Controlled-Potential Coulometric Titration of Antimony

Journal Article · Sat Mar 31 23:00:00 EST 1962 · Analytical Chemistry

DOI:https://doi.org/10.1021/ac60184a016· OSTI ID:4797141

Dunlap, L. B.; Shults, W. D.

BS>Two procedures were developed for the determination of antimony by controlled-potential coulometric titration. The first method involves reduction of Sb(III) to Sb(Hg) at a mercury cathode controlled at -0.28 volt vs S.C.E. in a supporting electrolyte of 0.4M tartaric acid (H₂C₄ H₄O₆) and approximately 1M HCl. Antimony(V) must be reduced to the trivalent state prior to electrolysis; hydrazine hydrate is a satisfactory reductant. The second procedure involves electrolytic reduction of Sb(V) to Sb(III) and of Sb(III) to Sb(Hg), at --0.21 volt and -0.35 volt vs S.C.E., respectively, in a supporting electrolyte containing 0.4M tartaric acid and 6M HCl. It is therefore possible to determine each oxidation state, as well as total antimony, by this method. Each procedure is characterized by a relative standard deviation of about 0.5% at the 5-mg level. Reasonable amounts of As, Pb, Sn, Fe, Ni, and U do not interfere, or their interference can be eliminated easily.

• Research Organization: Oak Ridge National Lab., Tenn.
• Sponsoring Organization: USDOE
• NSA Number: NSA-16-012964
• OSTI ID: 4797141
• Journal Information: Analytical Chemistry, Journal Name: Analytical Chemistry Journal Issue: 4 Vol. 34; ISSN 0003-2700
• Publisher: American Chemical Society (ACS)
• Country of Publication: Country unknown/Code not available
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
ANTIMONY
ANTIMONY COMPOUNDS
CATHODES
COULOMETRY
ELECTRIC POTENTIAL
ELECTROLYSIS
ELECTROLYTES
ERRORS
HYDRAZINE
HYDROCHLORIC ACID
INTERFERING ELEMENTS
MERCURY
ORGANIC ACIDS
QUALITATIVE ANALYSIS
QUANTITATIVE ANALYSIS
REDUCTION
TARTARIC ACID
TITRATION