Basic Laboratory Techniques

APPARATUS AND CHEMICALS

Triple beam balance 25-mL Erlenmeyer flask Clamp

150-mL beaker 125-mL Erlenmeyer flask Rubber bulb
50- or 100-mL graduated cylinder Iron ring and ring stand Thermometer
10-mL pipet Bunsen burner and hose Wire Gauze
Test tube holder 2 – Test tubes Evaporating dish

DISCUSSION

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
mastery of these fundamental operations. It is important that the data recorded will reflect the accuracy
of the device used in the measurement. The present system of weights and measurements, the metric
system, was originally based mainly upon fundamental properties of one of the world's most abundant
substances, water. The system is summarized in Table 1.1. Conversions within the metric system are quite
simple once you have memorized the meaning of the prefixes given in Table 1.2. Recently, scientists have
started to use a briefer version of the metric system of units in which the basic units for length, mass, and
time are meter, kilogram, and second, respectively. This system of units, known as the International
System of Units, is commonly referred to as the SI system and is preferred in scientific works. A
comparison of some common SI, metric, and English units presented in Table 1.3. Conversions within the
metric system are quite easy if you know the definitions for the prefixes and use dimensional analysis in
problem solving.

Table 1.1 Units of Measurement in the Metric System

Measurement Unit and definition
Mass or weight Gram (g) = mass of 1 cubic centimeter (cm3 ) of water at 4°C & 760 mm Hg
Mass = quantity of material
Weight = mass x gravitational force
Length Meter (m) =100 cm =1000 millimeters (mm) =39.37 in.
Volume Liter (L) =volume of 1 kilogram (kg) of H2O at 4° C
Temperature °C, measures heat intensity:
0 5 9
𝐶 = ( 0𝐹 − 32) 𝑜𝑟 0𝐹 = ( × 0𝐶 ) + 32
9 5
Heat 1 calorie (cal), amount of heat required to raise 1 g of water 1°C
1 cal = 4.184 joules (J)
Density ρ, usually g/ml, for liquids and g/L for gases:
𝑚𝑎𝑠𝑠
𝜌 = 𝑢𝑛𝑖𝑡 𝑣𝑜𝑙𝑢𝑚𝑒
Specific gravity Sp gr, dimensionless
density of a substance
𝑆𝑝 𝑔𝑟 = density of a reference substance,usually water

The quantities presented in Table1.1 are measured with the aid of various pieces of apparatus. A brief
description of some measuring devices follows.
 Table 1.2 The Meaning of Prefixes in the Metric System
Prefix Meaning (power of 10) Abbreviation
atto 10-18 A
-15
femto- 10 f
pico- 10-12 p
nano- 10-9 n
-6
micro- 10 µ
milli- 10-3 m
centi- 10-2 c
-1
deci- 10 d
kilo- 103 k
6
mega- 10 M
giga- 109 G
tera 1012 T
15
peta 10 P
exa 1018 E

Table 1.3 Comparison of SI, Metric, and English Units

Physical Quantity SI Unit Some Common Metric Units Conversion Factors
Length Meter (m) Meter (m) 1 m = 100 cm
Centimeter (cm) 1 m = 39.37 in
1 in = 2.54 cm
3
Volume Cubic Meter (m ) Liter (L) 1 L = 1000 cm3
3
Milliliter (mL) = 1 cm 1 L = 10-3 m3
1 L = 1.06 qt
Mass Kilogram (Kg) Gram (g) 1 kg = 1000 g
Milligram (mg) 1 kg = 2.205 lb
1 lb = 453.6 g
Energy Joule (J) Calorie (cal) 1 cal = 4.184 J
Temperature Kelvin (k) Degree Celsius (°C) 𝐾 = ℃ + 273.15
0 5
𝐶 = ( 0𝐹 − 32)
9

Laboratory Balance
A laboratory balance is used to obtain the mass of various objects. There are several different varieties of
balances, with various limits on their accuracy. Two of these balances are shown in Figure 1.1. Most
modern laboratories possess single-pan balances. These are the most accurate balances; generally, they
are the simplest to use and most delicate. 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 instantly when an object to be
weighed is placed on the pan.

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 has 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. A liter (L) is divided into milliliters (mL) such that
1 mL = 0.001 L and 1 L = 1000 mL.
 Thermometers

Most thermometers are based upon the principle that liquids

expand when heated. Most common thermometers use
mercury as the liquid. These thermometers are made so that a
uniform-diameter capillary tube surmounts a mercury
reservoir. To calibrate a thermometer, one defines two
reference points, normally the freezing point of water (0°C,
32°F) and the boiling point of water (100°C, 212°F) at 1 atm of
pressure (1 atm = 760 mm Hg). Once these points are marked
on the capillary, its length is then sub-divided into uniform
divisions called degrees. There are 100° between these two
points on the Celsius, (°C, or centigrade) scale and 180°
between those two points on the Fahrenheit (°F) scale.

Pipets

Pipets are glass vessels 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 25°C. Always use a rubber bulb to fill a pipet. NEVER USE YOUR MOUTH!
A TD pipet should not be blown empty.

It is important to be aware that every measuring device, regardless of what it may be, has limitations in
its accuracy. Moreover, to take full advantage of a given measuring instrument, you should be familiar
with its accuracy. Careful examination of the subdivisions on the device will indicate the maximum
accuracy you can expect of that particular tool.
 Figure1.2 A typical volumetric pipet and rubber bulbs

In this exercise, the accuracy of the 10-ml pipet will be determined. The approximate accuracy of some
of the equipment is given in table 1.4.

Table 1.4 Equipment Accuracy

Equipment Accuracy
Analytical balance ±0.0001 g (±0.1 mg)
Triple beam balance ±0.10 g
Graduated cylinder ±0.1 mL
Pipet ±0.02 mL
Buret ±0.02 mL
Thermometer ±0.2°C

A. The Bunsen Burner

The Bunsen burner is a convenient source of heat in the laboratory. Although there are several
varieties, their principle of operation is the same and is similar to that of the common gas stove. The
Bunsen burner requires gas and air that mix various proportions. The amount of air and gas mixed in
the chamber is varied by use of the collar illustrated in Figure 1.3. The relative proportions of gas and
air determine the temperature of the flame.

barrel

Figure 1.3 Typical Bunsen burner.

 Figure 1.4 Regions of the flame for temperature measurement.

Color of the Wire Gauze Approximate Temperature

no change below 500 0C
dull red 501 0C – 650 0C
cherry red 651 0C – 750 0C
orange 751 0C – 900 0C
yellow 901 0C – 1100 0C

B. The Graduated Cylinder

Examine the 100-mL graduated cylinder and notice that it is scribed in milliliters. Fill the cylinder
approximately half full with water. Notice that the water meniscus (curved surface of the water) is
concave (see Figure 1.5).
When water is the liquid to be measured, the lowest point on the curve is always read as the
volume, never the upper level. Avoid errors due to parallax. Different and erroneous readings are
obtained if the eyes are not perpendicular to the scale. Read the volume of water to the nearest 0.1
mL. Record this volume. Measure the maximum amount of water that your 125-mL Erlenmeyer flask
will hold. Record this volume.

Figure 1.5 Proper eye position for taking volume readings. The meniscus reading here is 50.0mL.
C. Using the balance to calibrate your 10-mL pipet
Weighing an object on a single-pan balance is very simple. Because of the sensitivity of the balance,
the student must be careful in its use. Directions for operation of single-pan balance vary with its
brand and model. The laboratory instructor will explain how to use the balance. Regardless of the
balance to be used, proper care of the balance requires the following to be observed:

1. Do not drop an object on the pan.

2. Center the object on the pan.
3. Do not place chemicals directly on the pan. Use a beaker, watch glass, weighing bottle, or
weighing paper.
4. Do not weigh hot or warm objects. Objects must be at room temperature.
5. Return all weights to zero position after weighing.
6. Clean up any chemical spills in the balance area.
7. Inform your instructor if the balance is not functioning correctly. Do not attempt to repair it
yourself.
The following method is used to calibrate a pipet or other volumetric glassware. Fill about 40 mL of
distilled water in a 150-mL beaker. Record and weigh an empty, dry 25-mL Erlenmeyer flask (tare) to
the nearest 0.1 mg. Measure and record the temperature of the water. Pipet exactly 10.00 mL of
water into this flask and weigh the flask with the water in it (gross) to the nearest 0.1 mg. Obtain the
weight of the water by subtraction. Using the equation below and the data given in Table 1.5, obtain
the volume of water and therefore the volume of your pipet.
𝒎𝒂𝒔𝒔 𝒎
𝒅𝒆𝒏𝒔𝒊𝒕𝒚 = =
𝒗𝒐𝒍𝒖𝒎𝒆 𝒗

Normally, density is given in units of grams per milliliter (g/mL) for liquids, grams per cubic centimeter
(g/cm3) for solids, and grams per liter (g/L) for gases. Repeat this procedure in triplicate-that is,
deliver and weigh exactly 10.00 mL of water three separate times.
Table 1.5 Density of pure water (g/cm3) at temperatures ranging from 10.0°C to 30.9°C by 0.1°C
increments (example: density at 20.6 0C = 0.998078 g/cm3)
EXAMPLE 1.1
Using the procedure given above, a weight of 10.0025 g was obtained as the weight of the water delivered
by one 10-mL pipet at 22.0°C. What is the volume delivered by the pipet?
𝑚
SOLUTION: From the density equation given above, we know that 𝑉 =
𝑑

For the mass, we substitute our value of 10.0025 g. For the density, refer to Table 1.6. At 22.0°C, the
density is 0.997770 g/mL. The calculation is:
𝟏𝟎. 𝟎𝟎𝟐𝟓 𝒈
𝑽= = 𝟏𝟎. 𝟎𝟐𝟒𝟗 ≈ 𝟏𝟎. 𝟎𝟐 𝒎𝒍
𝟎. 𝟗𝟗𝟕𝟕𝟕𝟎 𝒈/𝒎𝒍
The volume must be rounded off to 10.02, because the pipet's precision can be determined only to within
±0.02 mL.

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.

EXAMPLE 1.2
The following values 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:
𝟏𝟎. 𝟏𝟎 + 𝟗. 𝟗𝟖 + 𝟏𝟎. 𝟎𝟎
𝒎𝒆𝒂𝒏 = = 𝟏𝟎. 𝟎𝟑
𝟑
Deviations from the mean: |value – mean|

|10.10 -10.03| = 0.07

|9.98 - 10.03| = 0.05

|10.00 - 10.03| = 0.03

𝟎. 𝟎𝟕 + 𝟎. 𝟎𝟓 + 𝟎. 𝟎𝟑
𝐀𝐯𝐞𝐫𝐚𝐠𝐞 𝐝𝐞𝐯𝐢𝐚𝐭𝐢𝐨𝐧 𝐟𝐫𝐨𝐦 𝐭𝐡𝐞 𝐦𝐞𝐚𝐧 = = 𝟎. 𝟎𝟓
𝟑
The reported value is therefore 10.03 0.05 mL.