Novel colorimetric method overcoming phosphorus interference during trace arsenic analysis in soil solution

A sensitive (method detection limit, 2.0 microg As L(-1)) colorimetric determination of trace As(v) and As(iii) concentrations in the presence of soluble phosphorus (P) concentrations in soil/water extracts is presented. The proposed method modifies the malachite green method (MG) originally developed for P in soil and water. Our method relies upon the finding that As(iii) and As(v) do not develop the green color during P analysis using the MG method. When an optimum concentration of ascorbic acid (AA) is added to a sample containing up to 15 times P > As (microM) concentrations, the final sample absorbance due to P will be equal to that of As(v) molecules. The soluble As concentration can then be quantified by the concentration difference between the mixed oxyanion (As + P) absorbance (proposed method) and the MG method absorbance that measures only P. Our method is miniaturized using a 96-well microplate UV-VIS reader that utilizes minute reagent and sample volumes (120 and 200 microL sample(-1), respectively), thus, minimizing waste and offering flexibility in the field. Our method was tested in a suite of As-contaminated soils that successfully measured both As and P in soil water extracts and total digests. Mean% As recoveries ranged between 84 and 117%, corroborating data obtained with high-resolution inductively-coupled plasma mass-spectrometry. The performance of the proposed colorimetric As method was unaffected by the presence of Cu, Zn, Pb, Ni, Fe, Al, Si, and Cr in both neutral and highly-acidic (ca. pH 2) soil extracts. Data from this study provide the proof of concept towards creating a field-deployable, portable As kit.     

Studies of cyclohexane/TX 100 + ethylpropionate/water system: effect of ethylpropionate as cosurfactant

 Pseudoternary phase diagram of cyclohexane/TX 100-ethylpropionate/water system was determined at 30 ^°C. One phase microemulsion was obtained over a small area. The surfactant/cosurfactant ratio was both kept at 1:1 and 1:2 w/w. Viscosity, conductance, adiabatic compressibility values at various temperatures show the expected trend. The addition of NaCl changes one phase microemulsion to Winsor II system and no Winsor III system was obtained. Contact angle data, conductance, etc., show oil continuous system at a constant surfactant weight fraction. The microstructure of Winsor IV microemulsion seems to be W/O. Received: 14 May 1996 Accepted: 23 October 1996     

Studies of adsorption of polyacrylonitrile and polyacrylates at solid-liquid interface

The adsorption of poly(acrylonitrile), poly(methyl acrylate), poly(ethyl acrylate) and poly(butyl acrylate) was studied at different temperatures fromN,N-dimethyl formamide solution on various solid surfaces, i.e. silica gel, alumina and calcium carbonate. The thermodynamic quantities for adsorption processes were computed by using a) infinite dilution and b) surface coverage approaches. Both procedures tend to give similar conclusions. These reveal the importance of polymer-adsorbent interactions besides many other properties including solvent power.     

Development of a Liquid‐liquid Extraction System for Rhodium(III) by 2‐octylaminopyridine from Weak Malonate Media

We have developed the extraction method of rhodium(III) from malonate media with 2‐octylaminopyridine (2‐OAP) in xylene at pH 8.0. The quantitative extraction of rhodium(III) with extractant was found by screening of different physicochemical parameters like malonate concentration, extractant concentration, pH, diluents, effect of temperature, aq: org phase ratio, loading capacity of 2‐OAP. The optimum condition was malonate=0.025 M, pH=8.0, 2‐OAP=0.05 M in xylene. The complete stripping of rhodium(III) from the loaded organic phase was carried out with 2 M HCl. Log‐log plot was investigated to determine the stoichiometry of the extracted species and it was found to be 1 : 2 : 1 (metal : acid :extractant). The versatility of the proposed method was checked for extraction and separation of rhodium(III) from binary, ternary mixture of associated metal ions as well as platinum group metals and from the synthetic solution of rhodium minerals and alloys.     

Structure and Dynamic of Three Indole Alkaloids from the Campylospermum Genus (Ochnaceae)

A new indole alkaloid, calanthumindole ( 4 ), and three known biflavonoids, amentoflavone, sequoiaflavone, and podoscarpusflavone B, were isolated from Campylospermum calanthum (Ochnaceae). Calanthumindole is a new indole alkaloid of the serotobenine family characterized by the presence of a C?C bond between atoms C(7′) and C(8′) of the furan ring. This is the first compound to have a fully unsaturated furan ring among the members of this family. The combination of NMR and DFT allowed the determination and comparison of the 3D structures and relevant conformational characteristics of serotobenine ( 1 ), flavumindole ( 2 ), and calanthumindole ( 4 ).     

A method for estimation of Pu-isotopes in urine samples using TEVA resin and alpha spectrometry

The conventional method used for estimation of Pu-isotopes in urine samples involves anion exchange resin followed by alpha spectrometry, which takes nearly one working week for complete sample analysis. Since the results of the analysis form an important input for decision making by the plant authorities, it is always preferable to reduce overall analysis time for the estimation of Pu-isotopes in bioassay samples. This paper deals with standardization of a relatively faster method for estimation of Pu-isotopes in bioassay samples using TEVA resin and ²³⁶Pu tracer for radiochemical recovery. The method involves oxidation of urine followed by co-precipitation of plutonium along with calcium phosphate and separation of Pu was carried out using TEVA resin. Pu-fraction was electrodeposited and activity estimated using tracer recovery by alpha spectrometer. Routine urine samples of radiation workers were analyzed and consistent radiochemical tracer recovery was obtained in the range 65–87 % with a mean and SD of 75 and 7.4 %, respectively. The standardized chromatographic technique reduces the analysis time by about 1 day as compared to conventional method for estimation of Pu-isotopes in urine samples.     

Polypyrrole–polyvinyl alcohol stable nanodispersion: A prospective conducting black ink

Chemical polymerization of pyrrole within aqueous polyvinyl alcohol (PVA) solution gives rise to a nanodispersion with unique stability and monodispersity. The nanodispersion has shown uniform distribution of perfectly spherical ～110 nm polypyrrole particles (from transmission electron microscopy and dynamic light scattering) with high doping level (from UV‐Vis analysis) and sufficient electrical conductivity (10^?3 S/cm). The dispersion with optimum stability and conductivity was subjected to viscoelastic studies. The viscosity of the system was adjusted by dilution with water and shear thinning (under steady shear) was generally observed. Dynamic mechanical studies have shown that the dispersion behaves like a semidiluted polymeric solution that roughly follows the Zimm model of viscoelasticity. This behavior accounts for its unique stability and miscibility with water at any proportion without precipitation. On drying or leaving the sample for 7 days, Fe³⁺ induced partial crosslinking of PVA chains takes place via –OH groups, although complete gelling does not occur. The dispersion forms flexible and uniform films on glass and metal surfaces that does not dissolve after complete drying; this observation combined with shear thinning encourages its application as ink or paint. © 2011 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys, 2011