Neutron-absorption deformable boron-rich ferrous alloys

The structure of the eutectic-type iron-boron alloys (up to 3.5 wt% B) crystallized at various velocities has been studied. It was established that due to temperature increase a coarse structure of the eutectic Fe+Fe₂B transforms into a fine dendritic structure. High-temperature annealing leads to the destruction of columnar construction of the eutectic phase and boride dendrites subsequently transform into the inclusions of spherical shape. These processes are more active at high velocities leading to decrease of strength properties and increase of elasticity of the alloys. Such treatment makes possible hot repartition of the ingots from the alloys Fe+3%B through their forging so that the ingots can be rolled into 3-5 mm thick platelets. The obtained product may serve as a material applicable for the preparation of neutron-absorption protective constructions.     

The microchemical analysis of ferrous and non-ferrous alloys

Satisfactory methods are described for the determination of certain of the alloying constituents in small quantities of steels, aluminium alloys and white metals. In steels, lead is determined by using an extraction procedure with dithizone, whereas the stable colour produced by vanadium with 3 : 3' dimethylnaphthidine is used for determining this element. In aluminium alloys, absorptiometric procedures are recommended for determining copper, nickel, iron and manganese. The determination of silicon is advocated by the absorptiometric technique. For the determination of antimony, in white metals, a micro volumetric procedure with standard potassium bromate is recommended using α-naphthaflavone as indicator.     

Determination of cerium in minerals with sulphanilic acid

Cerium can be determined colorimetrically in minerals with sulphanilic acid. Cerium(III) ions are oxidized with silver(II) in 1-7% sulphuric acid. Sulphanilic acid is oxidized by cerium(IV) ions in 20% sulphuric acid. The absorbance is determined at 540 nm. In the presence of maganese or chromium, cerium can be separated by precipitation as the oxalate. Lanthanum can be used as a gathering agent if necessary.     

Determination of aluminium in molybdenum and tungsten metals, iron, steel and ferrous and non-ferrous alloys with pyrocatechol violet

A method for determining 0.001-0.10% of aluminium in molybdenum and tungsten metals is described. After sample dissolution, aluminium is separated from the matrix materials by chloroform extraction of its acetylacetone complex, at pH 6.5, from an ammonium acetate-hydrogen peroxide medium, then back-extracted into 12M hydrochloric add. Following separation of most co-extracted elements, except for beryllium and small amounts of chroinium(III) and copper(II), by a combined ammonium pyrrolidincdithiocarbamate-cupfen-on-chlorofonn extraction, aluminium is determined spectrophotometrically with Pyrocatechol Violet at 578 nm. Chromium interferes during colour development but beryllium, in amounts equivalent to the aluminium concentration, does not cause significant error in the results. Interference from copper(II) is eliminated by reduction with ascorbic acid. The proposed method is also applicable to iron, steel, ferrovanadium, and copper-base alloys after preliminary removal of the matrix elements by a mercury cathode separation.     

Anodic behavior of aluminum-zirconium alloys microalloyed with strontium and cerium

The potentiodynamic method was used to study in solutions of 3% NaCl and 0.01 N NaOH the corrosion-electrochemical behavior of aluminum alloyed with zirconium, strontium, and cerium.Translated from Zhurnal Prikladnoi Khimii, Vol. 77, No. 8, 2004, pp. 1295–1298.Original Russian Text Copyright © 2004 by Ganiev, Barotov, Inoyatov.     

Rapid spectrophotometric determination of copper in iron,steel and ferrous alloys

A rapid spcctrophotometric mcthod for the determination of copper in iron, steel and ferrous alloys without separating the copper has been developed. The sample is dissolved in acid and ammonium citrate is added to complex the iron and other alloying elements. The pH is then adjusted to 8.0–9,5 with ammonium hydroxide. A solution of bis-cyclohexanone-oxalyldihydrazone ia finally added and the absorbance of the blue copper complex formed is measured.     

The determination of boron in ferrous and non-ferrous alloys by neutron transmission

A method has been developed for the determination of 0.1 to over 20% of boron in aluminium-and complex ferro-alloys, based on the neutron-absorbing properties of the¹⁰B nucleus. It has also been applied to stainless steel. The determination is fully automatic and results are conveniently processed by computer.     

Determination of ferrous ion in microsamples of hexagonal ferrites

Summary A sensitive and accurate method is described for determining microgram amounts of ferrous iron associated with a large excess of ferric iron and various bivalent cations, in hexagonal ferrites. Ferrous iron is complexed with bathophenanthroline, extracted into a chloroform-ethanol mixture and spectrophotometrically measured at 540 nm against a 13 v/v chloroform-ethanol mixture. Ferric iron is masked with ammonium dihydrogen phosphate. The analytical conditions are stated for determination of iron(II) in both solvents used for ferrites, viz., hydrochloric and phosphoric acids. Cobalt, copper, and nickel do not interfere if the procedures suggested are used. Ferrous iron down to 0.02% can be determined in samples weighing only a few milligrams.

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Zusammenfassung Eine empfindliche und genaue Methode zur Bestimmung von Mikrogrammengen Eisen(II) in Gegenwart eines großen Überschusses von Eisen(III) und verschiedener zweiwertiger Kationen in hexagonalen Ferriten wurde beschrieben. Eisen(II) wird mit Bathophenanthrolin komplex gebunden, mit einer Chloroform-Äthanol-Mischung extrahiert und bei 540 nm gegen eine Chloroform-Äthanol-Mischung (13 v/v) spektrophotometrisch gemessen. Eisen(III) wird mit NH₄ · H₂PO₄ maskiert. Die Arbeitsbedingungen für die Bestimmung von Eisen(II) in beiden für Ferrite verwendeten Lösungsmitteln — Salzsäure und Phosphorsäure — wurden festgelegt. Co, Cu und Ni stören die empfohlenen Verfahren nicht. Bis zu 0,02% Eisen(II) können in Einwaagen von wenigen Milligramm bestimmt werden.

     

Determination of ferrous and total iron in refractory spinels

Accurate and precise determination of the redox state of iron (Fe) in spinels presents a significant challenge due to their refractory nature. The resultant extreme conditions needed to obtain complete dissolution generally oxidize some of the Fe(II) initially present and thus prevent the use of colorimetric methods for Fe(II) measurements. To overcome this challenge we developed a hybrid oxidimetric/colorimetric approach, using Ag(I) as the oxidimetric reagent for determination of Fe(II) and 1,10-phenanthroline as the colorimetric reagent for determination of total Fe. This approach, which allows determination of Fe(II) and total Fe on the same sample, was tested on a series of four geochemical reference materials and then applied to the analysis of Fe(Ni) spinel crystals isolated from simulated high-level-waste (HLW) glass and of several reagent magnetites. Results for the reference materials were in excellent agreement with recommended values, with the exception of USGS BIR-1, for which higher Fe(II) values and lower total Fe values were obtained. The Fe(Ni) spinels showed Fe(II) values at the detection limit (ca. 0.03 wt% Fe) and total Fe values higher than obtained by ICP-AES analysis after decomposition by lithium metaborate/tetraborate fusion. For the magnetite samples, total Fe values were in agreement with reference results, but a wide range in Fe(II) values was obtained indicating various degrees of conversion to maghemite. Formal comparisons of accuracy and precision were made with 13 existing methods. Accuracy for Fe(II) and total Fe was at or near the top of the group. Precision varied with the parameter used to measure it but was generally in the middle to upper part of the group for Fe(II) while that for total Fe ranged from the bottom of the group to near the top.     

Effect of cerium on electrochemical and mechanical properties of aluminum-iron alloys

Effect of cerium on the corrosion-electrochemical and mechanical properties of aluminum alloys with an iron content of up to 3% was studied in order to use secondary aluminum in development of sacrificial formulations.     

Transpassive dissolution mechanism of ferrous alloys in phosphoric acid/acetic acid mixtures

The transpassive dissolution of Fe-12%Cr and Fe-25%Cr alloys in near-anhydrous phosphoric acid/acetic acid mixtures has been studied by conventional voltammetry and electrochemical impedance spectroscopy. Both steady-state and transient techniques point to two parallel pathways for the process involving oxidative dissolution of Cr as Cr(VI) and isovalent dissolution of Fe most probably mediated by an electrolyte-originating species. A simplified kinetic model of the process including only surface kinetic steps has been found to reproduce successfully both the steady-state and the small-amplitude AC response of the studied materials. The kinetic parameters of the model are determined and their relevance regarding the influence of the alloy and electrolyte composition on the relative importance of the two parallel pathways is discussed. The experimental data and model calculations indicate that the effect of acetic acid on the reaction steps related to dissolution of Fe is more significant.     

Determination of ferrous and ferric iron in aqueous biological solutions

A solvent extraction method was employed to determine ferrous and ferric iron in aqueous samples. Fe³⁺ is selectively extracted into the organic phase (n-heptane) using HDEHP (bis(2-ethylhexyl) hydrogen phosphate) and is then stripped using a strong acid. After separation, both oxidation states and the total iron content were determined directly by ICP-MS analysis. This extraction method was refined to allow determination of both iron oxidation states in the presence of strong complexing ligands, such as citrate, NTA and EDTA. The accuracy of the method was verified by crosschecking using a refinement of the ferrozine assay. Presented results demonstrate the ability of the extraction method to work in a microbiological system in the presence of strong chelating agents following the bioreduction of Fe³⁺ by the Shewanella alga BrY. Based on the results we report, a robust approach was defined to separately analyze Fe³⁺ and Fe²⁺ under a wide range of potential scenarios in subsurface environments where radionuclide/metal contamination may coexist with strongly complexing organic contaminants.     

Determination of cerium(III) and cerium(IV) in nanodisperse ceria by chemical methods

Percentages of different valence cerium species have been determined in powdery samples, redispersible compositions, and aqueous sols of nanodisperse ceria prepared from cerium(IV) and cerium(III) salts by various methods with or without organic stabilizers. Cerium(III) is shown to be virtually absent in nearly all of the CeO₂ samples studied. Organic stabilizers are shown to be capable of reducing cerium(IV) in aqueous CeO₂ sols.     

Simultaneous determination of trace niobium, tantalum and tungsten in ferrous and non-ferrous alloys

A method is presented for the determination of niobium, tantalum and tungsten in steel and non-ferrous alloys, based on hydrolysis with sulphurous acid followed by X-ray fluorescence measurements. The limit of determination is about 0.002% and the standard deviation is 0.002 at the 0.05% level. Results below 0.01% by this method are only semiquantitative.     

Determination of niobium in zirconium-niobium alloys

A rapid control determination of niobium in 50% zirconium/50% niobium master-alloy is described; it is a direct spectrophotometric procedure, based on the reaction of niobium ions with hydrogen peroxide in concentrated sulphuric acid. The procedure is suitable for the examination of zirconium alloys containing niobium in the range 0.1 to about 60%. At least 1% of chromium, cobalt, copper, manganese, nickel or tantalum, does not interfere. Interference due to optical absorption by the peroxy-complexes of titanium, tungsten, molybdenum and vanadium is not significant in the determination of niobium above about 1%, provided that these metals are not in excess of about 0.5%, 0.25%, 0.1% and 0.02%, respectively. To compensate for optical absorption due to iron(III), a solution of the sample, not treated with peroxide, is used.     

Determination of tin in titanium alloys

Tin-titanium alloys are becoming increasingly important; consequently a good method is needed for the determination of tin in this type of material. In this paper an accurate iodometric procedure is proposed for the determination. The sample is dissolved in sulfuric acid and the titanium oxidized with potassium permanganate. Tartaric acid is added and the tin precipitated with hydrogen, sulfide. The sulfide precipitate is dissolved in a mixture of sulfuric, perchloric and nitric acids and the solution evaporated to fumes of sulfuric acid. Water and hydrochloric acid are added, and the tin is reduced with lead and antimony trichloride and titrated with iodine. A study was made of the interfering elements that might be found in titanium alloys. The effect of antimony trichloride in reducing interference from copper was investigated. The method is recommended for titanium alloys containing 0.05 to 5.0 per cent. tin.     

Determination of nickel in gold-nickel alloys

An ion exchange separation based on the difference in adsorption from a chloride solution combined with an EDTA titration is suggested as a rapid and accurate method for the determination of nickel in nickel-gold alloys.     

Determination of niobium and tantalum in binary alloys and zirconium alloys

Recent developments in the metallurgy of niobium, tantalum and zirconium have necessitated provision of analytical procedures for determining niobium and tantalum in the presence of each other and in the presence of zirconium. For this purpose, absorptioinetric procedures based on the formation of yellow coloured complexes, between pyrogallol and niobium or tantalum, have been critically examined. Direct absorptiometric procedures are described, which are suitable for determining niobium or tantalum in the range 2 to 7%; when either of these metals exceeds 7%, differential absorptiometric procedures are recommended. Corrections must lie made for absorption due to the presence of other metals which form complexes with pyrogallol. In tlie determination of niobium or tantalum up to 5%, the precision of the method is about ±0.05%. About 12 determinations can be made in a day, by one analyst.     

硫酸高铈铵分光光度法测定葡萄籽提取物中原花青素

建立了葡萄籽提取物中原花青素测定的新方法 硫酸高铈铵分光光度法。它是基于原花青素与Ce4 在强酸性介质中反应生成无色的Ce3 ,通过测定黄色高铈盐的吸光度,间接测定原花青素,Ce4 在319nm波长处具有最大吸收。该方法的线性范围为0.12～10μg mL,RSD为0.98%～1.1%,回收率为97.2%～102.8%,相关系数r=0.9992,检出限为0.04μg mL。