Catholic Junior College H2 Chemistry 9729 2018 Practical Handbook - Part 1

CATHOLIC JUNIOR COLLEGE
H2 CHEMISTRY 9729
2018 PRACTICAL HANDBOOK – Part 1

Content
Page
1 List of JC1 Chemistry Experiments and Experimental Techniques 2
2 Laboratory Safety Rules 4
3 Chemistry Practical Assessment 8
4 Volumetric Analysis
4.1 Introduction 9
4.2 Experimental Techniques 12
4.2.1 Common Laboratory Apparatus & Equipment Used
4.2.2 Manipulation of Apparatus
4.2.3 Preparing a Standard Solution from a Solid Solute
4.2.4 Carrying Out a Titration
4.3 Presentation Skills 23
4.3.1 Experimental Errors
4.3.2 Uncertainty in Measurements
4.3.3 Examples of Data Recording and Data Presentation
4.4 Calculations & Analysis 27
4.4.1 Calculations Involved in Volumetric Analysis
4.4.2 Calculations in Uncertainty
4.4.3 Calculations in Experimental Error
4.5 Generic Checklist 32
Page 1
1 List of Chemistry Experiments and Experimental Techniques
Experiment Experimental techniques (syllabus

Description
no. requirement)
Acid-base titration 1 Titration e.g. acid-base titration (with
1  Back titration suitable indicators such as methyl
 Planning orange, screened methyl orange,
Acid-base titration 2 thymolphthalein and thymol blue), redox
 Preparation of standard titration, iodimetric titration, indirect
solution by dilution titration, including preparation of standard
2
 Use of double indicators solutions. Other types of titrations may
also be required, where appropriate,
 Planning
sufficient working details will be given.
Redox titration
 Preparation of standard
3
solution from solid
 Planning
Gas collection Gas collection
4  using an inverted burette
 Planning
Gravimetry Gravimetric analysis, e.g. volatilisation
 Driving off water of gravimetry
5
crystallisation
 Planning
Chemical Energetics Thermochemistry, including thermometric
6
 Planning titration
Thermometric titration
7
 Planning
Sulfur clock Chemical Kinetics, e.g. continuous and
8  Initial rate method initial rate method
 Planning
Iodine clock
9  Initial rate method
 Planning
Iodometric titration (serves as a
10 recap for redox titration)
 Planning
Iodination of propanone
11  Continuous method
 Planning
Organic Chemistry Qualitative organic analysis requiring a
12 (a series of short practicals) knowledge of simple organic reactions,
 Distinguishing tests e.g. test-tube reactions indicating
presence of unsaturation (C=C),
alcoholic, phenolic, carbonyl, carboxyl
Organic QA and amino groups, may be set, but this
13 would be for the testing of observation
 planning
skills and drawing general conclusions
only.
Page 2
Qualitative inorganic analysis involving an
Inorganic QA element, a compound or a mixture.
Systematic analysis will not be required.
14  Test on ….
Candidates should be familiar with the
 Planning
reactions of cations, reactions of anions
and test for gases as detailed in
Qualitative Analysis (QA) Notes.
Inorganic QA Reactions involving ions not included in
15  Test on …. the QA Notes may be tested: in such
 Planning cases, candidates will not be expected to
identify the ions but only to draw
conclusions of a general nature.
Inorganic QA Candidates should not attempt tests,
16  Test on …. other than those specified, on
 Planning substances, except when it is appropriate
to test for a gas.
Ethanedioic acid + KMnO4
titration
17
 redox titration
(autocatalysis)
Revision practicals (TBC)
Not addressed:
Simple organic synthesis and purification, including use of water bath, setting up and use of
reflux and distillation apparatus
Page 3
Practical Handbook (Part 1):
Volumetric Analysis (VA) 2018 Semester 1
2 Laboratory Safety Rules

GENERAL SAFETY
1 No student shall enter any laboratory except during the practical periods allocated to his
class or when instructed to do so for specific duties by the science teacher. Laboratory
store-rooms and preparation rooms are out of bounds to all students.
2 No food is to be brought into the laboratories. Eating and drinking are prohibited in
laboratories.
3 No indiscipline or foolery is allowed in the laboratories.
4 Students should seek clarification from the teacher if instructions for an experiment are
not thoroughly understood. Students should not proceed with an experiment if in doubt.
5 Students are expected to follow all instructions from the laboratory technicians without
question while working in the laboratories.
6 Unauthorised experiments are prohibited.
7 Long hair should be tied up neatly to avoid any interference with laboratory work.
8 Safety goggles must be worn whenever there is any risk of injury to the eyes, e.g., when
heating.
9 Protective gloves and clothing must be worn when handling hazardous materials.
10 Hands must always be thoroughly washed before leaving the laboratory, regardless of
whether gloves are worn.
11 Equipment used to handle or transfer hazardous materials must be inspected for leaks,
cracks and other forms of damage before use.
12 Damaged equipment, breakages, accidents and spillage should be reported

immediately to the teacher.
13 Unlabelled chemicals should not be used. Unlabelled containers should be reported to

the teacher.
14 Chemicals or other materials must never be tasted unless specifically directed by the
teacher.
15 Students should not take apparatus or chemicals out of the laboratory without the
permission of the teacher.
16 Pipetting should always be carried out using a pipette aid and never by mouth.
17 Sharp objects (such as needles, razors or pins) should not be discarded in waste-bins
or trash bags. A sturdy container should be used for disposal of sharp objects.
18 Chemical and biological wastes must be disposed appropriately.
Page 4
19 No solids are to be thrown into the sinks. Taps must be allowed to run for a few minutes
after chemicals (especially acids and alkalis) are discharged into the sinks.
20 Areas around electrical equipment should be kept dry and where appropriate, kept away
from water. Students should make sure that their hands are dry and appropriate
footwear is worn before using electrical appliances.
21 Laboratory work benches, sinks and apparatus must be cleaned by students before
leaving.
ACCIDENTS AND SAFETY MEASURES
22 All orders issued by the teacher-in-charge must be obeyed and carried out immediately
and without question.
23 All accidents must be reported immediately to the teacher-in-charge for treatment or

action.
24 All students must note the positions of

 the fire extinguishers,
 the first aid box,
 the main switch for gas,
 all exits in the laboratory.
USE OF APPARATUS
25 No chemicals or apparatus may be removed from the laboratories without written

permission of the teacher-in-charge.
26 All apparatus must be cleaned and returned to its proper place in the laboratories
immediately after use.
27 No students shall use any apparatus other than that authorised by the teacher-in-charge.
BREAKAGE OF APPARATUS (DAMAGE, DEFACING OF APPARATUS)
28 All apparatus is on loan to the students for their use.
29 All breakages must be reported to the laboratory technicians/assistants and particulars

concerning the breakages noted down in the breakages book.
30 Where students share one set of apparatus, such students shall be jointly responsible
for the good care of the apparatus. Damage reported by the students may render the
one previously using the same equipment liable for such damages.
Bench reagents for practical work
The list below is to guide schools in the use of GHS pictograms for standard reagents that are
generally made available in the laboratory for practical work.
GHS (Globally Harmonised System of Classification and Labelling of chemicals) pictograms

for practical work provided by CPDD A-Level Science Unit. You need to be aware of the hazard
of dealing with all standard reagents in the laboratory. Note the nature of aqueous ammonia
and hexane, among others!
Page 5
GHS Pictogram Product identifier Concentration
aqueous sodium approximately

hydroxide 2.0 mol dm−3
approximately
aqueous ammonia
2.0 mol dm−3
approximately
hydrochloric acid
2.0 mol dm−3
approximately
nitric acid
2.0 mol dm−3
approximately
sulfuric acid
1.0 mol dm−3
aqueous silver approximately

nitrate 0.05 mol dm−3
No pictogram is required for this reagent aqueous barium approximately

prepared in this concentration nitrate 0.2 mol dm−3
saturated
aqueous
limewater calcium
hydroxide,
Ca(OH)2
No pictogram is required for this reagent aqueous potassium approximately
prepared in this concentration manganate(VII) 0.02 mol dm−3
No pictogram is required for this reagent aqueous potassium approximately
prepared in this concentration iodide 0.1 mol dm−3
hexane -
CPDD A-Level Science Unit Nov 2016
Page 6
There are nine pictograms, each with a specific meaning. The following table shows these
pictograms and the types of hazards they represent.
GHS hazard pictograms
Severe
Health
health Acute toxicity
hazards
hazards
Explosive Flammable Oxidising
Gases
Environmental
Corrosive under
hazard
pressure
Page 7
3 Chemistry Practical Assessment

Paper 4 (2 h 30 min, 55 marks, 20% weighting)
Assessment Objectives (Experimental skills and investigations)

 To follow a detailed set or sequence of instructions and use techniques, apparatus and
materials safely and effectively.
 To make, record and present observations, measurements with due regard for
precision and accuracy.
 To interpret and evaluate observations and experimental data.
 To identify a problem, devise and plan investigations, select techniques, apparatus and
materials.
 To evaluate methods and suggest possible improvements.
Candidates will be assessed in the following skill areas:

Skill Weighting
P Planning 5%
MMO Manipulation, Measurement and Observation
PDO Presentation of Data and Observation 15%
ACE Analysis, Conclusion and Evaluation
In the course of the 2 years practical, you will be able to use appropriate apparatus/equipment
to record a range of measurements such as mass, time, volume and temperature. In addition,
you will be exposed to a range of experimental techniques in the following areas:
1. Volumetric Analysis (Titrations e.g. acid-base, redox, iodimetric/iodometric, indirect,

including the preparation of standard solutions). Acid-base titration involves the use of
suitable indicators such as methyl orange, screened methyl orange, thymolphthalein and
thymol blue. However, other type of titrations may also be required, where appropriate;
in such cases, sufficient working details will be provided.
2. Gravimetric Analysis, e.g. volatilization gravimetry (e.g. determination of water of

crystallization in a sample of a hydrated salt where direct heating and weighing are
required)
3. Gas Collection (by collection of gas over water/solution or gas syringe method)
4. Thermochemistry, including thermometric titration
5. Chemical Kinetics, e.g. continuous and initial rate methods
6. Qualitative Analysis (QA) - Inorganic (identification of cations and anions)
7. Qualitative Analysis (QA) – Organic (simple test-tube reactions indicating the

presence of various functional groups such as unsaturation (C=C), alcoholic, phenolic,
carbonyl, carboxyl and amino may be set)
8. Simple organic synthesis and purification, including use of water bath, setting up and
use of reflux and distillation apparatus.
You are not allowed to refer to notebooks, textbooks or any other information in the
practical examination. QA Notes will be included in the question paper for your use in the
examination.
Page 8
4 Volumetric Analysis
4.1 INTRODUCTION
VOLUMETRIC ANALYSIS is a qualitative technique used to determine the concentration of a

solution. It involves a method called titration to determine the stoichiometric amount of
reactants in the two solutions that have reacted.
Basic Principle of Titration:

Titration involves gradual addition of one solution (titrant) from a burette to another solution in
a conical flask, with or without the use of a visual indicator.
The instance when an excess drop of solution from the burette causes a colour change to the
solution in the conical flask is known as the end-point. This point is experimentally
determined. When stoichiometric amount of the reactants in the two solutions have reacted,
this point is known as the equivalence point. This point is deduced from their
stoichiometric ratio in the balanced equation.
When measures are taken to ensure reliability of titration results, the end-point determined
from the experiment will be close to the equivalence point.
Types of Titration:
(a) acid-base
(b) redox
Limitations of Titration:
 In a titration, the reaction between the two solutions must be instantaneous.
 There must be also a sharp / distinct colour change of either
o a visual indicator (acid-base titration), or
o a transition metal-containing compound (redox titration).
(a) ACID-BASE TITRATION:
An acid-base titration is the quantitative analysis of the concentration of an acid (or base)
by exactly neutralising the acid (or base) with a base (or acid) of known concentration.
In addition, acid-base titrations are also used for the following purposes:
 To determine chemical formula of an unknown compound
 To determine % by mass of an acidic/basic substance in a mixture.
 To determine % purity of an acidic/basic substance in a mixture.
Examples of acids and bases commonly used in the laboratory:

ACIDS BASES
Strong acids Strong bases
 hydrochloric acid (HCl)  sodium hydroxide (NaOH)
 nitric acid (HNO3)  potassium hydroxide (KOH)
 sulfuric acid (H2SO4)
Weak acids Weak bases

▫ ethanoic acid (CH3CO2H) ▫ aqueous ammonia (NH3(aq))
Page 9
Common indicators used in acid-base titrations:

pH
1 2 3 4 5 6 7 8 9 10 11
Indicator
Thymol Blue Red Orange Yellow Green Blue
Methyl Orange Red Orange Yellow
Screened
Red Grey Green
Methyl Orange
Bromocresol Yellow Green Blue
Green
Bromothymol Yellow Green Blue
Blue
Phenolphthalein Colourless Pink Red
Thymolphthalein Colourless Light blue Blue
Choice of indicators for different types of acid-base titrations:

Acid / Base Suitable indicator
strong acid – strong base All above are suitable
strong acid – weak base methyl orange, screened methyl orange or thymol blue
weak acid – strong base thymol blue, thymolphthalein or phenolphthalein
weak acid – weak base no suitable indicator
(b) REDOX TITRATIONS
A redox titration involves the stoichiometric reaction based on a redox reaction between the
two solutions involved. Similar to acid-base titration, titration is complete when end-point is
reached (as indicated by a distinct colour change).
Two main types of redox titrations:

(i) involving potassium manganate(VII), KMnO4 with reducing agents.
(ii) involving sodium thiosulfate and iodine (also known as iodometric titrations)
(i) Redox titrations involving ACIDIFIED POTASSIUM MANGANATE(VII), KMnO4
 KMnO4 is a powerful oxidising agent. It reacts with a wide range of reducing agents,
especially compounds of iron, and ethanedioic acid, H2C2O4, and its salts.
 KMnO4 acts as its own indicator. Hence redox titrations involving KMnO4 do not require
any indicator.
 End-point of titration is a permanent pink colour.
 Acidic medium for MnO4− titration is achieved by adding excess dilute sulfuric acid.
o HCl cannot be used because it reacts with MnO4− to give chlorine;
o HNO3 cannot be used because it is also an oxidising agent and might interfere with
the oxidising action of MnO4−.
Page 10
4.2 EXPERIMENTAL TECHNIQUES
4.2.1 Common Laboratory Apparatus & Equipment Used
Apparatus Capacity Purpose

Dropper / To transfer small
Teat pipette volume of solution
Conical flask 250 cm3 To hold solution for

reaction.
Beaker 50 cm3, 100 cm3, To hold liquid

250 cm3, 500 cm3 samples.
To contain reaction
mixture.
Measuring 10 cm3, 25 cm3, 50 For measuring

cylinder cm3, 100 cm3 volume of solution
where accuracy
is not critical.
Volumetric / 250 cm3 To prepare

Standard / standard solution
Graduated flask (i.e. solution of
known
concentration).
To prepare diluted
solution.
Filter funnel To direct solution

into another
apparatus with
small opening.
To hold filter paper

for filtration.
Pipette filler To draw up

(siphon) solution
into pipette.
Page 11
Pipette 10.0 cm3, 25.0 cm3 To measure a fixed

and precise
volume of liquid.
Burette 50.00 cm3 To measure a

precise volume of
liquid.
Retort stand with To hold burette or

clamp pipette upright.
White tile To see colour

change at end-
point more clearly.
Glass rod To stir and allow

for even mixing of
reactants.
To dissolve solid
substance into
solvent.
Wash bottle Contain deionised
water for rinsing of
apparatus.
Weighing balance To measure the

mass of
substance.
Weighing bottle To hold the

substance to be
weighed.
Page 12
4.2.2 Manipulation of Apparatus
(A) Use of pipette filler
“A” valve to release air

from pipette filler A
“S” valve to siphon solution

into pipette
E S
“E” valve to empty pipette
of solution
Insert pipette here Fig. 4.1
Procedure Details
Step 1 Hold the upper end of the pipette to insert the pipette filler to prevent breakage. Press
valve “A” (Air) and simultaneously squeeze the bulb to produce a vacuum.
Step 2 Draw the solution into the pipette by using the pipette filler by pressing valve “S” (Siphon)
until the solution level is above the calibration mark (of the pipette).
Ensure no air bubble is drawn up together with the solution.
If the bulb becomes inflated or the speed of drawing up the solution becomes too slow,
press valve “A” again to deflate the bulb.
Step 3 Lift the pipette tip above the surface of solution and adjust the solution level by
pressing valve “E” (Eject) of the pipette filler until the bottom of the meniscus touches
the calibration mark of the pipette.
Then drain the solution into a conical flask by pressing valve “E”. Alternatively, remove
the pipette filler to drain the solution.
What is the rationale for lifting the pipette tip above the surface of solution when
adjusting solution level to the mark?
Adjusting the solution level to the mark while the pipette tip is still immersed in solution will cause
the actual volume of solution pipetted to be less than expected.
This is because the solution pressure will cause the solution level to appear higher that what it
should be.
Page 13
(B) Use of pipette
W ash pipette with tap water and rinse with deionised water before use. Dry the exterior of the
pipette with paper towel. This is to avoid introducing water that will cause dilution of the solution.
1 2
Fig. 4.2
Procedure Details & Remarks

Step 1 Before pipette is used to draw solution for titration, rinse it with the solution to be
pipetted.
Use the pipette filler to draw up the solution above the calibration mark.
Lift tip of pipette above solution surface. Press the “E” valve on the pipette to adjust the
volume of solution until the bottom of meniscus is aligned to the calibration mark on the
pipette.
 For clear solutions, read from the bottom of meniscus.
 For dark-coloured solutions e.g. KMnO4, read from the top of meniscus instead.
Use a paper towel to wipe dry the exterior of the pipette.
Step 2 Remove the pipette filler and allow solution to drain into the clean conical flask.
DO NOT RINSE conical flask with the solution it is supposed to hold.
Step 3 Tilt the conical flask to one side. Then gently tap and rotate the pipette tip against the
bottom of the conical flask.
DO NOT BLOW OUT the last drop of solution from pipette as it has already been
calibrated for.
What is the impact on the titre volume if the exterior of the pipette is not wiped dry
before it is used to measure the volume of solution?
This will cause the titre volume to be lower than the actual value as the solution would
be diluted by the traces of water present on the exterior of the pipette.
Page 14
What is the impact on the titre volume if the pipette is not rinsed with the solution
to be pipetted?
This will cause the titre volume to be lower than the actual value as the solution would be
diluted by the traces of residual water in the pipette.
What is the impact on the titre volume if the conical flask is rinsed with the solution
it is supposed to hold?
This will cause the titre volume to be higher than the actual value as the amount of
unknown sample (analyte) in the conical flask is now higher than the amount that should
be originally present in 25.0 cm3 of the solution.
(C) Use of burette
W ash burette with tap water and rinse with deionised water before use.
Step 1 Before burette is used for titration, rinse it with the titrant solution to be measured.
 Half-fill burette with titrant solution.
 Open burette tap and run some solution through the burette tip.
 Hold the burette horizontally and rotate it to ensure even rinsing of the burette
walls.
 Lastly drain off the remaining solution through the mouth of burette.
Clamp the rinsed burette vertically upright onto the retort stand.
Step 2 Using a filter funnel, fill the burette with the titrant solution at eye level.
DO NOT transfer solution above eye level to prevent spillage. Bring down retort stand
with burette onto a stool (if necessary).
Flush out any air bubbles trapped in the burette tip. (See Fig. 4.3a)
Step 3 Top up the burette slightly above the ‘0’ cm3 mark.
 For clear solutions, read from the bottom of meniscus.
 For dark-coloured solutions e.g. KMnO4, read from the top of meniscus instead
Remove the filter funnel and adjust the solution level to ‘0’ mark before carrying out
titration.
Page 15
Burette
Correct volume
reading of 20.70 cm3
Air bubble at eye level
Fig. 4.3a
Fig. 4.3b
What is the impact on the titre volume if the burette is not rinsed with the titrant
solution?
This will cause the titre volume to be higher than the actual value as the titrant solution
placed in the burette would be diluted by the residual water present.
What is the impact on the titre volume if the filter funnel is not removed before
titration?
This will cause the titre volume to be lower than the actual value as residual liquid clinging
to the side of the funnel will flow into the burette.
What is the impact on the titre volume if the air bubbles are not removed before
titration?
This will cause the titre volume to be higher than the actual value if the bubble is present
when initial burette reading is taken but no longer present when final burette reading is
taken.
Page 16
(D) Use of weighing balance to measure solid mass

Procedure Details
Step 1 Use a dry and clean weighing bottle (or any other suitable container as instructed)
Ensure a draught-free environment by switching off fans nearest to the weighing balance.
Step 2 Press the TARE button to zero the electronic balance.
Step 3 Place the dry weighing bottle in the middle of the balance pan.
Record the mass reading of the empty weighing bottle.
Step 4 Add the solid into the weighing bottle outside of the balance to prevent spillage onto
the balance pan.
Add solid to ± 0.05g of the required mass (or as instructed).
Step 5 Reweigh the bottle and solid content.
The reading shown is the total mass of weighing bottle and mass of solid.
Step 6 Transfer the solid into a small beaker or other container as instructed.
*Step 7 Reweigh the empty bottle with residual solid.
Record the actual mass of solid used.
(mass of bottle with solid – mass of bottle with residual solid)
Note: Step 7 might not be necessary for some experiments e.g. in making up a standard solution from
solid solute.
What is the impact if the weighing bottle used is not dry and clean?
Presence of water droplets or impurity in the weighing bottle will contribute to additional
mass. This will affect the accuracy of the mass measured.
Page 17
4.2.3 Preparing a Standard Solution from a Solid Solute

Step 1 Weigh accurately a known mass of solute in a clean, dry weighing bottle and record the
weighings.(See Fig 4.4a)
Step 2 Dissolve the solute in a small volume of suitable solvent (usually water or dilute acid,
depending on nature of solute used) in a small beaker (usually 100 cm3 capacity).
Step 3 Transfer this small volume of solution into a standard flask with the aid of a glass rod
and filter funnel. (See Fig 4.4a) Use the glass rod to guide the solution into the standard
flask.
Step 4 Rinse the small beaker with deionised water and transfer the washing into the standard
flask. Repeat for 1 to 2 times to ensure 100% of the solute is transferred into the
standard flask.
Step 5 Fill the standard flask carefully up to the calibration mark (at eye level) with the
appropriate solvent. (See Fig 4.4b), using a teat pipette when approaching the mark.
BE CAREFUL to ensure solution level DOES NOT exceed the calibration mark on
the standard flask. (See Fig 4.4b)
If the solution level exceed the calibration mark, you will need to repeat the preparation
of the standard solution again.
Step 6 Stopper the standard flask.
Then invert the flask before shaking it well. Repeat this step for 3 to 4 times to ensure a
homogenous solution is obtained.
Leave the homogenous solution to stand for a while (till all air bubbles in the solution
have settled) before using the solution for the next phase of your experiment.
What is the rationale of using the dropper to make up the standard solution when
nearing the calibration mark?
This is to prevent addition of excess water, thus causing the standard solution to be diluted.
It is not possible to remove the excess water from the standard flask once it is added.
How do we determine the mass of solid to use to make up the standard solution?
Generally, it is assumed that the titre value is 25.00cm3. By calculating backwards, we can
determine the appropriate concentration of the standard solution, and in turn, the
corresponding mass of solid to use.
Page 18
Glass rod
Step 1 Step 2 Step 3

Deionised water
Deionised water
Step 6 Step 5 Step 4
Fig. 4.4a
250 cm3 mark
Take
note!
Fig 4.4b:
Solution is filled up to the mark indicated on the flask.
This is how the volume of solvent is accurately

measured.
Page 19
4.2.4 Carrying Out a Titration
The standard solution is usually placed

in the burette.
A standard solution is a solution whose

concentration is known accurately.
It is usually prepared by dissolving an

accurately weighed mass of a solute in
an accurately measured volume of
water.
Fig. 4.5
Procedure Details
Fill the 50.00 cm3 burette with standard solution. (usually up to 0.00 cm3 mark)
Step 1 Filling should be done below eye level to avoid spillage. Remove the filter funnel before
recording the initial burette reading.
Use a pipette filler to pipette a portion (usually 25.0 cm3) of the solution of unknown
Step 2
concentration into a conical flask.
Step 3 Add 2 to 3 drops of a suitable indicator (if required) into the conical flask.
Place a white tile beneath the conical flask so that the colour change of the solution can
Step 4
be observed more easily.
Adjust the burette (on the bench top) to a suitable height for titration.
Step 5 Ensure the burette tip is slightly inside the conical flask but not touching the sides of
the flask.
If you are a right-hander, hold the burette tap with the thumb and the forefinger of the left
Step 6
hand. Use the right hand to hold the neck of the conical flask. (See Fig 4.5)
Carry out the titration. Control the addition of titrant with the left hand while using the right
hand to swirl the solution in the conical flask continuously.
Step 7
Rinse the inner walls of the conical flask with deionised water to wash down any
adhering titrant (if necessary).
When the colour of the indicator takes longer to fade (depending on type of titration), the
end-point should be approaching.
Step 8 The titrant (from burette) should be added drop-wise towards the end point until the end-
point is reached (indicator changes colour). This is to prevent the addition of excess
titrant.
When 1 excess drop of titrant causes a distinct colour change, the end-point is reached.
Step 9
Record the final burette reading at eye-level.
Step 10 Repeat the titration to obtain consistent titre values (within ±0.10 cm3 of each other.)
The end-point indicates that stoichiometric amounts of the two reactants have reacted. (i.e.: both
reagents have completely reacted with each other)
From the titration results, calculations can be done to find the unknown concentration of solution and /
or any other unknown quantity.
Page 20
What is the rationale of using deionised water for rinsing during titration? Will the
additional water added affect the accuracy of titration results?
Rinsing the inner walls of the conical flask with deionised water washes down any traces
of adhering titrant.
This ensures all titrant added into the conical flask will react with the analyte in the flask.
The deionised water added will not reduce the amount of analyte present originally in
the flask. It will not reduce the amount of titrant added too.
The titrations seen so far have been fairly straightforward: two reagents added together in the
presence of an indicator to show the end-point. However, due to various reasons (e.g.: no
suitable indicator, precipitation upon reaction etc.) such a straightforward/direct titration may
not always be feasible. Hence, back titration will be used to determine the concentration of the
unknown.
BACK TITRATION
 A back titration is a titration method where the concentration of an analyte is determined

by reacting with a known amount of excess reagent.
 The remaining excess reagent is then titrated with another second reagent.
 The titre value will show how much of the excess reagent was not reacted with the analyte
and the concentration of the analyte can then be determined.
Back titration is often used when the end point is difficult to determine in a direct titration.
Some situations include:

o analyte is an insoluble solid which reacts slowly with the titrant (e.g. CaCO3 with HCl).
o analyte contains impurities which interferes with titrant.
o analyte reacts vigorously with titrant or produces effervescence which causes loss of
reagents due to acid spray. (e.g. Na and HCl).
o analyte and titrant are both weak acids / bases (e.g. NH3 and CH3COOH).
Example of back titration involving sodium thiosulfate(VI) Na2S2O3.5H2O, and iodine:
 Titrations involving sodium thiosulfate and iodine are known as iodometric titrations and
they work in the following way:
Page 21
Step 1:
Excess potassium iodide is added to an oxidising agent (O.A.) of unknown concentration.
The oxidising agent then oxidises the iodide ions from the potassium iodide solution to give
iodine, which gives a brown coloured solution.
The amount of iodine liberated is dependent on the amount of O.A. originally present. (The
relationship is shown in the stoichiometric equation).
Step 2:
The iodine formed is then titrated against sodium thiosulfate(VI) of a known concentration,
which is placed in the burette.
 Starch solution serves as indicator for such reaction and is only added near the end-
point when most of the I2 have reacted away.
 End-point: colour changes from blue-black to colourless.
From the volumes of titration (volumes of sodium thiosulfate(VI) used), the concentration of
the O.A. can be determined.
Based on the titration results (volume of sodium thiosulfate(VI) used), the amount of O.A. used
can be calculated.
What is the rationale for only adding the starch indicator when nearing end-point
i.e. when the brown iodine solution turns pale yellow?
Starch solution is not added at the beginning of the titration unlike other titrations.
This is because the adding starch solution at the beginning may cause lots of iodine molecules
to be ‘trapped’ as the starch-iodine complex. The release of iodine molecules from the starch
molecules takes time and as such, it might decrease the accuracy of the titration (as titre
volume will be higher than expected).
Page 22
4.3 PRESENTATION SKILLS
4.3.1 Experimental Errors
Experimental error is the difference between a measurement and the true value or between
two measured values. Experimental error, itself, is measured by its accuracy and precision.
Accuracy and Precision

Accuracy measures how close a measured value is to the true value or accepted value.
Precision measures how closely two or more measurements agree with other. Precision is
sometimes referred to as “repeatability” or “reproducibility”. A measurement which is highly
reproducible tends to give values which are very close to each other
The diagram below shows examples of accuracy and precision.
High precision High precision

High accuracy Low accuracy
Low precision Low precision

High accuracy Low accuracy
Types of Experimental Errors

Experiments in the laboratories come with a certain degree of uncertainty or error which can
be minimized. There are two basic types of error that affect results; these are ‘random errors’
and ‘systematic errors’.
There is a ‘range of uncertainty’, often termed ‘error’ associated with each piece of
measuring apparatus/equipment used; the greater the precision of a piece of
apparatus/equipment, the smaller is its ‘range of uncertainty’/‘error’. This uncertainty will
always be present no matter how skilled the operator might be, and will generate random
errors. Refer to section 4.3.2 for the precision of common apparatus used in VA.
Random errors are apparatus errors, which cause results to fluctuate around a mean value,
and data is made more reliable by averaging repeated readings. Upon averaging many
repeated readings, random errors will only affect precision of a measurement. Poor
experimental technique or poor calibration of a piece of apparatus/equipment can also
generate random errors.
Page 23
Systematic errors affect all measurements in the same way, producing either lower or higher
results than the true value, not both. These cannot be averaged out. Sometimes they are due
to the particular experimental procedure that has been adopted. For example, when one
person performs a rate experiment it may take time to mix the reagents and start the stop
clock.
Systematic errors affect accuracy of the final results. This error can be minimised, or even
eliminated, by using two people, one to do the timing and one to mix the reagents. Another
source of systematic error may be the measuring device itself. This can be checked by seeing
if two different instruments give the same values. For example, in heat experiment, there will
be unavoidable heat losses when trying to assess enthalpy change and this causes a
systematic error.
Calculating Experimental Errors

When reporting the results of an experiment, accuracy and precision of the experimental
measurements must be described. These can be described in terms of significant figures and
uncertainty. Refer to section 4.4.2 on Percentage Uncertainty.
Page 24
4.3.2 Uncertainty in Measurements
For fixed volume measuring apparatus, e.g. volumetric flask and pipette, the absolute
uncertainty is usually indicated on the apparatus itself.
For apparatus used to measure variable volumes, e.g. measuring cylinders and burette, the
absolute uncertainty is taken to be half of the smallest graduation of the apparatus.
Precision of common apparatus/equipment

Apparatus Smallest Uncertainty / Example of No. of Remarks
division Instrumental recording decimal
Error places
to
record
Pipette Depends on 10.0 cm3 1
the grades of 25.0 cm3
the
apparatus
Volumetric /  0.15 cm3 100 cm3, 0
Standard / 250 cm3
Graduated
flask
(250 cm3)
Measuring 1 cm3  0.5 cm3 26.0 cm3/ 1
cylinder 26.5 cm3
(50 cm3)
Measuring 0.2 cm3  0.1 cm3 7.0 cm3/ 1
cylinder 7.1 cm3
(10 cm3)
Burette 0.1 cm3  0.05 cm3 24.90 cm3 / 2
3
(50.00 cm ) 24.95 cm3 A burette must be
read twice in order
(record to 2 to obtain a particular
decimal volume, so the total
places.; 2nd error made in
d.p. either ‘0’ volume
or ‘5’) measurement using
a burette is  (0.05 +
0.05) cm3 =  0.10
cm3
Thermometer 0.2 C  0.1 C 32.0 C / 1

(-10 C to 110 32.2 C
C) The precision
Thermometer 1 C  0.5 C 32.0 C / 1 depends on the type
(-5 C to 150 32.5 C of the thermometer
C) (d.p. either ‘0’ used.
or ‘5’)
Page 25
4.3.3 Examples of Data Recording and Data Presentation
Mass Reading (Weighing by difference)

This is usually done for solids that are insoluble in water and a complete transfer of solids into
the standard flask is not possible. All readings should be recorded to 2 or 3 decimal places
depending on the precision of the weighing balance used.
Mass of empty weighing bottle / g a

Mass of weighing bottle + FA1 / g b
Mass of weighing bottle + residue / g c
Mass of FA1 / g b–c
Note: The value of (b – c) should be within the range of mass given in the question.
Mass Reading (when reweighing is not required)

This is usually done for solids that are soluble in water and can be completely transferred into
the standard flask by transferring the washings in to the flask. Similar to the above, all readings
should be recorded to 2 or 3 decimal places depending on the precision of the weighing
balance used.
Mass of empty weighing bottle / g a

Mass of weighing bottle + FA1 / g b
Mass of FA1 / g a–b
Burette Reading
All burette readings are to 2 decimal places and to the nearest 0.05 cm3.
1 2 3
Final burette reading / cm3 24.00 48.30 24.60
Initial burette reading / cm3 0.00 24.00 0.20
Volume of FA1 / cm3 24.00 24.30 24.40
Chosen titre values  
Note: Chosen titre values must be consistent, i.e. within 0.10 cm3. If the first two titre values
are consistent, there is no need to carry out the third titration.
24.30+24.40
Average volume of FA1 used = 2
= 24.35 cm3 Leave
answer to 2
d.p.!
Page 26
4.4 CALCULATIONS & ANALYSIS
4.4.1 Calculations Involved in Volumetric Analysis
Stoichiometric Route Map
a) Common Formulae
mass (g)
Number of moles =
molar mass (g mol -1 )
Number of moles = concentration (mol dm−3) x volume (dm3)
mass of solute (g)

Concentration in g dm−3, c =
volume of solution (dm 3 )
no. of mol of solute (mol)

Concentration in mol dm−3, c =
volume of solution (dm 3 )
b) Dilution:
no. of mole of substance before dilution = no. of mole of substance after dilution
c1V1 = c2V2
c1 = concentration of solution before dilution
V1 = volume of solution before dilution
c2 = concentration of solution after dilution
V1 = volume of solution after dilution
c) Scaling up:
Amount of HCl in 25 cm3 of FA 1 = 0.0100 mol
250
Amount of HCl in 250 cm3 of FA 1 = x 0.0100 = 0.100 mol
25
Scaling down:
Amount of HCl in 250 cm3 of FA 1 = 0.100 mol
25
Amount of HCl in 25 cm3 of FA 1 = x 0.100 = 0.0100 mol
250
Page 27
experimental mass (g)

d) Percentage yield of a substance = x 100%
theoretical mass (g)
mass of pure substance (g)

e) Percentage purity of a substance = x 100%
mass of impure sample (g)
Worked Example:
100 cm3 of a solution of hydrochloric acid were diluted to 250 cm3 with distilled water.
26.8 cm3 of this diluted acid were needed to neutralise 25.0 cm3 of a solution of sodium
carbonate of concentration of 0.0500 mol dm–3, with methyl orange as indicator.
What is the concentration in mol dm–3 and in g dm–3 of the original acid?
dilution Scaling
down
26.80 cm3
HCl used
original HCl in
100 cm3
conc? Diluted HCl
in 250 cm3 25.0 cm3 of
0.05 mol dm-3
Na2CO3 added
Solution:
2 HCl + Na2CO3  2 NaCl + CO2 + H2O
25
Amt of Na2CO3 used = 0.0500 × = 1.25 × 10–3 mol
1000
2 HCl ≡ Na2CO3
Amt of diluted HCl reacted = 2 × 1.25 × 10–3 = 2.50 × 10–3 mol
250
Amt of diluted HCl in 250 cm3 = 2.50 × 10–3 × = 0.0233 mol
26.80
The number of moles present in 250 cm3 of the dilute HCl

Dilution
= number of moles present in 100 cm3 of original HCl
concept
 100 cm3 of original HCl contained 0.0233 mol of HCl.
0.0233
Concentration of original HCl = = 0.233 mol dm–3 of HCl
100/1000
Concentration of original acid in g dm-3 = 0.233  36.5 = 8.50 g dm–3
Points to note:
The number of moles before dilution = number of moles after dilution (i.e. C1V1= C2V2)
Since the volume of HCl solution increases from 100cm3 to 250 cm3, the concentration of
the original acid would be 250 = 2.5 times higher.
100 Page 28
4.4.2 Calculations in Uncertainty
Every measurement contains a range of uncertainty and it is also called as apparatus

error. For some apparatus, the error is printed on it. There is no instrument or device is
capable of producing an exact result with no uncertainty.
Percentage uncertainty accounts for errors in measurements. The general formula for
calculating percentage uncertainty/percentage error of a measurement is as such:
 x
Percentage uncertainty/percentage error = x 100%
x
∆x = absolute uncertainty of apparatus
x = measurement made
Worked example:
A student weighed out 1.005 g of CaCO3. The solid was dissolved in deionised water
and make up to 100 cm3 in a volumetric flask. 25.0 cm3 of this solution was pipetted and
titrated against an aqueous solution of hydrochloric acid. A titre volume of 23.50 cm3 of
hydrochloric acid was obtained.
The uncertainties (errors) associated with each reading using a weighing balance,
volumetric flask, pipette and burette are ±0.001 g, ±0.20 cm3, ±0.06 cm3 and ±0.05 cm3
respectively.
Calculate the maximum total percentage uncertainty of this titre volume.
Page 29
Measurement Absolute Percentage

uncertainty uncertainty/percentage
Apparatus used error
Weighing balance 1.005 g ±0.001 g  0.001
x 100% = ±0.1%
1.005
Volumetric flask 100 cm3 ±0.20 cm3  0.20
x 100% = ±0.20%
100
Pipette 25.0 cm3 ±0.06 cm3  0.06
x 100% = ±0.2%
25.0
Burette 23.50 cm3 (±0.05 cm3) +  0.10
(±0.05 cm3) = x 100% = ±0.40%
23.50
±0.10 cm3
The burette is read twice in The number of decimal

obtaining a titration reading places or significant figures
of the results is important,
refer to Point to Note for
more information
Point to note:
To measure a volume using a burette, the burette is read twice and two burette readings (initial
and final) have to be taken.
Hence, the total absolute uncertainties for this volume
= absolute uncertainty of initial reading + absolute uncertainty of final reading
= 0.05 cm3 + 0.05 cm3 = ±0.10 cm3
(2 d.p.) (2 d.p.) (2 d.p.)
Total percentage uncertainty = 0.1 + 0.20 + 0.2 + 0.40 = ±0.9%
Point to note:
During addition and subtraction, the result must be reported to the same number of decimal
places as the data with the fewest decimal place.
Total percentage uncertainty = 0.1 + 0.20 + 0.2 + 0.40 = ±0.9%
(1dp) (2dp) (2dp) (2dp) (1dp)
During multiplication and division, the result must be reported to the same number of
significant figures as the data with the fewest significant figures.
 0.001 (1s.f.)
x 100% = ±0.1% (1sf)
1.005 (4s.f.)
Page 30
4.4.3 Calculations in Experimental Error
Experimental error is used when comparing an experimental result with a theoretical

value that is accepted as the “correct value”.
Theoretical value - experimental value

Experimental error = x 100%
Theoretical value
This value allows us to find out how much the experimental value deviates from the
theoretical value or how much error we have in the experiment.
If the experimental error is larger than the total percentage uncertainty, the result is
inaccurate. If the experimental error is smaller than the total percentage uncertainty, the
result is accurate.
Page 31
4.5 GENERIC CHECKLIST
1 Checklist for Manipulative Skills ()

Ensure that the weighing bottle is dry.
Transfer solid to beaker outside weighing balance.
Stir with a glass rod to dissolve solid completely in beaker.
Standard Solution
Transfer solution completely into the volumetric flask without spillage.

Rinse beaker, glass rod and filter funnel with deionised water a few times and
add washings to the volumetric flask.
Add distilled water from the distilled water bottle into the volumetric flask until
the solution level is near the calibration mark.
Add water dropwise using a dropper until the bottom of the meniscus is just
touching the calibration mark at eye level.
Stopper the volumetric flask, invert and shake the flask a few times to make a
homogenous solution.
Rinse the pipette with the solution to be filled.
Use of pipette
Hold the upper part of the pipette when fitting the pipette filler to prevent
breakage.
Use pipette filler to draw the liquid.
Adjust liquid level in the pipette with the tip of pipette above liquid surface.
Gently tap the pipette tip against the bottom of tilted conical flask a few times
and drain out the last portion of the solution (do not remove last drop in the tip).
Rinse the burette with the solution to be filled (titrant).
Use of burette
Clamp the burette vertically by clamping between the groves of the clamp.
Fill the burette using filter funnel at eye level or lower to avoid spillage without
climbing on a stool.
Ensure that there is no air bubble anywhere in the burette, particularly in the tip.
Remove the filter funnel from the burette before taking any readings.
Place conical flask on a white tile during titration to help in colour change
observation.
Ensure the burette tip is slightly inside the conical flask without touching the
sides of the conical flask.
Titrate with continuous swirling.
Titration
Ensure no titrant added adheres to the inners walls of the conical flask during
titration by washing the inner walls with distilled water from the distilled water
bottle if necessary.
Add titrant dropwise near end-point.
Stop titration at correct point (first permanent colour change)
Repeat titration until two consistent titres (within ±0.10 cm3) are obtained.
Take burette readings at eye-level to avoid parallax error.
2 Checklist for Presentation of Data ()
Draw tables with appropriate headings and units.
Reading
Record mass readings to 3 decimal places.

s
Record pipette readings to 1 decimal place.

Record burette readings to 2 decimal places (to nearest 0.05 cm3).
Page 32
Calculate average titre and express it to 2 decimal places (put ticks against
chosen titres used)
Write statements for calculations.
Calculations
Show working in all calculations.

Leave all final calculated answers to 3 significant figures unless otherwise
stated.
Leave Mr values to 1 decimal place.
Give appropriate units in all calculations.
Page 33

Catholic Junior College H2 Chemistry 9729 2018 Practical Handbook - Part 1

Uploaded by

Document Information

Original Description:

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

Catholic Junior College H2 Chemistry 9729 2018 Practical Handbook - Part 1

Uploaded by

Copyright:

Available Formats

CATHOLIC JUNIOR COLLEGE

2018 PRACTICAL HANDBOOK – Part 1

Experiment Experimental techniques (syllabus

2 Laboratory Safety Rules

3 No indiscipline or foolery is allowed in the laboratories.

6 Unauthorised experiments are prohibited.

12 Damaged equipment, breakages, accidents and spillage should be reported

13 Unlabelled chemicals should not be used. Unlabelled containers should be reported to

18 Chemical and biological wastes must be disposed appropriately.

ACCIDENTS AND SAFETY MEASURES

23 All accidents must be reported immediately to the teacher-in-charge for treatment or

24 All students must note the positions of

25 No chemicals or apparatus may be removed from the laboratories without written

BREAKAGE OF APPARATUS (DAMAGE, DEFACING OF APPARATUS)

28 All apparatus is on loan to the students for their use.

29 All breakages must be reported to the laboratory technicians/assistants and particulars

Bench reagents for practical work

GHS (Globally Harmonised System of Classification and Labelling of chemicals) pictograms

GHS Pictogram Product identifier Concentration

aqueous sodium approximately

aqueous silver approximately

No pictogram is required for this reagent aqueous barium approximately

CPDD A-Level Science Unit Nov 2016

GHS hazard pictograms

Explosive Flammable Oxidising

3 Chemistry Practical Assessment

Assessment Objectives (Experimental skills and investigations)

Candidates will be assessed in the following skill areas:

1. Volumetric Analysis (Titrations e.g. acid-base, redox, iodimetric/iodometric, indirect,

2. Gravimetric Analysis, e.g. volatilization gravimetry (e.g. determination of water of

4. Thermochemistry, including thermometric titration

5. Chemical Kinetics, e.g. continuous and initial rate methods

6. Qualitative Analysis (QA) - Inorganic (identification of cations and anions)

7. Qualitative Analysis (QA) – Organic (simple test-tube reactions indicating the

VOLUMETRIC ANALYSIS is a qualitative technique used to determine the concentration of a

Basic Principle of Titration:

(a) ACID-BASE TITRATION:

Examples of acids and bases commonly used in the laboratory:

Weak acids Weak bases

Common indicators used in acid-base titrations:

Methyl Orange Red Orange Yellow

Thymolphthalein Colourless Light blue Blue

Choice of indicators for different types of acid-base titrations:

(b) REDOX TITRATIONS

Two main types of redox titrations:

(i) Redox titrations involving ACIDIFIED POTASSIUM MANGANATE(VII), KMnO4

4.2 EXPERIMENTAL TECHNIQUES

4.2.1 Common Laboratory Apparatus & Equipment Used

Apparatus Capacity Purpose

Conical flask 250 cm3 To hold solution for

Beaker 50 cm3, 100 cm3, To hold liquid

Measuring 10 cm3, 25 cm3, 50 For measuring

Volumetric / 250 cm3 To prepare

Filter funnel To direct solution

To hold filter paper

Pipette filler To draw up

Pipette 10.0 cm3, 25.0 cm3 To measure a fixed

Burette 50.00 cm3 To measure a

Retort stand with To hold burette or

White tile To see colour

Glass rod To stir and allow

Weighing balance To measure the