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3 When 11-diethyl- and 3, 11-di-n-propyl-14-hydroxy-14-azadispiro[5.1. 5.2]pentadec-9-ene-7, 15-dione (E-IV and n-Pr-IV) are heated with polyphosphoric acid at 55–65°, the 14-hydroxyl group cyclizes at the 11-carbon to form E-VI and n-Pr-VI, the structures of which have been established. Compounds P-IV, i-Pr-IV and t-B-IV do not cyclize under these conditions. The Beckmann rearrangement of 12-hydroxy-12-azadispiro[4.1.4.2]tridec-8-ene-6, 13-dione-6-oxime (P-I) with polyphosphoric acid at 40–50° formed only the normal product, P-II, which could not be cyclized. Compound P-IV was the only ketone of this series which would add hydrogen cyanide to form a cyanohydrin. 相似文献
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Environmental Fenton chemistry has been poorly constrained within the marine environment at a multi-component level. A simple, unique, reconfiguration of a flow-injection analytical system combined with luminol chemiluminescence allows quasi-simultaneously the measurement, using a single load-inject valve and a single photon multiplier tube, of reduced iron, Fe(II), and hydrogen peroxide. The system enables rapid, every 22 s, measurements with good accuracy at environmentally relevant concentrations, less than 5% relative standard deviations on both a 5 nM Fe(II) standard and a 60 nM hydrogen peroxide standard. Limits of detection were as low as 40 pM Fe(II) and 100 pM hydrogen peroxide. The system showed excellent capability by measuring from within an organic rich seawater the photochemically induced production of Fe(II) and hydrogen peroxide and their subsequent cycling and Fenton like interactions. 相似文献
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Nightingale KR Palmeri ML Nightingale RW Trahey GE 《The Journal of the Acoustical Society of America》2001,110(1):625-634
A method of acoustic remote palpation, capable of imaging local variations in the mechanical properties of tissue, is under investigation. In this method, focused ultrasound is used to apply localized (on the order of 2 mm3) radiation force within tissue. and the resulting tissue displacements are mapped using ultrasonic correlation based methods. The tissue displacements are inversely proportional to the stiffness of the tissue, and thus a stiffer region of tissue exhibits smaller displacements than a more compliant region. In this paper, the feasibility of remote palpation is demonstrated experimentally using breast tissue phantoms with spherical lesion inclusions, and in vitro liver samples. A single diagnostic transducer and modified ultrasonic imaging system are used to perform remote palpation. The displacement images are directly correlated to local variations in tissue stiffness with higher contrast than the corresponding B-mode images. Relationships between acoustic beam parameters, lesion characteristics and radiation force induced tissue displacement patterns are investigated and discussed. The results show promise for the clinical implementation of remote palpation. 相似文献
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J. J. A. Wijs G. D. Elsdon J. R. Stubbs H. Lührig H. Atkinson A. Azadian G. Spitzer F. W. Epple C. H. Manley H. S. Shrewsbury L. V. Cocks E. Nightingale L. Hoton D. W. Steuart P. Smith G. H. Leopold W. J. de Mooy G. van B. Gilmour S. H. Blichfeldt T. Thornley E. L. Smith H. P. Kaufmann E. R. Bolton und C. Revis 《Fresenius' Journal of Analytical Chemistry》1930,80(7-8):303-314
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The role of the ocean in the cycling of oxygenated volatile organic compounds (OVOCs) remains largely unanswered due to a paucity of datasets. We describe the method development of a membrane inlet-proton transfer reaction/mass spectrometer (MI-PTR/MS) as an efficient method of analysing methanol, acetaldehyde and acetone in seawater. Validation of the technique with water standards shows that the optimised responses are linear and reproducible. Limits of detection are 27 nM for methanol, 0.7 nM for acetaldehyde and 0.3 nM for acetone. Acetone and acetaldehyde concentrations generated by MI-PTR/MS are compared to a second, independent method based on purge and trap-gas chromatography/flame ionisation detection (P&T-GC/FID) and show excellent agreement. Chromatographic separation of isomeric species acetone and propanal permits correction to mass 59 signal generated by the PTR/MS and overcomes a known uncertainty in reporting acetone concentrations via mass spectrometry. A third bioassay technique using radiolabelled acetone further supported the result generated by this method. We present the development and optimisation of the MI-PTR/MS technique as a reliable and convenient tool for analysing seawater samples for these trace gases. We compare this method with other analytical techniques and discuss its potential use in improving the current understanding of the cycling of oceanic OVOCs. 相似文献