CHEM 109

Introduction to Chemistry
Revision 3.0

Laboratory Exercise: The Precision of Volume Measurements

The accurate measurement of the volume of liquids tends to be difficult and chemists have a
number of different types of devices for making this measurement; beakers, graduated cylinders,
volumetric flasks, etc. Each of these devices has a specific purpose and a distinct level of
accuracy and precision associated with it.

Beakers are used primarily for crudely measuring out large volumes of liquids, mixing reagents
and carrying out chemical reactions. The graduated markings on a beaker are only approximate,
so a beaker should never be used for accurate volume measurements. Graduated cylinders are
specifically designed to measure out liquid volumes. Their tall narrow design makes for a more
precise reading of the liquid level. If more precision is needed, a volumetric flask can be used.
These flasks typically measure a single volume via a single mark on a tall narrow neck. These
flasks are generally used for solution preparation.

Beaker Graduated Cylinder

In accurate work it is never safe to assume that the volume delivered by or contained in any
volumetric instrument is exactly the amount indicated by the calibration mark. Manufacturers
only guarantee the device is manufactured to within some prescribed tolerance. Instead,
recalibration is usually performed by weighing the amount of water delivered by or contained in
the volumetric apparatus. The mass measurement is then converted into a volume measurement
using the known density of Water. Mass measurements can be made much more accurately and
precisely than can volume measurements.

Volume = Mass / Density

The density of Water is well known and tabulated values are provided in the Appendix.

In addition to recalibrating the volumetric device for accuracy, we can make replicate
measurements of the volume contained in or delivered by the device in order to gain an
understanding of the precision of the device. The precision can be estimated as the Standard
Deviation for the replicate measurements, although other more conventional measures, such as
the Confidence Interval, based on the standard deviation determination, are more widely used.
In our case, we will calibrate two graduated cylinders. The precision of these cylinders will then
be compared.
Procedure
1. Obtain about 700 mL of Distilled Water in an 800 mL Beaker. This Water will be used to
calibrate our Graduated Cylinders. In each case, we will measure the mass of Water, as
measured by the device, five times.

2. Measure the temperature of the Water. This is needed because the density of Water is
temperature dependent.

3. Obtain a 10 mL and a 50 mL Graduated Cylinder. Thoroughly clean each with a test tube
brush and some Alconox cleaning solution. (Cleanliness of volumetric glassware is critical
to ensure its correct performance.) Water will wet the sides of clean glassware but will not
bead-up in drops.

4. Make a note as to whether the Cylinder is a To Contain (TC) or a To Deliver (TD) device.

To Contain devices, as the name implies, contain the stated amount of liquid when filled to the mark.

To Deliver devices deliver the stated amount of liquid into another container. Account is taken for any
liquid remaining wetted on the walls of the device after the delivery.

If the Cylinder is a To Contain device:

5. Completely dry the Cylinder and weigh it empty using an Analytical Balance. (Your
laboratory instructor will demonstrate the use of the balance. Do not use the balance until
you have been shown how to properly use it.)

6. Fill the Cylinder with Distilled Water to the top mark. Make sure no droplets of Water are
sticking to the walls above the Water level. If this is the case, use a piece of paper towel to
blot them up. Your laboratory instructor will demonstrate how to do this effectively.
Make sure your eye is on a level with the mark. A Paralax Error will result, otherwise.
This will lead to a reading that is either too high or too low. Always read the meniscus
from the bottom.
 Measure the mass of the Cylinder filled with Water.

7. Completely dry the Cylinder and repeat the measurements four more times.

8. Determine the mass of Water contained in the Cylinder for each trial and then use the
density to convert this to a volume reading.

If the Cylinder is a To Deliver device:

5. Obtain and completely dry a 50 mL Plastic Beaker and weigh it empty using an Analytical
Balance. (Your laboratory instructor will demonstrate the use of the balance. Do not use
the balance until you have been shown how to properly use it.)

6. Fill the Cylinder with Distilled Water to the top mark. Make sure no droplets of Water are
sticking to the walls above the Water level. If this is the case, use a piece of paper towel to
blot them up. Your laboratory instructor will demonstrate how to do this effectively.
Make sure your eye is on a level with the mark. A Paralax Error will result, otherwise.
This will lead to a reading that is either too high or too low. Always read the meniscus
from the bottom.

7. Transfer the measured amount of Water from the Cylinder to the Plastic Beaker. Measure
the mass of the Beaker filled with Water.

8. Completely dry the Cylinder and repeat the measurements four more times.

9. Determine the mass of Water delivered by the Cylinder for each trial and then use the
density to convert this to a volume reading.
Appendix - Density of Water

Temperature (oC) Density (g/mL)

10 0.9997026
11 0.9996084
12 0.9995004
13 0.9993801
14 0.9992474

15 0.9991026
16 0.9989460
17 0.9987779
18 0.9985986
19 0.9984082

20 0.9982071
21 0.9979955
22 0.9977735
23 0.9975415
24 0.9972995

25 0.9970479
26 0.9967867
27 0.9965162
28 0.9962365
29 0.9959478

30 0.9956502
Appendix - Tolerances for Class A Graduated Cylinders at 20oC

Capacity (mL) Tolerances (mL)

5 0.05
10 0.10
25 0.17
50 0.25
100 0.50
250 1.00
500 2.00
1000 3.00

The Tolerances for Class B cylinder is typically twice that of a Class A device. (ASTM E
1272-02)
Volume Measurements
o
Water Temperature C

Water Density g/mL

10 mL Graduated Cylinder
TC or TD

Class

Mass Empty g

Trial 1 Trial 2 Trial 3 Trial 4 Trial 5

Mass Filled g

Mass Water g

Volume mL

Average Vol. mL

Per. Error %

Std. Dev.* mL

Within Tol.

50 mL Graduated Cylinder
TC or TD

Class

Mass Empty g
 Trial 1 Trial 2 Trial 3 Trial 4 Trial 5

Mass Filled g

Mass Water g

Volume mL

Average Vol. mL

Per. Error %

Std. Dev.* mL

Within Tol.

Name: Date:

Signature:
Additional Points to Consider
You do not need to submit answers to these questions. However, you should seriously ponder the answers to
these questions as they could reappear on an exam.

 If you are always reading from below the mark, will your volume measurements be infected with a
systematic or random error? In this case, will the accuracy or the precision of your measurement
suffer? Explain.
 Most precise volume measuring devices have markings along a narrow neck? Why do you think this is
important?