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    离子色谱法测定肥料中三聚氰胺的含量

    Determination of Melamine in Fertilizer by IC

    • 摘要: 采用离子色谱分析法检测肥料中三聚氰胺的含量。样品用氨水-甲醇-水(2+7+1)溶液超声振荡提取,离心后经氮气吹干,用3 mmol·L-1甲烷磺酸溶液定容,分离柱和保护柱均为Dionex IonPac R SCS1,淋洗液为含3 mmol·L-1甲烷磺酸的乙腈-水(15+85)。采用非抑制型电导检测器检测。三聚氰胺的线性范围为1.00~1 000 mg·L-1,检出限(3S/N)为5 mg·kg-1,测定下限(9S/N)为15 mg·kg-1。加标回收率在79.3%~116%之间,测定值的相对标准偏差(n=6)在3.4%~13%之间。

       

      Abstract: IC was applied to the determination of melamine in fertilizer. The sample was extracted ultrasonically with a mixture of NH3·H2O+CH3OH+H2O (2+7+1). After centrifuging, the extract was evaporated to dryness by N2-blowing, and the residue was dissolved with 3 mmol·L-1 methylsulfonic acid solution. Dionex IonPac R SCS1 columns were used both as separation and guard columns and a mixture of acetonitrile and 3 mmol·L-1 methylsulphonic acid solution (15+85) was used as eluent. Melamine was detected by non-suppressed conductivity detector. The linearity range of melamine was between 1.00-1 000 mg·L-1. The detection limit was 5 mg·kg-1 and the limit of quantification was 15 mg·kg-1. Values of recovery found by standard addition method were in the range of 79.3%-116% and RSD′s (n=6) were in the range of 3.4%-13%.

       

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