壳聚糖-盐酸溶液中温度敏感的相分离行为

研究了壳聚糖 盐酸溶液温度敏感的相分离行为.通过对壳聚糖-盐酸溶液浊度变化的考察以确定相分离温度.测定不同盐酸浓度、壳聚糖浓度以及不同脱乙酰度的条件下的相分离温度，并用DLVO理论(Deijaguin-Landau and Verwey-Overbeck Theory)进行了解释. FTIR、X-ray以及SEM分别描绘了壳聚糖经相分离过程后官能团、结晶状态、颗粒形态的特点.     

沉淀方法对Ru/CeO_2氨合成催化剂催化性能的影响

采用沉淀法制备了Ru/CeO_2氨合成催化剂,并运用N_2物理吸附、X射线衍射、X射线荧光光谱、CO吸附和H2程序升温还原等技术对其进行了表征,考察了沉淀时反应液的并流、反加、正加以及沉积一沉淀对所制备的Ru/CeO_2催化剂氨合成性能的影响.结果表明,不同制备方法所得到的催化剂,其氯残留量和载体的还原性能都存在明显的差别,最终影响了催化剂的氨合成活性,其中采用正加法制备的催化剂上氯残留量少,载体易还原,因而催化活性最高,在10MPa,10 000h~(-1),450℃反应时,NH_3浓度达到11.9%.     

微合金钢中稀土对沉淀相和性能的影响

在Nb(Ti,V）微合金钢中，主要沉淀相分别为Nb(C,N),(Nb,Ti)(C,N)和V（C，N）。稀土降低沉淀相完全溶解的温度，增大奥氏体中沉淀相析出的孕育期，降低析出速率，抑制奥氏体中沉淀相的析出，在铁素体相区，稀土提高沉淀相的析出速率和数量，促进沉淀相的析出，其中稀土对铌沉淀相析出的作用影响最强。锻态钢中，稀土有促进细化球化析出相的作用，随稀土含量增加，沉淀相析出数量增加，但过量稀土，促进作用又减弱，稀土在保持微合金钢强度的情况下，显著改善其冲击韧性，尤其是低温韧性，微合金钢中添加适量稀土可获得更佳的综合性能。     

Systematic front distortion and presence of consecutive fronts in a precipitation system

A new simple reaction-diffusion system is presented focusing on pattern formation phenomena as consecutive precipitation fronts and distortion of the precipitation front. The chemical system investigated here is based on the amphoteric property of aluminum hydroxide and exhibits two unique phenomena. Both the existence of consecutive precipitation fronts and distortion are reported for the first time. The precipitation patterns could be controlled by the pH field, and the distortion of the precipitation front can be practical for microtechnological applications of reaction-diffusion systems.     

Precipitation behavior of uranium in multicomponent solution by oxalic acid

A study on the precipitation of uranium by oxalic acid was carried out in a multicomponent solution. The precipitation method is usually applied to the treatment of radioactive waste and the recovery of uranium from a uranium-scrap contaminated with impurities. In these cases, the problem is how to increase the precipitation yield of target element and to prevent impurities from coprecipitation. The multicomponent solution in the present experiment was prepared by dissolving U, Nd, Cs and Sr in nitric acid. The effects of concentrations of oxalic acid and ascorbic acid on the precipitation yield and purity of uranium were observed. As results of the study, the maximum precipitation yield of uranium is revealed to be about 96.5% and the relative precipitation ratio of Nd, Cs and Sr versus uranium are discussed at the condition of the maximum precipitation yield of uranium, respectively.     

Simulation of a crossover from the precipitation wave to moving Liesegang pattern formation

Model simulations to investigate the precipitation wave phenomenon and a crossover from the precipitation wave to moving Liesegang patterns were performed. The chemical scheme contains four chemical species via the interaction of precipitation and redissolution (complex formation), in which the precipitation reaction term was based on Ostwald's supersaturation theory. In this article, for the first time, all the features and behaviors of the heterogeneous traveling waves are reproduced, which were observed experimentally in the work of Zrínyi et al. (Zrínyi, et al. J. Phys. Chem. 1991, 95, 1618.). The detailed investigation of the pattern formation showed three possible states of the system, which depend on the initial concentration of the inner and outer electrolytes, respectively. These are the precipitation wave (single moving precipitation band), the moving Liesegang pattern (moving precipitation bands), and the state where these two patterns coexist.     

Evaluation of extraction procedures for 2‐DE analysis of aphid proteins

Protein sample preparation is a crucial step in a 2‐DE proteomics approach. In order to establish a routine protocol for the application of proteomics analysis to aphids, this study focuses on the specific protein extraction problems in insect tissues and evaluates four methods to bypass them. The approaches of phenol extraction methanol/ammonium acetate precipitation (PA), TCA/acetone precipitation, PEG precipitation, and no precipitation were evaluated for proteins isolation and purification from apterous adult aphids, Sitobion avenae. For 2‐DE, the PA protocol was optimal, resulting in good IEF and clear spots. PA method yielded the greatest amount of protein and displayed most protein spots in 2‐DE gels, as compared with the TCA/acetone precipitation, PEG precipitation and no precipitation protocols. Analysis of protein yield, image quality and spot numbers demonstrate that the TCA/acetone precipitation protocol is a reproducible and reliable method for extracting proteins from aphids. The PEG precipitation approach is a newly developed protein extraction protocol for aphids, from which more unique protein spots can be detected, especially for detection of acid proteins. These protocols are expected to be applicable to other insects or could be of interest to laboratories involved in insect proteomics, despite the amounts and types of interfering compounds vary considerably in different insects.     

Precipitation of hematite nanoparticles via reverse microemulsion process

Hematite nanoparticles have been successfully synthesized via two processing routes:(i) conventional precipitation route and (ii) reverse microemulsion route.The particle precipitation was carried out in a semibatch reactor.A microemulsion system consisting of water,chloroform,1-butanol and surfactant was loaded with iron nitrates to form iron nanoparticles precipitation.The precipitation was performed in the single-phase microemulsion operating region.Three technical surfactants,with different structure and HLB value are employed.The influence of surfactant characterization on the size of produced iron oxide particle has been studied to gain a deeper understanding of the important controlling mechanisms in the formation of nanoparticles in a microemulsion.Transmission electron microscopy (TEM),surface area,pore volume,average pore diameter,pore size distribution and XRD were used to analyze the size,size distribution,shape and structure of precipitated iron nanoparticles.     

Maximizing recovery of water-soluble proteins through acetone precipitation

Solvent precipitation is commonly used to purify protein samples, as seen with the removal of sodium dodecyl sulfate through acetone precipitation. However, in its current practice, protein loss is believed to be an inevitable consequence of acetone precipitation. We herein provide an in depth characterization of protein recovery through acetone precipitation. In 80% acetone, the precipitation efficiency for six of 10 protein standards was poor (ca. ≤15%). Poor recovery was also observed for proteome extracts, including bacterial and mammalian cells. As shown in this work, increasing the ionic strength of the solution dramatically improves the precipitation efficiency of individual proteins, and proteome mixtures (ca. 80–100% yield). This is obtained by including 1–30 mM NaCl, together with acetone (50–80%) which maximizes protein precipitation efficiency. The amount of salt required to restore the recovery correlates with the amount of protein in the sample, as well as the intrinsic protein charge, and the dielectric strength of the solution. This synergistic approach to protein precipitation in acetone with salt is consistent with a model of ion pairing in organic solvent, and establishes an improved method to recover proteins and proteome mixtures in high yield.     

Gravimetric determination of thorium and cerium with n-benzoylphenylhydroxylamine

Benzoylphenylhydroxylamine has been used for the precipitation of thorium and trivalent cerium; the precipitates are ignited to the corresponding metal dioxide and weighed. Ceric ions are reduced before precipitation. The gravimetric separation of thorium and cerium is effected by precipitation at different pH values.     

Influence of the precipitation rate on the seasonal variation in the specific radioactivity of short-lived222Rn daughters in precipitation

Data of variations in the RaB/²¹⁴Pb/ and RaC/²¹⁴Bi/activities in precipitation obtained from observations made for a period of almost 5 years are given together with data on changes in precipitation rate measured simultaneously. It is concluded from analysis of these data that the precipitation rate variation contributes to approximately 40% to the seasonal variation in the specific activity of precipitation.     

Herstellung und Eigenschaften von geformtem Aluminiumoxid. I. Einfluß der Fällbedingungen des Böhmithydrogels auf die Porenstruktur des geformten Aluminiumoxids

Preparation and Properties of Formed Aluminium Oxide. I. Influence of the Precipitation Conditions of the Boehmite Hydrogel on the Pore Structure of Formed Aluminium Oxide A report is given on the influence of the precipitation conditions of boehmite (pH value, temperature, concentration and residence time in the precipitation suspension) on the cavity structure of aluminium oxide spheres, made by coagulation of boehmite hydrosol in ammonia liquor and subsequent thermal treatment at 110 and 600°C. The boehmite hydrogel was obtained at continuous precipitation conditions by neutralisation of sodium aluminate solution with nitric acid. It is shown that the difference in the pore structure of the formed aluminium oxide obtained by varying the precipitation conditions were caused by the special morphological features of the boehmite crystallization in the precipitation process.     

丹参提取液的树脂吸附及醇沉工艺对比研究

以丹参水提取液中丹参素及原儿茶醛含量为指标，HPLC检测不同工艺前后有效成分的含量变化，考察了不同浓度的醇沉除杂工艺，筛选出了大孔吸附树脂富集有效成分的最佳工艺。研究结果显示：单纯采用水醇法提取工艺时，以50％乙醇沉降为最佳工艺，D301大孔吸附树脂能够选择性的吸附丹参素和原儿茶醛，大幅度降低出膏率，提高丹参粗提物中有效成分含量，效果优于醇沉工艺。     

Applicability of reversed-phase liquid chromatography for the speciation of vanadyl and nickel metalloporphyrins in oil extracts

Summary Gradient reversed-phase liquid chromatography was examined with a view to using it as a separation technique for the speciation of vanadyl and nickel porphyrins in oil extracts. Poor separations were obtained when precipitation of the sample constituents occurred in the starting mobile phase. The reasons for the precipitation phenomena were found to be highly complex. Mixed crystal formation, slow dissolution kinetics and saturation may influence the elution behaviour of species present in the oil extracts. When precipitation was avoided the separation of the vanadyl porphyrins was significantly improved. Thus far, no satisfactory separations have been obtained for the nickel porphyrinic species.Although the occurrence of precipitation of the extracts hinders the distinct speciation of metalloporphyrins with reversed phase chromatography, the precipitation/dissolution phenomena showed some interesting features as a clean-up step for diluted crude oil samples and oil fractions.     

Pattern formation and self-organization in a simple precipitation system

Various types of pattern formation and self-organization phenomena can be observed in biological, chemical, and geochemical systems due to the interaction of reaction with diffusion. The appearance of static precipitation patterns was reported first by Liesegang in 1896. Traveling waves and dynamically changing patterns can also exist in reaction-diffusion systems: the Belousov-Zhabotinsky reaction provides a classical example for these phenomena. Until now, no experimental evidence had been found for the presence of such dynamical patterns in precipitation systems. Pattern formation phenomena, as a result of precipitation front coupling with traveling waves, are investigated in a new simple reaction-diffusion system that is based on the precipitation and complex formation of aluminum hydroxide. A unique kind of self-organization, the spontaneous appearance of traveling waves, and spiral formation inside a precipitation front is reported. The newly designed system is a simple one (we need just two inorganic reactants, and the experimental setup is simple), in which dynamically changing pattern formation can be observed. This work could show a new perspective in precipitation pattern formation and geochemical self-organization.     

PHASE BEHAVIOUR OF PHOSPHINOPOLYACRYLATE SCALES INHIBITOR

The influence of the Ca⁺⁺ and inhibitor concentrations, pH, and temperature on the phase behaviour and precipitation yield of a phosphinopolyacrylate scale inhibitor, PPAA, has been studied. The results are interpreted in terms of the chemical processes governing PPAA-Ca⁺⁺ complexation, and evidence for the role of inhibitor molecular weight in determining the degree of precipitation is produced. Comparative adsorption and precipitation squeezes, carried out in sandpacks, demonstrate that significant enhancement of the treatment lifetime can be achieved when conditions giving extensive inhibitor precipitation are used. The sandpack experiments and dissolution studies on the precipitated inhibitor both suggest strongly that kinetic phenomena influence the return level of inhibitor in the field. Together these studies point the way to approaches for optimising inhibitor precipitation squeeze treatments in order to control scale deposition in petroleum reservoirs.     

游离125I与血浆蛋白的结合及其对血药浓度测定的影响

通过体内、外实验, 研究了游离125I与血浆蛋白的结合及其在三氯乙酸(TCA)沉淀后的沉淀百分率, 并与125I-RGD-Sak在SD大鼠中不同时间血药浓度的结果进行了比较. 结果表明, 游离125I能与血浆蛋白结合, 并为TCA所沉淀, 且在一定范围内, 游离125I与血浆蛋白结合后的沉淀百分率与温育时间及游离125I的活度无关. 体内、外实验中, 游离125I与血浆蛋白结合后的沉淀百分率分别为(1.26±0.14)%及(1.38±0.33)%. 沉淀物中含有吸附在沉淀物表面的游离125I, 该吸附需要用TCA沉淀2~3次才能去除. 采用125I核素示踪法进行生物类制品的药代动力学研究时, 应对游离125I的影响进行校正.     

催化沉淀无线传感法测定痕量汞

基于汞对K4Fe(CN)6与K3Fe(CN)6的沉淀反应的催化作用和沉积于磁弹性片上的沉淀导致的磁弹性片共振频率的降低,建立了应用磁弹性传感器的催化沉淀无线传感法测定痕量汞的方法.磁弹性传感技术具有能无线检测磁弹性片的共振频率变化的独特性质,这种共振频率变化对应于磁弹性片的质量变化.研究了酸度、试剂等多种因素对测定的影响.在K4Fe(CN)6、K3Fe(CN)6和乙酸的浓度分别为0.001、0.01和0.15 mol/L,反应温度和时间分别为55 ℃和10 min的条件下,测定汞的线性范围为0.4～9.0 μg/L; 检出限为0.24 μg/L.应用本方法测定了水样中的痕量汞,回收率为97.0%～102.6%.     

Nanoscale precipitation in a maraging steel studied by APFIM.

This article summarizes findings from our previous investigations and recent studies concerning precipitation in a maraging steel of type 13Cr-9Ni-2Mo-2Cu (at.%) with small additions of Ti (1 at.%) and Al (0.7 at.%). The material was investigated after aging at 475 degrees C up to 400 h using both conventional and three-dimensional atom-probe analyses. The process of phase decomposition in the steel proved to be complicated. It consisted of precipitation of several phases with different chemistry. A Cu-rich phase was first to precipitate and Mo was last in the precipitation sequence. The influence of the complex precipitation path on the material properties is discussed. The investigation clearly demonstrated the usefulness of the applied techniques for investigation of nanoscale precipitation. It is also shown that, complementary methods (such as TEM and EFTEM) giving structural and chemical information on a larger scale must be applied to explain the good properties of the steel after prolonged aging.     

Precipitation of nickel dimethylglyoximate

The homogeneous precipitation method of Salesin and Gordon and the aqueous acetone precipitation described by Jones and Howick are examined for the determination of nickel as the dimethylglyoximate and where applicable comparisons are made with a direct (conventional) precipitation of this substance. The co-predpitation of iron and cobalt was studied radiometrically under various experimental conditions. Relevant solubility data are also presented. Application of the methods to the determination of nickel in alloy steels showed that in the absence of cobalt there is little to choose between them. For cobalt steels the method of Jones and Howick is more convenient than that of Salesin and Gordon and more satisfactory than a conventional precipitation and gravimetric finish.