Prac Manual CHE10001-CHE10004 PDF

CHE10004 Introduction to Chemistry
CHE10001 Chemistry 1
Laboratory Manual
Compiled by Marylou Molphy and Daniel Eldridge

Edited with the assistance of Sheila Curtis & Andrea Chisholm
Faculty of Science, Engineering & Technology

(2)
CONTENTS
Experiment Title Section
Lab Timetable Blackboard
1 Apparatus and Techniques in Chemistry 1.1
2 Investigating Chemical Reactions 2.1
3 Titration of Lemon Juice 3.1
4 What solution is that? 4.1
5 Identification of an unknown solid diprotic acid 5.1
6 Buffers & pH titrations 6.1
7 Spectroscopic analysis of sodium salicylate 7.1
8 Analysis of Ascorbic Acid 8.1
The experiments detailed in this manual require adequate knowledge of

appropriate techniques and safety precautions.
Before attempting any of the experiments, students should be familiar
with laboratory safety and must have passed the Online Safety Induction.
(3)
Assessments
Reports A report is to be submitted for each prac – due one week after completing
your experiment
Safety Induction Online Induction must be passed (100%) to enable you to commence the
practical component. This is accessed through Blackboard, Subject Code
Access Laboratories: Safety Induction*
Practical Techniques You will be asked to accurately determine a concentration of an unknown
Exam solution, using techniques and experienced gained through the course of
the semester. This exercise is done under exam conditions.
Assessment
There are two forms of assessment for the practical component:
1. Reports
Each report will be marked according to a marking scheme that is based on your raw
results, the interpretation of these results, and answers to questions. All reports will be
given the same weighting and contribute 15% of your overall mark for the unit.
Penalties for failing to observe safety and other rules will be deducted from your overall
mark and could result in a fail in the subject.
2. Practical Exam
At the end of the semester there will be a practical exam, worth 10% of the overall mark in
the unit. More information will be provided during the course of the semester.
These two components form the practical mark for this Chemistry unit, which is worth 25% of
the overall mark in the unit.
Safety Induction
You are required to read through the safety material online and complete a short online safety
induction. Only this information will be tested. By gaining a mark of 100% and thereby passing
this induction, it will enable you to commence the lab work. The first active lab session is in
Week 3 or 4 depending on your timetable. Please ensure that you have completed the induction
prior to this session. See the unit site on Blackboard for full details:
www.ilearn.swin.edu.au
MY UNITS > ACCESS LABORATORIES: SAFETY INDUCTION > ANNOUNCEMENTS
YOU WILL NOT BE ABLE START EXPERIMENTS UNTIL THIS IS DONE.

You will excluded from the lab and receive zero marks for any work missed.
For full and additional details, please refer to the Lab Reference Manual on
blackboard
(4)
Helpful hints!
Calculating averages and deviations
You will frequently be asked to calculate an average result and a

deviation, as a means of assessing accuracy and precision. There are
many different ways that scientists calculate deviation. Throughout the
unit, we will use the following convention:
1) Calculate the average of your best 3 results

- (sum of best 3 results, divided by 3)
2) Compare your average value to the 3 results that you used in

calculating your average. Identify which of the 3 values lies furthest
from the average.
3) Calculate the difference between your average value and the value
that was furthest away and quote this as your deviation. This is
referred to as the maximum deviation.
Eg. If 4 results are obtained to be 19.14,19.22, 19.23 and 19.25 mL:
1) Omit 19.14 – only use your best 3 to calculate the average:

- (19.21+19.22+19.25)/3 = 19.233 mL
2) Furthest value away is 19.25 mL
3) 19.25 – 19.233 = 0.0167 = 0.02 mL (just use one digit)
Result = 19.23 ± 0.02 mL
Unit conversions to be aware of…
1 cm3 = 1 mL
1 dm3 = 1L
1L = 1000 mL
1000 mg = 1 gram
(5)
Practical Write-Up Hints and Tips
DON’T use the first person (I, my, our, we).
DON’T use “flowery” language.
Try to write as “scientifically” as possible – use a very direct approach and don’t draw
out a statement to take up more space; be concise.
Aim: State what you wanted to do and how you wanted to do it – no fluffing around!
Example:
Aim: To determine the concentration and percent composition of tartaric acid in red
wine by pH titration.
Method: Write in paragraph (not dot points) a procedure for how you conducted the
experiment. Fine details are not necessary at this level. Someone should be able to
read your method and then, if necessary, repeat your work.
Example:
Method: A sample of fresh red wine was vacuum filtrated to remove all pips
sediment. An aliquot of 20 mL of the filtrate was taken and diluted to 200 mL.
Finally, 20 mL aliquots of the dilute red wine were titrated against ~0.1 M NaOH until
concordancy was obtained.
Results: Include calculations, tables and graph but do not discuss your data.
See next page for notes on writing discussions and conclusions

(6)
Discussion: Now is the time to analyse your data, make comparisons and draw
conclusions from your work. You should start by looking at your own results – are
they sensible? Are replicates reproducible? If not, any reasons why? What is the
significance (if any) of your findings? Then, expand the circle you’re looking in –
compare your results with class results and discuss in the same light. Then, step out
further – look at manufacturer’s specifications. Each step along the way, you should
‘flesh out’ any important points, discoveries or ideas that you come across.
In this subject, you are often given objectives that must be covered in your discussion
– be SURE that you’ve covered these points!
When you’ve finished your discussion, a reader should have knowledge of how
accurate and precise your results are, any significance that they have, a quantitative
comparison between them and class or manufacturer’s results and a good
understanding of any key conclusions that can be drawn from your experimentation.
Conclusion: Answer your aim! Again, no fluffing around! Briefly state your findings
and be sure to include quantitative results. No new information should be introduced
in the discussion.
If it’s applicable or of an important nature, you can briefly state any notable
comparisons to manufacturer’s specifications. An example of when this would be
appropriate is when you can say whether a tested sample did or did not meet the
manufacturer’s specifications.
Example:
Conclusion: The concentration of tartaric acid in red wine was determined by acid-
base titration to be 0.024 M.
1.1
Experiment 1: Apparatus and Techniques in Chemistry
Special Precautions
Chemical glassware is fragile and must be handed with due care. Broken glass can
lead to serious cuts to hands and unprotected feet. Shoes which cover the whole
foot must be worn. For your own safety, you will not be permitted to do practical
work unless correctly attired.
Electronic balances are used for accurately weighing small amounts of material.
These balances are extremely delicate and must be handled with care. Any
chemical material spilt on the balance may damage the components and must be
cleaned up immediately.
Introduction
All volumetric glassware is made to deliver or contain a certain volume of water under
specified conditions in accordance with specifications laid down by the Standards
Association of Australia. Thus a bulb pipette may deliver a nominal value of 20.00
mL of water under specific conditions with a tolerance of ± 0.06 mL (i.e. the volume
delivered would be in the range 19.94 – 20.06 mL for that specific pipette). A B-
grade burette is generally designed to deliver any volume between 0 – 25 mL to an
accuracy of ± 0.08 mL. A standard flask would contain for example 200 or 250 mL of
solution to an accuracy of ± 0.15 mL. A graduated pipette can also be used to deliver
a determined volume within an accuracy of 4%. However it should be noted that
tolerance is dependent on the manufacturer and the glassware itself, therefore a
tolerance can't be generally assumed in precise analytical experimental work.
By using the four pieces of apparatus mentioned, it is possible to carry out an
accurate determination of the amount of some constituent in a liquid or solid form.
For example, how much phosphate is in a given amount of soap powder or how
much hypochlorite is in a given volume of bleach solution?
The concentration of a liquid or a solid can be expressed in a variety of ways: gram
per 100 mL of solution (% w/v), mole per litre (mol L-1 = M), parts per million (ppm,
which is equivalent to milligrams per litre), gram per 100 gram (% w/w) and for liquids
only, mL per L or mL per 100 mL (% v/v).
An understanding of accuracy, precision and knowledge of the importance of
quantitative measurement is essential for any competent chemist.
In this experiment you will learn how to correctly use, take the care of, and the errors
associated with, each of the following pieces of apparatus: burette, bulb pipette,
graduated pipette, measuring cylinder and analytical balance. After mastering the
use of this equipment you will be able to accurately prepare dilute solutions, using
the apparatus discussed above.
1.2
Method (Overview)
Your primary task is to deliver 20 mL of water from 4 different pieces of equipment,
into a conical flask. You are required to carry out two measurements (duplicate) with
each piece of apparatus. Record all data for each piece of apparatus in the
appropriate place on the Results Sheet and hand in a copy at the end of the
experiment. You should also enter your results into the spreadsheet (computer at
the rear of the lab) for class analysis and discussion in your report. For each piece of
glassware, note the manufacturer's error value that has been stamped on the
glassware itself. Write these values on the results pages.
As you will be using distilled water all day and need to monitor the temperature, place
a beaker of water on your bench, leave a thermometer in the beaker and then record
the temperature as needed.
Weigh a clean, corked 100 mL conical flask on the analytical balance and record its
mass. Note the temperature at this time.
Deliver 20 mL of the distilled water from your apparatus into the conical flask, cork
the flask and reweigh using the same analytical balance. Determine the mass of
water delivered and then the volume by using the appropriate temperature/density
conversion value obtained from the density table below (remember D = r = m/V).
When delivering a second volume of water simply add to the previous addition. Your
initial mass of container and cork will be the mass of container plus cork plus water.
For example, if your final mass from your 1st test was 69.2486 g, then you can use
69.2486 g as the initial mass of your next measurement.
Temperature (°C) Density (g cm-3) Temperature (°C) Density (g cm-3)
15 0.9991 23 0.9975
16 0.9989 24 0.9973
17 0.9988 25 0.9970
18 0.9986 26 0.9968
19 0.9984 27 0.9965
20 0.9982 28 0.9962
21 0.9980 29 0.9959
22 0.9978 30 0.9957
EQUIPMENT TECHNIQUES
The Analytical Balance

The analytical balances are using for measuring highly accurate and precise masses.
Be careful not to spill anything on them. To use the balances:
Ø Do not move balances
Ø Make sure you use the same balance every time
Ø Close all doors on the balance
Ø Zero the balance
Ø Slide open a door, place your sample on the balance, and slide the door shut
Ø Once the reading has settled, record your mass. Include ALL FOUR decimal
places.
1.3
The Bulb pipette

To use a bulb pipette:
Ø Ensure that it is clean
Ø Always use a safety bulb
Ø Rinse the pipette with a small amount of solution to be delivered, by drawing
up approximately half the volume of the pipette and then swirling it around the
pipette. DO NOT allow liquid to get into the safety bulb. If this happens, ask
your demonstrator to teach you how to fix it (and don’t do it again!)
Ø Draw the liquid up, until the solution is ABOVE the line of 20 mL
Ø Remove the pipette from the solution and use paper towel to dry of the outside
of the tip of the pipette
Ø Drain the solution into a waste beaker until you are at the 20 mL mark. This is
when the bottom of the meniscus is sitting on top of the line
Ø Deliver the 20 mL aliquot into your flask, with the tip of the pipette touching the
side of the receiving flask
Ø Once the pipette has drained, leave the tip in contact with the side of the flask
for a further 15 seconds
The Graduated Pipette

The technique for the use of a graduated pipette is similar to that used for the bulb
pipette. When delivering 20 mL, try to drain from 0 to 20, as it is more accurate than
draining from 5 to 25.
The Burette
To use a burette:
Ø Ensure that it is clean
Ø Rinse the burette with the solution that you are going to use
Ø Clamp the burette into place in a retort stand
Ø Make sure the tap is closed (horizontal)
Ø Fill the burette, using a small funnel to assist you
Ø As soon as you finish filling, remove the funnel
Ø Make sure the outside of the burette is dry
Ø Open the tap (vertical) and run some liquid through the tap to fill the air-gap.
Make sure that no air bubbles are present
Ø Take an initial reading, to TWO DECIMAL PLACES (eg. 0.43 mL)
Ø Open the tap to deliver the solution. As we proceed through the semester,
you will need great control over the tap. Try getting a single drop to fall, or
getting a drop to form on the tip, but not quite fall!
Ø When you reach your desired volume, turn off the tap and again, read your
volume to TWO DEMICAL PLACES
Ø The volume delivered will be the difference between your final and initial
volumes
1.4
The Measuring Cylinder

Using a dropping pipette (plastic dropper), add as close as possible to 20 mL of
water to the measuring cylinder. Once you have 20 mL, pour the liquid directly into
the conical flask.
Note that the plastic pipettes are disposable – don’t try to clean them!
When you are packing up for the day, take care to ensure that you put your pipette
and burette back in your locker with the TIPS FACING UPWARDS.
Analysis of Errors in each Apparatus
Enter the volumes recorded for each piece of apparatus into a class spreadsheet
before leaving the laboratory. These values will be analysed by your demonstrator to
give an indication of the error obtained for in each piece of equipment as a class.
You can obtain a copy of the class result (through the unit website on Blackboard) for
analysis and interpretation/discussion as part of your report.
Report
Your report should be written on the results sheets provided.
You should include in the discussion:
Agreement of class average to the manufacturer’s specifications
Possible logical reasons for difference of class result to manufacturer’s stated
values
Reproducibility (precision) of your own results
Accuracy of your own results with the expected values
Variability of Error for different and the same glassware
Assessment of the most accurate piece of apparatus to be used for delivering a
volume in a given situation.
In the conclusion you should be able to indicate the most appropriate piece of
glassware to use for different applications. E.g. when an accurate volume is needed,
use a “…….” whereas for an approximate volume a more suitable piece of apparatus
is the “………”.
-
Manufacturer’s Specifications
Pipette: 20.00 ± 0.06 mL Graduated Pipette 20.0 ± 0.2 mL
Burette 20.00 ± 0.08 mL Measuring Cylinder 20.0 ± 0.5 to 1.0 mL
If you are after more clues on how best to structure a report, see pages 5 and 6
of this manual.
1.5
PRACTICAL SESSION (Day/time): NAME:
RESULTS SHEET
Experiment 1: Apparatus and Techniques in Chemistry
Use of Volumetric Glassware
Apparatus Bulb Pipette Graduated Pipette

Nominal volume delivered 20 mL 20 mL
Manufacturer's Stated Error
1 2 1 2
m(container)
m(container) + water
m(water)
Temp of water (°C)

Density
(from correlation table)
Calculated Volume
delivered (V = m/D)
Apparatus Burette Measuring Cylinder

Nominal volume delivered 20 mL 20 mL
Manufacturer's Stated Error
1 2 1 2
m(container)
m(container) + water
m(water)
Temp of water (°C)

Density
(from correlation table)
Calculated Volume
delivered (V = m/D)
When storing your pipette and burette in your locker, which end faces upwards?
1.6
Experiment 1
Accuracy and Precision of Glassware – Report Template
Instructions: Complete the blue text entry sections to complete your report. Sections in
purple represent tips on how best to complete the required information. Once you’ve
completed all text entry sections, you are ready to save and submit.
Aim
An example aim has been written for you. You don’t need to write one for this experiment.
To determine the accuracy of delivering a specific volume of water from commonly used
laboratory apparatus when used according to manufacturer’s procedures and to then
compare each piece of apparatus to each other and the manufacturer’s specifications. This
will allow the determination of the most appropriate use for each piece of apparatus
.
Method Summary
An example method summary has been written for you. You don’t need to write one for this experiment.
A clean bulb pipette, graduated pipette, burette and measuring cylinder were used to deliver
20 mL of water of a known temperature to a pre-weighed conical flask. The mass of this
volume of water was then converted to the true volume of water delivered with the assistance
of density tables.
1.7
Individual Results
Insert a copy of your individual results here.
Bulb pipette Bulb pipette Graduated Graduated

1 2 pipette 1 pipette 2
Mass of water
Temperature
(oC)
Density
Volume of water
(mL)
Burette 1 Burette 2 Measuring Cylinder 1 Measuring Cylinder 2
Mass of water
Temperature (oC)
Density
Volume of water
(mL)
Class results
Get a copy of your class results and enter them here.
Graduated Measuring
Bulb pipette Burette
pipette Cylinder
Average volume
(mL)
Standard deviation
(mL)
1.8
Discussion
You should include in the discussion:
• Accuracy and precision of your own results compared with the expected values.
• Agreement of class average to the manufacturer’s specifications and individual results.
• Possible logical reasons for difference of class result to manufacturer’s stated values.
• Assessment of the most accurate piece of apparatus to be used for delivering a volume in a given
situation.
Manufacturer’s Specifications
Pipette: 20.00 ± 0.06 mL Graduated Pipette 20.0 ± 0.2 mL

Burette 20.00 ± 0.08 mL Measuring Cylinder 20.0 ± 1.0 mL
1.9
Conclusion
In the conclusion you should answer your aim. In this case, you should be able to indicate the most appropriate piece of
glassware to use for different applications.
2.1
Experiment 2. Investigating Chemical Reactions
Special Precautions
This experiment relies on accurate observation of changes in colour, evolution of
gases, formation of insoluble precipitates and evolution of heat. Perform test tube
experiments with careful addition of reagents, with constant shaking. The simple
tests, used to identify the products of the chemical reactions, need to be performed
very carefully.
You will be using a wide variety of chemical solutions and compounds, including
acids and heavy metal solutions. Treat all chemicals as hazardous and handle
them with due care (refer to the Safety section of the Reference Manual). Beware of
spillages and glass breakages.
Some compounds will require heating using a bunsen burner. Due care must be
exercised with regard to this procedure to avoid hot liquids spurting out of test tubes
and causing burns to yourself and others. This can be avoided if test tubes are
directed away from yourself and other people.
Where instructed, dispose of chemicals to appropriate waste containers.
Introduction
Chemistry is an experimental science. The many thousands of reactions undergone
by chemical compounds are established by experiments, using in most cases quite
simple apparatus. Many of the products of chemical compounds can be established
by simple tests. A systematic use of these tests allows products of unknown
chemical reactions to be identified.
In this experiment you will study physical and chemical properties of compounds and
study their chemical behaviour in order to be able to identify unknown reactions. You
will be required to write chemical reactions and predict when chemical reactions will
take place.
If you are unfamiliar with these concepts and reactions, you should read carefully the
relevant sections of your textbook and lecture notes before attending the practical
class.
Theory
Often very apparent observations can be used to assist you in determining whether a
chemical reaction has taken place (e.g. change of colour, evolution of a gas). The
following pages provide helpful information to identify reactants and products of
chemical reactions.
2.2
Colours of Ions in Aqueous Solutions

Most coloured compounds involve transition metals as one of the elements.
Common ions (such as K+, Na+, Cl-, NO3-, SO42-) are colourless. The colours of
some ions in solutions are:
-
Cu2+ blue Fe2+ very pale green Ni2+ green
Co2+ pink Fe3+ orange to yellow Cr3+ bluish grey
MnO4- purple Mn2+ very pale pink Cr2O72- orange
CrO42- yellow
Neutralisation Reactions
Many chemical reactions involve the use of strong acids and bases. Strong acids will
form weak acids from compounds containing their conjugate bases, often forming
gases. Strong and weak bases often lead to the formation of insoluble hydroxides.
A summary of the common strong acids and bases are given below:
Strong Moderate Weak
(completely ionised) (partially ionised) (slightly ionised)
HF, CH3COOH, organic
Acids HCl, HBr, HI, HNO3, H2SO4 HSO4-, H3PO4
acids, HNO2, HOCl
Bases NaOH, KOH, Ba(OH)2 NH3
Thermal Decomposition Reactions

Thermal decomposition reactions lead to simple molecules being produced. The
effect of heat on solid metal salts is summarised below:
Type of Metal Salt Decomposition Product
Metal chlorides - stable (but often volatile)

Metal carbonates - Group I: stable
- others: metal oxide + CO2
Metal nitrates - Group I: metal nitrite + O2
- others: metal oxide + NO2 + O2
Metal hydroxides - Group I: stable
- others: metal oxide + H2O
Metal sulphates - Groups I and II: stable
- others: metal oxide + SO3
Ammonium compounds - readily decompose N containing gases
(various)
Heavy metal compounds - often form free metal (e.g. Hg, Ag, Pt, Au)
2.3
During this experiment you will be required to carry out a series of tests to establish
the products of different chemical reactions. Your demonstrator will assist you in
conducting these experiments most efficiently. The following is a table of
standard tests that will be used. The purpose of the test and the expected
observation are also included.
OBSERVATION(S) & RELEVANT

TEST PURPOSE
EQUATION (WHERE APPROPRIATE)
Glowing string Test for O2 String glows brighter and rekindles

Test for an acid gas
Wet blue
e.g. HCl, SO2, NO2, Blue litmus turns red
litmus
CO2
Moist red Test for a basic gas
Red litmus turns blue
litmus e.g. NH3
Film of Test for CO2 Film turns milky
Ba(OH)2 Ba (OH)2 + CO 2 ® BaCO 3 + H 2 O
SO2 also gives a similar reaction
Paper of Paper: Test for SO2 The purple solution on the paper will turn
KMnO4 brown and then colourless
2 MnO4- + 5SO + 2 H 2O ®
2
2 Mn 2 + + 5SO42 - + 4 H +
Ignition Test for H2 Gas mixture “pops”. Explosive reaction
between H2 and O2.
2H 2 + O 2 ® 2H 2 O
Colour Test for NO2 Brown gas
CO2, SO2, H2S, O2 and H2 are colourless
Odour Test for SO2, NH3, H2S SO2 – pungent
and NO2 NH3 – pungent
H2S – rotten eggs
NO2 – sickly sweet
Metal Replacement
Metal replacement reactions are redox reactions. In the example illustrated here, one
metal dissolves and becomes aqueous ions, while the others comes out of solution
as a solid.
Names of Compounds
When using chemical compounds in practical work, you will be required to identify
the compound by its name or chemical formula. Refer to our lecture and table of
cations and anions for a list of the names and formulae of some common inorganic
cations and anions.
2.4
Method
Colour of solid salts and their ions in solution.
Refer to the demonstration set-up and record the colour of all the following solids and
their solutions in distilled water.
MnCl2.4H2O FeSO4.7H2O CoCl2.6H2O NiCl2.6H2O CuSO4.5H2O
Cr2(SO4)3.15H2O FeCl3.6H2O K2Cr2O7 K2CrO4 KMnO4
Which ions are responsible for the colour in each solution?

(Note that K2SO4 and KCl form colourless solutions)
Precipitation Reactions
Mix the given quantities of the reagents listed in the Precipitation Reactions section
of the results sheets and record your observations.
Neutralisation Reactions
In a clean test tube, prepare the mixture given in the Neutralisation Reactions section
of the results sheet and warm gently in a water bath. Record your observations.
Evolution of Gases
Mix the given quantities of reagents listed in the Evolution of Gases section of the
results sheet and warm gently in a water bath. In each gas, test for the identity of the
evolved gas using the tests given in the Theory section of this prac.
Metal Replacement
To 5 mL of 0.1 M CuSO4 solution in a test tube, add a small strip of zinc metal (emery
paper should be used if the surface is oxidised). Carefully observe the zinc surface
and solution for any changes in appearance, colour etc.
Thermal Decomposition Reactions (Demonstration)
For each of the solids listed in the Thermal Decomposition section of the results
sheets, take enough solid to fill approximately 1/3 of the bulb of an ignition tube, and
then heat carefully over a bunsen burner. Record all changes in the physical state of
the solid, the colour and odour (carefully) of any gases evolved and finally test any
gases evolved to confirm the identification.
Report
Your report should be written on the sheets provided. In addition, there are additional
equations on Page 2.9 to be completed and submitted with your report.
Don’t forget your 4 known reaction types (molecular equations shown below):
Acid + carbonate ® CO2 + H2O + salt
Acid + sulphite ® SO2 + H2O + salt
Acid + base(OH) ® H2O + salt
Precipitation (solubility table)
2.5
Experiment 2
Chemical Reactions – Report Template
Instructions: Complete the blue text entry sections to complete your report. Sections in purple
represent tips on how best to complete the required information. Once you’ve completed all text entry
sections, you are ready to save and submit.
Note that there is no discussion required for this experiment – that way, you get time to see your
feedback on your last attempt before submitting another one.
Aim
To use chemical and physical properties to identify the products of chemical reactions, and
from these observations, write balanced meaningful chemical equations to summarise the
reaction.
Results
Complete each of the tables, including observations and reactions.

Remember when typing in your chemicals, you need to use superscripts and subscripts. In Adobe Acrobat, pressing Ctrl+E will
open up the panel to select these options. Or, you can highlight the text and push “Ctrl+Shift+=” for superscript, or press
“Ctrl+=” for subscript.
There are hints for how to do this quickly in the Report Writing Guide on Canvas.
2.6
Colour of solids and their solutions
Most coloured compounds involve transition metals as one of the elements. Common ions (such
as K+, Na+, Cl-, NO3-, SO42-) are colourless. The colours of some ions in solutions are:
Cu2+ blue Fe2+ very pale green Ni2+ green
Co2+ pink Fe3+ orange to yellow Cr3+ bluish grey
MnO4- purple Mn2+ very pale pink Cr2O72- orange
CrO42- yellow
Colour of Colour of
Ion Responsible for Colour
Solid Solution
MnCl2.4H2O
FeSO4.7H2O
CoCl2.6H2O
NiCl2.6H2O
CuSO4.5H2O Blue Blue Cu2+(aq)
Cr2(SO4)3.15H2O
FeCl3.6H2O
K2Cr2O7
K2CrO4
KMnO4
2.7
Precipitation Reactions
Make use of your solubility table
Initial Reagent Second Observation Ionic Equation

Reagent
White powdery
0.1 M AgNO3 0.1 M Na2CO3 2Ag++ CO32- ® Ag2CO3(s)
precipitate
0.1 M AgNO3 0.1 M NaCl
0.1 M AgNO3 0.1 M Na3PO4
0.1 M BaCl2 0.1 M Na2SO4
0.1 M BaCl2 0.1 M Na2CO3
0.1 M Zn(NO3)2 0.5 M NaOH
0.1 M Cu(NO3)2 0.5 M NaOH
Neutralisation Reaction
Have a close look at the two chemicals reacting – what type of chemicals are they?
Reaction Observation Ionic Equation

~0.1 g Ca(OH)2(s)
+ 1 mL 2M HCl
+ gentle warming
2.8
Evolution of Gases
Page 2.3 of your lab manual (or the evolution of gases section of your digital method) has all
kinds of interesting and useful information regarding the properties of different gases. Coupled
with your topic 4a lecture notes, you should have everything that you need.

General observations:
Odour:
0.1 g Na2CO3(s)
+ 1 mL of 2 M
H2SO4 + gentle
warming in Litmus test:
water bath
Ba(OH)2 film:
Odour:
0.1 g Na2SO3(s)
+ 1 mL of 2 M
H2SO4 + gentle
warming in Litmus test:
water bath
KMnO4 paper:
0.1 g ZnS(s) +
1 mL of 2 M
H2SO4 + gentle Odour:
warming in
water bath
Litmus test:
2.9
Metal Replacement
Metal replacement reactions are redox reactions, or electron transfer reactions.

In the example illustrated here, one metal dissolves and becomes aqueous ions, while the other
comes out of solution as a solid.

5 mL 0.1 M
CuSO4(aq) + small
strip of cleaned Zn
metal
Thermal Decomposition
We’ll do this reaction as a class – be sure to record the observations.

Page 2.2 has some strong hints on how to write these reactions (your digital lab instruction
does too) and page 2.3 of your lab manual has all kinds of interesting information regarding the
properties of different gases.
Reaction Observation Molecular Equation and conclusions

Glowing String:
Demonstration: Litmus paper:

What do you learn from the observations?
1/2 of the bulb of
an ignition tube
of Mg(NO3)2(s) + Colour (gas):
strong heat over
Molecular equation:
a Bunsen burner
flame
Odour:
Conclusion
In the conclusion you should answer your aim. In this case, it will be quite general.
2.10
Quetsions
Given what you’ve learned in the experiment, complete these reactions below:
1. Precipitation
Molecular K2CrO4(aq) + BaCl2(aq) ®

Ionic
2. Neutralisation
Molecular Cu(OH)2(s) + HCl(aq) ®

Ionic
3. Evolution of Gases
(i) Molecular Na2SO3(aq) + HCl(aq) ®

Ionic
(ii) Molecular CuCO3(s) + HCl(aq) ®

Ionic
4. Thermal Decomposition (See p2.2)
(i) Cu(NO3)2(s) heat

¾¾ ¾
¾®
(ii) Ca(OH)2(s) heat

¾¾ ¾
¾®
3.1
Experiment 3: Titration of Lemon Juice
Special Precautions
You will be using 0.1 M NaOH solution. This solution should only be pipetted using a
safety bulb, not by mouth. If a small quantity of this reagent is spilled, it should be
immediately cleaned up using paper towel or a sponge.
Introduction
This experiment relies on techniques explored in experiment 1. You will be required
to correctly use a bulb pipette, standard flask and a burette. You will also need to
know how to filter under reduced pressure, perform a titration and judge the end of a
titration using an indicator. WATCH THE DEMONSTRATION VIDEOS – you will be
much better prepared!
This experiment illustrates the theory and practical skills associated with an acid-
base titration. The substance to be analysed, lemon juice, is a commonly
encountered material, containing citric acid, and is analysed by titrating with a base.
The generalised equation for this titration is:
F.
HA + OH- ® H2 O + A-
Theory
Citric acid (HOOCCH2C(OH)(COOH)CH2COOH) is the major acidic component of
lemon juice. It is a weak triprotic acid (i.e. it has three hydronium atoms (protons) it
can donate) and therefore to remove all three acidic hydrogens, 3 moles of OH- are
required to neutralise 1 mole of citric acid.
HOOCCH2C(OH)(COOH)CH2COOH + 3NaOH ® Na3(OOCCH2C(OH)(COO)CH2COO) + 3H2O
Phenolphthalein is a suitable indicator for this titration, changing sharply from

colourless to pink upon reaching the equivalence point.
Solid NaOH is not a primary standard because it reacts with both water and
atmospheric CO2 (to form NaHCO3) and hence an accurate mass of pure NaOH is
difficult to obtain. The NaOH solution provided has been standardised by reaction
with a primary standard, whose mass was accurately measured, thus it has a
calculated error associated with the determined concentration (e.g. 0.1006 ± 0.0001
M).
Method
Take a plastic reagent bottle, use 10 mL of ~0.1 M NaOH to rinse the reagent bottle
and then discard the rinsings. Collect approximately 150 cm3 of ~0.1 M NaOH in the
ml
3.2
r
labelled stoppered plastic reagent bottle (Note: NaOH etches glass). Note the
accurate concentration of the base from the container.
A container of freshly squeezed lemon juice is provided for use amongst a group of
3-4 students. Each group is required to filter the juice under vacuum, according to
the method discussed in your prac talk, using Whatman No. 4 filter paper. The side
arm filter flask has been previously dried so that the lemon juice is not diluted.
Students should take approximately 50 cm3 of the filtered juice for use as their own
sample. Leave any unused filtered juice in the filter flask.
Clean and rinse a bulb pipette with the filtered juice, and then use to dilute the juice
sample by pipetting 20 cm3 of the filtered juice into a 200 cm3 standard flask. Using a
reagent bottle or similar, add distilled water to the flask until it is 1 cm3 from the mark.
If there is foam present, add a few drops of ethanol. Carefully make up to the mark
by adding distilled water using a dropping pipette. Thoroughly mix the final solution
by inverting 40 times.
Rinse the pipette with a small amount of the diluted juice. Place 20 cm3 aliquots of
the dilute juice into four separate conical flasks and add 3 drops of phenolphthalein to
each. Titrate the solutions with the standardised NaOH solution according to the
method described in your preliminary videos and prac talk. The endpoint (the
experimental measure of the equivalence point) corresponds to the first permanent
faint pink colour appearing, and should take place over a very small volume addition
(less than a drop). Record your titre on the result sheet provided. Repeat this
procedure until 3 concordant titres are obtained i.e. within ±0.05 cm3 of each other.
Note that you CAN do more than 4 titrations, if time permits.
Enter the average of the three concordant titres and the standard flask volume in the
spreadsheet provided on the computer in the laboratory. This will be used to
calculate an average class result. Results will be made available for you via
Blackboard, for discussion in your report. The actual class average result should be
quoted in your report.
Calculations
Use your titration results (the average of your concordant titres) to calculate the
concentration (in units of molarity) of the citric acid in the diluted and original (filtered)
sample. Use the undiluted juice volume to calculate the percentage composition by
mass of the juice with respect to citric acid i.e. grams of citric acid per 100 g of lemon
juice. (Hint: molarity = M º moles in 1 litre). Assume the density of lemon juice is 1.0
g cm-3.
Don’t forget your useful tools for calculations:

n = cv m = nM c1v1 = c2v2 And the three-step plan!
Report
Your report should be written on the report sheets provided, which includes a
discussion of the class results. A conclusion should also be written which answers
the aim and states the main or significant result.
3.3
Experiment 3: Titration of Lemon Juice
Results Sheet
Actual concentration of NaOH solution: NaOH (~0.1 M) M
Volume of standard flask used for juice dilution: cm3
Burette
Trial 1 2 3
Readings
Initial (cm3)
Final (cm3)
Titre (cm3)
Average titre of ~0.1 M NaOH = ± * cm3
* Note that the error recorded here is the maximum deviation (or spread) of the
individual titres and the average result. To find it, calculate the difference
between your average titre and whichever individual titre is furthest from the
average (excluding the value that you didn’t use). See page (4) of this practical
manual for more assistance if necessary.
When storing your pipette and burette in your lockers, which way should the tip be
facing?
____________________
If you’re not confident with your stoichiometry, take the time to discuss your strategy
with your practical demonstrator before you leave the lab.
3.4
Experiment 3
Analysis of citric acid in lemon juice by titration
Aim
To determine the concentration of citric acid in filtered lemon juice by titration with
standardised NaOH solution.
Method summary
An example method summary has been written for you. You don’t need to write one for this
experiment.
A sample of freshly squeezed and filtered lemon juice was quantitatively diluted by a factor of
10 using a 20 mL pipette and 200 mL standard flask. Then, 20 mL aliquots of the diluted
lemon juice were titrated against standardised ~0.1 M NaOH solution to the phenolphthalein
endpoint.
Equation
Citric acid
Results
Copy your data into the table below:
Concentration of NaOH (M) =
Titre 1 Titre 2 Titre 3 Titre 4
Average titre = ±
(Use your best 3 titres)
3.5
Calculations: Citric acid concentration in dilute lemon juice
Use your stoichiometry skills to determine the concentration of citric acid in the dilute lemon juice:

Citric acid
Concentration of NaOH = 0.0975 M

Average volume of NaOH used in the titration = 16.48 I 0.02
mL
Using this information, calculate the number of moles of NaOH consumed in the
reaction:
÷¥ 0.0016068 moles NaOH
yqmf×
=
( 6.
0.0975ft 00161 moles NaOH
×
I 0 .
Using your answer from the 1st step and the molar ratio for the chemical reaction
(shown above), calculate the number of moles of citric acid titrated by the NaOH:
0.60161 moles NaOH x = 0.000537 moles C. A

3. MOI NaOH
.
Volume of dilute lemon juice analysed for each individual titration = 20 mL

(Not the total amount of dilute lemon juice that you made)
Therefore, calculate the concentration of citric acid in the dilute lemon juice
sample:
0.000537 moles C. A .
X 1- X
1000mL
-
20 hL IL
T
. .
-
0.02678M
3.6
Calculations: Citric acid concentration in original lemon juice
Now that you know the concentration of citric acid in the dilute lemon juice, use
that to calculate the concentration of citric acid in the original, undiluted lemon
juice.
Dilution details:
Original concentration = ? M
Volume of original juice taken for dilution = 20 mL
Dilute concentration = O . 0026700 M (from previous calculation)
Final volume of dilute juice prepared = 200 mL
(i V, Cy Vy
.
0.02678Mt
Ci
-
0.0026-1,80×7002
-
= -
-
Calculations: %composition of citric acid in lemon juice
The concentration above tells you the number of moles of citric acid per litre of
lemon juice. Use this to calculate the Percentage composition of lemon juice
with respect to citric acid (w/v).
Hint: %w/v means, how many grams of citric acid would you find in 100 mL of
lemon juice?
1g 1mL
0.02678 Motes
-
x 4g×
1000mL (Moly
l
?
'
5. 14 0.514 .
.
=
.
Before moving on to your discussion, check your calculated results with those on blackboard.
If they don’t match up (within a small margin), go back and look over your work before you
proceed.
.
3.7
Using Feedback
Look at the feedback sheet that has been returned to you from your first practical submission.
Consider your strengths and weaknesses from your first report and tell us how that will influence
your approach to completing this report.
Question:
When completing the dilution in this experiment, why did we use a bulb pipette and
why did we use a standard flask?
Class Results
Get a copy of the class results and insert it here, you’ll need it for your discussion.
Average Standard deviation
Titre (mL)
[citric acid]dilute
[citric acid]original
%w/v citric acid

3.8
Discussion
Should include the following:
• Discussion of the molarity of the lemon juice from the class result (average concentration, standard
deviation) and comparison to your own results.
• How does your result compare to the expected range of 4.5 – 6.0% w/v?
• Potential causes of error in your result.
Conclusion
Answer your aim and include numerical results.
4.1
Which solution is that?!
Task: To discover the identity of a series of numbered test tubes using simple
chemical reactions, with minimal additional reagents.
Prize: This exercise is to be done in pairs (NO groups of 3). There are 2 sets of
unknown chemical solutions to solve. Once you are happy with your
identity allocation for each set, present your findings to the demonstrator
who will give you a score. A running total will be put up on the board for
each group. The highest score, after 2 sets of unknowns will be declared
the winner. In the event of a tie, the total time taken and the most sets with
full marks will decide the winner.
Method: Using only the contents of the five containers in each set, devise an
identification scheme that will allow the various solutions to be
distinguished, and ultimately identified.
(i) No other chemicals, reagents, indicators etc are allowed.
(ii) The only apparatus allowed is that which is commonly available, such as
test tubes, droppers, beakers, funnels and filter paper. No sources of heat
are to be used.
(iii) Devising the scheme involves your knowledge of solubility rules, gas
evolution and ion colours (contained within your lecture notes, the video
preview and also the tables within this document).
Report: A report as such is not required; however you will be required to document
your observations, any applicable equations that explain/support the
observations and a summary of your findings. This is to be handed in at
the end of the session on the sheets provided. This component will be
marked and a mark obtained as for a standard lab report.
4.2
"Rules of the Competition”/Procedure
This experiment will be conducted in pairs. You can assign a name to your pair for
purposes of the competition and then obtain the first set of unknown solutions to
determine. When you feel you have correctly assigned each solution, write one
example chemical equation for each chemical as proof and then hand in your sheet
with the appropriate number marked in the box adjacent to the solution name, and
any observations and equations associated with your findings (these will be marked
as in a normal lab report).
The demonstrator will award your group points for the number of correctly identified
solutions and then give your group the sheet detailing the second set of unknown
solutions to determine.
There are 2 sets of unknowns available to contribute to the highest aggregate score
of groups within the session. In event of several groups having the same highest
aggregate score, the winner will be decided on the number of sets identified correctly
as a whole, and the time taken to complete the 2 sets of unknowns. So you need to
work efficiently and carefully!
Preparation
The sets that you will be given in class will be a selection of cations & anions from
the following list. You should know what happens if each cation is mixed with each
anion in solution (Hint: look at the solubility tables on pages 4.5 and 4.6)
Cations Anions
Na+ H+ Cu2+ Cl- CrO42- SO42-
K+ Ba2+ Ca2+ Cr2O72- HCO3- SO32-
NH4+ Zn2+ Pb2+ NO3- OH- CO32-
Mg2+ Fe3+ Ag+
Mn2+ Co2+
4.3
Name that Solution! EXAMPLE Problem Set
Sample Set
Solution ID No.
Potassium carbonate K2CO3 E
Hydrochloric acid HCl B
Barium chloride BaCl2 A
Sodium sulphate Na2SO4 C
Results
Initial observation of unknown solutions:
A, B, C, E: all colourless solutions
Table of observations
Solution E B A C
E - - - -
Bubbles of gas
B - - -
(CO2) ?
No reaction
A White ppt - -
(Cl-) ?
C No reaction No reaction White ppt -

4.4
Discussion/Reasoning (including any chemical reactions that support your

observations) EXAMPLE
Solution Identity A / BaCl2
Observation(s)/Tests
Formed white ppt with 2 solutions, only cation that is insoluble with available anions
Equation(s), if applicable
Solution Identity B / HCl
Observation(s)
Doesn't form ppt with BaCl2, and causes gas to be produced when reacted with E (CO2)
Solution Identity E / K2CO3
Observation(s)
Gas produced when reacted with acid
CO 32 - + 2H + ® CO 2 (g ) + H 2 O
Solution Identity C / Na2SO4
Observation(s)
Forms ppt with BaCl2 (A)
SO 24 - + Ba 2 + ® BaSO 4 (s)
Solution Identity
4.5
Additional Information that may be useful
From Chang and Goldsby, “Chemistry“

4.6
H Na K NH4 Ag Pb(II) Ca Ba Mg Zn Cu(II) Mn(II) Fe(III) Al

Acetate S S S S sS S S S S S S S S S
Bromide S S S S I sS S S S S S S S S
Carbonate * S S S I I I I I I I I * *
Chlorate S S S S S S S S S S S S S S
Chloride S S S S I sS S S S S S S S S
Chromate S* S S S I I I I I I I I I I
Hydroxide S* S S S * sS sS S I I I I I I
Iodide S S S S I sS S S S S S S S S
Nitrate S S S S S S S S S S S S S S
Oxide * S S * I I sS sS I I I I I I
Phosphate S S S S I I I I I I I I I I
Sulphate S S S S sS I I I S S S S sS S
Sulphide d S S S I I * d d I I I d d
S = soluble sS = slightly soluble I = insoluble d = decomposes in water * = other
5.1
Experiment 5: Identification of an unknown solid diprotic acid
Special Precautions
You will be using a solution of ~0.1 M NaOH which is mildly corrosive. You will also
be working with solid diprotic acids, which are corrosive and classified as harmful or
as irritants. Avoid inhalation and wear gloves when handling the solid acids.
Introduction
This experiment looks to give you another opportunity to master your core laboratory
techniques. You will be required to correctly use a pipette, accurately weigh a solid
material by difference, make up a solution in a standard flask and complete accurate
titrations by correctly judging the end of a titration using an indicator. If you are
unfamiliar with these techniques you should consult the video demonstrations, the
written instruction in experiment 1 or your demonstrators.
This experiment illustrates the theory and practical skills with the use of an acid-base
reaction in a chemical analysis. You will be provided with one of a selection of
diprotic acids and asked to determine which one you have.
The techniques used in this experiment will be HIGHLY relevant for your
practical exam and for all of your future chemistry laboratory work.
5.2
Theory
A diprotic acid can be represented by the molecular formula, H2A, where the 2 H+ are
the two protons that the acid can give away and “A2-” represents the rest of the acid
molecule. These acids will react with a base to make water and a salt, Na2A.
The amount of acid present in a sample can be easily ascertained by titration with
NaOH. The chosen indicator for this titration, thymol blue, is yellow in acidic solution
and turns blue in basic solution.
In this experiment, we have provided you with a solid diprotic acid. Your task is to
determine which of the 5 acids shown on page 5.1 we have given you. To do this,
you will need to prepare an acid solution and then titrate it with standardised NaOH.
“Standardised” means that it is a NaOH solution of known concentration.
You will also do an analysis of experimental uncertainty to determine whether or not
you can definitively state which acid you have.
Method
Preparation of diprotic acid solution
Collect a dry weighing vial and use the top loading balance to weigh in approximately
0.9 – 1.0 grams of your solid diprotic acid. Then, take your weighing vial, glass
funnel, 200 mL standard flask and results sheet into the balance room. Accurately
weigh the mass of the weighing vial with the powder in it, to 4 decimal places.
Carefully transfer the solid through a glass funnel into the 200 mL standard flask,
ensuring that you don’t spill any powder. Then, re-weigh the vial, with any residue.
The difference between the 2 masses will be equal to the mass of powder transferred
to your standard flask.
Take your flask back out into the lab and thoroughly wash all of the solid acid through
the funnel into the 200 mL standard flask using distilled water. Dissolve by swirling
with the flask half full, then proceed to carefully make the solution up to the mark and
mix by inversion at least 40 times.
Analysis of the diprotic acid solution

Collect no more than 120 cm3 of ~0.1 M NaOH in a plastic reagent bottle. Make sure
all bottles are clean, dry and labelled before use, and stopper after reagent collection.
You should rinse each bottle with a small amount of the solution prior to filling. Note
down the exact concentration of the NaOH and the uncertainty in that concentration.
Question: Why should NaOH be collected in a plastic bottle and not glass?
After cleaning and rinsing your pipette and burette, deliver a 20 mL aliquot of your
diprotic acid solution into a conical flask. Add a few drops of thymol blue indicator to
the solution and titrate with the ~0.1 M NaOH solution. The endpoint is reached
when the indicator colour changes from yellow to green. The colour may fade, but
the solution should remain distinctly green after 10 seconds of swirling. Blue may
mean that you have slightly over-shot. Enter your results immediately onto your
results sheet.
Repeat the titration until 3 concordant titres are obtained (± 0.05 mL)
5.3
Calculations
Use your titration results (the average of your concordant titres) to determine the
number of moles of the diprotic acid in your 20 mL aliquot. Knowing that, you should
be able to determine the number of moles of acid in the original 200 mL solution.
Finally, re-arrange the equation, m = nM in order to determine the molar mass of your
diprotic acid.
You will also be completing an uncertainty determination (or error determination).

Assistance is provided in your laboratory write-up and below on this page.
Report
Your report should be written on the report sheets provided, which includes an aim,
method summary, calculations and discussion of your results. A conclusion should
also be written which answers the aim and states the main or significant result.
Experimental uncertainty:
Experimental uncertainty is an important concept. Once you have a numerical

answer, how sure are you of that value? If you know your molar mass to within 1
g/mol, you could be confident of your identification. However, if you were only certain
to within 10 g/mol, you might not definitively be able to identify your acid.
There are many ways to ascertain uncertainty. We will be using a typical error
analysis. This is calculated by determining the % error that each experimental step
contributes and adding them up to determine a total % error. Then, this % error is
multiplied by the final answer to determine the absolute uncertainty in the final result.
For example, an experiment that relies on a mass and a titration:
δresult δmass δtitre

= + , where “d” means “uncertainty in”
result mass Vtitre
δmass δtitre ö
Re-arrange: δresult = æç + ÷ ´ result
è mass Vtitre ø
Experimental uncertainty in the equipment you are using:
200 mL standard flask: ± 0.15 mL
25 mL burette (2 readings): ± 0.08 mL
20 mL pipette: ± 0.06 mL
Analytical balance (2 readings): ± 0.0004 g
These are your uncertainties, your values of “dx” for your uncertainty calculation.
5.4
Experiment 5: Identification of an unknown solid diprotic acid
Results Sheet
Preparation of diprotic acid solution
UNKNOWN ID:
Standard flask volume: mL
Mass of solid:
Mass of vial & powder (g)
Mass of vial & residue (g)
Mass transferred (g)
Analysis of diprotic acid solution
Actual concentration of standardised NaOH solution: ± M
Acid solution aliquot volume: mL
Burette Readings Flask 1 Flask 2 Flask 3 Flask 4

Initial (cm3)
Final (cm3)
Titre (cm3)
Average NaOH titre = ± mL

5.5
Experiment 5
Identification of a Diprotic Acid
Aim
A good aim tells the reader what you plan to achieve and very, very briefly, how you plan to do it.
Method summary
A good method summary should quantitatively tell a reader how the experiment was conducted,
without going into too much detail. You should assume the audience knowledge matches your
own, so there is no need to explain the inner workings of delivering an aliquot, or conducting a
titration.
5.6
Results
Copy your data into the table below:
Unknown ID = Mass of solid = Concentration of NaOH (M) =

Titre 1 Titre 2 Titre 3 Titre 4
Average titre = ±
(Use your best 3 titres)
Calculations
Use your stoichiometry skills and understanding of the mole concept to determine the molar
mass of your acid:
Number of moles of NaOH required to titrate the diprotic acid solution:
O.loutmoesNAOH-xiu.am/NaoHx-ooom-- o -
0015.291%77,81%11,9%4 .
Number of moles of diprotic acid that reacted with the NaOH:
Chemical Equation: H2A + 2NaOH " Na

,
At H2O
moles NaOH =
O 0007648335 moles H A
0.001529667 x -
2 moles 2 NaOH O 0007648 moles Hutt

y
-
Given that the value calculated above is the number of moles of acid in 20 mL of solution,
determine the number of moles of diprotic acid in the entire 200 mL solution:
0.0007648335 moles moles Hz A x a

0.007648335 moles
20mL
=
0.007648 moles
Molal mass -
me
Molar mass of the diprotic acid:
h
.
I. 0253g
134.0553205 glmol ?
acid
- =
007648
malic
G.
5.7
Calculation of experimental uncertainty

A result is only worthwhile if you’re relatively sure of it. We’re going to estimate the uncertainty in
your answer – of how sure you can be of the molar mass you just calculated.
To do this, we’ll need uncertainty data:
Experimental uncertainty in the equipment you are using:
200 mL standard flask: ± 0.15 mL

25 mL burette (2 readings): ± 0.08 mL
20 mL pipette: ± 0.06 mL
Analytical balance (2 readings): ± 0.0004 mL
These are your uncertainties, your values of “dx” for your uncertainty calculation.
Given that “d” means “uncertainty in”, calculate dM (the uncertainty in your molar mass) using
the following equation:
δM δstd.flask δmass δpipette δtitre δ[NaOH]
= + + + +
M Vstd.flask mass Vpipette Vtitre [NaOH]
( 200
to
1.0253
t t
14.61
81-0.0002
) M
0.1047=2.015819136
20
.
.
= 2.02
.
Therefore, dM, to one significant figure = 2. 0

(round up)
The molar mass of your acid is therefore 134 .
I ± 2. O
The likely identity of your acid (see below) is
O
5.8
Discussion
Include the identification of your acid and what your experimental uncertainty tells you about
your determination, along with comments on your accuracy and precision).
Conclusion
Answer your aim and include numerical results.
6.1
Experiment 6 Buffer Actions & pH Titrations
Special Precautions
The pH of a solution is measured using a special electrode called a pH electrode.
This electrode is fragile and must be handled with care.
A magnetic stirrer is used to stir solutions when doing a pH titration. A small magnet
encased in polythene, know as a "magnetic follower" is placed in the bottom of the
titration vessel and this is mounted on an instrument containing a revolving magnet
(which is driven by a variable speed electric motor). If stirring is too rapid, a vortex
will be produced in the solution and uncover the glass electrode. It may also cause
the magnetic follower to be thrown up and break the glass electrode.
Salts of toxic metals and weak acids and bases are used in this experiment. Despite
the fact that the concentrations of these solutions are low (and hence danger is
minimal), care should be taken.
General Instructions
• Data obtained for pH titrations is to be directly recorded and must be plotted on
graph paper during the course of each titration or marks will be deducted.
• Record all results directly onto the result sheets provided.
Introducing the pH meter

This experiment introduces students to the pH meter; an instrumental device for
determining the pH of solutions. The pH meter makes use of an electrochemical cell
to determine pH. The pH meter allows direct monitoring of pH at all times during a
titration. The meter needs to be calibrated using a buffer at a known pH.
The pH measurement is obtained using 2
electrodes, which have been combined to form
a single probe, termed a 'combination pH
electrode'. This consists of a pH half cell (or
measurement cell), whose voltage varies
proportionally to the hydrogen ion activity (H+)
of the solution being measured. The other half
of the probe is called a reference half cell,
which provides a stable and constant reference
voltage. The pH meter is connected to the pH
combination electrode and measures the
difference between the pH half cell and the
reference half cell in millivolts (mV) direct current. This mV reading is then converted
to a pH reading and displayed on the LCD display of the meter.
6.2
Theory
A. The Preparation and Properties of a Buffer.
All buffers arise from the combination of a weak acid and its conjugate base e.g.
CH3COOH/CH3COO-. The concentration of each component is relatively high (of the
order of 0.1 to 1M). The pH of a buffer depends on the pKa of the weak acid and the
relative amounts of the conjugate acid and base forms.
The interrelationship is given by the Henderson-Hasselbach Equation.
pH = pK a + log10
[A ]
-
[HA]
When a strong acid or base is added to the buffer solution the following reactions can
occur:
A- + H+ ® HA
HA + OH- ® A- + H2 O
These additions merely alter the relative amounts of A- and HA and hence the ratio of
A-/HA. The net effect is a very little change in pH. Or alternatively, a strong acid or
base is converted into a weak acid and base respectively and hence the H+ becomes
bound acidity (and not measured by the pH electrode).
Buffer solutions can resist a fairly large change in concentrations of one of the
component species before they cease to function. At this limit there is a sharp
change in pH. The pH of the buffer solutions is most conveniently determined using
a pH meter and a glass electrode.
B. Acid-Base Titration Curves.

The addition of an acid to a solution of base results in an increase of the hydrogen
ion concentration, [H+] and hence a change of pH. Near the stoichiometric
equivalence point, where n(acid) = n(base), there is a marked (rapid) change in the
[H+] for small additions of acid. The marked change in [H+] results in a large inflection
(change in direction of the gradient) in a plot of pH versus volume of added acid. The
exact stoichiometric point is found by identifying the inflection point. This can be done
by either obtaining a first differential plot at the inflection point (dpH/dV vs V) or by
suitable extrapolation of the graph. You will be using the second method.
A pH titration curve can also be used to aid in the choice of the best colour indicator
for a volumetric procedure. The appearance of the pH titration curve, or more
specifically the steepness of the change in pH around the equivalence point, will
ensure an appropriate indicator is chosen.
When a weak acid or base is titrated it is possible to determine not only the
concentration but also the pKa of the conjugate acid. This then allows the pKb of the
conjugate base to be calculated as well as the pH of the weak acid or base at any
point in the titration.
6.3
Cloudy ammonia contains the weak base, NH3. The concentration of NH3 in cloudy
ammonia can be determined by titration with standard acid.
NH3 + HCl ® NH4+ + Cl-
At half-neutralisation, a buffer solution exists and the Henderson-Hasselbach
equation applies.
[NH 3 ]
pH = pKa + log10
[NH ]
+
4
Since at half-neutralisation volume, [NH3] = [NH4+] therefore the corresponding
pH equals the pKa.
The literature value for Ka of NH4+ is Ka = 5.6 ´ 10-10 NB. pKa = -log(Ka)
Method
Calibration Check of the pH meter
Use the instructions and solutions provided to calibrate your pH meter.
A. BUFFERING ACTION
Question 1 of the report refers to this section.
Preparation of a Buffer (Record results on page 6.6)
Add 50 mL of 0.2 M CH3COOH to a 250 mL beaker, with the magnetic stirrer mixing
the solution. Record the pH
To the above solution, add 50 mL of 0.2 M CH3COONa, measure & record the pH.
This solution is now a buffer, 0.1 M with respect to acetic acid and 0.1 M with respect
to the acetate ion.
Split the solution into two portions of approximately 50 mL.
(i) Effect of Addition of Base to the buffer
Using one portion of the buffer solution, first remeasure the pH and then add 2 mL of
0.5 M NaOH, mix well and record the new pH.
For comparison, measure the initial pH of 50 mL of tap water. Measure the change
in pH when 2 mL of 0.5 M NaOH is added.
(ii) Effect of Addition of Acid to the buffer
To a second portion of the buffer solution, measure the pH and then add 2 mL of 0.5
M HCl, mix and record the new pH.
For comparison, measure the initial pH of 50 mL of tap water. Measure the change
in pH when 2 mL of 0.5 M HCl is added.
6.4
ACID-BASE TITRATION CURVES
Titration of dilute cloudy NH3 with ~0.1 M HCl
(Plot a titration curve as the titration proceeds, marks will be deducted otherwise).
NOTE DOWN THE DILUTION FACTOR FOR THE COMMERCIAL AMMONIA
Note: A dilution factor of 75 mL/L means that we have taken 75.0 mL of the
commercial product and diluted it to a final volume of exactly 1 litre with distilled
water.
Pipette 20 mL of the dilute cloudy NH3 (note from the container how this solution was
prepared) into a 250 mL beaker, add about 100 mL of distilled water (enough to
ensure that the electrode tip is covered) and mix. Immerse the glass electrode and
measure and record the initial solution pH (with no addition of acid).
Set up a burette containing ~0.1 M HCl so that the titrant can be added directly into
the solution on the magnetic stirrer.
For the titration, add suitable volumes of ~0.1 M HCl recording the pH after each
addition until 25 mL have been added. Make sure you wait the same amount of time
(eg. 10 seconds) after each addition of acid before taking a reading.
As the titration proceeds, suitable volumes for addition are judged from the pH
versus volume added titration curve, plotted during the course of the titration.
Suitable volumes are volumes that cause a change of approximately 0.1 to 0.2 pH
units or more. Such volumes will be large (1 to 2 mL) in the initial or final flat region
of the titration curve. Near the equivalence point (inflection point) these volumes will
be much smaller reducing to 0.25 to 0.5 mL and finally drops at the inflection point.
It is crucial that you obtain as many data points as possible in this region.
Mark on the titration curve the pH and volume at the equivalence point.
Questions 2 and 3 of the Report refer to this section.
Now determine the pH which corresponds to a volume equal to half that required to
reach the equivalence point and hence the pKa and compare this to the literature
value.
Hint: First, find the equivalence volume. The half-equivalence volume is exactly what
it sounds like – it is half the equivalence volume. Find that volume on your graph and
determine the pH of your reaction at that point in the titration. THAT volume is the pH
at half-equivalence.
Hint 2: A dilution factor of 65 mL/L (for example) means that to prepare the solution,
we took 65 mL of the original solution and diluted it up to a total volume of 1 litre with
water.
6.5
Report
The report should be written on the Results and Report Sheets provided. The
following points should be noted or included in your report:
• For the cloudy NH3 titration, include a properly labelled pH titration curve,
created using computer software (likely Excel) showing how you obtained the
equivalence point of the titration. See blackboard for assistance in making such
a graph. Mark on the graph the pH and volume at the equivalence point and the
pH at the point of half-neutralisation.
Use the volume of titrant required to reach the equivalence point to calculate the
concentration of the dilute cloudy ammonia and then the original concentration
of ammonia in the commercial product by using the dilution information supplied.
Estimate the pKa of the weak acid NH4+ from your titration curve and compare to
the literature value (see the Theory section).
Finally, compare your calculated concentration of NH3 with the expected

concentration of ~1.0 – 1.2 mol/L.
Additional Questions
Answer the questions at the end of the report. The table below is provided to aid in
your answer for Question 3.
Table 1 Some Common Acid-Base Indicators
Indicator pKa Colour Change
Acid Base
Methyl violet 1.0 Green Violet
Methyl orange 3.7 Red Yellow
Bromophenol blue 4.0 Yellow Blue
Bromocresol green 4.7 Yellow Blue
Methyl red 5.1 Red Yellow
Bromothymol blue 7.0 Yellow Blue
p-nitrophenol 7.1 Colourless Yellow
m-cresol purple 8.3 Yellow Violet
Thymol blue 8.9 Yellow Blue
Thymolphthalein 9.2 Colourless Blue
Phenolphthalein 9.2 Colourless Red
6.6

Results Sheet
EX6: Buffer Actions and pH titrations

A. Buffering Action
Preparation of a Buffer
pH of 0.2 M CH3COOH
pH of solution on addition of 0.2 M
CH3COONa
DpH on addition of 0.2 M CH3COONa

(i) Addition of Base
Initial pH of buffer
pH after addition of 2 mL 0.5 M NaOH
Initial pH of tap water
pH after addition of 2 mL of 0.5 M NaOH

(ii) Addition of Acid
pH after addition of 2 mL 0.5 M HCl
pH after addition of 2 mL of 0.5 M HCl
Summary of results: Change in pH on addition of acid or base

System (i) Addition of Base (ii) Addition of Acid
(± DpH) (± DpH)
Buffer
H2 O
6.7
B. Acid-Base Titration Curve
Titration of dilute NH3 with 0.1 M HCl Dilution factor of NH3: _____
Concentration of ~0.1 M HCl supplied = M
Volume pH Volume pH
added (mL) added (mL)
Equivalence Volume: _______ mL Half-Equivalence Volume: _______ mL

Equivalence pH: _______ Half-Equivalence pH*: _______
*The half-equivalence pH is the pH of your titration curve at the volume of half-
equivalence (see hint on page 6.4 for more information).
6.8
Approximate graph, to be done in the lab, as you titrate

6.9
Experiment 6
Buffers and pH Titrations
Buffer Results
Complete the table of data here
Preparation of the buffer
pH of 0.2 M CH3COOH
pH of solution on addition of 0.2 M CH3COONa
DpH on addition of 0.2 M CH3COONa
Addition of Base
pH after addition of 2 mL 0.5 M NaOH
pH after addition of 2 mL of 0.5 M NaOH
Addition of Acid
pH after addition of 2 mL 0.5 M HCl
pH after addition of 2 mL of 0.5 M HCl
System Addition of Base (± D pH) Addition of Acid (± D pH)

Buffer
Water
6.10
Buffer systems summary

Use the results for the change in pH when acids and bases are added to buffers and water to
write a general statement to summarise the observations made.
Aim (pH titration)

Method Summary
A method summary has been provided for you.
A calibrated pH meter was used throughout the experiment. A 20.0 mL aliquot of dilute
commercial ammonia solution was taken and delivered into a beaker. The solution was
bulked up with an addition of water to ensure that the pH electrode was covered at all times.
Then, a pH titration was performed, titrating with ~0.1 M HCl and taking data points at 1 mL
intervals except for regions near equivalence, where additions decreased to ~0.2 mL.
6.11
Results
Insert here – or attach a copy – of your titration curve, created digitally. Assistance for this can be
found on Canvas.
6.12
Calculation of the concentration of the dilute ammonia
Time to put your stoichiometry skills into practice again:
Concentration of HCl = M
Volume of HCl required to reach the equivalence point = mL
Chemical equation for titration:
Calculations:
Therefore, [NH3]dilute = M
Calculation of the concentration of the original ammonia solution
Remember the dilution factor. We pre-diluted the ammonia for you. For example, a factor of
58 mL/L means that we took 58 mL of the original product and diluted to 1 litre with water.
Dilution factor =
Calculations:
Therefore, [NH3]original = M
6.13
Determination of the pKa of NH4+
Details can be found on page 6.4.

The literature value for the Ka of NH4+ is 5.6 x 10-10.
pH at half the volume required to reach the equivalence point =
pKa calculated from the literature value =
Conclusion
Answer your aim and be quantitative.
Questions
Complete these 3 questions:
With the help of an appropriate equation, explain why the pH of the 0.2 M CH3COOH rose
on the addition of 0.2 M CH3COONa?
Why is the pH less than 7 at the equivalence point of the cloudy ammonia titration? Explain
using a chemical equation.
Would phenolphthalein be a suitable indicator for detecting the end-point of this titration? Use
the equation pH = pKa ± 1 to answer and the data given in Table 1 (page 6.5).
7.1
Experiment 7: Analysis of Sodium Salicylate by Spectroscopy
Introduction
This experiment relies on techniques described in the Standard Techniques section
of the Reference Manual. You will be required to correctly use a pipette, make
solutions up to accurate volumes using standard flasks and use a burette to deliver
precise volumes. If you are unfamiliar with these techniques you should consult the
Reference Manual.
From your theory, you should make sure you have a sound understanding of the
spectroscopy topic.
This experiment illustrates the theory and practical skills involved in UV/Visible
spectroscopy. The substance to be analysed is sodium salicylate.
Theory
Sodium salicylate (C6H4(OH)COO--Na+, Molecular weight = 160.1 g/mol) is a
chemical that is used medically as a pain-killer, anti-inflammatory and for reducing
body temperature. Conventionally, tablets are prepared by mixing the active
ingredient with another material (such as starch) before pressing the mixture into a
tablet that typically contains 325 mg of sodium salicylate. The amount of additive can
vary from approximately 10 to 50% of the tablet mass.
Sodium salicylate reacts with ferric iron to form a charged, soluble Fe-salicylate
molecule that is violet in colour. This species is referred to as a complex ion. As the
concentration of this species increases, so does the intensity of the colour in solution.
7.2
More importantly, the complex ion has the ability to absorb radiation of particular
wavelengths. Beer’s law can be used to relate the amount of absorbed radiation to
the concentration of the complex in solution,
A = ebc,
where:
Ø A represents absorbance, the amount of light absorbed.
Ø e represents the molar absorptivity co-efficient (a constant for a given analyte,
specifying how much radiation can be absorbed per mole of substance).
Ø b represents the path length (the amount of sample that the light passes
through, measured in metres or centimetres).
Ø c represents the concentration of the analyte in solution.
Rather than using pre-determined values of e in order to estimate the concentration

of salicylate, a more accurate determination of concentration can be obtained by
generating a standard curve, using a series of samples with a known salicylate
concentration. Once the absorbance of these samples is determined, an unknown
sample of similar composition can be directly compared to the standards.
In this experiment, we have provided a stock solution of sodium salicylate and an

unknown sodium salicylate formulation. Your task is to accurately determine the
concentration of sodium salicylate in the formulation. To do this, you will first need to
generate a standard curve using the stock solution provided.
Method
Preparation of Standards
Collect no more than 120 cm3 of standardised 150 ppm sodium salicylate in a
reagent bottle (rinse with a small amount of solution first). Rinse all standard flasks
with distilled water prior to use.
Your goal is to prepare standard solutions according to the table below:
Volume of Volume of Total volume

Solution #
Salicylate (mL) FeCl3 (mL) (mL)
0 0 5 100
1 5 5 100
2 10 5 100
3 15 5 100
4 20 5 100
5 25 5 100
Example: Preparation of standard #1:
After cleaning and rinsing your burette, use it to deliver 5 mL of the standardised
salicylate solution into a labelled 100 mL standard flask. Using the graduated
dropper on your bench, add ~5 mL of prepared 6.0 x 10-3 M FeCl3 solution and then
make up to the mark using distilled water. Mix the solution thoroughly.
Keep these solutions for your absorbance measurements.

7.3
Preparation of salicylate formulation (duplicate samples)
You will be provided with an individual solution containing an unknown concentration

of sodium salicylate. To prepare the solution for analysis, take a 20 mL aliquot and
transfer it to a clean 100 mL standard flask. Using the graduated dropper, add ~5 mL
of prepared 6.0 x 10-3 M FeCl3 solution and then make up to the mark using distilled
water. Mix the solution thoroughly by inversion. Repeat this procedure so that you
have prepared two independent unknown samples, which can be used as a means of
assessing your precision.
Analysis of standards and the unknown sample
Using the instructions provided, measure the absorbance of each of your 6 standards
at a wavelength of 530 nm, followed by your duplicate unknown samples.
Be sure that you:

Ø Start by using your blank (solution #0) to zero the instrument. This tells the
instrument what the maximum amount of transmitted radiation is, when there
is no Fe-salicylate present.
Ø Measure your solutions from lowest concentration to highest concentration
(why?).
Ø Rinse the sample cuvettes thoroughly between measurements with the new
solution about to be tested.
Ø Plot a graph of absorbance vs. concentration of your standards to make sure
that you have a linear data set.
DO NOT DISCARD YOUR SOLUTIONS YET!

Once you have collected your absorbance data, enter your results into the computer
at the back of the lab, so that you can retrieve values of m, c and R2. Show the R2
value and sketch of your standard curve to your demonstrator. Once they have
approved your results, you can discard your solutions and clean your glassware.
Calculations
Fill out the table provided in order to determine the concentration of each of your
standard solutions used to generate your standard curve.
Using the information provided in your lecture notes, calculate and plot a line of best
fit on your graph.
From the calculated line of best fit, determine the concentration of your dilute test
sample of sodium salicylate and consequently, the concentration of sodium salicylate
in the original unknown sample provided. All calculations should be completed in
units of ppm.
Hint: 1 ppm = 1 mg/L
Report
method summary, calculations and results (including a computer generated graph)
and discussion of the class results. A conclusion should also be written which
answers the aim and states the main or significant result.
7.4
Experiment 7: Analysis of Sodium Salicylate by Spectroscopy
Results Sheet
Actual concentration of standard sodium salicylate solution: _______ ppm
Preparation of Unknown (ID = ___________ ):
Volume of pipette = _______ mL
Volume of standard flask = _______ mL
Absorbance of Solutions:
Exact volume of
Solution # Absorbance
standard solution (mL)
0 0.00
1
2
3
4
5
Unknown
Unknown (repeat)
Line of Best Fit:
m (gradient) = _____________
c (y-intercept) = _____________
R2 = _____________
7.5
Experiment 7
Analysis of Sodium Salicylate by Spectroscopy
Aim
Method summary
titration.
7.6
Calculations
Complete the table below:
Volume of Concentration
Solution Volume of Volume of Total volume
150 ppm of salicylate
# FeCl3 (mL) water (mL) (mL)
Salicylate (mL) (ppm)
0 5 95 100
1 5 90 100
2 5 85 100
3 5 80 100
4 5 75 100
5 5 70 100
Show an example of how you calculated the final concentration of sodium salicylate in
solution #1 (note that you do NOT need your standard curve for this):
Average absorbance of the unknown solution = AU

7.7
Results: Graph
Insert or attach a computer generated version of your standard curve. Be sure to include an
appropriate title, labelled axes, a sensible scale and your calculated line of best fit. Assistance for
this can be found on Canvas.
From your graph:

m =
c =
2
R =
Therefore, the equation for the line of best fit is
7.8
Calculation of the concentration sodium salicylate
You’ll need your graph and values of m and c before you can begin:
Unknown ID:
Unknown Absorbance:
First measurement = Second measurement =
Using the equation for your line of best fit (y = mx + c) and the average absorbance of your
unknown, calculate the concentration (in ppm) of sodium salicylate in your dilute unknown
sample:
Calculate the concentration of sodium salicylate in your original unknown sample, in ppm:
7.9
Discussion
Include discussion of your standard curve, your R2 value and experimental reproducibility.
Conclusion
You know what to do!
8.1
Experiment 8: Analysis of Ascorbic Acid
Special Precautions
You will be using 0.1 M KOH and HNO3 solutions. These solutions should only be
pipetted using a bulb, not by mouth. If a small quantity of this reagent is spilled, it
should be immediately cleaned up using paper towel or a sponge.
Introduction
This experiment relies on techniques described in the Standard Techniques section
of the Reference Manual. You will be required to correctly use a pipette, accurately
weigh a solid material by difference and complete accurate titrations by correctly
judging the end of a titration using an indicator. If you are unfamiliar with these
techniques you should consult the Reference Manual.
In particular, make sure you have read up on how to use a top-loading balance and
an analytical balance (you should understand when to use each type of balance…
and why).
This experiment illustrates the theory and practical skills with the use of an acid-base
reaction in chemical analysis. The substance to be analysed is ascorbic acid,
commonly known as vitamin C.
This practical exercise will encourage you to practice many of the skills
required for your practical exam. Take this opportunity to perfect your
techniques and consult with your demonstrators to ensure you are making the
most of your abilities.
8.2
Theory
Ascorbic acid (C6H8O6) is better known as vitamin C, a vitamin essential for good
health. To meet our daily requirements, ascorbic acid is obtained through dietary
intake. It is not uncommon for people to take a supplement in the form of a tablet.
Conventionally, these vitamin C tablets also contain flavouring compounds and other
filler materials. The amount of additive can vary greatly from one manufacturer to
another.
Ascorbic acid is a weak mono-protic acid and will react in a 1:1 ratio with a strong
base:
C6H8O6 + OH- ® C6H7O6- + H2O
The chosen indicator for this titration, meta-cresol purple is an orange-yellow colour
in acidic solution and a light purple in basic solution.
In this experiment, we have provided a powdered formulation that contains an
unknown percentage of ascorbic acid. Your task is to accurately determine the
percentage by mass of ascorbic acid in the formulation. To do this, you will first need
to standardise an unknown KOH solution, using a dilute ~0.1 M HNO3 solution.
Note that whenever studying a commercial or unknown product, care should be

taken to ensure that the only chemical that participates in the analysis is the analyte
of choice.
Method
Standardisation of ~0.1 M KOH
Collect no more than 200 cm3 of ~0.1 M KOH in a plastic reagent bottle and not more
than 100 cm3 of the standardised ~0.1 M HNO3 in your other plastic reagent bottle.
Make sure all bottles are clean, dry and labelled before use, and stopper after
reagent collection. You should rinse each bottle with a small amount of the solution
prior to filling.
Question: Why should KOH (or NaOH) be collected in a plastic bottle and not glass?
After cleaning and rinsing your pipette and burette, deliver a 20 mL aliquot of ~0.1 M
HNO3 into a conical flask. Add a few drops of meta-cresol purple indicator to the
solution and titrate against the unknown KOH solution. The endpoint is reached
when the indicator colour changes sharply from orange-yellow to purple. The purple
colour will fade, but should remain after 10 seconds of swirling. Enter your results
immediately onto your results sheet.
Repeat the titration until 3 concordant titres are obtained (± 0.05 mL)
Record the exact concentration of the standardised HNO3 solution used. You will
need this for your calculations.
8.3
Analysis of ascorbic acid formulation
Collect a dry weighing vial and use the top loading balance to weigh in approximately
0.4 grams of the ascorbic acid formulation. Then, take your weighing vial, conical
flask and results sheet into the balance room. Accurately weigh the mass of the
weighing vial with the powder in it, to 4 decimal places. Carefully transfer the solid
into a numbered conical flask, ensuring that you don’t spill any powder. Then, re-
weigh the vial, with any residue. The difference between the 2 masses will be equal
to the mass of powder transferred to your conical flask.
Repeat this process 3 times, giving you a total of 4 numbered titration flasks, each
with an accurately known mass of formulation within.
Add ~30 to 40 mL of distilled water mixture to each of the titration flasks and then mix
them to dissolve the formulation. Be careful to make sure that any powder stuck on
the side of your flask is washed into the solution.
Titrate each of the samples with ~0.1 M KOH using the meta-cresol purple indicator.
You have reached the end-point when a purple colour is observed for 10 seconds.
Question: Do you expect the titre to be the same for each sample?
Record your titres on the result sheet provided.

After discussion with your demonstrator, enter your results from your KOH
standardisation and vitamin C formulation analysis in the spreadsheet provided on
the computer in the laboratory. This will be used to calculate an average class result.
Results will be made available for you via Blackboard, for discussion in your report.
The class average result should be quoted in your report.
Calculations
For the standardisation of KOH, use your titration results (the average of your
concordant titres against the HNO3) to calculate the concentration (in units of
molarity) of the ~0.1 M KOH solution. Combine this knowledge with the masses and
titres of your vitamin C analysis to determine the mass of ascorbic acid present in
each of your 4 samples. Using the best 3 results, calculate the percentage by mass
of ascorbic acid present in the formulation (grams of acid per 100 grams of
formulation).
Report
method summary and discussion of the class results. A conclusion should also be
written which answers the aim and states the main or significant result.
8.6
Experiment 8
Analysis of Ascorbic Acid Formulation
Aim
You should be good at these by now!
Method summary
titration.
Chemical equations:
Standardisation reaction: HNO3 (aq) + KOH (aq) "
Ascorbic acid reaction: C6H8O6 (aq) + OH- (aq) "

8.7
Results
Complete the tables below:
KOH standardisation
[HNO3] = M
Volume of HNO3 per titration = mL
Titre 1 (mL) Titre 2 (mL) Titre 3(mL) Titre 4 (mL)
Average of the best 3 titres = ± mL
Ascorbic acid analysis

Flask 1 Flask 2 Flask 3 Flask 4
Mass (g)
Titre (mL)
Calculation of the true [KOH]
Use your stoichiometry to find the exact concentration of the KOH solution provided:
Concentration of HNO3 used in standardisation = M

Volume of HNO3 used in standardisation = mL
Volume of KOH titre in standardisation = mL
Calculations:
8.8
Calculation of the %ascorbic acid in the formulation
Show each calculation step for your first analysis only (flask 1). Then complete the results summary
table, showing answers for all 4 flasks.
Example calculation, Flask 1
Calculate the number of moles of KOH required to titrate the powder sample:
Number of moles of ascorbic acid titrated by the KOH:
Mass of ascorbic acid present in powder sample:
Percentage ascorbic acid in the powder formulation:
Calculation Summary Table

Analysis 1 Analysis 2 Analysis 3 Analysis 4
Moles of KOH required to react
with powder (mol)
Mass of ascorbic acid in the

powder (g)
Percentage ascorbic acid
Tick box to show your 3 most

concordant results
Average of the best 3 results = ± %

8.9
Class Results
Complete the table below:
Average Standard Deviation

[KOH] (M)
% ascorbic acid
Discussion
Include discussion of the standardisation and ascorbic analysis, making use of individual
results (both accuracy and precision) and class results.
8.10
Questions
Complete these 3 questions, to help better understand this experiment and to better prepare you
for your laboratory exam.
What major assumption are you making about the reaction taking place in this experiment
between the formulation and the base? (see p8.2 for assistance)
Can the top-loading balance be used to determine accurate masses? What is the purpose of
using the top-loading balance?
Do you expect the titre to be the same for each of your 4 ascorbic acid analyses? Explain.
Conclusion
Finish it off!

Prac Manual CHE10001-CHE10004 PDF

Uploaded by

Copyright:

Available Formats

Prac Manual CHE10001-CHE10004 PDF

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Prac Manual CHE10001-CHE10004 PDF

Uploaded by

Copyright:

Available Formats

What is the purpose of conducting multiple analyses of the ascorbic acid formulation?

What is the purpose of conducting multiple analyses of the ascorbic acid formulation?

What assumptions are made about the reaction between the formulation and base?

What assumptions are made about the reaction between the formulation and base?

CHE10004 Introduction to Chemistry

Compiled by Marylou Molphy and Daniel Eldridge

Faculty of Science, Engineering & Technology

Experiment Title Section

Lab Timetable Blackboard

1 Apparatus and Techniques in Chemistry 1.1

2 Investigating Chemical Reactions 2.1

3 Titration of Lemon Juice 3.1

4 What solution is that? 4.1

5 Identification of an unknown solid diprotic acid 5.1

6 Buffers & pH titrations 6.1

7 Spectroscopic analysis of sodium salicylate 7.1

8 Analysis of Ascorbic Acid 8.1

The experiments detailed in this manual require adequate knowledge of

YOU WILL NOT BE ABLE START EXPERIMENTS UNTIL THIS IS DONE.

Calculating averages and deviations

You will frequently be asked to calculate an average result and a

1) Calculate the average of your best 3 results

2) Compare your average value to the 3 results that you used in

Eg. If 4 results are obtained to be 19.14,19.22, 19.23 and 19.25 mL:

1) Omit 19.14 – only use your best 3 to calculate the average:

2) Furthest value away is 19.25 mL

3) 19.25 – 19.233 = 0.0167 = 0.02 mL (just use one digit)

Result = 19.23 ± 0.02 mL

Unit conversions to be aware of…

Practical Write-Up Hints and Tips

DON’T use the first person (I, my, our, we).

DON’T use “flowery” language.

See next page for notes on writing discussions and conclusions

Experiment 1: Apparatus and Techniques in Chemistry

The Analytical Balance

The Bulb pipette

The Graduated Pipette

The Measuring Cylinder

PRACTICAL SESSION (Day/time): NAME:

Experiment 1: Apparatus and Techniques in Chemistry

Use of Volumetric Glassware

Apparatus Bulb Pipette Graduated Pipette

Temp of water (°C)

Apparatus Burette Measuring Cylinder

Temp of water (°C)

Bulb pipette Bulb pipette Graduated Graduated

Pipette: 20.00 ± 0.06 mL Graduated Pipette 20.0 ± 0.2 mL

Experiment 2. Investigating Chemical Reactions

Where instructed, dispose of chemicals to appropriate waste containers.

Colours of Ions in Aqueous Solutions

Thermal Decomposition Reactions

Metal chlorides - stable (but often volatile)

OBSERVATION(S) & RELEVANT

Glowing string Test for O2 String glows brighter and rekindles

Which ions are responsible for the colour in each solution?

Complete each of the tables, including observations and reactions.

Colour of solids and their solutions

CuSO4.5H2O Blue Blue Cu2+(aq)

Make use of your solubility table