固定源废气中二噁英及多氯联苯、溴代阻燃剂和溴代二噁英的分析

Determination of Polychlorinated Dibenzo-p-dioxins / Dibenzofurans,Dioxin Like Polychlorinated Biphenyls,Brominated Flame Retardants and Polybrominated Dibenzo-p-dioxins / Dibenzofurans in Flue Gas from Stationary Source

建立了同时分离分析固定源废气中二噁英（PCDD/Fs）、二噁英类多氯联苯（dl-PCBs）、溴代阻燃剂（BFRs）和溴代二噁英（PBDD/Fs）的方法。废气样品经甲苯索氏提取,硫酸处理和多层硅胶柱净化后,应用活性炭分散硅胶翻转淋洗技术分离4类目标物。气相色谱使用耐高温薄膜短色谱柱配合高压进样,高分辨质谱使用低能量电离,一次性测定高/低溴代化合物。方法检出限分别为：PCDD/Fs 0.081-1.2 pg、dl-PCBs0.10-0.32 pg、多溴联苯醚（PBDEs）0.14-12 pg、新型BFRs 0.26-16 pg、四-七溴代PBDD/Fs 0.44-3.6 pg、八溴代PBDD/Fs（OBDD/F）8.2-12 pg。废气空白基质加标回收率（RSD）分别为：PCDD/Fs 88%-115%（2.9%-6.1%）、dl-PCBs 84%-118%（3.2%-10%）、PBDEs 71%-135%（2.1%-18%）、新型BFRs 71%-114%（2.9%-7.4%）、四-七溴代PBDD/Fs 83%-127%（5.2%-10%）、OBDD/F 52%-149%（23%-24%）。将本方法用于废气样品分析,所有质量控制指标均符合相关标准规定。

A method for simultaneous determination of PCDDs,dl-PCBs,BFRs and PBDD / Fs in flue gas from stationary source was developed. The sample was extracted by Soxhlet apparatus with toluene,and followed by purification through sulfuric acid partition and multi-layer silica gel column separation. The target compounds were then all separated by passing through the active carbon-dispersed silica gel column and reversal eluting. Gas chromatography coupled with a thermostable capillary column（ short length, thin stationary phase film） was operated at pulse injection mode. High resolution mass spectrometry set at lowelectron-energy ionization was used for quantification. The high- and low-brominated compounds were determined simultaneously. The detection limits of this method were 0. 081- 1. 2 pg for PCDD / Fs,0. 10-0. 32 pg for dl-PCBs,0. 14-12 pg for PBDEs,0. 26-16 pg for new BFRs,0. 44-3. 6 pg for tetra- to heptaBDD / Fs and 8. 2- 12 pg for OBDD / F. Recoveries（ RSDs） in spiked flue gas samples were 88%- 115%（ 2. 9%-6. 1%） for PCDD/Fs,84%-118%（ 3. 2%-10%） for dl-PCBs,71%-135%（ 2. 1%-18%） for PBDEs,71%-114%（ 2. 9%-7. 4%） for new BFRs,83%-127%（ 5. 2%-10%） for tetra- to hepta-BDD /Fs and 52%- 149%（ 23%- 24%） for OBDD / F. All quality control data fell within the acceptable range specified in analysis standards for flue gas.