Improvement of an efficient separation method for chemicals in diesel exhaust particles: analysis for nitrophenols

GOAL, SCOPE, AND BACKGROUND: Diesel exhaust is believed to consist of thousands of organic constituents and is a major cause of urban pollution. We recently reported that a systematic separation procedure involving successive solvent extractions, followed by repeated column chromatography, resulted in the isolation of vasodilatory active nitrophenols. These findings indicated that the estimation of the amount of nitrophenols in the environment is important to evaluate their effect on human health. The isolation procedure, however, involved successive solvent extractions followed by tedious, repeated chromatography, resulting in poor fractionation and in a significant loss of accuracy and reliability. Therefore, it was crucial to develop an alternative, efficient, and reliable analytical method. Here, we describe a facile and efficient acid-base extraction procedure for the analysis of nitrophenols. MATERIALS AND METHODS: Diesel exhaust particles (DEP) were collected from the exhaust of a 4JB1-type engine (ISUZU Automobile Co., Tokyo, Japan). Gas chromatography-mass spectrometry (GC-MS) analysis was performed with a GCMS-QP2010 instrument (Shimadzu, Kyoto, Japan). RESULTS: A solution of DEP in 1-butanol was extracted with aqueous NaOH to afford a nitrophenol-rich oily extract. The resulting oil was methylated with trimethylsilyldiazomethane and subsequently subjected to GC-MS analysis, revealing that 4-nitrophenol, 3-methyl-4-nitrophenol, 2-methyl-4-nitrophenol, and 4-nitro-3-phenylphenol were present in significantly higher concentrations than those reported previously. DISCUSSION: Simple acid-base extraction followed by the direct analysis of the resulting extract by GC-MS gave only broad peaks of nitrophenols with a poor detection limit, while the GC-MS analysis of the sample pretreated with (trimethylsilyl)diazomethane gave satisfactorily clear chromatograms with sharp peaks and with a significantly lowered detection limit (0.5 ng/ml, approximately 100 times). CONCLUSION: The present method involving an acid-base extraction, in situ derivatization, and GC-MS analysis has shown to be a simple, efficient, and reliable method for the isolation and identification of the chemical substances in DEP.     

碱熔融法合成NaA和NaX型粉煤灰沸石的品质表征

以粉煤灰为原料采用碱熔融法合成了2种单一沸石矿物种的NaA和NaX型沸石,并对产物的结构、性能和应用指标进行了详细表征.经x射线衍射和IR光谱分析,表明合成产物是无杂晶生成的NaA和NaX型沸石相;在扫描电镜观察下,产物分别具有NaA和NaX型沸石的立方体和八面体晶体骨架结构.DTA分析表明了合成产物中沸石水的存在,且产物热稳定性较好.通过对比,粉煤灰合成的NaA和NaX型沸石的比表面积达到了相应商品沸石的66.9%和83.6%;孔容为41.1%和70.2%;阳离子交换容量(CEC,cation exchange capacity)为82.93%和84.31%.通过比较化学组成表明,大规模应用合成产物不会对环境造成危害.     

甲胺生产废水中氨氮资源化的试验研究

利用MgSO4·7H2O和Na2HPO4·12H2O作为试验药剂,通过正交试验和单因素优化试验,对化学沉淀法处理甲胺生产废水中氨氮的工艺条件进行优化.结果表明,在pH=9.4、反应时间15 min、搅拌速度150 r/min、Mg:N(摩尔比值)=1.1、P:N(摩尔比值)=1.0时,化学沉淀法处理300 mL甲胺生产废水,氨氮去除率维持在92%以上,COD去除率可达37%以上.同时为验证工艺条件适应性和沉淀物(MgNH4PO4)作为农作物肥料使用的价值性,对最优条件下得到的沉淀物进行研究.与MgNH4PO4纯度为100%相比,沉淀物MgNH4PO4纯度达到86%以上.因此,化学沉淀法处理氨氮不仅具有良好的效果,而且得到的MgNH4PO4含有较高N、P,可以用作农作物肥料.     

压力板仪法测土-水特征曲线试验研究

非饱和土土-水特征曲线(SWCC)表示了土中含水量与吸力之间的关系。针对非饱和土干-湿循环过程中的吸力变化特征,开展试验研究。采用体积压力板仪实现非饱和土的脱湿和吸湿过程。试验成果显示:(1)土-水特征曲线是不稳定的,它与土体含水率的变化路径有关;(2)在干湿循环过程中,相同的基质吸力具有不同的含水量。     

Extended geometric method: a simple approach to derive adsorption rate constants of Langmuir-Freundlich kinetics

A new and simple equation has been presented here for calculation of adsorption and desorption rate constants of Langmuir-Freundlich kinetic equation. The derivation of new equation is on the basis of extension and correction to the geometric method which has been presented by Kuan et al. [Kuan, W.-H., Lo, S.-L., Chang, C.M., Wang, M.K., 2000. A geometric approach to determine adsorption and desorption kinetic constants. Chemosphere 41, 1741-1747] for the kinetics of adsorption/desorption in aqueous solutions. The correction is to consider that the concentration of solute is not constant and changes as adsorption proceeds. The extension is that we applied Langmuir-Freundlich kinetic model instead of Langmuir kinetic model to consider the heterogeneity and therefore it is more applicable to the real systems. For solving Langmuir-Freundlich kinetic model, some geometric methods and also Taylor expansion were used and finally a simple and novel equation was derived (Eq. (20)) for calculation of adsorption rate constant. This new method was named "extended geometric method". The input data of the obtained equation can be simply derived from initial data of adsorption kinetics. Finally the adsorption of methyl orange onto granular activated carbon was carried out at dynamic and equilibrium conditions and the capabilities of extended geometric method were examined by the experimental data.     

双碱法脱硫技术研究

脱硫过程主要是二氧经硫与氢氧化钠生发化学反应,反应生成物亚硫酸钠溶于水,含亚硫酸钠的脱硫循环水与投加的氢氧化钙反应可生成氢氧化钠和亚硫酸钙。通过沉淀分离可将难溶钙从循环水中清除,氢氧化钠易溶于水可循环使用,脱硫过程中消耗氢氧化钙。达到脱硫效率高,运行费用低的目的。     

从顽拗植物荔枝中提取基因组DNA技术的研究

针对荔枝体内含有大量影响ＤＮＡ提取质量的多酚等次生代谢物质的特点,在常规ＳＤＳ和ＣＴＡＢ提取方法的基础上做了技术改进,即在核裂解之间先破碎细胞,将存在于细胞质中次生物质除去后再裂解细胞核,同时加入活性炭以吸咐杂质反复清洗几次后加入核型解液释放基因组ＤＮＡ,纯化之后经外观和电泳检测,以及Ｄ２６０ｎｍ和Ｄ２８０ｎｍ比值的测定,限制性内切酶反应,ＰＣＲ扩增的结果表明,用改进方法提取的ＤＮＡ无论在纯度上还     

重视城市污水集中处理投资,收费与运营市场化

本文深入研究了国外城市污水处理的成功经验。就城市污水处理市场化进程中,建立什么样的投资,收费与运营模式进行了讨论。     

Prognosis of the spatiotemporal dynamics of ecosystems by means of universal kriging

The use of quantitative data for constructing prognostic maps of the dynamics of ecosystem degradation and restoration by nonlinear simulation methods is a topical field of landscape ecology. This method of dynamic cartography is based on fiberwise comparison of data on the state of Chernye Zemli (the Kalmyk Republic, Russia) in different years and the detailed analysis of the period on which the prognosis was based. For this purpose, materials of repeated aerial and satellite photography obtained during a long period (1954–1993) were used. Comparison of maps characterizing the dynamics of Chernye Zemli between 1958 and 1993 allows prognostic electronic maps for the next 10–15 years (with a five-year interval) to be drawn and land prognosis for the next 20–30 years (1998–2023) to be obtained. Deceased     

Characteristics of the Predator–Prey Interactions and the Horizontal Distribution of Macrozoobenthos in Small Lakes of Different Types

The horizontal distribution and quantitative characteristics of macrozoobenthos were studied in small lakes of the Darwin Nature Reserve (southern Vologda oblast). The aggregation index varied in the open areas of acid lakes, which indicated that communities of small acid water bodies were unstable. The aggregation was the lowest in the open area of a neutral lake. In acid lakes, the number and biomass of macroinvertebrates were the highest near the coasts. In the neutral lake, conversely, these values were maximum in open areas and low near the coast due to a strong pressure of predatory invertebrates and fish. An aggregating effect of invertebrate predators was observed near the coasts of lakes of different types.