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  • 1
    Electronic Resource
    Electronic Resource
    Classical analysis including trace-matrix separation versus solid state mass spectrometry: A comparative study for the analysis of high purity Mo, W and Cr (1990)
    Springer
    Microchimica acta 101 (1990), S. 259-271 
    Details
    ISSN: 1436-5073
    Keywords: solid state mass spectrometry ; trace-matrix separation ; GDMS ; SIMS ; SSMS ; NAA ; ICP-AES ; ICP-MS ; AAS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The applicability of GDMS, SIMS, SSMS, NAA and TMS with AAS, ICP-OES and ICP-MS end determination for routine bulk ultratrace analysis of high purity refractory metals was investigated. Due to the heterogeneous distribution of trace elements in the sub-ppm range, sample consumption and analysis time have a tremendous influence on quantification with procedures of low sample consumption. As an example, GDMS, which is commonly used for ultrapure material certification by most of the manufacturers in Europe and the USA, exhibits discrepancies by more than one order of magnitude for repetitive analyses of a series of trace components in the same sample. Furthermore, results of different laboratories using the same instrument are frequently not comparable. Due to easy standardization and large sample consumption TMS procedures combined with FAAS, GFAAS, ICP-AES and ICP-MS as methods of end determination exhibit better precision and accuracy than GDMS and SIMS. Detection limits are comparably low or even better in case of ICP-MS end determination. TMS procedures are less expensive and less time consuming than highly sophisticated analytical techniques like GDMS, SIMS or NAA. Additionally, they can be easily applied by experienced personnel in a well equipped industrial analytical laboratory.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01244178
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  • 2
    Electronic Resource
    Electronic Resource
    The characterization of high-tech materials: Perspectives, challenges, trends (1991)
    Springer
    Microchimica acta 104 (1991), S. 177-214 
    Details
    ISSN: 1436-5073
    Keywords: atomic structure ; crystal structure ; microstructure ; constructions ; topochemistry ; graphite ; glassy carbon ; pyrolytic carbon ; microelectronics ; carriers of information ; refractory metal alloys ; life time ; recrystallization ; fatigue ; photon probe techniques ; electron probe techniques ; ion probe techniques ; electrical field probes
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract From the Stone Age on, developmental periods of mankind carry the names of materials. Materials determine the applicability of key technologies and these are in turn of major significance for the economic success and the social development in modern society. Today's high-tech materials are the consequence of an improved understanding of the structure and composition of matter and of the interplay of microstructure and minor and trace constituents. We can distinguish four basic dimensional structural categories of materials: (a) the atomic structure level; (b) the crystal, glassy or amorphous structural level; (c) the microstructural level; (d) the level of constructions. As an example, these structural levels are described in some detail for graphite, a material used extensively throughout Analytical Chemistry. Decisive differences at the microstructural level result in graphitic materials with very varying properties: polycrystalline electrographite, glassy carbon, and pyrolytic graphite. Examples for the use of these materials in ETAAS are discussed. Structural features together with topochemical and trace chemical characteristics are studied today by a wide variety of analytical instrumentation and methods of modern materials analysis which can be grouped into four categories of techniques: (a) photon probe techniques; (b) electron probe techniques; (c) ion probe techniques; (d) electrical field probes. The most important of those techniques are discussed shortly with respect to their main characteristics as lateral and depth resolution, detection sensitivity, additional bonding or structural information, depth profiling possibilities etc. The constructions are the ultimate level of a materials structure. Structures of microelectronic components reach dimensionally into the domain of microstructure whereas constructions in heavy industry are of meter-ton dimensions. Progress in the use of materials as carriers of information is visualized by a morphological comparison of the sound tracks of conventional records with the information imprinted in optical discs. It is important to conceive materials as dynamic systems with limited lifetime. Fatigue and recrystallization are prominent relevant phenomena which must be studied by microstructural and topochemical methods. Dispersion strengthened microalloys like TZM, HT-molybdenum and NS-tungsten are discussed as examples how materials can be improved with respect to their extended use under extreme conditions. Again, a thorough structural and topochemical characterization was the basis of a successful respective materials development although a multitude of relevant topochemical questions still remain to be solved. Lifetime investigations are an essential tool of materials development as well as quality control. Relevant investigations for various tube materials for ETAAS are discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01245508
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  • 3
    Electronic Resource
    Electronic Resource
    Accuracy of film thickness determination in electron probe microanalysis (1995)
    Springer
    Microchimica acta 119 (1995), S. 41-47 
    Details
    ISSN: 1436-5073
    Keywords: thin film analysis ; electron probe microanalysis ; Rutherford backscattering spectroscopy ; secondary ion mass spectrometry
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The thickness of copper films (100–450 nm) on silicon substrates was determined by electron probe microanalysis (EPMA) applying φ(ϱz) procedures of Pouchou and Pichoir. Film thickness was calculated from experimental k-ratios analyzed with electron energies between 6 and 30 keV using commercial software (LAYERF distributed by CAMECA). The influence of the incident electron energy and X-ray line chosen for analysis on the results was investigated. Accuracy of film thickness determination was evaluated by comparison with Rutherford backscattering spectroscopy (RBS) and secondary ion mass spectrometry (SIMS). The difference between layer thicknesses determined with EPMA and RBS is in general less than 2%, if EPMA measurements are performed with various electron energies. Layer thicknesses determined with Cu-Lα are mostly closer to values obtained by RBS than those derived from Cu-Kα radiation. Preliminary SIMS measurements yielded inconsistent results and, thus, cannot be used in this case to determine the layer thickness of Cu films on Si accurately.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01244852
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  • 4
    Electronic Resource
    Electronic Resource
    A comparison of X-ray fluorescence spectrometric (XRF) techniques for the determination of metal traces, especially in plastics (1994)
    Springer
    Microchimica acta 117 (1994), S. 95-108 
    Details
    ISSN: 1436-5073
    Keywords: X-ray fluorescence analysis ; standard sample preparation ; WDXRF ; EDPXRF ; EDXRF ; determination of metal traces ; plastic matrix ; plastic extruders ; annular slit tribometer
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A comparative study of energy-dispersive X-ray fluorescence techniques (without and with polarized radiation) and a wavelength-dispersive technique was carried out in order to investigate their sensitivity for the quantitative determination of 3d transition metal traces in plastic materials. For this purpose, liquid calibration samples in paraffin oil for the elements Cr, Mn, Co, Ni and Cu were prepared. Calibration lines in the concentration range of 1–100 μg/g were evaluated for commercially available XRF-instruments and the results were critically compared. Limits of detection (LOD) ranged from 0.1 to 0.7 μg/g for wavelength-dispersive XRF and energy-dispersive XRF with polarized radiation. The LOD's for energy-dispersive XRF without polarized radiation ranged from 0.9 to 8.6 μg/g for elements in the same atomic number range between 24 and 29. The application of these optimized methods to the quantitation of wear and corrosion phenomena in plastic extruders and in a relevant model test apparatus, the annular slit tribometer, is elucidated.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01243020
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  • 5
    Electronic Resource
    Electronic Resource
    Characterization of individual atmospheric particles by element mapping in electron probe microanalysis (1997)
    Springer
    Microchimica acta 125 (1997), S. 137-141 
    Details
    ISSN: 1436-5073
    Keywords: electron probe microanalysis ; element distribution mapping ; particle characterization
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract In this paper procedures for the characterization of individual aerosol particles by element mapping in the electron microprobe are presented. The number, size and qualitative chemical composition of particles is derived from a combination of secondary or backscattered electron images and element distribution maps. Accuracy of the size distribution and reliability of the qualitative analysis procedure were checked with silicate samples. In order to obtain a semi-quantitative estimate of the chemical composition of individual particles the count rates taken from element distribution maps are corrected for matrix and geometric effects using particle ZAF procedures.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01246176
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  • 6
    Electronic Resource
    Electronic Resource
    Tungsten grit as an accelerator material for C- and S-trace analysis by combustion in HF-induction furnaces (1984)
    Springer
    Microchimica acta 83 (1984), S. 263-281 
    Details
    ISSN: 1436-5073
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Zusammenfassung Fünf auf dem Markt angebotene Wolfram-Kornmaterialien wurden nach drei Gesichtspunkten vergleichend untersucht: -C- und S-Spurengehalt, -Morphologie (durch Rasterelektronenmikroskopie), -Siebanalyse zur Ermittlung der Korngrößenverteilung. Die Anforderungen an ein als Beschleunigungsmaterial verwendetes Wolfram-Korn zur C-und S-Spurenanalyse sind folgende: a) dichtes Material mit möglichst geringer spezifischer Oberfläche (vorzugsweise W-Korn, hergestellt aus gesintertem, verformtem und rekristallisiertem Wolfram ohne Restporosität); b) enge Korngrößenverteilung bei mäßig grobem Korn, z. B. zwischen 0,5 und 2 mm (35 bis 10 U. S. mesh), ohne Staubanteil; c) Wolframreinheit mindestens 99,5% ohne Verunreinigungen, die die Bestimmung stören (z. B. Mühlenabrieb) oder eine Verletzung der Sicherheitsvorschriften verursachen (thorierter W-Schrott).
    Notes: Summary Five commercially available tungsten grit materials are investigated for their: -C-and S-trace contents, -morphology (by scanning electron microscopy), -particle size distribution (by sieve analysis). Tungsten grit for this purpose should have the following properties: a) Dense material with as low a specific surface as possible (preferably grit fabricated from pure worked tungsten scrap with no residual porosity). b) Fairly narrow particle size distribution e. g. of 0.5 mm to 2 mm particle diameter (i. e. U. S. mesh 35 to 10) with no fines. c) High purity tungsten (99.5% min.) without trace components which could interfere with the C-and S-trace analysis (e. g. particles from mill wear) or lead to violation of safety regulations (thoriated W-scrap).
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01207074
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  • 7
    Electronic Resource
    Electronic Resource
    Extraction inductively coupled plasma-optical emission spectrometry (ICP-OES) determination of traces of phosphorus in tungsten (1989)
    Springer
    Microchimica acta 99 (1989), S. 399-412 
    Details
    ISSN: 1436-5073
    Keywords: phosphorus ; tungsten ; preconcentration ; ICP-OES
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A method for the separation and preconcentration of traces of phosphorus from tungsten was developed. Solid phase extraction of the phosphovanadomolybdate complex performed on a micro-column was applied. Phosphorus was determined by optical emission spectroscopy (OES) with inductively coupled plasma (ICP) excitation. A limit of detection of 0.4 μg/g P with respect to the solid phase is obtained. By directly coupling the extraction/elution step to the ICP instrument a detection limit of 0.06 μg/g P in W was achieved. Besides, the complexity of spectral evaluation in ICP-OES determinations of traces in spectralline-rich matrices is discussed.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01244696
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  • 8
    Electronic Resource
    Electronic Resource
    Trace-matrix separations for high-purity chromium, molybdenum and tungsten with cellulose collectors (1989)
    Springer
    Microchimica acta 99 (1989), S. 423-432 
    Details
    ISSN: 1436-5073
    Keywords: high purity Cr ; Mo and W ; separation of matrix ; preconcentration of trace metals ; cellulose collectors ; ICP ; AAS
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Trace metals (20 elements) in high-purity chromium, molybdenum and tungsten are collected and preconcentrated by precipitation and adsorption on cellulose collectors. The compound methods allow the application of AAS and ICP-AES as determination methods for the production control of highly pure refractory metals under routine conditions.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01244698
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  • 9
    Electronic Resource
    Electronic Resource
    High performance analytical characterization of refractory metals (1987)
    Springer
    Microchimica acta 91 (1987), S. 233-260 
    Details
    ISSN: 1436-5073
    Keywords: refractory metals ; ultratrace bulk analysis ; flame and graphite furnace atomic absorption spectrometry ; ICP-atomic emission spectrometry ; activation analysis ; mass spectrometric methods ; effect of trace impurities on metal properties
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract It is first shown what effects trace impurities generally exert on metal properties and why trace analysis is essential to modern applications of refractory metals in today's high technology. The effect of trace impurities in metals on complex systems like microelectronic components is also discussed. It is then shown, what principal analytical requirements are mandatory for trace characterization of refractory metals at levels of rising purity (4 N to 6 N). A survey of analytical methods for trace and ultratrace characterization of refractory metals is given including the following methods: flame and graphite furnace atomic absorption spectrometry, ICP and DCP-atomic emission spectrometry, X-ray fluorescence spectrometry, activation analysis, mass spectrometric methods, especially SIMS and GDMS.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF01199500
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  • 10
    Electronic Resource
    Electronic Resource
    Ultratrace analysis — Facts and fiction (1992)
    Springer
    Fresenius' Zeitschrift für analytische Chemie 343 (1992), S. 695-704 
    Details
    ISSN: 1618-2650
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Summary Ultratrace analysis is a term which still awaits a clear definition but it is gaining rising importance especially for hightech materials and processes. Relevant ultratrace levels of importance depend largely on the investigated matrix but generally range below 1 ppm. Some factors leading to fiction in ultratrace analysis are discussed such as: -The yet undefined terms typical analysis, actual analysis and guaranteed analysis -Misleading certificates of analysis for ultrapure materials -The listing of total purities according to the number of nines concept with a lot of exceptions -Purity data based exclusively on integral physical methods -Extremely small analytical volumes versus the degree of heterogeneous distribution of a trace component -In extreme cases, heterogeneous ultratrace distribution might limit the applicability of a respective material -The enormous economic pressure exerted on analysts in industry and non ideal conditions in relevant analytical laboratories. On the other hand, some of the most fascinating aspects of ultratrace analysis are elucidated: -Spectroscopic and other methods of end determination are approaching single atom detection -Topochemical materials characterization is today feasable with atomic resolution.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1007/BF00633545
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