Synthesis,characterization and monitoring of trans-[Ru{P(OMe)3}4Cl2] by reversed-phase high-performance liquid chromatography and 31P-n.m.r.

P(OMe₃)₃ reacts with RuCl₃ · 3H₂O to produce the complex trans-[Ru{P(OMe)₃}₄Cl₂] from which the complexes trans-[Ru{P(OMe)₃}₄S₂]²⁺ and cis-[Ru{P(OMe)₃}₂S₄]²⁺ (S = Solvent) can be prepared by solvation in neutral and acidic solution, respectively. The aquation takes place with a specific rate of 1.0 × 10^–2 min^–1 (pH = 3.0) and 5.4 × 10^–3 min^–1 (pH 7.0) The trans-[Ru{P(OMe)₃}₄Cl₂] complex has been characterized by elemental analysis; electronic spectra [_max = 408 nm] ( = 1.7 × 10² M^–1 cm^–1), _max = 250 nm ( = 3.5 × 10³ M^–1 cm^–1) and a shoulder at = 280 nm ( 8.3 × 10² M^–1 cm^–1)]; cyclic voltametry ( = 0.75 V versus s.c.e.); HPLC (t _R = 5.7 min); and ³¹P-n.m.r. ( = 131 p.p.m.). In acidic solutions the ³¹P-n.m.r. variations point to a reaction intermediate, characterized as the complex ion trans-[Ru{P(OMe)₃}₄S₂]²⁺ ( = 136 p.p.m.) followed by the formation of the proposed product, cis-[Ru{P(OMe)₃}₂S₄]²⁺ ( = 145 p.p.m.). For this same complex, at pH = 7.0, the results show the formation of the trans-[Ru{P(OMe)₃}₄S₂]²⁺ ( = 136 p.p.m.). The HPLC results for the trans-[Ru{P(OMe)₃}₄Cl₂] complex show that the different species are present at different pH values. In acidic media a less polar species (t _R = 4.3 min) compared with the starting material (t _R = 5.7 min) was formed. At neutral pH (t _R = 4.6 min) the species generated were not modified, however they exhibited different properties from the species obtained at a lower pH.     

ASBR Applied to the Treatment of Biodiesel Production Effluent: Effect of Organic Load and Fill Time on Performance and Methane Production

The effect of organic matter and fill time on anaerobic sequencing batch reactor (5 L, 30°C, 8-h cycles, 50 rpm) efficiency has been analyzed. Organic matter was increased by the influent concentration. Fill times investigated were in the batch mode and fed-batch followed by batch. In the batch mode organic matter removal were 93%, 81%, and 66% for influent concentration of 500, 1,000, and 2,000 mgCOD/L (0.6, 1.29, and 2.44 gCOD/L.d), respectively. At 3,000 mgCOD/L (3.82 gCOD/L.d) operational stability could not be achieved. Removal efficiency was improved by increasing the fill time, and was 85% for the 1,000 mgCOD/L condition and fill times of 2 and 4 h, and 80 and 77% for the 2,000 mgCOD/L condition and fill times of 2 and 4 h, respectively. Hence, gradual feeding seemed to improve and to smooth the profiles of organic matter and volatile acids along the cycle with 78 to 96 NmLCH₄/gCOD.     

An Electrochemical DNA Biosensor for the Detection of the Apa I Polymorphism in the Vitamin D Receptor Gene Using Meldola's Blue as a Hybridization Indicator

Electrochemical detection of nucleic acid base mismatches related to Apa I single nucleotide polymorphism (SNP) in the vitamin D receptor gene was performed successfully using 7‐dimethyl‐amino‐1,2‐benzophenoxazinium salt (Meldola's blue, MDB) with 10.9 pmol/100 μL of detection limit. MDB reduction signals obtained from probe, mismatch(probe‐SNP containing target) and hybrid(probe‐target) modified pencil graphite electrode(PGE) increased respectively. The sensor was able to clearly distinguish perfect match from mismatch DNA in a 30 min. detection time. Several factors affecting on the hybridization and indicator response are studied to maximize sensitivity and selectivity. The advantages of the biosensor are discussed in comparison with previous electrochemical assays for DNA hybridization.     

Purification and Characterization of Paraoxonase 1 (PON1) from Swiss Black,Holstein, and Montofon Bovines

Paraoxonase 1 (PON1: EC 3.1.8.1) is a calcium-dependent enzyme associated with high-density lipoproteins (HDLs) and has a protective effect against oxidation of low-density lipoproteins (LDLs) in mammals. PON1 is the best-studied member of a family of enzymes called serum paraoxonases, or PONs, identified in mammals and other vertebrates as well as in invertebrates. PONs exhibit a range of important activities, including drug metabolism and detoxification of organophosphates such as nerve agents. This study reports, for the first time, purification and biochemical characterization of serum PON1 from different bovine breeds namely Swiss Black, Holstein, and Montofon. Bovine serum PON1s were purified using ammonium sulfate precipitation followed by Sepharose-4B-l-tyrosine-1-naphthylamine hydrophobic interaction chromatography. SDS–polyacrylamide gel electrophoresis of the purified enzymes indicates a single band with an apparent MW of 43 kDa. The purified enzymes had a specific activity of 10.78, 27.00, and 22.38 U/mg for Swiss Black, Holstein, and Montofon bovines, respectively. The overall purification rates of our method were 262.47-, 2,476.90-, and 538.06-fold for Swiss Black, Holstein, and Montofon bovines, respectively. Furthermore, using phenyl acetate as a substrate, we determined the K _M and V _max values of the purified enzymes, as 0.80 mM, 1428.5 U/ml for Swiss Black; 0.40 mM, 714.3 U/ml for Holstein; and 0.50 mM, 1,111.1 U/ml for Montofon bovine. The present study has revealed that there is no substantial difference in PON1 activities among the studied bovine breeds.     

Analysis and Review of Chemical Reactions and Transport Processes in Pulsed Electrical Discharge Plasma Formed Directly in Liquid Water

Electrical discharges formed directly in liquid water include three general cases where (a) streamer-like plasma channels form in, but do not span, the electrode gap, (b) spark discharges produce transient plasma channels that span the electrode gap, and (c) arc discharges form plasma channels with relatively longer life times. Other factors including the input energy (from <1?J/pulse to >1?kJ/pulse) as well as solution properties and the rates of energy delivery affect the nature of the discharge channels. An understanding of the formation of chemical species, including the highly reactive hydroxyl radical and more stable molecular species such as hydrogen and hydrogen peroxide, in such plasma requires determination of temporal and spatial variations of temperature, pressure, plasma volume, and electrical characteristics including current, voltage (electric field), and plasma conductivity. In spark and arc discharges analysis of the physical processes has focused on hydrodynamic and thermal characterization, while only a limited amount of work has connected these physical processes to chemical reactions. On the other hand, the most successful model of the chemical reactions in streamer-like discharges relies on simple assumptions concerning the temperature and pressure in the plasma channels, while analysis of the physical processes is more limited. This paper reviews the literature on the mathematical modeling of electrical discharges in liquid water spanning the range from streamer-like to spark and arc discharges, and compares the properties and processes in these electrical discharges to those in electron beam radiolysis and ultrasound.     

Thermo-oxidative evaluation of new cardol derivatives as antioxidants for mineral oils

In this study, the thermo-oxidative stability of two new phosphorylated derivatives of cardol, a compound from the cashew (Anacardium occidentale L.) industry waste CNSL (cashew nutshell liquid), were evaluated. The antioxidant capacity of these new molecules upon two mineral oils, NH10 and NH20 were also studied by thermogravimetric analysis (TG/DTG), observing the onset and offset temperatures variation. The results showed that both MP and DP Cardol increased considerably the onset and offset temperatures of NH10 and NH20 oils.     

Comparative Methodology for Isolation of Flavonoid Glycosides from Clusia criuva Cambess

The family Guttiferae belongs to the superorder Theiflorae, order Theales and according to Dahlgren's system of classification, it is equivalent to Hypericaceae (=Clusiaceae) [1]. This family consists of 49 genera encompassing over 1000 species of wide distribution in the tropics as shrubs and trees [2]. Plants of the genus Clusia have been used in folk medicine for the treatment of different kind of illness such as: febrifuge, anti rheumatic, purgative, for stomach problems and, in Brazil, they are very commonly used to heal wounds [3]. The key of any study of material from natural sources is the availability of suitable separation methods for the isolation of pure products [4–6]. Tentatives for separations using chomatography on solid support phases were not very efficients in the fractionation of Clusia criuva Cambess methanolic/ethyl acetate extracts. However, the use of counter-current chromatography, an all liquid technique, showed advantages in comparison with the more traditional liquid-solid separation methods and even with HPLC. In this sense it was possible to isolate flavonoid glycosides from ethyl acetate extract of Clusia criuva, in a very short operation time.     

Some difference sequence spaces defined by a sequence of <Emphasis Type="Italic">ϕ</Emphasis> -functions

Abstract  In this paper, we introduce new difference sequence spaces combining with de la Vallee-Poussin mean using by a sequence of modulus functions and ϕ -functions. We also studied connections between statistically convergence related with this space. Keywords Difference sequence, Modulus function, ϕ -function, De la Vallee-Poussin means, Statistical convergence Mathematics Subject Classification (2000) 46A45, 40F05, 46A80     

Synthesis and characterization of two new bulky tris(mercaptoimidazolyl)borate ligands and their zinc and cadmium complexes

The sodium salts of the tris(2-mercapto-1-benzylimidazolyl)borate [Tm^Bz]⁻ and tris(2-mercapto-1-p-tolylimidazolyl)borate [Tm^p-Tol]⁻ anions have been readily prepared in very good yield from NaBH₄ and 2-mercapto-1-benzylimidazole or 2-mercapto-1-p-tolylimidazole, respectively. These new monoanionic tripodal sulfur-donor ligands have been used to prepare the Group 12 derivatives (Tm^R)MBr (M=Zn, Cd; R=Bz, p-Tol), all of which have been characterized by a combination of analytical and spectroscopic techniques, including electrospray ionization mass spectrometry (ESI MS) and, in the case of both benzyl-substituted derivatives, single-crystal X-ray diffraction.     

Synthesis and characterization of Mn:CdS nanoflower thin films prepared by hydrothermal method for photocatalytic activity

Journal of Sol-Gel Science and Technology - Mn-CdS nanoflowers were successfully deposited using hydrothermal technique at 150 °C for 2 h. The effect of changing the dopant...