固相萃取-气质联用法测定固体废物浸出液中的二硝基苯

建立了一种利用固相萃取法对固体废物浸出液(TCLP)中二硝基苯进行萃取,DB-5石英毛细管柱(30 m×0.25 mm×0.25μm)进行分离,质谱检测器检测二硝基苯的方法。方法在0.002 0~0.020 0 mg/L之间线性关系良好,二硝基苯三种同分异构体的检出限均为0.5μg/L,模拟样品加标回收率为93%~96%,RSD≤2%;实际固体废物样品测定的加标回收率为95%~98%。     

气相色谱-质谱法测定沉积物中的有机氯和多氯联苯

采用加速溶剂萃取法提取沉积物中的有机氯和多氯联苯,提取液用凝胶色谱法净化后用气相色谱-质谱法测定。方法在5.00μg/L~200μg/L范围内线性良好,当取样量为10.0 g时,方法检出限为0.03μg/kg~0.37μg/kg,空白样品2个质量比水平的加标回收率为70.8%~121%,测定结果的RSD为2.7%~11.5%。用该方法测定实际样品,结果 12个抽检的沉积物样品中多氯联苯均未检出,9个样品中有机氯检出。     

固相微萃取-气质联用法测定水中痕量土臭素和二甲基异崁醇

采用固相微萃-气相色谱/质谱法(SPME-GC/MS)对GSM和2-MIB进行富集检测。实验对萃取富集和仪器条件进行了优化,得出最佳实验条件：NaCl投加量30%,萃取温度65℃,萃取时间40 min,解吸3 min,不分流进样,SIM模式采集数据。实验还对萃取头的使用次数和维护进行了探讨。利用已经建立的SPME-GC/MS法对佛山市28家水厂的出厂水和原水、佛山典型景观千灯湖和亚艺公园湖水进行普查。该法具有操作简单快速、能实现自动化连续检测、准确、灵敏度高等特点,适用于饮用水中嗅味物质定性和定量。     

Pyrolysis of waste animal fats in a fixed-bed reactor: Production and characterization of bio-oil and bio-char

Several animal (lamb, poultry and swine) fatty wastes were pyrolyzed under nitrogen, in a laboratory scale fixed-bed reactor and the main products (liquid bio-oil, solid bio-char and syngas) were obtained. The purpose of this study is to produce and characterize bio-oil and bio-char obtained from pyrolysis of animal fatty wastes. The maximum production of bio-oil was achieved at a pyrolysis temperature of 500 °C and a heating rate of 5 °C/min. The chemical (GC–MS analyses) and spectroscopic analyses (FTIR analyses) of bio-oil showed that it is a complex mixture consisting of different classes of organic compounds, i.e., hydrocarbons (alkanes, alkenes, cyclic compounds…etc.), carboxylic acids, aldehydes, ketones, esters,…etc. According to fuel properties, produced bio-oils showed good properties, suitable for its use as an engine fuel or as a potential source for synthetic fuels and chemical feedstock. Obtained bio-chars had low carbon content and high ash content which make them unattractive for as renewable source energy.     

便携式GC-MS法快速测定固定污染源废气中的VOCs

采用便携式GC-MS法快速测定固定污染源废气中VOCs,32种VOCs在2×10~(-7)~1×10~(-6)范围内线性良好,方法检出限为2×10~(-9)~1×10~(-8),标准气体样品6次测定结果的RSD为1.9%~19.1%,环境空气样品的加标回收率为66.2%~116%。在实际现场监测固定污染源中VOCs时,使用速查(Survey)功能可初步判断样品浓度,确定稀释倍数。比对试验结果表明,气袋和玻璃注射器采样法对VOCs测定结果无显著性差异。     

气相色谱-质谱联用测定水产品中的合成麝香

利用快速溶剂萃取（ASE）和在线吸附净化,气相色谱-质谱（GC/MS）联用测定水产品中8种合成麝香.以正己烷为萃取溶剂,中性氧化铝为吸附剂,在100℃的温度下对水产品进行萃取.实验结果表明,方法的检测限为0.1—0.5 ng·g-1;在浓度1—80 ng·g-1的范围内,峰面积与样品浓度呈良好线性关系;8种合成麝香的回...     

混凝-生物接触氧化处理合成橡胶碱洗废水

对化学合成橡胶碱洗废水进行了有机组分和可生化性分析，废水主要含有氯甲烷、六甲苯、异丁醇、甲醇等污染物质，生化降解实验中废水TOC可在6d内从60．9mg／L下降至0．0mg／L，可生化降解性好，适于生化处理。选择混凝．生物接触氧化组合工艺对废水进行处理，采用优化条件（pH=8、PAC=40mg／L、PAM=8mg／L）进行混凝，碱洗废水COD去除率为9．95％～72．94％（平均31．51％）；混凝后的碱洗废水与冲洗废水1：5混合进行接触氧化处理，在HRT为36h的情况下，COD去除率为65．6％-72．6％（平均70．4％），出水COD为134～331mg／L，满足企业废水排放市政管网的要求；同时，实验发现COD去除率与COD容积负荷存在指数函数变化关系。     

微波萃取肉类样品中的多氯联苯方法研究

用丙酮和正己烷（1＋1）的混合溶剂做萃取剂，采用微波萃取的方法提取动物肉类中的9个多氯联苯（PCBs）单体，通过弗罗里硅土和氧化铝净化后，在带ECD检测器的气相色谱上测定。取样量为2g时，多氯联苯（PCBs）在GC—ECD上响应的线性范围为11～100ng／g，研究的样品加标测定范围为11—500ng／g，检出限从5．3—13．3ng／g，平均加标回收率在98．7％-118％。     

Multiresidue determination of carbamate,organochlorine, organophosphorus,and dicarboximide pesticides in lettuce by GC/MS

An extraction method based on matrix solid-phase dispersion was developed to determine pirimicarb, methyl parathion, malathion, procymidone, α -endosulfan and β -endosulfan in lettuce using gas chromatography-mass spectrometry. The best results were obtained using 4.0 g of lettuce, 2.0 g of silica as dispersant sorbent, 0.1 g of activated carbon as clean up sorbent and acetonitrile as eluting solvent. The method was validated using lettuce samples fortified with pesticides at six different concentration levels (0.1 to 2.0 mg/kg). Average recoveries (7 replicates) ranged from 50 to 120 %, with relative standard deviations between 0.6 and 8.0 %. Detection and quantification limits for lettuce ranged from 0.01 to 0.02 mg/kg and 0.04 to 0.10 mg/kg, respectively.     

环境中总石油烃的气相色谱分析测定

将总石油烃划分为挥发性汽油类(C6～C10)、可萃取柴油和重油类(C10～C40)两部分,分别建立了通过吹扫捕集、液液萃取和超声溶剂萃取分离富集,气相色谱-火焰离子化检测器(GC-FID)测定环境水体和土壤中总石油烃的分析方法。以汽油、柴油、润滑油标准溶液进行外标校正,以色谱出峰总面积进行定量。汽油类(C6～C10)的检出限分别为0.04mg/L和0.42mg/kg,柴油和重油类(C10～C40)的检出限分别为0.06mg/L和4.9mg/kg。方法的精密度和准确度均良好。