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Acetone and Acrolein:Analytical Challenges

机译:丙酮和丙烯醛:分析挑战

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Acetone and acrolein are both monitored in ambient air,but both compounds present analytical challenges because of their polarity and reactivity.Acetone and acrolein are listed as compounds of interest in EPA Compendium Method TO-15 and Method TO-11A.Method TO-15 requires collection of an ambient air sample in a canister with subsequent analysis by gas chromatography/mass spectrometry(GC/MS).Method TO-11A requires collection of an ambient air sample on a silica gel tube coated with 2,4-dinitrophenylhydrazine(DNPH),with subsequent extraction and analysis by high performance liquid chromatography(HPLC).The analytical challenge posed by acetone arises from the discrepancies between results obtained from two different analytical modes:results obtained by Method TO-15 for acetone are consistently higher(as much as an order of magnitude)than the results obtained by Method TO-11A.To evaluate which method is more accurate,laboratory studies were performed to simultaneously collect test canister and coated sorbent tube cartridges while sampling a test atmosphere containing a known quantity of acetone.Method TO-11A has been disqualified as the methodology of choice for determination of acrolein because of the tautomerization of the acrolein hydrazone derivative on acidified DNPH cartridges.This results in the inability to accurately quantify acrolein at the expected retention time.To evaluate alternative methods,analysis of acrolein in canisters was studied using the analytical methodology of Method TO-15,with GC/MS analysis.In addition,modification of Compendium Method TO-11A with HPLC analysis in cartridges was also evaluated for acrolein recovery by quantifying multiple peaks for acrolein(and its unknown breakdown product)using DNPH cartridges spiked with underivatized standards.
机译:丙酮和丙烯醛均在环境空气中监测,但由于它们的极性和反应性,两种化合物都存在分析挑战。丙酮和丙烯醛被列为EPA纲要方法至15中的目的化合物,并对-11.方法是-15的方法通过气相色谱/质谱(GC / MS)的随后分析罐中的环境空气样品。方法在涂有2,4-二硝基苯肼(DNPH)的硅胶管上需要收集环境空气样品。随后通过高效液相色谱(HPLC)提取和分析。丙酮占据的分析攻击产生从两种不同的分析模式获得的结果之间的差异:通过对丙酮的方法得到的方法得到的结果始终如一(尽可能多幅度比通过方法获得的结果为-11a.pto评估哪种方法更准确,进行实验室研究以同时收集测试罐r和涂覆的吸附剂管盒,同时取样含有已知量的丙酮的测试气氛。方法是对丙烯醛测定的选择的方法,因为丙烯醛腙衍生物对酸化的dnph cartridges的互化化。结果在无法准确地定量预期保留时间的丙烯醛。使用方法至15的方法对饮用方法进行评估,研究罐中的丙烯醛分析,GC / MS分析。添加,改进概要方法 - 11A还通过使用尖刺筒(及其未知的击穿产品)的多峰来评价盒中的HPLC分析,用于使用尖刺盒掺入很好的标准的DNPH盒来评估丙烯醛恢复。

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