#1 ANACHEM

INTRODUCTION Qualitative analysis is what.

Quantitative analysis is how much.
What is it? What is it all about?
 Scientific discipline used to study
the chemical composition, For example: Application of Analytical
structure & behaviour of matter Chem & Questions They Answer.
 Measurement science consisting
of ideas & methods that are  Identification/Qualitative: What is
useful in all fiends of science, the identity of the substance in
engineering & medicine the sample?
 Involves the application of a  Detection: Does the sample
range of techniques & contain substance X?
methodologies to obtain & assess  Quantitative: How much of
qualitative, quantitative & substance X is in the sample?
structural information on the  Separation: How can the species
nature of matter of interest be separated from the
sample matrix for better
quantitation & identification.
 Qualitative analysis- is the
identification of elements, species
& or compounds present in the
sample. It establishes the
chemical identity of the species in
the sample.
 Quantitative analysis- is the
determination of the absolute or
relative amounts of elements,
species & or compounds present
in the sample.
 Structural analysis- is the
determination of the spatial
arrangement of atoms in an
element or molecule or the
identification of characteristic
groups of atoms (functional
groups). Analytical Chemistry involves
- Analyte- component of a sample ANALYSIS
that is determined or analysed.
- Matrix- the remainder of the
material or sample of which the An analysis involves several steps and
analyte forms a part. operations which depend on:
  The particular problem
 Your expertise
 The apparatus or equipment
available.
 The analyst should be involved
in every step.
- The most important aspect of an
analysis is to ensure that it will
provide useful & reliable data on
the qualitative & or quantitative
composition of a material or
structural information about the
individual compounds present.
- Selection of the best technique
3. Sampling
- Selection of a small sample to be
analysed; if it is heterogeneous,
special procedures need to be
used to ensure that a genuinely
representative sample is obtained
4. Sample pre-treatment of
conditioning.
- conversion of the sample into a
form suitable for detecting or
measuring; may involve
dissolving it, converting the
analyte into a specific chemical
form or separating the analyte
from components of a sample
(the sample matrix).

5. Qualitative/quantitative analysis.

6. Preparation of report or certificate

of analysis.

- Includes summary of the

analytical procedure, results &
their statistical assessment &
details of any problems
encountered.

STEPS IN ANALYSIS 7. Review of the original problem.

1. Definition of the problem.

2. Choice of a technique & method.

Case study illustrating the use of organic matrix to CO2 &
Analytical Chemistry to solve a problem H2O by the process of dry
in toxicology. ashing. It serves to free
the analyte from organic
Problem: Deer Kill.
material & convert it into
- The park ranger found a dead arsenic pentoxide As2O5.
white-tailed deer near a pond. The dry solid in each
The ranger enlisted the help of a crucible was then
chemist from a veterinary lab to dissolved in dilute HCl,
determine the cause of death. which converted As2O5 to
They observed that the grass soluble arsenic acid
surrounding the are was withered H3AsO4.
& discolored. They speculated
that a herbicide might have been
used. Common ingredient in
herbicides is arsenic in a variety
of forms but CH3AsO (OH)2 is
very soluble in water.
Selecting a method:
- Quantitative measurement is
found in the Association of
Official Analytical Chemists. In
this method, arsenic is distilled as
arsine, AsH3 & is then determined
by colorimetric measurements.
Sample collection:
- Dissected the deer, removed Measuring the amount of analyte:
both kidneys. Spectrophotometer
- Each kidney was homogenized in
a blender.  Highly colored complex of arsenic
was found to absorb light at a
Processing of the sample: wavelength of 535 nm.
- Three 10-g samples of the
homogenized tissue were placed
in porcelain crucibles. This
serves as replicates for analysis.
- Dissolving the sample.
• To obtain an aqueous
solution for analysis, it was
necessary to convert its
 results the investigators recommended
that the use of arsenical herbicides be
suspended in the wildlife area to protect
the deer & other animals that might eat
plants there.

#2 ANACHEM
ANALYTICAL TECHNIQUES AND
METHODS
Analytical techniques
Calculating the Concentration  Chemical or physic-chemical
ppm = (Absorbance -.005)/0.0282 processes that provide the basis
for analytical measurements.
Deer 1: (0.61 - 0.005)/0.0282 = 22 ppm
Analytical methods
Deer 2: (0.43 -0.005)/0.0282 = 15 ppm
 A method is a detailed set of
Arsenic in the kidney tissue of animals is instructions for a particular
toxic at levels above about 10 ppm. analysis using a specified
Grass Samples showed about 600 ppm technique.
arsenic. ANALYTICAL TECHNIQUES
Reliability of the data:

 The data were analyzed using

statistical methods. For each of
the standard arsenic solutions &
the deer samples, the average of
the three measurements were
calculated.

Conclusion:

In this analysis, the formation of the

highly colored product of the reactions
served both to confirm the probable
presence of arsenic & to provide a
SPECTROMETRIC TECHNIQUES &
reliable estimate of its concentration in
PRINCIPAL APPLICATIONS
the deer & in the grass. Based on their
SEPARATION TECHNIQUES &
PRINCIPAL APPLICATIONS
 MEASUREMENT DEVICES,
GLASSWARES & PLASTIC
WARES
A. Measuring mass
 Analytical balance has a
maximum capacity that ranges
from 1 g to several kilograms & a
precision at maximum capacity of
at least 1 part in 105.
1. Macro balance- most common
type of analytical balance with
maximum load of 160-200 g & a
precision of 0.1 mg.
2. Semi micro analytical- has a
maximum load of 10 to 30 g & a
precision of 0.01 mg.
3. Micro analytical- has a maximum
load of 1 to 3 g & a precision of
0.001 mg or 1 µg

#3 ANACHEM
B. Equipment & manipulations
associated with weighing

GLASSWARE
Types of glass:
C. Laboratory Glassware
 Used for storage, measurement
& containment
 Must meet certain tolerances of
accuracy; Class A
 Vessels holding or transferring
liquid are designed either “ to
contain (TC)” or “ to deliver (TD)”
 Divided into 2 main categories
according. to use:
1. containers/receivers (e.g.
beakers, test tubes, Erlenmeyer
flasks, reagent bottles)
2. volumetric ware (e.g. pipettes,
volumetric flasks, graduated
cylinders, burets)
 Thermal-resistant glass
(borosilicate)
- Resistant to heat, corrosion &
other thermal shock, has low
alkali content
- Used whenever heating or
sterilization by heat is employed
- Ex. Pyrex, Kimax
 Alumina-silicate glass
- High silica content which makes it
comparable to fused quartz in its
heat-resistance, chemical stability
& electrical characteristics
- It is strengthened chemically
rather than thermally
- Used for high precision analytical
work; radiation resistant; can also
be used for optical reflectors &
mirrors & cuvettes not used for
the general type of glassware
found in the lab
- Ex. Corex
 Acid-resistant & Alkali-resistant used for specific volume or
glass reagents or lab solutions

- High resistance to acids or alkali  Graduated Measuring

for use with strong acids or
alkaline solutions
- Boron free
- Ex. Vycor
 Low-actinic (amber-colored)
glass
- Reduce the amount of
transmitted through to
substance in the glassware
Cylinders
- Long, straight sided, cylindrical
piece of glassware with calibrated
markings
- Used to measure volumes of
liquid when a high degree of
accuracy is not essential; TD
light
the

 Flint glass (soda lime)

- Composed of a mixture of oxides

of silicon, calcium & sodium
- Inexpensive but low resistance to
heat & chemicals
- Ex. disposable test tubes
 Containers & receivers

- Beakers or Griffin low form

- Erlenmeyer flasks- often used for  Pipettes
preparing reagents & for titration
procedures - Are used for reconstitution of
- Test tubes controls & calibrators, preparing
- Reagent bottles serum or plasma dilutions &
aliquoting specimens
 Volumetric glassware - High degree of accuracy &
precision is required
- Must go through rigorous process
of volume calibration to ensure
accuracy of the measurements
required for lab determinations

 Volumetric flask- flasks with

round bulb at the bottom; TC
Classified according to:
Type
 Measuring or graduated

- delivers particular amount of

liquid contained between 2
graduation marks on a cylindrical
tube

 Mohr- calibrated between 2

marks on a stem

 Serologic- larger orifice;

graduation marks down to the
tip

 Volumetric or transfer

- calibrated to deliver a fixed

volume of liquid by drainage

- have cylindrical bulb joined at

both ends to narrow glass tubing

 Volumetric- calibrated to
deliver accurately a fixed
volume of dilute aqueous
solution

 Ostwald-Folin- similar to
volumetric but bulb is
closer to the delivery tip &
are used for accurate
measurement of viscous
fluids such as blood or
serum