Flame Atomic Absorption Spectrometry

1 Flame Atomic Absorption Spectrometry Analytical Methods 2 Flame Atomic Absorption Spectrometry Analytical Methods Notices Agilent Technologies, Inc. 1989, 1991, 1994, 1999, 2000, 2004, 2007, 2010-2013, 2015, 2017 No part of this manual may be reproduced in any form or by any means (including electronic storage and retrieval or translation into a foreign language) without prior agreement and written consent from Agilent Technologies, Inc. as governed by United States and international copyright laws. Manual Part Number 8510000900 Edition Fourteenth edition, May 2017 Agilent Technologies Australia (M) Pty, Ltd.

2 679 Springvale Road Mulgrave, Victoria, Australia 3199 Safety Notices A CAUTION notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in damage to the product or loss of important data. Do not proceed beyond a CAUTION notice until the indicated conditions are fully understood and met. A WARNING notice denotes a hazard. It calls attention to an operating procedure, practice, or the like that, if not correctly performed or adhered to, could result in personal injury or death.

3 Do not proceed beyond a WARNING notice until the indicated conditions are fully understood and met. CAUTION WARNING Flame Atomic Absorption Spectrometry Analytical Methods 3 Important Warning WARNING Eye, Explosion and Hearing Hazard Aspiration of perchloric acid and perchlorates into a nitrous oxide-acetylene Flame can create an explosion hazard, which can result in death or serious personal injury including temporary or permanent impairment of hearing. Do not use perchloric acid unless it is absolutely essential for sample preparation.

4 If perchloric acid must be used, it may be possible to reduce the risk of an explosion by taking the following measures: Use an air-acetylene Flame instead of a nitrous oxide-acetylene Flame . Reduce the concentrations of perchloric acid and metal in all analytical solutions to the lowest practical level. The concentration of perchloric acid should be reduced in the digestion stage and further reduced by extending the fuming stage. Aspirate all solutions for the shortest practical period. Always aspirate distilled water between samples.

5 Minimize the aspiration of air. Use separate spray chamber/liquid trap assemblies for perchloric acid analyses and organic solvent analyses to prevent perchloric acid from mixing with organic solvent residues. NOTE When solvent extractions of perchloric acid solution are performed, some of the acid may dissolve in the organic solvent that is subsequently aspirated. In addition, if the organic solution is aspirated whilst floating on the surface of the acid, do not allow the capillary tube to drop below the organic solvent and suck up aqueous perchloric acid.

6 Clean the burner frequently never allow the burner to clog, and wash it thoroughly both inside and out. Minimize the amount of acetone which is carried over with the acetylene by: Cracking the bottle before use by gently opening the valve to check for any drops or spray of acetone. Any bottle showing acetone should be returned to the supplier for replacement. Storing and using the bottles in the vertical position. Using only one instrument per bottle. Using only instrument grade acetylene. Replacing bottles when the pressure drops to 750 kPa (100 psi).

7 Ensure that all safety covers are in position, and wear approved ear protectors and safety glasses. Ensure the pressure relief bung of the spray chamber can be easily removed by hand. Refit the bung according to the operation manual. 4 Flame Atomic Absorption Spectrometry Analytical Methods This page is intentionally left blank. Contents Flame Atomic Absorption Spectrometry Analytical Methods 5 Contents 1. Introduction 11 General 11 Safety Aspects 11 Reagents and Apparatus 12 Sample Preparation 12 Standard Preparation12 Automation 13 Matrix Effects 13 Precipitation 13 Physical Properties of Standard and Sample 13 Chemical Interferences 13 Incomplete Dissociation of Compounds 13 Ionization 14 Nebulizers 15 Organic Solvents 15 Adjustable Nebulizer 15 Spray Chamber 15 Recommended Instrument Parameters 15 Working Conditions (Fixed)

8 15 Working Conditions (Variable) 15 General References 16 2. Standard Conditions 17 Ag (Silver) 17 Recommended Instrument Parameters 17 Interferences 17 Al (Aluminium) 17 Recommended Instrument Parameters 17 Interferences 18 References 18 As (Arsenic) 18 Recommended Instrument Parameters 18 Interferences 19 References 19 Au (Gold) 19 Recommended Instrument Parameters 19 Interferences 19 B (Boron) 20 Recommended Instrument Parameters 20 Interferences 20 Ba (Barium) 20 Recommended Instrument Parameters 20 Interferences 21 Be (Beryllium) 21 Recommended Instrument Parameters 21 Interferences 21 References 21 Bi (Bismuth) 21 Recommended Instrument Parameters 21 Interferences 22 Vapor Generation Method 22 References 22 Ca (Calcium)

9 22 Recommended Instrument Parameters 22 Interferences 22 References 23 Cd (Cadmium) 23 Contents 6 Flame Atomic Absorption Spectrometry Analytical Methods Recommended Instrument Parameters 23 Interferences 23 Co (Cobalt) 23 Recommended Instrument Parameters 23 Interferences 24 References 24 Cr (Chromium) 24 Recommended Instrument Parameters 24 Interferences 24 References 25 Cs (Cesium) 25 Recommended Instrument Parameters 25 Interferences 25 Cu (Copper) 25 Recommended Instrument Parameters 25 Interferences 26 Dy (Dysprosium) 26 Recommended Instrument Parameters 26 Interferences 26 References 26 Er (Erbium) 27 Recommended Instrument Parameters 27 Interferences 27 References 27 Eu (Europium)

10 27 Recommended Instrument Parameters 27 Interferences 28 References 28 Fe (Iron) 28 Recommended Instrument Parameters 28 Interferences 28 References 28 Ga (Gallium) 29 Recommended Instrument Parameters 29 Interferences 29 Gd (Gadolinium) 29 Recommended Instrument Parameters 29 Interferences 30 Ge (Germanium) 30 Recommended Instrument Parameters 30 Interferences 30 Hf (Hafnium) 30 Recommended Instrument Parameters 30 Interferences 31 Hg (Mercury) 31 Recommended Instrument Parameters 31 Interferences 31 References 31 Ho (Holmium) 32 Recommended Instrument Parameters 32 Interferences 32 In (Indium) 32 Recommended Instrument Parameters 32 Interferences 32 Ir (Iridium) 33 Recommended Instrument Parameters 33 Interferences 33 References 33 K (Potassium)