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A complete metrological traceability system for measurement results of chemical analysis was set up. Core components are pure substances (national standards) characterised at the highest metrological level, primary solutions prepared from these pure substances and secondary solutions deduced from the primary solutions and intended for sale. The relative uncertainty of the element mass fraction of the primary substances and solutions is < 0.01 and < 0.05%, respectively. For the certification of transfer solutions and for stability testing, a precision measurement method for element contents has been developed by means of optical emission spectrometry (ICP OES) by which uncertainties between 0.1 and 0.05% can be achieved. The dissemination to field laboratories is effected with the aid of a calibration laboratory of the German Calibration Service (DKD) which certifies the element content of the secondary solutions with an uncertainty <= 0.3%. Calibration with these solutions enables the user to establish traceability of his measurement results to the International System of Units (SI). Currently, the system comprises Cu, Fe, Bi, Ga, Si, Na, K, Sn, W, and Pb.
Die Größenbewertung von Anzeigen und die Bestimmung der Nachweisgrenze spielen bei der Ultraschallprüfung eine zentrale Rolle: Sie stellen sicher, dass kritische Ungänzen erfasst und bruchmechanisch behandelt werden können.
Bei SAFT wurde bisher die Größe von Ungänzen dadurch bestimmt, dass die räumliche Anzeigenausdehnung im Rekonstruktionsergebnis ausgewertet wird, d.h. die Anzahl von Voxel über die sich eine Anzeige erstreckt. Auf diese Weise lassen sich jedoch nur Defektanzeigen bewerten, die größer oder gleich der Wellenlänge sind. Bei kleinen Defekten versagt diese Methode, d.h. es ist keine Größenbewertung möglich. Außerdem bietet diese Methode keine Aussage über die Nachweisgrenze des Verfahrens.
Ein Hauptvorteil von SAFT gegenüber der konventionellen Ultraschallprüfung ist aber gerade die Verbesserung der Nachweisgrenze, denn SAFT steigert das Signal-Rausch-Verhältnis (SNR) gegenüber dem Gefügerauschen und reduziert statistisches Rauschen. Um diesen Hauptvorteil nutzen (und quantifizieren) zu können, wird für SAFT eine Methode zur Nachweisgrenzenbestimmung und zur Größenbewertung der Anzeigen kleiner Ungänzen benötigt.
Neben ihrer räumlichen Ausdehnung lassen sich Anzeigen im SAFT-Ergebnis auch durch ihre Amplitude charakterisieren, wenn die Prüfkopfeigenschaften und die geometrischen Verhältnisse beim Scan berücksichtigt werden. Genauer gesagt durch die Amplitudensumme, in die - neben der Echoamplitude - auch die winkelabhängige Streucharakteristik eingeht.
Im Folgenden wird dargelegt, dass sich die Amplitudensumme zur Nachweisgrenzenbestimmung und zur Größenbewertung kleiner Ungänzen eignet.
Es wird der Zusammenhang zwischen der Amplitudensumme und der Größe von Ungänzen dargestellt, und es wird gezeigt, dass auch die Anzeigenposition und die Form des Prüfobjektes eine Rolle spielen können. Auf dieser Basis wird eine Methode zur Größenbestimmung kleiner Anzeigen im SAFT-Ergebnis entwickelt.
Damit lässt sich das SAFT-Ergebnis als Ersatzfehlergröße darstellen, so wie das bei konventioneller Ultraschallprüfung z.B. mit Hilfe von AVG-Diagrammen erfolgt.
Durch die Vervollständigung um die Größenbewertung ist SAFT nicht mehr nur ein bildgebendes Verfahren, sondern es kann vielmehr als vollwertiges Messverfahren dienen.
The performance of glow discharge mass spectrometry (GD-MS) is investigated for the accurate quantification of metallic impurities and oxygen in solid samples using the fast flow source GD-MS instrument ELEMENT GD.
Different quantification approaches based on relative and absolute sensitivity factors are evaluated for the determination of metallic impurities using three sample matrixes (Al, Cu and Zn). The effect of the discharge conditions (voltage, current, discharge gas pressure/flow) on the sensitivity is investigated and the parameters are optimized to favour matrix independent calibrations. Improved standard relative sensitivity factors (StdRSFs) are calculated under optimal conditions based on multi-matrix calibrations. The sputtering rate corrected calibration is also presented as a multi-matrix calibration approach.
The capabilities of GD-MS for oxygen determination are also investigated using a set of new conductive samples containing oxygen with mass fractions in the percent range in three different matrices (Al, Mg and Cu) produced by a sintering process. Poor limits of detection (in the order of g/kg) were obtained as consequence of the reduced sensitivity of oxygen in GD-MS and high oxygen background signal intensity as well as its variations. The absolute sensitivity procedure is shown as a matrix-independent approach, which provides quantitative values consistent with those obtained by carrier gas hot extraction (CGHE).
This key comparison aims to assess the core capabilities of the participants in gas analysis. Such competences include, among others, the capabilities to prepare Primary Standard gas Mixtures (PSMs), perform the necessary purity analysis on the materials used in the gas mixture preparation, the verification of the composition of newly prepared PSMs against existing ones, and the capability of calibrating the composition of a gas mixture. According to the Strategy for Key Comparisons of the Gas Analysis Working Group, this key comparison is classified as an RMO track A key comparison.
The artefacts were binary mixtures of propane in nitrogen at a nominal amount-of-substance fraction level of 1000 μmol/mol. The values and uncertainties from the gravimetric gas mixture preparation were used as key comparison reference values (KCRVs). Each transfer standard had its own KCRV. The results are generally good. All results are within ± 1 % of the KCRV.
Core–shell nanoparticles (CSNPs) have become indispensable in various industrial applications. However, their real internal structure usually deviates from an ideal core–shell structure. To control how the particles perform with regard to their specific applications, characterization techniques are required that can distinguish an ideal from a nonideal morphology. In this work, we investigated poly(tetrafluoroethylene)–poly(methyl methacrylate) (PTFE–PMMA) and poly(tetrafluoroethylene)–polystyrene (PTFE–PS) polymer CSNPs with a constant core diameter (45 nm) but varying shell thicknesses (4–50 nm). As confirmed by transmission scanning electron microscopy (T-SEM), the shell completely covers the core for the PTFE–PMMA nanoparticles, while the encapsulation of the core by the shell material is incomplete for the PTFE–PS nanoparticles. X-ray photoelectron spectroscopy (XPS) was applied to determine the shell thickness of the nanoparticles. The software SESSA v2.0 was used to analyze the intensities of the elastic peaks, and the QUASES software package was employed to evaluate the shape of the inelastic background in the XPS survey spectra. For the first time, nanoparticle shell thicknesses are presented, which are exclusively based on the analysis of the XPS inelastic background. Furthermore, principal component analysis (PCA)-assisted time-of-flight secondary-ion mass spectrometry (ToF-SIMS) of the PTFE–PS nanoparticle sample set revealed a systematic variation among the samples and, thus, confirmed the incomplete encapsulation of the core by the shell material. As opposed to that, no variation is observed in the PCA score plots of the PTFE–PMMA nanoparticle sample set. Consequently, the complete coverage of the core by the shell material is proved by ToF-SIMS with a certainty that cannot be achieved by XPS and T-SEM.
This is a corrigendum to the original article "Determining the thickness and completeness of the shell of polymer core-shell nanoparticles by X-ray photoelectron spectroscopy, secondary ion mass spectrometry, and transmission scanning electron microscopy" that was published in "The journal of physical chemistry C", vol. 123 (2019), no. 49 pp. 29765-29775.
This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material.
An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state.