SKU3073 Chemistry

Semester 1 2020/2021

EXPERIMENT 2

APPARATUS AND MEASUREMENT IN THE LABORATORY

2.1 OBJECTIVES

Upon completion of this activity, students should be able to:

1. determine the correct apparatus to be used for transferring samples e.g.: solids and liquids

2. apply the concept of accuracy and precision in measurement

3. operate the electronic balance and record data with the correct figures

4. use volumetric apparatus correctly; e.g.: pipette and graduated cylinder

5. determine the density of solids

2.2 INTRODUCTION

2.2.1 Apparatus

In general, glassware used for standard laboratory procedure is made of borosilicate glass.
Borosilicate glass withstand thermal shock and chemical attack better than most other glass. Prior
to carrying out an experiment the following steps should be done:

• Check glassware for cracks/chips before use

• Select the appropriate glassware for the job: heating/vacuum applications/under pressure

• Glassware under pressure or vacuum should be shielded

• If it is necessary to apply pressure to glassware, wear thick leather gloves

• Never heat or apply pressure/vacuum to a chemical in a stock bottle

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Clay triangle

Crucible tong

Retort stand
Goggle

Crucible with lid

Funnel Beaker

Wire gauze

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Test tube holder

Test tube Graduated cylinder Plastic wash bottle Test tube rack

Condenser Burette Thermometer Pipette

Figure 2.1 Common laboratory apparatus

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2.2.1.1 Burette

A burette is a volumetric container to deliver different amounts of liquids or measure

changes in volume during titration, or for calibrating other scientific glassware such as graduated
cylinders. It is a long glass cylinder open at one end and fitted at the opposite end with a
stopcock valve. This valve controls the flow of liquid from the cylinder through the burette tip.
The burette used in this course has a 50.00 mL volume. The burette is etched with calibration
marking at 0.01 mL. Thus, we should be able to estimate liquid levels to the hundredths of
a millilitre (more accurate than graduated cylinder). Note that the liquid level markings begin
at the top (open end) of the burette.

2.2.1.2 Pipette

Pipettes are glass or plastic tubes, usually open at both ends which are used to transfer specific
amounts of liquid. Pipettes come in several designs for various purposes with differing levels of
accuracy and precision, from single piece glass pipettes to more complex adjustable or electronic
pipettes. Pipette is more accurate than graduated cylinder. Some pipettes have graduations and
some have only one line for measuring volume. Types of pipettes are as follows:

i. Volumetric pipettes
ii. Graduated pipettes
iii. Pasteur pipettes

2.2.1.3 Erlenmeyer flask

An Erlenmeyer flask, also known as conical flask, features a flat bottom, cone-shaped body, and
a cylindrical neck. Erlenmeyer flasks are used for simple measuring, storing and mixing of
liquids. Most Erlenmeyer flasks are made of borosilicate glass so that they can be heated over a
flame or autoclaved. The most common sizes of Erlenmeyer flasks are 250 mL and 500 mL. They
can also be found in 50, 125, 250, 500, 1000 mL.

2.2.1.4 Volumetric flask

A volumetric flask has a flat bottom bulb and a long neck, usually fitted with a stopper. The neck
has a single ring graduation mark and a label. The marking indicates the volume of liquid
contained when filled up to that point. Volumetric flask is designed to contain an accurate volume
of liquid and is used in analytical chemistry to produce accurate solutions. A typical volumetric
flask is assumed to be accurate to four significant figures. For instance; if a 40 mL volumetric flask
is filled to the mark, then it contains 40.00 mL.

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2.2.1.5 Graduated cylinder

Graduated cylinders are used for accurate measurements of small volumes of liquid that
cannot be done with beakers and Erlenmeyer flasks. They are less accurate and precise than
volumetric flask or volumetric pipette. A graduated cylinder should be made of borosilicate glass
if you need to use oxidizing material and certain hydrocarbon.

2.2.1.6 Beaker

Beakers are generally cylindrical in shape, with a flat bottom and a beak for pouring. They are
available in a wide range of sizes. Borosilicate beakers can be used for routine mixing,
measuring and boiling.

2.2.1.7 Boiling flask

The borosilicate boiling flasks a r e highly resistant to heating or chemical attack. A flat
bottom flask can be used on a wire gauze; a n d a round bottom one needs a clamp and boss
head. These flasks are used instead of an Erlenmeyer flask if vigorous boiling is required.

2.2.1.8 Balance

Two types of balance are normally used in the laboratory; top loading and analytical balance.
The top loading balance is accurate to 0.01 g and an analytical is accurate to 0.0001g (Figure
2.2).

Figure 2.2 Top loading balance

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The weighing procedure of a top loading balance consists of three steps:

• Press ‘tare’ button to reset the balance to zero.

• Place the object to be weighed on the pan.

• After waiting for the stability, read the mass of the object.

Figure 2.3 Analytical balance

The weighing procedure of analytical balance (Figure 2.3) consists of three steps:

1. Set the balance to zero point. This must be done each time the balance is used.

• Unload the pan. Clean it if necessary.

• Close the sliding panels of the balance.

• Switch on the display by pressing the control bar once.

2. Place the object to be weighed on the pan. Use a pair of tweezers or tongs to avoid
transmitting moisture and oil from your skin to the object. Close the sliding panels of the
balance immediately.

3. Read the mass.

• Wait until the display is stable and the stability indicator goes out.

• Read the mass.

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2.2.1.9 Thermometer

The thermometer is a device that measures temperature. The temperature scales commonly
employed in scientific studies are the degree Celsius (°C) and Kelvin (K) scales.

2.2.1.10 Bunsen burner

The burner ( F i g u r e 2 . 4 ) is a device widely used in chemistry laboratory. Since the first
laboratory burner was perfected by Robert Bunsen, many people give his name to any simple
burner.

Figure 2.4 Bunsen burner

To use the burner, connect one end of a rubber hose to the gas inlet at the base of the burner.
Attach the other end to the gas jet on the bench. Slowly open the gas valve and light up the top
of the burner. Adjust the flame by controlling the gas-air mixture at the bottom of the burner. To
obtain the hottest flame, open the valve all the way, and then open the mixture control until the
burner starts to produce a hissing sound. The hottest position in the flame is about 1 cm above
the top of the burner. It is just above the tip of the blue part of the flame. When the burner is
adjusted properly, the flame will be non-luminous and totally blue. There should be a mild hiss
and no yellow colour is present. When the air vents are entirely closed, the burner produces a
yellow, smoky flame known as a luminous flame (Figure 2.5).

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Figure 2.5 Parts of a flame

2.2.2 Measurement

Chemistry is an experimental science, and measurements are fundamental to most of the

experiments. It is important to learn how to make and use these measurements properly.

2.2.2.1 Accuracy

The accuracy of a measurement reflects its nearness to the ‘true’ value, Xtrue. The difference
between measurement X1 and Xtrue is the error of the measurement.

error = 𝑋1 − 𝑋𝑡𝑟𝑢𝑒

Note that accuracy is not the same thing as precision, which only compares one measured
quantity with others. The “true” value is seldom known – that is the reason why we do
experiments to determine a value. Thus, it is difficult to arrive at an estimate of the error of the
measurement. The relative error is the difference between a measured quantity and the true
value divided by the true value and multiplied by 100%.

𝑋1 − 𝑋𝑡𝑟𝑢𝑒
relative error = × 100
𝑋𝑡𝑟𝑢𝑒

The relative error is one method of expressing the accuracy of a measured quantity.

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2.2.2.2 Precision

Every measurement has a degree of uncertainty associated with it that scientists strive to
reduce to an acceptable level. The analysis is often repeated several times to obtain a replicate
set of measurements for comparison. The reproducibility of a result obtained by the same
experimental method is termed precision. If the variations between individual measurements
were sufficiently small, then an average of the measurements called the mean; is calculated.
The mean is obtained by summing the individual measurements and divide it by the number of
the measurements. For series of measurements X1, X2 and X3, the mean Xav is given by the
following expression.

𝑋1 + 𝑋2 + 𝑋3
𝑋𝑎𝑣 =
3

The difference between any individual measurement and the mean is used to express the
precision of the experimental value ( X1 - Xav ). The relative deviation is the quotient of the
deviation for a measured quantity and the mean multiplied by 100%.

𝑋1 − 𝑋𝑎𝑣
relative deviation = × 100
𝑋𝑎𝑣

Apparatus

Top loading balance

Analytical balance

Crucible and lid

100 mL beaker

50 mL beaker

10 mL graduated cylinder

10 mL pipette

Thermometer

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2.3 PROCEDURE

Activity 1: Mass

1. Determine the mass of each of the following using the top loading balance.

a. Crucible only.

b. Crucible lid only.

c. Crucible and crucible lid together.

2. Determine the mass of each item (a), (b) and (c) again as a second trial. For each
measured quantity, indicate the number of decimal points that gives reliable data.

3. Compare the sum of (a) and (b) with the directly determined quantity (c). Are they the
same? Calculate the difference.

4. Calculate the average and the relative deviation.

5. Calculate for any differences between the two trials.

6. Replace the top loading balance with analytical balance.

7. Repeat step 1 – 5.

8. Compare the result obtained using the top loading balance with those obtained by the
analytical balance. How do they differ?

Activity 2: Volume

1. Add about 100 mL of distilled water to a beaker (label A) and determine the temperature of
the water. Record the temperature and find the corresponding density of water from the
following table.

Table 3.1: The density of water at different temperature

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

15 0.9991 21 0.9980
16 0.9990 22 0.9977
17 0.9988 23 0.9975
18 0.9986 24 0.9973
19 0.9984 25 0.9970
20 0.9982 26 0.9968

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2. Determine the mass of a dry 50 mL beaker using the analytical balance. Measure 10.0
mL of distilled water from beaker A using the graduated cylinder. Transfer the 10.0 mL
distilled water into the 50 mL beaker and weigh the mass of the beaker and the water.
Using the density of water from Table 1 at the measured temperature, calculate the mass
of water in the beaker.

3. Compare the calculated mass of water and mass of the 10.0 mL water that has been
transferred by the graduated cylinder.

4. Calculate the relative error.

5. Repeat step 2 – 4 for the second trial.

6. Calculate the average value and relative deviation.

7. Repeat step 2 – 6. Replace the graduated cylinder with pipette.

2.4 QUESTIONS

1. Based on your results, which instrument is more precise and accurate? Explain your answer.

2. Explain why precision and accuracy are important in chemistry measurement.

3. Suggest ways to enhance precision and accuracy in conducting chemistry experiments.

2.5 REFERENCES

1. Carr, Kevin. (2018). Importance of Measurements in Chemistry. Sciencing,

https://sciencing.com/importance-measurements-chemistry-8589096.html. 11 May 2018.

2. Betz, J. M., Brown, P. N., & Roman, M. C. (2010). Accuracy, precision, and reliability of
chemical measurements in natural products research. Fitoterapia, 82(1), 44-52.

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2.6 WORKSHEET

Activity 1: Mass

Top-Loading Balance

Reading

I II

(1) Mass of crucible

(2) Mass of crucible lid

(3) Sum of (1) and (2)

(4) Mass of crucible and lid

(5) Difference between (3) and (4)

(6) Average value of (4)

(7) Relative deviation of (4)

Data (4)- Data (6)

x 100
Data (6)

(8) Average of relative deviation

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Analytical Balance

Reading

I II

(1) Mass of crucible

(2) Mass of crucible lid

(3) Sum of (1) and (2)

(4) Mass of crucible and lid

(5) Difference between (3) and (4)

(6) Average value of (4)

(7) Relative deviation of (4)

Data (4)- Data (6)

x 100
Data (6)

(8) Average of relative deviation

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Activity 2: Volume

Graduated cylinder

Reading

I II

(1) Mass of beaker

(2) Mass of beaker and water

(3) Mass of water (2) – (1)

(4) Average value of (3)

(5) Calculated mass of water

(6) Relative error of (3)

𝐷𝑎𝑡𝑎 (3) − 𝐷𝑎𝑡𝑎 (5)

𝑥 100
𝐷𝑎𝑡𝑎 (5)

(7) Average of relative error

(8) Relative deviation of (3)

𝐷𝑎𝑡𝑎 (3) − 𝐷𝑎𝑡𝑎 (4)

𝑥 100
𝐷𝑎𝑡𝑎 (4)

(9) Average of relative deviation

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Pipette

Reading

I II

(1) Mass of beaker

(2) Mass of beaker and water

(3) Mass of water (2) – (1)

(4) Average value of (3)

(5) Calculated mass of water

(6) Relative error of (3)

𝐷𝑎𝑡𝑎 (3) − 𝐷𝑎𝑡𝑎 (5)

𝑥 100
𝐷𝑎𝑡𝑎 (5)

(7) Average of relative error

(8) Relative deviation of (3)

𝐷𝑎𝑡𝑎 (3) − 𝐷𝑎𝑡𝑎 (4)

𝑥 100
𝐷𝑎𝑡𝑎 (4)

(9) Average of relative deviation

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DATE LECTURER’S SIGNATURE/STAMP