2021 JC1 H2 Chemistry (9729)

Volumetric Analysis Practical Notes

Practical Assessment (Paper 4) General Information

Assessment Objectives
Candidates should be able to
 follow a detailed set or sequence of instructions and use techniques, apparatus and materials
safely and effectively;
 make, record and present observations and measurements with due regard for precision and
accuracy;
 interpret and evaluate observations and experimental data;
 devise and plan investigations, select techniques, apparatus and materials;
 evaluate methods and techniques, and suggest possible improvements.

Skills Assessed
The assessment of practical skills is conducted by reference to four skill areas.
 Planning (P)
 Define the question/problem using appropriate knowledge and understanding.
 give a clear logical account of the experimental procedure to be followed.
 describe how the data should be used in order to reach a conclusion.
 assess the risks of the experiment and describe precautions that should be taken to keep risks
to a minimum.

 Manipulation, Measurement and Observation (MMO)

 demonstrate a high level of manipulative skills in all aspects of practical activity.
 make and record accurate observations with good details and measurements to an appropriate
degree of precision.
 make appropriate decisions about measurements or observations.
 recognise anomalous observations and/or measurements (where appropriate) with reasons
indicated.

 Presentation of Data and Observations (PDO)

 present all information in an appropriate form.
 manipulate measurements effectively in order to identify trends/patterns.
 present all quantitative data to an appropriate number of decimal places/ significant figures.

 Analysis, Conclusions and Evaluation (ACE)

 analyse and interpret data or observations appropriately in relation to the task.
 draw conclusion(s) from the interpretation of experimental data or observations and underlying
principles.
 make predictions based on their data and conclusions.
 identify significant sources of errors, limitations of measurements and/or experimental
procedures used, and explain how they affect the final result(s).
 state and explain how significant errors/limitations may be overcome/ improved.

H2 Chemistry Practical Notes (VA) Page 1 of 13 JPJC Chemistry Unit 2021

Scheme of Assessment:
 Subject code: 9729
 Paper 4: Practical Paper
 Duration: 2 h 30 min
 Practical assessment weighting: Overall 20%
 Marks: 55
 The assessment of Planning (P) will have a weighting of 5% (around 1315 marks).
The assessment of MMO, PDO and ACE will have a weighting of 15%.
 One, or more, of the questions may incorporate some assessment of Skill P, set in the context
of the syllabus content, requiring candidates to apply and integrate knowledge and
understanding from different sections of the syllabus. It may also require the treatment of given
experimental data to draw a relevant conclusion and analyse a proposed plan.
 The assessment of skills PDO and ACE may also include questions on data-analysis which do
not require practical equipment and apparatus.
 Candidates will not be permitted to refer to books and laboratory notebooks during the
assessment.

Volumetric Analysis (VA)

AT THE START OF PRACTICAL:

 Wash all glassware (beakers, conical flasks, filter funnel, pipette, burette, glass dropper, volumetric
flask, glass rod) with tap water and then rinse them with deionised water.
 Beakers used to collect solutions must be rinsed with that solution, prior to use.
 Conical flasks should be rinsed with tap water, followed by deionised water only!

END OF PRACTICAL:
 Wash all used apparatus thoroughly with tap water only. Do not waste deionised water!

SAFETY DURING PRACTICAL:

 Wear eye protection (safety goggles).
 Keep work bench organised and neat.
 Pipette & burette must be clamped at all times.
 Filter funnel does not roll about.
 No breakage or dangerous act.
 Gloves are available on request.

H2 Chemistry Practical Notes (VA) Page 2 of 13 JPJC Chemistry Unit 2021

1. APPARATUS USED IN TITRATION
A. BURETTE
A burette is used to deliver variable volumes of a solution accurately. Burettes are usually of
50.00 cm3 capacity and calibrated in 0.10 cm3 divisions.

(a) Manipulative skills

(i) Rinsing of burette with solution
eye level
1. Rinse a filter funnel with the titrating solution
(titrant). burette

2. Use the filter funnel to pour some (about 10 cm3)

titrating solution into the burette.
3. Remove the filter funnel
4. Drain off some solution to rinse the tip of the
burette.
swirl the flask
5. Invert the burette. Pour out the solution from the continuously
top to rinse the top part of the burette (rotate the
burette while pouring out the solution). conical flask
6. Clamp the burette on the retort stand and drain off
white tile
all the remaining solution.

Figure 1: Correct titration technique

(ii) Topping up the burette
1. Use the filter funnel to fill up the burette to slightly above the 0.00 cm3 mark.
2. Remove the filter funnel.
3. Drain off some solution to fill the burette tip completely with the solution. Check that there
is no air bubble/column.
4. Adjust the solution level to a convenient initial burette reading. Check that the burette is
clamped vertically and read burette reading at eye level.
5. When a colourless or transparent solution is used in titration, the burette reading is taken
from the bottom of the meniscus.
For dark coloured and non-transparent solutions (e.g. KMnO4(aq)), the burette reading is
taken from the top of the meniscus.

(b) Recording of data

Burette readings are to be recorded to two decimal places and to the nearest 0.05 cm3.

Initial burette reading Final burette reading Sample recording of burette readings:
9.00
40.00
Final burette reading / cm3 40.15
40.15
9.80 Initial burette reading / cm3 9.80
10.00
Volume of HCl used / cm3 30.35
41.00

(c) Safety Precautions

1. Use a filter funnel to fill the burette to prevent spillage and avoid contact with the chemicals.
2. Fill up the burette at or below eye level to prevent spillage of chemicals onto eyes and body.
3. Do not climb on the stool when filling the burette.

H2 Chemistry Practical Notes (VA) Page 3 of 13 JPJC Chemistry Unit 2021

B. PIPETTE Valve A: to A
evacuate bulb
The pipette is a calibrated piece of glassware that can be
used to obtain a fixed volume of solution. bulb

10.0 cm3 and 25.0 cm3 pipettes are commonly used.

Valve S: to fill
A pipette filler (see Figure 2) is used to draw up the pipette
solution to reach the graduation mark of the pipette. Keep
the insides of a pipette filler dry at all times. S
E

Valve E: to empty
pipette
pipette

Figure 2: The pipette filler

(a) Manipulative Skills
(i) Rinsing of pipette with solution
1. Rinse the tip of the pipette with some solution.
2. Compress valve A and deflate the bulb of the
pipette filler.
3. Fit the pipette filler to the pipette.
(See Figure 3 for the correct technique of fitting
the pipette filler).
4. Place the tip of the pipette well below the
surface of the solution.
5. Compress valve S to fill the pipette to slightly
above the graduation mark.
6. Lift the pipette tip out of the solution.
7. Compress valve E gently to discard the solution
into the sink.
Figure 3: Correct technique of fitting the
pipette filler

(ii) Pipetting of solution into conical flask (See Figure 4 on page 5)

Repeat steps 2 to 6.
8. Compress valve E gently to dispense the solution until the bottom of the meniscus is at the
graduation mark.
(When checking the level of solution, ensure that the bottom of the meniscus is at the same
level with your eyes)
9. Remove the pipette filler while compressing valve E to dispense all the solution from the pipette
into the conical flask.
10. Allow the tip of the pipette to touch the side/ base of the conical flask. Do not blow out the
last drop from the pipette (the pipette has been calibrated to deliver the specified volume
taking into account this last drop).

H2 Chemistry Practical Notes (VA) Page 4 of 13 JPJC Chemistry Unit 2021

 Press S to suck
up solution until
2-3 cm above
graduated mark

Lift the pipette

tip out of the
solution when
adjusting the
solution to the
mark.

Step 4: Step 6 & 8: Step 10:

Tip of pipette must be Touch the tip of
Lift the pipette tip out of the pipette against the
well below solution
solution. inner side of conical
surface.
Compress valve E gently to flask.
dispense the solution until the
bottom of the meniscus is at Do not blow out the
the graduation mark.

Figure 4: Correct technique of pipetting a solution into conical flask

(b) Recording of Data

Pipette readings are to be recorded to one decimal place, either 25.0 cm3 or 10.0 cm3.

(c) Safety Precautions

1. Use a pipette filler to fill the pipette. No mouth pipetting!
2. Handle pipette filler safely when fitting the pipette filler (refer to Figure 3).

C. CONICAL FLASK
Manipulative skills:
1. Conical flasks used for titration should be washed clean with tap water and then rinsed with
deionised water. Never rinse a conical flask with the solution to be pipetted.
2. The conical flask need not be dry. Although it may contain some water which will dilute the
solution pipetted in, this dilution will not change the number of moles of the substance in
the flask.
3. During titration, the tip of the burette should be just inside the conical flask (see Figure 1 on
page 3) and a white tile should be placed below the conical flask, which makes it easier to see
the colour of the solution.

D. MEASURING CYLINDER

(a) Manipulative skills

1. Wash measuring cylinder with tap water and rinse it with deionised water.
2. Rinse measuring cylinder with the solution to be filled in.
3. Place the measuring cylinder on the bench top while pouring the solution into the cylinder and
read the bottom of the meniscus at eye level when taking the volume reading.
(b) Recording of data
Record all readings to the precision of the measuring cylinder provided (refer to page 11):
one decimal place and to the nearest 0.1 cm3 (for 10 ml measuring cylinder)
one decimal place and to the nearest 0.5 cm3 (for 50 ml and 100 ml measuring cylinders)
two decimal places and to the nearest 0.25 cm3 (for 25 ml measuring cylinder)

H2 Chemistry Practical Notes (VA) Page 5 of 13 JPJC Chemistry Unit 2021

 Video on pipetting techniques, burette
2. THE TITRATION preparation and titration techniques

A. Some Tips on Titration https://tinyurl.com/titration101

(a) The first titration may be carried out rapidly to obtain a rough value of the titre.
(b) For subsequent titrations, the solution (titrant) is added rapidly from the burette (with continuous
swirling) until the volume added is about 1 cm3 below the rough titre value.
(c) To obtain an accurate end-point, the titrant should be added dropwise until the first permanent
change of colour is observed.
(d) Titrations should be repeated until two consistent titre values within 0.10 cm3 in difference
are obtained to ensure reliability of results.

B. Acid-Base Indicators

The choice of indicators for acid-base titrations is summarised below:

Strong acid – strong base
Strong acid – weak base
Weak acid – strong base
Weak acid – weak base
Methyl orange, screened methyl orange, phenolphthalein, thymolphthalein,
thymol blue,
Methyl orange, screened methyl orange
Phenolphthalein, thymolphthalein, thymol blue
No suitable indicator

The table below lists the common indicators, their working pH range and the colour changes that can
be observed.

Working Colour
Indicator
pH range In acid At end point In alkali
Methyl orange 3–5 Red Orange Yellow
Screened methyl orange 3–5 Violet Grey Green
Phenolphthalein 8 – 10 Colourless Pale pink Red
Thymolphthalein 9 – 10 Colourless Pale blue Blue
1–3 Red Orange Yellow
Thymol Blue
8 – 10 Yellow Green Blue

C. Recording of Results

(a) Record all burette readings and titre values to 2 decimal places and to the nearest 0.05 cm3 in a
proper table with clear headings and units.
(b) Place ‘’ under two titre values which are consistent within 0.10 cm3 in difference.
(c) Calculate the average value (with units) of the two selected titres to 2 decimal places for
consistency of precision.

Sample recording of titration results:

Titration number 1 2 3
3
Final burette reading / cm 31.00 30.40 20.45
Initial burette reading / cm3 10.00 10.00 0.00
3
Volume of HCl used / cm 21.00 20.40 20.45
 

20.40  20.45
Average volume of hydrochloric acid used = = 20.43 cm3
2

H2 Chemistry Practical Notes (VA) Page 6 of 13 JPJC Chemistry Unit 2021

3. WEIGHING OF SOLID
The sample to be weighed should be placed
on the centre of the weighing pan.
draught-
The Tare pad resets the balance reading to protection
zero and thus the tare facility allows the shield
mass of the sample to be read directly.
weighing
The draught-protection shield will ensure that pan
the reading is not affected by wind or
movement.

Mass readings obtained from a weighing

balance capable of reading to 0.001 g are to
be recorded to 3 decimal places.
Tare button
Figure 5: The weighing balance

A. Manipulative skills
Note: The weighing bottle should be washed with tap water, rinsed with deionised water and then
wiped dry with a clean tissue paper before use.
Weighing of solid sample into the weighing bottle:
Step 1. With all doors of the shield closed, press the ‘Tare’ button to set the balance
reading to zero.
Step 2. Place a clean and dry empty weighing bottle on the centre of the weighing pan
and close the door of the shield. When the reading stabilises, record the mass of
the empty weighing bottle.
Step 3. With the empty weighing bottle on the weighing pan, press the Tare button to set
the balance reading to zero.
Step 4. Remove the weighing bottle from the weighing pan. Add the required mass of
solid sample into the weighing bottle and put it back on the weighing pan.
Close the door of the shield.
(Do not add solid to the weighing bottle when it is on the weighing pan. This is to
ensure that no solid will spill onto the pan.)
Step 5. Remove the weighing bottle with the solid sample from the weighing pan and close
the door of the shield.
Press the Tare button to set the balance reading to zero.
Step 6. Place the weighing bottle with the solid sample on the centre of the weighing pan
and close the door of the shield. When the reading stabilises, record the total mass
of solid sample and weighing bottle.

H2 Chemistry Practical Notes (VA) Page 7 of 13 JPJC Chemistry Unit 2021

 0.000 3.451 0.000
g
 Press the  Record the mass  Press the
TARE button. of empty bottle. TARE button.

5.454 0.000 2.003

 Record the mass of  Remove the bottle with  Remove the bottle and add
in the required mass of
bottle and solid solid and press the
TARE button solid. Reading observed is
the mass of solid in the
bottle
B. Recording of data
All mass readings obtained from a weighing balance capable of reading to 0.001 g are to be
recorded to 3 decimal places.

Sample mass recording 1:

[This task requires students to weigh accurately between 4.50 g and 5.00 g of solid FA 1 into the
weighing bottle.]
mass of weighing bottle + FA 1 / g 10.418
mass of empty weighing bottle / g 5.672
mass of FA 1 used / g 4.746

Sample mass recording 2:

[This task requires students to find out the mass of solid FA1 used in the experiment when a
sample of FA 1 is provided in a weighing bottle.]

mass of weighing bottle + FA 1 / g 9.309

mass of weighing bottle + residual FA 1 / g 5.686
mass of FA 1 used / g 3.623

Note: Use the correct terminology, “mass” not “weight”.

H2 Chemistry Practical Notes (VA) Page 8 of 13 JPJC Chemistry Unit 2021

4. PREPARATION OF A SOLUTION
A. Standard/ Graduated/ Volumetric flask
The graduated/volumetric flask is a calibrated piece of glassware that can be graduation mark
used to prepare a fixed volume of solution. A 250 cm3 volumetric flask is
commonly used. A volumetric flask is often used for dilutions and the
preparation of standard solutions from a solid.
250

Manipulative skills:
1. Wash the volumetric flask with tap water and rinse it with deionised water. Never rinse a
volumetric flask with the solution to be added.
2. The volumetric flask need not be dry as deionised water will be added later to make up to the
mark.
3. To make up the solution in the volumetric flask to the graduation mark, add deionised water,
until the level is about 1 cm below the graduation mark. Add deionised water dropwise
to bring the bottom of the meniscus to the mark. (see Figure 6)
4. Insert the stopper (ensure the stopper is tight-fitting) and shake thoroughly by inverting the
flask at least ten times to obtain a homogeneous solution.

Figure 6:
Fill the volumetric flask such
that the bottom of the meniscus
touches the graduation mark.
Eye position is level with
the surface of the liquid

B. Dilution
Manipulative skills: Preparing solution by dilution of concentrated solution

Step 1. A known volume of concentrated solution is placed into a volumetric flask either
by using a pipette or burette.
Step 2. Add deionised water, until the level is about 1 cm below the graduation mark.
Step 3. Pour some deionised water into a clean small beaker. Using a dropper (already
washed and rinsed with deionised water), add deionised water (from the beaker)
dropwise to bring the bottom of the meniscus to the mark (see Figure 6).

Step 4. Insert the stopper (ensure the stopper is tight-fitting) and shake thoroughly by
inverting the flask at least ten times to obtain a homogeneous solution.

http://tinyurl.com/hqep5g
e (from 6:47 – 9.19)
OR Video on manipulative
skills for dilutionIn this
section of the video,
the solution to be
diluted is already in the

 &  
Using either pipette or Add deionised water until about Stopper, invert & shake
burette, add a known 1cm below graduation mark. the volumetric flask at
volume of solution into a Add deionised water dropwise to least ten times to obtain
volumetric flask. bring the meniscus to the mark. homogeneous solution.

H2 Chemistry Practical Notes (VA) Page 9 of 13 JPJC Chemistry Unit 2021

C. Standard solution preparation (from solid)
Video on preparation of standard
This involves weighing out accurately a known mass of the solution from solid.
solid sample and dissolving it to make a fixed volume of
https://tinyurl.com/standard
solution. (usually 250 cm3). solutionprep

Manipulative skills: Preparing solution from the weighed solid sample

Step 1. Transfer the weighed solid sample into a clean small beaker.
Step 2. Rinse out the remaining solid from the weighing bottle with some deionised water
and transfer the washings into the small beaker. Rinse a second time and transfer
the washings into the small beaker.
Step 3. Add more deionised water until the solution level is about 60 cm3. Use a glass rod
to stir until all solids have completely dissolved.

Step 4. Transfer the solution into the graduated flask via the filter funnel, using a glass
rod to direct the solution into the flask.
Using deionised water,
 rinse the beaker;
 rinse the glass rod;
 rinse the filter funnel and remove the funnel;
making sure that all the washings go into the graduated flask.
Important Note: Keep track of the solution level at all times. Rinse slowly and
sparingly to ensure that the solution level does not exceed the graduation mark.
Step 5. Add deionised water, until the level is about 1 cm below the graduation mark.
Step 6. Pour some deionised water into a clean small beaker. Using a dropper (already
washed and rinsed with deionised water), add deionised water (from the beaker)
dropwise to bring the bottom of the meniscus to the mark.

Step 7. Insert the stopper (ensure the stopper is tight-fitting) and shake thoroughly by
inverting the flask at least ten times to obtain a homogeneous solution.

beaker
glass rod

beaker


Use a glass rod
to stir until all
solids dissolve.
Transfer solution Rinse the glass rod,
,,
into the volumetric
flask.
 filter funnel and
beaker to ensure
Make up the solution
to the mark using
complete transfer. deionised water.

H2 Chemistry Practical Notes (VA) Page 10 of 13 JPJC Chemistry Unit 2021

 ERROR ANALYSIS

1. SOURCES OF ERROR
Two main sources of error:
(a) 'Apparatus Error', an error which is inherent in the use of a particular piece of equipment/
apparatus. That is, there is a 'range of uncertainty' associated with measurements made with
that piece of equipment. This uncertainty will be present no matter how skillful the operator
might be.
(b) 'Experimental Error', an error which is a direct consequence of the level of incompetence of
the operator or of flaws in the experimental procedure.

2. PRECISION / UNCERTAINTY OF INSTRUMENT

A measuring instrument is a device with either a scale or read-out mechanism that allows
measurement of a physical quantity to be read off.

In general, the read-out mechanism (for electronic balance or stop-watch) has a smallest division
or unit. This smallest division determines the precision/uncertainty of the instrument.

However, when taking readings from a scale, the precision/uncertainty in each reading of such
instruments is then half of the smallest division.

The following table summarises the precision/uncertainty of some common equipment and
apparatus:

Apparatus/Equipment Smallest Uncertainty in Examples of

Division/Unit each reading Recording

Volumetric/ graduated flask _ varies according 250 cm3, 100 cm3

to grade

Pipette _ varies according 25.0 cm3, 10.0 cm3

to grade

Burette 0.10 cm3 0.05 cm3 23.50 cm3, 23.55 cm3

10 ml Measuring cylinder 0.2 cm3 0.1 cm3 5.0 cm3, 5.1 cm3

25 ml Measuring cylinder 0.5 cm3 0.25 cm3 5.00 cm3, 5.25 cm3

50 ml Measuring cylinder 1.0 cm3 0.5 cm3 15.0 cm3, 15.5 cm3

100 ml Measuring cylinder 1.0 cm3 0.5 cm3 70.0 cm3, 70.5 cm3

Thermometer 1.0 oC 0.5 oC 31.0 oC, 31.5 oC

(1 oC Interval)

Thermometer 0.2 oC 0.1 oC 23.1 oC, 23.2 oC

(0.2 oC Interval)

Electronic balance 0.001 g 0.001 g 3.526 g, 3.527 g

(3 decimal places)

Digital Stop-watch 0.01 s 0.01 s Read the procedure for

actual precision of
recording. (nearest s /
nearest 0.1 s)

H2 Chemistry Practical Notes (VA) Page 11 of 13 JPJC Chemistry Unit 2021

 Example:
Burette 50 ml Measuring cylinder

Precision/Uncertainty Precision/Uncertainty
= 0.05 cm3 (2.d.p) = 0.5 cm3 (1.d.p)
(1/2 smallest division) (1/2 smallest division)

Burette reading = 24.80 cm3 (2.d.p.) Measuring cylinder reading

= 43.0 cm3 (1.d.p)

3. EXPRESSING ERRORS

 Standard format: (quantity measured  uncertainty)

 Each error can also be expressed as a percentage of the quantity measured (percentage
error).

% error associated with making a single measurement

uncertainty of that apparatus
= quantity measured  100%

 The total/overall apparatus error is the sum of the % errors associated with each piece of
apparatus.

Illustration 1 (burette reading):

Compare the % error if a student uses a 50.00 cm3 burette to measure 50.00 cm3 and 5.00 cm3 of a
solution separately.

Each burette reading is subject to an error of 0.05 cm3 as the burette measures volumes to the
nearest 0.05 cm3.

The burette is read twice (initial and final readings) and the total error to obtain a single volume
measurement is 0.05  2 = 0.10 cm3.

% error in the volume measurement using a burette

= 0.10  100%
volume measured

When 50.00 cm3 of solution is measured using a 50.00 cm3 burette,

0.10
% error =  100 = 0.200%
50.00

When 5.00 cm3 of solution is measured using a 50.00 cm3 burette,

0.10
% error =  100 = 2.00%
5.00

The % error in measuring 5.00 cm3 will be ten times higher than that in measuring 50.00 cm3.
Note: The larger the quantity measured, the smaller the specific apparatus error.

H2 Chemistry Practical Notes (VA) Page 12 of 13 JPJC Chemistry Unit 2021

Illustration 2 (pipette reading):
Calculate the percentage error when pipetting 25.0 cm3 of solution using a 25.0 cm3 pipette with
a precision of 0.06 cm3.
0.06
% error =  100 = 0.240%
25.0

Illustration 3 (burette reading & measuring cylinder reading):

Compare the % error if a student measures 20.0 cm3 of solution using a 50.00 cm3 burette and a
50.0 cm3 measuring cylinder separately.

When 20.0 cm3 of solution is measured using a 50.00 cm3 burette,

% error = 0.10  100 = 0.500%

uncertainty arising from
two readings
20.00

When 20.0 cm3 of solution is measured using a 50.0 cm3 measuring cylinder,

0.5 uncertainty arising from

% error =  100 = 2.50% one reading
20.0

Using a burette instead of a 50.0 cm3 measuring cylinder reduces the % error and improves
the accuracy of the volume measured.

Illustration 4 (total apparatus error):

A student prepares 250 cm3 of FA 1 solution in a 250 cm3 graduated flask. He pipettes 25.0 cm3
of FA 1 into a conical flask and then titrates it with FA 2 from a burette. He repeats the titration
and obtains a mean titre of 25.40 cm3.
The errors (uncertainties) associated with each reading using a graduated flask, pipette and
burette are, 0.15 cm3, 0.1 cm3 and 0.05 cm3 respectively.
Calculate the maximum total percentage error (uncertainty) of this mean titre volume.

Volume of FA 1 prepared = 250 cm3

% error = 0.15  100 = 0.0600%
250

Volume of FA 1 pipetted = 25.0 cm3

0.1
% error =  100 = 0.400%
25.0

Mean titre value = 25.40 cm3

% error = *0.10  100 = 0.394%
25.40

Maximum total percentage error = 0.0600 + 0.400 + 0.394 = 0.854%

*The mean titre value is obtained by averaging two accurate titre values.
Each accurate titre value has an error of (0.05  2) cm3 (as the burette is read twice).

Therefore, error in the mean titre value =  (0.10  0.10) = 0.10 cm3
2

H2 Chemistry Practical Notes (VA) Page 13 of 13 JPJC Chemistry Unit 2021