A new reagent for the detection and determination of small amounts of the sulphate Ion

An aqueous solution of 2-aminoperimidine hydrochloride is proposed as a new reagent for the detection and determination of the sulphate ion. As little as 0.05 p.p.m. can be detected by precipitation of the corresponding amine sulphate. Suspensions of the precipitate show remarkable stability and no colloidal stabilizers are needed. The reagent is applied to the nephelometric determination of 0.1–5 p.p.m. of sulphate ion; at the 0.5 p.p.m. level, the relative standard deviation is 4.5%. Although many ions form precipitates with the reagent at high concentrations, very few of the common anions provide significant interference in the nephelometric determination. The reagent seems promising for the determination of sulphate in natural waters, and for traces of sulphur in organic compounds after oxygen flask combustion.     

Some notes on the reaction between ferric and thiocyanate ions

A spectrophotometric study has been made of the reaction between ferric and thiocyanate ions in sulphuric acid solution. The effects of acidity, thiocyanate concentration, persulphate concentration, temperature, light and added beryllium sulphate upon the stability and colour intensity of the solution are described.For analytical applications in the absence of added sulphate ions the best results are obtained at an acid normality of 1.5 to 2.0, while in the presence of beryllium sulphate at molar concentration it is desirable to increase the acid normality to 3.0. Precise control of thiocyanate concentration and temperature is required. The solutions obey Beer's law and an ultimate sensitivity of 0.035 p.p.m. of Fe is obtained when using a I cm cell.     

配位体SO2-4对激发态铀(VI)去活化的影响

The dependence of the luminescence decay of electronically excited uranyl ions on the concentrations of uranium and sulphate in aqueous solution has been investigated with a pulsed nitrogen laser as a light source and a programmable transient recorder for lifetime measurements. Single exponential decay of the Luminescence is observed. The deactivation process of the excited uranyl ions should include radiative, nonradiative, water quenching and uranium self quenching and the measured lumine-scenec lifetime inidcates the result of all these processes. The Luminescence lifetime of uranyl ions increases with increasing concentration of sulphate and becomes constant when the equilibrium concentration of sulphate reaches 3.0 mol·L~(-1). The dependence of the Luminesence lifetime is similar to that of the UO_2(SO_4)_3~(4-) formation. This phenomenon can be interpreted in terms of the fact that in aqueous solution uranyl ions exist as aquo-uranyl ions. As the concentration of sulphte increaes the water molecule of hydrated uranyl ions will be replaced by sulphate ions via complex formation, and the quenching of excited uranyl ions by water is reduced. The self quenccing and the water quenching rate constants of UO_2(H_2O)_6~(2+) and UO_2(SO_4)_3~(4-) are estimated. Based on the experimental results a model for the deactivation mechanism of excited uranyl ions in sulphate solution is proposed.     

配位体 SO_4~(2-)对激发态铀(Ⅵ)去活化的影响

近年来,随着激光、微弱信号测量以及瞬态测量技术等发展,对溶液中激发态离子的化学和物理行为的研究已日益受到人们的重视,激发态铀酰离子发光衰减的研究尤为活跃.Marcantonatos 等、Formosinho 等以及郑企克、王志麟等对高氯酸溶液中激发态铀酰离子的发光衰减过程进行了详细的研究.探讨了ClO_4~-溶液中pH 等对激发态铀酰离子的发光衰减的影响,观察到了一定的pH 条件下激发态铀(Ⅵ)的非单一指数衰减,并各自提出了不同的解释.值得提出的是,上述的一系列研究都是在高氯酸溶液中,其它体系中铀(Ⅵ)的发光哀减的研究进行得很少,报导则更少.1983年Joshi 等曾研究了80K 时SO_4~(2-)     

Effects of sulphate,calcium and aluminum ions upon the hydration of sulphoaluminate belite cement

In the model sulphoaluminate belite cement, the process of hydration is governed by the diffusion and transport phenomena of the main ionic species. The sulphate components and combined sulphate and aluminium ions, exert an accelerating effect upon the kinetics of sulphoaluminate belite cement hydration. Aluminium and calcium ions delay the hydration by creating a retarding layer which can be considered a co-precipitate of aluminium and calcium hydroxides. This is revealed in the calorimetric curves by the duration of induction period and also by the intensities of the main peaks. The appearance of small additional peaks characterizes the formation of primary ettringite, due to the presence of sulphate ions in aqueous solution. The intensities of these peaks depend on the ion concentration too.     

The microdetermination of chloride,sulphate, phosphate and nitrite by reflectance spectrometry

Quantitative spot tests with a reflectance spectrometer have been developed for chloride (10–320 p.p.m.), sulphate (10–120 p.p.m.), phosphate (2–30 and 10–180 p.p.m.) and nitrite (1–35 and 10–100 p.p.m.). There are few interferences with these tests, and their effects can be overcome by standard techniques except for the interference from phosphate when it is present in the sulphate test, in large concentrations.     

The application of differential pulse polarography to the determination of a pharmacologically active benzhydrylpiperazine derivative and its major electroactive metabolites in the plasma and urine of animals.

A method for the determination of 1–500 p.p.m. of acid-soluble aluminium and 2–500 p.p.m. of acid-insoluble aluminium in low-alloy and stainless steels by flameless atomic absorption with a HGA 74 graphite furnace is described. A typical value of the relative standard deviation for acid-soluble aluminium at concentrations larger than 10 p.p.m. was 5 %. The steel sample was dissolved in hydrochloric and nitric acid and filtered. Ammonium sulphate was added to the filtered sample in order to overcome interferences caused by hydrochloric acid. No concentration steps were used. Acid-soluble aluminium was determined within 20 min. The influence of iron, chromium, nickel, molybdenum, hydrochloric acid, nitric acid and ammonium sulphate respectively was investigated.     

The indirect spectrophotometric determination of the sulphate ion with 2-aminoperimidine

A new spectrophotometric determination of the sulphate ion is described which uses 2-aminoperimidine hydrochloride as a precipitating reagent. The excess of the reagent is measured at 305 nm. The procedure deals with sulphate in the range 4–120 p.p.m., and relies on simple calibration. The relative standard deviation for 50 p.p.m. of sulphate is 3.7%. The interference of 100 p.p.m. of phosphate, fluoride and nitrate is only slight in the determination of 50 p.p.m. of sulphate. The method is recommended for the determination of sulphate in rain and surface waters.     

The spectrographic determination of total barium in bone ash

Samples of bone ash are mixed with graphite and anhydrous copper sulphate as spectrographic buffer and lanthanum oxide as internal standard. The mixture is pressed into 30-mg pellets and burnt in a d.c. arc surrounded by a mantle of oxygen and argon. The spectra are evaluated by non-recording microphotometry. The effective concentration range is 2–25 p.p.m. of barium in the ash, and the coefficient of variation is 8% for single exposures at the 8-p.p.m. level     

Determination of nitrate and nitrite in mixtures with a nitrate ion electrode

A rapid method for the determination of nitrate and nitrite ions is described. The potential of a mixture of nitrate and nitrite was measured with a nitrate ion selective electrode. The nitrite in the mixture is then oxidized to nitrate with permanganate in acid solution, and the potential of the oxidized solution is also measured with the electrode. The fundamental equations for the response of the nitrate ion electrode to nitrate ion in the presence of interfering ions were used, and a new equation was developed for calculating the original nitrate concentration of the mixture. The absolute errors for solutions of known concentrations (2.5–100 p.p.m. each) were 1.8 p.p.m. nitrate and 2 p.p.m. nitrite. When the results are calculated by computer, five determinations can be performed in 30 min. The method was applied to the determination of the oxides of nitrogen in cigarette smoke as nitrite and nitrate after dissolution in basic solution.     

Heterogeneous and homogeneous nucleation of strontium sulphate

Heterogeneous and homogeneous nucleation processes of strontium sulphate have been studied, using a homogeneous precipitation technique together with electronic particle counting. Four different heterogeneous nucleation processes were observed in solutions purified by conventional filtration. In solutions purified by continued circulation through a fibre-glass filter mat, homogeneous nucleation was observed at supersaturations about 10.75. The rate of homogeneous nucleation was found to depend on the 27th power of the sulphate concentration, indicating that the nucleus contains 52 ions. The results support the theory of homogeneous nucleation presented by Nielson.     

slow release rubber formulations containing ZnSO4

Styrene butadiene (SBR) and natural rubber (NR) can be used as binding matrices to control the release of zinc (Zn) which is a micro-nutrient for plants. The leaching rate of zinc in an aqueous medium depends on the concentration of zinc sulphate loaded in the two types of rubber used, the temperature of the surrounding environment and the pH of the aqueous medium. Water uptake was increased with increasing concentration of ZnSO₄. The sustained release of zinc ions from the investigated formulations was prolonged for over five months. The mechanical properties of the vulcanizates were affected as the concentration of zinc sulphate changed.     

The determination of microgram amounts of sulphur in nitrate or chloride solutions

It is shown that μg quantities of sulphate can be “collected” with barium chromate when the latter is precipitated from solutions at a pH of about 1. The sulphate in this precipitate can be converted to hydrogen sulphide when the precipitate is treated at red heat with a mixture of hydrogen and hydrogen chloride vapour. The above procedure has been made the basis of a method for determining traces of sulphur, down to about 0.2 p.p.m. on a 10 g sample, when the hydrogen sulphide is determined absorptiometrically as Lauth's violet.     

The interference effect of more than one anion and cation in graphite furnace atomic absorption spectrometry. Part 2: Effect of sodium,magnesium, sulphate and chloride mixtures on the atomization of manganese

Although there are numerous cations and anions in real samples generally, the interference effects of a matrix consisting of one cation and one anion on the atomization of an element in graphite furnace atomic absorption spectrometry (GFAAS) have been investigated. Therefore, it would be more realistic to investigate the interference of a matrix containing more than one cation and anion. In this study, the simultaneous interference effects of sodium, magnesium, sulphate and chlorine, which are the most common and abundant ions in many samples, e.g. sea water, on the atomization of manganese in GFAAS were studied. As a first step, the individual interferences of some possible salts consisting of simple combinations of the ions studied such as sodium chloride, magnesium chloride, sodium sulphate and magnesium sulphate, were investigated. It was found that in the presence of these four ions and in their wide concentration range, sodium chloride and magnesium sulphate are the major salts formed after the drying step which were supported by X-ray diffraction (XRD) studies. Sodium chloride causes a significant depressive effect at low pyrolysis temperatures. The interference of sodium chloride originates from expulsion of the analyte with matrix and gas phase reaction between manganese and chloride ions during atomization. Magnesium sulphate does not cause any depression and in fact higher pyrolysis temperatures compared to matrix-free manganese can be applied without loss of any analyte. The depressive effect of sodium chloride on manganese markedly decreased in the presence of magnesium sulphate due to its protecting effect. The mutual interaction mechanism of these two salts and their effects on manganese have been discussed.     

Radiochemical determination of intracellular ionic concentrations in alga Hydrodictyon reticulatum

Algal nets of Hydrodictyon reticulatum have been cultivated in the radioactivity labelled medium of different chemical composition. It has been found that the intracellular concentration of sodium, potassium, ammonium, chloride, sulphate and phosphate ions changed in a great extent in the dependence of the experimental conditions. The influx of cations from neutral chloride solutions decreases in the order: ammoniumpotassium, thallium/I/rubidium>cesium>lithiumsodium ions. The intracellular chloride ions can be reversible displaced by bromide or sulphate anions.     

Thermal behaviour of polyacrylamidoxime-copper chelates

The purpose of this work was to investigate the effect of several factors (anion type in the copper salt, pH and concentration of the salt solution) on the structure and thermo-oxidative degradation of the polyacrylamidoxime-copper chelates, by using elemental analysis, IR spectroscopy and dynamic thermogravimetry. The chelates containing copper ions as sulphate exhibit a better initial thermal stability than the polyacrylamidoxime fibre presumably due to the crosslinking generated by the intermolecular complexation of the ions; the removal of the sulphate anions takes place concomitantly with the second step of polymeric chain decomposition. The initial thermal decomposition of the chelates formed by copper ions as nitrate begins at lower temperatures as compared to the polyacrylamidoxime fibre, probably by the nitrate anion release, which partly overlaps the initial decomposition of the copper ion-crosslinked polymeric chains. Copper ions as either sulphate or nitrate catalyse the reactions involved in the main step of polyacrylamidoxime fibre decomposition; the higher the copper amount, the stronger the catalytic effect.     

(Series Editor) Transform Techniques in Chemistry,P.R. Griffiths,D. Hercules (Eds.), in: Modern Analytical Chemistry Series,Plenum, New York,NY (1978), 385 pp. $47.40

Concentration potentials in zinc sulphate, copper sulphate, nickel sulphate and cobalt sulphate solutions across liquid membranes based on myristates and laurates of zinc, copper, nickel and cobalt and caprate and caprylate of copper have been studied in concentration cells in which the liquid membrane separates the two solutions of the same electrolyte. The behaviour of the cell with heavy metal soap liquid ion-exchange membranes becomes more and more nernstian as the number of carbon atoms in the hydrocarbon chain of the fatty acid soap increases. Concentration potential values with copper, zinc, nickel or cobalt soap follow the order of their insolubility in water. The failure to record the theoretical potentials as calculated by Nernst's equation has been explained by considering the transport of water across organic phase by hydrated ions and the dissolution of heavy metal soaps in aqueous solutions. Liquid membranes based on heavy metal myristate soaps when used in concentration cells could measure the activities of zinc, copper, nickel and cobalt ions in the concentration range of 10^?4–10^?1M.     

Application of displacement reactions in flame photometry-II Emission flame photometric determination of alkaline earth metals in the presence of interfering anions

For the emission flame photometric determination of strontium and barium in the presence of interfering ions such as phosphate, sulphate, arsenate and oxalate, calibration or simple standard addition methods cannot be used. Greatly reduced errors can be achieved by dividing the sample solution into four equal parts and adding to each certain known amounts of two metal ions. One of these is identical to the determinand (e.g., strontium or barium) the other has similar characteristics to it (e.g., calcium). The amounts of these metals are chosen so that the total (molar) concentration of these should be identical in all solutions, but the ratio of the concentrations of the two metals should be different. The emission of the determinand metal must be measured, and a standard addition plot produced. The amount of determinand present in the sample can be obtained from the intersection of the emission vs. concentration line with the concentration axis.     

Über die Verwendung von Anionenaustauschern in Verbindung mit Atom-Absorptions-Spektroskopie zur Bestimmung von Phosphat und Sulfat

Zusammenfassung Mit Hilfe stark basischer Anionenaustauscher werden Phosphat-und Sulfationen aus einem Gemisch getrennt. Als Eluierungsmittel wird verdünnte Salzsäure verwendet. Die Detektion und quantitative Bestimmung dieser Anionen erfolgt indirekt mittels Flammenabsorption, wobei die Schwächung der Kalziumabsorption bei 422,7 nm durch Phosphat- und Sulfationen als Maß für deren Konzentration verwendet wird.

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The determination of phosphate and sulfate by means of ion exchange chromatography in combination with atomic absorption spectroscopy

Summary Phosphate and sulphate ions can be separated by strongly basic anion exchangers. Diluted hydrochloric acid is used as eluent for these anions. The detection and quantitative determination of phosphate and sulphate ions is done indirectly by atomic-absorption of calcium. The decrease of the calcium absorption correlates with the concentration of these anions.

     

Investigation of gettering effects in CZ-type silicon with SIMS

Ion implantation is a well-known standard procedure in electronic device technology for precise and controlled introduction of dopants into silicon. However, damage caused by implantation acts as effective gettering zones, collecting unwanted metal impurities. This effect can be applied for proximity gettering reducing the concentration of impurities in the active device region. In this study the consequences of high-energy ion implantation into silicon and of subsequent annealing were analysed by means of secondary ion mass spectrometry (SIMS). Depth profiles were recorded of such impurities as copper, oxygen and carbon to obtain information about their gettering behaviour. The differences in impurities gettering behaviour were studied as a function of the implanted ions, P and Si, of the implantation dose and annealing time at T=900°C. Besides impurities gettering at the mean projected range (Rp) of implanted ions, Rp-effect, defects at around half of the projected ion range, Rp/2-effect, and even in some cases beyond Rp, trans-Rp-effect, have also been found to be effective in gettering of material impurities.