醛、酮类腙衍生物校正因子的预测与测定  

Prediction and Measurement of the Relative Mass Calibration Factor of Aldehydes and Ketones Derivatives

作　　者：魏晓兵[1] 范国樑[1] 宋威[2] 宋崇林[3] 周维义[2] 张仲荣[1] 

机构地区：[1]天津大学材料学院,天津300072 [2]天津大学分析中心,天津300072 [3]内燃机燃烧学国家重点实验室,天津300072

出　　处：《分析化学》2005年第6期781-784,共4页Chinese Journal of Analytical Chemistry

基　　金：国家重点基础研究发展计划(973)项目(No.2002CB211600)资助课题

摘　　要：利用2,4二硝基苯肼(DNPH)与醛、酮类化合物反应生成稳定的衍生物2,4二硝基苯腙,对所生成的DNPH衍生物溶液直接进行气相色谱分析;以苯为内标物,分别对6种醛、酮衍生物的校正因子进行了预测和回归,校正因子的实际测定值与理论预测值的最大相对误差不超过0.4%。实验说明对反应生成物直接进行校正因子测定的方法是可靠的,且方法操作简单;同时也说明使用理论计算方法预测醛、酮DNPH衍生物校正因子的可行性,为使用理论计算方法预测其它醛、酮DNPH衍生物的校正因子奠定了基础。2,4-Dinitrophenylhydrazine(DNPH) and aldehyde or ketone can react and form 2,4-dinitrophenyl-hydrazone that can be injected directly on the gas chromatography( GC). In the course, aldehydes and ketones preferably were converted into stable derivatives that can be ascertained by gas chromatography-mass spectrum (GC-MS). Then,benzene was used as an internal standard. The relative mass calibration factors of six kinds of aldehyde and ketone derivatives were determined. By right of a new calculation formula for the calculating relative mass calibration factor based on the flame ionization detector ( FID), the calibration factors of aldehyde and ketone derivatives were calculated. The most relative error between experiment and prediction was less than 0.4%. The method of direct using reaction solute to obtain calibration factor is simple and credible. However, the calculation formula for the calculating relative mass calibration factor based on the FID was feasible and the exact correction of Y in the calculation formula was got. It can give good results of relative mass calibration factor for other aldehyde and ketone derivatives in favor of farther researching the content of aldehydes and ketones of atmosphere or the exhaust of automobiles.

关 键 词：校正因子 理论计算方法 醛 气相色谱分析 DNPH 最大相对误差 二硝基苯肼 酮类化合物 二硝基苯腙 反应生成物 酮衍生物 内标物 预测值 测定值 溶液 回归 

分 类 号：O622.4[理学—有机化学]