Maurice Codell

Colorimetric determination of tantalum in titanium alloys

Abstract Experimental work on tantalum-titanium alloys has been handicapped by the lack of accurate methods for the determination of the tantalum. In this paper a colorimetric procedure is proposed for the determination. The tantalum is separated completely from the titanium by two tannin precipitations with an intervening digestion with tannin. The tannin precipitate is ignited, fused with potassium bisulfate and the melt taken up with ammonium oxalate solution. Pyrogallol is then added and the intensity of the yellow color is measured. A study was made of the tantalum pyrogallol color to obtain optimum conditions. Elements that would be found in the usual tantalum-titanium alloys do not interfere with the method. More than 0.0025 gram of niobium interferes by cauaing occlusion of titanium by the tannin precipitate. This causes high results for tantalum, since titanium reacts with pyrogallol to produce a yellow color. The presence of more than 0.0050 gram of tungsten causes high results for tantalum because tungsten is partially precipitated by the tannin and reacts with pyrogallol to produce a yellow color. The proposed method is recommended for tantalum-titanium alloys containing 0.05 to 5 percent, tantalum.

Colorimetric determination of niobium in titanium alloys

Abstract There is need for a method for the determination of niobium in titanium alloys, since niobium-titanium alloys are becoming increasingly important. The determination of niobium in this type of alloy is an extremely difficult matter. Many approaches were tried before the problem was solved. In the method proposed in this paper the sample is dissolved in a mixture of hydrofluoric and nitric acids, the solution evaporated to a small volume, and boric acid added. Two tannic acid separations are then made to separate the niobium from the bulk of the titanium. The niobium, is determined colorimetrically by the thiocyanate method using a water-acetone medium. A study was made of the possible interference of elements that might be present in titanium alloys. It was found that the presence of tantalum causes two opposing tendencies. Tantalum can cause high results for niobium because it forms a complex with thiocyanate which is visually colorless but shows some absorption. Tantalum can cause low results for niobium by hindering the development of the niobium color. The resultant effect of the tantalum depends upon the amount of tantalum present, the amount of niobium present and the ratio of tantalum to niobium. The presence of more than one per cent. tungsten can lead to high results for niobium. Other elements that might be present in titanium alloys do not interfere with the method. The procedure is designed for titanium alloys containing 0.05 to 10 per cent. niobium. The method is reasonably rapid. Six determinations can be finished in two days. The method should be applicable to many other materials besides titanium alloys.

Polarographic determination of aluminum in titanium alloys

Abstract Considerable interest has been shown in titanium metal because of its combination of desirable properties, including its favorable strength to weight ratio and its resistance to corrosion. Since titanium-aluminum alloys are fairly common, there is need for an accurate method of determining aluminum over a wide range of concentrations. This paper describes an accurate and fairly rapid polarographic method for determining aluminum based on the reduction of an aluminum-azo dye complex after removing titanium, and other interferences by cupferron precipitation, followed by electrolysis at a mercury cathode when necessary. The reduction takes place at — 0.44 volt versus the saturated calomel electrode in a solution buffered at pH 4.6 with acetate. The method is sensitive from 0.01 mg to 0.50 mg of aluminum per 50 ml, covering a range of 0.005 to 10.0 per cent aluminum.

DETERMINATION OF BORON IN TITANIUM ALLOYS BY MEANS OF ION EXCHANGE

Abstract 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.

The determination of nitrogen in copper-titanium alloys

Abstract An experimental program on the casting of copper-titanium alloys is being conducted in this laboratory. It was suspected that nitrogen was absorbed from the atmosphere during these casting operations and possibly caused embrittlement of these alloys. An accurate means of determining nitrogen in copper-titanium alloys was therefore necessary. A rapid and accurate method is proposed for determining nitrogen in copper-titanium alloys which is satisfactory for quantities of nitrogen as low as 0.01 per cent. In the development of the procedure, a study was made of possible digestion solutions. A moderately concentrated solution of perchloric acid was found to be most practical for decomposing the sample. When solution of the sample is completed, the mixture is transferred to the flask of a micro-Kjeldahl dihtillation apparatus. Sodium hydroxide is added until the solution is distinctly alkaline, and the liberated ammonia is steam distilled into a solution of boric acid and titiated with standard acid.

COLORIMETRIC DETERMINATION OF CHROMIUM IN TITANIUM ALLOYS

Abstract Chromium-titanium alloys are becoming increasingly important because of their strength and corrosion, resistance. Therefore, accurate methods for the determination of chromium in this type of alloy are needed. A colorimetric procedure for the determination of chromium in titanium alloys is proposed. In this method the chromium is oxidised to the chromate state by means of ammonium persulfate and potassium permanganate in the presence of silver nitrate as a catalyst. Diphenylcarbazide is then added to an aliquot of the solution, and the violet color read in 10 to 40 minutes at 580 millimicrons. None of the elements found in commercial titanium alloys, including iron, vanadium, molybdenum, and tungsten, interferes with the method. The proposed method is superior to the volumetric method for the determination of small amounts of chromium. The method is designed for titanium. alloys containing 0.02 to 4 per cent chromium.

Colorimetric determination of iron in titanium alloys

Abstract There is need for an improved method for the determination of iron in titanium alloys. In this paper a colorimetric method using o -phenanthroline is proposed. The method is applicable to the range of 0.02 to 9 per cent. iron. Two modifications of a basic procedure are described. One modification, applicable to ordinary titanium alloys, is a direct method. A second modification, applicable to alloys containing large amounts of certain alloying elements, calls for a prior separation of the iron by an ether extraction. In a direct method a one gram sample is dissolved in hydrochloric acid and an aliquot of the solution taken. Hydroxylamine and ammonium tartrate are added, the pH of the solution is adjusted by the addition of sodium acetate, and o -phenanthroline added. A study was made to find the best pH and optimum amount of o -phenanthroline for the development of the color.

COLORIMETRIC DETERMINATION OF CARBON IN TITANIUM

Abstract A method is proposed for the colorimetric determination of carbon in titanium. In the method the sample is dissolved in a mixture of sulfuric and fluoboric acids, and nitric acid is added to dissolve the titanium carbide. The solution is boiled and filtered, and the yellow coloration from the nitrated organic complex is read with a spectrophotometer. A spectrophotometric study of the color was made. A comparison was made between the colorimetric determination of carbon in titanium and the colorimetric determination of carbon in steels. The proposed method is rapid and is readily adaptable to the determination of carbon in a large number of samples at one time. The procedure is designed for titanium containing up to 0.7 per cent. carbon. None of the elements encountered in “commercially pure” titanium metal interferes.

Determination of tin in titanium alloys

Abstract 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 hydrogen in magnesium by combustion

Abstract The difficulties of determining hydrogen in magnesium are discussed An improved combustion method is proposed. An all glass apparatus is used to reduce the blank to 0.1 mg or less. Up to a 15 g sample can be combusted by placing the sample in a large porcelain or alumina boat which is then inserted in a sillimanite protective tube. Argon is used to control the combustion and prevent suck back of gases from the laboratory atmospheric, which frequently contains hydrogen and hydrogen compounds It is essential that the boats be pie-ignited at1100°C and stored in a muffle at 500°C.