Abstract: The ambient carbonyl compounds have become one of the research hotspots in atmospheric environment. Carbonyl compounds are difficult to detect because of their relatively higher reactivity and chemical instability. In order to detect ambient carbonyl and dicarbonyl compounds accurately, the sampling and analysis methods of 18 kinds of carbonyl and dicarbonyl compounds with relatively higher concentration or higher reactivity in ambient air were investigated and the optimized methods were applied to study the pollution characteristics of ambient carbonyl compounds in the typical urban area in Beijing in May 2018. The results showed that:(1) The automated multi-port sampler can collect sample continuously, under the same sampling conditions compared with the single-port sampler, the collected data had no obvious difference (R²=0.9997), and the maximum sampling flow rate was set to be 0.8 L/min. The highest impurity content in the sampling tube was 0.01 μg for one DNPH-cartridge, which was less than the standard limit of 0.10 μg for one DNPH-cartridge (HJ 683-2014 Ambient Air-Determination of Aldehyde and Ketone Compounds-High Performance Liquid Chromatography). (2) Two dicarbonyl compounds which are glyoxal and methyl glyoxal could be successfully detected by adopting the determined derivatization method of dicarbonyl compounds and the corresponding mass spectrometry scanning conditions; The standard curves of 18 kinds of carbonyl compounds were established and the correlation coefficients R² of the standard curves were higher than 0.9950. (3) The mass concentrations of 18 carbonyl compounds in the ambient of the typical area in Beijing in this study period were 17.73-88.42 μg/m³.