EXPERIMENT 1

BASIC LABORATORY TECHNIQUES

INTRODUCTION
Chemistry is an experimental science. It depends upon careful observation and the use of good
laboratory techniques. Most of the experiments in the chemistry laboratory involve quantitative
analytical procedure. It is involve the use of common glassware for example burette, pipette,
volumetric flask etc. These glassware are used to measure the volume of solutions at certain
temperature. The volume of a liquid change with temperature, to get the accuracy, the apparatus
involve to measure the volume of solutions have to be calibrated before used.

Mistakes and errors can happen during an experiment. A mistake is a blunder or unintentional
action whose consequence is undesirable. Error on the other hand, account for the range of
values obtained from successive measurements of the same quantity, even though there was no
mistake in any of the measurement. Error may be either systematic or random. A systematic
error can happen when an apparatus which is not calibrated is used. The measurement will
always be too large or, alternatively, too small. A systematic error will influence the accuracy of
a measurement, that is, the agreement between a measured value of a quantity and its true value.
A random error will be the evident when a measuring device, even a very accurate one, is used a
number times to make the same measurement. Both error can be reduce by using calibrated
apparatus and careful when doing experiment.

a) Volumetric flask

A volumetric flask is glassware designed to deliver the standard solution at precise known
volume of liquid at given temperature. The actual volume of liquid in the flask can be
determined by weighing the empty flask then flask and distilled water. The difference between
both readings is equal to the mass of water. The volume of water in the flask can be calculated
from Table 1. Volumetric flasks are used to make solutions of known concentration by the
dissolution of a known mass of solid or the dilution of a more concentrated solution. Before use,
always wash the flask and then pre-rinse with the solvent. Some frequently used volumes in
General Chemistry lab are 10.00, 25.00, 50.00, 100.00, and 250.0 mL flasks. At times the zeros
to the right of the decimal point are omitted. However, these zeros must always be considered in
calculations, as they indicate the accuracy of the volume measurement. (i.e., they are significant
figures).

1
b) Pipette

Pipettes are glass vessels that are constructed and calibrated so as to deliver a precisely known
volume of liquid at a given temperature. Transfer and Mohr pipette are two types of common
pipette usually found in the laboratory. A transfer pipette is calibrated to deliver only one
volume, whereas a Mohr pipette is graduated so that it can deliver any volume (usually to nearest
tenth of a milliliter) up to maximum volume. Transfer pipettes come in many size, but 5 mL, 10
mL, 20 mL, 25 mL pipette are usually found in general chemistry laboratories. Common volume
of Mohr pipette are 1 mL, 5 mL and 10 mL volume. The correct use of a pipette requires
considerable manipulatory skill. Step-by step procedures for correct usage are:

a) Rinse the pipette with the solution to be used.

b) Insert the pipette into the solution and suck using pipette filler (suction bulb). The
solution is about 1 to 2 cm above the etched line on the pipette.
c) Drain the excess into a waste container until the bottom of the meniscus coincides with
etched line.
d) Allow the liquid in the pipette to drain into the flask to be used in the experiment. Touch
off the last drop. (Do not blow the remaining liquid from the pipette. The pipette was
calibrated to deliver the correct volume with this liquid remaining in it).

The actual volume of solution (pipette volume) can be measured by weighing the solution that
has been transferred using that pipette. From the density of the solution, we can calculate the
volume of solution (pipette volume).

c) Burette

A burette (also buret) is a vertical cylindrical piece of laboratory glassware with a volumetric
graduation on its full length and a precision tap, or stopcock, on the bottom. It is used to dispense
known amounts of a liquid reagent in experiments for which such precision is necessary, such as
a titration experiment. Burettes are extremely accurate - a 50 mL burette has a tolerance of 0.1
mL (class B) or 0.06 mL (class A). The difference between starting and final volume is the
amount dispensed. The spacing between the lines will allow you to estimate the volume to the
nearest 0.01 mL. Thus, typical burette readings would be two decimal points, for example, 9.34
mL or 17.60 mL. Reading such as 9.3 mL or 17.6 mL are not acceptable. The following are the
step will help you to have a burette that operates as it should:

a) Clean and rinse the burette with tap water, then distilled water.
b) Rinse the burette with about 5-10 mL of the solution.
c) Fill burette above the zero mark with the stop cork closed. Open the stopcock fully so
that the liquid drain rapidly to flush out air bubble in the tip of the burette. Drain the
burette until the meniscus rest at a certain number, for example, 1 mL marks (or 0 mL
marks). Read the burette to 2 decimal places with your eye on the same level as the
meniscus.
d) To obtain the volume of the solution (liquid) that you use in titration, subtract the initial
reading from the final reading.

2
To calibrate the burette, transfer several volumes of solution from the burette and weigh
accurately. From the density of the solution, we can calculate the volume of solution that has
been transferred.

Table 1: Density of Water (g/mL) at Various Temperatures (°C)

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

22 1.0032
23 1.0034
24 1.0037
25 1.0039
26 1.0042
27 1.0045
28 1.0047
29 1.0050
30 1.0053
35 1.0059

OBJECTIVES
1. To learn the qualitative and quantitative aspects of common laboratory equipment.
2. To expose student to the factors that affect the accuracy of an experiment.

APPARATUS
Analytical balance
Burette
Pipette (20 mL or 25 mL)
Volumetric flask (25 mL)
Beaker (50 mL)
Thermometer
Pipette filler or suction bulb
Retort stand
Burette clamp
Dropper

3
CHEMICAL

Distilled water

PROCEDURE
A. Calibration of Volumetric Flask

1. Clean and dry a 25 mL volumetric flask and weigh accurately using analytical
balance. Record the mass of empty volumetric flask.
2. Add distilled water until the calibration mark (use a dropper to add the last few
drops of distilled water) and weigh again (use the same balance). Record the mass
of distilled water and volumetric flask.
3. Record the temperature of the distilled water.
4. From the Table 1, determine the actual volume of the volumetric flask.

B. Calibration of Pipette

1. Clean and dry a 50 mL beaker and weigh accurately using analytical balance.
Record the mass of empty beaker.
2. Clean a pipette (20 or 25 mL) and rinse with distilled water.
3. Fill the pipette with distilled water using the procedures that have been discussed
in the introduction part.
4. Drain the distilled water into the beaker and weigh again. Record the mass of
distilled water and beaker.
5. Repeat step 1-4 one more time and record the temperature of the distilled water.
6. From the Table 1, determine the actual volume of the pipette.

C. Calibration of Burette

1. Clean and dry a 50 mL beaker and weigh accurately using analytical balance.
Record the mass of empty beaker.
2. Clean and rinse the burette using distilled water and fill in the burette with the
distilled water until the zero mark. (Make sure there are no bubbles in the tip of
the burette)
3. Drain 5 mL of the water from the burette into the beaker and weigh as soon as
possible. Record the mass.
4. Repeat step 3 by draining water from the burette until the following burette
reading become 10 mL, 15 mL and 20 mL. (Each time 5 mL distilled water has
been added from the burette). Record the mass (distilled water + beaker) every
time after adding 5 mL of water.
5. Record the temperature of the distilled water.
6. From the Table 1, determine the actual volume for every addition of 5 mL of
distilled water.
4
QUESTIONS
1. How do you overcome or reduce the problem of random error and systematic error while
doing an experiment?

2. In what situation do you use a volumetric flask, conical flask, pipette, and graduated
cylinder? Explain your answer from the accuracy aspects of these apparatus.

3. Explain how to read a burette. What are the factors to be considered while using the
burette?

5
 DATASHEET EXPERIMENT 1

BASIC LABORATORY TECHNIQUES

Name : Date :

Student ID : Group :

RESULTS
Data:

a. Calibration of Volumetric Flask

Mass of empty volumetric flask (g)

Mass of volumetric flask + distilled water (g)

Mass of distilled water (g)

Temperature of distilled water (oC)

Density of water (from Table 1) (g/mL)

b. Calibration of Pipette

(i) (ii)

Mass of empty beaker (g)

Mass of beaker + distilled water (g)

Mass of distilled water (g)

Temperature of distilled water (oC)

Density of water (from Table 1) (g/mL)

6
c. Calibration of Burette

Mass of empty beaker (g) : …………………..

Temperature of distilled water (oC) : …………………..

Density of water (from Table 1) (g/mL) : …………………..

After the addition of distilled water:

Mass of distilled water

Reading of Mass of beaker + Mass of distilled
for each 5 mL burette
burette (mL) distilled water (g) water (g)
reading (g)
5

10

15

20

7
Calculations:

a. Determine the actual volume of the volumetric flask based on calculation.

b. Determine the actual volume of the pipette based on the calculation for experiment (i)
and experiment (ii).

c. Determine the actual volume of distilled water (in mL) for each 5 mL burette reading
based on calculation.

Reading of burette (mL) Volume of water (mL)

0-5

5-10

10-15

15-20

Lecturer’s signature,

8
 EXPERIMENT 2

DETERMINATION OF PERCENT COMPOSITION IN

HYDRATE COMPOUNDS

INTRODUCTION
Several salts that occur naturally in nature or purchased from local retailer are hydrated salts. A
hydrated salt is a salt which has a number of chemically bound water molecules attached to the
salt within its crystalline structure. These water molecules maybe referred to as the waters of
crystallization or water hydration. In most situations the number of moles of water will remain
fixed as a function of the moles of salt present. The formula for a hydrated salt is represented by
the formula for the anhydrous salt followed by a dot and the appropriate number of water
molecules. The formula for copper (II) sulphate pentahydrate is CuSO4.5H2O, which indicates
that 5 waters of hydration are present for each 1 mole of CuSO4 salt. Copper sulphate
pentahydrate is a blue crystal, while anhydrous salt, meaning without water.

CuSO4. 5H2O(s) CuSO4 (s) + 5H2O (g)

Δ

However, some salt have their water bound so tightly that producing an anhydrous salt is nearly
impossible as in the case of iron (III) chloride hexahydrate. The salt would decompose before the
anhydrous salt would be formed. The mass percentage of water in a hydrate can be determined
by heating a known amount of a sample until complete dehydration is accomplished.

Hydrate salt Anhydrous salt + water

Δ

The dehydration step will result in a lower mass reading, so it is possible to determine the
amount of water that was present within the salt sample.

Total mass of hydrate salt is a sum of mass of the anhydrous salt and mass of water of hydration.

Total mass of hydrate salt = mass of the anhydrous salt + mass of waters of hydration

The percent mass of water in the hydrate may also be easily calculated using a formula:

Percentage of water = mass of water loss x 100

mass of sample

9
OBJECTIVES

1. To calculate the mol of water (x) in barium chloride hydrate (BaCl2.xH2O) using percent
composition concept and the atomic mass.
2. To identify molecular formula of compound A from the thermal decomposition.

APPARATUS
Crucible and lid
Clay triangle
Ring clamp
Retord stand
Bunsen burner
Crucible tongs
White tile

CHEMICALS

Barium chloride hydrate (BaCl2.xH2O)

Compound A (Compound A can be any of the following: Li2SO4.H2O, MgSO4.7H2O,
FeSO4.7H2O, SrCl2.6H2O or CaSO4.2H2O)
6 M HNO3
1 M HCl

PROCEDURE
To complete two trials in one lab period, your instructor may require you to perform both trials
simultaneously.

1. Obtain a crucible and lid. Clean the crucible and check for any stress cracks, fractures or
fissures before use. (If the crucible is dirty, move the apparatus to hood and add 1-2 mL
of 6 M HNO3 and gently evaporate to dryness then inspect the crucible after cooling for
any defects. If no defects are found the crucible and lid should supported on a clay
triangle).
2. Record an initial mass of the crucible and lid.
3. Heat the crucible and lid gentle for 5 minutes with an intense flame until the bottom of
the crucible has become red. Allow the crucible and lid to cool on the clay triangle before
proceed the experiment.
4. Determine the mass of the “fired” cool crucible and lid, then record. Repeat step 2 until
you have two crucible and lid mass readings that differ by no more than 10 mg or
0.010 g.

10
5. Setup the heating process as shown in Figure 1 below. Tilt the lid so that it is slightly
ajar, then heat strongly (bottom of crucible should turn red) for about 5 minutes. Turn off
the Bunsen burner, and use tongs to close the lid so that water from the air does not get
inside the dry crucible. Allow the crucible and lid to cool (this should take 5 minutes).

Figure 1: Setup of the Heating Process

6. Add between 1.5 and 2.0 g of hydrated salt to the crucible and measure the combined
mass of the crucible, lid and salt, then record.
7. Place the crucible with the sample on the clay triangle. With the lid slightly ajar, heat the
sample slowly for 2 minutes and drastically heat the sample at a high temperature for 10
minutes. Cover the crucible once the heat is removed and allow cooling at room
temperature in desiccators. Record the mass of the crucible, lid and anhydrous salt using
the same analytical balance as used in the earlier steps.
8. Reheat the sample for an additional 2 minutes with intense heat. Weigh the combined
mass of the crucible, lid and anhydrous salt and continue repeating this process until two
concurrent reading within 10 mg of each other were obtained.
9. Apply this procedure for Compound A.

DISPOSAL

Dispose of all waste anhydrous salt in the “Solid Waste” container.

CLEAN-UP

Rinse the crucible with 2-3 mL of 1 M HCl and discard in the “Acid Waste” container. Rinse the
crucible three times with tap water and once with distilled water.

11
QUESTIONS
1. Give the reason why the empty crucible should be heated before starting the experiment.

2. Why the process of heating hydrate compound should be started slowly first?

3. What is the important of percent composition of water in the hydrate compounds?

12
 DATASHEET EXPERIMENT 2
DETERMINATION OF PERCENT COMPOSITION IN
HYDRATE COMPOUNDS

Name : Date :

Student ID : Group :

RESULTS
Data:

a. Determination of Percent Water in Barium Chloride Hydrate (BaCl2.xH2O)

Mass of empty crucible and lid g

First heating g

Second heating g

Mass of crucible + lid + hydrate before heating g

Mass of crucible + lid + hydrate after,

1) First heating g

2) Second heating g

3) Third heating g

13
b. Determination of Water Composition and Molecular Formula of Compound A.

Crucible and lid

Mass of empty crucible and lid g

First heating g

Second heating g

Mass of crucible + lid + hydrate before heating g

Mass of crucible + lid + hydrate after,

1) First heating g

2) Second heating g

3) Third heating g

14
Calculations:

a. Determination of Percent Water in Barium Chloride Hydrate (BaCl2.xH2O)

Calculate:

1. Mass of BaCl2.xH2O.
2. Mass of barium chloride anhydrous.
3. Mass of water in BaCl2.xH2O.
4. Percent composition of water in BaCl2.xH2O.
5. Formula of barium chloride hydrate.

b. Determination of Water Composition and Molecular Formula of Compound A.

Calculate:

1. Mass of Compound A.
2. Mass of Compound A anhydrous.
3. Mass of water in Compound A.
4. Percent composition of water in Compound A.
5. Identification of Compound A (compare your result to the nearest percent
composition of water in the hydrates listed)

Li2SO4.H2O, MgSO4.7H2O, FeSO4.7H2O, SrCl2.6H2O or CaSO4.2H2O

Lecturer’s signature,

15
 EXPERIMENT 5

INTRODUCTION TO TITRATION-DETERMINATION OF THE

MOLARITY AND CONCENTRATION OF SULPHURIC ACID
BY TITRATION WITH A STANDARD SOLUTION OF SODIUM
HYDROXIDE

INTRODUCTION
Titration is a process in volumetric analysis that involved the reaction of analyte with a measured
volume of reagent of known concentration. In this process, a solution of accurately known
concentration, called a standard solution, is added gradually to another solution of unknown
concentration until the chemical reaction between the two solutions is complete.

An acid-base titration involves a neutralization reaction in which an acid is reacted with an

equivalent amount of base. An indicator solution is used to determine the end point i.e. point at
which an acid has exactly neutralized a base, or vice versa. A suitable colour change shows
equivalent amounts of acids and base are present. Indicators change colours at different pH
values. Phenolpthalein for example changes from colourless to pink at a pH of about 9.

In this experiment, you will determine the molarity and concentration of sulphuric acid from data
obtained by titrating it with a standard solution of sodium hydroxide until the end point. The
molarity of sulphuric acid can be calculated by using the formula:

M a Va a
=
M b Vb b

where,

Ma = concentration of acid
Mb = concentration of base
Va = volume of acid
Vb = volume of base
a = coefficient of acid
b = coefficient of base

The concentration of the sulphuric acid can be determined using the formula:

Concentration (g/L) = Molarity x Molar mass

16
OBJECTIVES
To determine the molarity and concentration of sulphuric acid using titration technique.

APPARATUS
Burette
Burette clamp
Retort stand
Volumetric pipette (20 mL)
Pipette filler or suction bulb
Conical flask (250 mL)
White tile / white paper

CHEMICALS
Sodium hydroxide solution, NaOH, approximately 0.2 M (must be accurately standardized by
the instructor before the laboratory session)
Dilute sulphuric acid, H2SO4 of unknown molarity
Phenolpthalein

PROCEDURE
1. Wash the burette with distilled water and then rinse with about 5-10 mL of NaOH
solution, running the second rinsing through the burette tip. Clamp the burette to the
retort stand.
2. Fill the burette with the NaOH solution. Make sure the tip is completely filled and
contain no air bubbles. Record the initial burette reading to two decimal places.
3. Using a volumetric pipette, transfer 20 mL H2SO4 to a clean 250 mL conical flask. Add 2
or 3 drops of phenolphthalein indicator. Place this conical flask on a piece of white paper
(DO NOT USE FILTER PAPER!) under the burette and lower the burette tip into the
conical flask.
4. Setup the titration apparatus (Figure 3). Titrate the H2SO4 solution by adding NaOH
solution until the end point is reached. During the titration, keep swirling the conical
flask. The end point is indicated when the entire solution retain a FAINT PINK colour
for at least 30 seconds. Record the final burette reading. This is the result of the ROUGH
TITRATION.

17
 6

1. Burette
1 2. Stopcock
3. Conical flask
4. White tile / white paper
5 2 5. Retort Stand
6. Burette clamp

Figure 3: Setup of the Titration

5. Repeat the titration process until two consecutive titrations (meaning, one titration
after another) agree to ±0.10 mL. For example:

Volume of titration #1 = 15.15 mL

Volume of titration #2 = 15.12 mL
So, the difference in volume = ±0.03 mL (which is within the given limit of ±0.10 mL).
This means you may stop doing anymore titrations. You will use the average volume as
(15.15 mL + 15.12 mL)/2 = 15.14 mL. DO NOT includes the volume from the ROUGH
titration.

However, if you obtain results as follows:

Volume of titration #1 = 15.15 mL

Volume of titration #2 = 16.12 mL
So, the difference in volume = ±0.97 mL (which is HIGHER than the given limit of
±0.10 mL). This means you CANNOT stop doing the titrations. You must continue until
the ±0.10 mL limit is obtained, as follows:

Volume of titration #1 = 15.15 mL

Volume of titration #2 = 16.12 mL
Volume of titration #3 = 16.08 mL

Using the volumes from consecutive titrations #2 and #3, the difference in volume
= ±0.04 mL (which is within the given limit of ±0.10 mL). This means now you may stop
doing the titrations. You will use the average volume as (16.12 mL + 16.08 mL)/2
= 16.10 mL. DO NOT includes the volume from the ROUGH titration and the volume
from titration #1.

18
 Make sure you understand this step. Show all results to the laboratory instructor to
ensure you are on the right track.
6. Record the readings from ALL titrations in the space provided on the datasheet.
7. When you are finished with the titration, empty the burette and rinse it at least twice with
tap water and once with distilled water.

QUESTIONS
1. Why phenolphthalein is used in this experiment?

2. NaOH is a hygroscopic compound and all NaOH solutions must be standardized before
it can be used for analysis. Using references, explain the given terms:

a. hygroscopic
b. standardization

19
 DATASHEET EXPERIMENT 5

INTRODUCTION TO TITRATION-DETERMINATION OF THE

MOLARITY AND CONCENTRATION OF SULPHURIC ACID
BY TITRATION WITH A STANDARD SOLUTION OF SODIUM
HYDROXIDE

Name : Date :

Student ID : Group :

RESULTS

Data:

ROUGH Titration Titration Titration Titration

Number of titration
Titration 1 2 3 4
Final burette reading (mL)

Initial burette reading (mL)

Volume of NaOH used (mL)

Molarity of standard NaOH solution (Mb) = ........................................M

(record the exact molarity as shown on the reagent bottle)

Volume of H2SO4 solution (Va) = ....................................... mL

Average volume of NaOH used (Vb) = ........................................ mL

20
Calculations:

1. Determine the unknown molarity of the H2SO4 (Ma) solution.

2. Determine the unknown concentration in g/L of H2SO4 solution.

Lecturer’s signature,

21