83 resultados para Isotope dilution technique

em Chinese Academy of Sciences Institutional Repositories Grid Portal


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A new approach for the synthesis of polyaniline nanofibers under pseudo-high dilute conditions in aqueous system has been developed. High yield nanoscale polyaniline fibers with 18-110 nm in diameter are readily prepared by a high aniline concentration 0.4 M oxidation polymerization using ammonium persulfate (APS) as an oxidant in the presence of hydrochloric acid (HCl), perchloric acid (HClO4), (1S)-(+)-10-camphorsulfonic acid (CSA), acidic phosphate PAEG120 (PA120) and sulfuric acid (H2SO4) as the dopants. The novel pathway always produces polyaniline nanofibers of tunable diameters, high conductivity (from 10(0) to 10(1) S/cm) and crystallinity.

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Phenyl-capped trianiline and tetraaniline in the leucoemeraldine oxidation state were synthesized through a modified-pseudo-high-dilution technique. The chemical oxidation process of these compounds were studied by UV-Vis spectra. It was found that phenyl-capped trianiline in the leucoemeraldine oxidation state was oxidized to its EB form and then decomposed, Phenyl-capped tetraaniline was oxidized to its EB form and then to the pernigraniline oxidation state.

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Monodispersed phenyl-capped trianiline and tetraaniline were successfully synthesized by the reactions of diphenylamine with acetaldehyde-based Sckiff's bases of N-phenyl-1,4-phenylenediamine and 1,4-phenylenediamine, respectively, in the presence of ammonium persulfate and hydrochloric acid, subsequent deprotonation and reduction with phenylhydrazine. The reaction mechanism probably involves the slow hydrolysis of the Sckiff's bases and subsequent oxidative coupling reactions of the formed ammonium salts with diphenylamine at pseudo-high dilution condition of the salts.

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Kunyushan composite granite pluton is located in northeast part of the Sulu UHP collisional belt, Jiaodong peninsula, eastern China. It is regarded as the boundary of the Jiaodong block and the Sulu UHP collisional belt. The body is unique in the Dabieshan-Sulu UHP collisional orogen for its feature of multiple intrusions of diverse types granitoid rocks in a long span after UHP the collision between the North China and the Yangtze plates in late Triassic. It can be grouped into four series on the basis of petrology and petrochemistry. They are mid-K calc-alkaline granitoids, strongly peraluminous granites, high-K calc-alkaline granitoids and syenitic granite of shoshonitic series. In this thesis, the later three types of rocks are investigated geochronologically in detail. The grain zircon U-Pb isotope dilution dating technique has been employed in this study. Zircon morphology are presented and discussion on the chemical and physical conditions of the granite formation have been carried out in addtion. Strongly peraluminous granites comprises foliated monzogranite and garnet bearing leucogranite. They occupy more than half of the area of the Kunyushan composite body. Three zircon samples of foliated monzogranites have been analyzed, they yield lower intercept ages mainly in the range of 140-150 Ma. The formation of these rocks was likely to be at 700-600 ℃, implied by zircon morphology. Two zircon samples of the garnet bearing leucogranite yield lower intercept ages from 130 Ma to 140 Ma. Zircon morphology indicate that the liquidus temperature of the magma was about 750 °C. Syenitic granite of shoshonitic series occur in the north central part of the body, and the volume is quite small contrast to other types. One zircon sample was chosen from this rock, and yield lower intercept age of 121+1.8/-2.1 Ma. Zircon morphology indicate that the liquidus temperature of this rock is up to 900 °C, which is much higher than others'. High-K calc-alkaline granitoids can be divided into two types on the basis of rock texture and structure. One is Kf-porphyritic monzogranite. It's outcrop is quite small. Zircon ages of one sample constrain the emplacement of this rock at about 112 Ma. The other is medium-grain to coarse-grain monzogranite. Zircons from it yield lower intercept age of 100.5+2.9/-4.6 Ma. The variation of zircon morphology suggest that these two monzogranites were outcomes of a single magma at different stage. The former emplaced earlier than the latter. The liquidus temperature of the magma was about 800 ℃ Inherited zircon is ubiquitous in the Kunyushan composite body. Most of the samples yield upper intercept ages of late Proterozoic. It was considered that only the Yangtze plate underwent a crustal growth during late Proterozoic among the two plates which involved into the UHP collision. Inherited zircon of about 200 Ma can also be observed in strongly peraluminous and high-K calc-alkaline granitoids. Two samples out of eight yield upper intercept ages of Achaean.

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To investigate the environmental levels and profiles of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs), polybrominated diphenyl ethers (PBDEs), and polychlorinated biphenyls (PCBs), tree bark samples (n = 22) were collected from Luqiao, an E-waste recycling area, in east China in July 11-13, 2006. The average concentrations of PCDD/Fs, PBDEs, and PCBs determined by isotope dilution-high resolution gas chromatography (HRGC) coupled with high resolution mass spectrometer (HRMS) were 0.1 +/- 0.0, 1.4 +/- 0.2, and 6.5 +/- 0.8 lg g (1) lipid weight, respectively. PCDD/F-toxic equivalent (TEQ, WHO-1998), PCB-TEQs, and total dioxin-like TEQs were 1.3 +/- 0.1, 0.5 +/- 0.0, and 1.8 +/- 0.2 ng g (1) lipid weight, respectively. The profiles of these pollutants in the tree bark were also discussed. Tetra-CDFs, deca-BDE and tri-CBs were the main homologues and accounted for 47% of total PCDD/Fs, 79.3% of total PBDEs, and 33.2% of total PCBs, respectively; As for TEQs, 2,3,4,7,8-PeCDF and PCB126 were the main contributors and accounted for 36% of the total PCDD/F-TEQs and 81.2% of the total PCB-TEQs, respectively. High accumulation of PCDD/Fs, PBDEs, and PCBs detected in the tree bark indicated heavy contaminations of these pollutants in Luqiao area. (C) 2008 Elsevier Ltd. All rights reserved.

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By using modern techniques of isotope dilution, high-resolution gas chromatography/high-resolution mass spectrometry and multiple ions detection, an effective cleanup, qualitative and quantitative method was developed for polychlorinated dibenzo-p-dioxins/furans (PCDD/F) and polychlorinated biphenyls analysis. Based on the chromatographic relative retentions of PCDD/F, a software was established for automatic peak recognition of all the isomers from tetra- to octachlorine PCDD/F. It ensured good reliability and accuracy of the analytical data.

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Novel macrocyclic oligomers were synthesized through the condensation of phenolphthalein and m-phthaloyl-dichloride with triethylamine as catalyst in the mixed solution of methylene chloride and THF via pseudo-high-dilution technique. The oligomers were characterized by IR, H-1 NMR, MS, WAXD, TGA and DSC. It was found that the 3 : 3 adduct (molar ratio of phenolphthalein to m-phthaloyl-dichloride) and the 4 : 4 adduct were the main products and there was a small amount of crystalline in the macrocyclic mixtures. When the mixtures were heated to 360 degrees C, the crystalline disappeared.

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氮循环是水生生态系统中重要的营养循环,对它的研究能够为水环境评价以及解决日益严重的湖泊富营养化问题中的氮治理提供理论依据。水体中的有机质分为颗粒态有机质(POM)和溶解态有机质(DOM)两部分,它们在水体中与无机氮相互转化、相互作用,共同控制着整个水生生态系统内部的氮循环过程。稳定氮同位素技术作为有效的地球化学工具能够被用于追溯水生生态系统中的物质来源以及指示相关的生物地球化学循环作用。因此对有机质稳定氮同位素比值的测定有利用帮助我们了解它在水生生态系统中所扮演的角色,尤其是得到有机质参与的地球化学循环作用的直接证据,从而进一步完善对水生生态系统内部整个氮循环过程的研究。 本研究首先从根本上解决了限制溶解有机氮(dissolved organic nitrogen,DON)稳定氮同位素比值应用的测定技术上的难题。然后选择贵州高原湖泊―红枫湖和百花湖作为研究对象,测定了2003~2004年两湖水体中颗粒态有机氮同位素比值(δ15NPON)的季节及剖面变化,探讨了两湖季节性变化存在差异的原因以及红枫湖纵向水体剖面上δ15NPON的变化规律及影响因素。最后,在前人对红枫湖研究的基础上重点选择了2006~2007年间湖泊热分层不同时期具有代表性的几个月份进行了剖面采样。测定了不同月份纵向水体剖面上的DON、PON与NO3-三种氮形态的含量、δ15N值以及其它水化学参数,揭示了水体内部氮循环过程中的相关生物地球化学作用。同时,结合冬季湖泊枯水期外源输入河流以及湖泊水体横向剖面上的DON、PON与NO3-三种氮形态的含量及其δ15N值的变化,追溯了湖泊水体中各种氮形态的来源以及外源输入河流对湖泊水体的贡献。本研究得到以下几点结论: 1. δ15NPON值的季节性变化可以用于评价水生生态系统的营养状况,指示外源人为活动产生的工业废水和生活污水的影响。对2003~2004年间红枫湖和百花湖两湖表层湖泊水体中PON的δ15N季节性变化研究表明,红枫湖表层颗粒态有机质δ15NPON的变化范围为+3.7~+14.9‰;百花湖颗粒态有机质δ15NPON的变化范围为+1.3~+8.7‰。其季节性变化趋势不同。红枫湖表现为冬季(2月)和夏末秋初(9月)出现高值;冬季高值的出现主要受外源输入的工业废水中富含15N的无机氮源和有机颗粒的影响。百花湖在冬季(2月)出现最低值,夏末秋初(9月)出现高值;冬季最低值的出现则可能归功于生活污水中富含14N的有机颗粒的贡献。 2. 首次从整体角度得到了δ15NDON值变化区间的信息。红枫湖2006~2007年不同采样月份水体内部的δ15NDON测定结果显示,δ15NDON的变化范围为+1.0~+12.3‰,它与δ15NNO3-的变化范围:5.9~+22‰和δ15NPON变化范围:+2.8~+16.8‰接近。同时,研究还发现在浮游植物生长季节,表层水体不同形态氮的同位素比值普遍存在下述规律:δ15NNO3->δ15NPON>δ15NDON。原因是此时浮游植物是PON的主要组成部分,且吸收利用NO3-的过程是δ15NPON变化的主要控制因素,浮游植物通过分泌细胞外液等方式分解产生了的富含14N的DON,从而使得三种形态的氮同位素具有一定的继承关系。 3. 三种氮形态δ15N值的季节性变化趋势能够反映其来源的差异。纵向剖面水体中,2007年1月的δ15NNO3-最大,湖泊受外源河流携带的高δ15N及高含量NO3-的影响。2006年4月和2007年3月的δ15NNO3-较小,水体内部发生的强烈的硝化作用产生了大量富含14N的NO3-,是湖泊水体NO3-的重要内源。δ15NDON值表现为:除2007年3月表现异常外(出现异常高值),浮游植物生长季节(2006年4月和2006年7月)的 δ15NDON普遍小于其余月份,且纵向水体剖面上变化幅度均不太大,这与浮游植物生长季节DON主要来源于浮游植物分泌等作用产生的富含14N的组分有关。δ15NPON值表现为冬季(2007年1月)具有最高值,受外源输入河流中富含15N的有机颗粒的影响。 4. PON降解方式的不同可能引起生成的δ15NDON存在差异。PON在有氧条件下发生硝化降解时,由于富含14N的组分优先被释放,因此生成的DON组分的δ15N值较小,如2006年4月10m以上水体和2006年7月10m以上水体;而当PON在厌氧条件下发生反硝化降解时,富含15N的组分则优先被释放,从而使得生成的DON其δ15N较大,如2006年4月18m以下水体和2006年7月10m以下水体。 5. 纵向水体剖面上δ15NPON的显著变化来源于其组成的变化,并且不论是硝化细菌还是反硝化细菌,当它们作为PON的主要组分时均会造成δ15NPON的减小,如2006年7月和2007年3月中下部水体。 6. 三种氮形态同位素比值的结合能够更加有效地示踪有机质来源的变化。如2007年1月纵向水体剖面,整个水体剖面氮含量无明显变化,而氮同位素比值则有显著变化。20m处δ15NPON、δ15NNO3-和δ15NDON均在此发生转折,显示20m可能是外源输入与内部水体的分界层。此时,横向水体剖面上,采样点4处NO3-显著增加,而δ15NNO3-保持不变;δ15NDON显著减小。说明采样点4处可能有新的氮源出现。初步估计是由于先前网箱养鱼的积累影响还有高含量的NO3-,低δ15N值的DON输出。 以上的研究结果充分证实了有机质的稳定氮同位素比值的变化能够更加直接地用于追溯有机质的来源以及追踪有机质在湖泊水体中参与的生物地球化学循环作用。

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The measurement of void fraction is of importance to the oil industry and chemical industry. In this article, the principle and mathematical method of determining the void fraction of horizontal gas-liquid flow by using a single-energy gamma-ray system is described. The gamma-ray source is the radioactive isotope of Am-241 with gamma-ray energy of 59.5 keV. The time-averaged value of the void fraction in a 50.0-mm i.d. transparent horizontal pipeline is measured under various combinations of the liquid flow and gas flow. It is found that increasing the gas flow rate at a fixed liquid flow rate would increase the void fraction. Test data are compared with the predictions of the correlations and a good agreement is found. The result shows that the designed gamma-ray system can be used for measuring the void fraction in a horizontal gas-liquid two-phase flow with high accuracy.

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The hydrogen dilution profiling (HDP) technique has been developed to improve the quality and the crystalline uniformity in the growth direction of mu c-Si:H thin films prepared by hot-wire chemical-vapor deposition. The high H dilution in the initial growth stage reduces the amorphous transition layer from 30-50 to less than 10 nm. The uniformity of crystalline content X-c in the growth direction was much improved by the proper design of hydrogen dilution profiling which effectively controls the nonuniform transition region of Xc from 300 to less than 30 nm. Furthermore, the HDP approach restrains the formation of microvoids in mu c-Si: H thin films with a high Xc and enhances the compactness of the film. As a result the stability of mu c-Si: H thin films by HDP against the oxygen diffusion, as well as the electrical property, is much improved. (c) 2005 American Institute of Physics.

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Novel hydrogen dilution profiling (HDP) technique was developed to improve the uniformity in the growth direction of mu c-Si:H thin films prepared by hot wire chemical vapor deposition (HWCVD). It was found that the high H dilution ratio reduces the incubation layer from 30 nm to less than 10 nm. A proper design of hydrogen dilution profiling improves the uniformity of crystalline content, X-c, in the growth direction and restrains the formation of micro-voids as well. As a result the compactness of mu c-Si:H films with a high crystalline content is enhanced and the stability of mu c-Si:H thin film against the oxygen diffusion is much improved. Meanwhile the HDP mu c-Si:H films exhibit the low defect states. The high nucleation density from high hydrogen dilution at early stage is a critical parameter to improve the quality of mu c-Si:H films. (c) 2006 Published by Elsevier B.V.

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Novel hydrogen dilution profiling (HDP) technique was developed to improve the uniformity in the growth direction of mu c-Si:H thin films prepared by hot wire chemical vapor deposition (HWCVD). It was found that the high H dilution ratio reduces the incubation layer from 30 nm to less than 10 nm. A proper design of hydrogen dilution profiling improves the uniformity of crystalline content, X-c, in the growth direction and restrains the formation of micro-voids as well. As a result the compactness of mu c-Si:H films with a high crystalline content is enhanced and the stability of mu c-Si:H thin film against the oxygen diffusion is much improved. Meanwhile the HDP mu c-Si:H films exhibit the low defect states. The high nucleation density from high hydrogen dilution at early stage is a critical parameter to improve the quality of mu c-Si:H films. (c) 2006 Published by Elsevier B.V.

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Planktonic foraminiferal faunas, oxygen isotope and modern analog technique sea surface temperature records were obtained in piston core DGKS9603 (28degrees08.869'N, 127degrees16.238'E, water depth 1100 in) collected from the middle Okinawa Trough. During the last glaciation, four cold events were identified and correlate Heinrich events (HE) H2-5 of the last 45 ka. During the last deglaciation, core DGKS9603 has begun to be influenced by the Kuroshio since about 16 cal ka BP. Three weakenings of this warm current occurred at about 2.8-5.3, 11.4 and 15.5 cal ka BP respectively. Among the three fluctuations, the oldest one is synchronous with HE1 and could be a response to the strong cooling observed in the North Atlantic Ocean. The fluctuation occurring at about 11.4 cal ka ago corresponds to the Younger Dryas within the age error bars. Our observations provide new evidence that the HEs documented from Greenland and the northern North Atlantic had a global climatic impact. Changes in the intensity of the East Asian monsoon could be the main mechanism responsible for the paleoccanographic variations observed in the Okinawa Trough. (C) 2001 Elsevier Science B.V. All rights reserved.

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Measurement while drilling (MWD) has become a popular survey technology to monitor directional data, drilling data, formation evaluation data and safety data in the world. And closed loop drilling shows promise in recent years. Obviously, the method of tr