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本文研究了新显色剂5—溴水杨基荧光酮(5—Br—SAF)在阳离子表面活性剂溴化十六烷基三甲铵(CTMAB)存在下,测定微量锑的显色反应,该体系的摩尔吸光系数较高,ε=9.1×10~4,高于Sb—苯芴酮—CTMAB(ε=3.7×10~4)、Sb—5—Br—PADAP—OP(ε=4.3×10~4)、Sb—二溴苯基荧光酮—CPB(ε=5.6×10~4)、Sb—KI—SAF—乳化剂OP(ε=7.1×10~4)等体系。我们采用巯基棉分离方法,能同时消除多种金属离子的干扰,提高了体系的选择性。本法富集倍数大,用于纯锡中微量锑的测定,结果满意。 1 试验部分1.1 试剂与仪器锑标液:准确称取Sb_2O_3 0.1156g,加入浓硫酸24ml,小火加热溶解后,用盐酸(2mol·L~(-1))稀至100ml。此浓度为1.0mg.ml~(-1),临用时再稀释成5.0μg·ml~(-1)锑标准溶液。 5—Br—SAF酒精溶液:2.0×10~(-3)mol·L~(-1) CTMAB水溶液:1.0×10~(-2)mol·L~(-1) 巯基棉:按文献[5]制备 721—B型数字显示分光光度计1.2 试验方法于25ml比色管中,依次加入盐酸(5mol·L~(-1))2.00ml,一定量锑标准溶液,5—Br—SAF 1.0ml,CTMAB 3.0ml,用水稀至刻度,摇匀,于波长515nm处,用2cm比色皿,以试剂空白为参比测量吸光度。 2 结果与讨论
In this paper, the color reaction of 5-Br-SAF with 5-Br-SAF in the presence of cationic surfactant cetyltrimethylammonium bromide (CTMAB) was studied. The molar absorption coefficient of the system is higher, ε = 9.1 × 10 -4, higher than that of Sb-Benzene fluorenone-CTMAB (ε = 3.7 × 10-4) ~ 4), Sb-dibromophenylfluorone-CPB (ε = 5.6 × 10 ~ 4) and Sb-KI-SAF-emulsifier OP (ε = 7.1 × 10 ~ 4). We use the method of thiol cotton separation, which can simultaneously eliminate the interference of a variety of metal ions and improve the selectivity of the system. This method enrichment multiple, for the determination of trace antimony in pure tin, the results are satisfactory. 1 Experimental 1.1 Reagents and Instruments Antimony standard solution: Weigh accurately Sb_2O_3 0.1156g, add concentrated sulfuric acid 24ml, heated to dissolve small heat, with hydrochloric acid (2mol · L -1) dilute to 100ml. The concentration of 1.0mg.ml ~ (-1), when used and then diluted into 5.0μg · ml ~ (-1) antimony standard solution. 5-Br-SAF alcohol solution: 2.0 × 10 -3 mol·L -1 CTMAB solution: 1.0 × 10 -2 mol·L -1 thiol cotton: According to the literature [5 ] Preparation of 721-B digital display spectrophotometer 1.2 Test Method In a 25ml colorimetric tube, followed by hydrochloric acid (5mol · L -1) 2.00ml, a certain amount of antimony standard solution, 5-Br-SAF 1.0ml , CTMAB 3.0ml, diluted with water to the mark, shake, at a wavelength of 515nm, with 2cm cuvette, reagent blank as a reference to measure the absorbance. 2 results and discussion