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Eingeladener Vortrag
- nein (138)
Bringing isotopic spike calibration solutions for isotope dilution to a broader analytical community
(2000)
Comparative performance study of ICP mass spectrometers by means of U "isotopic measurements"
(2000)
The performance of four commercially available ICPMS instruments of three different types was compared by means of uranium "isotopic measurements". Examined were two quadrupole sector (different generation, different manufacturer), one single detector double focusing magnetic sector and one multiple collector double focusing magnetic sector instruments. The same samples of the IRMM-072 series were used under routine conditions to measure the 233U/235U and the 233U/238U ratios which, in these samples, vary over almost three orders of magnitude from ~ 1 to ~ 2 · 10-3. Within expanded (k = 2) uncertainties, good agreement was observed between the certified values and the data internally corrected for mass-discrimination effects. The magnitude of the evaluated uncertainties was different for each type of instrument. With the multiple collector instrument, expanded uncertainties varied from - 0.04% to- 0.24% for the 233U/235U ratio, and from - 0.08% to - 0.27% for the 233U/238U ratio. They were ~ 1 to 5 times larger with the single detector magnetic sector instrument, and ~ 10 to 25 times larger with both quadrupole sector instruments. With the multiple collector instrument, repeatability of the measurements seemed to be limited by the difficulty of correcting properly for instrumental background, whereas with the single detector magnetic sector instrument the counting statistics was the only limitation (on smallest ratios). Apparent mass-discrimination was clearly found to be larger but more reproducible (and hence easier to correct for) in the case of magnetic sector instruments than for both quadrupole sector instruments. If space charge effects were the main source of mass-discrimination for all instruments, these results are in contradiction with the hypothesis of the size of mass-discrimination decreasing with the acceleration voltage. With the single detector magnetic sector instrument in particular (when operated by changing the ion energy only), our results pointed at more than only one major source of mass-discrimination, with variable size depending on the ratios measured.
The present paper describes the certification of the amount content of Cd, Cr and Pb in two different polyethylene materials within the third phase of the Polyethylene Elemental Reference Material (PERM) project. The analytical procedure to establish the reference values for Cd, Cr and Pb amount contents in these materials is based on isotope dilution mass spectrometry used as a primary method of measurement. Cd and Pb were measured with inductively coupled plasma-mass spectrometry and Cr with positive thermal ionization-mass spectrometry. The decomposition of the polymer matrix was carried out using a high pressure asher. Reference values for amount content, traceable to the SI-system, have been obtained for these three elements in both of the polyethylene samples of PERM. For each of the certified amount content values an uncertainty budget was calculated using the method of propagation of uncertainties according to ISO and EURACHEM guidelines. The measurement procedures, as well as the uncertainty calculations, are described for all three elements. In order to keep the whole certification process as transparent as possible, the preparations of various reagents and materials as well as the sample treatment and blending are described in detail. The mass spectrometry measurements and the data treatment are also explained carefully. The various sources of uncertainty present in the procedure are displayed in the uncertainty budgets. The obtained combined uncertainties for the amount content values were less than 2% relative (k=1) for all investigated elements. The amount contents were in the ?mol/kg range, corresponding to mg/kg levels.
The present paper describes the contribution of the Institute for Reference Materials and Measurements to the certification of B, Cd, Mg, Pb, Rb, Sr, and U amount contents in a natural water sample, in round 9 of the International Measurement Evaluation Programme (IMEP-9). The analytical procedure to establish the reference values for B, Cd, Mg, Pb, Rb, Sr, and U amount contents was based on isotope dilution inductively coupled plasma-mass spectrometry used as a primary method of measurement. Applying this procedure reference values, traceable to the SI, were obtained for the natural water sample of IMEP-9. For each of the certified amount contents presented here a total uncertainty budget was calculated using the method of propagation of uncertainties according to ISO and EURACHEM guidelines. The measurement procedures, as well as the uncertainty calculations are described for all seven elements mentioned above. In order to keep the whole certification process transparent and so traceable, the preparations of various reagents and materials as well as the sample treatment and blending, the measurements themselves, and finally the data treatment are described in detail. Explanations focus on Pb as a representative example. The total uncertainties (relative) obtained were less than 2% for all investigated elements at amount contents in the pmol/kg up to the high 7mol/kg range, corresponding to low 7g/kg and mg/kg levels.
Changes in the structure of single-crystal (SC) superalloy SRR99 during creep at 980 °C and 200 MPa were investigated. Geometrical parameters of the y/y'-microstructure, y/y'-misfit, stresses in the phases and local misorientation of the structure were determined at defined points of the dendritic structure by use of X-ray diffraction (XRD), wavelength dispersive X-ray spectroscopy (WDXS), scanning (SEM) and transmission (TEM) electron microscopy. Correlation of the microstructural period and local misorientation of the structure with creep strain were found.
Im Hinblick auf das Verhalten von Bauteilen aus ferritischen Stählen im Übergangsbereich vom Gleitbruch zum Spaltbruch wurden in einem vom BMBF geförderten Forschungsvorhaben, über das nachfolgend auszugsweise berichtet wird, u.a. folgende Ziele verfolgt:
• Abgrenzung des Anwendungsbereichs der elastisch-plastischen Bruchmechanik zu tiefen Temperaturen hin,
• Möglichkeiten und Grenzen der Nutzung von Zähigkeitspotentialen im Übergangsbereich,
• Ermittlung des Einflusses des Spannungszustandes auf das Bruchverhalten im Übergangsbereich und
• Übertragbarkeit auf Bauteile.
Polymeroberflächenfunktionalisierungen im gepulsten Plasma mit nachfolgender chemischer Behandlung
(2000)
Eine neue Generation von alterungsbeständigen Plasmapolymeren mit definierter chemischer Struktur
(2000)
First results of an inter-laboratory comparison (27 participants in Europe, Japan and USA) of XPS data obtained with non-conducting samples are presented. Binding energies of Al 2s for alumina, N 1s and imide C 1s for Kapton and Sr 3p3/2 for a strontium titanate film on glass were obtained after static charge referencing with the help of 15 nm gold particles deposited at the surface of the test samples. For the alumina sample C 1s static charge referenced data are also presented. Repeat standard deviations (sr), between standard deviations (sb), reproducibility standard deviations (sR) and total means are evaluated from the experimental data. It can be stated that although the repeat standard deviation is as small as 0.05 eV in the best case, the standard deviation characterizing the reproducibility of the method is obviously not better than 0.15 eV in the best case at the present time. The knowledge of these standard deviations is important for metrology, validations of analytical procedures relying on qualitative photoelectron spectroscopy and XPS databanking.
Explosionsdruckentlastung
(2000)
Quality assurance according to ISO or EN norms entails a periodical check of critical instrumental parameters. Not yet all commercial software purchased with instruments supports the related measurements and their fast evaluation. EDXTOOLS consist of a programme library which complements the existing software for electron excited energy dispersive X-ray spectrometry (EDS) in this respect. EDXTOOLS can be used to check the detection efficiency by the evaluation of the L/K intensity ratio in a copper or nickel spectrum or by the calculation of the thickness of absorbing detector layers from experiments, which can be performed on any scanning electron microscope. Moreover, measured spectra can be modified by the transmission curve of absorbing media to estimate their influence on the result of quantitative analysis. EDXTOOLS allow the determination of the signal to background ratio from an Fe-55 spectrum and the fitting of measured FWHM's of K-lines to find the resolution curve DE = Ö{DE 2el + DE 2det}. They are completed by the possibility of calculating EDX spectra for the K-lines of light elements and to compare the resulting spectra for different formulae, physical data tables, and detector parameters chosen for the calculation. EDXTOOLS are written in MATLAB®, a wide spread interpreter language. This has the advantage that the programmes are readable text files. A user can check each computational step and modify it. The installation of MATLAB® and its optimization toolbox is necessary to work with EDXTOOLS.
Eine neue Generation von alterungsbeständigen Plasmapolymeren mit definierter chemischer Struktur
(2000)
Zum Stand des Ringversuchs "Stufenhöhen" und erste Auswertung der Umfrage zur QS in der Nanoanalytik
(2000)
The applicability of excimer laser at 308 nm and Nd:YAG laser at 532 nm with fluences below 0.86 J/cm2 for cleaning of cellulose and paper materials was evaluated. The extent of degradation of purified cotton cellulose and Fabriano paper after laser treatment as well as after a period of accelerated humid oven ageing was determined by following the changes in the degree of polymerization. While irradiation of paper with the excimer laser at 308 nm results in depolymerization of cellulose accompanied by a decrease in ISO brightness, no detrimental effects of Nd:YAG laser treatments were observed.