FG Luftchemie und Luftreinhaltung
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A new method for the determination of sucrose in honey with derivatization solid-phase microextraction and gas chromatography/mass spectrometry (D-SPME–GC/MS) was developed. The method incorporates a sample derivatization with acetic anhydride using N-methylimidazole as the catalyst and the subsequent enrichment of the analyte in a Polyacrylate-SPME fiber. Results show that 100 µL N-methylimidazole and 800 µL acetic anhydride were sufficient to complete the acetylation for sucrose in 100 µL aqueous sample at room temperature. For SPME, an enrichment time of 30 min was sufficient. SPME was performed by immersing the fiber into the solution with additional vibration. Then, the analyte was desorbed for 5 min at 280°C in the GC/MS injection port with splitless mode. The present method exhibits good linearity at a concentration range of 0.3–8% of sucrose in honey with excellent regression (R = 0.9993). The method has been successfully applied to the control of sucrose adulteration in honey.
Determination of volatile organic compounds (VOCs) in crude oil, such as super volatile organic compounds (super VOCs) and simple polycyclic aromatic hydrocarbons (PAHs), is vital for targeting crude oil spill spots. In this study, a static headspace gas chromatography flame ionization detection method was established for determination of super VOCs in crude oil with both external and internal standard determination, which can be used in the field when using portable gas chromatography. Identification was done by comparing the retention time with the corresponding standards and quantitation was done with a new one-drop method. Another simplified and efficient method was performed to analyze volatile PAHs in crude oil, which can also be used in field analysis. Toluene was used as the extraction solvent for PAHs in crude oil. Method validation for both analyses was satisfactory. The result showed that n-butane and n-pentane were maximum super VOCs and naphthalene, phenanthrene and fluorene were the main PAHs in the crude oil studied. The super VOCs quantity ranged from 3 to 6% and the main PAHs consisted of 0.02–0.06% of studied crude oil.
Results of cloud physical and chemical measurements in low clouds observed at Mt. Brocken, Germany
(2001)