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.     

A microvolumetric determination of tin in tin-base and lead-base alloys

The authors have elaborated a rapid and exact microvolumctric method fur the determination of tin in metallic tin and in tin-base and lead-base alloys.     

Chelatometric titration of tin in non-ferrous alloys with hedta

A new titrimetric method for determination of tin (4%) in aluminium alloys, tin- and lead-base alloys, solders, white bearing alloys, special bronzes and silver brazing alloys is proposed. HEDTA, Semi-Xylenol Orange and bismuth perchlorate are used as titrant, indicator and back-titrant respectively. Measures are taken to overcome the hydrolysis of Sn(IV). Monochloroacetic acid and ethylene glycol are added as auxiliary agents. The standard deviation of this method was found to be 0.2 mg and its coefficient of variation to vary from 0.25 to 2%, according to amount of tin. A novel method of sample decomposition and a modified method for separating Sn(IV) are also suggested.     

十二烷基硫酸钠—水杨基荧光酮痕量锡的光度测定

提出一种高选择性、高灵敏度吸光光度测定痕量锡的方法。试验表明阴离子表面活性剂十二烷基硫酸钠具有特殊的选择性,在十二烷基硫酸钠的存在下,锡与水杨基荧光酮在强酸性介质中形成高灵敏度的三元配合物,常见干扰离子均不发生类似的显色反应,具有很高的选择性,不需分离可直接测定钢铁样品中的痕量锡。     

Selective complexometric determination of tin, with mercaptans as releasing agents

A method is proposed for selective complexometric determination of tin, mercaptans being used as releasing agents. To a solution containing tin and other cations, excess of EDTA is added and the surplus is back-titrated at pH 5-6 with lead nitrate (Xylenol Orange as indicator). Thioglycollic acid or mercaptopropionic acid is then added to decompose the tin-EDTA complex and the liberated EDTA is titrated with lead nitrate. The interference of various cations has been studied and the method has been employed for the estimation of tin in a variety of alloys.     

三氯化钛存在下碘酸钾滴定法测定锡

提出了采用铝加铁混合还原剂还原,三氯化钛存在下碘酸钾滴定法测定锡的绝对测量方法,研究了三氯化钛抑制氧的作用效果及作用机理。应用于巴氏合金中锡含量的测定,方法简便、快速,结果准确可靠。     

Dosage colorimétrique de l'antimoine dans les zincs,aluminiums et étains et dans leurs alliages

The colorimetric method using methyl violet is applied to the determination of antimony in zinc, aluminium, tin, and in their alloys.Applying the method to the determination of small quantities of antimony, the following domains of strengths are covered : Zinc alloys : Sb < 0.015 % Aluminium alloys : Sb < 0.030 % Tin : Sb < 0.15 %The amounts of metal used in the determination can be decreased in order to raise the maximum of these strengths, and conversely the latter can be lowered, with the correlative increase in the sensitivity of the determination, increasing conveniently the importance of the aliquot parts withdrawn in the course of the analysis.     

Differential pulse polarographic determination of tin in alloys and environmental samples after preconcentration with the ion pair of 2-nitroso-1-naphthol-4-sulfonic acid and tetradecyldimethylbenzylammonium chloride onto microcrystalline naphthalene or by column method

A highly selective, sensitive, rapid and economical differential pulse polarographic method has been developed for the determination of trace amount of tin in various standard alloys and environmental samples after adsorption of its 2-nitroso-1-naphthol-4-sulfonic acid-tetradecyldimethylbenzylammonium chloride on microcrystalline naphthalene in the pH range of 8.7-10.6. After filtration, the solid mass is shaken with 8-10 ml of 3.5 M hydrochloric acid and tin is determined by differential pulse polarography (DPP). Tin can alternatively be quantitatively adsorbed on 2-nitroso-1-naphthol-4-sulfonic acid-tetradecyldimethylbenzylammonium-naphthalene adsorbent packed in a column and determined similarly. The detection limit is 0.15 mug ml(-1) (signal to noise ratio=2) and the linearity is maintained in the concentration range 0.5-220 mug ml(-1) with a correlation coefficient of 0.9995 and relative standard deviation of +/-0.88%. Characterization of the electroactive process included an examination of the degree of reversibility. Various parameters such as the effect of pH, volume of aqueous phase and interference of a number of metal ions on the determination of tin has been studied in detail to optimize the conditions for determination in standard alloys and environmental samples.     

Applications of a slotted tube atom trap and flame atomic absorption spectrometry: Determination of tin in copper-based alloys after hydride generation

A sensitive system is reported for the determination of tin in copper-based alloys by flame atomic absorption spectrophotometry. Use of a slotted quartz atom trap coupled with hydride generation improved the sensitivity by a factor of 200, compared with that obtained using conventional flame AAS. The determination of tin in a series of reference samples demonstrates the usefulness of the system for the analysis of metallurgical samples.     

Analysis of brass by anion-exchange chromatography

A method is described for the determination of each constituent in alloys of nickel, copper, lead, iron, zinc, tin, manganese and aluminum. The essential feature of the method is the separation of the constituents by anion-exchange chromatography. The separation requires only 3.5 h. The accuracy and precision are good.     

The atomic absorption determination of antimony,arsenic, bismuth, cadmium, lead, and tin in iron, copper,and zinc alloys with the graphite furnace

Antimony, arsenic, bismuth, cadmium, lead, and tin can be determined in metallurgical samples by flame atomic absorption spectrometry at levels of 0.005 wt%, but lower concentrations frequently necessitate preconcentration. The graphite furnace allows determination of these elements at concentrations 1–2 orders of magnitude lower than is possible with flame techniques. All six elements have detection limits at or below 1μg g⁻¹ in a variety of alloys. Calibration for antimony and load was done with standards containing the principal component of the alloy as a synthetic matrix. Bismuth, cadmium, and tin could be determined accurately only by the standard addition method. Arsenic could be determined in iron alloys with synthetic standards, but standard additions were required for copper alloys.     

The differential pulse polarographic determination of trace amounts of tin and its application to zinc-aluminium alloys

A differential pulse polarographic procedure for the determination of 0.001-0.02% of tin in zinc-aluminium alloys is described. The tin is first separated from interfering elements such as copper and lead by homogeneous co-precipitation with aluminium succinate. The tin is determined polarographically in a 1M hydrochloric acid + 4M ammonium chloride electrolyte. After the tin has been masked with alkaline citrate a second polarogram is recorded to ascertain whether residual lead is present and, if so, a correction is applied.     

A microanalytical volumetric method for the determination of antimony in lead-base and tin-base alloys

Indications are given for the constructions of simple and efficient immersion filters and bicarbonate valves.The authors have elaborated a rapid and exact microvolumetric method for the determination of antimony in alloys based on lead or tin, containing up to 18% antimony.     

Determination of tin in copper based alloys using a modified quartz atom-trap (STAT) and flame-atomic absorption spectrophotometry

Summary An improved system is reported for the determination of tin in copper-based alloys by flame-atomic absorption specved sensitivity and precision by factors of 2–3 compared to that obtained using conventional flame AAS. Determination of tin in a series of certified references samples demonstrates the improved precision of the proposed procedure.     

Determination of bismuth by electrochemical stripping analysis; elimination of interferences by using a mercury film electrode modified with tri-n-octylphosphine oxide, and application to copper alloys

A mercury film electrode modified with a film consisting of tri-n-octylphosphinc oxide in a poly(vinyl chloride) matrix is used for a galvanostatic stripping determination of bismuth in copper and copper alloys. The method can be used to determine from 0.002 to 0.5% of bismuth. It is very selective, simple and rapid. The precision and accuracy are good and the only serious interference is caused by tin(IV).     

Analyse des alliages légersá base d'aluminium par les méthodes spectrophotométriques II

Colorimetric methods of analysis of light alloys of aluminium have been examined by the spectrophotometric method.In particular, four methods of determination of iron have been studied. The method which makes use of sulphophenyl pyrazolone carboxylic acid is recommended; the accuracy is of the same order as that of the phenanthroline method; the reagent is a much used product and is less expensive than phenanthroline.Simple and rapid methods are proposed for the determination of chromium, cobalt and titanium, and studies have been made leading to relatively new and original techniques for bismuth, tin and zirconium.     

Spectrophotometric determination of tin in copper-based alloys using pyrocatechol violet

In the present paper, a new procedure using Pyrocatechol Violet (PCV) for the determination of tin in copper-based alloys is proposed. The use of HEDTA as masking agent allowed tin to be determined in the presence of large amounts of copper, without any separation procedure. The method is more selective than previous methods. Cetyltrimethylammonium bromide (CTAB) and Tween-20 are used to increase the stability of the system.

The method can be applied directly to an acidic solution of Sn(IV) in the range 2.0–60.0 μg with a final volume of 50 ml. The pH is adjusted to 2.0 ± 0.2 with glycine buffer and, after 30 min, the absorbance is measured at 660 nm. Al(III), Cd(II), Co(II), Mg(II), Ca(II), Mn(II), Ni(II) and Pb(II) do not interfere at the 500 mg level; 20 000 μg of Cu(II) and 400 μg of NaCl can be present. The interference at 100 μg of Fe(III) can be masked with ascorbic acid. Bi(III), Sb(V), Ti(IV), Mo(VI), EDTA, tartrate, citrate and iodide interfere. The proposed method was used for tin determination in several copper-based alloys and a comparison of the analytical results with certified values indicates that the procedure provides accurate and precise results.     

Quantification of Tin and Lead in Binary Alloys Using Voltammetry of Immobilized Microparticles

Voltammetry of immobilized microparticles (VMP) has been used in this work for the quantitative determination of tin and lead particles in their binary alloys. Carbon paste electrodes, which contained small amounts of tin and lead or their mixtures, were used as working electrodes and square wave voltammograms of each electrode were recorded. Quantification was performed using optimum experimental conditions, obtained by an experimental design technique. The calibration was made by measuring the percentage peak height of each metal taking the sum of peak currents of the both metals as 100 %. The results were compared with quantitative results of X‐ray fluorescence (XRF) technique to evaluate the capability of VMP method in its quantitative determination of solid samples.     

The accurate determination of bismuth in lead concentrates and other non-ferrous materials by AAS after separation and preconcentration of the bismuth with mercaptoacetic acid

A method for determining 0.0001% and upwards of bismuth in lead, zinc or copper concentrates, metals or alloys and other smelter residues is described. Bismuth is separated from lead, iron and gangue materials with mercaptoacetic acid after reduction of the iron with hydrazine. Large quantities of tin can be removed during the dissolution. An additional separation is made for materials high in copper and/or sulphate. The separated and concentrated bismuth is determined by atomic-absorption spectrometry using the Bi line at 223.1 nm. The proposed method also allows the simultaneous separation and determination of silver.     

Atomic-absorption spectrophotometric determination of tin by hydride generation in non-aqueous medium after extraction

Tin at the microgram level was extracted into chloroform with N-nitrosophenylhydroxamic acid (ammonium salt) from 0.5-1.5M hydrochloric acid medium. Tin hydride was generated from 1 ml of the chloroform extract mixed with 3 ml of 1% sulphuric acid solution in N,N-dimethylformamide. by injection of 3 ml of 2% sodium tetrahydroborate solution in N,N-dimethylformamide through the septum of the hydride generator. Tin was then determined by AAS at 224.6 nm with an acetylene-air flame, and nitrogen as carrier gas. The peak-height of the signal was linearly related to amount of tin up to 20 mug. The sensitivity of the determination was improved by the extraction. The method was applied to determination of tin in tinned foods and aluminium-base alloys with good accuracy and precision.