ERM, a New Landmark for Reference Materials.

Abstract not availableJRC.D-Institute for Reference Materials and Measurements (Geel

ERM - A New Landmark for Reference Material

Modern analytical quality assurance relies on three main components, namely the application of validated methods, the participation in proficiency testing and the use of certified reference materials (CRMs).JRC.D.2-Reference material

Calibration of double focusing Glow Discharge Mass Spectrometry instruments with pin-shaped synthetic standards

Calibration of two commercially available glow discharge double focusing mass spectrometers, the VG 9000 and Element GD, is described using synthetic pin standards pressed from solution doped copper and zinc matrices. A special pressing die was developed for this purpose and optimal results were obtained with the highest possible pressures, i.e., 95 kN\u2022cm - 2. This calibration approach permits the determination of trace element mass fractions down to \u3bcg\u2022kg -1 with small uncertainties and additionally provides traceability of the GD-MS results in the most direct manner to the SI (International System of Units). Results were validated by concurrent measurements of a number of compact copper and zinc certified reference materials. The impact of the sample pin cross-section (circular or square) was investigated with the use of a new pin-sample holder system for the Element GD. The pin-sample holder was designed by the manufacturer for pin-samples having circular cross-section; however, samples with square pin cross-section were also shown to provide acceptable results. Relative Sensitivity Factors for some 50 analytes in copper (VG 9000, Element GD) and zinc matrices (VG 9000) are presented. The field of applicability of GD-MS may be considerably extended via analysis of pin geometry samples based on their ease of preparation, especially with respect to the accuracy and traceability of the results and the enhanced number of analytes which can be reliably calibrated using such samples. \ua9 2011 Elsevier B.V. All rights reserved.Peer reviewed: YesNRC publication: Ye

Procedure for the impurity-related correction at the indium fixed-point

Determining the influence of impurities on the fixed-point temperatures of the ITS-90 requires the completion of several tasks. In this paper, the progress made at Physikalisch-Technische Bundesanstalt (PTB) and BAM Federal Institute for Materials Research and Testing is presented and remaining questions are discussed. The projected characterization procedure at PTB, which is based on the established SIE method (sum of the individual estimates), using a new indium fixed-point cell is described as an example. This procedure includes an SI-traceable chemical analysis of the material in the fixed-point cell with sufficiently low uncertainties, the individual experimental determination of the influence of the quantified impurities on the fixed-point temperature, and the establishment of direct links to the phase-transition temperatures of the national standard and of an assumed material of ideal purity. A characteristic difference to the common practice is the chemical analysis of the fixed-point metal being done after determining the cell's freezing temperature. This allows for the detection and consideration of contamination and purification effects due to the filling process, or due to the contact with the carbon crucible and other parts of the fixed-point cell. A chemical analysis of an indium fixed-point was carried out by BAM with relative measurement uncertainties below 30 % which have not been previously achieved. The results provide evidence for the precipitation of some impurities, which is apparently inconsistent with the corresponding binary phase diagrams, but was explained in a recent publication. Implications for the use of the SIE method shall be described briefly at the end. \ua9 2011 Springer Science+Business Media, LLC.Peer reviewed: YesNRC publication: Ye

Structural characterization of a coarse-grained transparent silicon carbide powder by a combination of powder diffraction techniques

Diffraction of hard synchrotron radiation as well as constant-wavelength and time-of-flight neutron diffraction were used for the structural characterization of a silicon carbide powder having extremely low levels of chemical impurities, high perfection of the crystalline lattice and a grain size of up to 150 \u3bcm. The presence of three polytypes was ascertained and the ratios of their mass fractions were determined to be w15R : w6H = 0.002,3(8) and w4H : w6H = 0.000,6(2).Peer reviewed: YesNRC publication: Ye