The accurate determination of antimony in steel is important to the steel industry, because grain boundary segregation of antimony causes the decrease in toughness of steel owing to the temper embrittlement. Spectrometric methods 1,2 are commonly used for the determination of antimony in iron and steel, but they require a preconcentration procedure, which generally involves much skill, labor or time, and the use of toxic organic solvents such as toluene, 1 to avoid any interference from iron matrix. Furthermore, the methods exhibit poor sensitivity.Stripping voltammetry is a powerful electroanalytical technique for the determination of trace antimony and has been extensively applied in studying antimony in various samples. It includes anodic stripping voltammetry (ASV) at mercury, [3][4][5][6][7][8][9][10][11][12][13][14][15][16][17][18][19][20] Only a few papers have been published to date on the stripping voltammetric determination of antimony in steels. [33][34][35] Wang et al. 33 and Hofbauerova et al. 34 used ASV at mercurybased electrodes in a hydrochloric acid-alcohol medium for the determination of antimony in steels. Zhou et al. 35 developed 1.5th-order derivative linear-sweep adsorptive stripping voltammetry of antimony(III) complexed with morin (2′,3,4′,5,7-pentahydroxyflavone) at a static mercury drop electrode. However, those methods involve a troublesome procedure such as filtration or require a time-consuming and laborious standard additions method because of removing interferences from coexisting elements. Furthermore, mercury, which is toxic and difficult to use, is employed exclusively as the working electrode.The present paper describes a simple, rapid and accurate method for the direct determination of antimony at trace levels in steel based on ASV of antimony(III) at a gold film electrode without any preconcentration step.
Experimental
ApparatusVoltammetric determinations were performed using a BAS-50W electrochemical analyzer with an RDE-1 rotating disk electrode (Bioanalytical Systems, West Lafayette, IN, USA) and a BJC-240J printer (Canon, Tokyo, Japan). A platinum wire was used as a counter electrode. A saturated calomel reference electrode (SCE) was connected to a glass voltammetric cell (25 mm×22 mmφ) by a 4% agar-saturated potassium nitrate bridge.
ReagentsKanto Chemicals "Ultrapure" grade mineral acids were used throughout, and other chemicals were of analytical-grade without further purification. Water was distilled from a vitreous silica sub-boiling still. An acid mixture solution was prepared by mixing one volume of 10 mol dm -3 nitric acid and one volume of 10 mol dm -3 sulfuric acid. Standard antimony(III) solutions were prepared daily by diluting a commercially available stock standard solution (1 mg cm -3 of animony(III) in 2.5 mol dm -3 hydrochloric acid) to the desired concentration with the acid mixture solution.
Preparation of gold plated glassy-carbon electrodeThe surface (7 mm 2 area) of a glassy carbon disk electrode (Bioanalytical Systems) was polished to a mirror fin...