2021 JC1 H2 Chemistry (9729) Volumetric Analysis Practical Notes
2021 JC1 H2 Chemistry (9729) Volumetric Analysis Practical Notes
2021 JC1 H2 Chemistry (9729) Volumetric Analysis Practical Notes
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.
END OF PRACTICAL:
Wash all used apparatus thoroughly with tap water only. Do not waste deionised water!
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
Valve E: to empty
pipette
pipette
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) 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
Strong acid – strong base Methyl orange, screened methyl orange, phenolphthalein, thymolphthalein,
thymol blue,
Strong acid – weak base Methyl orange, screened methyl orange
Weak acid – strong base Phenolphthalein, thymolphthalein, thymol blue
Weak acid – weak base 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.
20.40 20.45
Average volume of hydrochloric acid used = = 20.43 cm3
2
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.
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.
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.
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.
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.
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:
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
Precision/Uncertainty Precision/Uncertainty
= 0.05 cm3 (2.d.p) = 0.5 cm3 (1.d.p)
(1/2 smallest division) (1/2 smallest division)
3. EXPRESSING ERRORS
Each error can also be expressed as a percentage of the quantity measured (percentage
error).
The total/overall apparatus error is the sum of the % errors associated with each piece of
apparatus.
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.
0.10
% error = 100 = 0.200%
50.00
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.
When 20.0 cm3 of solution is measured using a 50.0 cm3 measuring cylinder,
Using a burette instead of a 50.0 cm3 measuring cylinder reduces the % error and improves
the accuracy of the volume measured.
*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