The inorganic ceramic compounds based on the CeO2 belong into the group of high-temperature pigments. The pigments have been prepared by the classical dry process (i.e. solid-state
reaction) in the temperature range from 1,300 to 1,600 °C and by the coprecipitation at the three different temperatures:
400, 600 and 1,100 °C. The principal of these pigments makes the host lattice of the CeO2, which is doped by terbium ions. This incorporation of the doped ions leads to obtaining of the interesting dark orange colour
after application into ceramic glaze. The aim of our research was to improve and optimize the synthesis conditions of these
pigments. The samples were submitted to thermal analysis (TG–DTA) for determination of the temperature interval of the pigment
formation and the thermal stability of pigments. The compounds were also measured from the point of view of their colouring,
structure and particle size distribution. 相似文献
The initial growth stage of C(60) thin film on graphite substrate has been investigated by scanning tunneling microscopy in ultrahigh vacuum at room temperature. The C(60) layer grows in a quasi-layer-by-layer mode and forms round, monolayer high islands on the graphite surface. The islands are confined by terraces on the graphite surface and the mobility of C(60) fullerenes across steps is low in all layers. The second and all subsequent layers adopt a fractal-dendritic shape, which was confirmed by calculating the fractal dimension (D=1.74 prior to island coalescence) and is in agreement with a diffusion limited aggregation. The profound differences between the growth of C(60) layers on graphite (first layer) and on C(60) surfaces (second and higher layers) are caused by the restriction of the C(60) mobility on the highly corrugated fullerene surfaces. The orientation of the fractal islands follows the hexagonal symmetry of the densely packed (111) surface of the fullerene lattice, which introduces a bias in the direction of molecule movement. The differences in surface topography on the nanoscale determine the mode of film growth in this van der Waals bonded system. 相似文献
The paper describes in detail how to evaluate interlaboratory studies for the measurement of authorised and non-permitted veterinary drugs. Examples of different kinds of evaluation will be presented including the results of two interlaboratory studies for anthelmintics in bovine milk and muscle. As compared to an interlaboratory study 2008, a clear development regarding the proficiency of the laboratories of the European Residue Control System could be noted in 2009. As a result of this development, the percentage of false-negative and false-positive results had decreased considerably. The described improvements in the analysis of the included anthelmintics were also reflected in the overall assessment. While in 2008 ten (38.5?%) out of 26 NRLs fulfilled the proficiency criteria of the interlaboratory study, this number had increased to fourteen (53.8?%) by 2009. In some cases, the correct quantification needed to be improved. 相似文献
Acrylamide and acrolein are two short-chained hazardous compounds with neurotoxic, carcinogenic, and mutagenic effects. The aim of this paper is to describe a fast and simple procedure for simultaneous determination of both acrylamide and acrolein under standard conditions, suggest a suitable calibration protocol for custom analysis, and demonstrate its applicability to the analysis of gaseous products from, e.g., cigarettes, cigars, or electronic cigarettes. A gas chromatography–mass spectrometry (GC–MS) method was developed to quantify acrylamide and acrolein in smoke vapor from electronic cigarettes, tobacco cigarettes, and cigars. Nonionic and highly polar molecules with a low boiling point and molecular mass need a suitable derivatization method to achieve appropriate retention and selectivity on commonly used relatively nonpolar stationary phases and to enhance the molecular mass for easy MS detection. The derivatization of acrylamide and acrolein was carried out by a bromination method with elemental bromine. The dibromo derivatives were extracted into an organic solvent and following a dehydrobromination procedure the samples were injected into the GC–MS system. Important experimental parameters were varied, after which the bromination time was defined as 30 min, and the injector temperature and the starting temperature of gradient were set at 280 and 50 °C respectively. Acrolein was found in all tested samples, while acrylamide was detected only in smoke from normal tobacco. Possible mechanisms for the formation of these unsaturated compounds in the samples are discussed. After its validation the newly developed method was successfully and reliably applied to the analysis of both compounds. This short method provides an easy way to determine acrylamide and acrolein in gaseous samples.
The alditol acetate method is a common procedure for sugar analysis, also applied to determine the substituent distribution
in monomer units of polysaccharide ethers like methyl cellulose by gas liquid chromatography. Consisting of several preparation
and work-up steps this procedure is both time consuming and prone to side reactions that promote discrimination of single
constituents, especially when no peralkylation step is performed prior to hydrolysis. As a consequence results scatter in
dependence on individual treatment and conditions. In the context of this work these critical points were overcome by strict
but simplified work-up procedures and using acid instead of alkaline catalyzed acetylation. Under the acidic conditions the
tedious removal of borate is no longer necessary and a reduced time requirement was achieved as well as good reproducibility.
Comparison with independent reference methods excluded a systematic error of the method and confirmed the results obtained.
Without peralkylation, i.e. in the presence of free hydroxyl groups, another fast modification of the method using DMSO as
solvent, no removal of borate, and 1-methylimidazole as catalyst for acetylation was found to produce a systematic error. 相似文献
A confidence interval for the probability of detection across laboratories (LPOD) for qualitative methods, described in the AOAC INTERNATIONAL guidelines for validation of microbiological methods for food and environmental surfaces, is considered. It is demonstrated that under certain conditions, the observed confidence of this confidence interval can be rather low, so that statistical minimum requirements are not fulfilled. A new profile likelihood confidence interval based on a latent random laboratory effect approach is proposed. Observed confidence levels for this confidence interval demonstrate its applicability already for a small number of laboratories. 相似文献