Interaction of NO and NO2 on 12-tungstophosphoric acid

On exposure of the solid 12-tungstophosphoric acid (H₃PW₁₂O₄₀· nH₂O (HPW)) to NO₂ at 150°C NO₂ is sorbed, while HNO₃ is produced. NO₂ is found to penetrate into the bulk structure whose reaction occurs with the water hydrogen-bonded to the protons to produce HNO₃. The NO₂ retained on the catalyst is stoichiometrically equivalent to the total number of protons on and in the solid. This, together with infrared spectra, suggests that NO₂ is associating (1/1) with the protons, producing a nitronium salt of the solid acid. Although insignificant quantities of NO are taken up by HPW, after exposure to NO₂, approximately stoichiometric quantities of NO are sorbed and the infrared spectra show the presence of N₂O₃.     

Identification of organochlorines and organobromines in coals

Four Chinese bituminous coals were extracted with CS₂, n-hexane, benzene, methanol, acetone, tetrahydrofuran (THF) and THF/methanol (1: 3 vol/vol) mixed solvent sequentially. The resulting 28 extracts were analyzed with GC/MS. Six organochlorines (OCs) and two organobromines (OBs) were identified in eight extracts from the coals. Our experiments provide, for the first time, the information on the molecular structure of OCs and OBs in coals.     

Bi_4Ge_3O_(12):TR(TR=Pr,Eu,Ce)晶体的吸收和发光光谱

测量了Bi_4Ge_3O_(12)(BGO):Pr、Eu和Ce的吸收、激发和发光光谱。掺杂BGO吸收和激发带相应于pr~(3+)、Eu~(3+)和Ce~(3+)离子特征跃迁。Xe灯中不同波长激发所得到掺杂BGO的发光光谱可通过Bi~(3+)心和掺杂材料之间能量传输过程加以解释。Bi~(3+)心400—600mm发射强度因受到Ce杂质影响变弱,这现象在高Ce浓度晶体里更为显著。     

Synthesis of Organotin Polyamine Ethers Containing Acyclovir and their Preliminary Anticancer and Antiviral Activity

Organotin polyamine ethers containing acyclovir in their backbone were synthesized in moderate to high yield employing the aqueous interfacial polycondensation system. The products are high molecular weight polymers. Infrared spectroscopy of the products shows new bands characteristic of the formation of Sn–N and Sn–O bonds consistent with the proposed structure. MALDI-TOF MS below 2000 Da shows the presence of organotin and acyclovir units containing these two moieties. The products show moderate inhibition of a number of cancer cell lines and exhibit the ability to inhibit a number of viruses, particularly the herpes simplex virus-1 and varicella zoster virus that are responsible for herpes, chicken pox and shingles.     

Volatile compounds of original African black and white shea butter from Tchad and Cameroon

Shea butter is used as an edible vegetable fat in many African countries. It can be utilized as a substitute or complete replacement for cocoa butter in various applications and plays an important role in traditional African medicinal practice. Although detection of volatile compounds by solid‐phase micro‐extraction gas‐chromatography mass‐spectroscopy (SPME‐GC‐MS) is a very reliable and reproducible technique, which can be used as an important part of authenticity checking, production monitoring and contamination detection, no published data about volatile compounds of shea butter are available so far. In this investigation, the characteristic volatiles in the headspace of original African shea butter samples were identified by using SPME‐capillary‐GC coupled to a mass selective detector. Almost 100 different volatile components were identified, e.g. fatty acids, saturated and unsaturated aldehydes and ketones, terpenes, and typical Maillard reaction products such as methylfuranes and pyrazines. Furthermore, the samples have been olfactorily evaluated by a panel of professional flavorists and trained analytical chemists. It can be stated that variations in processing conditions of shea butter result in considerable differences in the composition of headspace volatiles, detected by SPME‐GC‐MS and human olfaction.     

12-tungstophosphoric and 12-tungstosilicicacid supported onto hydrous zirconia for liquid phase tert-butylation of m-cresol

Supported 12-tungstophosphoricacid (12-TPA) and 12-tunstosilicicacid (12-TSA) were used as heterogeneous catalysts for liquid-phase tert-butylation of m-cresol, an industrial important reaction. Alkylation reactions have been carried out with supported 12-TPA by varying different parameters such as % loading of 12-tungstophosphoricacid onto support, mole ratio of alcohol to m-cresol, reaction temperature, amount of the catalyst, reaction time and calcination temperature to optimize the conditions. To see the effect of the acidity on the reaction, the same reaction was studied over supported 12-TSA. Both the catalysts give 100% selectivity for o-isomer with different % conversion. The difference in catalyst performance of both the catalyst was correlated with the value of total acidity as well as Bronsted acidity.     

Accurate determination of hexanal in beef bouillons by headspace solid‐phase microextraction gas‐chromatography mass‐spectrometry

Lipid oxidation has great impact on the quality of food products through flavor and taste deterioration, reduction in nutritive value, and potential toxicity of the oxidized food components. Flavor and taste deterioration can be easily perceived and it represents one of the major causes of consumer complaints in the food industry. The deterioration of sensory properties is due to the decomposition products of hydroperoxides that easily isomerize and degrade into volatile compounds. Volatile products are responsible for flavor and taste deterioration. In this study, we present the development of the solid‐phase microextraction gas chromatography‐mass spectrometry (SPME‐GC‐MS) technique to quantify low amounts (μg/g range) of secondary oxidation products, i.e. hexanal. The optimization of SPME parameters is a difficult task because of the possibility of further formation of volatile products during analysis. Different parameters such as type of fiber, exposure time of the fiber to the sample headspace and the optimal temperature of absorption have also been investigated. The complete validation of the method was achieved by the determination of linearity, limits of detection and quantification and repeatability. We demonstrated that the SPME method is a valuable tool for the quantification of low amounts of secondary oxidation products such as hexanal. Therefore, this technique can be used to detect early formation of volatiles.     

Air sampling of volatile sex pheromone components in a closed jar

A cotton wool plug, used as the source for pheromone release, was placed in closed 1-quart Mason jars, either at the mouth or at the rear of the jar. Air sampling of the two components of the sex pheromone (total 2.2 mg at the source) of the almond moth (Ephestia cautella) female showed that the saturation period near the source in still air was 20–22 hr and that far from the source was 40–50 hr, reaching a level of less than 1 ng/ml air. The ratio between the components (Z,E)-9,12-tetradecadienyl acetate, designated D, and (Z)-9-tetradecenyl acetate designated M, in the air was close to the original ratio for both sampling sites, albeit somewhat richer in the more volatile (Z)-9-tetradecenyl acetate (source 77.023.0 DM, air 73.0– 74.327.0–25.7; source 80.119.9, air 77.622.4; source 25.174.9, air 23.976. 1 DM). The total amount of pheromone per milliliter of air was two to three times larger near the source than far from it at the early stages of the evaporation and saturation process. When the amount of pheromone applied to the source was tripled (7 mg), the amount far from the source was almost tripled, or the saturation time was cut by factor of two to three.     

不同品牌郫县豆瓣酱挥发性成分的比较研究

采用同时蒸馏萃取,结合气-质联机对2种不同品牌郫县豆瓣酱的挥发性成分进行了比较研究.研究结果表明：不同品牌的郫县豆瓣酱挥发性成分的差别比较大,如川花牌豆瓣酱鉴定出86种,丹丹牌78种;2种品牌豆瓣酱挥发性成分都是酯类最多,其次是醇类,然后是醛酮类等,其中含量较大的成分有3-甲基丁醇、糠醇、芳樟醇、苯乙醇、3-甲基丁醛、糠醛、苯乙醛、3-羟基-2-丁酮、乙酸乙酯、十六碳酸乙酯、亚油酸乙酯、十八碳酸乙酯、4-乙基苯酚、4-乙基-2-甲氧基苯酚和2-甲氧基-4-乙烯基苯酚等.     

Orientation of Bi<Subscript>3.2</Subscript>La<Subscript>0.8</Subscript>Ti<Subscript>3</Subscript>O<Subscript>12</Subscript> ferroelectric thin films with different annealing schedules

Fatigue-free Bi_3.2La_0.8Ti₃O₁₂ ferroelectric thin films were successfully prepared on p-Si (100) substrates using metalorganic solution deposition process. The orientation and formation of 5-layers thin films were studied under different processing conditions using XRD. Experimental results indicate that increase in annealing time at 700 °C after preannealing for 10 min at 400 °C can remarkably increase (200)-orientation of the films derived from the precursor solutions with two contents of citric acid. Meanwhile, high content of citric acid increases the film thickness and is conducive to the a-orientation of the films with the preannealing, and low concentration of the solution is conducive to the c-orientation of the films without the preannealing.