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(00215)Validation of a multistep derivatization method for the determination of polar species in organic aerosol.

机译:(00215)验证有机气溶胶中极性物种测定的多步衍生方法。

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Secondary organic aerosol (SOA)is a significant constituent of airborne fine particles. A multistep derivatization method was developed, optimized, and validated for the determination of organic compounds in the atmospheric aerosol with mono- and multi-functional species, with GC/MS. The first step includes the alkylation of the carbonyl (C=O)moieties using o-methylhydroxylamine hydrochloride as the derivatization reagent. The second step refers to the conversion of carboxylic acids to methyl ester derivatives using TMSD/methanol or BF3/methanol. Finally, alcohols are converted to trimethylsilyl ethers with BSTFA+ 1% TMCS. The use of TMSD/methanol as the derivatization reagent in step 2 is preferred for the procedure, achieving higher sensitivity. Additionally, BF3/MeOH was ineffective at converting some mono/dicarboxylic acids and species with more than 2-OH moieties. The derivatization procedure in stage 3 was optimized yielding the appropriate reaction temperature and time, while in stage 2 yielding the appropriate amounts of the derivatization reagents. The method was validated for twenty-two compounds which are possible SOA tracers. Detection limits ranged from 0.31 to 0.98 ng m-3 and recoveries from 73.5% to 108%. The method was applied to field samples from rural and industrial areas with concentration levels ranging from below limits of detection to 42 ng m~(-3).
机译:二次有机气溶胶(SOA)是空气传播细颗粒的重要组成部分。开发,优化了多步衍生化方法,并验证了用GC / MS测定大气和多功能物种中的大气气溶胶中的有机化合物。第一步包括使用盐酸O-甲基羟胺作为衍生化试剂的羰基(C = O)部分的烷基化。第二步骤是指使用TMSD /甲醇或BF3 /甲醇将羧酸转化为甲酯衍生物。最后,用BSTFA + 1%TMC转化醇转化为三甲基甲硅烷基醚。在步骤2中使用TMSD /甲醇作为衍生化试剂,优选用于该程序,实现更高的灵敏度。另外,BF 3 / MeOH在转化一些单一/二羧酸和具有超过2 oh部分的物种时无效。阶段3中的衍生化程序优化,得到适当的反应温度和时间,而在第2阶段,产生适量的衍生化试剂。该方法验证了二十二种化合物,这是可以SOA示踪剂的化合物。检测限范率范围为0.31至0.98ng m-3,回收率为73.5%至108%。将该方法应用于来自农村和工业区的现场样本,其浓度水平从低于检测限度到42ng m〜(-3)。

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