HEAVY METALS DETERMINATION BY ATOMIC
ABSORPTION SPECTROMETER
Aim of Course
• Developing further knowledge and understanding of some core scientific
concepts and principals about heavy metals contaminations
• Improving ability to understand and express scientific knowledge about
instrumentation
• Preparing for the further study and practical work for the determinations of heavy
metals
• Preparing for further practice applications in Science and Engineering
Scope of Learning
This book is basically about
• The heavy metals determination in water waste water,
• Heavy metal contamination in water and wastewater
• Sources of heavy metal contaminations and health implication
• Instrumental techniques used in heavy metal testing
• Concept and principal of Atomic Absorption Spectrometer instrumentation
• Methods of determination of Hydride Mode, Graphite Furnace Mode and Flame
Mode
• Solutions and Reagent preparation for each determination
• Calibration and quality control of the testing results.
i
, Table of Contents
1 HEAVY METALS & TRACE ELEMENTS ........................................................... 1
1.1 Definition ............................................................................................................ 1
1.2 Sources of Heavy Metals .................................................................................... 2
1.3 Heavy Metal Toxicity........................................................................................... 3
1.4 Methods of Heavy Metal Determination .............................................................. 5
2 INSTRUMENTATION ......................................................................................... 6
2.1 Atomic Absorption Spectrometer ........................................................................ 6
2.2 Working Principal of Atomic Absorption Spectrometer (AAS) ............................. 6
2.3 Major Components of Atomic Absorption Spectrometer (AAS) .......................... 6
2.3.1 Light Source ....................................................................................................... 7
2.3.2 Atomizer ................................................................................................... 7
2.3.3 Light Separation........................................................................................ 7
2.3.4 Detector .................................................................................................... 8
2.3.5 Background Correction System ................................................................ 8
2.4 Working Modes of Atomic Absorption Spectrometers (AAS) .............................. 8
2.4.1 Flame Mode .............................................................................................. 9
2.4.2 Hydride Generation Mode (HGAAS) ....................................................... 10
2.4.3 Graphite Furnace Mode .......................................................................... 12
3 DETERMINATION OF HEAVY METALS ......................................................... 14
3.1 Testing/Determination of Arsenic by Atomic Absorption Spectrometer ............. 14
3.1.1 Purpose .................................................................................................. 14
3.1.2 Scope ..................................................................................................... 14
3.1.3 References ............................................................................................. 14
3.1.4 Instrument ............................................................................................... 14
3.1.5 Principle .................................................................................................. 14
3.1.6 Glassware Required ............................................................................... 15
3.1.7 Reagent Required................................................................................... 15
ii
, 3.1.8 Preparation of 1000 ppb Stock Solution of Arsenic in Deionized
Water ...................................................................................................... 15
3.1.9 Preparation of Working Standards of Arsenic ......................................... 16
3.1.10 Calibration of AAS for Arsenic in Hydride Generation Mode ................... 17
3.1.11 Analysis of Arsenic on AAS .................................................................... 18
3.2 Testing/Determination of Copper (Cu) on Flame Mode of Atomic
Absorption Spectrometer.................................................................................. 19
3.2.1 Purpose .................................................................................................. 19
3.2.2 Scope ..................................................................................................... 19
3.2.3 References ............................................................................................. 19
3.2.4 Instrument ............................................................................................... 20
3.2.5 Principle .................................................................................................. 20
3.2.6 Glassware ............................................................................................... 20
3.2.7 Reagents ................................................................................................ 20
3.2.8 Preparation of Stock Solution and Working Standards of Copper
for Flame Mode....................................................................................... 20
3.2.9 Calibration of Copper on Flame Mode .................................................... 22
3.2.10 Analysis of Copper on Flame Mode ........................................................ 22
3.3 Testing/Determination of Manganese (Mn) on Flame Mode of Atomic
Absorption Spectrometer.................................................................................. 24
3.3.1 Purpose .................................................................................................. 24
3.3.2 Scope ..................................................................................................... 24
3.3.3 References ............................................................................................. 24
3.3.4 Instrument ............................................................................................... 24
3.3.5 Principle .................................................................................................. 24
3.3.6 Glassware ............................................................................................... 24
3.3.7 Reagents ................................................................................................ 25
3.3.8 Preparation of Stock Solution and Working Standards of
Manganese for Flame Mode ................................................................... 25
3.3.9 Calibration of Manganese on Flame Mode ............................................. 26
3.3.10 Analysis of Copper on Flame Mode ........................................................ 27
iii
, 3.4 Testing/Determination of Zinc (Zn) on Flame Mode of Atomic Absorption
Spectrometer.................................................................................................... 29
3.4.1 Purpose .................................................................................................. 29
3.4.2 Scope ..................................................................................................... 29
3.4.3 References ............................................................................................. 29
3.4.4 Instrument ............................................................................................... 29
3.4.5 Principle .................................................................................................. 29
3.4.6 Glassware ............................................................................................... 29
3.4.7 Reagents ................................................................................................ 30
3.4.8 Preparation of Stock Solution and Working Standards of Zinc for
Flame Mode ............................................................................................ 30
3.4.9 Calibration of Zinc on Flame Mode ......................................................... 31
3.4.10 Analysis of Zinc on Flame Mode ............................................................. 32
3.5 Testing/Determination of Lead (Pb) by Atomic Absorption Spectrometer
on Graphite Furnace Mode............................................................................... 33
3.5.1 Purpose .................................................................................................. 33
3.5.2 Scope ..................................................................................................... 34
3.5.3 References ............................................................................................. 34
3.5.4 Instrument ............................................................................................... 34
3.5.5 Principle .................................................................................................. 34
3.5.6 Glassware ............................................................................................... 34
3.5.7 Reagents ................................................................................................ 34
3.5.8 Preparation of 1000 ppb Stock Solution of Lead ..................................... 34
3.5.9 Preparation of Working Standards for Lead ............................................ 35
3.5.10 Calibration for Lead on Graphite Furnace Mode ..................................... 37
3.5.11 Analysis of Lead on Graphite Furnace .................................................... 37
3.6 Testing/Determination of Chromium (Cr) on Graphite Furnace Mode ............... 39
3.6.1 Purpose .................................................................................................. 39
3.6.2 Scope ..................................................................................................... 39
3.6.3 References ............................................................................................. 39
iv
ABSORPTION SPECTROMETER
Aim of Course
• Developing further knowledge and understanding of some core scientific
concepts and principals about heavy metals contaminations
• Improving ability to understand and express scientific knowledge about
instrumentation
• Preparing for the further study and practical work for the determinations of heavy
metals
• Preparing for further practice applications in Science and Engineering
Scope of Learning
This book is basically about
• The heavy metals determination in water waste water,
• Heavy metal contamination in water and wastewater
• Sources of heavy metal contaminations and health implication
• Instrumental techniques used in heavy metal testing
• Concept and principal of Atomic Absorption Spectrometer instrumentation
• Methods of determination of Hydride Mode, Graphite Furnace Mode and Flame
Mode
• Solutions and Reagent preparation for each determination
• Calibration and quality control of the testing results.
i
, Table of Contents
1 HEAVY METALS & TRACE ELEMENTS ........................................................... 1
1.1 Definition ............................................................................................................ 1
1.2 Sources of Heavy Metals .................................................................................... 2
1.3 Heavy Metal Toxicity........................................................................................... 3
1.4 Methods of Heavy Metal Determination .............................................................. 5
2 INSTRUMENTATION ......................................................................................... 6
2.1 Atomic Absorption Spectrometer ........................................................................ 6
2.2 Working Principal of Atomic Absorption Spectrometer (AAS) ............................. 6
2.3 Major Components of Atomic Absorption Spectrometer (AAS) .......................... 6
2.3.1 Light Source ....................................................................................................... 7
2.3.2 Atomizer ................................................................................................... 7
2.3.3 Light Separation........................................................................................ 7
2.3.4 Detector .................................................................................................... 8
2.3.5 Background Correction System ................................................................ 8
2.4 Working Modes of Atomic Absorption Spectrometers (AAS) .............................. 8
2.4.1 Flame Mode .............................................................................................. 9
2.4.2 Hydride Generation Mode (HGAAS) ....................................................... 10
2.4.3 Graphite Furnace Mode .......................................................................... 12
3 DETERMINATION OF HEAVY METALS ......................................................... 14
3.1 Testing/Determination of Arsenic by Atomic Absorption Spectrometer ............. 14
3.1.1 Purpose .................................................................................................. 14
3.1.2 Scope ..................................................................................................... 14
3.1.3 References ............................................................................................. 14
3.1.4 Instrument ............................................................................................... 14
3.1.5 Principle .................................................................................................. 14
3.1.6 Glassware Required ............................................................................... 15
3.1.7 Reagent Required................................................................................... 15
ii
, 3.1.8 Preparation of 1000 ppb Stock Solution of Arsenic in Deionized
Water ...................................................................................................... 15
3.1.9 Preparation of Working Standards of Arsenic ......................................... 16
3.1.10 Calibration of AAS for Arsenic in Hydride Generation Mode ................... 17
3.1.11 Analysis of Arsenic on AAS .................................................................... 18
3.2 Testing/Determination of Copper (Cu) on Flame Mode of Atomic
Absorption Spectrometer.................................................................................. 19
3.2.1 Purpose .................................................................................................. 19
3.2.2 Scope ..................................................................................................... 19
3.2.3 References ............................................................................................. 19
3.2.4 Instrument ............................................................................................... 20
3.2.5 Principle .................................................................................................. 20
3.2.6 Glassware ............................................................................................... 20
3.2.7 Reagents ................................................................................................ 20
3.2.8 Preparation of Stock Solution and Working Standards of Copper
for Flame Mode....................................................................................... 20
3.2.9 Calibration of Copper on Flame Mode .................................................... 22
3.2.10 Analysis of Copper on Flame Mode ........................................................ 22
3.3 Testing/Determination of Manganese (Mn) on Flame Mode of Atomic
Absorption Spectrometer.................................................................................. 24
3.3.1 Purpose .................................................................................................. 24
3.3.2 Scope ..................................................................................................... 24
3.3.3 References ............................................................................................. 24
3.3.4 Instrument ............................................................................................... 24
3.3.5 Principle .................................................................................................. 24
3.3.6 Glassware ............................................................................................... 24
3.3.7 Reagents ................................................................................................ 25
3.3.8 Preparation of Stock Solution and Working Standards of
Manganese for Flame Mode ................................................................... 25
3.3.9 Calibration of Manganese on Flame Mode ............................................. 26
3.3.10 Analysis of Copper on Flame Mode ........................................................ 27
iii
, 3.4 Testing/Determination of Zinc (Zn) on Flame Mode of Atomic Absorption
Spectrometer.................................................................................................... 29
3.4.1 Purpose .................................................................................................. 29
3.4.2 Scope ..................................................................................................... 29
3.4.3 References ............................................................................................. 29
3.4.4 Instrument ............................................................................................... 29
3.4.5 Principle .................................................................................................. 29
3.4.6 Glassware ............................................................................................... 29
3.4.7 Reagents ................................................................................................ 30
3.4.8 Preparation of Stock Solution and Working Standards of Zinc for
Flame Mode ............................................................................................ 30
3.4.9 Calibration of Zinc on Flame Mode ......................................................... 31
3.4.10 Analysis of Zinc on Flame Mode ............................................................. 32
3.5 Testing/Determination of Lead (Pb) by Atomic Absorption Spectrometer
on Graphite Furnace Mode............................................................................... 33
3.5.1 Purpose .................................................................................................. 33
3.5.2 Scope ..................................................................................................... 34
3.5.3 References ............................................................................................. 34
3.5.4 Instrument ............................................................................................... 34
3.5.5 Principle .................................................................................................. 34
3.5.6 Glassware ............................................................................................... 34
3.5.7 Reagents ................................................................................................ 34
3.5.8 Preparation of 1000 ppb Stock Solution of Lead ..................................... 34
3.5.9 Preparation of Working Standards for Lead ............................................ 35
3.5.10 Calibration for Lead on Graphite Furnace Mode ..................................... 37
3.5.11 Analysis of Lead on Graphite Furnace .................................................... 37
3.6 Testing/Determination of Chromium (Cr) on Graphite Furnace Mode ............... 39
3.6.1 Purpose .................................................................................................. 39
3.6.2 Scope ..................................................................................................... 39
3.6.3 References ............................................................................................. 39
iv
