CHEM F313: Instrumental Methods of Analysis

Lecture 01
Analysis, Signal & Data
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Outline

 Today’s Class

 Overview of the course

 Analytical Chemistry
 Sensitivity and Detection Limit
 Handout discussion

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Analytical Chemistry
Analytical chemistry provides the methods and tools for getting
insight into the materials world for obtaining definite answers to

1. What ?
2. How much?
3. What arrangement/ structure/ form etc.?

Want more details?

www.acs-analytical.duq.edu/whatisanalyticalchem.html
Qualitative Analysis Quantitative Analysis

Defining the problem – what do we really need to know?

(not necessarily everything)
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 Analytical Chemistry

• Inorganic chemistry deals with elements, minerals, reactions etc

• Analytical chemistry deals with the qualitative and quantitative
analysis, to know the composition, structure, phase etc
• Analytical chemistry is now a central chemical discipline. It provides
critical information to clinical medicine, environmental studies,
forensics, food and drug safety
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Pioneer in Analytical Chemistry
Izaak Maurits Kolthoff
(1894–1993)
• Regarded as the father of
modern analytical chemistry.
• His research transformed the
ways by which scientists
separate, identify, and quantify
chemical substances.
• Total 945 publications.

Kolthoff's best-known research contribution was the development of

the "cold process" for producing synthetic rubber, which he undertook
under the U.S. synthetic rubber program during World War II.
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 Sample
MANY Professional societies have specified definite instructions for sampling
of given materials, such as
• ASTM (American Society for Testing and Materials),
• AOAC International (Association of Official Analytical Chemists)
• APHA (American Public Health Association)
 By appropriate application of experience and statistics, materials can be
sampled as accurately as possible.
 Complexity of sampling depends on the NATURE of the material

Relevant terms
GROSS SAMPLE: Sample constituted from portions from several parts of the
material (batches, boxes, sections)
LABORATORY SAMPLE: A portion of a homogeneous mixture of the gross
sample used for lab scale testing
ANALYSIS SAMPLE: The portion which is actually analyzed
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 Steps in Analysis
Sample need to be handled into appropriate form for it to be analyzed using a
particular method

• Destructive/ Invasive
• Non-destructive/ Non-invasive
Performing the measurement – YOU DECIDE THE MODE
SAMPLE PREPARATION is a CRUCIAL step
Analytical Technique:
The fundamental scientific phenomenon that has been proven to obtain
information for analysis of a substance. e.g. IR spectroscopy, UV, NMR, XRD etc
Analytical Method:
It is a specific application of a technique to solve an analytical problem. E.g.
Analysis of acetone using IR spectroscopy is a method
Instrumentation is the backbone to any Instrumental Method of
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Sensitivity
Sensitivity (S) is defined as the ratio of the change in instrument response
(I0) to a corresponding change in stimulus (e.g. C, conc. of analyte). This is
expressed as

This can also be expressed as the minimal concentration of an analyte

required to obtain a defined minimal signal value

• Linear response (constant

sensitivity)
Slope
• Sensitivity of the method is much
greater for B than A

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Sensitivity and Detection Limit

• Non-linear response (constantly

changing sensitivity)

• Measurement of substance C
become less sensitive with
increasing concentration

Detection limit

Detection limit is defined as the concentration of an analyte that gives a

minimal signal (x), significantly different from the “blank” or
“background”(xB). Current guideline is
x – xB = 3sB,
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Detection Limit
• The results of atomic absorption is shown here
• Two solutions of A and B elements have the equal conc
• The sensitivities of the instrument system are identical for both elements

• But detection limit for B is lower than A (because of the noise difference)
• It means the B can be detected at much lower value
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Signal & Noise

• Signal: Instrumental output responding to the chemical system of

interest (analytes)

• Noise: Instrumental output caused by other components (matrix)

and instrument during operation
Noise reduction is one primary consideration in obtaining meaningful
information during analysis

TWO principle methods for signal enhancement

1. Use of electronic hardware devices (filters etc.) or software
algorithms to process signals
2. Post-measurement mathematical methods (statistical)
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Conclusions

 Analytical Chemistry
 Sensitivity and Detection Limit

 Next Class

 Precision and Accuracy

 Electromagnetic waves
 Width of Spectral Lines

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