Statistical suitability testing of the Aliquat-336, AnaLig® Pu-02 and TRU® Resin use for the 239,240Pu, 238Pu determination

In this paper three different methods were used for plutonium separation and statistical tested-molecular recognition technology products AnaLig^® Pu-02, liquid–liquid extraction with Aliquat-336 and extraction chromatography with TRU^® Resin. The methods performance was investigated by analysis of NPL (High Alpha–Beta 2005) intercomparison sample. Regression diagnostics procedures were used for examination of the regression triplet and pair t test were applied for comparison of methods for the separation of ^239,240Pu, ²³⁸Pu with Aliquat-336, TRU^® Resin and AnaLig^® Pu-02. The presented results were evaluated as correct for all experimental data.     

Rapid determination of 239,240Pu, 238Pu, 241Am and 90Sr in radioactive waste using combined SPE sorbents AnaLig? Pu02, AnaLig? Sr01 and TRU? Resin

A rapid separation method has been developed which allows measurement of plutonium, americium and strontium isotopes in the radioactive sludge from Nuclear power plant A1 Jaslovske Bohunice (NPP A1) with high chemical recoveries and effective removal of matrix interferences. This method uses different commercial products stacked AnaLig^? Pu02, AnaLig^? Sr01 and TRU^? Resin cartridges from IBC Advanced Technologies and Eichrom Technologies. The method allows the rapid separation of plutonium, strontium and americium using a single multi-stage column in the vacuum box (cartridge technology) with rapid flow rates to minimize sample separation time. The ^239,240Pu, ²³⁸Pu and ²⁴¹Am were determined by alpha spectroscopy, ⁹⁰Sr was counted on TRICARB 2900 TR by Cerenkov counting of its progeny ⁹⁰Y.     

Determination of 239,240Pu, 238Pu isotopes in soil samples using molecular recognition technology product AnaLig?Pu-02 gel

Procedure for analysis of plutonium isotopes in soil samples was developed using a new molecular recognition technology product AnaLig^?Pu-02 gel. Extraction chromatography TEVA^? Resin was used for purification of plutonium phase to remove thorium impurities which interfere in Pu determination by alpha spectrometry. The performance of the method was successfully tested by analysis of a sand stimulant sample and a soil sample spiked with known activity of ²³⁹Pu. The results obtained for procedures were compared in terms of activities and recoveries.     

Statistical suitability testing of 3M Empore™ Sr disc and AnaLig® Sr-01 use for 90Sr determination

In this paper rapid separation methods for strontium determination using molecular recognition technology products 3M Empore? Sr disc, AnaLig^® Sr-01 and extraction chromatography Sr^® Resin were presented and statistical tested. The methods performance was investigated by analysis of NPL (High Alpha–Beta 2003) and (High Alpha–Beta 2005) intercomparison samples. The presented results were evaluated as correct for all experimental data. We used linear regression (with regression diagnostics), t test and the mean of variable using ⁹⁰Sr with 3M Empore? Sr disc, AnaLig^® Sr-01 and Sr^® Resin.     

Contents of238Pu,239,240Pu and137Cs in sediments and shore depositions of the Vltava river in 1995–1996

The²³⁸Pu,^239,240Pu and¹³⁷Cs concentrations in sediments and shore deposition samples of the Vltava river were determined.^239,240Pu and¹³⁷Cs concentrations in sediment samples (five locations) ranged from 19.6 to 124.8 mBq·kg⁻¹ and from 1.8 to 28.2 Bq·kg⁻¹, respectively. The²³⁸Pu,^239,240Pu and¹³⁷Cs concentrations in shore deposition samples (four locations) ranged from 2 to 16.8, from 26.8 to 477.2 mBq·kg⁻¹, and from 1.6 to 86.3 Bq·kg⁻¹, respectively. The superficial activity of studied radionuclides in shore deposition areas was determined and radionuclide origin at studied locations was discussed.     

Spectra and dose with ANN of 252Cf, 241Am–Be, and 239Pu–Be

Artificial neural networks have been applied to unfold the neutron spectra and to calculate the effective dose, the ambient equivalent dose, and the personal dose equivalent for ²⁵²Cf, ²⁴¹Am–Be, and ²³⁹Pu–Be neutron sources. The count rates that these neutron sources produce in a Bonner Sphere Spectrometer with a ⁶LiI(Eu) were utilized as input in both artificial neural networks. Spectra and the ambient dose equivalent were also obtained with BUNKIUT code and the UTA4 response matrix. With both procedures spectra and ambient dose equivalent agrees in less than 10%. The Artificial neural network technology is an alternative procedure to unfold neutron spectra and to perform neutron dosimetry.     

Detection of diazepam in urine,hair and preserved oral fluid samples with LC-MS-MS after single and repeated administration of Myolastan® and Valium®

Sedative agents are used to facilitate sexual assault due to their ability to render the victim passive, submissive and unable to resist. The primary pharmacological effect of the benzodiazepine tetrazepam is muscle relaxation, whereas the benzodiazepine diazepam acts on the central nervous system (CNS) exerting mainly sedation effects. Therefore, contrary to tetrazepam, diazepam is an often-abused drug, which can potentially be used as a date-rape drug. In this study, we describe the detection of low amounts of diazepam in Myolastan (Sanofi-Synthelabo S.A., Brussels, Belgium) and Epsipam (Will-Pharma, Wavre, Belgium) 50 mg tablet preparations by LC-MS-MS, GC-FID and HPLC-DAD. Considering the important forensic implication of this finding, a study was conducted with volunteers receiving a single or repeated dosage of Myolastan. Urine, hair and preserved oral fluid samples were analysed using a previously described sensitive and specific LC-MS-MS detection method allowing for the simultaneous quantification of tetrazepam, diazepam, nordiazepam, oxazepam and temazepam. This study demonstrates that diazepam can be observed in urine samples even after a single dose of Myolastan. In addition, maintaining therapy for 1 week results in the detection of both diazepam and nordiazepam in urine samples and of diazepam in the first hair segment. Importantly, comparing urine and hair samples after a single intake of diazepam versus the single and 1 week administration of Myolastan shows that the possible metabolic conversion of tetrazepam to diazepam is a more plausible explanation for the detection of diazepam in biological samples after the intake of Myolastan. As such, these results reveal that the presence of diazepam and/or nordiazepam in biological samples from alleged drug-facilitated assault cases should be interpreted with care.     

Synthesis,structure, computational modeling and biological activity of two new Casiopeínas® complexes and their nanoparticles

Abstract

This study was conducted to prepare new complexes and their metal-based nanodrugs in order to reduce the growth of human carcinoma cell lines. For this purpose, an extensive study was performed. First, the mixed-chelate Cu(II) complexes Casiopeínas^® ([Cu(TTA)(phen)(C1O₄)] 1 and [Cu(TTA)(phen)(N₃)Cu(TTA)(phen)H₂O] (C1O₄)·H₂O 2 (TTA = 4,4,4-trifluoro-1-(2-furyl)-1,3-butanedione) were synthesized and characterized by X-ray, FT-IR, UV–Vis spectroscopy, conductivity measurements, diffuse reflection spectroscopy and elemental analysis studies. Complexes 1 and 2 exhibited tetragonal pyramidal geometry. In the following, nanoparticles (NPs) of complexes 3 and 4 with the average size of 81 and 33?nm, respectively, were prepared by an ultrasonic process. Scanning Electron Microscope (SEM) images of samples 3 and 4 showed that the morphologies of the obtained materials are rod and sphere, respectively. Furthermore, the cytotoxic activity of complexes and nanoparticles was investigated against MKN-45 cell lines. The cell proliferation was inhibited for all compounds and nanocompounds in a dose-dependent manner 1?>?2 > 3?>?4 on MKN-45 cells. Finally, docking calculations were performed to describe the mode of binding to DNA of these complexes. Docking simulations suggested that the compounds bind in the minor groove and preferentially bind to A-T base pair regions. Both complexes also interacted with DNA through one hydrogen-bond.     

Formal Synthesis of Ambrox® and 9-Epiambrox

(-)-Drimenol (5) was used as starting material for the synthesis of diastereoisomeric diols 3 and 4, through the nitrile 7, Compounds 3 and 4 are the direct precursors of Ambrox® (1) and 9-epiambrox (2).     

π-Stacking between Casiopeinas® and DNA bases

Casiopeínas? are copper complexes with the general formula [Cu(N-N)(N-O)]NO(3) and [Cu(N-N)(O-O)]NO(3) where N-N denotes a substituted bipyridine or phenanthroline, N-O indicates α-aminoacidate or peptide and O-O represents acetylacetonate or salicylaldehyde. This family of compounds has been evaluated in vitro and in vivo showing cytotoxic, genotoxic, and antineoplastic activity. The action mechanism is still not completely elucidated, but the possibility exists that these compounds interact with DNA by intercalation due to the aromatic moiety. In this work we found, using the properties of the electron density of a π-complex model base-Casiopeína?-base, that the stacking mechanism between Casiopeínas? and DNA bases is due to an electron density deficiency of the ligand of the Casiopeína? which is compensated for by an electron transfer from adenines by a π-π interaction.     

Thermal analysis of Vectran® fibers and films

Vectra^® liquid crystalline polymers (LCP's) were introduced as commercial products in the mid-1980's. The first of these (Vectra A130) was a wholly aromatic thermotropic copolyester ofp-hydroxybenzoic acid and 6-hydroxy-2-naphthoic acid. Vectra A130 is a thermotropic LCP that can be melt spun into filaments that on heat treatment are characterized by high strength and high modulus. Vectra resin can also be extruded into films. In the fiber or film form this material is commercially known as Vectran^®. Heat treatment enhances the tensile strength of Vectran fiber variants. Because of this, the elucidation of the physical transformations taking place in the internal structure of the material during heating has always been an important subject. Several thermal techniques are used to indicate clearly that what is observed as a glass transition is unlike the conventional glass transition in typical semicrystalline polymers. There is also an indication of the presence of multiple states of mesophase aggregation that collapse into a single state when taken to high enough temperatures.     

Boron environments in Pyrex® glass--a high resolution, Double-Rotation NMR and thermodynamic modelling study

It is shown, using the important technological glass Pyrex? as an example, that 1D and 2D (11)B Double-Rotation (DOR) NMR experiments, in combination with thermodynamic modelling, are able to provide unique structural information about complex glasses. (11)B DOR NMR has been applied to Pyrex? glass in order to remove both dipolar and quadrupolar broadening of the NMR lines, leading to high resolution spectra that allow unambiguous, accurate peak fitting to be carried out, of particular importance in the case of the 3-coordinated [BO(3)] (B3) trigonal planar environments. The data obtained are of sufficient quality that they can be used to test the distributions of borate and borosilicate superstructural units predicted by the thermodynamics-based Model of Associated Solutions. The model predicts the dominant boron-containing chemical groupings in Pyrex? glass to be those associated with B(2)O(3) and sodium tetraborate (with smaller amounts of sodium triborate, sodium diborate, sodium pentaborate, danburite and reedmergnerite). Excellent agreement is found between model and experiment provided the (11)B peaks with isotropic chemical shifts of -1.4 ppm and 0.5 ppm are assigned to B4 species from borosilicate units ([B(OSi)(4)] and [B(OSi)(3)(OB)]) and borate superstructural units (mainly triborate rings with some pentaborate and diborate) respectively. The peaks with isotropic shifts of 14 ppm and 18.1 ppm are then assigned to B3 in borate superstructural units (mainly triborate and pentaborate along with connecting B3) and boroxol rings respectively. The assignments of the DOR NMR peaks, are supported by the presence of cross-peaks in (11)B spin-diffusion DOR NMR spectra which can be used to develop a structural model in which B(2)O(3)-like regions are linked, via borate and borosilicate superstructural units, to the majority silica network. Pyrex? is thus shown to have a heterogeneous structure, with distinct molecular groupings that are far removed from a random distribution of network polyhedra with only short-range order.     

Acylation and O-sulfonylation of Quincorine® and Quincoridine®. Efficient intramolecular catalysis

A convenient preparation of enantiopure O-acyl and O-sulfonyl derivatives of Quincorine^® and Quincoridine^® is described.     

Formulation study on retinoic acid gel composed of iota-carrageenan, polyethylene oxide and Emulgen® 408

In the present study, all-trans retinoic acid (RA) gels formulated with various compositions of polyethylene oxide (Emulgen?) and iota-carrageenan (ι-CG) were prepared and their physicochemical properties were evaluated. The compression energy, which is the work required to compress the product through a fixed distance, increased with increasing amount of ι-CG or Emulgen?. The adhesion energy and displacement decreased with increasing amount of ι-CG or Emulgen? due to the progression of gel formation. From the results of the sensory tests, the properties of RA gels such as adhesiveness, gel strength and spreadability seemed to be adjustable depending on the condition of skin by varying the components of RA gels. Through photostability study, the expiration date and storage conditions of RA gels were determined as "4°C for 28?d with no exposure to light."     

Cs, Am and Pu isotopes as tracers of sedimentation processes in the Curonian Lagoon–Baltic Sea system

¹³⁷Cs, ²⁴¹Am and Pu isotopes were analyzed in seawater, bottom sediments (BS) and suspended particulate matter samples collected in the Baltic Sea during 1997–2011. The particle size distribution and sequential extraction studies were carried out with the aim to better understand the association of radionuclides with particles and their bonding patterns in the BS. δ¹³C_org was applied for identification of sources of organic matter in the studied area. It has been found that massic activities of ¹³⁷Cs in BS varied from 2.1 to 588 Bq/kg. High correlation of ¹³⁷Cs massic activities with total organic carbon (TOC) in BS (r = 0.75) and with clay minerals (r = 0.95) was found. ^239,240Pu massic activities in BS varied from 0.03 to 7.5 Bq/kg. High correlation with TOC was found for ^239,240Pu (R = 0.98) as well as for ²⁴¹Am (r = 0.96). δ¹³C_org in the studied samples ranged from ?22.3 to ?31.8 ‰.     

Synthesis and characterization of nanosized NiO2 and NiO using Triton® X-100

Nanosized NiO₂ particles with an average diameter of 15 nm are prepared by treating of Ni(NO₃)₂ · 6H₂O with an aqueous solution of KClO in the presence of Triton® X-100. This black fine powder of nickel peroxide was characterized by XRD diffraction, energy dispersive spectroscopy (EDS) and scanning electron microscopy (SEM). The as-prepared NiO₂ can be easily transformed to nanosized NiO merely by washing it with acetone. The obtained NiO has an average diameter of 40 nm and was characterized by the same means used for NiO₂. The nanoparticles of NiO₂ and NiO were obtained in high yields and purities.      

A comparison of the FAST,Premi® and KIS™ tests for screening antibiotic residues in beef kidney juice and serum

Three microbial inhibition-based screening methods, the fast antimicrobial screening test (FAST), the Premi test, and the kidney inhibition swab (KIS) test, were evaluated using penicillin G, sulfadimethoxine, oxytetracyline, tylosin, danofloxacin, streptomycin, neomycin, and spectinomycin at a range of fortified concentrations in beef kidney juice and beef serum. Each antibiotic was individually tested simultaneously using the different assays in replicate experiments. Detection threshold concentrations for each analyte in each screening assay were determined for the different matrices. Each assay gave a different detectability profile for the different antibiotics, with the largest differences related to neomycin, which was more sensitively detected by the FAST, and penicillin G, which was detected at lower levels by the Premi and KIS tests. In addition to practical considerations, analysts can use the information presented in this study to evaluate each kit for applicability to their monitoring needs.     

Thermal stability and decomposition of nafion® membranes with different cations

The thermal decomposition of Nafion has been studied by means of high-resolution and constant heating rate thermogravimetry (TG), under nitrogen and synthetic air atmospheres. Nafion membranes have been studied in acid and salt (alkali chlorides) forms. The TG curves of Nafion with alkali countercations show similar profiles, whichever the atmosphere employed. The kinetics of thermal decomposition of the Nafion-Cs⁺ has also been studied. The method employed to calculate the kinetic parameters and to estimate the polymer lifetime from the data was based on Kissinger's method. This revised version was published online in August 2006 with corrections to the Cover Date.     

Preparation,characterization and electrochemical properties of Nafion® doped poly(ortho-anisidine) Langmuir–Schaefer films

Langmuir–Schaefer (LS) films of poly(ortho-anisidine) (POAS) were fabricated by utilizing water and water acidified HCl as subphases, respectively. The uniformity of the films formation and the doping with Nafion were verified by UV–Vis spectroscopy. The morphology and the thickness of the POAS, HCl post-doping POAS and Nafion post-doping POAS LS films were investigated using atomic force microscopy. The electrochemical properties of POAS LS films, HCl post-doping POAS and Nafion post-doping POAS were investigated and compared with our previously published work. The electrochemical switching time of HCl post-doping POAS and Nafion post-doping POAS LS films were also estimated.     

Transfer Hydrogenation of Nitriles with 2-Propanol and Raney® Nickel

Abstract

Raney nickel in refluxing 2-propanol containing 2% KOH is an effective catalytic system for reducing nitriles to amines.