CHEM 401- LEC
P3.1 NATURE OF ANALYTICAL CHEMISTRY
I. HISTORY OF ANALYTICAL METHODS
• Classical methods
- early years (separation of analytes) via
precipitation, extraction or distillation
o Qualitative
- recognized by color, boiling point,
solubility, taste
o Quantitative
- gravimetric or titrimetric
measurements
• Instrumental Methods
- newer, faster, more efficient
o Physical properties of analytes
- conductivity, electrode potential,
light emission absorption, mass to
charge ratio and fluorescence,
many more
II. QUALITATIVE METHODS OF ANALYSIS
● Chemical Test
- A reagent or reagents are added to the
sample to determine its composition.
➢ Benedict’s test for glucose
➢ Salkowski’s test for cholesterol
➢ Phosphate test shows yellow precipitate
● Flame Test
- detect the presence of certain elements,
primarily metal ions, based on each element's
characteristic emission spectrum.
➢ Sodium
- intense yellow flame
➢ Calcium
- red flame
Trans makers: Garrigues, M.
Editor: Ismael, Y.
John Michael Lico | February 02,2022
III. QUANTITATIVE ANALYSIS
Quantitative analysis can be divided into:
1. Classical Chemical Analysis
- It depends on simple classical technique to
determine the mass, volume, and the
corresponding techniques used in this type
of analysis are;
▪ Volumetric (measurement in volume)
▪ Gravimetric (measurement in mass)
2. Instrumental Analysis
- This analysis depends on the physical
properties of the sample where there is no
reaction involved.
- Instrumental analysis depends on more
complex devices such as spectroscopic
(interaction of light with matter) and electro
analytics (measures electrical potential,
resistance, etc.) which can help in estimate
the sample precisely especially in low
concentrations.
IV. QUANTITATIVE METHODS OF ANALYSIS
● Volumetric method
- the volume of a solution of a known
concentration, containing sufficient
reagent to react completely with the
analyte is measured.
➢ Acid-base titration
● Gravimetric method
- determine the mass of the analyte or
some compound chemically related to it.
- In this analysis, the analyte (substance of
interest) is converted to an insoluble
substance (precipitate) that is isolated
and weighed.
➢ In the analysis of lead (II), it is
precipitated as lead sulfate.
● Instrumentation methods
- with the use of scientific instruments
o Electroanalytical method
- study an analyte by measuring
potential and/or current in an
electrochemical cell containing the
analyte.
1

➢ Measuring pH using pH meter that uses
glass membrane electrode. The pH then
is related to the concentration of
hydronium ions in an analyte.
● Instrumentation methods
- with the use of scientific instruments
o Spectroscopic method
- based on the measurement of the
interaction between
electromagnetic radiation and
analyte atoms or molecules
➢ UV-VIS
Spectrophotometry
which measures the
concentration of solution
by the amount of light
absorbed by the
substance across UV-
Visible ranges of the
electromagnetic
spectrum.
Other Instrumentation methods:
• Flame photometry
• Mass spectrometry
• Chromatography
• Electrophoresis
• Optical activity
• Refractive Index
Capillary Electrophoresis
High-Performance Liquid Chromatography (HPLC)
Flame Photometry
Trans makers: Garrigues, M.
Editor: Ismael, Y.
CHEM 401- LEC
P3.1 NATURE OF ANALYTICAL CHEMISTRY
John Michael Lico | February 02,2022
V. BASIC ANALYTICAL PROCESSESS
● SELECT A METHOD
Considerations:
1. Level of Accuracy required
2. Number of samples to be analyzed
3. Complexity of sample and number of
components to be analyzed
● ACQUIRE THE SAMPLE
The sample should be carefully identified and
collected as to represent the entire bulk material
● PROCESS THE SAMPLE
1. Preparing laboratory samples
2. Defining replicate samples
3. Preparing Solutions
- perform physical or chemical changes
● ELIMINATING INTERFERENCES
o Interferences
- is a species that causes error by
enhancing or attenuating the quantity
being measured. Selection of
reagents or methods to be used that
minimize interferences should be
done. This is what we call selectivity.
● CALIBRATING AND MEASURING
CONCENTRATION OF PROPERTY
● CALCULATING RESULTS
- These computations are based on the raw
data collected in the measurement step,
the characteristics of the measurement
Instruments, and the stoichiometry of the
analytical reaction.
● EVALUATING THE RESULTS BY
ESTIMATING RELIABILITY
- The experimenter must provide some
measure of the uncertainties associated
with computed results if the data are to
have any value.
VI. TYPES OF SAMPLES
● Qualitative
- determination of identity of the
chemical species
● Quantitative
- determination of the relative amount of
the chemical specie in each amount of
sample
VII. SAMPLE SIZE
● Macro analysis
- amount of analyte is more than 0.10 grams
(100 mg)
o Suspected pollutant in a 1-gram soil
sample
● Semimicro analysis
- amount of analyte is between 0.010 – 0.10
grams
o Amount of drug in a 5-mg sample of
powder, determination of glucose in a
blood sample
● Micro analysis
- amount of analyte is 10-4 to 10-2 grams
o Determination of creatinine in a urine
sample
o
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 CHEM 401- LEC
P3.1 NATURE OF ANALYTICAL CHEMISTRY
John Michael Lico | February 02,2022

● Ultramicro analysis
- amount of analyte is less than 10-4 grams
o Determination of arsenic, boron, nickel
or silicon in the body through urine test

VIII. ANALYTE LEVEL

● Major Constituent
– amount of analyte is 1-100% of the
population
● Minor Constituent
– amount of analyte is 0.1-1% of the
population
● Trace Constituent
– amount of analyte is .01-0.1% (1ppb-
100ppm) of the population
● Ultratrace Constituent
– amount of analyte is below 1ppb

IX. SAMPLING
→ is the process of collecting a small mass of a material
whose composition accurately represents the bulk of
the material being sampled. It is the most difficult
aspect of analysis.
→ “Samples are analyzed, but species or
concentrations are determined”
● Real samples
- Analysis of real samples are complicated
because of the presence of sample matrix

➢ Sampling of human blood for the

determination of blood gases illustrates
the difficulty of acquiring a
representative sample from a complex
biological system. The concentration of
oxygen and carbon dioxide depends on
different variables. By applying a
tourniquet incorrectly or hand flexing by
the patient, this may cause the blood
oxygen concentration to fluctuate

Goal: Sampling process must ensure that the items

chosen are representative of the bulk of material or
population.
● Gross samples
- these are representative samples that are
collected from the source
● Laboratory samples
- these are samples that are reduced in size
and being homogenized so that they are
measurable in the lab

Trans makers: Garrigues, M. 3

Editor: Ismael, Y.