An Automated Method for the Determination of Arsenic and Antimony

Abstract

An automated method for determining arsenic and antimony by atomic absorption spectrophotometry based on the evolution of the corresponding hydride by sodium borohydride is reported. This method is rapid and sensitive, and is most suitable for the routine monitoring of the arsenic and antimony levels in surface and ground water, as well as in polluted water.     

Synthesis of Thin-Film Acidic Ti(IV) and Zr(IV) Phosphates Deposited on Surface of Fiber and Investigation their Properties

Abstract

Cellulosic fibres present great interest as matrix for non-organic synthesis with the use of ion-molecular layering method [I]. This method consists in realization of the successive reactions with the surface functional groups. Synthesized materials can he of scientific and technical interest.     

The Role of the Specific Surface Area of an Adsorbent in the Optimization of Mixture Separation Conditions in Thin-Layer Chromatography

Abstract

The very important aspect of effect of the magnitude of specific surface area on R_M values obtained by using TLC method is presented. In experiments were performed on 4 adsorbents of different specific surface areas 50 – 500 m²/g and with mixed binary mobile phases.

It is shown that R_M values of chromatographed substances aromatic hydrocarbons are lineary dependente upon the specific surface area of adsorbents for each composition of mobile phase. This relationship can be described by a straight line, with the parameters a and b that can be tabularized. These lines can be used to calculate the R_M values of chromatographed substances for any adsorbent if is specific surface area is known. The illustrational comparison of experimentally obtained and theoretically predicted R_M values for different chromatographic system are presented.     

Determination of Very Volatile Halogenated Organic Compounds in Water by Means of Direct Head-Space Analysis

Abstract

Haloforms are formed during chlorination in drinking water treatment. Toxic industrial solvents such as trichloroethylene, tetrachloromethane and tetrachloroethylene endanger precious raw water sources destined for human consumption.

A simple and reliable technique is required to measure these compounds rapidly and accurately. A direct head space technique has been developed, avoiding the need for preconcentration or pre-handling of the sample, reducing the introduction of systematic errors and meeting the requirements of a good separation of the individual compounds and a detection limit below the μg/l level.

The method can be used for the analysis of rather pure water such as tap water and groundwater as well as for the monitoring of polluted surface waters.

Deterioration of the delicate G.C. column is avoided as only very volatile compounds are introduced, which is a definite advantage of the head space technique over extraction.     

Development of a Rapid,Economical and Safe Method,for the Dissolution of Particulate Beryllium,for Atomic Absorption Spectrophotometry

Abstract

Current methods, for the dissolution of particulate beryllium, on static, surface smear or personal air sampler (PAS) filter papers, have, as drawbacks, high acid emissions, the risk of acid burns to staff, the possibility of perchloric acid induced explosions and a high labour requirement, because they rely on digestion of samples by concentrated strong acids.

An alternative method is presented, which overcomes these difficulties. The sample is boiled with a mixture of 2% nitric acid and 0.1% potassium bisulphate. The resulting solution may be determined for beryllium by atomic absorption spectrophotometry directly.

The method has been validated by analysing samples doped with up to 15 μg of particulate beryllium in the particle size range 1–150μm.     

Applications of Optimization Strategies in the Design of Intelligent Laboratory Robotic Procedures

Abstract

Laboratory robots are being used to perform sample preparation and routine analytical determinations 1,2. In addition to these routine applications, laboratory robots should be able to analyze the analytical procedure itself and select the optimal experimental condition for any analytical method. The application of the fixed-sized SIMPLEX algorithm, the Nelder and Mead variable sized SIMPLEX algorithm and response surface fitting methods in analytical robotics is presented ³.     

Temperature Dependence of the Surface Tension of Alkali Metals: A Unified Correlation

Abstract

In this work, new definitions of the normalized temperature and surface tension are proposed which result in a single plot for the surface tension of molten alkali metals. The functional dependence of the reduced surface tension on the reduced temperature can be adequately described by a straight line; the intercept and slope have been obtained using the linear regression approach. The method proposed herein predicts the values of surface tension at various temperatures with an average error of about 5%.     

Surface Tension of the Liquid Hg-In Alloys

Abstract

The measurements of the surface tension of the liquid Hg-In alloys were made by means of a maximum drop pressure method. The surface tension increases monotonously with increasing the In concentration. It is thermodynamically shown that the composition of the Hg atoms adsorbed on the surface is larger than that in the bulk. Experimental results are compared with calculated results due to various model theories; in particular the hard sphere model with a density-dependent cohesive potential is found to be in qualitative agreement with experimental results of both surface tensions and its temperature coefficients.     

Surface Tension of Ternary Liquid Mixtures

Abstract

Surface tension has been measured by the differential capillary rise method for three ternary mixtures containing alkanes (hexane + cyclohexane+benzene, pentane + hexane + benzene and cyclohexane + heptane + toluene at 298.15\pm 0.1°K). The sign and magnitude of the excess surface tension and excess volume depend ultimately upon the chain length of the component of the mixtures. The results of the surface tension were compared with theoretical values obtained from Flory theory, Sanchez method, Brock-Bird relation and volume fraction statistics. There is reasonable agreement between theory and experiment.     

Optimisation of a Gas Stripping Concentration Technique for Trace Organic Water Pollutants

Abstract

The application of gas stripping for the concentration prior to analysis of organic water pollutants at the parts per million and parts per billion level has been studied. Solutes are stripped from solution by a stream of inert gas and subsequently adsorbed onto active carbon from which surface they are taken up in a solvent for analysis.

The method is shown to be applicable to the analysis of a wide range of compounds including pesticides and polychlorinated biphenyls. The effect of gas flowrate, the time of stripping, adsorbent particle size, and desorbing solvent on the percentage recovery of a range of organic compounds has been measured.

Problems of contamination of aqueous solutions by absorption of atmospheric vapours prior to analysis are considered, and the analysis of a typical water sample is demonstrated.     

Struktur von 7,11-Diphenyl-2,4-diazaspiro[5,5]undecan-1,3,5,9-tetraonen durch LIS-NMR

A semi-quantitative method for determining distances between a possible coordination centre and protons from LIS-NMR values is developed for the title compounds3, although these have four coordination points. This makes it possible to propose structures and conformations for the isomers of3.

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Mit 4 Abbildungen

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H.-H. Otto undH. Yamamura, Ann. Chem., im Druck.     

Characterization of Liquid-Solid Adsorption Systems by Using TLC Data

Abstract

The thin-layer chromatography (TLC) method is used to measure the excess adsorption isotherms for different binary liquid mixtures on silica gel. These isotherms are interpreted by means of the Langmuir-Freundlich equation, which involves the adsorbent heterogeneity and the difference in the molecular sizes of the components. This equation makes possible the evaluation of the surface phase capacity, equilibrium constant and heterogeneity parameter, which characterize liquid-solid adsorption systems.     

A Method For Measuring The Vapour Pressures Of Pah'S Adsorbed On The Surface Of Soot

Abstract

A new method is reported that utilizes a low-temperature quartz microbalance in combination with Knudsen cells to obtain adsorption isotherms for substances with very low equilibrium pressures (< 10^?5 Pa). The method allows for the first time to measure directly thermodynamic properties of important aerosol/pollutant systems at typical environmental temperatures. Application is demonstrated by an investigation of fluoranthene and pyrene adsorbed on carbon aerosol particles (T = 293.15 K?302.13 K). Both PAHs are unable to form extended multilayers on the surface. Slightly above monolayer coverage the three-dimensional crystalline solid phase is thermodynamically more stable.     

High-Performance Liquid Chromatographic Determination in Human Plasma of a Anticonvulsant Benzodiazepine: Clonazepam

Abstract

A rapid and specific high-pressure liquid chromatography method for determination of clonazepam in human plasma is described.

The analysis is linear for concentrations ranging from 5 to 100 ng. ml^-1 plasma for clonazepam.

The method is applicable to quantitation of clonazepam in human plasma of subjects receiving 0.05 at 0.20 mg.kg^-1 orally, with satisfactory accuracy and precision.     

Preparation of Hair and Nail Samples for Trace Element Analysis

Abstract

The method of washing of human hair and nail samples is examined by neutron activation and γ-ray analysis. The amounts of Na, K, Br, Au, Zn and La that are removed by successive washings determine the optimum number of washing for removing these trace elements as surface contaminants. A total solution contact time with the nails is 5 minutes, and leaching effects are observed after 6 washings.     

A Fast Made Disposable Glucose Biosensor Incorporating the Oxidase and a Ferrocene in an Alginate Gel

Abstract

A simple procedure is described for co-immobilization of glucose oxidase and dimethylaminomethylferrocene in a sodium alginate gel on the surface of pyrolytic graphite electrode. The film is electrochemically active and the peak current is a function of D-glucose concentration with the apparent Michaelis-Menten constant K_m = (1.2±0.3) × 10^?2 M. The optimal concentration range for biosensoric applications in 0.001–0.010 M.

     

Adsorption of Methylene Blue on Montmorillonite

ABSTRACT

Adsorption of Methylene Blue ( MB) on Na-, Fe- and Al-montmorillonite suspensions at 298.15 K were studied. The effect of different exchangeable cation on the adsorption amount of MB was determined. The results show that methylene blue cations( MB⁺ ) replace Na? more easily than they do Fe³⁺ and Al^{3 +} The adsorption isotherms on the three montraorillonites were all of Langmuir type, except that the isouHerm of MB on Na-montmorillonite presents nonmonotonic curve at low surface coverage. The specific surface areas in suspension were calculated by( MB ^{3 +} )method, and Na^? is more effective to determine the specific surface area by MB method in suspension than Fe^{3 +} and A^{3 +} The discrepancy of the specific surface area measured by MB and BET method was discussed.     

Determination of Surface Silanols of Silica Gels and HPLC Bonded Phases

Abstract

A rapid method determining the surface silanols of silica gels and HPLC bonded phases involves a titration of silica gel with sodium hydroxide, in a medium of any of the following 10% aqueous salts: sodium chloride, sodium nitrate, sodium sulfate, potassium chloride, potassium nitrate and potassium sulfate. The silanols are quantified as m eg/g. It is possible to determine cation exchange capacity of a cation-exchanger due to an acid as an end group and surface silanols separately.     

Correlation Between Specific Surface Area and Methyl Red Adsorbed on Silica Gel

Abstract

The amount of methyl red, adsorbed on bare silica gel, has been determined for 32 samples having a specific surface area ranging from 10 m²/g to 500 m²/g, as determined by a BET method. A linear relationship between amount of dye adsorbed and specific area exists up to about 300 m²/g. Beyond this value the amount of adsorbed dye does not increase correspondingly, which is believed to be due to the relative increase of micropores in the silica gel structure. It is proposed that the easily performed determination of the adsorbed methyl red can serve to estimate that part of the silica gel surface which is available for chromatographic interactions.     

Electron Capture Gas Chromatography of Nitrazepam in Human Plasma as Methyl Derivative

Abstract

A method for quantitative determination of nitrazepam in human plasma in the range 5 - 100 ng/ml is presented.

Nitrazepam is extracted with benzene from plasma samples of 0.5 ml, methylated with methyl iodide and determined gas chromatographically with an electron capture detector of ⁶³Ni-type.

Acid dissociation constants of nitrazepam are determined and the partition properties studied with benzene, methylene chloride and diethyl ether as organic phases.

The selectivity of the method with respect to the metabolites has been thoroughly studied.