Electrochemical treatment of olive mill wastewater: Treatment extent and effluent phenolic compounds monitoring using some uncommon analytical tools

Problems related with industrials effluents can be divided in two parts: (1) their toxicity associated to their chemical content which should be removed before discharging the wastewater into the receptor media; (2) and the second part is linked to the difficulties of pollution characterisation and monitoring caused by the complexity of these matrixes. This investigation deals with these two aspects, an electrochemical treatment method of an olive mill wastewater (OMW) under platinized expanded titanium electrodes using a modified Grignard reactor for toxicity removal as well as the exploration of the use of some specific analytical tools to monitor effluent phenolic compounds elimination. The results showed that electrochemical oxidation is able to remove/mitigate the OMW pollution. Indeed, 87% of OMW color was removed and all aromatic compounds were disappeared from the solution by anodic oxidation. Moreover, 55% of the chemical oxygen demand (COD) and the total organic carbon (TOC) were reduced. On the other hand, UV- Visible spectrophotometry, Gaz chromatography/mass spectrometry, cyclic voltammetry and 13 C Nuclear Magnetic Resonance (NMR) showed that the used treatment seems efficaciously to eliminate phenolic compounds from OMW. It was concluded that electrochemical oxidation in a modified Grignard reactor is a promising process for the destruction of all phenolic compounds present in OMW. Among the monitoring analytical tools applied, cyclic voltammetry and 13 C NMR are among the techniques that are introduced for the first time to control the advancement of the OMW treatment and gave a close insight on polyphenols disappearance.     

顶空／气相色谱-质谱法测定水中四乙基铅

建立了顶空,气相色谱-质谱法测定水中四乙基铅方法。水样中的四乙基铅直接顶空进样,质谱分析。实验结果表明,在0．10-5．00μg几范围内线性关系良好,方法检出限为0．02μg/L,得到了良好的分离效果与较高的灵敏度和精密度。方法简便快捷,能达到《生活饮用水卫生规范》（GB/T5750．8—2006）中规定的要求。     

GC/MS法测定生物样品中多溴联苯醚类化合物

本研究建立了多溴联苯醚（PBDEs）生物样品分析方法,获得了优化的前处理条件、气相色谱和质谱检测条件.对定性定量方法及实验条件必须满足的要求进行了评价.通过质量控制（quality control, QC）对整个方法进行了验证.结果证明,本研究所建立的分析方法满足生物样品PBDEs测定的要求,回收率在50.5%～112.3%之间,回收率相对标准偏差在5.3%～9.9%之间,方法检测限在7.1～161.8 pg/g之间.在建立的方法基础上,测定了部分养殖和野生鱼类样品,测得的野生鳜鱼和鲫鱼以及2个养殖鲈鱼样品的结果分别为1.53、1.11、5.31和6.15 ng/g(干重),其中主要的同族体为BDE47.     

STAC有机膨润土的表征及其处理垃圾渗滤液的研究

文章以钙基蒙脱石为原料,经钠化后与十八烷基三甲基氯化铵(又称1831,简称STAC)进行离子交换反应,合成有机膨润土,通过XRD、IR 、SEM等测试仪,对有机膨润土的结构进行了分析,同时利用改性后的STAC有机膨润土对某垃圾填埋场中的渗滤液进行处理,用GC/MS对处理前后垃圾渗滤液中主要有机组分进行了分析,结果表明,...     

戊唑醇残留分析方法实验室内质量控制研究

文章确立了小麦、香蕉中戊唑醇残留检测方法,小麦样品加水10 mL用丙酮为萃取溶剂,石油醚液液分配,中性氧化铝柱层析净化,用气相色谱(GC-NPD)检测。香蕉样品加水5 mL用丙酮为萃取溶剂,石油醚液液分配,浓缩后用气相色谱(GC-NPD)检测。分别设置不同时间批次,同一批次间的平行样及实验室内人员分析,分别从方法灵敏度、方法准确度、方法精密度及其质量控制图、标准工作液的稳定性来探讨该方法的可靠性,结果表明该方法可以作为香蕉和小麦种戊唑醇残留检测的标准分析方法。     

用GC/MS分析火灾后苯板产生固体废物中的有机物

采用GC/MS方法对某苯板厂火灾后产生的固体废弃物进行检测分析.结果表明,在苯板火灾后产生的固体废弃物中检测出61种化合物,其中被美国EPA列入优先污染物的苯系物、萘和蒽等占总有机物12.2％.     

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.     

Solid‐phase extraction and GC analyses of select agricultural pesticides and metabolites in stream water

Abstract

The occurrence of agricultural pesticides in surface waters around the USA has created a concern over the status of safe drinking water. Solid‐phase extraction (SPE) or liquid‐liquid extraction (LLE) is usually employed to concentrate trace levels of pesticides in water samples to concentrations that are measurable with advanced chromatographic instruments. We describe here a SPE and capillary gas chromatographic (GC) procedure to extract and concentrate trace levels of select agricultural pesticides and metabolites from stream water. Our SPE and GC method provides high sensitivity, with recoveries between 85% to 95%, and high reproducibility for 9 of the pesticides studied. The described method provided marginal recoveries of 19 and 60% for the atrazine metabolites.     

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。     

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。