Wu X L, Mu B C, Yang G Q, Huang X F
Department of Material and Chemical Engineering, Liaoning Institute of Technology, Jinzhou 121001, China.
Se Pu. 2001 Sep;19(5):472-4.
The reversed-phase ion pair high performance liquid chromatographic determination of scandium, tin and aluminum with diammonium stilbene-4,4'-bis(1-azo)-3,4-dihydroxybenzene-2,2'-disulfate as precolumn chelating reagent on Spherex C18 column has been investigated with the detection wavelength of 500 nm. Various parameters such as pH, reagent concentration, ion pair reagents, interference of foreign ions have been studied. The mobile phase was methanol-water (40:60, V/V) containing 20 mmol/L acetate buffer of pH 6.0 and 10 mmol/L sodium dodecyl sulfonate. Three complexes could be completely separated within 17 min. The method has been successfully used for the determination of the three metals in mineral samples, with recoveries of 98%, 101%, 103% respectively, and RSD was less than 3.6%. Beer's Law was obeyed over the concentration range 0.01 mg/L-3.80 mg/L, 0.06 mg/L-4.50 mg/L and 0.04 mg/L-3.40 mg/L respectively. The detection limits were 0.9 microgram/L, 1.0 microgram/L and 1.2 micrograms/L for scandium, tin and aluminum when the ratio of signal to noise was 3. Most of other metals did not interfere with the determination. The present method is sensitive and selective.
研究了以二铵基芪-4,4'-双(1-偶氮)-3,4-二羟基苯-2,2'-二硫酸盐为柱前螯合试剂,在Spherex C18柱上反相离子对高效液相色谱法测定钪、锡和铝,检测波长为500nm。研究了pH值、试剂浓度、离子对试剂、外来离子干扰等各种参数。流动相为甲醇-水(40:60, V/V),含有pH 6.0的20 mmol/L醋酸盐缓冲液和10 mmol/L十二烷基磺酸钠。三种配合物可在17分钟内完全分离。该方法已成功用于矿物样品中三种金属的测定,回收率分别为98%、101%、103%,相对标准偏差小于3.6%。钪、锡和铝分别在0.01 mg/L - 3.80 mg/L、0.06 mg/L - 4.50 mg/L和0.04 mg/L - 3.40 mg/L浓度范围内符合比尔定律。当信噪比为3时,钪、锡和铝的检测限分别为0.9 μg/L、1.0 μg/L和1.2 μg/L。大多数其他金属不干扰测定。本方法灵敏且具有选择性。