Determination of Titanium in Rocks and Minerals. Mercury Cathode Polarographic Method

Graham, R. P.; Maxwell, J.A.

doi:10.1021/ac60056a020

Cited by 3 publications

(4 citation statements)

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“…When the results were considered in groups of 40, i.e., all the results for a given aliquot grouped together, the standard deviations in the six sets of this kind of measurement ranged from 0.7 to 1.1 mm., with an average standard deviation of 0.8 mm. These deviations are akin to those found for similar measurements in an earlier study (4).…”

Section: Accuracy and Precisionsupporting

confidence: 86%

“…Electrolysis in a mercury-cathode cell has subsequently been used widely to separate interfering elements before the determination of titanium by colorimetric or gravi~netric methods, e.g., in the determination of titanium in ores (18), in rocks and minerals (4), in ferro-titanium (19), in nickel-base alloys (13), in chromium steels (6), and in high-temperature (20) and other alloys (2,22). We have made careful wave-height measurements on polarograms given by both electrolyzed and nonelectrolyzed aliquot portions of a solution of titanium and the data (240 wave-height measurements by two readers) confirm the view that titanium is quantitatively retained in the electrolyte during electrolysis with a mercury cathode.…”

Section: Removal O F I N T E R F E R E N C E Smentioning

confidence: 99%

“…(See Table 111 in which are given the percentages of the constituents, other than titanium, which are present in one alloy or another t o an extent greater than O.l%.) We have s~iccessfully analyzed samples of stainless steel type 321 by this method and have found it applicable to a wide variety of rocks and minerals (4). We are now investigating the usefulness of the method in the analysis of high-temperature alloys.…”

Section: Applicationsmentioning

confidence: 99%

“…Recent work in this laboratory on the polarographic deternliilation of titanium in rocks and minerals (4) has shown that very good polarographic waves for titanium are obtained in a medium containing tartaric acid, sulphuric acid, and ammonium sulphate. Interfering ions are removed by prior electrolysis of the solution in a mercury-cathode cell.…”

Section: Introductionmentioning

confidence: 99%

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The Polarographic Determination of Titanium in Steels and Nickel-Base Alloys

Graham¹,

Hitchen²,

Maxwell³

1952

Can. J. Chem.

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Titanium in steels and nickel-base alloys can conveniently be determined polarographically after electrolysis of a solution of the alloy in a n~ercur)l-cathode cell. A well-formed wave, the height of which is directly proportional to the concentration of titanium in the solution, is recorded using a supporting electrolyte that is 1.0 111 in tartaric acid, 0.5 AT in sulphuric acid, and 1.2 n/f in ammonium sulphate.The method is one of good precision arid yields values in excellent agreement with those given by umpire methods for samples of basic ope~l-hearth steel, 18-11 chromium-nickel steel, Monel, Inconel "W", and Nimonic 75 and 80. INTRODUCTIONThe only earlier work on the polarographic determination of titanium in metallurgical products appears to be that of Zan'ko, Geller, and Nilcitin (25) who proposed a method for the determination of this element in cast irons and steels. They report the determination of titanium in an acid tartrate medium after treating a solution of the alloy with aluminum dust. We have not been able to remove the interference of iron (111) by the use of this reducing agent; furthermore, the introduction of an appreciable concentration of aluminum ion is undesirable (3).Recent work in this laboratory on the polarographic deternliilation of titanium in rocks and minerals (4) has shown that very good polarographic waves for titanium are obtained in a medium containing tartaric acid, sulphuric acid, and ammonium sulphate. Interfering ions are removed by prior electrolysis of the solution in a mercury-cathode cell. The application of such a method t o the determination of titanium in steels and nickel-base alloys is discussed in the present paper. REMOVAL O F I N T E R F E R E N C E SBecause the half-wave potential for copper (11) in an acid tartrate medium is less negative than that of titanium, there is a limit to the concentration of copper that can be present without the occurrence of interference in the polarographic determination of titanium. Iron (111) also constitutes an interference (23). Electrolysis in a mercury-cathode cell is a very convenient and efficient way of removing from solution iron, copper, and nickel-and a score of other elements (12)-all without the introduction of foreign salts, and often in less time than that required by other procedures. In such an electrolysis chromium is not easily removed quantitatively but the chromium remaining in solution causes no interference in the determination of titanium, even in alloys high (20%) in chromium. The chromium content of the solution being polarographed should be Manuscript received Febrzrary 25, 1952.

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Section: Accuracy and Precisionsupporting

confidence: 86%