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Wysłany: Śro 22:01, 09 Lut 2011 |
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Determination of line preconcentration of PAHs in drinking water
Performance liquid chromatography of polycyclic aromatic hydrocarbons in drinking water Jia-Yuan Yin Yang Yaling Mengdong Ling Yang Guorong Solid Phase Extraction (Students of the University of Kunming,[link widoczny dla zalogowanych], Kunming 650224) (Department of Chemistry, Yunnan University, Kunming 650106, China) 1 Introduction PAHs are an important class of carcinogenic substances , Trace analysis of polycyclic aromatic hydrocarbons is important. A procedure in which high performance liquid chromatography fluorescence detection wavelength is to measure the most common method of polycyclic aromatic hydrocarbons. UV photodiode array detector with a peak purity test to compare the unknown spectra and spectral library spectra assisted qualitative features, the reliability of their test results than the wavelength of fluorescence detection high program. But the UV detection sensitivity lower than the fluorescence detector nearly two orders of magnitude, for clean water samples, PAHs in UV detection difficult to achieve the quantitative range. To address the cleaning of PAHs in water samples by UV diode matrix detector, we study the column line enrichment method, greatly improving the enrichment factors of PAHs, polycyclic aromatic hydrocarbons in clean water samples after enrichment by its concentration can reach the linear range of UV detection may Simultaneous determination of one injection ng / L level dozen polycyclic aromatic hydrocarbons: Method for the clean determination of polycyclic aromatic hydrocarbons in water samples with satisfactory results. 2 Experimental 2.1 Instruments and reagents main operation line preconcentration with a six-way switching valve high performance liquid chromatography (Waters Corporation USA) to complete. Acetonitrile,[link widoczny dla zalogowanych], methanol, tetrahydrofuran: High performance liquid chromatography-specific (Fisher Company); water for the quartz sub-boiling distilled water and used MiUi-Q50 (U.S. MiUipore company) ultra-pure water treatment apparatus, resistance �� 18Mfl; 16 polycyclic aromatic hydrocarbons mixture (UltraScientific company). 2.2 Sample analysis steps enrichment column and analytical column are SupeleosilLC-PAH Liquid Chromatography (4.6inln �� 150inln): take 50mL water, add 15mL of methanol, the 0.45ptm filter membrane to a .5mL/min Waters510 pumping flow rate through the enrichment column enrichment, after concentration to 1.5m1. / Min flow rate with 10% methanol wash 10min, switching six-way switching valve to change your direction, so that by the Waters2690 pumping the mobile phase flow rate to 1.5mL/min wash down from the enrichment column sample enrichment, flows through the analytical column and use gradient elution, and then flow detector. Mobile phase gradient conditions: A. Methanol / water (30/70); B. Acetonitrile, according 0rain (9o% A +10% B), 5rain (90% A +10% B), 15min (70% A +30% B), 30rain (100% B), 35rain (100% B), linear increasing gradient of conditions, return to the starting gradient equilibrium after 15min of the next sample. Under these conditions,[link widoczny dla zalogowanych], the retention time of PAHs: naphthalene 7.26min,[link widoczny dla zalogowanych], acenaphthene 9.58min, dihydro acenaphthylene 10.60rain, fluorene 11.18min, Philippines 12.12rain, anthracene 13.06min, fluoranthene 13. 98min, water chestnut 14.76min, benzo (a) anthracene 15.72rain, acenaphthene l7.09min, benzo (b) fluoranthene unhappy 18.02min, benzo (k) fluoranthene unhappy 18.87min, benzo (a) pyrene 19.32rain, dibenzo (g, h) anthracene 20.75min, benzo (g, h, i) anthracene 21.56min, indeno (1,2,3-ed) Xiaochaihu 23.28min. The peaks were resolved peak purity were made to confirm the conditions in the non-overlapping peaks. 3 the results of samples was determined using the tap water, commercial mineral water, commercially available pure water, groundwater 4 polycyclic aromatic hydrocarbons in water samples, recoveries were 92% -107%; relative standard deviation of 1. A 3.7% 6% Q, with satisfactory results. 4 Conclusion Methods SupeleosilLC-PAH column line preconcentration, UV diode array detection, high performance liquid chromatography of polycyclic aromatic hydrocarbons in drinking water; chromatography line enrichment can be achieved high multiple enrichment of polycyclic aromatic hydrocarbons in water, clean water After enrichment of polycyclic aromatic hydrocarbons can be achieved by UV photodiode array detector linear range. UV photodiode array detector with a peak purity test to compare the unknown spectra and spectral library spectra assisted qualitative features the ability to make the results more reliable. The method is based on a certain extent, for clean water samples ng / L level analysis provides a method for polycyclic aromatic hydrocarbons. Received 2002-08-20; 2003-03-25 accepted
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