Lange J, Eckhoff S
Institut für Verbrennungskraftmaschinen, Universität Hannover, Welfengarten 1A, D-30167, Hannover, Germany.
Anal Bioanal Chem. 1996 Oct;356(6):385-9. doi: 10.1007/s0021663560385.
The determination of carbonyl compounds in gaseous samples is usually accomplished by enrichment methods, in which 2,4-dinitrophenyl-hydrazine (DNPH) as a derivatization reagent has become established to a large extent. However, the conventional methods of DNPH-impingers and of DNPH-cartridges are applicable to emission measurements in a limited way only, depending on the NO(2)-concentration in the exhaust gas. It could be proved that DNPH-derivatives, as well as DNPH, are also decomposed by NO(2) at a different speed, in which the hydrazones of unsaturated carbonyl compounds are probably more sensitive than those of the saturated carbonyl compounds. In view of this fact, the collecting methods had to be modified to avoid losses with the enrichment. The analysis of the compounds is carried out by HPLC with an effective gradient-system which is able to separate and detect the carbonyl compounds in exhaust gas within 16 min. Furthermore, a simple working-up procedure is presented which facilitates a parallel analysis by GC.
气态样品中羰基化合物的测定通常通过富集方法完成,在这些方法中,2,4-二硝基苯肼(DNPH)作为衍生试剂已在很大程度上得到应用。然而,传统的DNPH冲击瓶法和DNPH柱法仅在有限程度上适用于排放测量,这取决于废气中的NO₂浓度。可以证明,DNPH衍生物以及DNPH也会被NO₂以不同速度分解,其中不饱和羰基化合物的腙可能比饱和羰基化合物的腙更敏感。鉴于这一事实,必须修改收集方法以避免富集过程中的损失。化合物的分析通过具有有效梯度系统的高效液相色谱法进行,该系统能够在16分钟内分离和检测废气中的羰基化合物。此外,还介绍了一种简单的后处理程序,便于通过气相色谱法进行平行分析。