高温液相二醇还原法制备钴纳米粒子

应用高温液相二醇还原法,首次用1,10-癸二醇作还原剂,在两种表面活性剂存在下制备出磁性钴纳米粒子。用X射线衍射、X射线光电子能谱、透射电镜、激光光散射仪和热分析仪分别对钴纳米粒子的结构、价态、颗粒尺寸与热性能进行了表征分析。结果表明该方法制备的钴纳米粒子具有hcp相,平均粒径大约为50nm。     

藤茶干粉提取液还原制备金纳米粒子

用藤茶干粉提取液生物还原氯金酸溶液实现了金纳米粒子绿色制备,通过紫外-可见分光光度计、透射电子显微镜和粒度分布等技术手段对金纳米粒子形态等物性进行了表征,运用控制变量法探究了金纳米粒子生物合成的规律。研究发现,金纳米粒子的粒径、粒径分布、形状和稳定性受反应体系pH值、温度以及氯金酸的用量影响。pH6.47或藤茶干粉提取液过量时会引起纳米金的团聚;温度升高,金纳米粒子平均粒径会减小。通过变量控制,可以实现金纳米粒子绿色合成的有效控制。     

极谱法测定二苯胺磺酸钠的研究

本文报道两种测定二苯胺磺酸钠的极谱方法，它们是基于在Ｈ２ＳＯ４和ＮａＮＯ２介质中二苯胺磺酸钠被定量亚硝化，然后用极谱法测定其亚硝化产物。这两种方法分别是以标准ＮａＮＯ２作基准的极谱测定法和以纯二苯胺磺酸钠为基准的单扫描示波极谱法。应用这两种方法于化学试剂二苯胺磺酸钠含量的测定，结果令人满意。     

维生素E绿色还原法制备银纳米粒子的研究

采用一种绿色还原法制备银纳米粒子,以维生素E为还原剂,淀粉为稳定剂,在液相中还原硫酸银,通过改变溶液的pH值和反应时间,得到不同粒径的黄色银纳米粒子,并分别采用透射电镜、红外光谱、紫外-可见吸收光谱、扫描电镜和电化学方法对银纳米粒子进行表征。结果表明:维生素E在溶液中被氧化生成苯醌,反应得到的银纳米粒子为球形,粒径为8~25 nm;在较强碱性条件下,得到的银纳米粒子尺寸较小,分布较均匀,其平均粒径约为10 nm;不同条件下生成的银溶胶分别在417、411、409、408 nm处出现紫外吸收峰,这些吸收峰均为银纳米粒子的表面共振吸收;生成的银纳米粒子具有很好的电化学性质,并对L-半胱氨酸的电化学反应显示了良好的催化活性。     

植物还原法制备负载型金纳米催化剂催化乙醇选择氧化反应

采用侧柏叶提取液还原氯金酸制备负载型金纳米催化剂,通过乙醇选择氧化反应,筛选出催化性能较好的TiO2载体。以TiO2载体为载体,考察了Au负载量、焙烧温度、催化剂用量、碳酸氢钠添加量及催化剂反应条件(时间、温度、压力)等因素对乙醇选择氧化反应的影响。结果表明,1.5%Au/TiO2催化剂(Au负载量为1.5%,质量分率,下同)催化乙醇选择氧化反应性能最佳,产物为乙醛、乙酸乙酯和缩醛,0.5%碳酸氢钠添加剂可抑制缩醛的生成,并可显著提高乙醇转化率和乙酸乙酯选择性。通过优化催化反应条件(1.5%Au/TiO2催化剂焙烧温度为400℃、用量为0.4 g、反应温度为100℃、氧气压力为3 MPa、反应时间为3 h时),乙醇转化率为47.9%,乙酸乙酯选择性为89.1%。     

大粒径单分散金纳米粒子的水相合成

近年来,随着纳米科技的兴起,纳米尺度的金颗粒以其独特的光学、电学性质［１-３］在许多领域表现出潜在的应用价值,引起了人们浓厚的研究兴趣［４-７］．迄今为止,已有多种制备金纳米粒子的方法见诸报导．制备简便、单分散性好、粒径可控,一直是各种方法追求的目标．...     

乳液聚合法制备纳米金/聚苯乙烯复合粒子

以氯金酸为前驱体,十二烷基硫醇和硼氢化钠分别作为稳定剂和还原剂,采用相转移法制备了单分散的金纳米粒子.将金纳米粒子通过乳液聚合的方法制备了纳米金/聚苯乙烯复合粒子.通过紫外-可见吸收光谱(UV-Vis)研究了纳米金和纳米金/聚苯乙烯复合粒子的光吸收特性,使用傅立叶变换红外光谱(FT-IR)、X射线衍射(XRD)、透射电子显微镜(TEM)和动态光散射(DLS)对产物的组成、晶体结构、形貌、以及粒径进行了表征.结果表明,复合粒子为粒径分布较窄的球形,其中的金纳米粒子为面心立方结构.热失重分析(TGA)说明制备的纳米金/聚苯乙烯复合粒子具有很好的热稳定性.     

金纳米粒子-β-环糊精可视化识别苯胺异构体

建立了基于金纳米粒子-β-环糊精(β-CD@AuNPs)的可视化检测苯胺异构体的方法。实验中β-CD同时起着稳定剂和还原剂的作用,水热合成法一步得到β-环糊精包裹的AuNPs。β-CD可以选择性识别3种苯二胺的位置异构体,以纳米金作为信号的转换元件,实现了3种异构体的选择性识别。研究表明,β-CD@AuNPs与对苯二胺的相互作用最强,AuNPs发生明显的团聚显色,最大吸收峰发生明显红移由519 nm变化至650 nm,据此建立了废水中对苯二胺的比色测定方法。在最佳条件下,方法的线性范围0.36～10.8 mg/L,检出限0.12 mg/L,回收率为97.3%～99.7%。该方法可以应用于废水中苯胺类污染物的检测。     

抗坏血酸还原法制备金纳米花的机理

研究了以抗坏血酸和氯金酸为生长溶液制备金纳米花的反应机理. 结果表明, 通过改变生长溶液中抗坏血酸浓度可以调节小尺寸的初级金粒子在种子表面的聚集方式及金纳米花的熟化速度, 从而影响金纳米花的形貌和光学性质. 协同改变抗坏血酸浓度和pH值, 可实现对金纳米花形貌及光学性质的有效调控. 表面增强拉曼散射(SERS)性能评价结果表明, 抗坏血酸还原法制备的金纳米花表面较清洁, 对罗丹明6G有较好的拉曼增强效果.     

各向异性金纳米粒子的制备及其在催化中的应用

尽管有关金纳米粒子催化的研究工作很多,但其中大多数都是采用传统的浸渍法将金盐负载到载体上、共沉淀或沉积-沉淀法制得负载的纳米粒子,但这些方法并未吸收最新的纳米技术。最近,金催化剂的研究者开发了在胶态悬浮液中制取金属纳米粒子,然后进行固载,从而使得单金属和双金属催化剂的催化活性和形貌控制取得较大进展。另一方面,最近十年出现了金纳米粒子合成的高级控制技术,得到了许多各向异性的金纳米粒子,且很容易制得新的形貌,可以控制纳米粒子的表面原子配位数和光学特性(可调的等离子体带),这些都与催化密切相关。这些形貌包括纳米棒、纳米星、纳米花、树枝状纳米结构或多面体纳米粒子等。除了高度关注各向异性金纳米粒子的最新开发的制备方法和性质,本综述也清楚地总结了这些纳米粒子独特的催化性能,以及通过提供更高催化性能的金催化剂、控制暴露的活性位,以及热、电和光催化的鲁棒性和可调性,从而给多相催化领域带来令人惊奇的潜在变革。     

Photothermal ablation of amyloid aggregates by gold nanoparticles

Amyloid peptide (Aβ) is found in the brain and blood of both healthy and diseased individuals alike. However, upon secondary structure transformation to a β-sheet dominated conformation, the protein aggregates. These aggregates accumulate to form neuritic plaques that are implicated in the pathogenesis of Alzheimer's disease. Gold nanoparticles are excellent photon-thermal energy converters. The extinction coefficient of the surface plasmon band of gold nanoparticles is very large when compared to typical organic dyes. In this study, gold nanoparticle–Aβ conjugates were prepared and the photothermal ablation of amyloid peptide aggregates by laser irradiation was studied. Monofunctional gold nanoparticles were prepared using a recently reported solid phase modification method and then coupled to fragments of Aβ peptide, namely Aβ(31–35) and Aβ(25–35). The conjugates were then mixed with Aβ fragments in solution. The aggregated peptide formation was studied by a series of spectroscopic and microscopic techniques. The peptide aggregates were then irradiated by a continuous laser. With gold nanoparticle–Aβ conjugates present the aggregates were destroyed by photothermal ablation. Gold nanoparticles without Aβ conjugation were not incorporated into the aggregates and when irradiated did not result in photothermal ablation. With gold nanoparticle–Aβ conjugates the ablation was selective to the site of irradiation and minimal damage was observed as a result of thermal diffusion. In addition to the application of photoablation to a protein-based sample the nanoparticles and the chemistry involved provide an easily monofunctionalized photothermal material for the biological conjugation.     

十二烷基苯磺酸钠共振瑞利散射法测定蛋白质

在酸性条件下，十二烷基苯磺酸钠与牛血清白蛋白形成离子缔合物，使共振瑞利散射（RRS）急剧增强。研究了相应的光谱特征，影响了因素和适宜的反应条件。在此条件下，不同蛋白质在一定浓度范围内与散射强度呈线性关系。方法的检出限在17.8ng/mL至135.4ng/mL之间，可用于多种蛋白质的测定。本法已用于合成样品以及人血清样品中蛋白质量的测定。     

半乳糖保护的Au纳米颗粒的制备及性能研究

通过一种简易的方法,利用D-半乳糖胺和氯金酸制备出了能够用于肝癌细胞靶向识别的Au纳米颗粒探针.该纳米颗粒形貌和尺寸均一并且生物相容性良好.通过改变反应体系的pH能够对Au纳米颗粒的尺寸进行调控.此外,这种新型的纳米颗粒对RCA120还具有超高的检测灵敏度,实验结果显示其检测限度可以达到2μg·L^-1.     

Size-controlled flow synthesis of gold nanoparticles using a segmented flow microfluidic platform

Segmented flow is often used in the synthesis of nanomaterials to achieve narrow particle size distribution. The narrowness of the distribution is commonly attributed to the reduced dispersion associated with segmented flows. On the basis of the analysis of flow fields and the resulting particle size distribution, we demonstrate that it is the slip velocity between the two fluids and internal mixing in the continuous-phase slugs that govern the nature of the particle size distribution. The reduction in the axial dispersion has less impact on particle growth and hence on the particle size distribution. Synthesis of gold nanoparticles from HAuCl(4) with rapid reduction by NaBH(4) serves as a model system. Rapid reduction yields gold nuclei, which grow by agglomeration, and it is controlled by the interaction of the nuclei with local flow. Thus, the difference in the physical properties of the two phases and the inlet flow rates ultimately control the particle growth. Hence, a careful choice of continuous and dispersed phases is necessary to control the nanoparticle size and size distribution.     

电导法测定无机盐对十二烷基磺酸钠溶液临界胶束浓度的影响

在40℃时利用电导法测定了无机盐NaCl、KCl、CuCl2、ZnSO4、Fe(NO3)3及AlCl3对十二烷基磺酸钠(SDS)溶液临界胶束浓度(CMC)的影响,并推导了表示无机盐浓度和SDS溶液CMC值之间关系的线性方程.结果表明,随着各种无机盐浓度的增加,SDS溶液的CMC值降低,且不同价态的金属无机盐对SDS溶液...     

Separation of rutin nona(H-) and deca(H-) sulfonate sodium by ion-pairing reversed-phase liquid chromatography

Ion-pairing reversed-phase liquid chromatography (RPLC) was used to separate two polysulfonates, rutin nona(H-) sulfonate sodium and rutin deca(H-) sulfonate sodium, which have very similar chemical structures. The final product always contained both of them when one of the compounds was synthesized. Baseline separation was achieved on a C8-bonded silica column at ambient temperature. The eluent was acetonitrile-15 mM phosphate buffer solution containing 20 mM TBA (pH 6.0) (46:54, v/v). The calibration plot was linear in the concentration range 0.5-200 microg ml(-1) for both analytes. The limits of detection (LODs; 254 nm) were 0.03 microg ml(1-) for rutin nona(H-) sulfonate sodium and 0.04 microg ml(-1) for rutin deca(H-) sulfonate sodium. Three batches of rutin deca(H-) sulfonate sodium were analyzed using the assay; the results showed that the analytical performance is really satisfactory.     

Size-controlled assembly of gold nanoparticles induced by a tridentate thioether ligand

The ability to control the size and shape of nanoparticle assemblies is essential for the ultimate applications in sensors, catalysis, medical diagnostics, information storage, and quantum computation. This report demonstrates a novel mediator-template strategy toward this ability by exploring molecular driving forces exerted by a tridentate thioether as a mediator and tetraoctylammonium bromide as a templating agent. A combination of the ligand mediation, the surfactant templating, and their relative concentrations served as the driving forces. This combination leads to unprecedented spherical assemblies of gold nanoparticles in controllable sizes via manipulation of the relative concentrations of mediating and templating components.     

卡络磺钠与牛血清蛋白荧光光谱的研究

采用荧光光谱法研究了卡络磺钠CSS (Carbazochrome Sodium Sulfonate)与牛血清蛋白(BSA)结合反应的特征, 测定了结合常数(K=1.32×105 L/mol) 和结合位点数(n=1.28). 依据Foster非辐射能量转移理论, 确定了给体-受体间的结合距离(r=4.896 nm)和能量转移效率, 采用同步荧光技术考察了CSS对BSA构象的影响.     

聚对苯乙烯磺酸钠添加剂的分子量对水煤浆浆体性质的影响

选用了变质程度不同的八种煤和三种不同分子量的聚对苯乙烯磺酸钠（PSS）添加剂,详细考查了该添加剂的分子量对水煤浆浆体性质的影响。结果发现,在考查PSS相对分子量的范围内（质均分子量为5.34×104～33.39×104）,八种煤的水煤浆成浆性随着分子量的增大而增加,水煤浆成浆性与PSS添加剂的平均分子量的关系可归因于添加剂在煤粒上的吸附,分子量小的PSS在煤粒上的吸附量大于分子量大的PSS;PSS分子量的增加有利于水煤浆的流变性由胀性向假塑性转变;PSS分子量的增加使水煤浆的静态稳定性得到显著的改善。