高效液相色谱法检测污水中的亚硝酸氮的试验研究

The research on nitrite nitrogen detection in waste water by HPLC

利用高效液相色谱仪—二极管阵列检测器(HPLC-DAD)的方法检测污水中亚硝酸氮(NO2--N)的试验进行了流动相比例和流速、色谱柱温度、进样量和DAD检测波长的研究。实验结果表明:样品经过简单处理、外标法定量,保留时间为2.38min。使用十八烷基固定相(ODS)的色谱柱(5μm,125mm×4.6mm)和磷酸二氢钾缓冲溶液(2 mmol.L-1 H3PO4-17.5 mmol.L-1KH2PO4,pH=3.3)-乙腈(体积比93∶7)的流动相,流速0.8mL.min-1,柱温30℃,进样体积5μL,DAD检测波长为204nm;线性范围是0.1～15.0mg.L-1,线性相关系数为0.997,回收率在81.1%～100.2%之间,相对标准偏差(RSD)小于0.18%,最低检测限为0.043μg.mL-1(S/N=5)。

In this paper,an experiment has been made to detect nitrite nitrogen(NO-2-N) in waste water by the method of HPLC(High-performance liquid chromatography)-DAD(diode array detector).The experiment includes the proportion of mobile phase and flow rate,column temperature,injection volume,and DAD detecting wave length.The results show that the retention time of samples after simple treatment and external standard is 1.7 min.While a hypersil ODS(5 μm,125 mm×4.6 mm)column is selected as the chromatographic column:the mobile phase of V(A)∶V(B)=93∶7(A:2 mmol·L-1 H3PO4-17.5 mmol·L-1 KH2PO4,pH=3.3,B:acetonitrile);the flow is 0.80 mL·min-1;temperature is 30.0 ℃;the injection volume is 5.0 μL;the detecting wavelength is 204 nm,the column the range of linearity was 0.1～15.0 mg·L-1,and the correlation coefficient between concentrations and peak areas were 0.997;the recovery rate was around 81.1%～100.2%;and the RSD was below 0.18%.The lowest detection limits was 0.043 μg·mL-1(S/N=5).