Conversion of carbon into CF4 for SI-traceable measurements of absolute carbon isotope amount ratios: a feasibility study

The feasibility of performing SI-traceable carbon isotope amount ratio measurements following conversion of carbon into CF4 was studied. A procedure for the direct fluorination of carbon with elemental fluorine was developed, and the conversion step was checked for losses, blank contributions, and the absence of systematic isotope effects. Gas chromatography was used to identify and quantify the gaseous fluorination products and to isolate CF4 from byproducts. After fluorination of graphite carbon, CF4 and perfluoroalkanes with up to six carbon atoms were observed as reaction products. Within an uncertainty of 10%, the graphite carbon was fully recovered in the gaseous carbon fluorides, with the main product being CF4 (80-90%) and C2F6 as the major byproduct. The fluorination and GC procedures were found to introduce an alteration not bigger than 0.03 +/- 0.04/1000 on the isotopic composition of CF4. Carbon blank contributions introduced during the fluorination procedure were below 0.5% relative to a typical sample of 4 mg of carbon. For two of the materials investigated, the carbon isotope ratios measured on a differential mass spectrometer were reproducible within a standard deviation of approximately 0.1/1000 for several individual fluorinations. For these materials, the developed fluorination procedure is a straightforward process, which can be used as a foundation to establish SI-traceable measurements of carbon isotope amount ratios. However, for the third graphite material the formation of byproducts (C2F6-C6F14) was found to induce significant isotopic fractionation.     

Determination of main and minor components of silicon based materials by a combustion with elemental fluorine. Separation of gaseous fluorination products by carrier gas distillation and gas mass spectrometry

For the determination of main and minor components in silicon-based ceramic powders, a decomposition by a combustion with elemental fluorine and separation of the volatile fluorination products by a carrier-gas distillation with a subsequent detection by quadrupole mass spectrometry is described. The necessity and success of the separation step is demonstrated for the determination of boron as a minor constituent in SiC, where the spectral interferences of silicon on the boron signals are decreased considerably. The method developed is shown to be directly applicable to determination of silicon in Si3N4, SiC, and SiO2. The determination of nitrogen in Si3N4 requires additional effort, to separate nitrogen from the excess of fluorine. For the determination of boron, a complete mobilization of BF3 is assured by the presence of an adequate amount of GeF4. Analysis results obtained with different types of calibration show a precision of 30 microg for boron at the milligram-per-gram level and a precision between 0.5 and 2% (m/m) for the main components, silicon and nitrogen. Within these standard deviations, the results agree well with the values expected from the stoichiometry, with the results for silicon and boron obtained by wet chemical decomposition and slurry techniques in combination with ICP-OES and with the results for nitrogen obtained by carrier gas heat extraction.     

Accident-induced pseudarthroses of the dens axis. Etiology, follow-up and therapy]

Several studies have shown that combining the change in the ST-segment with another exercise variable improves the predictive value of stress testing. However, no method has been able to combine many stress test variables with the ST-segment change simultaneously and help the clinician better predict future cardiac events. Fuzzy Cluster Analysis (FCA) was used to combine 5 stress test variables with ST-segment deviation to classify each of 232 positive outpatient stress tests as mildly, moderately, or severely abnormal. Cardiac events were recorded in these 3 patient groups up to 96 months (mean 65 months) after the stress tests. Coronary angiography was performed on 159 of these patients within 1 month of their stress tests. FCA better separated the 3 event-free survival curves than classifying the stress tests by three ST-segment (0.5-1.5 mm, 2-2.5 mm, > 3 mm) groups (p < 0.05). At 2 years, 90% of the FCA mild group were compared with 70% for the 0.5-1.5 mm group (p < 0.01). Moderate and severe tests by FCA separated patients with an intermediate from those with a poor prognosis while the 2-2.5 mm and 3 mm or more ST-segment curves did not (p < 0.05). FCA showed overall better correlation with coronary score (r = 0.71) than did the graded ST-segment groups (r = 0.48). FCA predicted both mild and high-grade (triple-vessel and left main) coronary disease better than ST-segment alone. Thus FCA better predicts future cardiac events in patients with positive stress tests than the ST-segment alone. This combined with its usefulness in predicting the extent of coronary disease provides the basis of a clinical strategy for managing patients with positive stress tests.     

RF-induced heating of interventional devices at 23.66 MHz

Objective

Low-field MRI systems are expected to cause less RF heating in conventional interventional devices due to lower Larmor frequency. We systematically evaluate RF-induced heating of commonly used intravascular devices at the Larmor frequency of a 0.55 T system (23.66 MHz) with a focus on the effect of patient size, target organ, and device position on maximum temperature rise.

Materials and methods

To assess RF-induced heating, high-resolution measurements of the electric field, temperature, and transfer function were combined. Realistic device trajectories were derived from vascular models to evaluate the variation of the temperature increase as a function of the device trajectory. At a low-field RF test bench, the effects of patient size and positioning, target organ (liver and heart) and body coil type were measured for six commonly used interventional devices (two guidewires, two catheters, an applicator and a biopsy needle).

Results

Electric field mapping shows that the hotspots are not necessarily localized at the device tip. Of all procedures, the liver catheterizations showed the lowest heating, and a modification of the transmit body coil could further reduce the temperature increase. For common commercial needles no significant heating was measured at the needle tip. Comparable local SAR values were found in the temperature measurements and the TF-based calculations.

Conclusion

At low fields, interventions with shorter insertion lengths such as hepatic catheterizations result in less RF-induced heating than coronary interventions. The maximum temperature increase depends on body coil design.