A simple oxidation procedure for biological material prior to analysis for mercury

The stability constants of aluminium(III), gallium(III), indium(III) and scandium(III) with 8-hydroxyquinoline and its 2-methyl derivative have been determined by potentiometric titration, with computation by the SCOGS program. In contrast to previous work, the results show that protonated species occur in several of the equilibria. The constants are discussed in terms of the nature of metal-to-ligand bonding in the complexes. X-ray photoelectron spectroscopy of the ligand coordinating atoms in the solid complexes confirms the significantly increased covalency of the gallium—oxygen bond compared to the same bond in the aluminium complex.     

A simple and efficient procedure for the synthesis of benzimidazoles using air as the oxidant

Direct one-step synthesis of various benzimidazoles from phenylenediamines and aldehydes is described using air as the oxidant. The salient features of this method include a simple procedure, mild conditions, no coupling agents or commercial oxidants/additives used, no waste produced (only by-product being water), easy purification, and high generality.     

A new approach to isoindoloisoquinolinones. A simple synthesis of nuevamine

A convenient and versatile short step synthesis of isoindoloisoquinolinones, illustrated by the total synthesis of the alkaloid nuevamine 1a, is described. The tetracyclic lactam compounds were obtained by a tactical combination of the Parham procedure for the elaboration of the isoindolinone template and an aryne-mediated cyclization giving rise to the nitrogen containing six-membered heteroring unit.     

A rapid and simple microwave-assisted digestion procedure for spectrophotometric determination of titanium dioxide photocatalyst on activated carbon

Deposition of titanium dioxide (TiO₂) on activated carbon (AC) surface has been widely utilized for the production of TiO₂/AC photocatalyst, which can be used in photo-degradation of pollutants. In this work, a fast and simple digestion procedure has been developed for the spectrophotometric quantitative analysis of TiO₂ in TiO₂/AC photocatalyst. Microwave-assisted digestion was used in the procedure. The microwave-digestion procedure was optimized using the single-variable method. Variables optimized included time of ashing, effective digestion time, volume and concentration of sulfuric acid, effect of adding a digestion catalyst, effect of sample pulverizing and on–off time cycle of the microwave. The analysis was completed spectrophotometrically after addition of hydrogen peroxide to the digested solution. Procedure precision and accuracy was tested by application to photocatalyst samples containing known amounts of TiO₂, and compared with previously published spectrophotometric procedures. The proposed microwave procedure was capable of recovering 98.4–101.1% of TiO₂ in the catalyst in less than 10 min, without the need for sample ashing. Analytical precision is 1.42–2.39% relative standard deviation (R.S.D.). In terms of accuracy and precision, the proposed microwave procedure was comparable with other procedures, but the proposed microwave procedure was superior in terms of shorter procedure duration.     

Mathematical aspects of the LCAO MO first order density function (3): A general localization procedure

A general MO localization process based on Elementary Jacobi Rotations is described. The procedure is connected with Boys, Ruedenberg and Mezey MO localization algorithms.     

A green and novel procedure for the preparation of ionic liquid

A green and novel procedure is described for the preparation of a series of ionic liquid containing alkylimidazolium-based or N-alkylpyridinium-based cations and hexafluorophosphate-based or tetrafluoroborate-based anions in one-pot solvent-free conditions to give excellent yields with shortened time.     

A refinement of the terpolymer equation and its simple extension to two- and four-component systems

Terpolymer composition estimation with an established equation has been found to give results that vary with the feed monomer ratio substitution pattern used. A new copolymer equation has been derived that overcomes this difficulty to give the same composition results regardless of the order of monomer substitution. The new equation also gives comparable or better agreement with experimentally determined copolymer compositions than obtained by use of the established Alfrey-Goldfinger terpolymer equation. In addition, this new terpolymer equation demonstrates a versatility not shown by the present terpolymer equations in that it can be readily adapted by inspection to enable estimation of copolymer compositions for two- or for four-component polymer systems. It is also readily adaptable for copolymers with more than four components, and may also be valid for composition estimation of these because of the derivation method used, although it has not as yet been possible to test this possibility. © 1996 John Wiley & Sons, Inc.     

Use of pressure drop profiles to assess the accuracy of Total Pore Blocking measurements of the external porosity of chromatographic columns

By comparing the pressure drop in a column where the meso-pores of the particles have been blocked using the Total Pore Blocking (TPB) method to measure the interstitial volume of the column with that in the same column when the particle meso-pores are fully open, it could be demonstrated in a very sensitive way that the interstitial volume is completely devoid of any significant amount of remaining pore blocking agent in the final phase of a TPB experiment. Monitoring the pressure signal until it returns to its original value can hence be used as a reliable indicator that all blocking agent has been removed from the interstitial void at the end of the flushing period. As a consequence, any small molecular weight dead volume marker that is employed in this phase can explore the full interstitial volume, so that the value of the latter can be measured without being underestimated by the fact that some fractions of the interstitial void would still be occupied by the blocking agent.     

Thermodynamics of the conversion of aqueous glucose to fructose

The thermodynamics of the conversion of aqueous glucose to fructose has been investigated using both heat conduction microcalorimetry and high pressure liquid chromatography (HPLC). The reaction was carried out in both aqueous Tris/HCl buffer and in aqueous phosphate buffer in the pH range 7–8 using the enzyme glucose isomerase and the cofactors CoCl₂ and MgSO₄. The temperature range over which this reaction was investigated was 298.15–358.15 K. We have found that the enthalpy of reaction is independent of pH over the range investigated. A combined analysis of both the HPLC and microcalorimetric data leads to the following results at 298 15 K:ΔG° = 349 ± 53 J mol^-1, ΔH° = 2.78 ± 0.20 kJ mol^-1, and ΔC _p ^° = 76 ± 30 J mol^-1 K^-1. The stated uncertainties are based upon an analysis of both the random and systematic errors inherent in the measurements. Comparisons are made with literature data. The percent conversion of glucose to fructose has been calculated for the temperature range 300–373.15 K.     

Preparation of apolar glass capillary columns by the barium carbonate procedure

As an extension of previous reports, the barium carbonate procedure has been optimized in detail for the preparation of apolar columns. The aim was to produce optimum overall column characteristics, and to maintain them unchanged under the prolonged influence of the highest possible temperature. The main parameters under optimization were glass variety, leaching of glass surface with aqueous HCl, and amount of barium carbonate deposited, while deactivation and coating were kept constant. The basic column characteristics were adsorption properties and thermostability of deactivation, acid/base behaviour and separation efficiency. They were determined by a new, quantitative testing procedure. Intense leaching was able to eliminate almost totally the differences between glass varieties and to create a well-defined glass surface. While untreated glass, leached glass, and barium carbonate treated glass showed specific weak points in the respective column quality, the combination of leaching and barium carbonate treatment yielded the highest and most stable quality. Some technical modifications of the preparation procedure are described, including deactivation in the gas phase, and use of pentane as a solvent for static coating.     

A very simple solvent-free method for the synthesis of 2-arylchromones using KHSO4 as a recyclable catalyst

An efficient and solvent-free procedure for the synthesis of flavones using KHSO₄ as a recyclable catalyst is described. The methodology represents an environmentally friendly process in comprehensive consideration compared with other catalytic systems listed in publications. This method provides a clean, simple, solvent-free reaction and useful alternatives to prepare flavones and chromones. The use of KHSO₄ catalyst provides excellent yields, also leading to an easy separation and recovery of the catalysts, which allows both low environmental impact and low cost. Other green advantages of the method are the low formation of wastes and the replacement of corrosive, soluble mineral acids.     

A simple and convenient procedure for the synthesis of 1-aminophosphonates from aromatic aldehydes

A simple, efficient, possible industrial process has been developed for the synthesis of 1-aminophosphonic acids from simple starting materials. As described below, treatment of aromatic aldehydes with ammonia and reaction with diethyl phosphite gives diethyl N-(arylmethylene)-1-aminoaryl methylphosphonates, which can be easily hydrolyzed to diethyl 1-aminoarylmethylphosphonates. This method is easy, rapid, and good yielding for the synthesis of 1-aminoalkylphosphonates from simple starting materials.     

A simple one-pot procedure for the direct conversion of alcohols into azides using TsIm

A facile and efficient method for one-pot conversion of alcohols into azides using N-(p-toluenesulfonyl)imidazole (TsIm) is described. In this method, alcohols are refluxed with a mixture of NaN₃, TsIm and triethylamine in the presence of catalytic amounts of tetra-n-butylammonium iodide (TBAI) in DMF affording the corresponding alkyl azides in good yields. This methodology is highly efficient for various structurally diverse alcohols with selectivity for ROH: 1° > 2° > 3°.     

A simple oxidative procedure for the removal of ruthenium residues from metathesis reaction products

Ruthenium residues can be easily and rapidly removed from Grubbs metathesis products by washing with 15% aqueous hydrogen peroxide, which converts any ruthenium complexes into highly insoluble ruthenium dioxide, which then catalyzes the conversion of excess peroxide into water and oxygen. Ruthenium levels lower than 2 ppm can be routinely obtained; an additional advantage is that any phosphines are also rapidly oxidized to the corresponding, more polar phosphine oxides thereby facilitating their removal as well in many cases.     

An adaptive strategy for selecting representative calibration samples in the continuous wavelet domain for near-infrared spectral analysis

Sample selection is often used to improve the cost-effectiveness of near-infrared (NIR) spectral analysis. When raw NIR spectra are used, however, it is not easy to select appropriate samples, because of background interference and noise. In this paper, a novel adaptive strategy based on selection of representative NIR spectra in the continuous wavelet transform (CWT) domain is described. After pretreatment with the CWT, an extension of the Kennard–Stone (EKS) algorithm was used to adaptively select the most representative NIR spectra, which were then submitted to expensive chemical measurement and multivariate calibration. With the samples selected, a PLS model was finally built for prediction. It is of great interest to find that selection of representative samples in the CWT domain, rather than raw spectra, not only effectively eliminates background interference and noise but also further reduces the number of samples required for a good calibration, resulting in a high-quality regression model that is similar to the model obtained by use of all the samples. The results indicate that the proposed method can effectively enhance the cost-effectiveness of NIR spectral analysis. The strategy proposed here can also be applied to different analytical data for multivariate calibration.     

A simple procedure for the chromatographic isolation and determination of prostaglandins from human seminal plasma

Summary A relatively simple procedure for the isolation and determination of the prostaglandins present in human seminal fluid is described. It involves preliminary chromatographic purification of these compounds from the major non-prostaglandin impurities followed by their total elution in one solvent (one-step elution). The prostaglandins thus obtained were almost free from other lipids and were further resolved into prostaglandin-groups and individual prostaglandins by repeated thin-layer chromatography. Data are also presented for prostaglandin contents of fresh semen samples from five individuals and results compared with those from the stored samples.

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Einfaches Verfahren zur chromatographischen Isolierung und Bestimmung von Prostaglandinen aus menschlichem Sperma

Zusammenfassung Das Verfahren umfaßt eine chromatographische Abtrennung der Verbindungen von den hauptsächlichsten Verunreinigungen und die Gesamtelution mit einem Lösungsmittel. Die von anderen Lipiden fast völlig freien Prostaglandine werden durch wiederholte Dünnschicht-Chromatographie in Gruppen und Einzelverbindungen getrennt. Werte werden angegeben über die Prostaglandingehalte von frischem im Vergleich zu gelagertem Sperma.

     

A simple procedure for the rapid optimization of reversed-phase separations with ternary mobile phase mixtures

Summary A simple rapid procedure is described for estimating optimum compositions of ternary mobile phase mixtures for the separation of samples by reversed-phase liquid chromatography (RPLC). Retention data in two iso-eluotropic binary mobile phase mixtures (mixtures with equal retention times) are required to initiate the procedure. The logarithm of the capacity factor is assumed to vary linearly with the composition of isoeluotropic ternary mixtures formed by mixing the two limiting binaries. Using the product of resolution factors of adjacent peaks as the criterion, an optimum ternary composition is then calculated. After a chromatogram has been obtained with the predicted optimum ternary mobile phase, the procedure is repeated until no further improvement can be achieved. Examples of the application of the present procedure are described to illustrate its effectiveness.     

An evaluation of the modified BCR sequential extraction procedure to assess the potential mobility of copper and zinc in MSW

Copper and zinc were determined in municipal solid waste (MSW) samples with different deposit ages from Tianziling landfill site. The pseudototal metal contents of the MSW samples were determined following an aqua regia digestion. Operational speciation was performed using the modified BCR sequential extraction procedure. Analyses were carried out by AAS. Agreement between most of triplicate samples was acceptable. The amount of copper and zinc extracted in the sequential procedure (i.e. Step 1, Step 2, Step 3, residual) did not generally agree well with pseudototal digestion. Various MSW samples contained significant different levels of copper and zinc, but these were with different potential migrations. For example, 49.88%-76.34% of copper existed in five MSW samples was present as oxidable fraction while ~ 40% of zinc was present as acid soluble fraction. The study illustrates the feasibility and importance of modified BCR sequential extraction procedure used as evaluation method when assessing the potential mobility of heavy metal in MSW landfill.