Читать книгу X-Ray Fluorescence Spectroscopy for Laboratory Applications - Michael Haschke, Jörg Flock - Страница 4

1 Chapter 2Figure 2.1 Parts of the continuous spectrum of an X-ray tube.Figure 2.2 Line energy as a function of the atomic number.Figure 2.3 Electron transitions with the corresponding line names.Figure 2.4 Fluorescence yield as a function of the atomic number.Figure 2.5 Contributions to the attenuation coefficient for X-radiation of (...Figure 2.6 Elastic and inelastic scattering coefficients for selected elemen...Figure 2.7 (a) Influence of the sample type on the intensity of the scattere...Figure 2.8 Spectra of PMMA, Al, Ti, and Ni demonstrating the different scatt...Figure 2.9 PW 1540 from Philips.Figure 2.10 Analyst 0700 from KEVEX.Figure 2.11 Steps for an analytical procedure.

2 Chapter 3Figure 3.1 Information depth of fluorescence radiation.Figure 3.2 Information depth for different matrices.Figure 3.3 Cd intensities measured on polymer samples of different thickness...Figure 3.4 Analyzed volume limited by the measurement geometry.Figure 3.5 Specimen generated by sampling from a melt.Figure 3.6 Influence of surface roughness on the measured fluorescence inten...Figure 3.7 Dependence of fluorescence intensity on grinding time.Figure 3.8 Dependence of fluorescence intensity on the morphology of the sam...Figure 3.9 Press die for to produce pellets from small-sized materials.Figure 3.10 Pressed pellet (a) and cross section of a pressed pellet in bind...Figure 3.11 Influence of grain size distribution and different hardness of s...Figure 3.12 Calibration curves for the same powder material prepared as pres...Figure 3.13 Arrangement of layers of melting agent and sample in the fusion ...Figure 3.14 (a) Pt crucibles over a gas burner. (b) Temperature profile of t...Figure 3.15 Cooling curve to produce glass pellets.Figure 3.16 Glassy (a) and milky, too quickly cooled fusion bead (b).Figure 3.17 Sample cup for the analysis of liquids.Figure 3.18 Transmission of low-energy radiation of sample cup films.

3 Chapter 4Figure 4.1 Energy resolution of different ED spectrometer (blue) and WD spec...Figure 4.2 Spectrum of stainless steel, measured by WDS and EDS: (a) low-ene...Figure 4.3 Influence of the selected lattice plane (a) and the collimator si...Figure 4.4 Spectra of a gold alloy measured with a proportional counter and ...Figure 4.5 Energy dependence of energy resolution of ED-detectors (FWHM, ful...Figure 4.6 Detection efficiency of prop-counter and scintillation counter.Figure 4.7 Detection efficiency of ED-detectors.Figure 4.8 Throughput of ED-detectors and their influence on the detector re...Figure 4.9 Peak shape changes for very high count rates of WD spectrometers....Figure 4.10 Effect of the count rate on the peak-to-background ratios.Figure 4.11 Comparison of the ratios of the relative standard deviation (rel...Figure 4.12 Low-energy spectral background due to a Compton-induced escape e...Figure 4.13 Escape and pile-up peak of Ti radiation (y-axis in square root s...Figure 4.14 Pt spectrum measured without and with Al filter (y-axis in squar...Figure 4.15 Shelf and tail contributions to a Cu line (y-axis in square root...Figure 4.16 Principle layout of EDS instruments (MCA, multichannel analyzer)...Figure 4.17 Handheld instruments from various manufacturers: (a) XL5, Thermo...Figure 4.18 Portable instruments of different manufacturers: (a) FXL, Thermo...Figure 4.19 Various energy-dispersive spectrometers: (a) Epsilon 3, Panalyti...Figure 4.20 Principle layout of WDS instruments.Figure 4.21 A selection of wavelength-dispersive X-ray spectrometers: (a) Ze...Figure 4.22 A selection of multichannel X-ray spectrometers: (a) S8 Lion, Br...Figure 4.23 Principle setup of a TXRF instrument (MCA, multichannel analyzer...Figure 4.24 Total reflection X-ray spectrometers: (a) TXRF-310, Rigaku Corp....Figure 4.25 Layout of an X-ray spectrometer with monoenergetic excitation.Figure 4.26 Spectrum of an oil sample excited with Mo radiation.Figure 4.27 Measurement geometry for the excitation with polarized radiation...Figure 4.28 Energy-dispersive instruments using polarized radiation: (a) XEP...Figure 4.29 Basic layouts of position-sensitive X-ray spectrometers with a c...Figure 4.30 Coating thickness instruments with collimators: (a) XDAL, Helmut...Figure 4.31 Instruments utilizing X-ray optics for beam focusing: (a) M4 Tor...Figure 4.32 Macro-X-ray fluorescence spectrometer for the investigation of l...Figure 4.33 Confocal geometry for the investigation of 3D elemental distribu...Figure 4.34 Grazing incident measurement geometry.Figure 4.35 Grazing exit measurement geometry.

4 Chapter 5Figure 5.1 Characteristics of the Fe intensity for the Cr–Fe binary material...Figure 5.2 Characteristics of the Fe intensity for the Fe–Ni binary material...Figure 5.3 Characteristics of the Fe intensity for the Cr–Fe–Ni material sys...Figure 5.4 Excitation spectra for different tube parameters (y-axis in squar...Figure 5.5 Influencing the measured spectrum with an Al filter.Figure 5.6 Reduction of diffraction peaks and the scattered Rh-L radiation w...Figure 5.7 Transmission of X-rays in different measurement atmospheres.Figure 5.8 Standard deviation and error of repeated measurements.Figure 5.9 Energies of X-ray lines.Figure 5.10 Frequency distribution of X-ray lines as a function of the atomi...Figure 5.11 Typical line overlaps for energy-dispersive spectrometers.Figure 5.12 Methods for the determination of the peak intensity: (a) WDS ins...Figure 5.13 Spectrum of a tool steel sample fitted with pure element peaks (...Figure 5.14 Calibration curves based on net intensities (continuous line) an...Figure 5.15 Setting of background points.Figure 5.16 Background fit of an energy-dispersive measured spectrum (y-axis...Figure 5.17 Calculation and use of a calibration curve.Figure 5.18 Bracketing method for highly accurate analysis with two differen...Figure 5.19 Representation of the trueness of an analysis method: (a) compar...Figure 5.20 Determination of the limit of detection from the calibration fun...Figure 5.21 Deviations of the gold concentrations measured with SDD and prop...Figure 5.22 Comparison of the accuracy of standard-based and standard-free m...Figure 5.23 Typical calibration curves for the emission and absorption signa...Figure 5.24 Measurable layer thickness ranges for certain element groups and...Figure 5.25 Corrected calibration curve using two reference samples.Figure 5.26 Scheme of a principal component analysis.

5 Chapter 6Figure 6.1 Error distribution in the analytical process.Figure 6.2 Target model for the illustration of random and systematic errors...Figure 6.3 Results of repeated measurement with a high (a) and lower (b) sta...Figure 6.4 Specification limits of a process.Figure 6.5 Gaussian distribution of measuring results.Figure 6.6 Gaussian distributions with different standard deviations.Figure 6.7 Statistical distribution around the expected value and shifted by...Figure 6.8 Total measurement uncertainties of analytical results.

6 Chapter 7Figure 7.1 Setup of an atomic absorption spectrometer.Figure 7.2 Principal setup of an arc-spark spectrometer.Figure 7.3 Basic setup of an optical emission spectrometer with excitation b...Figure 7.4 Basic setup of a laser-induced breakdown spectrometer.Figure 7.5 Basic setup of a mass spectrometer.Figure 7.6 Excitation cross-sections of different elements for monoenergetic...

7 Chapter 8Figure 8.1 Absorption of radiation in a material layer.Figure 8.2 Half-width of organic tissues for different energies.

8 Chapter 9Figure 9.1 Pressed pellet of metals chips in a ring of steel.Figure 9.2 Change in measured Cr content as a function of grinding passes.Figure 9.3 Influence of acids on the measured signal of Cu.Figure 9.4 Spectra of high-purity gold with varying small silver contents (yFigure 9.5 Change of the boron intensity in a boron-silicate glass for sever...Figure 9.6 Matrix influence of different polymers on the Br-K intensities (A...Figure 9.7 Elastic and inelastic scattered tube radiation of various pure po...Figure 9.8 Comparison between mass fractions of hydrogen (a), carbon (b), an...Figure 9.9 Sample carriers for abrasion analyses: corundum disk for conventi...Figure 9.10 Relative differences for a bulk and an abrasive analysis of stee...

9 Chapter 10Figure 10.1 Limits of detection for geological material, measured with an ED...Figure 10.2 Limits of detection for element oxides in coal for EDS instrumen...Figure 10.3 Ferroalloy with different grain size.Figure 10.4 Crucible for remelting ferroalloys.Figure 10.5 Process scheme for the digestion of ferro-silicon.Figure 10.6 Sampling of a slag sample from the melt with a sampling probe (a...Figure 10.7 Spectra of a blank and a loaded filter.Figure 10.8 Element distribution along the trace of collected dust.Figure 10.9 Examples of raw secondary fuels (a) and crushed material (b).Figure 10.10 Pellets produced at different temperatures have different stren...

10 Chapter 11Figure 11.1 Plastic film with a drop of a solution (a), spectra of a solutio...Figure 11.2 LiTRap-sample holder, not used (a) and with metal particles from...Figure 11.3 Samples after complexation: a Chelex^®-100-pellet with synth...

11 Chapter 12Figure 12.1 Spectra of water fleas measured at conventional excitation geome...Figure 12.2 Element-dependent sensitivities of a TXRF spectrometer.Figure 12.3 Critical sample thicknesses for neglecting the matrix interactio...Figure 12.4 Secondary electron microscope (SEM) image of a TXRF sample (drie...Figure 12.5 Spectra of different amounts of fine-grained Zn-particles. esc, ...Figure 12.6 Limits of detection in aqueous solutions.Figure 12.7 Spectrum of NIST SRM 1640 – fresh water.Figure 12.8 Analysis results for Hg determined with and without EDTA-complex...Figure 12.9 TXRF spectrum of an environmental aerosol sample, particle size ...Figure 12.10 Calibration curve for platinum in blood serum.Figure 12.11 TXRF spectrum of lung tissue of a foundry worker.Figure 12.12 Depth profiles of As ions in a Si wafer determined with TXRF, R...

12 Chapter 14Figure 14.1 Calibration curves for Au-layers for both Au-L- and Au-M-fluores...Figure 14.2 Calibration curve for Al layer thickness based on Fe absorption....Figure 14.3 Results of coating thickness measurements in relative and emissi...Figure 14.4 0.2 mm wide Au/Ni/Cu coated area on PCB using a spot size of 0.1...Figure 14.5 Simulated spectra of a 5 μm NiP/Fe system with different P conte...Figure 14.6 Comparison of given and analyzed P contents in NiP layers.Figure 14.7 Spectrum of an Au–Pd–Ni layer system.Figure 14.8 Design of CIGS solar cells.Figure 14.9 Spectrum of a SnPb solder system.Figure 14.10 Layer structure form a vertical and tilted polished section.Figure 14.11 Element distribution in a cross section (a) and along a line pe...Figure 14.12 Spectra of a CIGS layer system measured with grazing incidence....Figure 14.13 Intensity profiles of the components of the CIGS layer system f...Figure 14.14 Distribution of pigment layers on both sides of a parchment (a)...

13 Chapter 15Figure 15.1 Example of a metal particle; the analysis spot is marked.Figure 15.2 Sample cup with particles.Figure 15.3 Spectra of two particles of the same material but of different s...Figure 15.4 Scores for different principal components for measurements on gl...Figure 15.5 Spectra of a PE specimen with toxic elements close to the RoHS l...Figure 15.6 Peak overlap of Br, As, Hg, and Pb.

14 Chapter 16Figure 16.1 Typical geological samples for distribution analyses: (a) bore c...Figure 16.2 Sum spectrum of the complete mapping (y-axis in square root scal...Figure 16.3 Element distributions of the bore core for (a) Si, (b) Ca, (c) T...Figure 16.4 Superposed element distribution of the pitchblende including ins...Figure 16.5 Element distributions of the overlapped As-Kα and Pb-Lα-lines (a...Figure 16.6 Sum and maximum pixel spectrum of the pitchblende (a) (y-axis in...Figure 16.7 Element distributions of thin sections measured with different s...Figure 16.8 (a) Photograph of a PCB of a mobile phone, (b) distribution of s...Figure 16.9 Image of a coin of 2 Reichsmark minted in Munich (D) (a) and spe...Figure 16.10 Distribution of Ag (a) and Cu (b) of a 2 Reichsmark coin.Figure 16.11 St. Jerome with the Bible. (a) Photograph of the painting. (b) ...Figure 16.12 Element distributions of a glass specimen: (a) Si distribution,...Figure 16.13 Relative standard deviations of repeated measurements on the sa...

15 Chapter 17Figure 17.1 High-throughput screening for the development of a catalyst.Figure 17.2 (a) Sample carrier with 10⁴ samples and (b) relations between ag...Figure 17.3 Energy-dispersive measured X-ray spectra of few sodium salts....Figure 17.4 Score plot of the principal components of different chemicals....Figure 17.5 S-Kβ spectra of different sulfur compounds.Figure 17.6 Al-Kβ spectra of Al nitride and Al oxide.Figure 17.7 Calibration curve for the concentration ratio of Al₂O₃/AlN by us...Figure 17.8 Si-Kβ spectra of SiO₂ and SiC.

16 Chapter 18Figure 18.1 Automated laboratory with instruments for sample preparation and...Figure 18.2 Scheme of an automated blast furnace laboratory for the analysis...Figure 18.3 Scheme of a preparation automat for oxidic materials.Figure 18.4 Pressed pellet from powder material in a ring of steel as a resu...Figure 18.5 Scheme of an automated fusion automat with inductive heated fusi...Figure 18.6 Fusion automat with two inductive heated fusion instruments.Figure 18.7 External (a) and internal (b) view of an automated sample prepar...Figure 18.8 Robot during loading of a resistance-heated fusion furnace (a) a...Figure 18.9 Scheme of an in-line analyzer for bulk material.Figure 18.10 Scheme of an on-line analyzer for liquids.Figure 18.11 Measuring heads for a continuous monitoring of material flow. (...

17 Chapter 19Figure 19.1 Elements of a quality management system.Figure 19.2 Scheme for the connection of secondary references to SI units.Figure 19.3 Scheme of a validation process.Figure 19.4 Methods for a validation.Figure 19.5 Determination of the parameter's precision and trueness.Figure 19.6 Influence of deviations of the measurement to the determination ...