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21.
Summary The problem is considered of orthogonal 1 fitting of discrete data. Local best approximations are characterized and the question of the robustness of these solutions is considered. An algorithm for the problem is presented, along with numerical results of its application to some data sets. 相似文献
22.
This paper extends previous research on listeners' abilities to discriminate the details of brief tonal components occurring within sequential auditory patterns (Watson et al., 1975, 1976). Specifically, the ability to discriminate increments in the duration delta t of tonal components was examined. Stimuli consisted of sequences of ten sinusoidal tones: a 40-ms test tone to which delta t was added, plus nine context tones with individual durations fixed at 40 ms or varying between 20 and 140 ms. The level of stimulus uncertainty was varied from high (any of 20 test tones occurring in any of nine factorial contexts), through medium (any of 20 test tones occurring in ten contexts), to minimal levels (one test tone occurring in a single context). The ability to discriminate delta t depended strongly on the level of stimulus uncertainty, and on the listener's experience with the tonal context. Asymptotic thresholds under minimal uncertainty approached 4-6 ms, or 15% of the duration of the test tones; under high uncertainty, they approached 40 ms, or 10% of the total duration of the tonal sequence. Initial thresholds exhibited by inexperienced listeners are two-to-four times greater than the asymptotic thresholds achieved after considerable training (20,000-30,000 trials). Isochronous sequences, with context tones of uniform, 40-ms duration, yield lower thresholds than those with components of varying duration. The frequency and temporal position of the test tones had only minor effects on temporal discrimination. It is proposed that a major determinant of the ability to discriminate the duration of components of sequential patterns is the listener's knowledge about "what to listen for and where." Reduced stimulus uncertainty and extensive practice increase the precision of this knowledge, and result in high-resolution discrimination performance. Increased uncertainty, limited practice, or both, would allow only discrimination of gross changes in the temporal or spectral structure of the sequential patterns. 相似文献
23.
Ji QC Zhang J Rodila R Watson P El-Shourbagy T 《Rapid communications in mass spectrometry : RCM》2004,18(19):2293-2298
Quantitative determination of drug concentrations in tissue samples can provide critical information for drug metabolism, kinetics, and toxicity evaluations. For analysis of tissue samples using liquid chromatography/tandem mass spectrometric (LC/MS/MS) detection, homogenization is a critical step in achieving good assay performance. Assay performance can be closely evaluated by spiking the drug directly into tissue samples prior to homogenization. It is especially important to include this assay evaluation for the analysis of artery tissue samples because artery tissue is very elastic, making it quite a challenge to develop an effective procedure for homogenization. An LC/MS/MS assay in 96-well format using liquid-liquid extraction was developed for analyzing ABT-578 in rabbit artery samples. Tissue quality control samples were prepared by spiking ABT-578 stock solutions directly into the tissue before homogenization. The usage of the tissue control samples gives a thorough evaluation of the sample preparation process that includes both homogenization and sample extraction. A 20% blood in saline solution was used as a homogenization solution. Calibration standards were made by spiking ABT-578 into rabbit whole blood. Blood quality control samples were also prepared by spiking ABT-578 into rabbit whole blood. These blood QC samples were used to confirm the validity of the calibration curve. A lower limit of quantitation of 0.050 ng/mL was achieved. The linear dynamic range of blood standards was from 0.050-30.3 ng/mL with the correlation coefficient (r) ranging from 0.9969-0.9996. Overall %CV was between 1.3 and 7.0%, and analytical recovery was between 98.2 and 105.8% for blood QC samples. The %CVs for tissue QC samples were between 6.7 and 13.0%, and analytical recovery after correction was between 93.5 and 114.3%. 相似文献
24.
Peter C. Cherry Derek N. Evans Christopher E. Newall Nigel S. Watson Peter Murray-Rust Judith Murray-Rust 《Tetrahedron letters》1980,21(6):561-564
1,4-Addition of sulphur nucleophiles to the diene () derived the pen-2-em () from clavulanic acid provides the thiadeoxa analogues (–). X-ray analysis of the ester () shows the thermodynamically stable isomers to have the same relative stereochemistry as clavulanic acid. 相似文献
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26.
Two new synthetic approaches to the title compounds are reported. In the first of these, starting with N-carbobenzyloxysarcosine, four synthetic steps are employed to finally assemble the C3? C4 bond of the 1,2-benzothiazine ring. In the second approach, an enol ether is employed as a protecting group to allow formation of the 3-carboxamide function, which is followed by cleavage of the ether function to yield the desired 4-hydroxy-1,2-benzothiazine-3-carboxamide 1,1-dioxide. 相似文献
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Saracoglu N Talaz O Azizoglu A Watson WH Balci M 《The Journal of organic chemistry》2005,70(14):5403-5408
[reaction: see text] endo- and exo-2,3,4,7-tetrahydro-1H-1,4-methanobenzocycloheptene-7-carboxylic acid ethyl esters have been synthesized, and their Diels-Alder cycloaddition reactions with maleic anhydride, dimethyl acetylenedicarboxylate and singlet oxygen have been investigated. The X-ray analysis of four adducts indicated the pyramidalization of the central double bond. Density functional theory calculations on the isolated products and model compounds showed excellent agreement between the experimental and theoretical determined butterfly angles. Furthermore, it has been shown that a cyclopropyl group fused to [2.2.2] system decreases significantly the degree of the pyramidalization which is attributed to the steric interactions between the cyclopropyl group and ethano bridge of the norbornene systems. Due to the instability of the bicyclic endoperoxides, their X-ray analysis could not be carried out. DFT calculations on model compounds showed increased bending in the case of the product obtained by the addition of singlet oxygen to endo-2,3,4,7-tetrahydro-1H-1,4-methanobenzocycloheptene-7-carboxylic acid ethyl ester. 相似文献
30.
The electron density distribution in potassiumbis-(carbonato)cuprate(II) has been analyzed using x-ray diffraction data from an earlier structure determination. While the
copper-ligand geometry is close to square planar the deformation density near the metal is strongly asymmetric. There are
local maxima near the copper atom along the line of the Cu-K vectors. These resemble features found in corresponding regions
in normal length metal-metal bonds. The observation is consistent with the long range nature of the Coulomb potential associated
with the potassium ion. 相似文献