萘相-分光光度法测定原油中痕量镍  

Naphthalene Phase-Spectrophotometric Determination of Trace Amount of Nickel in Crude Oil

作　　者：张维 沈春玉[2] 

机构地区：[1]石油化工学院 [2]化学与材料科学学院辽宁石油化工大学,抚顺113001

出　　处：《理化检验（化学分册）》2010年第9期1013-1014,1017,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

摘　　要：取原油样品(1.0 g)在电炉上加热,使完全燃烧,移入高温炉中在650℃灰化4.5 h,所得灰分溶于稀硝酸中,定容为25 mL。分取部分试液,于pH 10.0的氨性缓冲溶液中加入丁二酮肟(DMG)显色剂并加水至50 mL,使与镍(Ⅱ)生成镍(Ⅱ)-DMG络合物。在快速搅拌下,加入300 g.L-1萘丙酮溶液3.0 mL,使上述镍(Ⅱ)-DMG络合物完全吸附于析出的微晶萘之上。所得析出的呈微晶萘经自然干燥后转移至0.5 cm吸收皿中,以空白为参比,在548 nm波长处测得其吸光度。镍浓度在400μg.L-1以内的范围内符合朗伯-比耳定律。测得镍(Ⅱ)-DMG络合物在萘相中的摩尔吸光率为6.98×104L.mol-1.cm-1。The crude oil sample（1.0 g） was burned completely on hot-plate and then ashed in muffle furnace at 650 ℃ for 4.5 h.The ash was dissolved in dil.HNO3,evaporated to near dryness and diluted to 25 mL.Nickel（Ⅱ） in an aliquot of the solution was reacted with dimethylglyoxime（DMG） in an ammoniacal buffer of pH 10 and the solution was diluted to 50 mL.Three mL of 300 g·L^-1 naphthalene-acetone solution were added to the solution under rapid stirring to have the complex of Ni（Ⅱ）-DMG adsorbed completely on the microcrystalline naphthalene which separated out from solution quicely.The colored microcrystalline naphthalene was air-dried and transferred to a 0.5 cm absorption cell,and its absorbance measured at 548 nm with reference to a blank.Lambert-Beer′s Law was kept in the range within 400 μg·L-^1.Apparent molar absorptivity of the Ni（Ⅱ）-DMG complex in the naphthalene phase was found to be 6.98×10^4L·mol^-1·cm^-1.

关 键 词：萘相-分光光度法 镍(Ⅱ) 丁二酮肟 原油 

分 类 号：O657.32[理学—分析化学]