Order restricted randomized designs for control versus treatment comparison

We develop a method of randomizing units to treatments that relies on subjective judgement or on possible coarse modeling to produce restrictions on the randomization. The procedure thus fits within the general framework of ranked set sampling. However, instead of selecting a single unit from each set for full measurement, all units within a set are used. The units within a set are assigned to different treatments. Such an assignment translates the positive dependence among units within a set into a reduction in variation of contrasting features of the treatments. A test for treatment versus control comparison, with controlled familywise error rate, is developed along with the associated confidence intervals. The new procedure is shown to be superior to corresponding procedures based on completely randomized or ranked set sample designs. The superiority appears both in asymptotic relative efficiency and in power for finite sample sizes. Importantly, this test does not rely on perfect rankings; rather, the information in the data on the quality of rankings is exploited to maintain the level of the test when rankings are imperfect. The asymptotic relative efficiency of the test is not affected by estimation of the quality of rankings, and the finite sample performance is only mildly affected.     

A finite element-spherical harmonics radiation transport model for photon migration in turbid media

In this paper, we solve the steady-state form of the Boltzmann transport equation in homogeneous and heterogeneous tissue-like media with a finite element-spherical harmonics (FE-P_N) radiation transport method. We compare FE-transport and diffusion solutions in terms of the ratio of absorption to reduced scattering coefficient, (μ_a/μ_s′) and the anisotropy factor g. Two different scattering phase function formulas are employed to model anisotropic scattering in the slab media with high g-value. Influence of void-like heterogeneities, and of their boundaries with the surrounding medium on the transport of photons are also examined.     

Synthesis of 5,6-O-Cyclohexylidene-1-amino-3-azahexane and Its Co(II), Ni(II), Cu(II) Complexes

5,6-O-Cyclohexylidene-1-amino-3-azahexane (L) is synthesized from 1-chloro-2,3-O-cyclohexylidenepropane, which is prepared by the reaction between epichlorohydrin and cyclohexanone. In this reaction, BF₃ · OEt₂ is used as a catalyst. Complexes of Co(II), Ni(II) and Cu(II) acetates with this ligand are prepared. The structures of the ligand and its complexes are proposed based on elemental analysis, IR and UV-VIS spectroscopy, magnetic susceptibility, conductometry, and ¹H and ¹³C NMR spectroscopy.     

Conversion of Allylic Alcohols into Allylic Nitromethyl Compounds via a Palladium-Catalyzed Solvolysis: An Enantioselective Synthesis of an Advanced Carbocyclic Nucleoside Precursor(1)

A two-step reaction sequence to homoallylic nitro compounds from allylic alcohols is presented. Ethoxy carbonylation of the alcohols with ethyl chloroformate provides the corresponding allylic ethyl carbonates in high yields. Exposure of these substrates to catalytic palladium(0) in CH(3)NO(2) initiates a reaction sequence, ionization-decarboxylation-nitromethylation, that culminates with the formation of nitroalkenes. The regio- and stereochemical outcomes of the nitromethyl allylation reaction can be explained by the behavior of the transient pi-allylpalladium complexes. This methodology serves as a centerpiece for the synthesis of an important carbocyclic nucleoside intermediate.     

99mTc-labelled human serum albumin: Chemical and electrochemical labelling methods

The labelling of human serum albumin /HSA/ with^99mTc has been investigated using a chemical method /stannous citrate/ and electrolytically generated tin/II/ ions. A comparative study of various chemical parameters and current intensities has been carried out in order to find the optimal conditions for labelling. The labelling yield was over 95%, for the chemical and electrolytical methods.     

New 3-hydroxyflavone derivatives for probing hydrophobic sites in microheterogeneous systems

Nine new 3-hydroxyflavone derivatives as fluorescent molecular sensors having two well-separated emission bands were synthesized. These sensors can occupy well-determined locations and orientations in macromolecular ensembles, such as micelles due to their finely-tuned designs. These polarity-sensitive dyes can incorporate into the anhydrous hydrophobic core of aqueous micelles.     

The annealing behavior of implanted nitrogen in fcc stainless steel

Post-implantation annealing of N-implanted 304 stainless steel at 400 °C has been investigated by conversion electron Mössbauer spectroscopy, X-ray diffraction and Auger electron spectroscopy. After a 1 h anneal, the near complete dissolution of the as-implanted Fe₂N-like nitride phase results in a 9 at.% N fcc solid-solution phase. After the final anneal (64 h), N has diffused to a depth of about 2 m and remains in solid solution with an average content of 4 at.%. An average N diffusion coefficient at 400 °C is estimated to be 10^-12-10^-14 cm²/s, depending on anneal time, too small to explain the deep penetration observed in high-flux, high-dose N-implanted stainless steel. The present results provide additional evidence for beam controlled N migration where Cr plays an important role.     

Solid phase extraction and preconcentration of uranium(VI) and thorium(IV) on Duolite XAD761 prior to their inductively coupled plasma mass spectrometric determination

A simple and effective method is presented for the separation and preconcentration of thorium(IV) and uranium(VI) by solid phase extraction on Duolite XAD761 adsorption resin. Thorium(IV) and uranium(VI) 9-phenyl-3-fluorone chelates are formed and adsorbed onto the Duolite XAD761. Thorium(IV) and uranium(VI) are quantitatively eluted with 2 mol L⁻¹ HCl and determined by inductively coupled plasma-mass spectrometry (ICP-MS). The influences of analytical parameters including pH, amount of reagents, amount of Duolite XAD761 and sample volume, etc. were investigated on the recovery of analyte ions. The interference of a large number of anions and cations has been studied and the optimized conditions developed have been utilized for the trace determination of uranium and thorium. A preconcentration factor of 30 for uranium and thorium was achieved. The relative standard deviation (N = 10) was 2.3% for uranium and 4.5% for thorium ions for 10 replicate determinations in the solution containing 0.5 μg of uranium and thorium. The three sigma detection limits (N = 15) for thorium(IV) and uranium(VI) ions were found to be 4.5 and 6.3 ng L⁻¹, respectively. The developed solid phase extraction method was successively utilized for the determination of traces thorium(IV) and uranium(VI) in environmental samples by ICP-MS.     

Investigation of Raman,FT-IR,EPR spectra and antimicrobial activity of 2-(5-H/Me/Cl-1<Emphasis Type="BoldItalic">H</Emphasis>-benzimidazol-2-yl)-phenol ligands and their Fe(NO<Subscript>3</Subscript>)<Subscript>3</Subscript> complexes

2-(5-H/Me/Cl-1H-benzimidazol-2-yl)-phenol ligands form 1:1 electrolytes, 5-coordinate monometallic complexes with iron(III) nitrate. The geometry of the [Fe(L)(OH)(H₂O)₂](NO₃) complexes was derived from theoretical calculation in DGauss/DFT level (DZVP basis set) on CACHE. In all of the complexes the ligands are bidentate, via one imine nitrogen atom and phenolate oxygen atom. The coordination is completed with a hydroxide ion, and two water molecules, adopting a distorted square pyramidal geometry. The structures of the compounds were confirmed on the basis of elemental analysis, molar conductivity, magnetic moment, FT-Raman, FT-IR (mid-IR, far-IR), EPR and u.v.–vis. The antimicrobial activities of the free ligands, their hydrochloride salts, and the complexes were evaluated using the disk diffusion method in dimethyl sulfoxide (DMSO) as well as the minimal inhibitory concentration (MIC) dilution method, against nine bacteria and the results are compared with several known antibiotic agents. Antifungal activities were reported for Candida albicans, Kluyveromyces fragilis, Rhodotorula rubra, Debaryomyces hansenii, Hanseniaspora guilliermondii, and the results were referenced against nystatin, ketaconazole, and clotrimazole antifungal agents. In most cases, the compounds tested showed broad-spectrum (Gram⁺ & Gram⁻ bacteria) activities that were either more active or as potent as the references.     

Titrimetric determination of selenium in anodic slimes

The determination of selenium in the presence of tellurium and copper has been studied, to allow analysis of anodic slimes from electrolytic copper refining. Three methods have been developed for the determination of selenium in these slimes. They are based on the extraction of selenium with sodium sulphite, reduction of selenite with sodium sulphite, and separation of selenium and tellurium by adjustment of pH. Selenium (10(-3)-10(-2)M) is determined in the presence of tellurium, copper, iron, silver and lead. The methods are fast and simple, do not need expensive reagents, and give satisfactory results.