The application of high-speed TV-holography to time-resolved vibration measurements

We describe an electronic speckle pattern interferometer (ESPI) system that has enabled non-harmonic vibrations to be measured with μs temporal resolution. The short exposure period and high framing rate of a high-speed camera at up to 40,500 frames per second allow low-power CW laser illumination and fibre-optic beam delivery to be used, rather than the high peak power pulsed lasers normally used in ESPI for transient measurement. The technique has been demonstrated in the laboratory and tested in preliminary industrial trials. The ability to measure vibration with high spatial and temporal resolution, which is not provided by techniques such as scanning laser vibrometry, has many applications in manufacturing design, and in an illustrative application described here revealed previously unmeasured “rocking” vibrations of a car door. It has been possible to make the measurement on the door as part of a complete vehicle standing on its own tyres, wheels and suspension, and where the excitation was generated by the running of the vehicle's own engine.     

Low-background counting systems compared

A comparison of special low-background germanium counting systems used at the Pacific Northwest Laboratory will be presented. These vary from specially modified instruments in the laboratory to low-cosmic-exposure detectors operated deep underground. The underground detectors have copper cryostats completely electroformed from low-background copper. Electroforming is a process analogous to zone refining in its ability to remove chemical impurities. Shielding techniques and their merit are compared as to difficulty and benefit. Active cosmic veto is directly compared to passive overburden shielding. Special attention is paid to cosmic activation of the cryostat and the germanium crystal itself.Operated for the U. S. Department of Energy by Battelle Memorial Institute under Contract DE-AC06-76RL0 1830.     

Preparation of certain 2-N-alkylamino-and 2-N,N-dialkylamino-10-methylphenothiazines via phenothiazyne

The treatment of 2-chloro-10-methylphenothiazine, 1 , with lithium alkylamide/alkylamine or lithium dialkylamide/dialkylamine yields the corresponding 2-N-alkylamino-or 2-N,N-dialkylaminophenothiazines in good yields via phenothiazyne. No significant reduction of 1 to 10-methylphenothiazine is observed. Yields of amines obtained by this method are considerably higher than those obtained by reacting 1 with sodamide in refluxing amine solvent. Attempts to introduce the -CH₂CN moiety onto the phenothiazine nucleus by treating 1 with sodamide and acetonitrile in liquid ammonia produced only 2-amino-10-methylphenothiazine.     

Achieving ultralow background in a germanium spectrometer

A germanium diode gamma-ray spectrometer has been constructed that exhibits background levels three orders of magnitude lower than conventional low-background laboratory spectrometers in the energy region around 100 keV and five orders of magnitude lower in the energy region above 3 MeV. The steps necessary to achieve this reduction are described, and the application of this technology to construction of ultralow background laboratory based germanium diode gamma-ray spectrometers is discussed.Operated for the U.S. Department of Energy by Battelle Memorial Institute under Contract DE-AC06-76RLO 1830.     

Practical stereoselective synthesis of an alpha-trifluoromethyl-alpha-alkyl epoxide via a diastereoselective trifluoromethylation reaction

A practical stereoselective synthesis is reported for an alpha-trifluoromethyl-alpha-alkyl epoxide (1), which is an important pharmaceutical intermediate. The key step involves a chiral auxiliary-controlled asymmetric trifluoromethylation reaction for the introduction of the unique trifluoromethyl-substituted tertiary alcohol stereogenic center in the target molecule. The fluoride-initiated CF3 addition to chiral keto ester 6a proceeded with a diastereoselectivity up to 86:14. The major diastereomer was readily obtained with a >99.5:0.5 dr through a simple crystallization of the crude product mixture.     

Organometallic methods for the synthesis and functionalization of azaindoles

Azaindoles (also called pyrrolopyridines) constitute essential subunits in many pharmaceutically important compounds. The synthesis of azaindoles has been a great synthetic challenge for chemists. Many classical methods for indole synthesis (such as Fischer and Madelung cyclizations) often cannot be effectively applied to the synthesis of the corresponding azaindoles. In recent years, advances in organometallic chemistry have enabled a number of novel and efficient methodologies for azaindole formation as well as for the further functionalization of azaindole templates. In this tutorial review, we have surveyed the recent development of organometallic chemistry-based methods for azaindole synthesis.     

Phase Transfer Catalysis: Preparation of Alkyl Thiocyanates

Phase transfer catalysis has been employed for many nucleo-philic substitution reactions.¹ Generally these reactions have employed quaternary ammonium salts as catalysts. Among the displacement reactions reported is the formation of thiocyanates.² Tertiary amines have also been used as catalysts for phase transfer generation of carbenes.³ Recently we reported the preparation of alkyl cyanides to be catalyzed by amines under phase transfer conditions.⁴     

Role of attention in overshoot: frequency certainty versus uncertainty

Overshoot, the elevation in the threshold for a brief signal that comes on close to masker onset, was measured with signal frequency certain (same frequency on every trial) or uncertain (randomized over trials). In broadband noise, thresholds were higher 2 ms after masker onset than 200 ms later, by 9 dB with frequency certainty, by 6-7 dB with uncertainty. In narrowband noise centered on the signal frequency, thresholds at 2 ms were not elevated with certainty, but were elevated 4-5 dB with uncertainty. Thus, frequency uncertainty leads to less overshoot in broadband noise, to more overshoot in narrowband noise. Reduced overshoot in broadband noise may come about because the masker, given its many frequencies, disrupts focusing at onset as much under certainty as uncertainty. Once the initial disruption dissipates, threshold is lower with certainty so overshoot is greater. In contrast, a narrowband noise with frequencies only near the signal does not disrupt focusing when the signal frequency is known beforehand, so overshoot is absent. When frequency is uncertain, the narrowband noise serves to focus attention on the signal frequency; as this requires time, detection near noise onset is poorer than later on, so overshoot is present.