高硫石油焦高温热解过程及硫析出特性研究

为深入了解高硫石油焦在工业应用高温工况下的热解过程以及硫的析出特性,本研究采用高温固定床对青岛高硫石油焦进行了高温(900-1500℃)热解实验,考察了高温热解下热解气体释放规律,热解过程中焦的物理孔隙结构以及化学特性的演变,并对热解过程中硫的析出与演变特性进行了研究。结果表明,随着热解温度的升高,石油焦热解气中的H_2含量逐渐增加,CO含量变化不大,CH_4与CO_2含量则逐渐下降;热解焦的比表面积与平均孔隙均随热解温度的升高有所增加,颗粒的表面形态则受温度影响较小;热解温度的升高会降低石油焦中含有的非定型碳比例,提高其微晶结构的有序性以及石墨化程度;热解焦的气化活性随热解温度的升高先降低后升高,在1100℃附近有最小值; 1500℃高硫石油焦硫元素析出率达81.34%,仅少量硫醇类有机硫和噻吩环内的硫元素得以残存。     

Monitoring of the growth of microcrystalline silicon by plasma‐enhanced chemical vapor deposition using in‐situ Raman spectroscopy

Raman spectra of microcrystalline silicon layers have been recorded in‐situ during growth. The spectra have been collected under realistic conditions for solar cell deposition. To enable these measurements an electrode with an optical feed through has been developed. By using a metallic grid to shield the feed through it is possible to achieve homogeneous deposition of µc‐Si:H at a sufficient optical transmission. In‐situ Raman measurements were carried out during the deposition of a layer with an intentionally introduced gradient in crystallinity that was seen in‐situ as well in reference measurements performed on the same layer ex‐situ. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

VHF-PECVD低温制备微晶硅薄膜的拉曼散射光谱和光发射谱研究

采用拉曼散射光谱和PR650光谱光度计对VHF-PECVD制备的微晶硅薄膜进行了结构表征和在线监测研究.结果表明：功率对材料的晶化率（χc）有一定的调节作用，硅烷浓度大，微调作用更明显；SiH*的强度只能在一定的范围内表征材料的沉积速率，功率大相应的速率反而下降；I［Hα*］/I［SiH*］强度比值反映了材料晶化程度，此结果和拉曼散射光谱测试结果显示出一致性；I［Hβ*］/I［Hα*］的强度比表明氢等离子体中的电子温度随功率的增大而逐渐降低. 关键词： 甚高频等离子体增强化学气相沉积 微晶硅 拉曼散射谱 光发射谱     

Solid Phase Extraction of Uranium by Naphthalene‐Methyltrioctylammonium Chloride and Arsenazo(III) Adsorbent and Subsequent Spectrophotometric Determination

A simple and effective method has been presented for the preconcentration of uranium by solid phase extraction. For this purpose arsenazo(III) supported on naphthalene‐methyltrioctylammonium chloride was used as an adsorbent and uranium solution at pH 3.5 with flow rate of 1 mL·min⁻¹ was passed through the column. Therefore, uranium‐arsenazo(III) complex was formed onto column. Uranium was quantitatively eluted with 5 mL of a 0.1% ammonium tetraphenylborate and determined by spectrophotometric method at 652 nm. Several parameters such as pH, amount of reagents, sample volume, etc. were investigated. The effect of diverse ions on the preconcentration has also been studied and the optimized conditions developed have been utilized for the trace determination of uranium. A preconcentration factor of 100 was achieved. The relative standard deviation (N=8) was 0.5% for 3 ng· mL⁻¹ of uranium. The three sigma detection limit (36) was 0.045 ng·mL⁻¹     

磷酸铵镁结石患者尿微晶组分分析及其与结石形成的关系

采用X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、纳米粒度仪、扫描电子显微镜(SEM)和透射电子显微镜(TEM)研究了磷酸铵镁结石患者尿液中微晶的组分、形貌、粒径和Zeta电位,并对其结石进行了组分分析.结果表明,结石类型、尿微晶组分和尿液pH三者之间存在密切的联系:磷酸铵镁结石病人的尿液pH值较高,通常在6....     

射频激发热丝化学气相沉积制备硅薄膜过程中光发射谱的研究

采用射频(rf)激发,在热丝化学气相沉积(HWCVD)制备微晶硅薄膜的过程中产生发光基元,测量了rf激发HWCVD (rf-HWCVD)的光发射谱,比较了相同工艺条件下rf-HWCVD和等离子体增强CVD(PECVD)的光发射谱,分析了rf功率、热丝温度和沉积气压对rf-HWCVD光发射谱的影响.结果表明,在射频功率<0.1W/cm²时,rf-HWCVD发射光谱反映了HWCVD高的气体分解效率和高浓度原子氢的特点,能够解释气压变化与微晶硅薄膜微结构的关系,是研究HWCVD气相过程的有 关键词： HWCVD OES 微晶硅     

4-PICOLINE-o-DINITROBENZENE; A GENERAL CHROMOGENIC REAGENT FOR LOCATION OF ORGANOPHOSPHORUS PESTICIDES ON THIN-LAYER CHROMATOGRAMS

Abstract

A new general chromogenic reagent for location of organophosphorus pesticides and some of their breakdown products on thin-layer chromatograms has been developed. Chromatoplates are sprayed with 4-picoline and heated for 20 minutes at 100°C in an oven. After cooling, they are sprayed first with o-dinitrobenzene then with alkali. Pesticide spots appear blue in color.     

焦炭的微晶结构及其对反应性的影响

采用高分辨率透射电镜-数字图像分析技术HRTEM-DI研究了焦炭微晶结构。焦炭微晶结构参数中的长度、曲率和倾角,可分别用来表达焦炭微晶大小、微晶片层的有序度和微晶堆砌有序度。提出的表征焦炭微晶大小和有序度的结晶指数,能够很好地反映焦炭微晶结晶程度对反应性的影响。     

Preparation and Properties of Enterosorbents Based on Carboxylated Microcrystalline Cellulose

Features of a non-traditional method of preparation of cellulose-based cation-exchange enterosorbents using nitrogen (IV) oxide are discussed. The proposed approach involves sequential use of oxidative and acid-hydrolyzing functions of nitrogen (IV) oxide to convert ordinary cellulose into carboxylated microcrystalline cellulose. X-ray phase analysis and transmission electron microscopy data show evidence of a topochemical character of cellulose microcrystal modification with carboxyl groups. Factors are indicated causing enhanced stability and whiteness of the samples thus obtained as compared with oxidized cellulose fibres, as well as the ease of stable tixotropic gel formation from the samples prepared in a salt form. Exemplified by methylene blue sorption, a comparative assessment of the sorptive ability of enterosorbent powders and hydrogels prepared in acid and salt forms. Results of clinical trials conducted with the gel enterosorbents in the areas of gastroenterology and detoxication therapy are presented. In view of compatibility of carboxylated microcrystalline cellulose in hydrogel form with many biologically active ingredients, prospective character of using the enterosorbents not only as such but also as a matrix for the development of new dosage forms of other medications is pointed out. Examples showing advantages of such combinations in specific sustained release drug forms (ointments and microgranules) are given.