Chapter 2

Steps in a chemical analysis

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Plan of analysis 2.1
Before doing any quantitative analysis, the
:following questions should be answered
! what analytical information is needed -1
what analyses are necessary to provide these ! -2
information
! which analytical methods should be used -3
limits -
interferences -
2
instruments and equipment -
 Sampling 2.2
!What is the aim of sampling

To have a representative, measurable, sample can

be analyzed

Difficulties in sampling results from non-homogenous

sample particles size
Liquid samples i.e. water, are more homogenous than
solid ones i.e. soil
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Water samples are more homogenous than
wastewater samples
Types of samples
Grab: one single -
Composite: multi grab -

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Drying the sample 2.3
What is drying mean
Removing the water content

What is the goal of drying

Make the sample anhydrous-1
evaluating the water content (moisture) from the -2
:sample by
Moisture weight loss -
Collection of the moisture from the sample -
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Measuring the sample 2.4
The results of quantitative analysis are usually
reported in
% weight -1
% volume -2
% mole -3
,other units -4
.…i.e Molarities, Normality, ..PPM
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In measuring it is important for analytical steps to
use the most appropriate tool
i.e
- analytical balance in weighing small amounts
- The use of volumetric tools for liquid samples

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2.5 Dissolving the sample
The good solvent for a sample have to dissolve the
amount of the sample completely in as short time
as possible

The types of solvents used most commonly:

(principle like dissolve like)
Water: suitable for ionic polar substances -1
inorganic ones and some non-organic ones

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organic solvents: such as alcohols, ketones, -2
…,acetonitriles
mineral acids: concentrated or slightly diluted -3
.acids (i.e. HCl, H2SO4) specially for metals
Fusion: some samples fail to be dissolved in -4
any other ways, so they can be brought into
solution by fusing them with a high temperature
acid or base. i.e
Potassium pyrosulfate K2S2O7
Sodium carbonate Na2CO3
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2.6 separating interfering substances
The ideal quantitative method for a substance is
that can measure the maximum desired substance
in the presence of possible foreign substances.
(selectivity)
Interferences: species that present and prevent the
direct measurement or increase or decrease the
exact one of the analyte
Solution to interferences! !

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:Separation of interferences
Is important step to minimize the interferences
:It can be achieved by
precipitating: the analyte or the interferences -1
solvent extraction -2
ion exchange -3
adding inhibition substances -4

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2.7 measuring the desired substance
In this step, the quantity of the substance being
determined is actually measured
The measuring step is different from method to
another. i.e.
-In gravimetric: isolation and weighing the
precipitate
-In titremetric: measuring volumes of standard
solution required to react with substance.
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 The Measuring step usually needs some adjustment
of several conditions (pH), and within a specific
range (detection limit)
2.8 calculating and evaluating the results
The measurement step provide the data needed to
calculate the quantity of each species in the sample,
Then

expression of results with the appropriate unit is

needed and the final result expression is reported after
averaging when duplicates or replicates used, or after
correction by dilution factors when dilution is
performed
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