参考HJ 683-2014,用2,4-二硝基苯肼(DNPH)采样管在安徽省6个城市采集30个环境空气样品。采样管用5 mL乙腈洗脱,收集洗脱液,用乙腈稀释至5 mL,用0.45 μm针头过滤器过滤后供高效液相色谱法分析。以填充物粒径为2.7 μm的Agilent EC-C₁₈色谱柱为固定相,以不同体积比的乙腈和水的混合液为流动相进行梯度洗脱,分离后的目标物用二极管阵列检测器在360 nm检测波长下检测。结果显示:13种醛酮类化合物(甲醛、乙醛、丙烯醛、丙酮、丙醛、丁烯醛、甲基丙烯醛、丁酮、正丁醛、苯甲醛、戊醛、间甲基苯甲醛和己醛)的衍生物可在14 min内分离,其质量浓度(以醛酮计)均在0.1~2.0 mg·L^-1内与其对应的峰面积呈线性关系,检出限(3.143s)为0.11~0.37 μg·m^-3;对醛酮类衍生物混合标准溶液进行精密度试验,测定值的相对标准偏差(n=6)为0.080%~1.6%;在空白采样管中进行回收试验,其中甲醛、乙醛、丙酮的检出量分别为0.055,0.035,0.080 μg,13种目标物的回收率84.1%~108%;方法用于30个实际样品的分析,在6个城市的环境空气中,甲醛、乙醛、丙酮、丁酮、正丁醛、丙烯醛均有检出,正丁醛的检出量最高,丙醛、甲基丙烯醛、苯甲醛、间甲基苯甲醛、己醛检出量均较低,丁烯醛、戊醛均未检出;30个样品中13种目标物的检出总量为16.78~44.53 μg·m^-3。

A total of 30 ambient air samples was collected from 6 cities in Anhui Province using 2,4-dinitrophenylhydrazine (DNPH) sampling tubes with reference to HJ 683-2014. The sampling tube was eluted with 5 mL of acetonitrile, and the eluent was collected, diluted to 5 mL with acetonitrile, filtered with 0.45 μm needle filter, and analyzed by high performance liquid chromatography. Agilent EC-C₁₈ column with packing particle size of 2.7 μm was used as the stationary phase, and mixed solution composed of acetonitrile and water at various volume ratios was used as the mobile phase for gradient elution. The targets separated were detected by diode array detector at the detection wavelength of 360 nm. It was shown that derivatives of the 13 aldehydes and ketones (formaldehyde, acetaldehyde, acrolein, acetone, propionaldehyde, crotonaldehyde, methacrolein, butanone, butyraldehyde, benzaldehyde, valeraldehyde, m-tolualdehyde and n-hexaldehyde) could be separated within 14 min, and linear relationships between values of mass concentration (calculated by aldehydes and ketones) and peak area of the 13 targets were kept in the range of 0.1-2.0 mg·L^-1, with detection limits (3.143s) of 0.11-0.37 μg·m^-3. Test for precision on the mixed standard solution of aldehydes and ketones derivatives was made, and RSDs of the determined values (n=6) was 0.080%-1.6%. Test for recovery was made in the blank sampling tube, with detection amounts of formaldehyde, acetaldehyde and acetone in the blank sampling tube of 0.055, 0.035, 0.080 μg, and recoveries of the 13 targets in the range of 84.1%-108%. The proposed method was applied to the analysis of the 30 actual samples, and formaldehyde, acetaldehyde, acetone, butanone and butyraldehyde were all detected in the ambient air of the 6 cities. The detection amount of butyraldehyde was the highest, the detection amounts of propionaldehyde, methacrolein, benzaldehyde, m-tolualdehyde, n-hexaldehyde and acrolein were lower, and crotonaldehyde and valeraldehyde were not detected. The total detection amounts of the 13 targets in 30 samples were 16.78-44.53 μg·m^-3.