Chapter 1

Introduction to
Chemical Analysis

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What is Analytical Chemistry?

Qualitative
Q
Quantitative

Analysis Methods
Chemical Analysis
Instrumental Analysis

HPT P.I Chp 1

Chemical Analysis
Volumetric glassware
glassware: pipet,
buret, volumetric flask,
conical flask, graduated
cylinder beaker
cylinder,
beaker,
y
Electronic analytical
balance, desiccator,
furnaces and ovens, fume
hoods,
hoods

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Chemical analysis

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Instrumental analysis
Automatic tiration
(potential titration)

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Instrumental analysis
y
VIS spectrophotometry
D t
Determine
i iiron iin water
t sample
l

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7
1

2
3

Analysis
y
Methods
Chemical Analysis

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Instrumental analysis

Chemical analysis

Instrumental analysis

Concentrations of
analytes : 10-2 M 10

< 10-4 M

-4 M

Labor work, long time

Automatic work, short

time

Simple tools

Expensive instruments

Low selectivity

High selectivity

Classify
fy of
f analytical
y
m
methods
Methods
Chemical analysis
Physical analysis
Physico-chemical
Ph sic ch mic l
analysis
Spectrometry
Electrochemical
analysis
Chromatography

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Classify of analytical methods

Concentrations of analytes in the smaple
High concentrations (x > 0.01%)
High concentration (x = 0,1 100%)
Low concentration (x = 0,01 0,1%)

Trace analysis (x < 0.01%)

Sample preparation
Wet sample preparation
Dry
D sample
l preparation
ti

HPT P.I Chp 1

Classify of analysis methods example

0.3000 g clay sample + 3 g
KOH kept in oven at 500oC and
KOH,
then dissolved in HCl

- Al 3+, Ca2+ , Mg2+ :

titrated
d with
h EDTA
E
standard
4+ Fe
-Ti
Ti4+,
F 3+ : determined
d t
i db
by
VIS spectrometry

Analyte

Al2O3 Fe2O3 CaO MgO

TiO2

Concentration (%) 28.12 0.48 1.25 0.56

0.08

a) Method for sample preparation is

b) Analysis methods for determination of Al2O3,
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Fe2O3, CaO, MgO v TiO2 are.

10

Lab skills

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11

The Analytical process

Define the
Problem

Select a
Method

Obtain a
Representative
Sample

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Perform
P
f
the
th
necessary chemical
separation

Perform the
M
Measurement

Calculation the
Results and
p
Report
12
12

The Analytical Process

1.Define the
Problem

4.

What is the problem

(Qualitative and/or
quantitative?),
q

2.Select a Method

Sample type, sample size,

analytes,
n y
, concentrations
n n r
n
(large amounts or small
amounts), how much tools
or instrument available,
cost,, speed,
p
, sensitivity,)
y, )

3.Obtain a
Representative
S
Sample
l

Sample
type/homogeneity/size

Prepare the Sample for Analysis

5.

Sample type (gas, solid,

li id) di
liquid),
dissolve
l ((pH,
H
reagent), concentration,
derivatize
Distillation precipitation
Distillation,
precipitation,
solvent extraction, solid
phase extraction

Perform the Measurement

- Titrations, chromatography or

electrophoresis
6.

Calculation the Results and

R
Report
t

Example

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14

Sample

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15

The Analytical
y
Process
Select a Method

Sample
l type, sample
l size,
i
analytes,
l
concentrations (large amounts or small
amounts trace level (parts per trillion (ppt)
amounts,
or parts per billion (ppb) or parts per million
(ppm))
How much is needed, how sensitivity the
method must be
Tools or instrument available (cost, speed,
sensitivity,)
y
Are methods available in the chemical
literature?

The Analytical
y
Process

Obtain a Representative Sample

Grab or spot sampling
The gross sample consists of several portions of the
material to be tested.
tested
The laboratory sample is a small portion of this, made
homogeneous.
g
The analysis sample is that actually analyzed.
Replicate samples, or replicates, are portions of
material of approximately the size that are carried
through an analytical procedure at the same time and in
the same way.

The Analytical Process - Example

Analysis of dicamba (pesticide) in
water

Problem (Qualitative and quantitative)

Select a Method
What kinds of water (lake, river, tap or
agricultural water)
Concentration (ppm (mg/L) or ppb (g/L) (1 mg =
10 3 g; 1 g = 10 6 g)
Instrument (available,
(available cost,
cost sensitivity - Gas
Chromatography (GC) or High Performance
Liquid Chromatography (HPLC))
Are methods available in the chemical
literature?

The Analytical Process - Example

Analysis of dicamba (pesticide) in
water

Problem (Qualitative and quantitative)

Select a M
Method
What kinds of water (lake, river, tap or
agricultural water)
Concentration (ppm (mg/L) or ppb (g/L) (1 mg =
10 3 g; 1 g = 10 6 g)
Instrument (available,
(available cost,
cost sensitivity - Gas
Chromatography (GC) or High Performance
Liquid Chromatography (HPLC))
Are methods available in the chemical
literature?

The Analytical Process - Example

Analysis of dicamba (pesticide) in
water
t
Problem (Qualitative and quantitative)
Select a Method
Sample
Sampling
S
li method
th d

Prepare the Sample for Analysis

Concentration
C
t ti (li
(liquid-liquid
id li id extraction,
t
ti
solid
lid
phase extraction)

The Analytical Process Example

Prepare the sample for Analysis
Sample type (liquid)
Analyte? (acidic organic Cl
compound).
n n r
(Y
(Yes))
Concentrate
Eliminating Interferences.

Water samples
1000 ml

CO 2 H
OCH 3

Cl

Adjust
djust to p
pH 2

Extraction
(dichloromethane)
(2 x 50 ml)

Reduce solvent to final volume

for HPLC

HPLC analysis

Liquid-liquid extraction

HPLC: High Performance liquid chromatography

The Analytical Process - Example

Analysis of dicamba in water
Perform
P f
the
h measurement
Calibration
Replicates
R li t
Blanks

Calculate the Results and Report

The Analytical
y
Process

- Calculate the Results and Reports

Laboratory Notebook
Laboratory
y Report
p
Measurement Uncertainty
Significant
g
Figures
g
Stoichiometric calculations