113mIn radioisotope generator system

Tin-indium generator systems were made with commercial hydrated zirconium oxide, silica gel and hydrated zirconium oxide prepared by the AMPHLETT method. The adsorption capacity of tin has been determined by both spectrophotometric analysis and gammaspectrometry. Zirconium break-through has been determined and compared with the literature values. The dependence of the adsorption capacity on the particle size has been investigated. The effect of autoclaving on the generator systems has been examined.     

Spectroscopic studies of the reaction of iodine with 2,3-diaminopyridine

The charge-transfer interaction of 2,3-diaminopyridine (DAPY) and iodine has been investigated spectrophotometrically in the solvents chloroform and dichloromethane at room temperature. The results indicate the formation of 1:2 charge-transfer complex in each solvent with the observation of the two characteristic absorptions for triiodide ion around 355 and 295 nm. The iodine complex is formulated as [(DAPY)I]+.I3-. The formation of the triiodide ion, I3-, is further confirmed by the observation of the characteristic bands for non-linear I3- ion with C2v symmetry at 151 and 132 cm(-1) assigned to nu(as)(I-I) and nu(s)(I-I) of the I-I bonds and at 61 cm(-1) due to bending delta(I3-). The mid infrared spectra of (DAPY) and triiodide complex are also obtained and assigned.     

Solution-processable porous graphitic carbon from bottom-up synthesis and low-temperature graphitization

It is urgently desired yet challenging to synthesize porous graphitic carbon (PGC) in a bottom-up manner while circumventing the need for high-temperature pyrolysis. Here we present an effective and scalable strategy to synthesize PGC through acid-mediated aldol triple condensation followed by low-temperature graphitization. The deliberate structural design enables its graphitization in situ in solution and at low pyrolysis temperature. The resulting material features ultramicroporosity characterized by a sharp pore size distribution. In addition, the pristine homogeneous composition of the reaction mixture allows for solution-processability of the material for further characterization and applications. Thin films of this PGC exhibit several orders of magnitude higher electrical conductivity compared to analogous control materials that are carbonized at the same temperatures. The integration of low-temperature graphitization and solution-processability not only allows for an energy-efficient method for the production and fabrication of PGC, but also paves the way for its wider employment in applications such as electrocatalysis, sensing, and energy storage.

Porous graphitic carbon was synthesized through acid-mediated aldol triple condensation followed by low-temperature graphitization. The inherent thin film processability and the low temperature requirement of the synthesis enable various potential applications.     

Optimization Method for Phenolic Compounds Extraction from Medicinal Plant (Juniperus procera) and Phytochemicals Screening

Juniperus procera is a natural source of bioactive compounds with the potential of antitumor, antimicrobial, insecticidal, antifungal, and antioxidant activities. An optimization method was developed for total phenolic content (TPC), total flavonoid content (TFC), and total tannin content (TTC) in leaf and seed extract of Juniperus procera. Organic solvents (methanol (99.8%), ethanol (99%), and acetone (99.5%)), and deionized water (DI) were used for extraction. The estimation of TPC, TFC, and TTC in plant materials was carried out using UV-spectrophotometer and HPLC with the standards gallic acid, quercetin, and tannic acid. Recovery of TPC in leaf extract ranged from 2.9 to 9.7 mg GAE/g DW, TFC from 0.9 to 5.9 mg QE/g DW, and TTC ranged from 1.5 to 4.3 mg TA/g DW while the TPC value in the seed extract ranged from 0.53 to 2.6 mg GAE/g DW, TFC from 0.5 to 1.6 mg QE/g DW, and TTC ranged from 0.5 to 1.4 mg TA/g DW. This result revealed that methanol is the best solvent for recovery of the TPC value (9.7 mg) from leaf extract in comparison to other solvents. Ethanol recorded the highest result of TFC (5.9 mg) in leaf extract among the solvents whereas acetone was the best for TTC yield recovery from leaf extract (4.3 mg). In the case of the seed extract, ethanol was the best solvent for both TPC (2.6 mg), and TFC (1.6 mg) recovery in comparison to other solvents. Total tannin content in methanol resulted in significant recovery from seed extract (1.4 mg). Separation and quantification of gallic acid, quercetin, and tannic acid in plant materials were undertaken using HPLC. Gallic acid in leaf and seed of J. procera ranged from 6.6 to 9.2, 6.5 to 7.2 µg/g DW, quercetin from 6.3 to 18.2, 0.9 to 4.2 µg/g DW, and tannic acid from 16.2 to 29.3, 6.6 to 9.3 µg/g DW, respectively. Solvents have shown a significant effect in the extraction of phenolic compounds. Moreover, phytochemicals in plant materials were identified using GC-MS and resulted in very important bioactive compounds, which include anti-inflammatory, antibacterial, and antitumor agents such as ferruginol, phenanthrene, and n-hexadecanoic acid. In conclusion, the optimal solvent for extraction depends on the part of the plant material and the compounds that are to be isolated.     

C_(18)膜萃取/液相色谱-质谱联用法测定极地水体中有机磷酸酯

建立了C_(18)膜萃取/液相色谱-质谱联用技术测定极地水体中10种有机磷酸酯(OPEs)的方法。根据优化后的样品前处理及仪器方法,利用C_(18)膜富集4 L水体中的10种OPEs,经二氯甲烷超声提取,在电喷雾正离子模式下,采用选择反应监测(SRM)模式进行分析,线性相关系数为0.994 4~0.999 9。10种OPEs的加标回收率为64.1%~115%,方法检出限为0.08~0.55 ng/L。该方法适用于极地水体中10种OPEs的分析,利用该方法对北极水体样品中的10种OPEs进行检测,测得冰川融水中∑OPEs的质量浓度为0.64~6.64 ng/L,海水中∑OPEs的质量浓度为0.09~2.03 ng/L。     

碳化铁催化剂的制备及其对CO加氢的催化活性

 以Fe2O3为原料,采用两种预处理方法制备了碳化铁催化剂. 结果表明,直接在CO气氛下进行碳化处理,或者以H2预还原后再用CO进行碳化处理均可以制备出碳化铁催化剂. 碳化温度是制备过程中的关键因素. 对于Fe2O3样品,较适宜的碳化温度是350 ℃,而对于添加了K助剂的样品,只有经H2预还原处理后再于350 ℃用CO碳化处理4 h才能将样品完全转化为Fe5C2. 在CO加氢的评价实验中,碳化铁催化剂表现出很高的催化活性,生成的烃类产物中主要是饱和烷 烃,未检测到乙烯的生成. 而在K改性的催化剂上反应产物中烯烃的含量明显提高.     

Preparation of Anion Exchange Membrane Based on Imidazolium Functionalized Poly(arylene ether ketone)

The authors presented a novel synthetic route for the imidazolium functionalized poly(arylene ether ketone)s, derived from an engineering plastics polymer, a poly(arylene ether ketone) with 3,3',5,5'-tetramethyl-4,4'-dihydroxybiphenyl moiety(PAEK-TM). The preparation of anion exchange membranes comprised converting benzylic methyl groups to bromomethyl groups by a radical reaction, followed by the functionalization of bromomethylated PAEK with alkyl imidazoles, i.e., methyl, butyl or vinyl imidazole. The structure of imidazolium functionalized PAEK was proved by ¹H NMR spectra. A class of flexible and tough membranes was then achieved by subsequent film-forming and anion exchange processes. The water uptake and hydroxide conductivities of membranes are comparable or superior to those of quaternary ammonium(QA) anion exchange membranes. This work demonstrated a new route for non-QA anion exchange membrane design, avoiding the chloromethylation reagent and precisely controlling the degree and location of imidazolium groups.     

OMS-2/Al2O3/堇青石整体式催化剂的制备及其催化性能研究

以Al₂O₃/堇青石蜂窝陶瓷为载体,氧化锰八面体分子筛(OMS-2)为活性组分,采用涂覆法制备了系列整体式催化剂。考察了黏合剂种类和活性组分涂覆次数对二甲醚(DME)催化燃烧性能的影响,并对催化剂进行XRD、BET、SEM、H₂-TPR、O₂-TPD等表征。结果表明,以甲氧基聚乙二醇为黏合剂经一次涂覆制备的整体式催化剂的性能最佳,活性组分OMS-2以相互交织的簇体均匀分布在载体上,并与Al₂O₃之间存在较强的相互作用。涂层的添加有效增加了催化剂的比表面积,提高了催化剂的性能,最佳催化活性t₉₀为257 ℃。     

三维开放骨架镧系金属有机配位聚合物Tm(BTC)(DMF)(DMSO)的合成、结构和性质

以稀土元素铥(Tm) 作为金属中心, 均苯三甲酸(H3BTC)作为有机配体制备了一个新型的三维配位聚合物 Tm(BTC)(DMF)(DMSO), 并通过X射线单晶衍射、元素分析、热重分析、吸附测试等手段对其进行了表征.     

含有脂肪族侧链的聚醚醚酮的合成、表征及结构与性能关系

以苯酚和含有不同链长的长链脂肪酮作为原料, 制备了与双酚A结构相似的双酚单体, 并与4, 4'-二氟二苯酮共聚, 合成了几种含有不同长度脂肪族侧链结构的聚醚醚酮类(PEEKs)聚合物. 利用元素分析和核磁共振氢谱(1H NMR)对所合成的双酚单体进行了表征, 并用红外光谱(FTIR)\, 示差量热扫描仪(DSC)、热失重分析仪(TGA)和电子拉力机对所合成的聚合物结构和性能的关系进行了研究.