Total-Reflection X-Ray Fluorescence Analysis and Related Methods E-Book

Reinhold Klockenkämper

• Herausgeber: John Wiley & Sons
• Kategorie: Wissenschaft und neue Technologien
• Serie: Chemical Analysis: A Series of Monographs on Analytical Chemistry and Its Applications
• Sprache: Englisch

Seitenzahl: 989

Veröffentlichungsjahr: 2014

Beschreibung

Explores the uses of TXRF in micro- and trace analysis, and in surface- and near-surface-layer analysis
• Pinpoints new applications of TRXF in different fields of biology, biomonitoring, material and life sciences, medicine, toxicology, forensics, art history, and archaeometry
• Updated and detailed sections on sample preparation taking into account nano- and picoliter techniques
• Offers helpful tips on performing analyses, including sample preparations, and spectra recording and interpretation
• Includes some 700 references for further study

Leseprobe

CONTENTS

Cover

Series Page

Title Page

Copyright

Foreword

Acknowledgments

List of Acronyms

List of Physical Units and Subunits

List of Symbols

Chapter 1: Fundamentals of X-Ray Fluorescence

1.1 A Short History of XRF

1.2 The New Variant TXRF

1.3 Nature and Production of X-Rays

1.4 Attenuation of X-Rays

1.5 Deflection of X-Rays

References

Chapter 2: Principles of Total Reflection XRF

2.1 Interference of X-Rays

2.2 X-Ray Standing Wave Fields

2.3 Intensity of Fluorescence Signals

2.4 Formalism for Intensity Calculations

References

Chapter 3: Instrumentation for TXRF and GI-XRF

3.1 Basic Instrumental Setup

3.2 High and Low-Power X-Ray Sources

3.3 Synchrotron Facilities

3.4 The Beam Adapting Unit

3.5 Sample Positioning

3.6 Energy-Dispersive Detection of X-Rays

3.7 Wavelength-Dispersive Detection of X-Rays

3.8 Spectra Registration and Evaluation

References

Chapter 4: Performance of TXRF and GI-XRF Analyses

4.1 Preparations for Measurement

4.2 Acquisition of Spectra

4.3 Qualitative Analysis

4.4 Quantitative Micro- and Trace Analyses

4.5 Quantitative Surface and Thin-Layer Analyses by TXRF

4.6 Quantitative Surface and Thin-Layer Analyses by GI-XRF

References

Chapter 5: Different Fields of Applications

5.1 Environmental and Geological Applications

5.2 Biological and Biochemical Applications

5.3 Medical, Clinical, and Pharmaceutical Applications

5.4 Industrial or Chemical Applications

5.5 Art Historical and Forensic Applications

References

Chapter 6: Efficiency and Evaluation

6.1 Analytical Considerations

6.2 Utility and Competitiveness of TXRF and GI-XRF

6.3 Perception and Propagation Of TXRF Methods

References

Chapter 7: Trends and Future Prospects

7.1 Instrumental Developments

7.2 Methodical Developments

7.3 Future Prospects by Combinations

References

Index

End User License Agreement

List of Tables

Table 1.1

Table 1.2

Table 1.3

Table 1.4

Table 1.5

Table 1.6

Table 1.7

Table 1.8

Table 1.9

Table 1.10

Table 1.11

Table 2.1

Table 3.1

Table 3.2

Table 3.3

Table 3.4

Table 3.5

Table 3.6

Table 3.7

Table 3.8

Table 3.9

Table 3.10

Table 4.1

Table 4.2

Table 4.3

Table 4.4

Table 5.1

Table 5.2

Table 5.3

Table 5.4

Table 5.5

Table 5.6

Table 6.1

Table 6.2

Table 6.3

Table 6.4

Table 6.5

Table 7.1

List of Illustrations

Figure 1.1

Figure 1.2

Figure 1.3

Figure 1.4

Figure 1.5

Figure 1.6

Figure 1.7

Figure 1.8

Figure 1.9

Figure 1.10

Figure 1.11

Figure 1.12

Figure 1.13

Figure 1.14

Figure 1.15

Figure 1.16

Figure 1.17

Figure 1.18

Figure 1.19

Figure 1.20

Figure 1.21

Figure 1.22

Figure 1.23

Figure 1.24

Figure 1.25

Figure 1.26

Figure 1.27

Figure 1.28

Figure 1.29

Figure 1.30

Figure 1.31

Figure 1.32

Figure 1.33

Figure 1.34

Figure 1.35

Figure 1.36

Figure 1.37

Figure 1.38

Figure 2.1

Figure 2.2

Figure 2.3

Figure 2.4

Figure 2.5

Figure 2.6

Figure 2.7

Figure 2.8

Figure 2.9

Figure 2.10

Figure 2.11

Figure 2.12

Figure 2.13

Figure 2.14

Figure 2.15

Figure 2.16

Figure 2.17

Figure 2.18

Figure 2.19

Figure 2.20

Figure 2.21

Figure 2.22

Figure 2.23

Figure 2.24

Figure 2.25

Figure 2.26

Figure 3.1

Figure 3.2

Figure 3.3

Figure 3.4

Figure 3.5

Figure 3.6

Figure 3.7

Figure 3.8

Figure 3.9

Figure 3.10

Figure 3.11

Figure 3.12

Figure 3.13

Figure 3.14

Figure 3.15

Figure 3.16

Figure 3.17

Figure 3.18

Figure 3.19

Figure 3.20

Figure 3.21

Figure 3.22

Figure 3.23

Figure 3.24

Figure 3.25

Figure 3.26

Figure 3.27

Figure 3.28

Figure 3.29

Figure 3.30

Figure 3.31

Figure 3.32

Figure 3.33

Figure 3.34

Figure 4.1

Figure 4.2

Figure 4.3

Figure 4.4

Figure 4.5

Figure 4.6

Figure 4.7

Figure 4.8

Figure 4.9

Figure 4.10

Figure 4.11

Figure 4.12

Figure 4.13

Figure 4.14

Figure 4.15

Figure 4.16

Figure 4.17

Figure 4.18

Figure 4.19

Figure 4.20

Figure 4.21

Figure 4.22

Figure 4.23

Figure 4.24

Figure 4.25

Figure 4.26

Figure 4.27

Figure 4.28

Figure 4.29

Figure 4.30

Figure 4.31

Figure 4.32

Figure 4.33

Figure 4.34

Figure 5.1

Figure 5.2

Figure 5.3

Figure 5.4

Figure 5.5

Figure 5.6

Figure 5.7

Figure 5.8

Figure 5.9

Figure 5.10

Figure 5.11

Figure 5.12

Figure 5.13

Figure 5.14

Figure 5.15

Figure 5.16

Figure 5.17

Figure 5.18

Figure 5.19

Figure 5.20

Figure 5.21

Figure 5.22

Figure 5.23

Figure 5.24

Figure 5.25

Figure 5.26

Figure 6.1

Figure 6.2

Figure 6.3

Figure 6.4

Figure 6.5

Figure 6.6

Figure 6.7

Figure 6.8

Figure 6.9

Figure 6.10

Figure 6.11

Figure 6.12

Figure 6.13

Figure 6.14

Figure 7.1

Figure 7.2

Figure 7.3

Figure 7.4

Figure 7.5

Figure 7.6

Figure 7.7

Figure 7.8

Figure 7.9

Figure 7.10

Figure 7.11

Figure 7.12

Figure 7.13

Figure 7.14

Figure 7.15

Figure 7.16

Figure 7.17

Figure 7.18

Figure 7.19

Figure 7.20

Figure 7.21

Figure 7.22

Figure 7.23

Figure 7.24

Figure 7.25

Figure 7.26

Figure 7.27

Figure 7.28

Figure 7.29

Figure 7.30

Guide

Cover

Table of Contents

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Chemical Analysis

A Series of Monographs on Analytical Chemistry and its Applications

Series Editor

Mark F. Vitha

Volume 181

A complete list of the titles in this series appears at the end of this volume.

Total-Reflection X-Ray Fluorescence Analysis and Related Methods

Second Edition

Reinhold Klockenkämper

Alex von Bohlen

Leibniz-Institut für Analytische Wissenschaften - ISAS - e.V. Dortmund and Berlin, Germany

Copyright © 2015 by John Wiley & Sons, Inc. All rights reserved

Published by John Wiley & Sons, Inc., Hoboken, New Jersey

Published simultaneously in Canada

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Library of Congress Cataloging-in-Publication Data:

Klockenkämper, Reinhold, 1937- author.

Total-reflection X-ray fluorescence analysis and related methods.—Second edition / Reinhold Klockenkämper, Alex von Bohlen, Leibniz-Institut für Analytische Wissenschaften-ISAS-e.V., Dortmund und Berlin, Germany.

pages cm

Includes bibliographical references and index.

ISBN 978-1-118-46027-6 (hardback)

1. X-ray spectroscopy. 2. Fluorescence spectroscopy. I. Bohlen, Alex von, 1954- author.

II. Title.

QD96.X2K58 2014

543′.62–dc23

2014022279

Foreword

This second edition of the first and only monograph on total reflection X-ray fluorescence (TXRF) is thoroughly revised and updated with important developments of the last 15 years. TXRF is a universal and economic multielement method suitable for extreme micro- and trace analyses. Its unique and inherent features are elaborated in detail in this excellent monograph. TXRF represents an individual method with its own history and special peculiarities in comparison to other XRF techniques, and is well established within the community of elemental spectroscopy. In particular, TXRF has been realized and understood as a complementary rather than competitive instrument within the orchestra of ultramicro and ultratrace analytical instrumentation. In different round-robin tests, TXRF demonstrated its performance quite well in comparison with methods such as ET-AAS, ICP-OES, ICP-MS, RBS, and INAA.

Total reflection XRF is widely used in the analysis of flat sample surfaces and near-surface layers. Here, it may be applied as a nondestructive method especially suitable for the quality control of wafers in the semiconductor industry. It can be used for the determination of impurities at the ultratrace level and for mapping of the element distribution on flat surfaces. In addition to the composition, the nanometer-thickness of thin layers can be determined by tilting the sample at grazing incidence. Direct density measurements are a special and unique feature of TXRF after sputter-etching.

The authors have built a successful and well established team in the field of TXRF for about 25 years. In the first edition of this book, R. Klockenkämper described the principles and fundamentals of TXRF, the performance of analyses, and its applications. After his retirement, he cooperated with A. von Bohlen in order to examine the latest developments and to place TXRF in a leading position of analytical atomic spectrometry.

Several new sections of this second edition demonstrate the essential progress of TXRF. The new generation of silicon drift detectors, which are cooled thermo-electrically, is highlighted. About 80 synchrotron facilities around the whole world are listed—with work places that are dedicated solely to TXRF offering an extremely brilliant and tunable radiation. The previous fields of applications are enumerated and diversified, contamination control of wafers is shown to be standardized, and many new fields are represented especially in the life sciences. Combinations of different methods of spectrometry, such as NEXAFS and XANES, with excitation under total reflection build a trend and have been presented as future prospects. The worldwide distribution of TXRF's instrumentation and its different fields of applications are evaluated statistically.

This articulate monograph on TXRF with several color pictures provides fundamental and valuable help for present and future users in the analytical community. Many disciplines, such as geo-, bio-, material-, and environmental sciences, medicine, toxicology, forensics, and archaeometry can profit from the method in general and from this outstanding monograph in particular.

Geesthacht, May 2014

Prof. Dr. Andreas Prange

Helmholtz-Zentrum Geesthacht

Institute for Coastal Research

Head of the Department for

Marine Bioanalytical Chemistry

Acknowledgments

The authors are grateful to all the colleagues of our TXRF community for their laborious and important investigations and for manifold publications that build the basis of this monograph. Special thanks go to the attendees of the last conference on TXRF, who took part in the survey described in Chapter 6.

We also wish to thank Mrs. Maria Becker for carefully adapting the first edition in a readable word document, and for the diligent compilation of all references and all the data of synchrotron beamlines. Furthermore, we thank our former colleague Prof. Dr. Joachim Buddrus for proofreading chemical terms and formulas. Scientific and technical assistance of the Leibniz-Institut für Analytische Wissenschaften – ISAS – e.V., represented by members of the Executive Board, Prof. Dr. Albert Sickmann and Jürgen Bethke, is gratefully acknowledged. ISAS in Dortmund is supported by the Bundesministerium für Bildung und Forschung (BMBF) of Germany, by the Ministerium für Innovation, Wissenschaft und Forschung of North Rhine-Westphalia, and by the Senatsverwaltung für Wirtschaft, Technologie und Forschung, Berlin.

It is a pleasure for the authors to thank our friend Prof. Dr. Andreas Prange for providing a felicitous and penetrative foreword. The authors are also obliged to the publishers John Wiley and particularly to Bob Esposito and Michael Leventhal for their reliable assistance, and to Dr. Mark Vitha for his great care in editing the manuscript. We also pay tribute to the printers for the excellence of their printing, especially to our project manager, Ms. Shikha Pahuja, for the diligent organization.

List of Acronyms

AC

Alternating current

ADC

Analog-to-digital converter

AFM

Atomic force microscopy

AITR

Attenuated internal total reflection

ALS

Amyotrophic Lateral Sclerosis

AMC

Adiabatic microcalorimeter

ANNA

A

ctivity of Excellence and

N

etworking for

N

ano- and Microelectronics

A

nalysis

APS

Advanced photon source

or

American Physical Society

ASTM

American society for testing and materials

ATI

Atom institute

AXIL

Analytical X-ray analysis by iterative least squares

BB

Black body

BCR

Breakpoint cluster region (protein or gene)

or

British Chemical Standard - Certified reference material

BESSY

Berliner Elektronen Speicherring Gesellschaft für Synchrotronstrahlung

BRM

Blank reference material

CAS

Chemical Abstracts Services

CCD

Charge-coupled device

CHA

Concentric hemispherical analyzer

CHESS

Cornell high-energy synchrotron source

CMA

Cylindrical mirror analyzer

CMOS

Complementary metal oxides

CMOS

Complementary metal oxides semiconductor

CRM

Certified reference material

CVD

Chemical vapor deposition

CXRO

Center for X-ray Optics and Advanced Light Source

DC

Direct current

DCM

Double-crystal monochromator

DESY

Deutsches Elektronen Synchrotron

DIN

Deutsches Institut für Normung

DMM

Double multilayer monochromator

DORIS

Doppel Ring Speicher

EDS

Energy-dispersive spectrometry or spectrometer

EDTA

Ethylene-diaminetetraceticacid

EPMA

Electron probe microanalysis

ESCA

Electron spectroscopy for chemical analysis

ET-AAS

Electrothermal atomic absorption spectrometry

EXAFS

Extended X-ray absorption fine structure

FAAS

Flame atomic absorption spectrometry

FCM

Four-crystal monochromator

FEL

Free-electron laser

FET

Field effect transistor

FPS

Flat panel sensor

FT-IR

Fourier transform-infra red

FWHM

Full width at half maximum

GC-MS

Gas chromatography-mass spectrometry

GeLi

Ge(Li) detector; Germanium drifted with Lithium ions

GE-XRF

Grazing exit X-ray fluorescence

GF-AAS

Graphite furnace-atomic absorption spectrometry

GI-XRD

Grazing incidence X-ray diffractometry

GI-XRF

Grazing incidence X-ray fluorescence

GIE-XRF

Grazing incidence/exit X-ray fluorescence

GLP

Good laboratory practice

HASYLAB

Hamburger Synchrotron Strahlungslabor

HOPG

Highly ordered (oriented) pyrolytic graphite

HPGe

HPGe detector; high-purity Germanium

HPLC

High-performance liquid chromatography

HS

Humic substances

IAEA

International Atomic Energy Agency

IC

Integrated circuit

ICDD

International Centre for Diffraction Data

ICP

Inductively coupled plasma

ICP-MS

Inductively coupled plasma-mass spectrometry

ICP-OES

Inductively coupled plasma-optical emission spectrometry

IDMS

Isotope dilution-mass spectrometry

IEEE

Institute of Electrical and Electronics Engineers

IFG

Institut für Geräteentwicklung

IMEC

Interuniversity Microelectronics Center

INAA

Instrumental neutron activation analysis

IR

Infrared

IRMM

Institute of Reference Materials and Measurements

ISO

International Standard Organization

ITRS

International Technology Roadmap for Semiconductors

IUPAC

International Union for Applied Chemistry

JCPDS

Joint Committee on Powder Diffraction Standards

JFET

Junction Gate FET

KFA

Kernforschungsanlage

LED

Light emitting diode

LINAC

Linear accelerator

MBI

Max-Born Institut

MCA

Multichannel analyzer

MRI

Magnetic resonance imaging

MRT

Magnetic resonance tomography

NEXAFS

Near extended X-ray absorption fine structure

NIES

National Institute for Environmental Studies

NIST

National Institute of Standards and Technology

NSF

Nephrogenic Systemic Fibrosis

NSLS

National Synchrotron Light Source

PES

Photoelectron spectrometry

PGM

Plane grating monochromator

PIN

Positive-intrinsic-negative

PIXE

Proton or particle induced X-ray emission

PMM

Primary methods of measurement

PTB

Physikalisch-Technische Bundesanstalt

PVD

Physical vapor deposition

QM

Quality management

QXAS

Quantitative X-ray analysis system

RBS

Rutherford backscattering spectrometry

RMS

Root mean square (of the mean squared deviations)

ROI

Region of interest

RSD

Relative standard deviation

SAXS

Small angle X-ray scattering

SD

Standard deviation, absolute value

SDD

Silicon drift detector

SDi

Strategic Directions International

SEM

Scanning electron microscopy

SGM

Spherical grating monochromator

SiLi

Si(Li) detector; Silicium drifted with Lithium ions

SIMS

Secondary ion mass spectrometry

SOP

Standard operating procedure

SPM

Suspended particulate matter

SQUID

Superconducting quantum interference device

SR

Synchrotron radiation

SRM

Standard reference material

SSD

Solid-state detector

SSRL

Stanford Synchrotron Radiation Laboratory

STJ

Superconducting tunnel junction

STM

Scanning tunneling microscope or microscopy

SW

Standing wave

TDS

Total dissolved solids

TES

Transition edge sensor

TR

Total reflection

TRIM

Transport and range of ions in matter

TR-XPS

Total reflection XPS

TR-XRD

Total reflection XRD

TR-XRR

Total reflection XRR

TXRF

Total reflection X-ray Fluorescence

UCS

Ultra-Clean Society

UHV

Ultra-high-vacuum

ULSI

Ultra-large-scale integration

UPS

Ultraviolet photoelectron spectrometry

USB

Universal serial bus

UV

Ultraviolet

VAMAS

Versailles Project on Advanced Materials and Standards

VLSI

Very-large-scale integration

VPD

Vapor-phase decomposition

WDS

Wavelength-dispersive spectrometry or spectrometer

XAFS

X-ray absorption fine structure

XANES

X-ray absorption near-edge structure

XPS

X-ray photoelectron spectrometry

XRD

X-ray diffractometry

XRF

X-Ray fluorescence

XRR

X-ray reflectometry

XSW

X-ray standing waves

Chemical Compounds

APDC

Ammonium pyrrolidine dithiocarbamate

DNA

Deoxyribonucleic acid

h-BN

hexagonal form of boron-nitride

HMDTC

Hexamethylene-dithiocarbamate

mQC

murine Glutaminyl cyclase

MIBK

Methyl isobutyl ketone

NaDBDTC

Sodium dibutyldithiocarbamate

PEDOT:PSS

Polyethylenedioxythiophene: Polystyrene sulfonate

PEG

Polyethylene glycol

PFA

Polyfluoroalkoxy (polymers)

PEI

Polyethylenimine

PEO

Polyethylene oxide

PP

Polypropylenes

PTFE

Polytetrafluoro-ethylenes

PMMA

Polymethyl methacrylate

RNA

Ribonucleic acid

ROS

Reactive oxygen species

TEAB

Triethylamine borane

TMAB

Trimethylamine borane

TMB

Trimethylborazine

List of Physical Units and Subunits

A

ampere

a

year (annum)

°C

°Celsius

or

centigrade

C

coulomb

cm

centimeter

d

day

eV

electronvolt

F

farad

ft

foot

GHz

gigahertz

GeV

giga-electronvolt

g

gram

h

hour

or

hecto

hPa

hectopascal

Hz

hertz

in

inch

J

joule

K

kelvin

keV

kilo-electronvolt

kg

kilogram

km

kilometer

kPa

kilopascal

kV

kilovolt

kW

kilowatt

l

liter

m

meter

or

milli

mA

milliampere

MeV

mega-electronvolt

min

minute

ml

milliliter

mm

millimeter

mol

mole

mrad

milliradian

N

newton

nl

nanoliter

nm

nanometer

Pa

pascal

pl

picoliter

rad

radian

rpm

revolutions per minute

s

second

sr

steradian (squared radian)

T

tesla

V

volt

W

watt

kΩ

kiloohm

μl

microliter

μrad

microradian

Ω

ohm

%

per cent (10

−2

)

‰

per mill (10

−3

)

ppm

parts per million (10

−6

)

ppb

parts per billion (10

−9

)

ppt

parts per trillion (10

−12

)

List of Symbols

Symbols for Physical Quantities (in general they are unambiguous; in exceptional cases their meaning becomes clear by their individual context; for a detailed definition and distinction they can have indices)

α

Glancing angle of incident primary beam