Method development using ICP-MS and LA-ICP-MS and their application in environmental and material science [Elektronische Ressource] / Izmer Andrei

Horvath

Informations

• Publié par: johannes_gutenberg-universitat_mainz
• Publié le: 01 janvier 2006
• Nombre de lectures: 13
• Langue: English
• Poids de l'ouvrage: 2 Mo

Extrait

Method development using ICP-MS and
LA-ICP-MS and their application in environmental and material science






Dissertation
zur Erlangung des Grades
„Doktor der Naturwissenschaften“
(Dr. rer. nat.)




Fachbereich Chemie, Pharmazie und Geowissenschaften
der Johannes Gutenberg-Universität Mainz



Izmer Andrei
geboren in Berezino, Weissrussland

 
Mainz 2006

Index
1. Introduction........................................................................................................ 3
1.1. Motivation ............................................................................................................................ 3
1.2. Summary of results............................................................................................................... 6
1.2.1. Environmental research ................................................................................................. 6
1.2.2. Material science............................................................................................................. 8
2. Measurements techniques................................................................................ 10
2.1. Radionuclide analysis in environmental samples............................................................... 10
2.1.1. Overview of most important techniques for radionuclides analysis............................ 10
2.1.2. Capability of ICP-MS and LA-ICP-MS for analysis of radionuclides........................ 11
2.2. Surface analysis in material science ................................................................................... 15
2.2.1. Overview of most important techniques for surface analysis...................................... 15
2.2.2. Capability of LA-ICP-MS for surface analysis ........................................................... 17
3. Fundamentals ................................................................................................... 20
3.1. ICP-MS............................................................................................................................... 20
3.1.1. Sample introduction systems....................................................................................... 21
3.1.2. Ion generation in inductively coupled plasma............................................................. 23
3.1.3. Ion extraction............................................................................................................... 24
3.1.4. Mass analyzers............................................................................................................. 25
3.1.4.1. Quadrupole mass spectrometer............................................................................. 26
3.1.4.2. Double-focusing sector field mass spectrometer.................................................. 27
3.1.5. Ion detection ................................................................................................................ 29
3.1.5.1. Faraday cup........................................................................................................... 30
3.1.5.2. Electron multiplier................................................................................................ 30
3.1.5.3. “Daly”-type detector............................................................................................. 32
3.2. Reaction/collision cells in ICP-MS .................................................................................... 33
3.3. Sample introduction in ICP-MS by means of laser ablation (LA-ICP-MS)....................... 36
3.3.1. Principles ..................................................................................................................... 36
3.3.2. Instrumentation............................................................................................................ 39
3.4. Capillary electrophoresis .................................................................................................... 41
3.4.2. Principles ..................................................................................................................... 41
3.4.1. Experimental setup ...................................................................................................... 43
4. Experimental .................................................................................................... 45
4.1. Instrumentation................................................................................................................... 45
4.1.1. ICP-MS........................................................................................................................ 45
4.1.2. Sample introduction systems....................................................................................... 49
4.1.2.1. Design of sample introduction device for iodine isotopic measurements............ 49
4.1.2.2. Capillary electrophoresis ...................................................................................... 49
4.1.2.3. Laser ablation ICP-MS with cooled LA-chamber................................................ 51
4.1.2.4. Laser ablation using a microflow nebulizer adapted on an ablation chamber...... 52
4.2. Samples, standard reference materials and sample preparation ......................................... 54
5. Results and discussions .................................................................................... 57
5.1. Application of ICP-MS and LA-ICP-MS to environmental science.................................. 57
1
129 1275.1.1. Determination of I/ I isotope ratios in liquid solutions and environmental soil
samples by ICP-CC-QMS ........................................................................................... 57
1295.1.1.1. Figures of merit of ICP-CC-QMS for determination of I................................. 58
129 1275.1.1.2. Sample introduction device for direct determination of I/ I isotope ratio in
soils.................................................................................................................................... 64
1295.1.1.3. Improvement of the LOD for I in sediments .................................................... 67
5.1.2. Determination of lanthanides in standard samples by CE-ICP-MS ............................ 70
905.1.3. Determination of Sr by ICP-MS ............................................................................... 74
905.1.3.1. Application of the ICP-MS with collision cell for Sr determination................. 75
5.1.3.2. Cool plasma mode for separation of Sr and Zr..................................................... 77
5.1.4. Determination of U isotopic ratios on the surface of biological samples by
LA-ICP-MS ................................................................................................................. 80
5.1.5. Determination of uranium by on-line LA-ID-ICP-MS in NIST-SRM 1515............... 86
5.2. Application of LA-ICP-MS in materials science ............................................................... 90
5.2.1. Investigation of diffusion processes in NiCrAlY-based alloys using LA-ICP-MS..... 91
5.2.1.1. Optimization of the surface analytical method..................................................... 91
5.2.1.2. Quantification semiquantitatively and by solution-based calibration .................. 96
5.2.1.3. Lateral element distribution of NiCrAlY-based coatings on high temperature
alloy ...................................................................................................................... 97
6. Conclusion....................................................................................................... 106
7. References ....................................................................... 108

















2
1. Introduction

1.1. Motivation

Developments of new technologies in material science, space research, clinical medicine or
energy production strongly requests analytical methods for measuring the chemical composition
of applied materials to meet the constantly arising demands on improved quality and safety.
Recently, the European spallation source (ESS) project has been started which aims the design
and construction of a next generation facility for research with neutrons. The neutron beams
produced in such spallation source can be used for fundamental and applied research in physics,
chemistry, biotechnology, engineering and material science.
In particular, the ESS project requires further improvement of analytical techniques for
monitoring of particular radionuclides as well as for the analysis of chemical composition of
special construction materials. Numerous spallation products are present in the irradiated
material, whereas their composition and induced activity depends on the applied target material.
For example, when irradiating a tantalum target with high-energy protons a significant amounts
-1 -1of lanthanides with different abundances in the µg g to low ng g concentration range are
[1]produced . Information about nuclide abundances and their concentrations is necessary for
accessing the dose levels and for assuring irradiation safety when handling these types of