Experimental investigation of the efficiency of triple rinsing of agricultural containers regarding their characterization as non-hazardous wastes

The efficiency of water rinsing for removing fenthion from non-combustible used pesticide containers was investigated. Four hundred empty containers from four olive oil producing areas in Greece were studied. Following triple rinsing cleaning procedures, the amount of fenthion retained in the container ranged from 0.01% to 0.1% w/w of its initial concentration. Extraction was accomplished with acetone, and the extracts were analyzed with a capillary gas chromatographic system coupled with flame ionization detector. The results obtained showed that triple rinsing is an effective procedure for removing fenthion from used pesticide containers, since the remaining pesticide concentration was below the legislated threshold value. Consequently, the containers can be handled as non-hazardous solid wastes.     

气相色谱法测定大气中乙酸乙酯和甲基丙烯酸甲酯

建立了用气相色谱法测定大气中乙酸乙酯和甲基丙烯酸甲酯的方法。大气中乙酸乙酯和甲基丙烯酸甲酯活性炭吸附,二硫化碳解吸,DB-200毛细管柱分离,直接进样分析,氢火焰离子化检测器检测,时间定性,峰面积定量。本方法前处理简便,分离度好,分析灵敏度高,满足环境分析要求。     

顶空气相色谱法同时测定空气中甲醇和乙醇

顶空气相色谱测定空气中甲醇和乙醇含量,以蒸馏水吸收空气中甲醇和乙醇,顶空进样经DB-624毛细管柱分离,氢火焰离子化检测器检测。实际操作证明,该法能满足工业废气和空气中的甲醇和乙醇的监测。     

离子色谱法测定环境空气中丁酸

建立了用离子色谱法测定环境空气中丁酸的新方法。对实际样品进行分析,丁酸的回收率为94．5％-103．8％,当采样体积为60L时环境空气中丁酸的检出限为0．003mg／m^3。本方法分析速度快,所需样品量少,且无需复杂的前处理,简便、灵敏、可靠。     

Application of comprehensive two-dimensional gas chromatography with mass spectrometric detection for the analysis of selected drug residues in wastewater and surface water

Pharmaceutical residues have become tightly controlled environmental contaminants in recent years, due to their increasing concentration in environmental components. This is mainly caused by their high level of production and everyday consumption. Therefore there is a need to apply new and sufficiently sensitive analytical methods, which can detect the presence of these contaminants even in very low concentrations. This study is focused on the application of a reliable analytical method for the analysis of 10 selected drug residues, mainly from the group of non-steroidal anti-inflammatory drugs (salicylic acid, acetylsalicylic acid, clofibric acid, ibuprofen, acetaminophen, caffeine, naproxen, mefenamic acid, ketoprofen, and dicofenac), in wastewaters and surface waters. This analytical method is based on solid phase extraction, derivatization by N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) and finally analysis by comprehensive two-dimensional gas chromatography with Time-of-Flight mass spectrometric detection (GC×GC- TOF MS). Detection limits ranged from 0.18 to 5 ng/L depending on the compound and selected matrix. The method was successfully applied for detection of the presence of selected pharmaceuticals in the Svratka River and in wastewater from the wastewater treatment plant in Brno-Modrice, Czech Republic. The concentration of pharmaceuticals varied from one to several hundreds of ng/L in surface water and from one to several tens of μg/L in wastewater.     

氟虫双酰胺在水稻和稻田中的残留动态研究

采用超高效液相色谱法(UPLC)测定了氟虫双酰胺19.8%悬浮剂(SC)在水稻及稻田环境中的残留动态.结果表明,当氟虫双酰胺及其代谢产物NNI-des-iodo的添加量为0.05～1.0 mg·kg-1时,其在水稻田土壤、田水、稻秆、稻米和稻壳中的平均回收率为78.2%～104.8%,变异系数为1.1%～4.4%.氟虫双酰胺在2011年三地(福建福州、天津、江苏南京)的稻田水中的降解半衰期为9.8～17.3 d,土壤中10.8～22.4 d,植株中7.6～17.3 d,其在稻田水样品中检出了代谢产物NNI-des-iodo,而在土壤和植株样品中未检出.在推荐使用剂量下,于末次施药10 d后,氟虫双酰胺在水稻稻米中的残留量均低于美国规定的在稻谷上的最大残留允许量(0.5 mg·kg-1).     

微波-亚临界水萃取底泥中两种多氯联苯的研究

微波亚临界水萃取模拟土样中的2,3-二氯联苯和3,3′-二氯联苯,用气相色谱进行分析。与亚临界水萃取方法相比,该法缩短了萃取时间,分析物的萃取回收率有所提高。对微波亚临界水的萃取条件进行优化,确定了最佳萃取条件为时间20min、温度区段为210℃～225℃。方法对长江镇江段内江的底泥中的多氯联苯进行分析,测定结果与索氏提取-GC分析结果吻合,且不受底泥中腐殖质等有机物影响。     

超声波提取-GC/MS法测定生物体内硝基苯类化合物

以洪泽湖中6种代表性生物为研究对象，采用超声波法提取样品中硝基苯类化合物，用凝胶色谱净化、浓缩，气相色谱／质谱联用法测定。该法与索氏提取法在同等试验条件下进行加标回收试验，前者回收率高且稳定，简便可行。方法检出限为0．008μg／g～0．030μg／g，平均加标回收率为76．5％～109％，重复测定3次的RSD为1．5％～13．0％。     

顶空进样-气相色谱法测定大气中吡啶的研究

采用硫酸溶液为吸收液,顶空进样气相色谱法测定大气中的吡啶,毛细管柱分离,FID检测器分析。吡啶标准溶液在0～98.3 mg/L范围内线性良好,当采样体积为30 L时,最低检出质量浓度为0.006 mg/m³,标准溶液平行测定的RSD≤3.1%,加标回收率为95.3%～99.6%。     

煤炭自燃指标性气体确定的实验研究

矿井火灾是矿井五大灾害之一,煤炭自燃则是矿井火灾最主要的起因。为了了解煤炭氧化、自燃规律,本文采用TG-DSC技术研究了不同煤种在水分蒸发、吸氧增重、受热分解及燃烧等不同氧化阶段的氧化特征值;并采用TG-DSC-GC联用技术研究了不同煤种在整个氧化阶段的气体产物生成规律及其特征。在煤的低温氧化阶段,找出了CO等可作为判别煤自燃的指标性气体及C2H4等辅助指标性气体;并得出了各煤种氧化阶段的耗氧规律。