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Nitrite Interference in the Analysis of Nitrophenols In Wastewater Effluents

机译:废水流出物中硝基苯酚分析的亚硝酸盐干扰

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Elevated concentrations of 2-nitrophenol (ONP) and 4-nitrophenol (PNP) were measured in a municipal treatment plant’s effluent when nitrite ion (NO2 -1) was present. ONP and PNP concentrations were determined using USEPA’s method 3520 continuous liquid-liquid extraction in conjunction with gas chromatography/ mass spectrometry (GC/MS) analysis by USEPA method 8270. It was also observed that surrogates, compounds added during testing to check the extraction efficiency, were at unusually low levels when nitrite was present. It was determined that nitrite reacts with the surrogates producing low surrogate recoveries and also that nitrite reacts with phenol present in the sample to produce false positive effluent concentrations of ONP and PNP. It was determined in an inter-laboratory study that nitrite interference occurs with the separatory funnel extraction method 3510 also. Modification of method 3520’s extraction pH to 4.5 corrected this interference problem; however, certain of the target analytes for method 8270 cannot be recovered in acceptable concentrations at this modified extraction pH. Therefore, the modified method cannot be used for all phenolic compounds typically analyzed by method 8270.
机译:在存在亚硝酸盐离子(No2 -1)时,在城市治疗植物的流出物中测量升高的2-硝基苯酚(ONP)和4-硝基苯酚(PNP)。使用使用PA方法8270结合气相色谱/质谱(GC / MS)分析使用USEPA方法3520连续液 - 液萃取确定ONP和PNP浓度。还观察到替代物,在测试期间添加化合物以检查提取效率当存在亚硝酸盐时,在异常较低。确定亚硝酸盐与产生低替代回收的替代物以及亚硝酸盐与样品中存在的苯酚反应,以产生伪阳性流出浓度的ONP和PNP。在实验室内测定,亚硝酸盐干扰也与分液漏斗提取方法3510也发生。方法3520的提取pH至4.5修改纠正了这种干扰问题;然而,方法8270的某些靶分析物不能在该改性的提取pH下以可接受的浓度回收。因此,改性方法不能用于通过方法8270分析的所有酚类化合物。

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