Magnetic Mercury Cathode

Overbeck, R; Chase, D.L.

doi:10.1021/ac60056a024

Cited by 22 publications

(3 citation statements)

References 8 publications

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“…The rate a t which iron is deposited in a mercury-cathode cell is favorably affected by the use of fresh mercury, a low concentration of sulphuric acid, , agitation of the mercury, and by the proper choice of spacing for the anode relative to the cathode (1,5,14,15,17). The rate of iron removal increases with increasing current density, but care must be taken to prevent undue boiling of the solution.…”

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

confidence: 99%

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

confidence: 99%

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

Graham¹,

Hitchen²,

Maxwell³

1952

Can. J. Chem.

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“…Magnetic stirring with a water-cooled bath w'as found greatly to facilitate separation of iron from such elements as aluminum with the mercury cathode and improved apparatus was designed to effect this separation (42). Facilities necessary for electrolytic separation were described by Ashley (10).…”

Section: Analytical Separationsmentioning

confidence: 99%

Ferrous Metallurgy

Beeghly¹

1952

Anal. Chem.

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“…of the sulfuric acid is evaporated off. On cooling, the contents of the beaker are washed out quantitatively into a cell of the mercury cathode electrode for removal of iron as described by Center, Overbeck, et al (1951). This step may not be necessary if the iron is present at concentrations below 10 times that of the beryllium in the sample or in the diluted sample in the case of high concentrations of beryllium.…”

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confidence: 99%

Gas chromatographic determination of beryllium in biological materials and in air

Noweir¹,

Cholak²

1969

Environ. Sci. Technol.

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The gas chromatographic determination of ultratrace quantities of beryllium in urine, blood, tissue, and air-borne dust is described. Except for air-borne dust, the procedure involves a doiible extraction, first with acetylacetone in benzene and then with a benzene solution of trifluoroacetylacetone. Beryllium in air-borne dust is extracted only by trifluoroacetylacetone in benzene. Levels as low as 1 X 10"10 gram (0.0001 µg.) of beryllium per sample can be determined by this method. Except for Fe3+ and Al3+, none of the ions usually present in air-borne dust or biological material interferes with the analysis. Fe3+ is removed in a magnetic mercury cathode. Al3+ can be precipitated with 8-quinolinol in chloroform. Recovery of beryllium ranged from 70 to 90% at levels from 1 X 10-9 gram (0.001 µg.) to 1 X 10~7 gram (0.10 µg.) per sample. The method is reliable, as shown by the results of analysis of air-borne dust and lung tissues. Beryllium has been determined in air-borne dusts and biological materials using colorimetric, fluorometric, or spectrographic methods (Cholak, 1959; Smythe and

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Magnetic Mercury Cathode

Cited by 22 publications

References 8 publications

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

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

Ferrous Metallurgy

Gas chromatographic determination of beryllium in biological materials and in air

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