Continuous chromatographic separation of glucose-fructose mixtures using anion-exchange resins

Summary A semi-continuous, counter-current chromatographic refiner (SCCR) was packed with an anion resin in the bisulphite form and used to separate mixtures of sugars from different feedstocks. Products with purities of more than 99% were achieved and solid concentrations of the fructose products of 12% w/v were possible. The deterioration of the anion resin was controlled by simple precautions and thus its useful life was substantially prolonged.     

Spectroscopic investigations in molecularly organized solvent media. Part 3. Examination of the nitromethane selective quenching rule in aqueous anionic + cationic and anionic + nonionic mixed surfactant solutions

Applicability of the nitromethane selective quenching rule for discriminating between alternant versus nonalternant polycyclic aromatic hydrocarbons (PAHs) is examined for 20 representative PAH solutes dissolved in micellar sodium dodecylsulfate (SDS) + cetyltrimethylammonium bromide (CTAB), SDS + dodecyltrimethylammonium bromide (DTAB), SDS + Brij-35, and SDS + sodium octanoate (SO) mixed surfactant solvent media. Experimental results show that nitromethane quenched fluorescence of all 8 alternant PAHs studied in the four different solvent systems. Unexpected quenching behavior was observed, however, in the case of nonalternant PAHs. Nitromethane quenched fluorescence emission of nonalternant PAHs dissolved in the SDS + SO solvent media, which is contrary to the selective quenching rule. In the case of the mixed anionic + cationic surfactant solvent media, nitromethane quenching selectivity was restored at concentration ratios of approximately 4 : 1 (anionic:cationic) or less. Received: 22 May 1997 / Revised: 29 September 1997 / Accepted: 3 October 1997     

Theoretical aspects of a preparative continuous chromatograph

Summary Equipment which has been used or suggested for preparative scale chromatography is reviewed. Particular attention is paid to one form of equipment for continuous counter-current chromatography which employs a moving mechanical seal. The theoretical effects of practical operating conditions and the mode of operation of this equipment are discussed. The influence of these effects on polymer fractionation is also considered. A theoretical model, based on the equilibrium stage concept, is proposed for the simulation of continuous gel permeation chromatography of a binary feed on such an apparatus. Examples of the results obtained from the computer simulation are given.     

Effect of flashlamp diameter on luminescent coolants for a solid-state laser

Reducing the diameter of the flashlamp was found to increase the percent improvement in output of a solid-state laser caused by using luminescent coolants. However, this change in diameter also reduced the effectiveness of the flashlamp in producing long (150 s) laser pulses so that an overall decrease in laser output was observed. In the formation of short (40 s) laser pulses, on the other hand, larger absolute values were obtained using the smaller diameter flashlamp.     

Long range transport of biomass aerosol to Greenland: Multi-spectroscopic investigation of particles deposited in the snow

Summary Results are given from the NIST component of a pilot (“winter-over”) study of seasonal patterns of natural and anthropogenic species in air and snow transported to Summit, Greenland. Central to this research is the quantitative apportionment of fossil and biomass particulate carbon, based on advanced (micromolar) ¹⁴C accelerator mass spectrometry (AMS) applied to remote snow samples containing as little as 9 µg C/kg. The measurements were made practicable through stringent attention to the nature and sources of the isotopic-chemical blank, resulting in a blank reduction from »5 µg C to <0.5 µg C. An important result of this work is the first evidence of a seasonal pattern in biomass-C particles in Greenland snow. Although ¹⁴C AMS data serve to resolve fossil and biomass carbon quantitatively, a deeper understanding of the aerosol sources and character demands a multidisciplinary approach. This is illustrated with “multi-spectrometric” macro- and micro-analytical data for two cases involving substantial incursions of biomass aerosol to the Summit, Greenland snow.     

Amides as precursors of imidoyl radicals in cyclisation reactions

Amides have been successfully used as precursors of imidoyl radicals for radical cyclisation. The amides have been converted to imidoyl selanides via reaction with phosgene to yield imidoyl chlorides followed by reaction with potassium phenylselanide. Imidoyl selanides were reacted with tributyltin hydride (Bu₃SnH) as the radical mediator with triethylborane or AIBN as initiators to yield imidoyl radicals for cyclisation reactions. Imidoyl radicals have been cyclised onto alkenes to yield 2,3-substituted-indoles and -quinolines and also onto pyrroles and indoles to give bi- and tricyclic heteroarenes.