Effkemann S, Brødsgaard S, Mortensen P, Linde S A, Karst U
Westfälische Wilhelms-Universität Münster, Abteilung Analytische Chemie, Germany.
J Chromatogr A. 1999 Sep 10;855(2):551-61. doi: 10.1016/s0021-9673(99)00734-7.
The first selective HPLC methods for the determination of peroxyacetic acid (PAA) in gas phase samples have been developed. PAA reacts with 2-([3-{2-[4-amino-2-(methylsulfanyl)phenyl]- 1-diazenyl}phenyl]sulfonyl)-1-ethanol (ADS) to form the corresponding sulfoxide. Sampling may be performed in impingers using aqueous solutions of the reagent or by test tubes with the reagent coated on a solid sorbent. Sulfide and sulfoxide are separated by means of HPLC and detected at a wavelength of 410 nm. The method is highly selective for PAA in the presence of hydrogen peroxide when sampling in impingers. A 10,000-fold excess of hydrogen peroxide leads to the same peak area compared to PAA. Limit of detection is 10(-8) mol PAA, thus corresponding to PAA concentration of 46 ppb when using a sampling time of 10 min with a flow-rate at 500 ml/min. Another sulfide reagent, methyl-p-tolyl sulfide (MTS) has been used in a similar way with impinger sampling. Major advantages of ADS towards MTS are improved UV-Vis spectroscopic properties and reduced volatility.
已开发出用于测定气相样品中过氧乙酸（PAA）的首批选择性高效液相色谱法。PAA与2 -（[3 - {2 - [4 - 氨基 - 2 - （甲硫基）苯基] - 1 - 重氮基}苯基]磺酰基）- 1 - 乙醇（ADS）反应形成相应的亚砜。采样可在冲击式吸收管中使用试剂水溶液进行，或通过涂覆有试剂的固体吸附剂的试管进行。硫化物和亚砜通过高效液相色谱法分离，并在410 nm波长处检测。当在冲击式吸收管中采样时，该方法对存在过氧化氢情况下的PAA具有高度选择性。与PAA相比，过量10000倍的过氧化氢会导致相同的峰面积。检测限为10^(-8) mol PAA，因此当使用10分钟采样时间和500 ml/min流速时，对应于46 ppb的PAA浓度。另一种硫化物试剂，对甲苯基甲基硫醚（MTS）已以类似方式用于冲击式吸收管采样。ADS相对于MTS的主要优点是改善的紫外 - 可见光谱性质和降低的挥发性。
