Analytical Chemistry 2

Analytical Chemistry 2
1 st lec

CHEMICAL ANALYSIS
Chemical analysis provides information about the composition of a sample:
Qualitative i.e. what is present in a sample.
Quantitative i.e. determine how much analyte is present in a sample

QUANTITATIVE CHEMICAL ANALYSIS

There are two broad categories of quantitati ve chemical analysis:

Classical methods of analysis. These are the older
methods of analyses and are based on e.g. volumetric
analysis

Instrumental methods of analysis.Tend to be
relatively modern and involve instrumentation

IS THERE A DIFFERENCE BETWEEN CLASSICAL AND INSTRUMENTAL
METHODS OF ANALYSIS
There is no real difference!
All forms of chemical analyses result in an analytical signal.
Classical analysis tends to use indicators to signal the presence of
an analyte or detect anendpoint. The analytical signal is usually a change in colour
or the appearnce of
precipitate.
Examples of classical methods of analysis you have carried out:
Quantitative: Acid/base titration using an indicator to determine the end.
Qualitative: Reaction of metal ions with selective reagents.

Instrumental analysis involves an instrument that converts a signal that is not usually
directly detectable into a form that is.
In an instrumental technique, some physico-chemical property of the analyte is measured
electronically, e.g. the absorption of light (if the analyte is coloured).
o electric potential
o Emission absorption or diffraction of radiation
o mass

Components of an instrument
You will come across a number of different instruments
throughout this module. You will use some expensive and
sophisticated instruments in the practical sessions. However,
most instruments contain 4 fundamental components:
Signal Generator: These produce the analytical signal from the
components of the sample. This may simply be the sample itself
or by a device which produces a signal which the analyte
interacts with. It is the change in this signal that is measured.

Input Transducer or Detector: This is a device that converts one type of signal
to

Signal processor: The signal processor modifies the signal
into a form that is more convenient for the readout device .
Usually this is simply amplification but can be others e.g. for
voltage AC DC .
Readout Device: This can range from a simple meter or
chart recorder or mostly likely with modern instruments a PC
based data system

.

In some cases components
may be merged together
e.g. detector and signal
processor often occur
together e.g. photomultiplier.

Why do we have Analysis of signal & Separation of signal?
Some methods of detecting a signal measure a property that is not specific to an analyte.
For example, take a solution containing Na
+
and K
+
ions.
If we measure the conductivity of the solution we cannot differentiate between Na
+
.and K
+
.
i.e. conductivity is not specific.
However, if we aspirate the solution into a flame, the
elements will emit radiation at a specific (different)
wavelength. We can measure this and differentiate
between Na
+
and K
+
ions (signal separated and
analysed).
We could carry out chromatography and separate the
ions then measure e.g. conductivity. (analytes
separated and individual analytes analysed).

Comparison of Analytical Methods
Approximate working ranges

Gravimetry ___________________
Titrimetry __________________________
Potentiometry ____________________________________
Electrogravimetry ____________________________
Voltammetry ________________________________
Photometry _____________________
Fluorimetry _____________________
Atomic Spectroscopy ______________________ _____________
Chromatography ___________________________________
g/L 10
-1
10
-2
10
-3
10
-4
10
-5
10
-6
10
-7
10
-8
10
-9
10
-10

Calibration
How do we relate the signal from the instrument to the concentration of a
solution?
The various methods of determining an analyte can be classified as either absolute or
relative. Absolute methods rely on accurately known fundamental constants for calculating
the amount of analyte, e.g. the atomic mass of elements in gravimetric analysis. However,
most instrumental methods are relative. Usually (hopefully!) the response of the instrument is
proportional to the analyte concentration, so we get:
Response Concentration
or
Response = Constant Concentration
and we can find the analyte concentration from the instrument output if we know the value of
the proportionality constant. We can find the proportionality constant by calibrating the
instrument. This is normally achieved by using a series of standard solutions. The instrument
response is measured for these known concentrations and a graph of response against
concentration of analyte can be constructed.

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