CHM421:

ANALYTICAL CHEMISTRY

EXPERIMENT 1:

CALIBRATION OF A VOLUMETRIC FLASK

NAME : FARZANA BT MOHD SANUSI

STUDENT ID : 2017157363
GROUP : ED2605A
DATE OF EXPERIMENT : 3rd MARCH 2020
DATE OF SUBMISSION : 10th MARCH 2020
NAME OF LECTURER : DR. KHAIRIL ANUAR BIN JANTAN

ABSTRACT:
This experiment is aimed at calibrating volumetric flask and determining the new calibration
mark of the volumetric flask. This can be done by comparing its volume capacity with the
calculated volume of the liquid contained. Based on the comparison and calculation, the new
calibration mark can be determined. The theoretical volume was determined by dividing the
mass liquids with its reference density at a specified temperature. The correction factor was
obtained which is 0.04mm. From this correction factor, it is known that the volumetric flask
contained lesser than the actual volume. With this condition, it can lead to an error during the
reading of the measurement. Thus the calibration method is important and useful in
producing reliable, accurate and repeatable measurements.

OBJECTIVE:

1. To calibrate a used volumetric flask.

2. To determine the new calibration mark of the volumetric flask.

INTRODUCTION:

Volumetric flask is one of the example for the volumetric glassware. Other examples
are graduated cylinder, pipettes and burettes. Volumetric glassware is placed under the class
of glass vessel that go through the process of calibration. According to Chowdhury, M.
(2012), as stated in the International Vocabulary of basic and general terms in metrology,
calibration means the establishment of the set of operation under specified conditions.
According to Philip, S. D. et al (2001), calibration has a concept that is associated with the
statement that related with accuracy of a standard, gauge or measuring instrument. Moreover,
the calibration of the volumetric glassware is necessary to contain or to deliver the certain
amount of volume of the substances. According to the manufacturer, most of the measuring
instrument or measures usually are adjusted not calibrated within specified tolerances. It is
because liquids and glass can expand or contract when the temperature is increasing or
decreasing. Besides, all these volumetric glassware must always be calibrated to avoid errors
in measurements. It is because all these glassware is extensively used in performing
gravimetric and titrimetric analysis. For a better and precise result, the volume delivered by
or contained by these glassware must never be assumed correctly. In this experiment,
volumetric flask will be calibrated by determining the differences of the mass between the
filled and empty volumetric flask. It is done to correct the error encountered based from the
changes that has been occurred by the glassware in the morphology of the glassware itself.

METHOD:

The volume of 200 ml of distilled water was measured and equilibrated. Then, the 200
ml of distilled water was transferred into a clean beaker and was let to stand at room
temperature for about 10- 15 minutes. Onto a clean and dried 100 ml volumetric flask, a
sticker was pasted at the centre of the calibrated mark on the flask. Then, the volumetric flask
was weighed accurately. After the 15 minutes has ended, the room and the equilibrated water
temperature was measured before proceeding to the next step. Then, the flask was filled up
until the calibrated mark with the equilibrated distilled water. After that, the weight of the
water in the flask was converted into volume by using the table provided in the lab manual.
Next, a new mark was made on the calibrated mark as after the calculation, the volume in
flask is less than the standard volume which is 100 ml. The range of the new mark is between
5 mm each at both side (up and bottom) from the original calibrated mark. After the addition
of the new mark, more distilled water was added until it reach the new mark. One again, the
filled volumetric flask was weighed and the new volume was calculated with the same
method as before. The exact distance for the new mark to be was determined by using the
ratio of volume and distance.

DATA/ RESULTS:

Temperature of the room (̊C) 24 ̊C

Temperature of equilibrated water (̊C) 24 ̊C
Weight of dry 100 ml volumetric flask (g) 54.74 g
Weight of volumetric flask + distilled water 154.22 g
at current 100 ml mark (g)
Weight of volumetric flask + distilled water 154.95 g
of 5 mm mark (g)

CALCULATION/ANALYSIS:
DISCUSSION:
 Volumetric flask is one of the volumetric glassware that have a function to prepare a
Standard Solution or to dilute a sample. It is calibrated To -Contain (TC) a given volume of
liquid. Generally, the calibration of the volumetric glassware is by measuring the mass of
water that is contained- in or delivered- by the device. As for the volumetric flask, it is
calibrated by measuring the mass of water that is contained in-.

Based from the calculation, firstly, the mass data obtained between the empty and
filled volumetric flask is converted to volume data by using the table of the density of the
water at the temperature of calibration from the lab manual. Then, the same method of
calculation is repeated but this time the mass data is obtained between the filled volumetric
flask and the filled volumetric flask + new mark. Lastly, the true value of the calibrated mark
is obtained by calculation of ratio between the mass data of filled volumetric flask and filled
volumetric flask + new mark. The result obtained which is 4.96 mm is then subtracted from 5
mm. 5mm is the range of new calibrated mark from the original calibrated mark. With the
result obtained from the subtraction which is 0.04mm, the volume data can be corrected to
the standard temperature. It can be said that the correction factor of the volumetric flask is
0.04 mm. From the correction factor, it means that the volumetric flask can contained more
actual volume than it was expected to contain. In addition, it can be prove that the original
calibrated mark is not accurate. The calibrated mark of the volumetric flask need to be raised
for about 0.04 mm from the original mark. There are many reasons that can cause the
inaccuracy of the volumetric glassware, in this case volumetric flask. According to Rahman,
M. A., (2015), the inaccuracy is because of the temperature that can affect the sensitivity of
balance and volume of the volumetric glassware. It can be said that the temperature have a
major role on the calibration process of the volumetric glassware. The reason is because the
glass material has a characteristics that can expand or shrink when there is a changes in
temperature. However, different types of glass have different expansion coefficient.
However, the correction factor value is considerably low and not really that inaccurate in
term of the measurement. The reason to this is because all the volumetric flask is new and not
really been using in the laboratory. So, that’s why it still have a lower value of correction
factor.
 Based from the experiment, there are also some errors encountered during handling
the volumetric flask that can affect the data obtained. There are two types of error that can
happened during the experiment. The first error is human error. This type of error is usually
occur which is the parallax error from the incorrect lines of sight. To overcome this error,
during the measurement of the volumetric flask, make sure the eye level is not parallel to the
meniscus of the calibration mark. The second error that could happened is instrumental error.
This type of error can happened during the weighing process by using the analytical balance.
It is because of the improper location of the balance as it is placed on the lab table. The error
can occurred when other student intentionally leans on the table. However, it can be
overcome by make sure no other person is near to balance when the glassware being weighed
to minimize the vibration.

CONCLUSION:

As a conclusion, the calibration of the volumetric glassware, can be done by

determining the correction factor from the standardized set of a signal which is from the
density of water at specified temperature. This can be achieved from the standardized volume
and calibrated balance differences. From the calibration process, more accurate result can be
obtained for the instrument being analyzed and in this experiment volumetric flask was used.
Form the experiment, the volumetric flask undergo calibration process and yielded a
correction factor of 0.04 mm. Based on the result, it is meant that the glassware only can
contain a lesser amount of the actual volume than it was expected to contain which is 100 ml.
Thus, the measure volume of the volumetric flask without the calibration is actually lesser
than the actual volume. Conclusively, it is an important procedure to calibrate the volumetric
glassware to achieve a reliable, accurate and repeatable measurements.
REFERENCES:

1. Chowdhury, M. (2012). General Concept of Calibration. International Journal of

Pharmaceutical and Life Sciences, 1(3). https://doi.org/10.3329/ijpls.v1i3.12981
2. Phillips, S. D., Estler, W. T., Doiron, T., Eberhardt, K. R., & Levenson, M. S. (2001).
A Careful Consideration of the Calibration Concept. Journal of research of the
National Institute of Standards and Technology, 106(2), 371–379.
https://doi.org/10.6028/jres.106.014
3. Rahman, M. A. et al (2015). Source of Uncertainty Estimation of Analytical Balance
and Volumetric Glassware Calibration. World Applied Sciences Journal, 33 (11):
1740- 1745. DOI: 10.5829/idosi.wasj.2015.33.11.15618
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