Analytical Chemistry

Chapter 1

Dept. of Chemistry
University of Santo Tomas
 What is Analytical Chemistry?
It is the branch of chemistry concerned with the
ANALYSIS of chemical substances
2 types of ANALYSIS:
identifying substances present in a material
(qualitative analysis)
determining the exact amount or
concentration of the identified substance(s)
(quantitative analysis)
Improvement in techniques of chemical measurement
Quantitative vs. Qualitative Analysis
Analyze vs. Determine

Samples are ANALYZED,

while specific constituents are DETERMINED

The constituent of interest = ANALYTE

In analyzing blood for its chloride content,

we determine the chloride concentration

DETERMINATION of blood glucose

ANALYSIS of blood glucose
USES/APPLICATIONS OF ANALYTICAL CHEMISTRY
USES/APPLICATIONS OF ANALYTICAL CHEMISTRY

Medicine

clinical lab tests guide physicians

in diagnosing diseases &
in tracking progress during recovery

e.g.
monitoring of blood glucose in diabetics
levels of ionized Ca in blood used to
diagnose parathyroid disease
USES/APPLICATIONS OF ANALYTICAL CHEMISTRY

Industry

quality control of raw materials and finished products

e.g.
household products (shampoo, toothpase)
paints
fuels
pharmaceuticals
USES/APPLICATIONS OF ANALYTICAL CHEMISTRY

Environment

testing for the presence of suspected pollutants

to assess environmental quality

e.g.
carbon monoxide in air
cyanide in oceans
heavy metal ions in water supply
USES/APPLICATIONS OF ANALYTICAL CHEMISTRY

Food

nutritional value determined by the chemical analysis

of proteins and carbohydrates, as well as
vitamins and minerals

contaminants such as pesticide residues, formalin,

etc. are also determined
USES/APPLICATIONS OF ANALYTICAL CHEMISTRY

Forensics

gun powder testing on an accused murderer

DNA testing to prove paternity

Figure 1-1
The relationship
between analytical
chemistry, other
branches of chemistry,
and the other sciences.
The central location of
analytical chemistry in
the diagram signifies its
importance and the
breadth of its
interactions with many
other disciplines.
 CLASSIFICATION OF ANALYTICAL METHODS
(BASED ON EXTENT OF ANALYSIS)

1. COMPLETE (Ultimate) ANALYSIS

determination of ALL constituents

e.g. CBC
elemental analysis of gasoline

2. PARTIAL ANALYSIS

determination of SOME constituents only

e.g. amount of salicylic acid impurity
in an aspirin tablet
Classification of Analytical Methods
(based on the size of sample available for analysis)

ANALYSIS SAMPLE MASS SAMPLE VOL

1. Macro > 100 mg > 100 L

2. Semimicro 10 - 100 mg 50-100 L
3. Micro 1 - 10 mg < 50 L
4. Ultramicro < 1 mg ---
Classification of Analytical Methods
(based on the amount of analyte)

1. MACRO ANALYSIS

determination of the major constituent (>1%)

2. TRACE ANALYSIS

determination of constituent that is present in

small amounts (<0.1%)
Classification of Analytes

1. Major constituent: > 1% of sample

2. Minor constituent: 0.01 1% of sample
3. Trace constituent: 0.001 0.01% of sample
4. Ultratrace constituent: < 0.001% of sample
 CLASSIFICATION OF ANALYTICAL METHODS
BASED ON TYPE OF FINAL MEASUREMENT INVOLVED

1. GRAVIMETRIC ANALYSIS
weight of analyte or a chemically
related compound is measured
2. TITRIMETRIC ANALYSIS
volume of a solution containing sufficient reagent
to react completely with the analyte is measured
3. PHYSICOCHEMICAL (INSTRUMENTAL)
ANALYSIS
measurement of some physical or chemical
properties, such as conductivity, electrode potential,
light absorption or emission, mass-to-charge ratio,
and fluorescence
*1 & 2, a.k.a CLASSICAL METHODS of ANALYSIS
Classical vs. Instrumental Methods of Analysis
Classical Instrumental
separation of analytes perform multianalyte analysis
by precipitation, measure lower concentration:
extraction, or distillation
10-12-10-6 M / 10-3-10-6 M
qualitative analysis by shorter analysis time
reaction of analytes with
reagents that yield
compatible with computers
products that could be amenable to automation
recognized by their analyze more samples
colors or solubilities less personnel
generally cheaper perform analysis that are difficult or I
generally of higher impossible using classical methods
precision
 TYPES OF INSTRUMENTAL METHODS
A. Spectroscopic Methods

gamma ray
x-ray
ultraviolet
Visible
Infrared
Interaction
Microwave
radiowave Sample
(solid, liquid, gas)
Electromagnetic
radiation
 TYPES OF INSTRUMENTAL METHODS
A. Spectroscopic Methods

Emission of radiation x-ray, UV, visible, electron, Auger Emission

spectroscopy; fluorescence, phosphorescence, and
luminescence

Absorption of radiation X-ray, UV, visible, IR absorption spectrophotometry ;

photoacoustic spectroscopy; nuclear magnetic
resonance, and electron spin spectroscopy

Scattering of radiation Turbidimetry, nephelometry, Raman spectroscopy

Refraction of radiation Refractometry; interferometry

Diffraction of radiation X-ray and electron diffraction methods

Rotation of radiation Polarimetry; optical rotary dispersion; circular

dichroism
TYPES OF INSTRUMENTAL METHODS (CONT.)
B. Chromatographic Methods
Gas chromatography
High performance liquid chromatography
Supercritical fluid chromatography

C. Electrochemical Methods
electric potential Potentiometry and chronopotentiometry
electric charge Coulometry
electric current Polarography; amperometry
electric resistance Conductometry

D. Miscellaneous Methods
mass-to-charge ratio Mass spectrometry
rate of reaction Kinetic methods
thermal properties Thermal conductivity and enthalpy methods
Radioactivity Activation and isotope dilution methods
Steps in
Chemical
Analysis

Fig 1-2, p. 6
STEPS IN A QUANTITATIVE ANALYSIS
Level of accuracy
time and money
Number of samples
Nature of sample
and number of
components
Sample collected for
analysis should be
representative of the
composition of the bulk
material from which it was
taken from
May be omitted in some cases
For solids-drying, grinding, mixing
For liquids-sealed to prevent
evaporation and contamination
Preparation of replicate samples
Dissolution of sample in suitable
solvent
 STEPS IN A QUANTITATIVE
May be omitted in
ANALYSIS
some cases
Interferences are
species other than
the analyte that
affect the final
measurement e.g. silicates,
Apply proper polymers,
separation method animal tissues
(pption, extraction) Heating with
strong acids,
strong bases,
Convert analyte to OA, RA
a form that is Igniting in air
compatible with
measurement step
e.g., Mn2+ MnO4-
STEPS IN A QUANTITATIVE ANALYSIS
Physical or chemical property, X,
should ideally be directly
proportional to the concentration,
cA, of the analyte: cA = k X
Calibration process required to
determine value of k

Calculators
Computer software

Give a measure of statistical

uncertainties and confidence
limits
Feedback
system

Fig 1-3, p.11