Application of low-temperature CP-Sil 88 column for the isomeric analysis of toxic 2,378-substituted PCDD/Fs in incinerator flyash and sewage sludge using a triple quadrupole GC-MS/MS.
Application of low-temperature CP-Sil 88 column for the isomeric analysis of toxic 2,378-substituted PCDD/Fs in incinerator flyash and sewage sludge using a triple quadrupole GC-MS/MS.
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DOI：
10.1016/j.talanta.2011.09.053
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发表时间：
2011-12
期刊：
影响因子：
6.1
通讯作者：
J. Onwudili;Y. Hajizadeh;S. Zainal;J. Upton;Paul T. Williams
中科院分区：
文献类型：
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作者：
J. Onwudili;Y. Hajizadeh;S. Zainal;J. Upton;Paul T. Williams
使用 CP-Sil 88 色谱柱（50m×0.25mm 内径，0.25μm 膜厚）在污水污泥和焚烧炉飞灰样品中分离和分析了 17 种 2378 取代的多氯二苯并对二恶英和二苯并对呋喃 (PCDD/F) 同系物，最高烘箱温度为 240°C。该色谱柱用于带有 Varian 320-MS 三重四极杆的 Varian 450-GC。校准标准品用于测定气相色谱/质谱 (GC-MS/MS) 系统中 2378 取代的 PCDD/F 同系物的过渡化学性质。每种同系物的五点校准曲线显示出非常好的线性，R2 值大于 0.999。标记化合物的回收率为 50% 至 120%。参考粉煤灰 (BCR-490) 和参考污水污泥 (BCR-677) 的分析结果与认证值进行了很好的比较，I-TEQ（国际有毒当量）的百分比偏差分别为 4.93% 和 0.53%。 “真实”飞灰样本的结果强调了在减少焚烧炉二恶英排放方面所取得的进展水平；旧焚烧炉飞灰中的 PCDD/F 浓度比现代焚烧炉高得多。此外，来自两个英国废水处理厂 (WWTP) 的“真实”污水污泥中 PCDD/F 的浓度分布显示，其中一个处理厂的 PCDD/F 总含量为 314 ngI-TEQkg−1，而另一个的 PCDD/F 总含量为 53 ngI-TEQkg−1。在 18 个月的运行期间，没有观察到低温色谱柱的分析性能出现明显损失。
The seventeen 2378-substituted polychlorinated dibenzo-p-dioxins and dibenzo-p-furans (PCDD/Fs) congeners have been separated and analyzed in sewage sludge and incinerator flyash samples using a CP-Sil 88 column (50m×0.25mm I.D., 0.25μm film thickness) operating at a maximum oven temperature of 240°C. The column was used on a Varian 450-GC with a Varian 320-MS Triple Quadrupole. Calibration standards were used to determine the transition chemistries of the 2378-substituted PCDD/F congeners in the gas chromatography/mass spectrometry (GC–MS/MS) system. The five-point calibration curve for each of the congeners showed very good linearity with R2values greater than 0.999. The recovery of labelled compounds ranged from 50% to 120%. Analytical results from a reference flyash (BCR-490) and a reference sewage sludge (BCR-677) compared very well with the certified values, giving percentage deviations in I-TEQ (international toxic equivalents) of 4.93% and 0.53%, respectively. Results from ‘real’ flyash samples underscored the level of progress made in the abatement of dioxin emissions from incinerators; the old incinerator flyash contained much higher PCDD/F concentrations than the modern one. In addition, the concentrations profiles of PCDD/Fs in the ‘real’ sewage sludge from two UK wastewater treatment plants (WWTPs) showed that one contained a total PCDD/Fs content of 314ngI-TEQkg−1, while the other gave a total of 53ngI-TEQkg−1. Over an 18-month period of operation, no significant loss of analytical performance was observed from the low-temperature column.