Oxidations with alkaline permanganate using monovalent thallium for the back-titration: Determination of iodate,iodide and ferrocyanide

Iodate, iodide, iodine and ferrocyanide can be estimated by oxidation with KmnO₄ in alkaline media; the excess is back-titrated with TI⁷. I^- and I₂ are oxidized to IO₄^- in the presence of Ba⁺² ions but only to IO₃^- in absence of such ions. The direct titration of IO₃^-, I^- with KmnO₄ proved valueless.Ferrocyanide is oxidized by KmnO₄ in alkaline solutions and MnO₂ is formed. In the presence of telluric acid and 0.025–0.1 N NaOH satisfactory results are obtained. Reduction of MnO₄^- with ferrocyanide gives MnO₄^-2 and the results are variable, depending on the rate of adding the ferrocyanide.     

Capillary gas chromatographic analysis of pyrrolidinedithiocarbamate metal chelates

Pyrrolidinedithiocarbamate (PDTC) chelates of Zn(II), Cu(II), Ni(II), Co(III), Fe(III), Mn(II), Cr(III), and VO(II) were analysed by capillary GC on a DB-1701 column (30 m x 0.25 mm id) with flame ionisation detection (FID). Linear calibrations were attained within "1-30 microg/mL" for Ni(II), Fe(III), Mn(II), Cr(III), Cu(II), and VO(II), and within "2-50 microg/mL" for Co(III) and Zn(II). The limits of detection were in the "150-500 ng/mL" range, corresponding to 15-50 pg amounts reaching the FID system. The optimised method was applied to the determination of Cu(II) and Ni(II) in coins, and that of Zn(II), Cu(II), Ni(II), Fe(III), Mn(II), Cr(III), and VO(II) in pharmaceutical preparations with relative standard deviations within 1.1-5.2%. The results obtained are in good agreement with sewage water samples and the declared values for the pharmaceutical formulations, or with the results of AAS of metal contents in coins, pharmaceutical preparations, and sewage water samples.     

Incorporation of ferrocene into polypyrrole films via an ionic adduct with boron trifluoride

1-(Ferrocenyl)ethanol has been immobilized within polypyrrole films during their electrochemical deposition, or following their deposition, via its adduct with boron trifluoride. Dissociation of H⁺ from this adduct, formed in a solution of boron trifluoride diethyl ether (BFEE) in acetonitrile, produces an anion that can act as a counterion for oxidized polypyrrole. Its subsequent hydrolysis produces a polypyrrole film containing neutral 1-(ferrocenyl)ethanol which was found to be strongly retained. In addition to producing a novel type of polypyrrole–ferrocene composite, this work provides clear evidence to support the efficacy of this methodology for the incorporation of neutral species within conducting polymer films.     

N‐(Ferrocenecarbonyl)‐N′‐(quinolin‐8‐yl)thio­urea

In the title compound, [Fe(C₅H₅)(C₁₆H₁₂N₃OS)], the 8‐am­inoquinoline and acyl­thio­urea moieties are almost planar. There are two perpendicular arrangements of the mol­ecules in the crystal with slightly different conformations. The two cyclo­penta­dienyl rings in each mol­ecule are parallel and eclipsed.     

Indirect potentiometric titration of sulphamethoxazole in the presence of trimethoprim in co-trimazole tablets using copper based mercury film electrode

A simple and rapid indirect potentiometric titration of sulphamethoxazole in the presence of trimethoprim contained in co-trimazole tablets is described. The method is based on the formation of a complex of sulphamethoxazole with a known excess of silver ions and the titration of unreacted silver ion potentiometrically using an inexpensive lab-made copper based mercury film electrode (CBMFE). The titration conditions have been optimized for the determination of 1.0-10.0 mg of sulphamethoxazole in pure and dosage forms. The precision and accuracy of the method have been assessed by the application of lack of fit test and other statistical methods. Overall mean recovery and relative standard deviations obtained were 99.88% and 1.32% (n=7) respectively. No interference was caused by other excipients present in pharmaceutical dosage forms. The application of this method for sulphamethoxazole assay in the presence of trimethoprim in tablets was validated by the comparison of results obtained by the proposed method with that of the British Pharmacopoeia (BP) method using F- and t-statistical tests of significance.     

Electrical and electrochemical characteristics of La<Subscript>0.6</Subscript>Sr<Subscript>0.4</Subscript>CoO<Subscript>3-δ</Subscript> cathode materials synthesized by a modified citrate-EDTA sol-gel method assisted with activated carbon for proton-conducting solid oxide fuel cell application

The electrical conductivity and electrochemical performance of a La_0.6Sr_0.4CoO_3-δ (LSC) cathode produced by a modified citrate-EDTA sol-gel method assisted with activated carbon are characterized for a proton-conducting solid oxide fuel cell (H⁺??SOFC) application at intermediate temperature. Thermogravimetric analysis revealed that the decomposition of the unrequired intermediate compounds in the precalcined powder was completed at 800?°C. A single LSC perovskite phase was formed at a calcination temperature of 900?°C, as confirmed by X-ray diffraction analysis. The particle size, crystallite size, and BET-specific surface area of the powder are 219–221?nm, 18?nm, and 9.87?m²?g^?1, respectively. The high index value of the extent of agglomeration (5.53) showed that the powder was barely agglomerated. Bulk LSC sintered at 1200?°C for 2?h showed the highest direct-current electrical conductivity (σ_d.c) compared to that of bulk LSC sintered at 1000?°C and 1100?°C. The value of σ_d.c was affected by the density and porosity of the sintered samples. The area specific resistance (ASR) of screen-printed LSC working on a proton conductor of BaCe_0.54Zr_0.36Y_0.1O_2.95 (BCZY) decreased from 5.0?Ω?cm²–0.06?Ω?cm² as the temperature increased from 500?°C to 800?°C with an activation energy of 1.079?eV. Overall, in this work, the LSC material produced with the aid of activated carbon meet the requirements for the application as a cathode in an intermediate temperature H⁺-SOFC.

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Dispersion of polymeric-coated–silica aerogel particles in unsaturated polyester composites: Effects on thermal-mechanical properties

The thermal-mechanical properties of unsaturated polyester (UP) composite were enhanced by the dispersion of silica aerogel (SA) with preserved pores. Low-cost SA was prepared from rice husk via the sol-gel process and ambient pressure drying. A new method was proposed to encapsulate the hydrophobic aerogel surface pores with hydrophilic polyvinyl alcohol (PVA) film using the fluidized-bed coating process. The dispersion of PVA-coated aerogel with preserved pores in the polyester matrix resulted in an increase of specific compressive strength (44.1?MPa?·?cm³?g^?1), thermal insulation (0.23?W?m^?1?K^?1), and thermal stability (T_onset?=?310°C), but decreased the glass transition temperature (T_g?=?260°C).     

Human Health Risk Surveillance Through the Determination of Organochlorine Pesticides by High-Performance Liquid Chromatography in Water,Sediments, and Fish from the Chenab River,Pakistan

The current study assessed the spatiotemporal variations and human health surveillance associated with organochlorine pesticide (OCP) contamination in water, sediments, and fish from Chenab River, Pakistan. The OCP determinations were performed using high-performance liquid chromatography with a reverse-phase C18 column. The total OCP levels ranged from 13.33 to 274.59?ng/L in water, 4.63 to 239.11?ng/g in sediments, and 23.79 to 387.12?ng/g in fish species. The overall pattern of mean OCP concentrations followed the order as ΣDDTs?>?Σendosulfan?>?aldrin and OCP pollution pattern among the headworks were Khanki Barrage?>?Qadirabad Barrage?>?Trimmu Barrage?>?Marala Barrage in all three environmental matrixes during both seasons. The estimated daily intake (EDI) for ∑OCPs was found to be 22.44?ng/kg/day. The hazard ratios calculated to assess the carcinogenic risk indicated that the values for ∑DDT and aldrin at the 95th percentile concentrations were greater than one, indicating the probability of carcinogenic risk occurrence of one in million populations due to fish consumption. Therefore, these high levels of OCPs and carcinogenic risk through fish consumption highlight the needs of immediate elimination of OCPs from riverine environment of Chenab River and we recommend long-term monitoring-based freshwater ecological studies to be conducted in the study area.     

O‐Ethyl and O‐methyl N‐(2,3,4,6‐tetra‐O‐acetyl‐β‐d‐glucopyranosyl)thiocarbamate

In both the title structures, O‐ethyl N‐(2,3,4,6‐tetra‐O‐acetyl‐β‐d ‐gluco­pyran­osyl)­thio­carbam­ate, C₁₇H₂₅NO₁₀S, and O‐methyl N‐(2,3,4,6‐tetra‐O‐acetyl‐β‐d ‐gluco­pyran­osyl)­thiocar­bam­ate, C₁₆H₂₃NO₁₀S, the hexo­pyran­osyl ring adopts the ⁴C₁ conformation. All the ring substituents are in equatorial positions. The acetoxy­methyl group is in a gauche–gauche conformation. The S atom is in a synperi­planar conformation, while the C—N—C—O linkage is antiperiplanar. N—H?O intermolecular hydrogen bonds link the mol­ecules into infinite chains and these are connected by C—H?O interactions.     

Bis­(O,O′‐di‐p‐tolyldithiophosphato‐S,S′)(1,10‐phenanthroline‐N,N′)nickel(II)

The title coordination complex, [Ni(C₁₄H₁₄O₂PS₂)₂(C₁₂H₈N₂)] or [Ni(pMePh‐dtp)₂(phen)] (phen is 1,10‐phenanthroline; dtp is di­aryl­di­thio­phosphate), has a non‐crystallographic twofold axis of symmetry through the Ni atom and the phen moiety. Two O,O‐di‐p‐tolyl­di­thio­phosphate (dtp) ions act as bidentate ligands. The central metal atom is coordinated by four S atoms from two dtp groups and two N atoms from the phen ligand. The title compound displays distorted octahedral geometry around the central Ni atom.