Removal of Metals at Mercury Cathode

Parks, T. D.; Johnson, H. O.

doi:10.1021/ac60014a013

Cited by 26 publications

(24 citation statements)

References 7 publications

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“…For the determination of lead in organic samples, the organic material is removed by wet oxidation, the precipitated lead sulfate is dissolved in 1 Ñ hydrochloric acid, an4 the lead ion is determined polarographically using a potential range of -0.2 to -0.6 volt. In the procedure for the determination of sodium, most of the interfering elements are removed by means of the mercury cathode (7, 23), and the remainder are removed by treatment with ammonium carbonate and ethyl alcohol. The sodium is then determined polarographically using tetraethylammonium hydroxide as the supporting electrolyte (31).…”

Section: Polarographic Methodsmentioning

confidence: 99%

Potentiometric, Amperometric, and Polarographic Methods for Microanalysis

Parks¹

1950

Anal. Chem.

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A review is given of various practical methods for the microdetermination o f common constituents in petroleum products by potentiometric, amperometric, and polarographic means. A brief description or mention is included of the equipment used in these methods, together with typical applications to microanalysis. Methods are outlined for the determination of acidity, basicity, saponification number, and halogens .by potentiometric titration; sulfate ion, halogens, silver, lead, iron, and copper by amperometric titration; and lead, aluminum, and sodium by polarographic analysis.ANY investigators have, recognized the value of electro-M metric methods in the determination of small amounts of material (3, 6, 9, 10, 28, 89, 30). Benedetti-Pichler, for example, points out the general advantages of a potentiometric end point in microanalysis when dealing with colored or very dilute solutions ( 3 ) . Stock (89) recently reviewed microchemical applications of potentiometry with emphasis on special apparatus used for very small volumes (drop-scale analysis). Polarographic methods are inherently suited to microchemical VI ork bzcaiise they utilize dilute solutions (10-0 to lo-* molar). Majer has described various cells for the polarographic examination of very small volumes of solution (81 ). Amperometric titrations, either a t a dropping mercury or a rotating platinum electrode, are useful in the analysis of small volumes of dilute solutions (28).

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Section: Polarographic Methodsmentioning

confidence: 99%

Potentiometric, Amperometric, and Polarographic Methods for Microanalysis

Parks¹

1950

Anal. Chem.

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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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“…Electrolytic separations with a mercury cathode have also been recommended by Johnson, Weaver, and Lykken (38), who developed a convenient immersion type of mercury cathode, and by Rabbitts (93), who described an improved form of the Melaven type cell. The optimum conditions for the removal of such metals as iron, copper, zinc, nickel, cobalt, chromium, lead, tin, and molybdenum by constant current electrolysis with a mercury cathode have been studied by Parks, Johnson, and Lykken (90).…”

Section: Electrolytic Separations Prior To Polarographic Analysismentioning

confidence: 99%

Polarographic Theory, Instrumentation, and Methodology

Lingane¹

1949

Anal. Chem.

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Removal of Metals at Mercury Cathode

Cited by 26 publications

References 7 publications

Potentiometric, Amperometric, and Polarographic Methods for Microanalysis

Potentiometric, Amperometric, and Polarographic Methods for Microanalysis

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

Polarographic Theory, Instrumentation, and Methodology

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