摘要
制备了一种二维的[Zn(benzotriazole)2]n配位聚合物,并经过XRD、SEM及元素分析法的表征,将其用于富集萃取环境水样中的6种重质多环芳烃,该配合物对于含多苯环的化合物显示出较强的吸附力。实验中分别对填料用量、淋洗剂、洗脱剂的种类及用量、穿透体积等参数进行考察,并将其与同等上样量及加标量的C18固相萃取小柱进行对比,建立了水样中6种多环芳烃的气相色谱-质谱联用检测方法。结果表明,使用200mg[Zn(benzotriazole)2]n配合物作为固相萃取填料,以10%甲醇为淋洗剂,0.5mL丙酮和5mL二氯甲烷作为洗脱剂,在上样体积为200mL、流速为4mL/min的条件下,6种多环芳烃均具有较高的回收率。荧蒽(Flan)、苯并(b)荧蒽(BbF)、苯并(g,h,i)芘(BghiP)的质量浓度在20～1000μg/L范围内,苯并(k)荧蒽(BkF)、苯并(a)芘(BaP)、茚并(1,2,3-Cd)芘(InP)在10～500μg/L范围内与峰面积呈良好线性关系,相关系数为0.9968～0.9993。方法的检出限为0.45～10.7ng/L,加标回收率为77%～112%,相对标准偏差为3.8%～8.5%。结果表明,该方法具有成本低、灵敏度高等特点,能够满足实际水样中6种多环芳烃的测定要求。
A kind of 2D [Zn（benzotriazole）2]n coordination polymer was synthesized,and used to concentrate and extract six heavy polycyclic aromatic hydrocarbons（PAHs） in environmental water samples.The prepared coordination polymer was characterized by X-ray powder diffraction（XRD）,scanning electron microscope（SEM） and elemental analysis,and the polymer showed a strong affinity to aromatics.In the experiment,amount of coordination polymer,washing solvent,kind and usage of eluent,flow rate and breakthrough volume were all investigated.The final result was compared to the C18 solid phase extraction（SPE） column with the same sample volume and spiked level,thus an analytical method by gas chromatography-mass spectrometry（GC-MS） was established to determinate six PAHs in water samples.A good extraction efficiency could be obtained by using 200 mg coordination polymer as SPE adsorbent,10% methanol as washing solvent,0.5 mL acetone and 5 mL dichloromethane as eluent,with a flow rate of 4 mL/min and a sample volume of 200 mL.Good linearities were obtained over the ranges of 20-1 000 μg/L for fluranthene（Flan）,benzo[b] fluoranthene（BbF） and benzoperylene（BghiP）,and 10-500 μg/L for benzo[k] fluranthene（BkF）,benzo[a]pyrene（BaP） and indeol[1,2,3-Cd]pyrene（InP）,with correlation coefficients（r2） of 0.996 8-0.999 3.The detection limits ranged from 0.45 ng/L to 10.7 ng/L.The spiked recoveries of six PAHs were in the range of 77%-112% with RSDs of 3.8%-8.5%.The established method showed advantages of low-cost and high-sensitivity,and could meet the requirements for determination of six PAHs in real environmental water samples.
出处
《分析测试学报》
CAS
CSCD
北大核心
2013年第5期575-580,共6页
Journal of Instrumental Analysis
基金
国家自然科学基金资助项目(21207121)
广东省科技计划项目(2011A030200001)
