AN INTRODUCTION TO

ANALYTICAL CHEMISTRY

Dr. Naureen Shehzadi

 What is analytical chemistry?
“Analytical chemistry deals with chemical characterization of natural
and artificial materials”
 What is pharmaceutical analysis?
Application of analytical procedures to determine the identity, quality,
purity and strength of drugs and chemicals.
 What is analyte?
Chemical constituent of interest in an analytical procedure is called
analyte.
 What is analysis?
It refers to separation, identification and characterization of analyte in
the given sample.
 What is sample?
A representative part of the material to be characterized is called
sample.

Gross sample:
Several portions of the material to be tested
Laboratory sample:
Small portion of the gross sample, made homogenous
Analysis sample:
A small representative sample from laboratory sample to be analyzed
 Areas of chemical analysis
Identification
What is the identity of the substance?
Detection
Does the given sample contain the substance?
Separation
How can the specie of interest be separated/isolated from the sample
matrix for better identification and quantitation?
Quantification
How much of the substance is present in the sample?
 Information generated from analysis
Identity
Presence or absence of analyte in the given sample
Quality
Quality of analyte (pure/impure)
Purity
Percentage of analyte actually present in the given sample with
reference to the labeled claim
Strength
Quantity of analyte in the given sample
CATEGORIES OF CHEMICAL ANALYSIS

Chemical analysis

Qualitative analysis Quantitative analysis

 Qualitative analysis (What it is?)
It provides information about the identity of an atomic, molecular or
biomolecular specie.
OR
The determination of the components of an unknown sample.

e.g.
Molisch’s test identifies that the given specie is carbohydrate
 Quantitative analysis (How much?)
It provides numerical information as to the relative amounts of
species.
OR
The determination of the quantity of the components in a sample.

e.g. Amount of drug in the blood/urine sample determined using HPLC

ANALYTICAL PROCESS
Understanding and defining
the problem

Analysis process Selecting a method for analysis

Sampling

Preparation of sample for

analysis

Analysis (measurement)

Calculation of results and

reports
 Understanding and defining the problem
What is the problem?
What needs to be found?
What is the required outcome of analysis?
Qualitative results or quantitative results
What will the information be used for? And who will use it?
When will it be needed?
How accurate and precise the analysis needs to be?
Budget?
 Selecting a method for analysis
Depends on;
• Sample type (solid/liquid/gas)
• Sample preparation needed/not needed
• Size of sample
• Constituents in the sample
– Major (>1%)
– Minor (0.1-1%)
– Trace (<1%)
– Ultra-trace (PPM or less)
• Concentration and range (sensitivity needed?)
• Selectivity needed (interferences/not)?
• Accuracy and precision requirements?
 Conti…
• Instruments/tools available
• Cost
• Speed
• Availability of expertise
• Automation needed/not
• Availability of analytical methods in standard books or literature
 Sampling
Material needs to be sampled for analysis may be solid, liquid or gas.
It may be homogenous or heterogeneous in its composition.

Sampling from homogenous material:

Single time “grab sample” randomly taken

Sampling from heterogeneous material:

Several individual samples of the material randomly taken

Avoid contamination while sampling!

Preparation of sample for analysis
 Measurement of sample being analyzed (weight/volume)
 Dissolution of the sample (In case of solid)
 Making of dilutions (serial/parallel, in triplicates)
 Need of ashing/digesting
 Need to concentrate the analyte
 Need to derivatize the analyte
 Need to adjust solution conditions (pH)
 Need of chemical separations

Always run a blank!

SERIAL DILUTION
PARALLEL DILUTION
 Analysis (measurement)
Already available method Method not available
1. Construction of calibration 1. Development of analytical
curve of standard method
2. Analysis of sample 2. Validation of the method
1. Linearity
2. Range
3. Accuracy
4. Precision
5. Specificity
6. Sensitivity
7. Robustness
3. Analysis of sample
 Calculation of results and reports
Extrapolation of analysis sample results to the laboratory sample
and gross sample level
Results reported as mean value ± standard deviation

99.99% Purity ± 0.45 SD

 ANALYZE Vs. DETERMINE
The sample is analyzed to determine the amount of analyte

COMPLETE Vs. PARTIAL ANALYSIS

An analysis is complete if all the constituents in a sample are
analyzed whilst incomplete if only selected constituents are analyzed
 1. What is a blank?
2. List some separation processes
employed in analytical chemistry?
3. Serially dilute a compound from a stock

CLAS
solution of concentration 100mg/mL to
10 folds
4. Write parallel dilutions of amikacin
sulphate stock solution having

S
concentration 1mg/mL to yield 20
dilutions
5. What do it mean by validation?
6. A drug inspector takes some samples

TASK
for inspection of whether the drug is
actually present or not, what kind of
analysis be performed on the sample?