反相高效液相色谱法测定镍(Ⅱ)和铁(Ⅲ)

Reversed-phase high performance liquid chromatographic determination of nickel(Ⅱ)and iron(Ⅲ)

以2-[（5-溴-2-吡啶）-偶氮]-5-二乙氨基苯酚（5-Br—PADAP）作为柱前衍生试剂，Chro—matorex C18 ODS色谱柱作为固定相，流动相为微乳液[十六烷基三甲基溴化铵（CTMAB）＋正丁醇＋庚烷＋水]／乙腈35：65（体积比），在波长560nm处进行光度检测，在柱温30℃时，15min内分离测定了镍（Ⅱ）和铁（Ⅲ）。该方法的线性范围Ni^2＋为0．08～2．0μg／mL，Fe^3＋为0．2～2．0μg／mL，检出限分别为9．62μg／L和20．11μg／L。方法应用于浑河水样和生活污水水样的分析，结果同原子吸收光谱法测定值相-致，相对标准偏差为3．0％～3．7％。

A reversed-phase high performance liquid chromatographic method for the determination of nickel （Ⅱ） and iron （Ⅲ） has been developed with the mobile phase of 35 ： 65 （V/V） microemulsion（CT- MABq-butanol＋heptane＋kwater）/acetonitrile . Two complexes of nickel （Ⅱ） and iron （Ⅲ） of pre-column deriving reactions with 2-（ 5-bromo-2-pyridylazo）-5-diethylaminophenol （5-Br-PADAP） can be separated and determined quantitatively within 15 minutes on Chromatorex C18 ODS column at column temperature of 30 ℃ at 560 nm. The linear range is 0.08-2.0μg/mL for Ni^3＋ and 0.2-2.0μg/mL for Fe^3＋. The detection limit is 9.62 μg/L for Ni^2＋ and 20.11 μg/L for Fe^3＋. The proposed method has been applied to the determination of nickel and iron in Hunhe river and domestic sewage water samples. The results were consistent with those of atomic absorption spectrometry. The relative standard deviation is 3.0%-3.7%.