毛细管气相色谱法同时测定工业废水中微量的萘、α-萘酚及蒽

Simultaneous Determination of Trace Naphthalene,α-Naphthol and Anthracene in Industrial Wastewater by Capillary Gas Chromatograph

本文建立了同时测定工业废水中微量的萘、α-萘酚及蒽的毛细管气相色谱方法。以二氯乙烷和氯化钠的混合液萃取水样,利用毛细管柱气相色谱-FID进行检测,以外标法定量。该方法测定的萘、α-萘酚、蒽的标准工作曲线方程分别为y=23.091x＋0.688（r=0.9996）,y=17.788x-13.136（r=0.9992）,y=25.123x-10.756（r=0.9991）,检出限（S/N=3）分别是5.3×10-4μg.mL^-1,6.9×10-4μg.mL^-1,4.9×10-4μg.m^L-1,线性范围分别是1.8×10^-3 - 40μg.mL^-1、2.3×10^-3 - 60μg.mL^-1、1.6×10^-3 - 50μg.mL^-1。对此多环芳烃体系标准混合物溶液进行了3个不同水平的添加,每个水平重复6次进样,萘、α-萘酚、蒽的平均加标回收率分别为89%-104%、97%-113%、90%-106%,相对标准偏差分别为1.7%-2.6%、1.9%-3.7%、1.8%-3.5%。相同条件下,实际工业废水样品经富集后检测,萘,α-萘酚,蒽的平均浓度分别为196.7μg.mL^-1、20.65μg.mL^-1、100.8μg.mL^-1。实验结果表明：本方法操作简便、快速、准确、灵敏度高、线性范围较宽,测定结果令人满意。

Capillary gas chromatography was cstablishod for simultaneous determination of trace naphthalene, α- naphthol and anthracene in industrial wastcwatcr. The samples, extracted with mixture of dichloroethane and sodium chlofide, quantified by external standards using a capillary column with a flame ionization detector. The equations for linear regression calibration curves of naphthalene,α- naphthol and anthracene were y = 23. 091x ＋ 0. 688 （ r = 0. 999）, y = 17 · 788x - 13. 136 （r = 0. 9992）, y = 25. 123x - 10. 756 （r = 0. 9991）, respectively, and detection limits to them （ S/N =3） were 5.3 × 10^-4μ g· mL^-1, 6. 9 × 10^-4μ g· mL^-1, 4. 9 × 10^-4μ g· mL^-1, individually. The linear ranges for measuring these polycyclic aromatic hydrocarbons （PAHs） were 1.8 × 10^-3 -40μ g· mL^-1, 2. 3 × 10^-3 -60μ g· mL^-1, 1.6 × 10^-3 -50μ g· mL^-1 , separately. Three different levels of standard additions, at each level performed on six replicate samples, were applied to these standard mixture so/utions of PAHs. The average recoverie from spiked samples were 89% - 104% for naphthalene, 97% - 113% for α - naphthol and 90% - 106% for anthracene, with the relative standard deviation 1. 7% - 2. 6% for naphthalene, 1.9% - 3.7% for α- naphthol and 1.8% - 3.5% for anthracene. Under the same condition, industrial wastewater samples were concentrated and measured. The average mass concentrations of naphthalene, α - naphthol and anthracene were 196. 7μg · mL^-1, 20. 65μg · mL^-1 and 100. 8μg · mL^-1. The satisfying result showed the proposed method several attributes, such as, performing easily, less time - and labor - intensive, high sensitivity, quantifying accurately, wide linear range and so on.