摘要
将1g尿素水溶液样品置于烘箱105℃下浓缩,在1 100℃马弗炉中加热灰化;取出冷却,使用盐酸(1+1)溶解灰分。采用Al 237.312nm、Ca 393.366nm、Cr 267.716nm、Cu 324.754nm、Fe 238.204nm、Mg 279.553nm、Ni 231.604nm、Zn 213.856nm作为分析线,建立了使用电感耦合等离子体原子发射光谱(ICP-AES)法测定尿素水溶液中铝、钙、铬、铜、铁、镁、镍和锌8种杂质元素的方法。结果表明,铝、钙、铬、铜、铁、镁、镍和锌的线性范围在0.02-2μg/mL时,校准曲线的线性相关系数均不小于0.999 5;方法中各元素的检出限为0.001-0.010μg/mL。将方法应用于尿素水溶液样品中8种杂质元素的测定,结果的相对标准偏差(RSD,n=7)均小于5.0%,加标回收率为91%-108%。方法可一次性完成对多种元素的测定,准确度、精密度较高,方法简便快速,适用于各级检验机构进行多批次、多项目产品的元素检测。
1. 000 0 g of vehicle urea was accurately weighted and concentrated in an oven at 105℃. After cooling, the samples were heated in a muffle furnace at 1 100 ℃ until they were ashed completely. Then 20 mL HCl(1+1) was added to dissolve the ashes. The spectral lines (A1 237. 312 nm, Ca 393. 366 nm, Cr 267. 716 nm, Cu 324. 754 nm, Fe 238. 204 nm, Mg 279. 553 nm, Ni 231. 604 nm and Zn 213. 856 nm) were chosen as analytical lines, and a method for the determination of 8 impurities (Al, Ca, Cr, Cu, Fe, Mg, Ni and Zn) in vehicle urea by inductively coupled plasma atomic emission spectroscopy (ICP-AES) was established The results showed that the linear ranges of 8 impurities were 0. 02-2 μg/mL. The correlation coefficients were higher than 0. 999 5. The detection limits were 0. 001-0. 010 μg/mL. The proposed method was successfully used to determine 8 impurities in vehicle urea with satisfactory results. The relative standard deviations (RSDs, n=7) were all less than 5. 0%, and the recoveries of standard addition were 91 %-108 %. This method has some advantages (rapid, simplicity, good accuracy and high precision) for batch analysis simultaneously.
出处
《中国无机分析化学》
CAS
2016年第2期61-63,共3页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家科技部
国家重大科学仪器设备开发专项基金项目(2011YQ140147)资助