Inorganic Chemistry Laboratory (CHEM 1204 LAB)

Department of Chemistry
-1-

CALIBRATION OF VOLUMETRIC GLASSWARE

Santiago, Rose Angelyn G., Antonio, Sofia M. Cueva, Loissa M. Gabriel, Erica O., Nilo, Juliana Mae, P.

Abstract: The purpose of the experiment of calibration of volumetric glassware is to calibrate

certain measurement by using volumetric glassware. The calibration was done by measuring the
mass of water contained in or delivered by the glassware. The density of water at a particular
temperature which is measured is used to convert mass into volume. Pipettes is calibrated to deliver
specific volumes whereas volumetric flasks are calibrated on a contain basis. For the accuracy and
precision of the measurement, scientists need to calibrate their volumetric glassware periodically.
For the calibration of 250 mL volumetric flask wherein the results were increased from Trial 1 to
Trial 2 but decreased from Trial 2 to Trial 3. Next is the calibration of 5 mL volumetric pipet
experiment, the results were increased from Trial 1 to Trial 3. For the calibration of 50 mL burette,
the results were decreased from Trial 1 to Trial 3. When the results are compared to the theory, the
students concluded that the results obtained in this experiment were not accurate but precise. It is
not accurate because of the different factors from the surrounding that causes. But then, the results
are precise because all the measurement recorded shows the same results and have relatively low
standard deviation. However, since there are some errors that occur during the experiment, the
results obtained were not accurate as it is expected to be. Some of the errors were first, errors
occurred during measurement of glassware on the top loading balance. Second, the glassware may
not be thoroughly dried and cleaned. Third, was the occurrence of parallax error during
measurement of the water in the glassware.

Keywords: Oxidation, reduction mixture, sulfur, acid, base, combustion, heating, bottom, litmus paper, reaction,
product

1. Introduction reaction method. The general procedure is to balance the

Electrochemistry constitutes one of the most
important interfaces between chemistry and everyday life
(Zumdahl, 2012). Electrochemistry is best defined as the
study of the interchange of chemical and electrical energy. It
is primarily concerned with two processes that involve
oxidation–reduction reactions.
An oxidation-reduction (redox) reaction is a type of
chemical reaction that involves a transfer of electrons
between two species. An oxidation-reduction reaction is any
chemical reaction in which the oxidation number of a
molecule, atom, or ion changes by gaining or losing an
electron. Redox reactions are common and vital to some of
the basic functions of life, including photosynthesis,
respiration, combustion, and corrosion or rusting. (Priya,
2014)
Most oxidation-reduction processes involve the
transfer of oxygen atoms, hydrogen atoms, or electrons.
Those were the three major classification of redox reaction.
Describing the redox reaction processes conveys no
information about the mechanism by which changes take
place. Redox processes are defined as reactions accompanied
by oxidation-state changes wherein an increase in an atom’s
oxidation corresponds to an oxidation while a decrease
corresponds to a reduction.
Moreover, oxidation–reduction reactions can occur
in basic solutions (the reactions involve OH- ions) as well as
in acidic solutions (the reactions involve H+ ions). One
method that can be used to balance redox reaction is the half-
equations for the half-reactions separately and then to add
them to obtain the overall balanced equation. The half-
reaction method for balancing oxidation–reduction equations
differs slightly depending on whether the reaction takes place
in acidic or basic solution. (Brown, 2012)
In this laboratory experiment, the three types of
glassware typically used by an analytical chemist: a
volumetric flask, volumetric pipet and burette will be
calibrated. These tools are used extensively when performing
gravimetric and titrimetric Analyses. In order to avoid
introducing systematic errors into measurements, each of
these instruments must be properly calibrated. And, to reduce
the random errors inherent when using these instruments,
their proper use must be thoroughly understood. The quality
of the measurements obtained from these tools depends
heavily on the care taken in calibrating and in using each
instrument.
2. Materials and Methods
2.1 Source of Materials
The materials needed in the experiment are mostly
provided by the laboratory including the reagents and
laboratory glass wares and equipment.
2.2 Calibration of Volumetric Flask
First, a volumetric flask was cleaned thoroughly and
dried until as much water as possible was removed from the
flask by inverting it and allowing it to drain for about ten
 Principle of Chemistry Laboratory (CHEM 1102 LAB)
Department of Chemistry
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3. Results and Discussion 3.3 Calibration of Burette
3.1 Calibration of Volumetric Flask
Table 3. Data gathered in the calibration of burette by
Table 1. Data gathered in the calibration of 250 mL transferring 10 mL of water in an Erlenmeyer flask
volumetric flask Trial 1 Trial 2
Trial 1 Trial 2 Trial 3 Initial mass (g) 148.982 g
Initial mass
120.403 g Mass of
(g)
Erlenmeyer with 158.744 g 159.263 g
Mass of flask H2O (g)
357.942 g 358.058 g 358.233 g
with H2O (g)
Mass of H2O 9.762 g 10.281 g
Mass of H2O
237.539 g 237.655 g 237.830 g
(g)
Temperature (˚C) 28.5 ˚C 28.5 ˚C
Mean (g) 237.675 g
Temperature
30˚C 30˚C 30˚C
(˚C) Apparent Volume 9.90 mL 10.00 mL
Volume (mL) 236.398 mL
True Volume 9.715 mL 10.232 mL
SD ±0.14649
Relative
54.408 ppt Difference ̶ 0.185 mL + 0.232 mL
Error
Mean Apparent
As indicated in the table above, the volume of a 9.95 mL
Volume
volumetric flask was calculated using the given value of 1
gram of water at a specific temperature. Since the SD ± 0.07
temperature of water in the three trials was 30˚C, the volume
of 1 gram of water is 1.0054 mL. Using stoichiometry, the
calculated volume is

3.2 Calibration of Volumetric Pipette

Table 2. Data gathered in the calibration of pipette through Table 4. Data gathered in the calibration of burette by
weighing the water in an Erlenmeyer flask transferring 20 mL of water in an Erlenmeyer flask
Trial 1 Trial 2 Trial 3 Trial 1 Trial 2
Initial mass Initial mass (g) 148.982 g
146.427 g
(g)
Mass of
Mass of flask Erlenmeyer with 169.095 g 169.373 g
152.186 g 157.837 g 163.413 g
with H2O (g) H2O (g)
Mass of H2O
5.759 g 5.651 g 5.576 g Mass of H2O 20.113 g 20.391 g
(g)
Mean (g) 5.662 g
Temperature (˚C) 28.5 ˚C 28.5 ˚C
Temperature
28.3˚C 28.5˚C 28.5˚C
(˚C)
Apparent Volume 20.10 mL 20.20 mL
Volume (mL) 5.635 mL
SD ±0.092
True Volume 20.02 mL 20.29 mL
Relative
126.99 ppt
Error
Difference ̶ 0.08 mL + 0.09 mL
Mean Apparent
20.15 mL
Volume
SD ± 0.07
 Principle of Chemistry Laboratory (CHEM 1102 LAB)
Department of Chemistry
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Table 5. Data gathered in the calibration of burette by Mass of
transferring 30 mL of water in an Erlenmeyer flask Erlenmeyer with 198.752 g 198.787 g
Trial 1 Trial 2 H2O (g)
Initial mass (g) 148.982 g Mass of H2O 49.770 g 49.805 g
Mass of
Temperature (˚C) 28.5 ˚C 28.5 ˚C
Erlenmeyer with 179.217 g 179.294 g
H2O (g)
Apparent Volume 50.00 mL 50.00 mL
Mass of H2O 30.235 g 30.312 g

Temperature (˚C) 28.5 ˚C 28.5 ˚C True Volume 49.53 mL 49.57 mL

Apparent Volume 30.20 mL 30.35 mL Difference -0.47 mL -0.43 mL

Mean Apparent
39.73 mL
True Volume 30.09 mL 30.17 mL Volume
SD ± 0.035
Difference -0.11 mL -0.18 mL
Mean Apparent
30.28 mL
Volume
Aliquots (Correction values vs.
SD ± 0.106
Apparent Volumes)
Table 6. Data gathered in the calibration of burette by 0.3
transferring 40 mL of water in an Erlenmeyer flask 0.2
Trial 1 Trial 2 0.1
Initial mass (g) 148.982 g 0
-0.1 Trial 1 Trial 2
Mass of
Erlenmeyer with 188.807 g 188.915 g -0.2
H2O (g) -0.3
Mass of H2O 39.825 g 39.933 g -0.4
-0.5
Temperature (˚C) 28.5 ˚C 28.5 ˚C -0.6

10 mL 20 mL 30 mL
Apparent Volume 39.70 mL 39.75 mL
40 mL 50 mL

True Volume 39.63 mL 39.74 mL Figure 1. Apparent volume of the water from 10-50 mL
respectively with respect to the correction values
Difference -0.07 mL -0.01 mL
Mean Apparent
39.73 mL
Volume
SD ± 0.035

Table 7. Data gathered in the calibration of burette by

transferring 50 mL of water in an Erlenmeyer flask
Trial 1 Trial 2
Initial mass (g) 148.982 g