Rameshwar DASS, Jitander Kumar KAPOOR, Sunita GAMBHIR

Spectrophotometric determination of molybdenum using surfactant-mediated liquid--liquid extraction

A new spectrophotometric method has been developed for determination of molybdenum using surfactant-mediated liquid--liquid extraction. Molybdenum(V) obtained by ascorbic acid reduction in 2.5 M H2SO4 reacted spontaneously with thiocyanate and cetyl trimethyl ammonium bromide (CTAB), forming an intense orange yellow complex that was extracted quantitatively into 1,2-dichloroethane and absorbed at 460 nm. The absorbance of the extract was found to be stable for more than 24 h. Beer's law was obeyed over the concentration range 0.1--4.2 m g Mo mL-1 of the extract. The linear range for an accurate determination was found to be 1.2--2.6 m g Mo mL-1. The molar absorptivity and LOD of the procedure were 4.01 \times 104 L mol-1 cm-1 and 0.00239 m g Mo mL-1, respectively. The stoichiometry of the orange yellow complex (Mo:SCN:CTAB) was found to be 1:3:2. The effect of a large number of cations, anions, and complexing agents was studied. For 10 replicate determinations of 1 m g Mo mL-1, the standard deviation was 0.014 concentration units with a relative mean error of \pm 0.38%. The method developed was applied for determination of molybdenum in various alloy steels and a wide variety of biological and environmental samples, including different types of water samples.

Anahtar Kelimeler:

Molybdenum, thiocyanate, spectrophotometry, extraction, cetyl trimethyl ammonium bromide, 1, 2-dichloroethane

Spectrophotometric determination of molybdenum using surfactant-mediated liquid--liquid extraction

Keywords:

Molybdenum, thiocyanate, spectrophotometry, extraction, cetyl trimethyl ammonium bromide, 1, 2-dichloroethane,

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number Mo(VI), HCl, SCN – , SnCl 2 i) Isopentyl alcohol ii) 467 i) 37 10 4 ii) 0.007 --27 Mo(VI), H 2 SO 4 , thiourea, KSCN i) --ii) 460 i) 96 10 4 ii) --0–0 30 Mo(V), SCN – , 2,2’-dipyridyl i) Chloroform ii) 505 i) 24 10 4 ii) 0.0075 0–0 31
Mo(VI), HCl, SCN – , pyridinethiosemicarbazone i) CHCl 3 ii) 470 i) 7 10 4 ii) 0.0056 0.1–5 32
Mo(V), HCl, SCN – , N 1 -OH-N’-N 2 diphenylbenzamidine i) Amyl alcohol in benzene ii) 470 i) 31 10 4 ii) --0.5–6 33 Mo(VI), H 2 SO 4 , ascorbic acid, KSCN, CTAB i) 1,2-Dichloroethane ii) 460 i) 01 10 4 ii) 0.00239 0.1–2 Proposed method Acknowledgments
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