Effect of synthesis parameters on single gas permeation through T-type zeolite membranes

In this research, nanoporous zeolite T membranes were synthesized at three levels of synthesis temperature: 100, 120 and 140 °C and synthesis time: 15, 30 and 50 h and characterized by gas permeation. Effects of synthesis parameters on CO₂ and CH₄ permeances and CO₂/CH₄ ideal separation factors were studied. All experiments were conducted at 1 bar feed pressure and 30 °C module temperature. Normally, it is anticipated that increasing synthesis temperature and synthesis time increase gas permeances and consequently decrease ideal separation factor. This prediction was not observed in the case of synthesis temperature increase from 100 to 120 °C as well as synthesis time increase from 15 to 30 h, due to the dual effect of increasing synthesis temperature and synthesis time on gas permeances and ideal separation factor. More zeolites are deposited and larger crystals are formed at higher synthesis temperatures and times. Forming the larger crystals accelerates the rate of zeolite layer integration, which is responsible for gas separation, in one hand and reduces the density of deposited zeolite layer on the support, due to the formation of more voids, on the other hand. In terms of maximizing the CO₂/CH₄ ideal separation factor, medium synthesis temperature and synthesis time (120 °C and 30 h) can be selected, however, maximum gas permeances are obtained at low levels of synthesis temperature and time (100 °C and 15 h). According to the ranges of gas permeances (10⁻¹¹ to 10⁻⁶ mol/m² s Pa) and CO₂/CH₄ ideal separation factors (1.4–70.3), it is concluded that the zeolite T membranes synthesized at optimum conditions can be employed for membrane separation of CO₂/CH₄ mixtures.     

全自动石墨消解原子吸收法测定土壤中的Pb

建立了用硝酸-氢氟酸-高氯酸体系全自动石墨原子吸收分光光度法测定土壤中的Pb的分析方法.土壤中Pb的检出限可达0.07 mg/kg,线性相关系数为0.9998,加标回收率为92.8％～98.4％.所建立的方法安全、快速、简单、灵敏度高、重现性好,是同时大批量分析土壤中Pb含量的可靠高效方法.     

Formation of multiple trimethylsilyl derivatives in the derivatization of 17α-ethinylestradiol with BSTFA or MSTFA followed by gas chromatography-mass spectrometry determination

N,O-bis(trimethylsily)trifluoroacetamide (BSTFA) and N-methyl-N(trimethylsily) trifluoroacetamide (MSTFA) are common derivatization reagents used in the GC-MS analysis of estrogen steroids such as estrone (E1) and 17(-ethinylestradiol (EE2). In this study, three trimethylsilyl (TMS) steroid derivatives, mono-and di-trimethylsilyl EE2 and mono-trimethylsilyl E1, were observed during the derivatization of EE2 with BSTFA or MSTFA and/or GC separation. Factors influencing the production of multiple TMS derivatives and their relative abundance were examined. It was found that both methanol and bisphenol A competed with estrogenic esteroids when reacting with silylation reagents, and thus affected the formation of TMS derivatives and their relative abundance in the derivatization products. Methanol was found to be more reactive than bisphenol A with the BSTFA reagent. None of the three solvents tested in this study could prevent the generation of multiple TMS derivatives during the derivatization of EE2 with BSTFA, followed by GC analysis. A similar result was observed using MSTFA as the derivative reagent followed by GC analysis. Thus, the suitability of BSTFA or MSTFA as the derivatization reagent for the determination of E1 and EE2 by GC-MS, under the conditions reported here, is questionable. This problem can be solved by adding trimethylsilylimidaz (TMSI) in the BSTFA reagent as recommended, and the performance of the method has been proved in this study.     

Application of multiwalled carbon nanotubes treated by potassium permanganate for determination of trace cadmium prior to flame atomic absorption spectrometry

In this study we investigated the enrichment ability of oxidized multiwalled carbon nanotubes (MWCNTs) and established a new method for the determination of trace cadmium in environment with flame atomic absorption spectrometry.The MWCNTs were oxidized by potassium permanganate under appropriate conditions before use as preconcentration packing.Parameters influencing the recoveries of target analytes were optimized.Under optimal conditions,the target analyte exhibited a good linearity (R~2=0.9992) over the concentration range 0.5-50 ng/ml.The detection limit and precision of the proposed method were 0.15 ng/ml and 2.06%, respectively.The proposed method was applied to the determination of cadmium in real-world environmental samples and the recoveries were in the range of 91.3%-108.0%.All these experimental results indicated that this new procedure could be applied to the determination of trace cadmium in environmental waters.     

布什政府温室气体减排政策评析

美国作为世界政治经济大国和世界第一大温室气体排放国家，其温室气体减排政策备受关注。布什政府上台后不久宣布拒绝接受《京都议定书》，并于2002年2月提出“全球气候变化计划”。布什政府实际上在以各种借口推托美国应该承担的温室气体减排国际责任，这将对以UNFCCC为基础的全球气候合作产生消极影响，并对全球气候政策提出挑战。     

水中砷的原子荧光光谱测定结果的不确定度评定

目的 对原子荧光光谱法测定水中砷含量的不确定度来源及其对测量不确定度的影响进行分析。方法 利用相对标准不确定度进行测量不确定度的评定。过程采用直观的因果图,建立有效的数学模型,利用相对标准不确定度分量进行测量不确定度评定,并在砷含量为1．7μg/L的水样测定中,获得其相对标准不确定度为3．4％,有效自由度为25。结论 原子荧光光谱法对水中砷浓度测量不确定度影响因素中,工作曲线拟合产生的不确定度较大。     

烟气气体常数的确定及与监测质量的关系

阐述了烟气气体常数的确定及与烟尘监测的关系。以各种煤的烟气组分和《锅炉烟尘测试方法》为依据，提出干、湿烟气气体常数代表值各为２７２．６和２７９、７Ｊ／ｋｇ．ｋ，并就代表值的适用性进行了讨论。指出将干烟气组分看作近于气所导致的误差，并对有关公式提出了修改意见。     

应用分光光度法监测大连湾海水COD

在大连湾采集了5个站位12个海水样品,应用分光光度法和规范法平行测定COD的含量。取1000mL现场海水用规范法平行测定5次,取平均值作为分光光度法的标准浓度值。用该海水的消光度计算未知样品的COD,计算公式:c2=c1E标/E测。测定结果表明两种方法基本相同,其相关系数r=0.9283。分光光度法可以代替规范法的硫代硫酸钠滴定法。     

气相色谱/串联质谱法分析水中痕量酞酸酯

采用C18固相萃取结合气相色谱/三重串联四极杆质谱联用仪建立了地表水中痕量酞酸酯(PAEs)类化合物的分析方法。使用串联质谱特有的多反应监测模式可以很好的去除基质的背景干扰,对列入美国环保局优先控制污染物名单的六种PAEs均实现基线分离,在50～1 000 ng/mL范围内线性良好,6种PAEs的相关系数均大于0.99,加标回收率在89.8%～103.4%之间,方法的精密度较好(RSD<10%)。应用于实际地表水样品中PAEs的分析表明,某市地表水中含有邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丁酯和邻苯二甲酸(2-乙基己基)酯,其中邻苯二甲酸二丁酯含量最高(均值为1.25μg/L),邻苯二甲酸丁基苄基酯和邻苯二甲酸二辛酯均未检出。     

西南典型区域夏季大气含氧挥发性有机化合物来源解析

含氧挥发性有机物（OVOCs）是大气光化学过程中的重要中间产物,是臭氧的重要来源之一.利用质子转移反应飞行时间质谱仪（PTR-TOF-MS）在成都平原对OVOCs进行观测,探讨其日变化特征、光化学反应活性、臭氧生成潜势和来源.结果表明,10个VOCs［乙醛、丙酮、异戊二烯、甲基乙基酮（methyl ethyl ketone,MEK）、甲基乙烯基甲酮（methyl vinyl ketone,MVK）、甲基丙烯醛（methacrolein,MACR）、苯、甲苯、苯乙烯、C8芳香烃和C9芳香烃］总浓度（体积分数）为（10.97±4.69）×10^-9,OVOCs为（8.54±3.44）×10^-9,芳香烃为（1.53±0.93）×10^-9,生物源VOCs为（0.90±0.32）×10^-9;光化学活性和臭氧生成潜势均排名前三的物种为：异戊二烯、乙醛和C8芳香烃;3个OVOCs物种（乙醛、丙酮和MEK）主要来源于本地生物源和人为二次源,且丙酮有较强的区域背景值,说明该地区的污染受到较为显著的区域传输的影响.本研究可加深对西南地区臭氧的区域形成机制的认识,为科学管控臭氧污染提供依据.