Lab Report

Name : LIM KAH HOU

Matric No. : U2103352/1
Experiment No. : 1
Date of Experiment : 1ST NOVEMBER 2021

Title
VOLUME MEASUREMENTS

Objectives
1. To recognize the different types of volume calibrations (in and out) and the impact it has
on measurements
2. To be aware of safe and clean operation in chemical laboratory

Procedure
The experiment was carried out according to the SIC1011 manual

Results and Analysis

3.3.1 Density of the calibration fluid
The mass of a 25 ml of empty volumetric flask (mo) : 17.7g
Repetition Mass of the filled Mass of the calibration Density of the
volumetric flask (m1) / g liquid (m) / g calibration liquid / g ml-1
1 43.1 25.4 1.016
2 43.1 25.4 1.016
Average density 1.016
Table 1

Standard deviation, σ = 0
Formula:
mass of the calibration liquid, 𝑚 = 𝑚1 − 𝑚𝑜
𝑚
Density of the calibration liquid, ρ =
𝑉
3.3.2 Evaluation of measurement accuracy for a pipette
The mass of the empty beaker (mo) : 45.9g
Density of the calibration liquid, ρ : 1.016 g ml-1
Volume of calibration Mass of the filled beaker / g
liquid measured / ml Trial 1 Trial 2 Trial 3
1 46.9 47.8 48.9
2 50.9 52.9 -
5 57.9 62.9 -
10 73.2 83.3 93.5
Table 2

Volume of Volume of calibration liquid calculated / ml Average volume of

calibration liquid Trial 1 Trial 2 Trial 3 calibration liquid
measured / ml calculated / ml
1 0.98 0.89 1.08 0.98
2 1.97 1.97 - 1.97
5 4.92 4.92 - 4.92
10 10.14 9.94 10.14 10.04
Table 3

Formula
62.9−57.9
Volume of calibration liquid calculated for 5 ml, trial 2 =
1.016

3.3.3 Evaluation of measurement accuracy for a measuring cylinder

The mass of the empty measuring cylinder (mo) : 41.0g
Density of the calibration liquid, ρ : 1.016 g ml-1
Volume of calibration Mass of the filled measuring cylinder (m) / g
liquid measured / ml Trial 1 Trial 2 Trial 3
1 42.1 42.1 -
2 43.1 43.2 43.1
5 46.2 46.3 46.3
10 51.3 51.3 -
Table 4
 Volume of Volume of calibration liquid calculated (v) / ml Average volume of
calibration liquid Trial 1 Trial 2 Trial 3 calibration liquid
measured / ml calculated / ml
1 1.08 1.08 - 1.08
2 2.07 2.17 2.07 2.10
5 5.12 5.23 5.23 5.19
10 10.14 10.14 - 10.14
Table 5

Formulae:
𝑚 − 𝑚𝑜
Volume of calibration liquid calculated, 𝑣 =
𝜌

3.3.4 Data Analysis

Volume of calibration Average volume of calibration liquid
liquid measured (vo) / ml calculated by using pipette (v) / ml Deviation Relative Error/%
(v – vo)
1 0.98 0.02 2.0
2 1.97 0.03 1.5
5 4.92 0.08 1.6
10 10.04 0.04 0.4
Table 6

Volume of calibration Average volume of calibration liquid

liquid measured (vo) / ml calculated by using measuring Deviation Relative Error/%
cylinder (v) / ml (v – vo)
1 1.08 0.08 8.0
2 2.10 0.10 5.0
5 5.19 0.19 3.8
10 10.14 0.14 1.4
Table 7

Formula:
Deviation
Relative error = × 100%
volume of calibration liquid measured
Graph of relative error against volume of calibration liquid measured
Relative Error, %

Volume of calibration liquid measured, ml

Graph 1

Note that the curve is drawn based on the data plotted, it does not necessarily reflect the actual trend.

Discussion
Based on the table 6 and 7, the volume calculated for 1ml, 2ml, 5ml and 10ml of calibration
fluid using pipette are 0.98ml, 1.97ml, 4.92ml and 10.04ml respectively with relative error of 2.0%,
1.5%, 1.6% and 0.4% whereas for measuring cylinder, the volume calculated are 1.08ml, 2.10ml,
5.19ml and 10.14ml with relative error of 8.0%, 5.0%, 3.8%, 1.4%. It can be observed that the
accuracy of pipette is higher than that of using measuring cylinder. However, in theory, the
accuracy of both volume measurements is expected to be similar.
 This is because the graduated pipette used in this experiment is calibrated ‘ex’ that designed
to deliver its content to another container while measuring cylinder is calibrated ‘in’ that is,
designed to contain the liquid it held. Theoretically, the volume of liquid a graduated pipette
contain will be more than what was written on the scale as it includes the volume for drainage
holdback error, that is, the liquid that remains on the tip of pipette as well as the wall of pipette
thus, an accurate volume of liquid will be transfer to another container. Meanwhile, the measuring
cylinder would hold the exact volume as the reading on the scale as it is designated to contain the
liquid.

In this scenario, both graduated pipette and measuring cylinder are used in accordance to their
calibration, in other word, pipette is used for delivery while measuring cylinder is used for
containment. Hence, both supposed to have similar accuracy. Nonetheless, in practical, measuring
cylinder is less accurate than pipette because measuring cylinder usually have larger meniscus as
opposed to pipette, as pipette usually are long, narrow with slender neck which makes reading
meniscus easier. Other possible factors that can contribute to such phenomena is by systemic errors
whereby the reading of the scale itself is slightly off or random errors such as parallax error.

Moving on, when the measuring cylinder is used as calibrated ‘ex’ whereby its content is
transferred to a beaker; unfortunately, due to experimenter’s mistake, the mass of liquid transferred
from measuring cylinder to a beaker is not measured and recorded. Due to this, the actual volume
of liquid that being transferred to the beaker by measuring cylinder cannot be determined.
Therefore, the comparison between the accuracy of volume measurements of pipette and
measuring cylinder can only be done theoretically. In theory, the volume of liquid transferred from
measuring cylinder to beaker should be less than the desired volume which makes it less accurate
than pipette. This is because measuring cylinder is calibrated ‘in’, that is, designed to contain the
liquid it held. Hence, when it is used to transferred liquid to another container, some of the liquid
remains in the measuring cylinder which caused the volume transferred to be less than the desired
amount. Hence, the accuracy of volume measurement for measuring cylinder when used as
calibrated ‘ex’ will be lower compared to use as calibrated ‘in’ and much lower when compared
to pipette.

In hindsight, pipette is a better instrument for volume measurement compared to measuring

cylinder as pipette is calibrated ‘ex’ which meant for delivering its content to another vessel
whereas for measuring cylinder, it is calibrated ‘in’ which meant to hold the content. To ensure
accurate reading, it is advised to use pipette for delivery whereas measuring cylinder for
containment.

Moving on, based table 6 and graph 1, it can be observed that when a 10 ml measuring cylinder
is used to measure 1 ml of calibration liquid, the relative error turns out to be rather large value
(8.0%, about one tenth of the desired value) in comparison to the other trials. Conversely, for 2 ml
and 5 ml, the relative errors decrease gradually to 5.0% and 3.8% respectively. This shows that as
the volume to-be measured increases, the relative error will gradually diminish until the maximum
volume of the measuring cylinder can measure is reached, that is 10 ml. At that point, the relative
error is only about 1.4%. From here, it can be deduced that the reading would be most accurate
when the volume desired matches with the maximum capacity of the measuring cylinder as it will
have the lowest possible relative error compared to measuring volume that is below the maximum
capacity. In other word, to measure 10 ml of liquid, one must use measuring cylinder that can only
measure up to 10 ml, to minimise the relative error made.

Based on the findings above, it can be concluded that measuring cylinder is not suitable to
deliver its content to another vessel as it will most likely to cause the data to be inaccurate.
However, there is an alternative procedure for the experimenter to follow in order to use measuring
cylinder and Pasteur pipette for volume measurement purposes without compromising its accuracy.
The alternative procedure is shown as below:

Procedure for reasonable accurate measurement of 1ml using measuring cylinder

1. Measure 10 ml of calibration fluid in the measuring cylinder

2. Measure and record the mass of an empty beaker

3. Use Pasteur pipette to draw 1ml of calibration fluid from the measuring cylinder to the beaker

4. Measure and record the mass of the filled beaker

5. Calculate the transferred volume based on the density from 3.3.1

6. Repeat the measurements. If the results for the measurements differ significantly, perform a
third measurement

Due to time constraint, the experimenter was not able to carry out the procedure. However,
theoretically speaking, the accuracy of the alternative procedure would be relatively better than
that of the original procedure. This is because the original procedure required the experimenter to
transfer the entire content of measuring cylinder to a beaker. It is almost impossible to achieve it
as liquid will tend to stick onto the wall due to its adhesive nature. Whereas the alternative
procedure does not require that, instead, the content is only partially removed using Pasteur pipette.
In that way, the liquid that stick onto the wall of measuring cylinder became insignificant to the
reading. Therefore, the measurement would be relatively accurate and close to desired value.

Next, throughout the experiment, there are few mistakes that have been done by the
experimenter. The major problem that happened is experimenter unable to have a good grasp of
the procedure. Due to this, there are 2 major steps that being skipped by the experimenter which
results in insufficient experimental data to archive one of the objectives and that is to recognize
the impact of different calibrations onto the volume measurements. In order to avoid similar
scenario to happen in the future, one should read the procedure thoroughly and highlight the
keywords on the manual thus to prevent from skipping any steps. Besides that, the results obtained
for volume measurement of pipette are opposite of what the theory stated indicates that there could
be a potential human error happen during the measurement. This could stem from the parallax
error whereby the experimenter failed to read the scale on eye level. To avoid such issue, one must
ensure that the scale is perpendicular to the observer’s eyes and the meniscus must reach to the
desired value before proceeding to the next step. A minor mistake that done by the experimenter
is to record the unit wrongly. In this experiment, the unit for volume used is millilitre (ml),
nonetheless, the experimenter used cm3 instead when recording the data in the jotter book. For
future reference, one should be consistent with the unit to avoid any miss interpretation of data
occur. Another thing that the experimenter should be aware of is that the measurement should be
recorded in 2 decimal places and above in order to ensure that the results are accurate.
 Moving to the safety element, during this experiment, the calibration liquid is seemed to
be a harmless coloured yellow water. However, when it is shaken vigorously, the colour
immediately turns into green colour solution which indicates that there are some chemical
reactions took place when it is being shaken. When the experimenter stop shaking the flask, the
colour turns back to the original state. This shows that as harmless as a solution might look like, it
may still be a potential threat to the handler. One should not be fooled by the appearance the
solution and should handle all chemicals equally cautious to ensure a safe and clean operation.

Conclusion

Based on the discussion above, 10 ml is the most accurate volume measurement for both
graduated pipette and measuring cylinder with minimal relative error compared to 5 ml, 2 ml and
1 ml. On the other hand, the volume transferred by pipette is most accurate followed by volume
contained by measuring cylinder and lastly, theoretically, the volume transferred by measuring
cylinder is the least accurate among the three volume measurements. Unfortunately, due to lack of
experimental data, the actual comparison among the three volume measurements was not able to
be done; hence, the first objective is said to be unable to achieve. On the other hand, the second
objective is to be aware of safe and clean operation in chemical laboratory. This objective was
achieved because, the change in colour of the calibration liquid has perfectly demonstrated the
important of handling an unknown liquid with caution as the appearance of the liquid does not
provide any information as to how dangerous it could be.

References

• SIC 1011 Safety and Basic Laboratory Techniques Lab-Manual

• http://beta-
static.fishersci.com/content/dam/fishersci/en_EU/suppliers/Brand_in_Wertheim/PDFs/V
olumetric/Brochuere_Volumenmessung_EN.pdf
• https://findanyanswer.com/what-is-the-difference-between-td-and-tc