ANALYTICAL CHEMISTRY

CHM 421

EXPERIMENT 1:

CALIBRATION OF A VOLUMETRIC FLASK

NAME MUHAMMAD ARIF BIN CHIK

STUDENT ID 2023699552
LECTURER NAME NUR VICKY BINTI BIHUD
EXPERIMENT DATE 26 MARCH 2024
ABSTRACT

Calibration can be defined as the act or process of determining, checking, or rectifying the
settings or gradations on a measuring instrument or other piece of precision equipment. To
simply put, calibration was carried out to make sure that we can used the equipment very
precisely with little to no error existed. Hence, we need to calibrate the glassware that were
commonly used in the laboratory. In this experiment, we want to find out the exact
measurement for volumetric flask by using 100 mL volumetric flask. To start the experiment,
a clean and dry 100 mL volumetric flask was prepared. The volumetric flask was handled
carefully to prevent any errors. Then, the volumetric flask was weighed, and a sticker was
pasted at the centre of the 100 mL mark. After that, the volumetric flask was filled with distilled
water until it reached the mark so that it can be weighed for the second time. It is important to
note that the weight of the water must be converted into volume to determine the actual volume
of the volumetric flask at room temperature. A new sticker was pasted 5 mm above or below
the present mark depending on whether the volume is more or less than the standard volume.
The volumetric flask was then weighed again for the last time after adding or reducing the
water according to the new mark, and the new volume was calculated using the ratio of volume
and distance.

OBJECTIVES

1. To calibrate a used volumetric flask.

2. To determine the new calibration mark for the volumetric flask.
INTRODUCTION

Reading error or tolerance for a 100 mL volumetric flask is ± 0.1 mL. Any 100 mL volumetric
flask with volume exceeding this tolerance needs to be calibrated. Calibration is an important
process because it ensures apparatus to contain or deliver good, accurate volume. In this
experiment, you will learn how to calibrate a volumetric flask in the laboratory. The same
procedure can be applied to other volumetric glasswares such as pipette and burette.

Volumetric glasswares must be calibrated by measuring the mass of a liquid (usually

mL water) of known density and temperature that is contained in (or delivered by) the
volumetric glassware. The weight obtained must be corrected for buoyancy since the density
of water is quite different from that of the standard weights of the analytical balance.

The calculations for the calibration are quite involved. First, the weighing data are
corrected for buoyancy. Next, this data is converted to the volume of the apparatus at the
temperature of calibration (T) by dividing the density of the liquid at that temperature. Finally,
this volume is corrected to the standard temperature of 20℃.

Use the table provided in your calculation for calibration. This table has already
incorporated the buoyancy error for stainless steel or brass weights (the density difference
between the two is very small that they can be neglected) and for the volume change of water
and of glass containers. Choose the factor at the appropriate temperature and multiply it with
the mass of water at temperature T to convert it to the corresponding volume at that temperature
or the volume at 20℃.
PROCEDURE

1. 200 mL of distilled water was equilibrated. The 200 mL distilled water was placed in a
clean beaker to let it stand at room temperature for 15 minutes.
2. A 100 mL volumetric flask was cleaned and dried. A sticker with about 2 cm was pasted
onto the 100 mL mark of the flask, letting the mark of the flask to be at the centre of
the sticker. The weight of the volumetric flask was determined accurately.
3. After 15 minutes, the temperature of the room and the equilibrated water was measured.
The two temperatures should be agreed before proceeding to the next step.
4. The flask was filled with equilibrated distilled water up to the mark. Dropper was used
towards the end. Then, the flask was weighed again accurately.
5. The weight of the water in the flask was converted into volume using the data provided
in the table.
6. If the volume is less than the standard volume which is 100 mL, a new mark on the
sticker was made 5 mm above the present mark on the volumetric flask. But, if the
volume is more than the standard volume, a new mark was made 5 mm below the
present mark.
7. Water was added or reduced to the new mark which has just been made. Then, the
volumetric flask was weighed again, and the new volume was calculated.
8. The exact distance for the new mark to be determined by using the ratio of volume and
distance, so that the volume of the flask is accurate.

DATA

Temperature, ℃ Volume 1.00 g Temperature, ℃ Volume 1.00 g

water, mL Water, mL
20 1.0028 27 1.0043
21 1.0030 28 13.0046
22 1.0032 29 1.0048
23 1.0034 30 1.0051
24 1.0036 31 1.0051
25 1.0038 32 1.0067
26 1.0041 33 1.0060
Data 1

Temperature of the room = 24℃

Temperature of the equilibrated water = 24℃

Weight of dry 100 mL volumetric flask (w1) = 52.3620 g

Weight of volumetric flask + H2O (at current 100 mL mark), (w2) = 151.5936 g

Weight of H2O (w3) = 99.2316 g

Weight of volumetric flask + H2O (at 5 mm mark), (w4) = 152.2029 g

Data 2

Temperature of the room = 28℃

Temperature of the equilibrated water = 28℃

Weight of dry 100 mL volumetric flask (w1) = 52.8534 g

Weight of volumetric flask + H2O (at current 100 mL mark), (w2) = 152.2365 g

Weight of H2O (w3) = 99.3831 g

Weight of volumetric flask + H2O (at 5 mm mark), (w4) = 152.9635 g

Data 3

Temperature of the room = 27℃

Temperature of the equilibrated water = 27℃

Weight of dry 100 mL volumetric flask (w1) = 64.5414 g

Weight of volumetric flask + H2O (at current 100 mL mark), (w2) = 164.7517 g

Weight of H2O (w3) = 100.3003 g

Weight of volumetric flask + H2O (at 5 mm mark), (w4) = 165.3884 g

Data 4

Temperature of the room = 28℃

Temperature of the equilibrated water = 28℃

Weight of dry 100 mL volumetric flask (w1) = 54.7842 g

Weight of volumetric flask + H2O (at current 100 mL mark), (w2) = 151.0579 g

Weight of H2O (w3) = 96.2737 g

Weight of volumetric flask + H2O (at 5 mm mark), (w4) = 151.7186 g

RESULTS AND CALCULATIONS

Weight of H2O at current 100 mL

= (Weight of volumetric flask + H2O (at current 100 mL mark)) – weight of dry 100 mL
volumetric flask

= 151.0579 g – 54.7842 g

= 96.2737 g

Volume of H2O at current 100 mL mark

= weight of H2O (at current 100 mL mark) X 1.0046

= 96.2737 g X 1.0046

= 96.7167 mL

Weight of H2O at 5 mm mark

= (weight of volumetric flask + H2O (at current 5 mm mark)) – weight of dry 100 mL
volumetric flask

= 151.7186 g – 54.7842 g

= 96.9344 g

Volume of H2O at 5 mm mark

= weight of H20 at 5 mm mark X 1.0046

= 96.9344 g X 1.0046

= 97.3803 mL

Volume of H2O

= 97.3803 mL – 96.7167 mL

= 0.6636 mL

5 mm = 0.6636 mL

1 mm = 0.1327 mL
DISCUSSION

In the experiment, the temperature for the room and the equilibrated water is 28℃. The weight
of the dry volumetric flask is 54.7842 g. The weight of the volumetric flask with water at 100
mL is 151.0579 g and weight of the volumetric flask with water at 5 mm is 151.7186 g.

The error that we encountered in this experiment was parallax error. We might have poured the
water in the volumetric flask lower or higher than the mark making the data not very accurate.

CONCLUSION

In conclusion, we had done the calibration for a volumetric flask to determine its new
calibration mark, which is 97.3803 mL. Some errors that happened during the experiment may
affect the new calibration mark that we obtained.

QUESTIONS

1. Why is calibration of glassware important?

Calibration is needed to ensure you are getting accurate results every time.

2. Which calibrated glassware is used in titration?

Burette and pipette.

REFERENCES

1) The Importance of Volumetric Glassware Calibration - NWI Weighing. (2021,

November 18). NWI Weighing. https://nwiweighing.com.au/the-importance-of-
volumetric-glassware-calibration/

2) Volumetric Glassware. (n.d.).

https://www.webassign.net/labsgraceperiod/tccgenchem1l1/glassware/manual.html