金属服装附件及仿真饰品中镍的快速比色检测法  

Rapid Colorimetric Detection of Nickel in Metallic Clothing Accessories and Imitative Ornaments

作　　者：高永刚[1] 叶曦雯[1] 牛增元[1] 张艳艳 李引[1] 

机构地区：[1]山东出入境检验检疫局技术中心,青岛266003 [2]青岛市产品质量检验技术研究所,青岛266022

出　　处：《理化检验（化学分册）》2013年第10期1196-1198,共3页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家质检总局课题(2006IK085)

摘　　要：应用在氧化剂存在下,镍(Ⅳ)离子在氨性介质中与丁二酮肟试剂形成水溶性络合物的显色反应作为金属服装附件及仿真饰品中镍的快速检测方法。将小体积样品置于离心管中,加入6 mol·L^(-1)盐酸溶液0.5 mL,振摇30 s;对体积较大样品,可用同量盐酸溶液逐滴滴加于样品表面淋洗30 s。从浸取的酸液中移取0.15 mL置于微量离心管中,依次加入40 g·L^(-1)过硫酸铵溶液1滴,300 g·L^(-1)酒石酸钠溶液1滴及10 g·L^(-1)丁二酮肟-氨水溶液3滴。如样品中有镍存在,则呈现橙红色;如无明显颜色变化,表明此样品含镍低于0.2μg·cm^(-2),则判定为合格品。The color reaclion between Ni（Ⅳ） and dimcthyglyaxime in an ammoniacal mcdium and in the presence of an oxidant to give a water soluble complex was applied to the apid colorimelric detection of nickel in metallic clothing accessories and imitative ornamenls. Sample with small size was shaked with 0.5 mL of 0. 6 mol·L^-1 HCl solution in a lesl tube for 30 s; for sample with large size, same amount of lhe HCl solution was added dropwise directly onto the surface of sample and rinsed for 30 s. An aliquot of 0. 15 mL of the HCI extract was taken find placed in a micro test tube, and it was reacted with 1 drop each of 40 g ·L^-1 （NH4）aS2O8 solution and 300 g ·L^-1 sodium tartrate solution, and 3 drops of 10 g ·L^-1 ammoniacal solution of dimethylglyaxime. A reddish orange coloration was observed if Ni ion was present in the extract; and if Ni ion was not present, or more strictly the content of Ni was lower than 0.2 μg·cm^-2, no significant color change was observed, and the sample was proved as up to standard.

关 键 词：镍的检测 丁二酮肟 服装附件 仿真饰品 

分 类 号：O657.32[理学—分析化学]