由冶金焦制备富勒烯的研究

以冶金焦为原料用电弧法制备富勒烯，所得烟灰用甲苯索氏萃取。用质谱，高压液相色谱和紫外光谱技术表征富勒烯产品。研究了实验操作条件及冶金焦性质与富协烯产率间的关系。结果表明，粗富勒烯的产率及组成与资金焦的挥发分密切相关；冶金焦的挥发分愈高粗富勒烯的产率愈低。     

在线钢板测长仪的研究

用光电转换方法把钢板在线上的长度信息输入到单片机进行自动记录,最终给出班次、规格、材质、长度等打印结果。     

A Study on Pre-Oxidation of Petroleum Pitch-Based Activated Carbons for Electric Double-Layer Capacitors

Electric double-layer capacitors (EDLCs) are an excellent electrochemical energy storage system (ESS) because of their superior power density, faster charge–discharge ability, and longer cycle life compared to those of other EES systems. Activated carbons (ACs) have been mainly used as the electrode materials for EDLCs because of their high specific surface area, superior chemical stability, and low cost. Petroleum pitch (PP) is a graphitizable carbon that is a promising precursor for ACs because of its high carbon content, which is obtained as an abundant by-product during the distillation of petroleum. However, the processibility of PP is poor because of its stable structure. In this study, pre-oxidized PP-derived AC (OPP-AC) was prepared to investigate the effects of pre-oxidation on the electrochemical behaviors of PP. The specific surface area and pore size distribution of OPP-AC were lower and narrower, respectively, compared to the textural properties of untreated PP-derived AC (PP-AC). On the other hand, the specific capacitance of OPP-AC was 25% higher than that of PP-AC. These results revealed that pre-oxidation of PP induces a highly developed micropore structure of ACs, resulting in improved electrochemical performance.     

Analytical Intercomparison Exercises and Harmonization within Environmental Laboratories from Developing Countries

Abstract

Since the early 60's, the IAEA implements a Quality Assurance (QA) programme for the Member States. As part of this programme, the IAEA organized more than 150 analytical intercomparison exercises and produced more than 70 Certified Reference Materials for a wide range of determinands, encompassing radionuclides, trace elements, petroleum hydrocarbons, pesticides and PCBs. From the IAEA — Marine Environment Laboratory in Monaco, analytical Quality Assurance services are provided for non-nuclear contaminants in marine materials.

Results of recently organized worldwide intercomparison exercises using the sample materials IAEA-142 (mussel tissue homogenate) and IAEA-140 (seaweed homogenate), show that some progress was achieved worldwide in the analyses of the more common environmental contaminants. However, results also show that difficulties in obtaining accurate data for trace elements and especially for organic contaminants are still widespread, particularly in developing countries. Therefore, the success of international cooperative programmes as well as of many regional environmental monitoring programmes, depends on improved quality and comparability of data which has to be achieved still through reinforced Quality Assurance programmes. To this aim, the IAEA/UNEP/IOC-UNESCO inter-agency programme on marine pollution promotes the adoption of Reference Methods for harmonization of techniques used in developing and developed countries, organizes frequent intercomparison exercises, and produces certified marine Reference Materials which are made available to laboratories worldwide.     

In Defense of Vapor Pressure Osmometry for Measuring Molecular Weight

The value of the average molecular weight of petroleum asphaltenes continues to be controversial. Usually the disagreement is about the measurement of a single asphaltene fraction when the need is for a consistent picture that comprises all fractions of petroleum and includes chemical changes during processing. By using one of the better solvents for carbonaceous materials, o‐dichlorobenzene, at the maximum instrument temperature, vapor pressure osmometry provides a consistent measurement of number average molecular weight not achieved by any other technique. This average molecular weight is consistent among petroleum fractions and gives predictable changes in asphaltene molecular weight with thermal processing.     

乙苯与二甲苯在超临界压力下的热裂解研究

采用连续流动装置, 在压力为4 MPa, 温度分别在700, 750和780 ℃条件下, 开展了乙苯和二甲苯在超临界压力条件下热裂解反应的实验研究. 对乙苯和二甲苯裂解的气相产物, 采用在线气相色谱进行分析; 而裂解的液相产物则通过色质联用仪进行定量分析. 研究发现乙苯和二甲苯裂解的气相产物组成基本相同, 而液相产物组成相差较大, 但都是芳香烃类化合物. 乙苯和二甲苯的转化率都随温度升高而增加; 在相同温度下, 乙苯比二甲苯转化率高. 此外, 裂解过程并未发现明显的结焦现象, 说明纯芳香烃物质的热裂解并不会导致严重积炭. 同时, 本文还采用密度泛函方法在BHandHLYP/6-31+G(d, p)水平上, 对乙苯和甲苯分别进行结构优化并计算相关的键能. 计算结果表明: 乙苯侧链乙基中的C—C键的键能最小, 从而说明乙苯侧链烷基更容易发生断键反应, 理论结果很好地解释了乙苯比二甲苯裂解转化率高的实验现象. 本文的工作对燃料裂解结焦机理的重新认识有重要的意义.     

天然焦-H2O气化反应特性

在加压热重分析仪上研究了气化温度和催化剂种类对沛城煤矿天然焦-H2O的气化反应特性的影响,用扫描电镜(SEM)观察不同温度下焦样的孔隙结构,并计算了动力学参数.结果表明,气化温度是影响天然焦-H2O气化反应性的一个主要因素,随着温度的升高,天然焦的孔隙越发达,碳转化率明显增大;K基、Ni基、Fe基三种催化剂均能有效地促进气化反应,其中K基催化剂效果最好,其次是Ni基和Fe基催化剂;天然焦的活化能为Eα=147.25 kJ/mol.     

饱和烃热裂化夺氢氢转移能力研究

研究了在热反应条件下石油渣油中饱和烃夺氢氢转移能力的测定方法和结果。饱和烃受热生成的自由基可从氢化芳烃四氢萘夺取活泼氢,由此可测定不同饱和烃的夺氢能力。研究结果表明,饱和烃可剧烈裂化而具有较强的夺氢能力,且这种夺氢能力随反应条件苛刻度增大而增强,对于正构烷烃或石蜡系列,其夺氢能力随分子量增大而增强,而对于不同来源石油渣油的饱和分,其夺氢能力的差别不大。沥青质的存在可诱导饱和烃剧烈裂化,增大饱和烃的夺氢能力。     

微波消解-分光光度法测定石油焦中的硅

重点研究了微波消解石油焦样品的方法,详细考察了微波消解时样品的最佳用量、消解压力、消解功率、消解时间,建立了最佳微波消解程序：在样品处理中也采用了常规溶样方法,并分别用两种样品处理方法测定石油焦中的硅。结果表明两种方法测定结果基本吻合,样品测定的RSD小于3．85％,加标回收率在97％～103％之间,但微波消解法的溶样速度是常规法的10倍。实验结果表明,微波消解分光光度法测定石油焦中的硅是一种快速、准确且无环境污染的绿色环保方法,具有一定的实用价值。     

Analysis of naphthenic acids in produced water samples by capillary electrophoresis-mass spectrometry

A capillary electrophoresis-mass spectrometry method was used to analyze naphthenic acids in produced water samples. It was possible to detect cyclopentanecarboxylic, benzoic, cyclohexanebutyric, 1-naphthoic, decanoic, 3,5-dimethyladamantane-1-carboxylic, 9-anthracenecarboxylic, and pentadecanoic acids within ca. 13 min using a buffer composed of 40 mmol/L ammonium hydroxide, 32 mmol/L acetic acid and 20% v/v isopropyl alcohol, pH 8.6. The proposed method showed good repeatability, with relative standard deviation (RSD) values of 6.6% for the sum of the peak areas and less than 2% for the analysis time. In the interday analysis, the RSD values for the sum of the peak areas and migration time were 10.3% and 10%, respectively. The developed method demonstrated linear behavior in the concentration range between 5 and 50 mg/L for benzoic, decanoic, 3,5-dimethyladamantane-1-carboxylic and 9-anthracenecarboxylic acids, and between 10 and 50 mg/L for cyclopentanecarboxylic, cyclohexanebutyric, 1- naphthoic, and pentadecanoic acids. The detection limits values ranged from 0.31 to 1.64 mg/L. Six produced water samples were analyzed and it was possible to identify and quantify cyclopentanecarboxylic, benzoic, cyclohexanebutyric, and decanoic acids. The concentrations varied between 4.8 and 98.9 mg/L, proving effective in the application of complex samples.