Free radicals in coal and coal conversions. 8. Experimental determination of conversion in hydroliquefaction

The results of conversion determinations on the products from Powhatan No.5 coal liquefied in an autoclave and in a high-pressure, high-temperature e.s.r. cavity are reported. Oil, asphaltene and preasphaltene yields, and overall conversion have been determined for Powhatan No.5 coal samples liquefied in tetralin, SRC-11 heavy distillate, and naphthalene at temperatures from 400 to 480 ° C in both reactor systems. The concept of reaction severity is introduced and used to formalize the relation between the effect of temperature and reaction time on oil yield and conversion. Oil is the predominant product in liquefaction in tetralin or naphthalene, asphaltene is the major product of liquefaction in SRC-II heavy distillate. Retrogressive reaction (THF-insoluble product formation) becomes severe when SRC-II heavy distillate is the liquefaction solvent and residence time of >10 min are used at temperatures >450 °C. Preasphaltenes appear to be the only intermediate species in Powhatan No.5 liquefaction.     

Programmed cooling crystallization of potassium sulphate solutions

The crystal size distribution from a batch cooling crystallizer is predicted by the numerical solution of a mathematical model which uses empirical kinetics of nucleation and crystal growth. The predictions clearly point out the potential advantages of controlled cooling at a constant nucleation rate for improving the product crystal size over that obtained by either natural or linear cooling.Experimental runs following programmed cooling curves for seeded potassium sulphate solutions showed reasonable agreement with the theoretical predictions. A size dispersion of the crystals was observed which contributes to a slight deviation from theory. Nevertheless, controlled cooling significantly reduced the quantity of nuclei formed and improved the product crystal size distribution.     

Characterisation of the neutral oil from a low-temperature coal tar

Tar resulting from fluidised-bed, low-temperature carbonisation of coal was treated to yield a neutral oil from which a series of six other samples was extracted. These were examined by proton magnetic resonance (p.m.r.) spectroscopy, low-ionising-voltage (11 eV) mass spectroscopy (m.s.), gel chromatography followed by fluorescent indicator analysis, and cryoscopy. Aliphatic fractions separated chromatographically were also examined by infra-red spectroscopy. Distributions of hydrogen between chemical types were found for the several fractions from 60 MHz p.m.r. spectra and presented in terms of average structural parameters. M.s. analysis indicated negligible cracking of paraffin components, and the average molecular weight of 197 agreed well with cryoscopic determinations. For the carbon ratio, f_a, between aromatic and total, agreement between m.s. and p.m.r. depends on the p.m.r. structural analysis scheme adopted. P.m.r. and m.s. structural analyses of the aromatics emphasise the predominance of di- and tri-nuclears, with about 40% of available sites substituted, and the importance of acenes in lowtemperature carbonisation material. Gas and gel chromatography showed urea-adductable paraffins to be largely straight-chain C₁₀-C₂₆, much as for tars from carbonisation at higher temperature.     

Soap-based detergent formulations: X. Nature of detergent deposits

The cumulative deposition of detergent residue on unsoiled cotton and polyester-cotton permanent press finish cloth was determined for a variety of detergent formulations after washing 25 consecutive times in 300 ppm hard water in a laboratory Tergotometer. Included in this study were: a phosphate-built laundry detergent, two carbonate-built detergents, tallow soap and various tallow soap formulations with anionic and amphoteric lime soap dispersing agents, and a glassy sodium silicate. Sample swatches washed with each formulation were analyzed for calcium, magnesium, and organic acid content. Fabric washed with the carbonate detergents showed the highest calcium and magnesium content, while those washed with the phosphate detergent and the soap-lime soap dispersant-builder formulations had the lowest. Fabric washed with soap alone had a much higher fatty acid residue than those washed with the other detergent formulations. However, the amount of organic acids left on the fabric after washing with a soap-lime soap dispersing agent formulation was no greater than that produced by phosphate- and carbonate-built detergents. The presence or absence of deposits also was verified visually with a scanning electron microscope. Each formulation also was tested for detergency by measuring the soil buildup in a multiwash procedure. Generally, the buildup of soil paralleled the deposit of detergent residue on the unsoiled cloths.     

Retarding effects of DNA on the autoxidation of liposomal suspensions

Deoxyribonucleic acid (DNA) is associated with the cell membrane of prokaryotes and the inner nuclear membrane of eukaryotes. The unsaturated fatty acids of phospholipids, which constitute the bilaminar structure of membranes, undergo autoxidation in the presence of O₂. Calf thymus DNA was incubated with methyl archidonate-enriched phosphatidyl choline liposomes in order to study the effect of DNA upon the oxidation of phospholipids while present in their natural in vivo bilayer configuration. DNA retarded the rate of lipid oxidation and the TBA test, but it did not alter the induction period. These results suggest that DNA is scavenging free radicals produced within the phospholipid bilayer.     

Cyclic alkanes as geochemical markers in coal liquefaction products

Branched-chain/cyclic alkanes have been obtained, by solvent extraction and molecular-sieve adsorption, from a UK low-temperature (Rexco) coal tar, a USA fluidized-bed pyrolysis (FMC COED) coal tar, and a novel supercritical-gas-extract of a Turkish (Elbistan) lignite. Mass spectrometry (with gas chromatography and field-desorption) established the presence of mono-, di (including sesquiterpanes), tri-, tetra- (steranes only), and pentacyclic (triterpanes only) alkanes, including several steranes and triterpanes not previously reported as coal-tar constituents. The potential of cyclic alkanes as geochemical markers, even for commercial coal products subjected to appreciable heat treatment, is demonstrated by the identification of C₁₂, C₁₃, C₁₅ and C₁₆ dicyclics (including isoprenoid alkanes), C₁₇-C₂₆ tricyclics, and C₂₇ and C₂₉ hopane-type pentacyclics (triterpanes) in FMC, and of C₁₆-C₃₈ monocyclics, C₃₄-C₃₆ dicyclics, C₂₂-C₃₆ tricyclics, C₂₇-C₃₀ tetracyclics (steranes), and C₂₇, C₂₉, C₃₀, C₃₁, C₃₂, and C₃₃ hopane-type pentacyclics (triterpanes) in Rexco tar. Tetra- and pentacyclic alkanes were also preserved in the lignite extract.     

Assessment of response function in two PET scanners with and without interplane septa

The authors have assessed the response function both experimentally and theoretically for two commercial tomographs: CTI 931/08-12 and CTI 953B with and without interplane septa. Monte Carlo simulations were undertaken using the GEANT package from CERN. Spatial resolution (tomographic and axial) was calculated for line sources at various positions in the field of view. Sensitivity and scatter fraction (SF) were calculated for various source geometries as a function of energy discrimination. A very realistic response function in positron emission tomography (PET) is obtained by Monte Carlo methods, using global parameters to account for unsimulated phenomena such as scintillation light transport inside a detector block and its sharing among the various phototubes. Minor discrepancies remain for sensitivity and SF at high energy thresholds and may probably be explained by introducing the observed dispersion in the energy response for the various crystals within a detector block.     

Noise equivalent count measurements in a neuro-PET scanner with retractable septa

The noise-equivalent count-rate (NEC) performance of a neuro-positron emission tomography (PET) scanner has been determined with and without interplane septa on uniform cylindrical phantoms of differing radii and in human studies to assess the optimum count rate conditions that realize the maximum gain. In the brain, the effective gain in NEC performance for three-dimensions (3-D) ranges from >5 at low count rates to approximately 3.3 at 200 kcps (equivalent to 37 kcps in 2-D). The gains of the 3-D method assessed by this analysis are significant, and are shown to be highly dependent on count rate and object dimensions.     

Corrosive Wear in Wet Ore Grinding Systems

JOM - Wear processes in ball and rod mills have recently received increased attention in order to increase efficiency and conserve grinding media. Direct removal of metal from the grinding media...