应用1-(2-吡啶偶氮)-2-萘酚(简写作PAN)-镍(Ⅱ)共沉淀体系,以锰(Ⅱ)为内标,在pH9的氨性缓冲溶液中对食盐中痕量铅(Ⅱ)进行快速共沉淀富集,并用火焰原子吸收光谱法测定铅的含量,对共沉淀条件作了优选。在优化的条件下,试液中作为内标的锰(Ⅱ)及铅(Ⅲ)离子均定量地与PAN—Ni(Ⅱ)共沉淀析出。锰(Ⅱ)、铅(Ⅱ)及镍(Ⅱ)均匀地存在于沉淀中,而且在铅(Ⅱ)、锰(Ⅱ)之间或镍(Ⅱ)、锰(Ⅱ)之间存在着一定的比例关系。因此,根据共沉淀中铅(Pb1)及锰(Mn1)的吸光度APb1,AMn0,的比值即可求得铅的含量(w%),原试样中铅含量(Pb0)可由下式计算:mPb0=APb2/AMn1·mMn0。试验结果表明,经过共沉淀分离,基体干扰已予消除。此方法的检出限为3.18×10^-2mg·L。应用于3种不同来源的食盐的分析,算得铅含量测定值的RSD(n=6)均小于4.3%,回收率测得值在95.4%至101.6%之间。
Trace amounts of lead in table salt were separated by co-precipitation with PAN-Ni ( Ⅱ ), and adding Mn( Ⅱ ) ion as internal standard. Conditions for co-precipitation were optimized. Under the optimized reaction conditions, the internal standard Mn( Ⅱ ) and Pb( Ⅱ ) ions in the sample were quantitatively co-precipitated by PAN-Ni( Ⅱ ), and both of the Mn(Ⅱ ) and Pb(Ⅱ), also including Ni( Ⅱ ) were present in the precipitate with good homogeneity, and a definite ratio was kept between Pb( Ⅱ ) and Mn( Ⅱ), or between Ni( Ⅱ) and Mn( Ⅱ ). The mass of lead in the sample was calculated from the ratio of absorbances APb1 and AMn1 of lead (Pb1) and manganese (Mn1) found in the co-precipitate. Lead content (Pb0) in the original sample was calculated by the following formula: mPb0 =Apb1/AMn1 · mMn0. It was Shown by experimental results that by the separation mentioned above, the matrix interference was effectively eliminated. Detection limit of this method was found to be 3.18×10^-2mg·L^-1. In the analysis of 3 kinds of table salt by this method. RSD's (n=6) obtained were less than 4. 3%, and recoveries in the range of 95. 4%-101.6% were found.