 𝟒𝟎𝟎 𝐦)(𝟏) = 𝟎. 𝟕𝟒𝟒 ℃

∆𝑻𝒇 = 𝑻𝒇 ° − 𝑻𝒇 ⟹ 𝑻𝒇 = 𝑻𝒇 ° − ∆𝑻𝒇 = 𝟎. 𝟎𝟎 ℃ − 𝟎. 𝟕𝟒𝟒 ℃ = −𝟎. 𝟕𝟒𝟒 ℃

• Therefore, the freezing point of the solution is −0.744 ℃.

• First calculate the freezing point change, ∆Tf :

∆𝑻𝒇 = 𝑻𝒇 ° − 𝑻𝒇 = 𝟎. 𝟎𝟎 ℃− (−𝟎. 𝟗𝟑𝟎 ℃) = 𝟎. 𝟗𝟑𝟎 ℃

_____mL _mL _mL _____mL

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2. Mass of glacial acetic acid (show calculation) _ g _ kg