EXPERIMENT 1.

LABORATORY TECHNIQUES

Objectives
• To learn the use of common, simple laboratory equipment.
• To become acquainted with procedures used in determining the densities of
objects and using these densities for identifying substances.

Introduction
Chemistry is an experimental science. It depends upon careful observation and the use
of good laboratory techniques. In this experiment you will become familiar with some
basic operations that will help you throughout this course. Your success as well as your
safety in future experiments will depend upon your mastering these fundamental
operations.
Because every measurement made in the laboratory is really an approximation, it
is important that the numbers you record reflect the accuracy and precision of the
device you use to make the measurement. Appendix B of this manual contains a
section on significant figures and measurements that you may find helpful in performing
this experiment.
Our system of weights and measures, the metric system, was originally based
mainly upon fundamental properties of one of the world's most abundant substances,
water.
In 1960 international agreement was reached, specifying a particular choice of
metric units in which the basic units for length, mass, and time are the meter, the
kilogram, and the second. This system of units, known as the International System of
Units, is commonly referred to as the SI system and is preferred in scientific work. A
comparison of some common SI, metric, and English units is presented in Table 1.1.

Table 1.1 Comparison of SI, Metric, and English Units

Quantity SI unit Common metric units Conversion Factors

Length Meter (m) Meter (m) 1 m = 102 cm = 39.37 inches

Centimeter (cm) 1 inch = 2.54 cm

Volume Cubic meter (m3) Liter (L) 1L = 103 cm3 = 10-3 m3 = 1.06 qt.
millileter (mL)

Mass Kilogram (kg) Gram (g) 1 kg = 103 g = 2.205 lb

Milligram (mg) 1 lb = 453.6 g

Energy Joule (J) Calorie (cal) 1 cal = 4.184 J

Temperature Kelvin (K) degree Celsius (EC) 0 K = -273.15EC

EC = 5/9 (EF - 32)

Expt. 1-1
 EXPERIMENT 1. LABORATORY TECHNIQUES

Laboratory Balance
A laboratory balance is used to obtain the mass of various objects. There are several
varieties of balances, with various limits on their accuracy. Two common kinds of
balances are depicted in Figure 1.1. These single-pan balances are found in most
modern laboratories. Generally they are simple to use, but they are very delicate and
expensive. The amount of material to be weighed and the accuracy required determine
which balance you should use.

Figure 1.1 Digital electronic balances. The balance gives the mass directly when an object to be weighed is
placed on the pan. (A) Analytical balance. (B) Top loader.

Graduated Cylinders
Graduated cylinders are tall, cylindrical vessels with graduations scribed along the side
of the cylinder. Since volumes are measured in these cylinders by measuring the height
of a column of liquid, it is critical that the cylinder have a uniform diameter along its
entire height. Obviously, a tall cylinder with a small diameter will be more accurate than
a short one with a large diameter.

Thermometers
Most thermometers are based upon the principle that liquids expand when heated. Most
common thermometers use mercury or colored alcohol as the liquid. These
thermometers are constructed so that a uniform-diameter capillary tube surmounts a
liquid reservoir. To calibrate a thermometer, one defines two reference points, normally
the freezing point of water (0EC, 32EF) and the boiling point of water (100EC, 212EF) at
1 atm of pressure (1 atm = 760 mm Hg = 1 torr). Once these points are marked on the
capillary its length is then subdivided into uniform divisions called degrees. There are

Expt. 1-2
 EXPERIMENT 1. LABORATORY TECHNIQUES

100E between these two points on the Celsius, (EC, or centigrade) scale and 180E
between those two points on the Fahrenheit (EF) scale.

Pipets
Pipets are glass vessels that are constructed and calibrated so as to deliver a precisely
known volume of liquid at a given temperature. The markings on the pipet illustrated in
Figure 1.2 signify that this pipet was calibrated to deliver (TD) 10.00 mL of liquid at
25EC. Always use a rubber bulb to fill a pipet. NEVER USE YOUR MOUTH! A TD pipet
should not be blown empty.
It is important that you be aware that every measuring device, regardless of what

Figure 1.2 A typical volumetric pipet, rubber bulbs, and the pipet filling technique.

it may be, has limitations in its accuracy. Moreover, to take full advantage of a given
measuring instrument you should be familiar with or evaluate its accuracy. Careful
examination of the subdivisions on the device will indicate the maximum accuracy you
can expect of that particular tool. In this experiment you will determine the accuracy of
your 10 mL pipet.
The approximate accuracy of some of the equipment you will use in this course is
given in Table 1.2.

Expt. 1-3
 EXPERIMENT 1. LABORATORY TECHNIQUES

Table 1.2 Typical Equipment Accuracy

Equipment Accuracy Equipment Accuracy

Analytical balance ± 0.0001 g Graduated cylinder ± 0.1 mL

Top-loading balance ± 0.01 g Pipet ± 0.02 mL

Thermometer ± 0.2 EC Buret ± 0.02 mL

Chemistry is distinctly an experimental science. The establishment of the

fundamental laws and theories of nature and behaviour of matter depends on the
careful measurement of various physical quantities such as mass, volume, length,
temperature, and time.
The determination of density requires measurements of two quantities: the mass
and the volume of a given amount of substance. The ratio of these two quantities, the
mass per unit volume, is called density:

mass (g)
density, ρ (g / ml) =
volume (mL)

In the metric system, this ratio can be expressed as g/mL, or g/cc, or kg/L.
The substances displayed in Figure 1.3 visually show the widely differing densities
of a variety of compounds. It is apparent that liquids and solids have much greater
densities than gases. Density is also influenced by temperature. The densities of liquids
and solids are affected only slightly by changes in temperature of the substance, but gas
densities are quite sensitive to temperature changes.
The density of a substance relative to that of pure water is called the specific gravity.
That is,
ρ of substance (g / mL)
Sp. grav. of substance =
ρ of pure water (g / mL)
Note that, in contrast to density which has units, specific gravity is a ratio and has no units.
Specific gravity is determined from measurements of the mass of a given volume of

Expt. 1-4
 EXPERIMENT 1. LABORATORY TECHNIQUES

Figure 1.3 The relationship of density to volume.

The cubes of different sizes represent the relative
volumes of equal weights (about 0.2 g) of the
various materials at 0EC.

substance, and the mass of an equal volume of pure water. For example, if 500 mL of
gasoline has a mass of 400 g, and 500 mL of water has a mass of 500 g, then

400
Sp. grav. of gasoline = = 0.800
500
For accurate specific gravity results, both water and substance must be at exactly
the same temperature.
The measurement of density (and relative density) is necessary for a variety of
important procedures in the science of chemistry. Examples include the calculation of
Avogadro’s number from unit-cell dimensions of crystals, the determination of the molecular
mass of a substance from its gas density, the conversion of hydrostatic pressure units, the
conversion from mass to volume, the measurement of densities of biopolymers in the
ultracentrifuge, and the determination of the concentration of a solute from density

Expt. 1-5
 EXPERIMENT 1. LABORATORY TECHNIQUES

measurements.
An understanding of density is also important outside the chemistry laboratory. For
example, the service station attendant determines the charge of an automotive battery by
measuring the density (and hence concentration) of the sulphuric acid solution in the
battery. Also, a wine maker (even the amateur who makes wine at home) measures the
density of the grape juice to determine whether the sugar content is sufficient for
fermentation.

PROCEDURE

A. The Thermometer and Its Calibration

This part of the experiment is performed to check the accuracy of your thermometer. These
measurements will show how measured temperatures (read from thermometer) compare
with true temperatures (the boiling and freezing points of water). The freezing point of water
is 0EC; the boiling point depends upon atmospheric pressure and is calculated as shown
in Example 1.1 at the end of this procedure.

1. Place approximately 250 mL of ice in a 400-mL beaker and cover the ice with
distilled water. Place a thermometer in a thermometer clamp and position it so that
the thermometer is submerged in the ice solution. Allow about 15 min for the
mixture to come to equilibrium and then measure and record the temperature of the
mixture. Theoretically, this temperature is 0EC.

2. Fill a 400 mL beaker about half full with distilled water and place it on a hot plate.
Begin heating the water to a boil. (Time can be saved if the water is heated while
other parts of the experiment are being conducted.) Periodically determine the
temperature of the water with the thermometer, but be careful not to touch the walls
of the beaker with the thermometer bulb. Record the boiling point (b.p.) of the water.

3. Using Example 1.1 but with the current atmospheric pressure, determine the true
boiling point at the observed atmospheric pressure. Obtain the atmospheric
pressure from your laboratory instructor.

4. Using graph paper , construct a thermometer-calibration curve similar to the one

shown in Figure 1.4 by plotting observed temperatures versus true temperatures for
the boiling and freezing points of water. Your graph should be more accurate and
have better scales than the one shown in the figure.

Expt. 1-6
 EXPERIMENT 1. LABORATORY TECHNIQUES

Figure 1.4. Typical thermometer-calibration curve.

Example 1.1
PROBLEM: Determine the boiling point of water at 659.3 mm Hg.
SOLUTION: Temperature corrections to the boiling point of water are calculated using the
following formula:
b.p. correction = (760 mm Hg - atmospheric pressure) X (0.037EC/mm)

The correction at 659.3 mm Hg is therefore

b.p. correction = (760 mm Hg - 659.3 mm Hg) x (0.037EC/mm) = 3.7EC

The true boiling point is thus 100.0EC - 3.7EC = 96.3EC

B. Using the Balance to Calibrate Your 10 mL Pipet

Weighing an object on a single-pan balance is a simple matter. Because of the
sensitivity and the expense of the balance (some cost more than $2500) you must be
careful in its use. Directions for operation of single-pan balances vary with make and
model. Your laboratory instructor will explain how to use the balance. Regardless of the
balance you use, proper care of the balance requires that you observe the following:

• Do not drop an object on the pan.

• Center the object on the pan.
• Do not place chemicals directly on the pan; use a beaker, watch glass, weighing
bottle, or weighing paper.
• Do not weigh hot or warm objects; objects must be at room temperature.

Expt. 1-7
 EXPERIMENT 1. LABORATORY TECHNIQUES

• Clean up any chemical spills in the balance area.

• Inform your instructor if the balance is not operating correctly; do not attempt to
repair it yourself.

Procedure
1. Obtain about 40 mL of distilled water in a 150-mL beaker. Measure and record
the temperature of the water.

1. Weigh and record the mass of an empty, dry 50-mL Erlenmeyer flask (tare) to the
nearest 0.1 mg.

2. Using your pipet and rubber bulb, pipet exactly 10 mL of water into this flask and
weigh the flask with the water in it (gross) to the nearest 0.1 mg.

3. Obtain the mass of the water by subtraction (gross -tare = net). Using the
equation for density and the data given in Table 1.3, obtain the volume of water
delivered and therefore the volume of your pipet.

4. Repeat this procedure in triplicate, that is, deliver and weigh exactly 10 mL of
water three separate times.

Table 1.3 Density of Pure Water at Various Temperatures

T (EC) d (g/mL) T (EC) d (g/mL)

15 0.999099 22 0.99777

16 0.998943 23 0.997538

17 0.998774 24 0.997296

18 0.998595 25 0.997044

19 0.998405 26 0.996783

20 0.998203 27 0.996512

21 0.997992 28 0.996232

C. Determination of Density
You are to calculate the density of five objects: water, ethanol, and three metal
cylinders. Please record the unknown numbers (or colours) of the metals on the right-
hand side of your lab notebook and on your report sheet (remember that no unknown
number on your report means no mark!)

Expt. 1-8
 EXPERIMENT 1. LABORATORY TECHNIQUES

(I) Density of Water

1. Using the triple beam balance at your station, weigh a clean, dry, 10 mL
graduated cylinder. Record its mass, to two decimal places, in your data table on
the right-hand side of your notebook. If you do not remember how to use the
balance, then learn from the instructions in Appendix C, and jot down a summary
on the left-hand side of your notebook before you come to the lab.

2. Add water to your graduated cylinder until you have approximately 10 mL of

water. Read the volume of the water to the nearest 0.1 mL and record the
volume in your data table. Read and record the temperature of the water.

3. Find the mass of the (water + graduated cylinder) and record it in your data table.
Find the mass of the water by subtraction and record this also.

4. Compute the density of the water by dividing the mass of the water by its volume.
Report to the proper number of significant figures and write this in your data
table. Using the literature value for water density from Table 1.3 compute the %
Relative Error in your experimental result from the following formula:
(literature value - your value
% Relative error = x 100
literature value
5. Transfer your results to your report sheet.

(II) Density of Ethanol

1. Using the triple beam balance, weigh a clean, dry, 25 mL graduated cylinder.
Record its mass, to two decimal places, in your data table in your notebook (right-
hand side).

2. Add ethanol to your graduated cylinder until you have approximately 20 mL of

ethanol. Read the volume of the ethanol to the nearest 0.1 mL and record the
volume in your data table. Find the mass of the (ethanol + graduated cylinder) and
record it in your data table. Find the mass of the ethanol by subtraction and record
this also.

3. Compute the density of the ethanol and report it to the proper number of significant
figures in your data notebook. Look up the literature density of ethanol from the
CRC Handbook of Chemistry and Physics (located in the lab) and record this value

Expt. 1-9
 EXPERIMENT 1. LABORATORY TECHNIQUES

in your notebook. Compute the % Relative Error in your experimental result.

Transfer your results to your report sheet.

(III) Density of Metal

For each of the metal objects, the following procedure is used to determine the density.

1. Using the triple beam balance, weigh the metal cylinder and record its mass in your
data table in your notebook.

2. The volume of the metal cylinder is found by the volume displacement method
(Archimede’s Principle). Fill a 100 mL graduated cylinder to the 50 mL mark with
distilled water (use a dropper for the last few drops). Record this initial volume in
the data table.

3. Gently place the object into the graduated cylinder (avoid splashes by tilting the
graduated cylinder on an angle so that the object slides down the wall) and measure
the volume. Record this new volume. Subtract off the original volume to find out the
volume of the object.

4. Calculate the density of the metal and record the value in your notebook, to the
correct number of significant figures. Transfer your result to our report sheet.
Repeat the procedure for the other metal objects. Remember to record the
unknown numbers.

Clean up your station and have it inspected by your instructor.

Notes on precision:
The precision of a measurement is a statement about the internal agreement among
repeated results; it is a measure of the reproducibility of a given set of results. The
arithmetic mean (average) of the results is usually taken as the "best" value. The simplest
measure of precision is the average deviation from the mean. The average deviation is
calculated by first determining the mean of the measurements, then calculating the
deviation of each individual measurement from the mean and, finally, averaging the
deviations (treating each as a positive quantity). Study Example 1.2 and then, using your
own experimental results, calculate the mean volume delivered by your 10 mL pipet. Also
calculate for your three trials the individual deviations from the mean and then state your
pipet's volume with its average deviation.

Expt. 1-10
 EXPERIMENT 1. LABORATORY TECHNIQUES

Example 1.2
The following volumes were obtained for the calibration of a 10 mL pipet:
10.10, 9.98, and 10.00 mL. Calculate the mean value and the average deviation from the
mean.

SOLUTION:
. + 9.98 + 10.00
1010
mean = = 10.03
3
Deviations from the mean: *experimental value - mean value*
*10.10 - 10.03*= 0.07
*9.98 - 10.03*= 0.05
*10.00 - 10.03*= 0.03

Average deviation from the mean

0.07 + 0.05 + 0.03
= = 0.05
3
The reported value is therefore 10.03 ± 0.05 mL.

Expt. 1-11
 EXPERIMENT 1. LABORATORY TECHNIQUES

REVIEW QUESTIONS
You should be able to answer the following questions before beginning this experiment.
You do not have to hand these in. Consult your TA for answers or if you have problems.
1. What are the basic units of length, mass, volume, and temperature in the SI
system?
2. A liquid has a volume of 1.35 liters. What is its volume in mL? in cm3?
3. If an object weighs 1.47 g, what is its mass in mg?
4. Why should you never weigh a hot object?
5. Why is it necessary to calibrate a thermometer and volumetric glassware?
6. What is precision?
7. Define the term density. Can it be determined from a single measurement?
8. What is the density of an object with a mass of 9.03 g and a volume of
0.1987 mL?
9. Weighing an object three times gave the following results: 10.2 g, 10.1 g, and 10.3
g. Find the mean mass and the average deviation from the mean.
10. Normal body temperature is 98.6EF. What is the corresponding Celsius
temperature?
11. What is the mass in kilograms of 950 mL of a substance that has a density of 1.274
g/mL?

Expt. 1-12
 EXPERIMENT 1. LABORATORY TECHNIQUES

REPORT SHEET

Name: ________________________________________ date: _______________

Laboratory instructor: _______________________________________________

A. The Thermometer and Its Calibration

Temperature of water and ice mixture _______________EC

Temperature of boiling water _______________EC

Atmospheric pressure _______________mm Hg

True (corrected) temperature of boiling water _______________EC

Percent relative error of thermometer _______________ %

(show calculation, use true temperature of
boiling water above as the literature value)

B. Using the Balance to Calibrate Your 10 mL Pipet

Measured temperature of water used in pipet ____________ EC

Corrected temperature (from your calibration curve) ____________ EC

trial 1 trial 2 trial 3

Mass of Erlenmeyer plus water
Mass of Erlenmeyer
Mass of water
Volume delivered by pipet
(show calculations below)

Expt. 1-13
 EXPERIMENT 1. LABORATORY TECHNIQUES

Mean volume delivered by 10 mL pipet _____________ mL

(show calculation)

Trial 1 Trial 2 Trial 3

Individual deviations from the mean _______ _______ ______

Average deviation from the mean (show calculation) _____________ mL

Volume delivered by your 10 mL pipet __________ mL ± ___________ mL

Expt. 1-14
 EXPERIMENT 1. LABORATORY TECHNIQUES

C. Determination of Density

Density (g/mL) % Relative Error

Object Mass Volume SHOW CALCULATIONS SHOW
(g) (mL) CALCULATIONS
Water

Ethanol

Metal
(
)
Metal
(
)
Metal
(
)
*Describe Metal samples briefly in table

QUESTIONS - Answer the following question on a separate sheet of paper. Show

all calculations.

1. (a) Using the defined freezing and boiling points of water, make a graph (see
Appendix A for proper graphing techniques) of degrees Fahrenheit versus
degrees Celsius on graph paper.
(a) Determine the Celsius equivalent of 40EF using your graph.
(b) The relationship between these two temperature scales is linear. Consult
Appendix A regarding linear relationships and using the method of least
squares determine the equation that relates degrees Fahrenheit to
degrees Celsius. Make sure to show all your work.
(c) Compute the Celsius equivalent of 40EF using this relationship.

Expt. 1-15
 EXPERIMENT 1. LABORATORY TECHNIQUES

MARKING SHEET

ITEM MAX. MARK YOUR MARK

Part A. 4
Part B. 4
Part C. Water 2
% Relative Error 1
Ethanol 2
% Relative Error 1
Metal Object 1 2
Metal Object 2 2
Metal Object 3 2
Significant figures 3
Final Question 5
FINAL MARK 28
(recorded out of 14)

Comments:

Expt. 1-16