Turbidimetric determination of some sulphur compounds in ethanol from fermentation

A simple method is described which can be used for the determination of certain sulphur compounds found in industrial ethanol obtained from fermentation of molasses. The method is based on the turbidimetric determination of sulphate after the sample has been treated with dilute hydrogen peroxide solution, by precipitation of the sulphate with barium chloride under appropriate conditions. Several samples of fermentation ethanol have been analysed by this method and the sulphur contents found compared with the total acidity.     

Determination of sulphur in petroleum products after sulphur dioxide generation and of sulphur dioxide in air by chemiluminescent flame emission

The determination of sulphur in petroleum products by combustion, concentration of the sulphur dioxide in sodium tetrachtoromercurate solutions and cool flame molecular emission is described. Improvements in burner design and optimization of analytical conditions result in a minimum detectable amount of 6 ng of sulphur. The absorption of sulphur dioxide from air samples and its determination by a similar method gives a detection limit of 1.3 μg SO₂ m^-3.     

Application of the iodine-azide reaction to the catalytic determination of divalent sulphur compounds in alcoholic medium: Determination of ethylenethiourea in some biological materials

A new catalytic method for the determination of divalent sulphur compounds, which are soluble or insoluble in water, based on the iodine–azide reaction in various alcoholic solutions is described. As model divalent sulphur catalysts the sodium sulphide and thiourea were chosen. Determination of ethylenethiourea in alcoholic extracts from apples and bananas was an example of practical application of the proposed method. To that purpose five previous elaborated techniques were adopted: titration, volumetric, gas chromatographic, enthalpimetric and potentiometric. The effect of other organic solvents, salts, acids and pH on the determination of divalent sulphur catalysts was also evaluated.     

Application of microwave heating to the determination of free, combined and total sulphur in rubber

An atomic absorption spectrometry (AAS) method for the determination of total and combined sulphur in rubber and a catalytic method for the determination of free sulphur in rubber are described. The catalytic method is based on the iodine-azide reaction and is followed by an extraction of free sulphur with benzene, toluene or acetone. The catalytic determination, with the aid of gas chromatography, was performed in N,N-dimethylformamide after expelling the more volatile solvents used in the extraction. The calibration is linear over the range 2 × 10⁻⁶ – 3 × 10⁻⁴ M. Before the determination of total and combined sulphur, the rubber samples were decomposed by microwave assisted heating (5 min, 110 W) in a Teflon closed vessel. After microwave heating the solution was clear and homogenous and all sulphur compounds contained in the rubber were quantitatively oxidized to sulphate. The sulphates were then precipitated as BaSO₄ and an excess of barium was determined by AAS. From the difference in the results of the determinations of total and free sulphur the amount of combined sulphur can be calculated, and from the difference in the determinations of total and combined sulphur the amount of free sulphur can be calculated. In the latter case the catalytic analysis is not needed.     

The preliminary investigation into the potential use of tomographic techniques for the examination of mechanical components

Tomographic techniques exploiting the measurement of transmitted gamma-radiation have been investigated as a means of providing information about the state of selected mechanical components. In this exploratory study, all samples were taken to a specially constructed laboratory rig for examination. Examples are given of the images generated.     

Determination of airborne mercury-203

A method is described for the determination of airborne compounds of²⁰³Hg. The method is based on the sorption of Hg on hopcalite (activated copper oxide/manganese oxide) with subsequent monitoring for the gamma-radiation of²⁰³Hg. Aerosol activity in the air is separated by sucking the air through a filter prior to the absorption tube. The sensitivity of the method permits the assessment of less than one tenth of the maximum permissible concentration in air. It is shown experimentally that the separation procedure used is suitable for the determination of airborne mercuric acetate and its thermal decomposition products.     

The accurate determination of total sulphur and disulphide and polysulphide compounds in petroleum products by metal reduction and flame emission spectrometry

Conditions for the determination of total sulphur and disulphide/polysulphide in petroleum products are described. The sulphur is reduced by heating with sodium or Devarda's alloy under reflux with subsequent liberation of H₂S and measurement of the chemiluminescent S₂ emission intensity in a hydrogen—argon diffusion flame. The precision and accuracy are good. Applications to light distillates and waxy residues are discussed.     

Relativkonduktometrisches Verfahren zur simultanen Bestimmung extrem niedriger Kohlenstoff- und Schwefelgehalte in Metallen

The simultaneous determination of carbon and sulphur in the ppb-range (or in rag-samples in the low ppm-range) in high purity metals is described. The combustion of the sample (1–1000 mg) is performed in purest oxygen without additives by means of induction heating (6 MHz, 3 kW). The combustion products CO₂ and SO₂, after separation in a gaschromatographic column, are detected using a relative conductometric method. The limits of detection for the determination of carbon and sulphur in vanadium, niobium, tantalum, tungsten, molybdenum, noble metals, copper, aluminium, iron, chromium are 5 ng. With amounts of 100 ng the relative standard deviations of ±5% for carbon and ±6% for sulphur were found. Problems in lowering the blank values (e.g. sample preparation, gas purification, combustion), in absorption of CO₂ and SO₂, and in conductivity measurement are discussed in detail and some calibration methods are compared.     

Rapid and precise determination of total sulphur in soda-lime-silica glasses

A method is described for the determination of total sulphur in small amounts of soda-lime-silica glasses (100 mg or less). The crushed glass is mixed with vanadium pentoxide and decomposed at 1450 degrees under oxygen. The sulphur is quantitatively removed from the glass and determined by a conductometric technique. The method is standardized by accurately injecting sulphur dioxide into the furnace tube. The analysis time is about 10 min and the overall precision (2s) is of the order of 5%.     

The spectrophotometric determination of sulphate after its extraction with methyltricaprylammonium chloride into cyclohexane

Improvements are described to Flynn's procedure for the extraction of sulphate with Aliquat-336 and its subsequent determination as sulphuric acid. A single-point photometric measurement with sodium 2,4-dinitrophenate is applied to the determination of sulphate (ca. 10 mg kg^?1) in soils, and also in sulphur in organic compounds after oxygen flask combustion.     

Manometric submicro determination of carbon and hydrogen in organic materials

A method is described for the determination of carbon and hydrogen in quantities of organic material ranging from 5 to 50 μg. The method involves catalytic combustion of the sample in oxygen and measurement of the pressures of the resulting carbon dioxide and water. Special attention has been paid to the reduction of the effect of water adsorption in the apparatus. The present submicro method can be applied to non-volatile, non-hygroscopic samples and is free from interferences by nitrogen, sulphur and halogens (except fluorine). The standard deviation in the 50-μg sample range is 0.13% for carbon and 0.10% for hydrogen. The average duration per analysis when carried out in series is 20 min.     

Determination of sulfide with chloranilic acid by biamperometric and automatic potentiometric end-point detection with a lead chloranilate selective electrode

A titrimetric method for determination of sulfide and of sulphur in steels with chloranilic acid by biamperometric and automatic potentiometric end-point detection is described. The construction of the sensor for potentiometric indication is also described. The results obtained agree with those of the iodine-thiosulfate method and with the certified values for the steels.     

Wet ashing of coal with perchloric acid mixed with periodic acid for the determination of sulphur and certain other constituents

A method is described for the determination of sulphur and some other inorganic constituents of coal. Organic matter is destroyed by wet combustion with perchloric acid and periodic acid. The method is rapid and efficient. Silica and sulphur are determined gravimetrically, iron, aluminium, vanadium, titanium, phosphorus, and arsenic spectrophotometrically, and calcium and magnesium volumetrically. No loss occurred by volatilisation. The complete analysis scheme devised was applied to a bituminous coal of Iowa origin.     

Determination of total sulphur in fuel oils by ion chromatography

A method is described for the determination of total sulphur in fuel oils. The oils are burnt in an oxygen flask and the resulting sulphur dioxide is oxidised with hydrogen peroxide to sulphate which is subsequently determined by ion chromatography. With a 50-mg oil sample the limit of detection is 0.007% sulphur. The procedure is simple and has a r.s.d. of 2.7%. Blanks are negligible and the only interferences can be from metal ions that form insoluble sulphates. The method is compared with m.e.c.a, x.r.f. and titrimetric procedures.     

A sensitive spectrophotometric method for the determination of methyl alcohol in air and water

A sensitive spectrophotometric method for the indirect determination of methyl alcohol in air and water is described. The methyl alcohol is oxidized to formaldehyde which is then determined in acidic medium with p-aminoazobenzene and sulphur dioxide. Beer's law is obeyed in the range 100-600 mug of methyl alcohol in 25 ml of final solution and the wavelength of maximum absorption is 505 nm. The lower limit of determination is 5 mug ml in the sample. Several common organic co-pollutants do not interfere. The method can be used for determination of methyl alcohol in blood.     

A simple spectrophotometric determination of endosulfan in river water and soil

Summary A simple spectrophotometric determination of endosulfan (Thiodan), a sulphur containing pesticide is described. The method is based on the liberation of sulphur dioxide from endosulfan which is subsequently absorbed into an absorbing reagent, malonyldihydrazide and estimated by using p-aminoazobenzene and formaldehyde to give a pink coloured dye which has an absorbance maxima at 505 nm. The Beer's law is obeyed in the range of 1–6 ppm for a standard solution of endosulfan. The method can be easily applied in river water and soil samples to determine endosulfan levels as low as 0.05 ppm and 0.25 ppm in river water and soil, respectively. The method is free from the interference of most of the commonly used pesticides and foreign ions.     

Determination of total sulphur in soil and plant material

A rapid and accurate method for the determination of the total sulphur content of soil or plant material is described. The sample is heated with sodium bicarbonate and silver oxide at 550° for ₃h, and the sulphur content of the whole residue is reduced to hydrogen sulphide and determined as methylene blue. The results compare favourably with those of other methods.In routine use, at least 30 analyses may be completed in a day.     

The determination of sulphur and phosphorus by atomic emission spectrometry with an induction-coupled high-frequency plasma source

An instrumental assembly is described which permits detection of the atomic emission at their resonance lines below 200 nm from sulphur and phosphorus introduced into a high-frequency induction-coupled plasma source as aqueous solutions of their anions. Optimal conditions for the determination of sulphur at 182.04 nm and phosphorus at 213.62 nm have been established, and detection limits of 1.7 and 0.08 p.p.m. have been obtained for these elements, respectively. The determinations are relatively free from chemical and physical interferences, although spectral interferences from metal ions are observed in both cases. The method established for phosphorus has been applied to its determination in soil extracts.     

Zur relativkonduktometrischer bestimmung des schwefels in erdölprodukten

The relative conductometric method for the determination of sulphur, which has already been used for microelemental analysis, is applied to various petroleum products. The results obtained show that the method is not only very suitable for the rapid determination of the total sulphur content but also gives information on the nature of the combustion processes for sulphur-containing compounds.     

A rapid and accurate determination of trace quantities of sulphur in tin

A method is described which permits the determination of 1–100 p.p.m. of sulphur in metallic tin. It is based on the complete combustion of the sample in a stream of oxygen and the determination of the change in electrical conductivity produced by the absorption of the gaseous combustion products (SO₂) in a suitable reaction liquid. Gas-borne tin (IV) oxide dust is removed from the oxidation products by electrostatic precipitation. The new technique is shown to be superior to the widely used methylene blue method.