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应用内标的PAN—Ni体系快速共沉淀分离富集和火焰原子吸收光谱测定食盐中铅
  • ISSN号:1001-4020
  • 期刊名称:《理化检验:化学分册》
  • 时间:0
  • 分类:O657.31[理学—分析化学;理学—化学]
  • 作者机构:[1]同济大学化学系,上海200092
  • 相关基金:国家自然科学基金资助项目(29973029)
中文摘要:

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。

英文摘要:

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.

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期刊信息
  • 《理化检验:化学分册》
  • 中国科技核心期刊
  • 主管单位:上海科学院
  • 主办单位:上海材料研究所
  • 主编:吴诚
  • 地址:上海市邯郸路99号
  • 邮编:200437
  • 邮箱:hx@mat-test.com
  • 电话:021-65556775-263
  • 国际标准刊号:ISSN:1001-4020
  • 国内统一刊号:ISSN:31-1337/TB
  • 邮发代号:4-182
  • 获奖情况:
  • 中国期刊方阵“双效”期刊
  • 国内外数据库收录:
  • 美国化学文摘(网络版),荷兰文摘与引文数据库,中国中国科技核心期刊,中国北大核心期刊(2004版),中国北大核心期刊(2008版),中国北大核心期刊(2011版),中国北大核心期刊(2014版),英国英国皇家化学学会文摘,中国北大核心期刊(2000版)
  • 被引量:20443