Oxygen incorporation in polyethylene implanted with 150 keV Sb+ ions

Samples of polyethylene (PE) loaded with carbon black up to 8 wt.% and implanted with 150 keV Sb⁺ ions to the doses from 2×10¹³–2×10¹⁵ cm^–2 were studied using standard Rutherford Back Scattering (RBS) technique. On the PE samples implanted to the doses above 2×10¹⁴ cm^–2, a considerable surface carbonization is observed. The measured parameters of the Sb depth profile are compared with theoretical TRIM estimations. The projected range is by 25% lower than the theoretical one and the range straggling is about twice of that predicted. The differences are explained by stepwise polymer degradation during the ion bombardment. Strong oxidation of the ion implanted polymers is also observed. The oxygen depth profiles from the sample surface up to the depth comparable with Sb⁺ ion range evolve from nearly uniform one for low ion doses to highly non-uniform one for doses above 1×10¹⁵ cm^–2. The total oxygen content in the sample surface layer 300 nm thick reaches a maximum for the doses of (1–2)×10¹⁴ cm^–2.On leave from Belorussian State University, 220050 Minsk, Belarus.The authors thank the member of electrostatic accelerator group at INP for help during RBS measurements. The work was partly (V.H. and J.K.) supported by the Internal Grant Agency of the Academy of Sciences of Czech Republic under the grant No. 14805 and by the Internal Grant Agency of the Ministry of Education of Czech Republic under the grant No. 1002 (V.., V.R., V.H. and J.K.). In the final stage, the work was also supported by the Grant Agency of Czech Republic under the grant No. 202/93/0121.     

Coordination compounds of nickel with trithiocyanuric acid. Part IV. Structure of [Ni(pmdien)(ttcH)] (pmdien = N,N,N′,N′,N′′-pentamethyldiethylenetriamine,ttcH3 = trithiocyanuric acid)

Ni^II mixed-ligand complexes of compositions [Ni(pmdien)(ttcH)] (1), [Ni(baphen)₂(ttcH)] · 4H₂O (2), [Ni-(dpa)(ttcH)(H₂O)] (3), [Ni(cyclam)(ttcH)] · 2H₂O (4), [Ni(hexaa)](ttcH) (5) and [Ni(hexab)(ttcH)] · 2H₂O (6), (baphen = 4,7-diphenyl-1,10-phenanthroline, dpa = 2,2-dipyridylamine, cyclam = 1,4,8,11-tetraazacyclotetradecane, hexaa = 1,3,6,9,11,14-hexaazatricyclo[12.2.1.1^6,9]-octadecane, hexab = 1,8-dimethyl-1,3,6,8,10,13-hexaazacyclotetradecane) have been prepared and characterized by means of i.r., u.v.–vis. spectroscopies and magnetochemical measurements. The redox properties of the complexes were studied by cyclic voltammetry. The crystal and molecular structure of [Ni(pmdien)(ttcH)] was determined. The nickel atom is penta-coordinated by three N atoms of pmdien, and by S and N atoms of trithiocyanurate(2–) anion.     

Xanthate complexes of nickel with nitrogen donor ligands. Part V

Nickel(II) xanthate complexes of general formula, [Ni(Rxa)₂(L)] [R = i-Pr, i-Am, xa = OCS^– ₂, L = 4,7-diphenyl-1,10-phenanthroline(baphen), 4,4-dimethyl-2,2-bipyridyl (me₂bpy), 2-9-dimethyl-1,10-phenanthroline(neo) or trans-1,2-diaminocyclohexane (dch)] and [Ni(Rxa)(cyclam)](Rxa) (= 1,4,8,11-tetraazacyclotetradecane) have been synthesized and characterized by elemental analyses, i.r. and electronic spectroscopy, magnetic and conductivity measurements. The complexes with cyclam were studied by cyclic voltammetry. Values of magnetic moments at room temperature lie within the 3.25–3.51 B.M. range and thus indicate the presence of two unpaired electrons, except for the complexes with cyclam, where the anomalous values of 1.76 and 1.74 B.M. were obtained in respect to the nickel(II) complexes. Magnetic susceptibility data for [Ni(i-Prxa)(cyclam)](i-Prxa) were measured over the 79–298 K range and indicate no exchange interaction between paramagnetic nickel(II) centres.     

Properties of two amide‐based hydrophilic interaction liquid chromatography columns

Hydrophilic interaction liquid chromatography is a separation technique suitable for the separation of moderately and highly polar compounds. Various stationary phases (SPs) for hydrophilic interaction liquid chromatography are commercially available. While the SPs based on the same type of ligand are available from different providers, they can display a distinct retention characteristics and separation selectivity. The current work is focused on characterization and comparison of the separation systems of two amide‐based HPLC columns from two producers, i.e. XBridge Amide column and TSK gel Amide‐80 column. Several characterization procedures (tests) were used to investigate the differences between these columns. The chromatographic behavior of selected analytes indicates that multimodal interactions are responsible for retention and separation on these columns. Multiple testing approaches were used in order to reveal subtle differences between the SPs. Both amide‐based columns showed certain differences in retention, selectivity, and plate counts. Based on the tests used in this study, we conclude that the investigated columns provide a different degree of H‐bonding interactions.     

HPLC Method for Chiral Separation and Quantification of Antidepressant Citalopram and Its Precursor Citadiol

HPLC method enabling chiral separation and determination of citalopram (CIT), a widely used antidepressant, and its synthetic precursor citadiol in one analysis was developed and validated. Moreover, supercritical fluid chromatography was also tested and was proved to be less effective for this separation purpose. The optimized HPLC system was composed of Chiralcel OD-H column and n-hexane/propane-2-ol/triethylamine 96/4/0.1 (v/v/v) as mobile phase, column temperature 25 °C, flow rate 1.0 mL min^?1, UV detection at 250 nm. The effects of amount of propane-2-ol, triethylamine addition, and temperature on enantioselectivity and resolution of the enantiomers were evaluated. The method was found to be suitable for determination of the enantiomeric purity of CIT in bulk drugs. Enantiomers of CIT were determined in two commercially available pharmaceuticals.     

Vapor pressure of selected aliphatic alcohols by ebulliometry. Part 2

Vapor pressures of six pentanols, 2-methyl-1-butanol (CAS Registry Number 137-32-6), 2-methyl-2-butanol (CAS Registry Number 75-85-4), 3-methyl-1-butanol (CAS Registry Number 123-51-3), 3-methyl-2-butanol (CAS Registry Number 598-75-4), 2-pentanol (CAS Registry Number 6032-29-7) and 3-pentanol (CAS Registry Number 584-02-1), were measured by the precision ebulliometry over an approximate pressure range from 9 to 99 kPa. The absolute uncertainties in pressure and temperature are estimated to be less than or equal to 7 Pa and 0.02 K, respectively. The results are represented by the Antoine equation and compared with available literature data.     

Single‐Crystal‐to‐Single‐Crystal Transition in an Enantiopure [7]Helquat Salt: The First Observation of a Reversible Phase Transition in a Helicene‐Like Compound

Here it is reported that crystals of an enantiopure [7]helquat salt undergo reversible thermal solid–solid phase transition at 404 K. Differential scanning calorimetry (DSC), capillary electrophoresis (CE), and X‐ray diffraction analysis were used to unravel the mechanistic details of this process. The single‐crystal‐to‐single‐crystal course enabled direct monitoring of the structural changes by in situ variable‐temperature X‐ray diffraction, thus providing the first direct evidence of a solid phase transition in a helicene‐like compound.     

Runge–Kutta Lawson schemes for stochastic differential equations

In this paper, we present a framework to construct general stochastic Runge–Kutta Lawson schemes. We prove that the schemes inherit the consistency and convergence properties of the underlying Runge–Kutta scheme, and confirm this in some numerical experiments. We also investigate the stability properties of the methods and show for some examples, that the new schemes have improved stability properties compared to the underlying schemes.