SummaryThree HRGC systems (1: 30m DB-XLB capillary with MS-SIM detection; 2: 60m DB-XLB capillary with full-scan, ion-trap MS detection; and 3: Parallel dual-column DB-17 and series-coupled HP5/HTS with ECD detection) were used to completely characterize multiple lots of 8 different-numbered Aroclor mixtures by quantitative calibration against 9 solutions containing primary standards of all 209 PCB congeners. Despite lower absolute sensitivity and more Aroclor congener coelutions than the dual-column ECD system, the MS systems enabled measurement of more congeners per Aroclor since their greater linear response range did not require dilution of samples and standards. Pairs of different lots of Aroclors 1248 and 1254 displayed markedly different proportions of congeners, and the 1254 pair displayed strong differences in the extent of ortho-chlorine substitution. The tables of congener weight percent distributions among Aroclors are more comprehensive and quantitatively precise than those of prior publications. However, the limitations of single-level calibration precluded measurement of all congeners to the +lo% accuracy desirable for establishing these Aroclors as secondary standards for comprehensive, quantitative congener-specific PCB analysis.
The peak capacity gain (Gn) of a GC×GC system is the ratio of the system peak capacity to that of an optimized one-dimensional GC analysis lasting the same time and providing the same detection limit. A near-theoretical maximum in Gn has been experimentally demonstrated in GC×GC-TOF based on a 60m×0.25mm primary column. It was found that Gn was close to 9 compared to the theoretical maximum of about 11 for this system. A six-sigma peak capacity of 4500 was obtained during an 80min heating ramp from 50°C to 320°C. Using peak deconvolution, 2242 individual peaks were determined in a Las Vegas runoff water sample. This is the first definitive experimental demonstration known to us of an order-of-magnitude Gn. The key factors enabling this gain were: relatively sharp (about 20ms at half height) reinjection pulses into the secondary column, relatively long (60m) primary column, the same diameters in primary and secondary columns, relatively low retention factor at the end of the secondary analysis (k≅5 instead of 15, optimal for ideal conditions), optimum flow rate in both columns, and helium (rather than hydrogen) used as the carrier gas. The latter, while making the analysis 65% longer than if using H2, was a better match to the reinjection bandwidth and cycle time.
A new open-atmosphere chemical vapor deposition (CVD) technique has been developed that we term combustion chemical vapor deposition (CCVD). During CCVD a flame provides the necessary environment for the deposition of a dense film whose elemental constituents are derived from solution, vapor, or gas sources. Ag, YSZ, BaTiO3, YIG, YBa2Cu3Ox, and Y2BaCuO5 have been deposited via CCVD with the combustion of a sprayed, cation-containing, organic solution as the sole heat source. CCVD could, for some applications, be less expensive and more flexible than conventional CVD.
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