EXPERIMENT 1

CALIBRATION OF VOLUMETRIC GLASSWARE

1.1 Learning Outcomes

At the end of the experiment, students should be able to:

(a) calculate the percentage error of measurements using various types of basic
laboratory glassware.
(b) calculate the accuracy of measurements using various types of basic laboratory
glassware.
(c) calculate the precision of measurements using various types of basic laboratory
glassware.

1.2 Introduction

Glass apparatus used to measure the volume of liquid or gas is called volumetric glassware. For
quantitative analysis of scientific experiments, the apparatus that you choose will depend on the
volume of the liquid and how precise you need to be. Ability to precisely measure volume of the
solution is crucial for the accuracy of chemical analysis. The volume of liquids needs to be
measured to exact amounts. For some experiments, being off by a few milliliters could alter the
result. Scientist needs the right tool for measuring the volume of liquid. This experiment will focus
on the volumetric glassware that you can use to accurately measure liquid volume. The apparatus
used are beaker, pipette, and burette. It will also emphasize the importance of significant figures
in expressing the precision of your volume measurements. Also, you are limited by the accuracy
of your measuring instruments for each measurement. It is possible to calculate the limits of
accuracy of different measuring instruments. Some errors which are not quantifiable also occur
in experiments. In this case, you cannot calculate their exact effect. For instance, you may not be
able to calculate heat losses in a thermochemical experiment.

1.2.1 Measuring Volumes

Volume of a liquid can be measured using a:

(a) beaker
(b) graduated pipette
(c) burette

1.2.1.1 Beakers

Beakers are designed to hold a particular amount of liquid and are not designed to accurately
measure volumes of liquids. If an approximate volume is needed with little accuracy, a beaker
may be used to contain the liquid. Beakers come in various sizes with different calibrations. An
examination of the 100 mL beaker shown reveals calibration lines every 10 mL between 20 and
80 mL. These measurements have a ± 5% error and are therefore approximations.
1.2.1.2 Graduated Pipettes

Pipettes are more accurate than beakers. Most pipettes are made to an accuracy of one drop if
they are used correctly. The volume of one drop is 0.05 ml. A 10 mL pipette has an error of ± 0.05
mL in 10 mL. The percentage error is 0.05/10 x 100 = 0.5%.

1.2.1.3 Burettes

Burettes are more accurate than beakers. They have graduations every 0.1 mL, so when you take
a reading, it should not be more than 0.05 mL too high or too low. However, when you use a burette
you take a reading at the start and at the end, so you have two errors of 0.05 mL i.e. total error =
0.10 mL. If you are using your burette to do a titration there may be another error of one or two
drops which is due to your judgement of when the indicator changes colour. This means that in a
titration (as opposed to just using a burette as a dispenser) you may have an error of 0.2 mL.

1.2.2 Calibrating Glassware

Calibration is the process by which a stated measure such as the volume of a container is checked
for accuracy. We can calibrate the glass by measuring the real volume of solution delivered or
contained by weighing mass of the water. By knowing the density of water (Table 1), we can
calculate the volume of the given water mass and the exact capacity of the glassware can be
determined. However, a relatively small change in temperature causes a change in the liquid’s
volume and thus its density. To calibrate the glassware, we need an electronic analytical balance,
distilled water of known temperature.

The glassware is calibrated either to contain (TC) or to deliver (TD) the stated volume. To
indicate this difference, volumetric glassware is normally marked TC or TD. For example, beakers
and conical flasks are designed to contain a certain volume of liquid and these are marked as TC.
Most pipettes (exception for micropipettes) and burettes are calibrated to deliver.

In calibrating the beaker, what you need to know is how much liquid is contained when the
glassware is filled to a given mark. Therefore, the mass of the empty container must be subtracted
from the mass of the container plus the liquid in order to determine the mass of liquid in the
container. The volume contained is then calculated using the density dimension.

Density () = Mass / Volume

Volume = Mass / Density
1.2.3 Apparatus

100 mL beaker, 25 mL graduated pipette and filler, 50 mL burette, thermometer, analytical

balance, dropper and kimwipes.

1.2.4 Chemicals

Distilled Water

1.2 Procedure

1.3.1 Beaker Calibration

Please click https://www.youtube.com/watch?v=4eUwHDaRqEM. Please watch the video
and complete the calculations.

(a) Weigh a clean and dry 100 mL beaker using an electronic balance.
(b) Record the reading in Table 2.
(c) Remove the beaker from the balance and fill the beaker with distilled water to the 50
mL mark.
(d) Reweigh the beaker and the water.
(e) Measure and record the temperature of the water.
(f) Dry the beaker with a paper towel and repeat the entire process for 3 times.

1.3.2 Pipette Calibration

Please click https://www.youtube.com/watch?v=zIHXxCIL6ps. Please watch the video
and complete the calculations.
.

(a) Measure and record the temperature of the water.

(b) Record the weight of the conical flask and stopper.
(c) Fill the pipette with distilled water and adjust the pipette volume to the calibration mark.
(d) Drain the water from the pipette into the conical flask.
(e) Place the conical flask and stopper containing the aliquot (water) on the balance
pan.
(f) Record the weight of the conical flask and stopper in Table 3.
(g) Remove the conical flask from the balance.
(h) Repeat the procedure (d) – (f) for another 2 times.

1.3.3 Burette Calibration-

Please click https://youtu.be/eSJmVrB8520. Please watch the video and complete the
calculations.

(a) Clean and rinse burette, beaker, funnel and other apparatus needed for this
experiment several times with distilled water and make sure to dry it.
(b) Pour some water into the beaker and put a thermometer into the beaker for at least
10 mins before taking the temperature. Record the temperature after 10 mins.
(c) Fill the burette with distilled water and carefully draw the liquid down to exactly 0.0
mL. Be sure that there are no air bubbles on the inner wall and at the tip of the
burette, and no water drop hanging at its tip.
(d) Weigh a clean and dry 100 mL beaker and record its weight in Table 4.
(e) Put the beaker underneath the burette’s tip and drain the water in the burette from
0.0 mL till the mark at 50.0 mL.
(f) Weigh and record the beaker filled with water.
(g) You will have to repeat the procedure from step (c) till (f) for 3 times.
 Table 1: Density of water at different temperatures

Temperature (°C) Density (g/mL) Temperature (°C) Density (g/mL)

19 0.9984 27 0.9955
20 0.9982 28 0.9952
21 0.9980 29 0.9949
22 0.9966 30 0.9944
23 0.9964 31 0.9941
24 0.9962 32 0.9940
25 0.9959 33 0.9938
26 0.9957 34 0.9935

RESULTS – EXPERIMENT 1

Table 2: Beaker

Trial 1 Trial 2 Trial 3

Weight of empty beaker (g) 48.0 48.1 48.2

Weight of beaker + water (g) 92.5 93.0 93.5

Weight of water (g)
Temperature of water (°C) 30.0 30.0 30.0
Density of water (g/mL)
Volume of water (mL)
Average volume of water (mL)

Table 3: Pipette

Trial 1 Trial 2 Trial 3

Weight of empty conical flask 46.4763 56.4489 57.5889
with stopper (g)
Weight of conical flask with 56. 4489 66.4156 67.5557
stopper + water (g)
Weight of water (g)
Density of water (g/mL)
Temperature of water (°C) 22.0 22.0 22.0
Volume of water (mL)
Average volume of water (mL)

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Table 4: Burette

Trial 1 Trial 2 Trial 3

Weight of empty beaker (g) 54.25 54.25 54.25
Weight of beaker + water (g) 104.23 104.13 103.99
Weight of water (g)
Temperature of water (°C) 22.0 22.0 22.0
Density of water (g/mL)
Volume of water (mL)
Average volume of water (mL)

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1.4 Calculations

1. Calculate the volume of water in the beaker, pipette and burette.

Trial 1 Trial 2 Trial 3

Beaker (mL)

Trial 1 Trial 2 Trial 3

Pipette (mL)

Trial 1 Trial 2 Trial 3

Burette (mL)

2. Calculate the average volume of water in the glassware.

Beaker (mL)

Pipette (mL)

Burette (mL)

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 3. Calculate the percent error to determine the accuracy of the volumetric
apparatus.

Beaker

Pipette

Burette

4. Calculate the standard deviation of each glassware to determine the precision

of the measurements

Using formula

Beaker

Pipette

Burette

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1.5 Questions

1. Explain the terms ‘precision’ and ‘accuracy’. How do they differ?

Precision Accuracy

2. Identify the statistical methods used to estimate the precision and accuracy
in this experiment.