气相色谱法测定橡皮擦中甲醛时衍生参数的影响分析

利用甲醛与2,4-二硝基苯肼的衍生反应,用气相色谱法测定橡皮擦中的甲醛时对衍生参数的影响进行分析。对关键衍生环节中的衍生因素如衍生剂用量、衍生温度、衍生时间、提取剂等进行试验,确定衍生剂用量为0.5mL,衍生温度为70℃,衍生时间15 min;提取剂为甲苯,用量为每次5 mL,充分振摇1 min,提取2次。橡皮擦中甲醛的质量浓度在0.105~10.5 mg/L范围内与色谱峰面积呈良好的线性,线性相关系数r=0.999 7,测定结果的相对标准偏差为2.1%(n=6),检出限为0.01 mg/L,平均加标回收率为88.4%。该衍生气相色谱法灵敏度高,稳定性好,可用于橡皮擦产品中甲醛的快速检测。

Analysis of Derivative Parameters in Determination of Formaldehyde in Eraser by Gas Chromatography

Influence of derivative parameters on the determination of formaldehyde in eraser by derivation gas chromatography using the derivative reaction of formaldehyde with 2,4-dinitrophenylhydrazine was analysed. The key derived factors such as derivative agent dosage,derived temperature,derived time,the extracting agent types and so on were tested. The dosage of derivative agent was 0.5 mL,the derived temperature was 70℃,the derived time was 15 min, fully shaking 1 min and extracting 2 times with 5 mL toluene each time. The concentration of formaldehyde was linear with chromatographic peak area in the range of 0.105–10.5 mg/L, r=0.999 7. The relative standard deviation of detection results was 2.1%(n=6),the detection limit was 0.01 mg/L and the average recovery rate was 88.4%. The method has high sensitivity and good stability, it can be used for quick detection of formaldehyde in eraser.