Determination of boron in titanium alloys by means of ion exchange

There is need for a rapid method for the determination of moderate amounts of boron in titanium alloys. In this paper a method is proposed which uses ion exchange. The method is applicable to titanium alloys containing 0.025 to 1 per cent. boron. One or two grams of the sample are dissolved in hydrochloric acid, and the titanium and boron are oxidized with nitric acid. The bulk of the titanium is removed by a cation exchanger. A calcium carbonate separation is made to remove the residual titanium and adjust the acidity. The boron is then titrated with sodium hydroxide, after the addition of mannitol. None of the elements found in commercial titanium alloys interferes with the method.     

Determination of sulfur in nickel-base alloys and alloy steels by isotope dilution mass spectrometry

An isotope dilution mass spectrometric method has been developed for the precise determination of 3–300 p.p.m. of sulfur in nickel-base alloys and alloy steels. The sample is dissolved in mixed acids, a spike is added, and nitrate ions are removed. Sulfate is reduced with a mixture of hydriodic, hypophosphorous, and hydrochloric acids; the hydrogen sulfide evolved is absorbed in cadmium acetate solution and converted to silver sulfide, which is burned to sulfur dioxide, for the isotope analysis. The relative standard deviation at the 50-p.p.m. level for 1-g samples is less than 3 %.     

Determination of trace impurities in iron and nickel-base alloys by graphite furnace atomic absorption spectrometry

Five approaches to the determination of trace amounts of lead, bismuth, thallium, selenium, tellurium, and silver in iron and nickel-based alloys were investigated. While all procedures produced satisfactory results, direct techniques yielded a significant times advantage over separation schemes. Matrix effects made calibration curves an impractical approach. A spiking technique was used to generate data on a wide range of standard alloy samples.     

Determination of boron in glass by neutron transmission method

Neutron transmission method has been used for the determination of boron in borosilicate glasses. The method is sensitive and rapid to control the spatial homogeneities of glass-product in the melting furnace.Dedicated to Academician J. Csikai on his 60th birthday.This work was supported by the National Foundation for Research (Contact No. 259).     

Determination of neodymium and boron in iron-neodymium-boron alloys by direct-current plasma atomic-emission spectrometry

Rapid, accurate methods for the determination of neodymium and boron in iron-neodymium-boron alloys are presented. The procedure involves dissolution of the alloy with nitric acid and measurement of the elemental concentrations by direct-current plasma atomic-emission spectrometry. Lithium is added in the determination of neodymium, to control interferences. The relative standard deviations are approximately 1%, and the accuracies comparable to those obtained by classical chemical methods.     

Determination of boron in silicon-bearing alloys, steel, and other alloys by pyrohydrolysis and inductively-coupled argon-plasma spectroscopy

Boron is quantitatively separated from silicon-bearing and other inorganic materials by pyrohydrolysis. Microgram amounts of boron are separated by passing oxygen-saturated steam over a sample mixed with vanadium oxide and copper oxide. The distillate is collected in dilute potassium hydroxide solution and determined by inductively-coupled argon-plasma spectroscopy.     

Determination of microgram quantities of silver in aluminium-, iron-, and nickel-base alloys

Trace quantities of silver in commercial nickel and its alloys are quantitatively extracted from 10% hydrochloric acid medium containing 2% ascorbic acid and 9% potassium iodide by a 5% solution of tri-n-octylphosphine oxide in 4-methylpentan-2-one (MIBK). The MIBK-extract containing the silver is then nebulized directly into an atomic-absorption flame. The sensitivity for the determination of silver in MIBK is about 6 times that for aqueous media. The proposed technique is accurate, rapid, and has a standard deviation of +/- 0.025 ppm at the 1 ppm level. The limit of detection is 0.2 ppm of silver. The method is also applicable to a number of elements in aluminium- and iron-base alloys.     

Correction method for X-ray fluorescent determination of chromium in high-alloy steels and nickel-base alloys

Summary A new interelement correction method has been developed for the X-ray fluorescent determination of chromium in high-alloy steels and nickel-base alloys. The calibration equation which was derived from the JIS (Japanese Industrial Standards) model is applicable over wide ranges of compositions by preparation of only Fe-Cr binary standards.The new approach gave better accuracy than that based on Rasberry-Heinrich correction model. The accuracies (_d) were 0.08% for high-alloy steels and 0.14% for nickel-base alloys.

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Korrekturmethode für die röntgenfluorescenzspektrometrische Bestimmung von Chrom in hochlegierten Stählen und Nickellegierungen

Zusammenfassung Die Eich-Gleichung für das neue Korrekturverfahren wurde vom JIS-Modell (Japanese Industrial Standards) abgeleitet und ist über einen weiten Bereich von Zusammensetzungen durch Herstellung von lediglich binären Fe-Cr-Standards einsetzbar. Das beschriebene Verfahren bietet eine bessere Genauigkeit als die Methode nach dem Korrekturmodell von Rasberry-Heinrich. Sie betrug 0,08% für hochlegierte Stähle und 0,14% für Nickellegierungen.

     

Determination of bismuth in nickel-base alloys by atomic absorption spectrometry with introduction of solid samples into an induction furnace

Atomic absorption spectrometry with an induction furnace is applicable'to the determination of bismuth at 0.02–10 μg g^-1 levels in 1–30-mg samples of nickel-base alloys dropped into the furnace. Calibration graphs of peak absorbance versus mass of bismuth are constructed by use of standardised alloys. Samples of alloys can be added to the furnace at 2.5-min intervals. Calibration graphs, accuracy, precision and limits of detection of the method are discussed for 26 alloys. Accuracy is assessed by comparing the induction furnace results with results supplied with the alloys, and with results obtained for solutions of the alloys by atomic absorption spectrometry in association with hydride generation or a mini-Massmann furnace. With alloys containing more than 0.1 μg Bi g^-1, relative standard deviations by the induction furnace method are usually < 15%. The limit of detection for bismuth is 0.02 μg g^-1     

Determination of lead in nickel-base alloys by atomic absorption spectrometry with introduction of solid samples into an induction furnace

Lead (0.2–26 μg g^?1) is determined in 1–9 mg samples of alloys dropped into the furnace. Standardized alloys were used for calibration. Data on accuracy and precision are presented for 23 nickel-base alloys.     

Determination of boron in copper and copper-, nickel- and cobalt-base alloys

Summary A pyrohydrolytic method for the extraction of boron from coppper and copper-, nickel- and cobalt-base alloys has been developed. For concentrations higher than 0.1 %, boron is determined by an alkalimetric method in the presence of mannitol and phenolphthalein or by a potentiometric method. For samples containing less than 0.1% of boron, it is determined by spectrophotometry with azomethine H. Standard deviations are in the range of 0.008 to 0.15% B.

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Bestimmung von Bor in Kupfer sowie Legierungen auf Kupfer-, Nickel- und Kobaltbasis

Zusammenfassung Zur Extraktion von Bor aus diesen Proben wurde ein pyrohydrolytisches Verfahren ausgearbeitet. Die Borbestimmung erfolgt bei Gehalten >0,1% B alkalimetrisch in Gegenwart von Mannit und Phenolphthalein oder potentiometrisch, bei Gehalten <0,1% B durch Spektralphotometrie mit Azomethin H. Die Standardabweichungen liegen im Bereich von 0,008–0,15% B.

     

Determination of boron in silicon by SIMS with the matrix ion species ratio method

Summary In quantitative SIMS, the oxygen content of the sample surface proves to be a very important analytical parameter. The matrix ion species ratio method (MISR) was used to investigate the influence of the presence of oxygen on the determination of boron in silicon. By analysing standard samples at conditions of different oxygen coverage, the relation between the sensitivity of boron and the oxygen content of the sample surface, as indexed by the SiO⁺/Si³⁺ matrix ion species ratio, was established. The influence of the primary ion current density on this relation was investigated. The MISR procedure proves to be a suitable method to perform quantitative determinations (relative error < 10%) in conditions of changing oxygen content on the sample surface.

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Bestimmung von Bor in Silicium durch SIMS mit der Matrix Ion Species Ratio Method

     

Determination of boron in glass by alpha-spectrometry

Alpha-spectrometric method has been used for the determination of boron in borosilicate glasses. For irradiation thermal neutrons with a flux of about 10⁵ n·cm^–2·s^–1, produced in a paraffin moderator surrounding a deuteron target of a small neutron generator, were used. Alpha-particles from the reaction¹⁰B(n, ) were detected by a Si solid state detector with a resolution of about 50 keV. The sensitivity of the method is 0.05 wt % boron in glass samples.This work was supported by the Hungarian Research Foundation (Contract No. 1734/91.).     

Determination of boron in soils by sequential scanning ICP-AES using side line indexing method

Summary This paper describes the method for the determination of boron in soils directly by sequential scanning ICP-AES using the side line indexing method. In order to overcome the spectral wing interference caused by iron which is the one of the major matrix constituents the side line indexing method was used, in which the B 249.678 nm line is found by referencing the side line Fe 249.653 nm. The background correction position was chosen to allow the interference from iron to be constant. The sample dissolution method was investigated to avoid losses of boron as BF₃ in the HNO₃/HClO₄/HF decomposition procedure. Instead of mannitol orthophosphoric acid was added with HNO₃/HClO₄/HF mixed acids with the result of 100% recoveries of boron. NBS SRM 1571 (Orchard Leaves) spiked with iron was used to verify the accuracy of this method.

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Borbestimmung in Böden durch Sequential Scanning ICP-AES mit Hilfe der Nebenlinien-Auswertung

Zusammenfassung Um die durch Eisen (einer der Hauptbestandteile) verursachte Störung zu überwinden, wurde das Verfahren der Nebenlinien-Auswertung eingesetzt, wobei die Borlinie 249,678 nm durch Vergleich mit der Nebenlinie Fe 249,653 nm gefunden wurde. Die Untergrundkorrektur wurde so gewählt, daß die Eisenstörung konstant war. Zur Vermeidung von Borverlusten als BF₃ beim Aufschluß mit HNO₃/HClO₄/HF wurde dem Säuregemisch an Stelle von Mannit Orthophosphorsäure zugesetzt. Dadurch konnten 100%ige Ausbeuten erzielt werden. Zur Überprüfung der Genauigkeit des Verfahrens diente das Referenzmaterial NBS SRM 1571 (Orchard Leaves) mit Zugaben von Eisen.

     

微波消解-分光光度法测定大豆中的硼量

研究了分光光度法测定大豆中的硼时样品的微波消解方法。建立了合理的分析步骤。进行了微波消解条件的选择及方法的精密度、准确度试验。试验结果表明:消解完全仅需20 min,相对标准偏差均小于7.6%,其方法的加标回收率为92%~105%。     

Determination of boron in glass by the nuclear track technique

Summary Determination of Boron in Glass by the Nuclear Track Technique The nuclear track technique using the¹⁰B(n)⁷Li reaction, has been applied to determine boron in concentration ranges (1.59 to 7.75%) ordinarily considered high for nuclear determinations. Factors limiting the overall precision of the method and restricting the linear dependence of track density on boron concentration are examined. Boron alpha track densities are used to construct planar profiles of boron distribution within the surface region of bulk glass and CVD films. Calibration curves for quantitative lateral profiling of surfaces are constructed and show the selective corrosion of borosilicate glass surface resulting in boron depletion.     

Spectrophotometric determination of cobalt in iron-, cobalt- and nickel-base alloys

A spectrophotometric method has been developed for the accurate determination of cobalt at milligram level, based on oxidation of the cobalt(II)-EDTA complex with gold(III) chloride at pH 4.0-6.5 and 100 degrees and measurement of the absorbance of the resultant violet cobalt(III)-EDTA complex at 535 nm. The precision is not affected by the presence of several metal ions; including coloured ones such as Cu(II), Ni(II) and Fe(III). However, chromium(III) interferes since it also forms a violet complex with EDTA, but can be removed by separation with pyridine. Practical application of the method is illustrated by the determination of cobalt in alloys based on iron, cobalt and nickel. Over the cobalt range 8-52% the error ranges from 0.1 to 0.3%.     

Determination of boron and nitrogen in boron nitride

Improved techniques are described for the determination of boron and nitrogen in pure boron nitride. Controlled fusion of boron nitride with sodium carbonate in a muffle furnace is followed by a potentiometric titration of the boric acid. A special quartz vessel is described for the determination of nitrogen. The boron nitride is fused with sodium hydroxide and the resulting ammonia is swept into a receiver and titrated with standard hydrochloric acid. Boron and nitrogen values with their standard deviation are given for a typical pure boron nitride.