Yatirajam V, Dhamija S
Department of Chemistry, B.N. Chakravarty University, Kurukshetra 132119, Haryana, India.
Talanta. 1977 Aug;24(8):497-501. doi: 10.1016/0039-9140(77)80033-7.
Phosphotungsten blue is produced by tin(II) reduction of tungstate solution complexed with phosphate at a w/w ratio of W/P = 5, in 4M hydrochloric acid medium, and extracted with isoamyl alcohol; thus tungsten is separated from Fe(III), Ni, Co, Cr(III), V(V), As(V), Sb(III), Bi, Si, U(VI), Ca and Cu(II). In presence of bismuth (0.5 mg/ml), 99.7% W is separated in a single extraction. After alkaline back-extraction, tungsten is determined spectrophotometrically as phosphotungsten blue; it is measured at 930 nm in aqueous solution or at 900-960 nm after isoamyl alcohol extraction, the Beer's law ranges being 0.08-0.6 and 0.16-0.72 mg/ml respectively. The methods are shown to give satisfactory results in the analysis of practical samples containing some milligrams of tungsten.
磷钨蓝是在4M盐酸介质中,以W/P = 5的重量比,用锡(II)还原与磷酸盐络合的钨酸盐溶液制得,并用异戊醇萃取;由此钨与铁(III)、镍、钴、铬(III)、钒(V)、砷(V)、锑(III)、铋、硅、铀(VI)、钙和铜(II)分离。在铋(0.5mg/ml)存在下,一次萃取可分离出99.7%的钨。经过碱性反萃取后,以磷钨蓝形式用分光光度法测定钨;在水溶液中于930nm处测量,或在异戊醇萃取后于900 - 960nm处测量,比尔定律范围分别为0.08 - 0.6和0.16 - 0.72mg/ml。这些方法在分析含几毫克钨的实际样品时显示出令人满意的结果。