Publications

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In the interest of providing an economically sensible use for the copious small-diameter wood in Northern New Mexico, an economic study is performed focused on mobile pyrolysis. Mobile pyrolysis was selected for the study because transportation costs limit the viability of a dedicated pyrolysis plant, and the relative simplicity of pyrolysis compared to other technology solutions lends itself to mobile reactor design. A bench-scale pyrolysis system was used to study the wood pyrolysis process and to obtain performance data that was otherwise unavailable under conditions theorized to be optimal given the regional problem. Pyrolysis can convert wood to three main products: fixed gases, liquid pyrolysis oil and char. The fixed gases are useful as low-quality fuel, and may have sufficient chemical energy to power a mobile system, eliminating the need for an external power source. The majority of the energy content of the pyrolysis gas is associated with carbon monoxide, followed by light hydrocarbons. The liquids are well characterized in the historical literature, and have slightly lower heating values comparable to the feedstock. They consist of water and a mix of hundreds of hydrocarbons, and are acidic. They are also unstable, increasing in viscosity with time stored. Up to 60% of the biomass in bench-scale testing was converted to liquids. Lower ({approx}550 C) furnace temperatures are preferred because of the decreased propensity for deposits and the high liquid yields. A mobile pyrolysis system would be designed with low maintenance requirements, should be able to access wilderness areas, and should not require more than one or two people to operate the system. The techno-economic analysis assesses fixed and variable costs. It suggests that the economy of scale is an important factor, as higher throughput directly leads to improved system economic viability. Labor and capital equipment are the driving factors in the viability of the system. The break-even selling price for the baseline assumption is about $11/GJ, however it may be possible to reduce this value by 20-30% depending on other factors evaluated in the non-baseline scenarios. Assuming a value for the char co-product improves the analysis. Significantly lower break-even costs are possible in an international setting, as labor is the dominant production cost.

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Sandia National Laboratories (SNL) conducted accelerated atmospheric corrosion testing for the U.S. Consumer Product Safety Commission (CPSC) to help further the understanding of the development of corrosion products on conductor materials in household electrical components exposed to environmental conditions representative of homes constructed with problem drywall. The conditions of the accelerated testing were chosen to produce corrosion product growth that would be consistent with long-term exposure to environments containing humidity and parts per billion (ppb) levels of hydrogen sulfide (H{sub 2}S) that are thought to have been the source of corrosion in electrical components from affected homes. This report documents the test set-up, monitoring of electrical performance of powered electrical components during the exposure, and the materials characterization conducted on wires, screws, and contact plates from selected electrical components. No degradation in electrical performance (measured via voltage drop) was measured during the course of the 8-week exposure, which was approximately equivalent to 40 years of exposure in a light industrial environment. Analyses show that corrosion products consisting of various phases of copper sulfide, copper sulfate, and copper oxide are found on exposed surfaces of the conductor materials including wires, screws, and contact plates. The morphology and the thickness of the corrosion products showed a range of character. In some of the copper wires that were observed, corrosion product had flaked or spalled off the surface, exposing fresh metal to the reaction with the contaminant gasses; however, there was no significant change in the wire cross-sectional area.

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Thermal decomposition of poly dimethyl siloxane compounds, Sylgard{reg_sign} 184 and 186, were examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a method of producing multiway data using a stepped thermal desorption. The technique involves sequentially heating a sample of the material of interest with subsequent analysis in a commercial GC/MS system. The decomposition chromatograms were analyzed using multivariate analysis tools including principal component analysis (PCA), factor rotation employing the varimax criterion, and multivariate curve resolution. The results of the analysis show seven components related to offgassing of various fractions of siloxanes that vary as a function of temperature. Thermal desorption coupled with gas chromatography-mass spectrometry (TD/GC-MS) is a powerful analytical technique for analyzing chemical mixtures. It has great potential in numerous analytic areas including materials analysis, sports medicine, in the detection of designer drugs; and biological research for metabolomics. Data analysis is complicated, far from automated and can result in high false positive or false negative rates. We have demonstrated a step-wise TD/GC-MS technique that removes more volatile compounds from a sample before extracting the less volatile compounds. This creates an additional dimension of separation before the GC column, while simultaneously generating three-way data. Sandia's proven multivariate analysis methods, when applied to these data, have several advantages over current commercial options. It also has demonstrated potential for success in finding and enabling identification of trace compounds. Several challenges remain, however, including understanding the sources of noise in the data, outlier detection, improving the data pretreatment and analysis methods, developing a software tool for ease of use by the chemist, and demonstrating our belief that this multivariate analysis will enable superior differentiation capabilities. In addition, noise and system artifacts challenge the analysis of GC-MS data collected on lower cost equipment, ubiquitous in commercial laboratories. This research has the potential to affect many areas of analytical chemistry including materials analysis, medical testing, and environmental surveillance. It could also provide a method to measure adsorption parameters for chemical interactions on various surfaces by measuring desorption as a function of temperature for mixtures. We have presented results of a novel method for examining offgas products of a common PDMS material. Our method involves utilizing a stepped TD/GC-MS data acquisition scheme that may be almost totally automated, coupled with multivariate analysis schemes. This method of data generation and analysis can be applied to a number of materials aging and thermal degradation studies.

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2-Chloroethyl phenyl sulfide (CEPS), a surrogate compound of the chemical warfare agent sulfur mustard, was examined using thermal desorption coupled gas chromatography-mass spectrometry (TD/GC-MS) and multivariate analysis. This work describes a novel method of producing multiway data using a stepped thermal desorption. Various multivariate analysis schemes were employed to analyze the data. These methods may be able to discern different sources of CEPS. In addition, CEPS was applied to cotton, nylon, polyester, and silk swatches. These swatches were placed in controlled humidity chambers maintained at 23%, 56%, and 85% relative humidity. At regular intervals, samples were removed from each test swatch, and the samples analyzed using TD/GC-MS. The results were compared across fabric substrate and humidity.

A large volume-headspace apparatus that permits the heating of pottery fragments for direct analysis by gas chromatography/mass spectrometry (GC/MS) is described here. A series of fermented-corn beverages were produced in modern clay pots and the pots were analyzed to develop organic-species profiles for comparison with fragments of ancient pottery. Brewing pots from the Tarahumara of northern Mexico, a tribe that produces a corn-based fermented beverage, were also examined for volatile residues and the organic-species profiles were generated. Finally, organic species were generated from ancient potsherds from an archeological site and compared with the modern spectra. The datasets yielded similar organic species, many of which were identified by computer matching of the resulting mass spectra with the NIST mass spectral library. Additional analyses are now underway to highlight patterns of organic species common to all the spectra. This presentation demonstrates the utility of thermal desorption coupled with GC/MS for detecting fermentation residues in the fabric of unglazed archaeological ceramics after centuries of burial. © 2008 Materials Research Society.

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Rapid detection and identification of bacteria and other pathogens is important for many civilian and military applications. The taxonomic significance, or the ability to differentiate one microorganism from another, using fatty acid content and distribution is well known. For analysis fatty acids are usually converted to fatty acid methyl esters (FAMEs). Bench-top methods are commercially available and recent publications have demonstrated that FAMEs can be obtained from whole bacterial cells in an in situ single-step pyrolysis/methylation analysis. This report documents the progress made during a three year Laboratory Directed Research and Development (LDRD) program funded to investigate the use of microfabricated components (developed for other sensing applications) for the rapid identification of bioorganisms based upon pyrolysis and FAME analysis. Components investigated include a micropyrolyzer, a microGC, and a surface acoustic wave (SAW) array detector. Results demonstrate that the micropyrolyzer can pyrolyze whole cell bacteria samples using only milliwatts of power to produce FAMEs from bacterial samples. The microGC is shown to separate FAMEs of biological interest, and the SAW array is shown to detect volatile FAMEs. Results for each component and their capabilities and limitations are presented and discussed. This project has produced the first published work showing successful pyrolysis/methylation of fatty acids and related analytes using a microfabricated pyrolysis device.

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To address lithium-ion cell safety issues in demanding power applications, electrical and thermal abuse tests were performed on 18650 sized cells. Video and electrically monitored abuse tests in air included short circuit, forced overcharge, forced reversal, and controlled overheating (thermal) modes. Controlled overheating tests to 200 C were performed in a sealed chamber under a helium atmosphere and the gases released from the cell during thermal runaway were analyzed at regular intervals using gas chromatography and mass spectrometry. In addition to alkane and alkene solvent breakdown fragments, significant H{sub 2} was detected and evidence that HF was evolved was also found.