顶空气相色谱法测定水中苯胺

采用顶空气相色谱法测定水中的苯胺,对盐类及其用量、顶空温度等条件进行了优化。当加入5 g NaOH,80℃进行顶空时,苯胺在0.02~0.50 mg/L范围内线性良好,方法检出限0.002 mg/L,样品加标平行测定的RSD<5.0%,回收率>95%。方法操作简单,检出限低,适用于水体中苯胺的测定。     

固定污染源废气中磷酸雾测定方法研究

目前,对固定污染源废气中磷酸雾的检测并无统一的方法,相关含磷污染物的控制指标主要是磷化氢、单质磷以及五氧化二磷。在调研国内外分析方法及相关文献的基础上,通过对几种典型含磷污染源的实样测试,提出了固定污染源废气中磷酸雾的检测方法。结果表明,使用石英滤筒捕集固定污染源废气中的磷酸雾,采样效率可达98%以上。捕集到的总磷酸雾不仅包含磷酸,还包含磷酸盐以及含磷氧化物等,是一项综合指标。该指标能够反映含磷污染物的排放特征,可为未来此类污染物的排放控制提供依据。     

Electrospray Ionization Mass Spectrometry (ESI-MS) monitoring of the photolysis of diazinon in aqueous solution: Degradation route and toxicity of by-products against Artemia salina

The photolytic degradation of diazinon, an organophosphorus pesticide, in aqueous medium under assorted pH values was continuously monitored by direct infusion electrospray ionization mass spectrometry (ESI-MS). The results indicated that the UV radiation was quite efficient in promoting the pesticide degradation at the three pH levels evaluated (5, 7 and 8). The m/z of the most abundant ions observed in the mass spectra (MS), in conjunction with the fragmentation patterns of such ionic species (MS/MS data), made possible the proposition of chemical structures for the main by-products formed. As a result, routes for the photodegradation of diazinon in aqueous solution could thus be suggested. In the assays using Artemia salina (brine shrimp) it was verified that the photodegradation products exhibited much lower toxicity than the primary substrate. Aiming at mimicking the conditions ordinarily found in water treatment plants, an additional series of tests was conducted with a solution containing sodium hypochlorite and diazinon. This solution, when not exposed to UV radiation, exhibited high toxicity against the microorganisms. Under the influence of UV radiation, however, the toxicity rates decreased dramatically. This result is relevant because it points toward the confident application of UV radiation to neutralize the deleterious effects caused by diazinon (and perhaps other organophosphorus pesticides) as well as sodium hypochlorite to the environment.     

Method validation for control determination of mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry

A method for the determination of total mercury in fresh fish and shrimp samples by solid sampling thermal decomposition/amalgamation atomic absorption spectrometry (TDA AAS) has been validated following international foodstuff protocols in order to fulfill the Brazilian National Residue Control Plan. The experimental parameters have been previously studied and optimized according to specific legislation on validation and inorganic contaminants in foodstuff. Linearity, sensitivity, specificity, detection and quantification limits, precision (repeatability and within-laboratory reproducibility), robustness as well as accuracy of the method have been evaluated. Linearity of response was satisfactory for the two range concentrations available on the TDA AAS equipment, between approximately 25.0 and 200.0 μg kg^?1 (square regression) and 250.0 and 2000.0 μg kg^?1 (linear regression) of mercury. The residues for both ranges were homoscedastic and independent, with normal distribution. Correlation coefficients obtained for these ranges were higher than 0.995. Limits of quantification (LOQ) and of detection of the method (LDM), based on signal standard deviation (SD) for a low-in-mercury sample, were 3.0 and 1.0 μg kg^?1, respectively. Repeatability of the method was better than 4%. Within-laboratory reproducibility achieved a relative SD better than 6%. Robustness of the current method was evaluated and pointed sample mass as a significant factor. Accuracy (assessed as the analyte recovery) was calculated on basis of the repeatability, and ranged from 89% to 99%. The obtained results showed the suitability of the present method for direct mercury measurement in fresh fish and shrimp samples and the importance of monitoring the analysis conditions for food control purposes. Additionally, the competence of this method was recognized by accreditation under the standard ISO/IEC 17025.     

电镀污泥的还原焙烧-酸浸

将电镀污泥作为一种重要的重金属资源加以回收利用,逐渐成为了国内外研究的重点。以电镀污泥为研究对象,在不同的温度及不同的焙烧时间下进行直接焙烧和还原焙烧,并对焙烧底渣进行酸浸,分别研究了污泥减量率以及Cu、Ni、Zn和Cr 4种重金属的含量和浸出率,并探索了还原剂(煤粉)和催化剂(CaCO3)投加量的影响。实验结果表明,原始电镀污泥中,Cu含量最高,达到10.05%,因此,电镀污泥中Cu具有回收价值;焙烧后电镀污泥得到了减量化,同时污泥中的金属得到了富集;还原焙烧比直接焙烧更有利于Cu的选择性浸出,当煤粉投加量为10%,CaCO3投加量为0.5%,在700℃下焙烧20 min时,Cu的浸出率达到98.73%,Cu的含量达到15.07%。     

石化废水挥发性有机物逸散量的估算方法

总结了实测法、物料衡算法、模型法、排放系数法、工程估算法等国内外石化废水挥发性有机物(VOCs)逸散量估算方法的主要特点及适用范围。应用排放系数法和实测法估算国内某石化厂废水收集处理系统VOCs逸散量为354.26 t/a。根据估算方法的实际应用研究,建议物料衡算法中废水油相VOCs逸散可结合油相敞口面积和油相性质,提供废水油相的排放系数;应用Water 9软件估算含油膜废水设施逸散量时,应单独估算油膜VOCs逸散量;建议排放系数法中废水收集系统排水口、检查井未密闭VOCs排放系数均确定为0.032 kg/h(每个逸散源),废水处理系统油水分离器、气浮装置按进水中石油类浓度的大小,分别提供VOCs排放系数。     

臭氧氧化四种偶氮染料废水的效果研究

以酸性大红、中性枣红、阳离子红、活性黑5四种模拟印染废水开展O3氧化偶氮染料的效果研究.实验中发现O3对染料具有非常好的脱色效果,30 min后除中性枣红外其他三种染料脱色率接近100％,但是单独O3的TOC去除率不高.光谱扫描表明,处理后染料的特征吸收峰很快消失,而紫外光区的吸收峰变化很小,推测O3氧化以直接氧化为主,打开了染料分子的发色基团,但并未将染料分子彻底氧化.还应加强O3氧化能力、彻底矿化去除污染物的研究.     

垃圾填埋场空气中微量挥发性有机污染物的分析

使用充填有Ｔｅｎａｘ、碳分子筛和硅胶的多层热解吸金属管,以０．２０Ｌ／ｍ ｉｎ 的流速采集垃圾填埋场空气样品,以Ｔｅｋ－ｍ ａｒ３０００／６０３２ 和ＨＰ５８９０／５９７２ ＧＣ－ＭＳＤ 组合仪器进行分析,共检测出６３ 种挥发性有机污染物（ＶＯＣｓ）,其中有１６ 种为ＵＳＥＰＡ 优先控制污染物;通过对大多数化合物进行定量分析所得的结果表明,以苯及其衍生物含量最高,为７．９４～２０２．５５μｇ／ｍ³;其它氯代有机物含量虽然相对较低,但由于它们的毒性,因此其对环境的影响亦不容忽视．     

土壤中多氯联苯监测分析方法

文章综述了国内外现有的土壤中多氯联苯的标准监测方法及其它文献报道方法,评述了各方法的优、缺点,介绍了本文所研制的适用性强、能满足监测需求的方法.     

FTIR对大气颗粒物PM2.5中硝酸盐的定量分析

大气细颗粒物PM2.5作为复合型大气污染的核心污染物之一备受人们关注,NO3-作为其中水溶性离子的主要成分之一,对大气降水和人体健康有着重要影响,因此实现对其快速可靠的检测是一项重要的研究工作.基于傅里叶变换红外光谱技术的优点,采用液态制膜的方法测量比较了颗粒物中NO3-和NH4NO3中NO3-的红外光谱图,结果保持一致.在此基础上测量了一系列不同质量NO3-的红外光谱,拟合其吸光度与质量,相关性达到0.994 8,线性范围为7.82～73.78μg,实现了对其定标.然后利用样品溶液与采样膜样品质量的对应关系,直接测量采样膜上样品的红外谱图,分析了合肥地区2012-03-20～2012-04-20为期1个月的硝酸根质量浓度,平均质量浓度为4.171 3μg.m-3.