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室内空气和降尘中邻苯二甲酸酯的分析研究
Research of Analyzing Phthalates in Indoor Air and Dust
【作者】 沈婷;
【导师】 王小逸;
【作者基本信息】 北京工业大学 , 环境科学, 2009, 硕士
【摘要】 研究了测定室内空气和降尘中的邻苯二甲酸酯含量的分析方法。对于DMP、DEP、BBP、DBP、DCHP、DEHP、DnOP这七种邻苯二甲酸酯,空气样品使用PS小柱(Waters)采集,并用5ml甲醇-丙酮-乙醚(5:5:90)进行洗脱;降尘样品使用毛刷进行采样,并用20ml甲醇-丙酮-乙醚(5:5:90)对HLB小柱进行固相萃取。利用HPLC进行分析,每次进样20μl。HPLC的测定条件为:初始流动相流速0.6ml/min;梯度洗脱(A高纯水,B甲醇)方式:0-5min,甲醇-水(85∶15,V/V);至6min时,B达到92%,流动相流速变为0.8ml/min且保持不变,到10min时,B达到100%。全程共17min。通过方法的实验研究得到:室内空气分析方法中BBP、DBP、DCHP、DEHP、DnOP的回收率是96.82%~103.9%之间,DMP和DEP的回收率分别是57.59%和68.64%;室内降尘分析方法中,当各邻苯二甲酸酯的量为30mg/kg时,BBP、DBP、DCHP、DEHP、DnOP的回收率是88.45%~122.0%之间,DMP和DEP的回收率分别是27.38%和44.97%;当各邻苯二甲酸酯的量为500mg/kg时,BBP、DBP、DCHP、DEHP、DnOP的回收率是96.35%~100.7%之间,DMP和DEP的回收率分别是56.29%和67.10%。邻苯二甲酸酯在空气和降尘样品的检测限分别是2ng/m3和0.06mg/kg。本文对来自于北京市区内30个房间的空气和降尘样品(各30个)进行了测定。在这些样品中,主要检测到BBP、DBP、DCHP、DEHP这四类邻苯二甲酸酯,空气中这四类邻苯二甲酸酯浓度的中值依次是988ng/m3、748ng/m3、949ng/m3、1004ng/m3、246ng/m3。此外,DEHP在室内降尘中浓度最高,占到降尘中邻苯二甲酸酯类的80%左右,中值是250mg/kg(范围:83~6232mg/kg)。经过初步分析,认为室内邻苯二甲酸酯的污染程度和类型与室内增塑剂产品的数量、室内清洁通风情况以及成员性别有关。对比欧美而言,我国室内空气中邻苯二甲酸酯类污染十分严重,应该引起足够重视。
【Abstract】 In this thesis, the separations and analysis method of phthalate esters in indoor air and dust was studied.The phthalate esters mainly included dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl-n-butyl phthalate (BBP), dibutyl phthalate (DBP), dicyclohexyl phthalate (DCHP), di-2-ethylhexyl phthalate (DEHP), Di-n-octyl phthalate (DnOP). Seven phthalate esters present in air were collected using a Waters Sep-Pak PS Air cartridge and SPE (Solid Phase Extraction) with methanol-acetone- ether (5:5:90), the range of recoveries of the five phthalate esters (BBP、DBP、DCHP、DEHP、DnOP) were 96.82%~103.9%, the recoveries of DMP and DEP were 57.59% and 68.64%. Seven phthalate esters were collected from the dust using solid phase extraction method on the HLB cartridge (6cc, 60mg) under the optimum condition. When the concentration of each phthalate ester was at 30mg/kg, the recovery of phthalate esters (BBP、DBP、DCHP、DEHP、DnOP) ranged from 88.45% to 122.0%, the recoveries of DMP and DEP were 27.38% and 44.97%. When the concentration of each phthalate ester was at 500mg/kg, the five phthalate esters ranged from 96.35% to 100.7%, and the recoveries of DMP and DEP were 56.29% and 67.10%. A quantity of 20μl of each extract was analyzed by HPLC. The determination limits were 2ng/m3 in indoor air and 0.06mg/kg in dust, respectively. The optimized results of HPLC were as follows: detection wave was 224nm. Use gradient elution.At the beginning,the flow phase was V(methanol): V(H2O)=85:15, kept it for 5min and rate was 0.6ml/min, then the proportion of methanol rose to 92% and rate was 0.8ml/min at the 6min, finally the proportion rose to 100% at the 10min, kept it for 7min.High Performance Liquid Chromatography (HPLC), was used to quantify Phthalate esters (PAEs) in settled indoor air and dust from 30 residences which concluded 10 apartments, 10 offices and 10 dorms in Beijing. BBP、DBP、DCHP、DEHP were found in each sample. These phthalates had the high concentration in indoor air, with median values 988ng/m3, 748ng/m3, 949ng/m3, 1004ng/m3 and 246ng/m3 in turns. Of phthalates, the main phthalate in dust was di-2-ethylhexyl phthalate (DEHP), with around 80% of all values and median values of 250mg/kg (range: 83~6232mg/kg).We conducted a preliminary analysis of the results and found the phthalate levels and major characteristics were interrelated with the quantities of phthalate products, cleaning habits, ventilation and the gender of members. In contrast with Europe and the United States, our indoor air pollution phthalates is very serious and should be attracted full attention.