Fundamental of

Kingdom of Saudi Arabia

Analytical Chemistry
Taibah University
Chemistry Department 232 CHEM

Practical
Fundamental of Analytical
Chemistry
Introduction
Use of Apparatus

A) Laboratory safety, Laboratory Information,

B) Introduction to Analytical Glassware and apparatus
 A) Laboratory safety
• Findthe location of these safety equipments in the
laboratory

Safety Shower
Eye Wash Fountain
Fire Extinguisher
Fire Alarm
Safety Chemicals
3
1. No food & No drinks.

2. You must wear protective lab wears (lab protective eye wear and proper
shoes that covers all your feet).

3. You should locate fire extinguisher, exit, safety shower(s), eye

fountains and fire blanket in your lab.

4. Do not remove any chemicals from fume hood.

5. Understand the danger of chemical you are working with and take care
during handling.

6. Inform the lab supervisor of any spill or broken glasses.

7. Clean around your working area and when you use the balance 4
 Lab Information
• Youshould have a good
understanding of the
purpose, details of the
procedure, the use of all
chemicals and any
significant hazards, and
the underlying science of
the experiment before
you come to lab.
 Report Format
• The report should include:
• Experiment ( )
(Write the experiment number and title)
• Aim:

It is a summary of the goals and objectives of the

experiment.
• Data:

Report all data, including appropriate units and

significant figures in tabular form according to the
attached file.
• Data Analysis and Results
You must clearly show each step of your
analysis, by writing out each equation used,
followed by the calculation plugging in the
relevant data, including the appropriate units
• Conclusions
• Discuss your results in the cases where values
are available for comparison, you should
quantify the difference between your
experimental values and the expected values.
• Discuss any problems encountered in your
experiment
B) Introduction to the use of Analytical Glassware
and apparatus
• Weight Measurements Tools
General Rules for Weighing
1) Never handle objects to be weighed with the fingers
2) Weigh at room temperature and avoid air convection currents
3) Never place chemicals directly on the pan
4) Always brush spilled chemicals off immediately with a soft
brush
5) Always close the balance case door before making the
weighing
• use a clean dry weighing bottle or dish

• Solid samples have to be dried to “constant weight” before

obtaining any accurate weight.
• Drying ovens and furnaces are used for drying and
igniting samples before weighing.

• Desiccators are used to cool a dried or ignited sample

using drying agents such as CaCl2
 Haw to Use Analytical Balance (Always use the
balance with extreme care)
1. Turn it on till the digital readout appear and show zero reading.
2. Open the sliding doors and clean it with a balance brush if the balance pan and
surrounding area is unclean.
3. Shut the doors and press the tare bar to insure appearance of zero readout.
4. Place the object to be weighed on the balance and measure the mass to  0.001 or 0.001
grams based on the uncertainty of the balance.
5. Use weighing paper, weighing dish or weighing bottles when weighing solids to protect
the balance. It should be on the balance pan and and it should not be touching the side.
6. Press the tare bar to insure appearance of zero readout.
7. Then add the required mass of solid and record the mass.
8. Always clean the balance carefully after use.
9. At the end, turn off the balance by raising the tare bar.
Volume Measurements Tools
The Lab. equipments commonly
used to measure liquid volumes are:
1) Graduate Cylinders (are usually
used for less accurate volume
compare to the following glass
wares)
2) Pipets,
3) Burets, and
4) Volumetric flasks.

Note: Borosilicate glassware (Pyrex,

Kimax) is normally used because it is
thermally stable.
11
1. Volumetric Flask
• Volumetric flasks are calibrated to contain an accurate
volume.
• This flasks are used to prepare standard solution usually by
transferring accurate mass or volume then it is diluted by
addition of a solvent to the mark.

2. Transfer or Volumetric Pipets:

They are used to accurately deliver a fixed volume.
A small volume normally remains in the tip and it is considered
during the pipet calibration.
12
3. Measuring Pipets:
• They are straight-bore pipets marked at different volumes.
• They are less accurate than volumetric pipets.

Reading a pipette

13

4.50 4.86 - 4.87 5.00

4. Burets
• A 50-mL buret is marked in 0.1 mL increments.
• It is good to about ±0.02 mL.
• Position a black field just below the meniscus.
• You have to avoid parallax error by reading at eye level

14
a) The meniscus of the liquid occurs at about 20.15? mL.
b) Meniscus illuminator occurs at about 0.7 mL.

15
 Analytical Chemistry

Analytical Chemistry
Quantitative
Qualitative

Manual
Instrumental

Volumetric or titrimetric
Gravimetric

Acid-
Base
Complexometri
c
Precipitation
Redox and
potentiometric 16
Volumetric Analysis

17
 Volumetric Analysis

 It is a general term for a method in quantitative

chemical analysis in which the amount of a
substance is determined by the measurement of the
volume that the substance occupies.

• Involves the preparations, storage, and

measurement of volume of chemicals for
analysis
• It is commonly used to determine the
unknown concentration of a known
reactant.
• Volumetric analysis is often referred to as titration

18
Types of Volumetric
Analysis
Acid-
base
titratio
n

Precipitati Complexome
on tric

Reduction-
oxidation
 TITRATION
 Titration
is a process in which a standard reagent is added to
a solution of an analyte until the reaction between
the analyte and reagent is judged to be complete.

 When the reaction involves an acid and a base,

the method is referred to as an acid-base
titration.

 When the reaction involves oxidation and

reduction, the method is referred to as a redox
titration.
21
TITRATION

• Two solutions are used:

• The solution of unknown concentration;
• The solution of known concentration – this is also known as the
standard solution

• Write
a balanced equation for the reaction between your two
chemicals
• Clean all glassware to be used with distilled water.
• Thepipettes and burettes will be rinsed with the solutions you are
adding to them

22
Process – The Setup
• The burette is attached to a clamp
stand above a conical flask
• Theburette is filled with one of the
solutions (in this case a yellow
standard solution)
• A pipetteis used to measure an
aliquot of the other solution (in this
case a purple solution of unknown
concentration) into the conical flask
• Prepare a number of flasks for repeat
tests
• Last,
an indicator is added to the
conical flask
23
Process – The Titration
• Read the initial level of liquid in the burette
• Turnthe tap to start pouring out liquid of the
burette into the flask. Swirl the flask
continuously. When the indicator begins to
change colour slow the flow.
• When the colour changes permanently, stop
the flow and read the final volume. The
volume change needs to be calculated (and
written down). This volume is called a titre
• Repeat the titration with a new flask now
that you know the ‘rough’ volume required.
Repeat until you get precise results

24
 Titrations

Titrant: The known solution added to the solution of

unknown concentration.

Equivalence point
 Quantity of added titrant is the exact amount
necessary for stoichiometric reaction with the analyte
- Ideal theoretical result

End point:
 What we actually measure
- Marked by a sudden change in the physical property of
the solution
- Change in color, pH, voltage, current, absorbance of
light, presence/absence ppt.

25
 Titrations

End point
 What we actually measure

CuCl Titration with NaOH

Before any addition of NaOH After the addition of End Point

8 drops of NaOH
26
 End Point & Equivalent Point
END POINT EQUIVALENT POINT
The point at which an equivalent or
The point at which the reaction is
stoichiometric amount of titrant is
observed to be completed
added to the analyte
The end point signal frequently occurs
at some point other than the equivalent
The point at which the reaction is
point.
complete
- tells the analyst to stop adding
TITRANT and record the volume.
Theoretically at the equivalence point
The selected indicator should change we can calculate the amount of titrant
color very near to the equivalent point. that is required to react EXACTLY
with the amount of analyte present.

27
How you can detect the End point?
• By using indicators

• Indicators are weak acids that

have a different color than their
conjugate base form.
• Each indicator has its own pH
range over which it changes color.
• An indicator can be used to find
the equivalence point in a titration
as long as it changes color in the
small volume change region
where the pH rapidly changes.
Strong base titrated
with a strong acid.
28
The Acid and Base Forms of the
Indicator Phenolphthalein

29
Types of Acid-Base Titrations
• Thequality of the titration depends on the strength of the acids
and bases you use. This, in turn, will affect the resulting pH curve.

Strong Base-Strong Acid Strong Acid-Strong Base

30
How you can detect the End point?
• By using indicators

• Indicators are weak acids that

have a different color than their
conjugate base form.
• Each indicator has its own pH
range over which it changes color.
• An indicator can be used to find
the equivalence point in a titration
as long as it changes color in the
small volume change region
where the pH rapidly changes.
Strong base titrated
with a strong acid.
31