超细稀土氧化物粉体粒度测定

采用美国布鲁克海文仪器公司制造的90 Plus粒度仪测定超细稀土氧化物粉体粒度. 以氧化钇为研究对象, 研究了分散剂、悬浮介质、待测样品浓度、分散时间等因素对亚微米级氧化钇粉体粒度测量精度的影响. 由此确定了能准确测定亚微米级氧化钇粉体粒度的测量条件.     

抑制型离子色谱测定纳米金刚石粉末表面吸附的阴离子

采用抑制型离子色谱法，以NaHCO3/Na2CO3作流动相，测定了纳米金刚石粉末表面吸附的F^-、Cl^-、SO4^2-、NO3^－等阴离子的浓度，研究了淋洗液浓度对离子保留的影响以及样品处理中超声洗脱分散时间对测定结果的影响。适宜的流动相为0.84mmol/L NaHCO3 0.9mmol/L Na2CO3；超声洗脱分散时间应在10min以上。在此流动相条件下测定了上述6种阴离子的检出限及其它定量参数。方法应用于纳米金刚石粉末试样的分析，结果良好。     

氧化钇粒度控制与测定

用氨水或碳酸氢铵与氯化钇溶液反应生成沉淀，煅烧沉淀制备了D50为0．45μmt 2-10μm的各种粒径的氧化钇粉末。分别采用Coulter MultisizerⅡ和90Plus粒度仪测定微米和亚微米级氧化钇粉体粒度，研究了分散剂，待测样品量，分散时间等因素对亚微米级氧化钇粉体粒度测量精度的影响。     

纳米ATO颗粒粒度分布的脉冲超声波测量研究

讨论了脉冲超声波测量纳米ATO颗粒粒度分布方法中的3个步骤,即超声波衰减谱测量、严格数学模型的选型以及颗粒粒度分布的反演计算.通过发射脉冲超声波并利用变声程方法测量25 ℃时2%(体积分数)的纳米ATO-H2O分散液的超声衰减谱;选取McClements理论模型叠加BLBL理论模型共同描述纳米ATO颗粒分散液中的超声衰减现象;采用最优正则优化反演算法反演得到纳米ATO颗粒的粒度分布以及平均粒径.脉冲超声法检测结果显示,纳米ATO颗粒的平均粒径为25.6 nm,粒度分布为11.4 ～47.1 nm,CPS离心沉降纳米粒度分析仪测定结果分别为22.1 nm和10.1 ～62.6 nm.脉冲超声法检测结果与透射电镜图像以及离心沉降纳米粒度分析仪检测结果吻合较好,证明了脉冲超声波测量纳米颗粒粒度分布以及平均粒径的可行性与可靠性.     

TMAH对TiN纳米粉体分散行为的影响

采用四甲基氢氧化铵(TMAH)作为分散剂,利用沉降法、ξ电位、粒度分析、TEM等研究了TiN纳米粉体在水介质中的分散稳定机制,探讨了pH值和分散剂对纳米颗粒分散行为的影响。结果表明：TiN纳米粉体的分散行为遵循静电稳定机制,pH值对TiN纳米粉体的分散性和稳定性有较大影响,在pH=8处TiN纳米粉体有较好的分散效果。有机阳离子型分散剂TMAH能在TiN纳米颗粒表面形成特征吸附,并通过静电作用和空间位阻作用提高TiN纳米颗粒的分散性。在pH=8、TMAH加入量为0.75wt%的条件下,TiN纳米粉体获得无团聚的最佳分散状态,悬浮液稳定时间可达1个月。     

纳米颗粒跟踪分析仪用于二氧化钛纳米颗粒分散及检测

以纳米颗粒跟踪分析仪为检测手段,建立了二氧化钛(TiO2)纳米颗粒分散和检测的方法,考察了分散剂种类、超声方式、超声时间、超声温度、分散试剂浓度、pH值对TiO2分散的影响,以及本分散方法对于一般商品TiO2的通用性.采用NTA测定粒径和颗粒数量浓度,对检测过程中稀释试剂浓度、稀释倍数等检测条件进行了优化,颗粒数量浓度...     

均匀沉淀法制备单分散纳米ZnS及发光性能

采用均匀沉淀法,乙酸锌和硫代乙酰胺(TAA)分别提供Zn源和S源,无水乙醇为分散介质,十八胺(ODA)为分散剂,成功制备了小于50nm的单分散ZnS纳米颗粒,并就反应温度、分散剂浓度、溶液浓度和陈化时间对ZnS纳米颗粒粒径的影响进行系统研究。用SEM、激光纳米粒度仪、XRD、PL、EL对样品进行了表征,结果表明:维持一定的分散剂和溶液浓度于0℃陈化24h,样品粒径最小且结晶度佳,干燥和退火后的发光样品在275nm的紫外光激发下发射出490nm左右的蓝绿光,在2kV(样品厚度1mm)激励下发射出520nm的绿光。     

聚己内酯型超分散剂对磁浆流变行为和分散效果的影响

研究了磁性悬浮体（磁浆）的流变行为和分散稳定性，在磁浆中加入聚己内酯型超分散剂可显著降低体系的剪切粘度，提高分散体的稳定性，超分散剂的分散效果与溶化链分子量和锚固基团种类密切相关，当溶剂化链分子量为７００、锚固基团为氨基和羧基混合物，分子结构为“梳状”时，超分散剂的分散效果最佳。     

高频超声照射下血卟啉镓配合物对脱氧核糖核酸的损伤

用紫外-可见(UV-Vis)光谱和荧光(FL)光谱研究了高频超声波激活血卟啉镓(HP-Ga)配合物对脱氧核糖核酸(DNA)的损伤，并探讨了超声波照射时间、HP-Ga浓度、溶液酸度和离子强度等因素对DNA损伤的影响。结果表明，在一定条件下，DNA的损伤程度随着超声波照射时间的增加和HP-Ga浓度的增大而加剧，而溶液酸度和离子强度的影响则较为复杂。     

分光光度法测定马来酰肼中痕量肼

采用碱溶中和法提高马来酰肼(MH)溶液试样中肼的浓度，分别采用对二甲氨基苯甲醛(DAB)和茚三酮测定MH中的痕量肼。结果表明，DAB的乙醇溶液和二甲基亚砜(DMSO)溶液作为显色剂时，在痕量肼浓度范围内具有良好线性关系，前者在0～0.1mg/L肼浓度范围内，线性方程为y=0.9733x-0.0018，线性相关系数(R²)为0.9987；后者在0～0.05 mg/L肼浓度范围内，线性方程为y=1.4672x-0.0016, R²为0.9982；茚三酮作显色剂时仅在较高肼浓度范围2.4～12 mg/L时呈线性关系，线性方程为y=0.0067x-0.003, R²=0.9899。加入乙醇有利于相关试剂和生成物溶解，而且比加入DMSO耐光照。     

超声衰减谱测量电池浆料的粒度分布

电池浆料中颗粒状活性物质的粒度大小和分散均匀性对电池的内阻、 电压、 局部表面电流和总极化程度等性能有直接影响, 实现对其的在线实时测量对电池的质量控制具有重要意义. 基于电池浆料的高固含量、 高黏度和低透光性的特点, 本文利用超声衰减谱的方式测量了其粒度分布(PSD). 应用于电池浆料的粒度分布测量的最大难点是其利用超声衰减谱法预测粒度分布的模型需要难以获得的分散相和连续相的物性参数. 本文采用主成分分析(PCA)结合误差反向传播(BP)神经网络建立预测模型解决了超声衰减谱法的难点, 并引入遗传算法(GA)优化BP神经网络的初始阈值和权值. 通过以LiCoO₂为活性物质的电池浆料进行了验证, 结果表明, PCA-GA-BP神经网络能够有效对不同固含量电池浆料的粒度分布进行预测, 预测值与真实值的峰形重合度高, 峰高偏差小, 两者的均方误差为0.1358, 拟合度(R²)为0.9816, 说明超声衰减谱法可作为测量电池浆料粒度分布的重要方式.     

动态光散射法测量颗粒粒径的溯源性

分别对动态光散射粒径测量仪的入射波长、散射角度、测量池温度进行校准,并对影响测量结果准确性各因素的不确定度分量进行了评价,校准后动态光散射仪的测量结果可溯源至国家计量标准。为消除多重散射、颗粒间相互作用、颗粒粒径分布对动态光散射测量结果的影响,建立了动态光散射测量结果修正方法。其中为消除多重散射及颗粒间相互作用的影响,需采用多浓度测量或线性回归的方法得到特定浓度下的颗粒粒径;为修正颗粒粒径分布对动态光散射测量结果的影响,需先采用SEM方法准确测量颗粒粒径分布,然后根据光强加权动力学平均粒径和数量平均粒径的理论公式,得到二者之间的差异。     

Development and Optimization of a Procedure for the Determination of Indium-Tin Oxide Particle Size and Concentration in Cellular Media

Indium-tin oxide (ITO) is a solid mixture often comprised of approximately 90% indium oxide and 10% tin oxide by weight. ITO is employed as a transparent conductive coating for flat panel, liquid crystal, and plasma displays and is typically deposited after sintering as a thin film on a substrate through a variety of processes. Unfortunately, there have been published reports of workers who have been adversely impacted through exposure to this compound. When these reports are coupled with the industrial utility of ITO, future toxicological investigations are likely. Comprehensive characterization of ITO test materials would be an essential component of these studies. Ideally, characterization would include assessment of ITO particle size as administered during dosing because this physicochemical parameter can significantly impact solubility. The objective of this task was to develop, optimize, and apply a dynamic light scattering (DLS) sample preparation and measurement protocol for determination of particle size for a suite of sintered/non-sintered ITO samples prepared in cellular growth media at nominal 0.3 mg/mL doses. Sonication time was evaluated from 15 to 90 minutes over a 24-hour, continuous DLS measurement period. Resulting suspensions from samples subjected to 30 minute sonication times were stable with respect to hydrodynamic particle size between 10 and 24 hours after sonication. Throughout the 24-hour DLS measurement period, suspension aliquots were analyzed by inductively coupled plasma mass spectrometry to determine indium concentration. The developed protocol enabled investigators to use ITO suspensions of known hydrodynamic particle size and concentration in their in vitro cellular study.     

同时测量纳米颗粒悬浊液粒度、密度及浓度的方法研究

提出了一种基于超声检测同时测量纳米颗粒悬浊液的粒度、密度和浓度的方法.设计了一套高频宽带脉冲超声波检测系统,以纳米掺锑氧化锡(ATO)悬浊液为研究对象,结合脉冲回波技术,获得了频率为17 ～ 26 MHz的声衰减谱.据此运用最优正则化方法求解粒度反演方程,得到纳米ATO颗粒的分布曲线,中位径为22.07 nm,该值与离...     

商用聚丙烯酸类高吸水树脂粒子尺寸及分布与其凝胶浓度的关系

研究了6种商用聚丙烯酸类高吸水树脂(SAP)粒子尺寸大小及分布对其形成凝胶的临界浓度的影响,通过傅里叶变换红外光谱、X射线光电子能谱对样品的成分进行了分析,使用光学显微镜和ImageJ软件统计了样品未吸水时粒子的尺寸及分布,通过测定样品吸水后的膨胀比,估算得到了样品吸水后的粒子的尺寸及分布,用流变学方法和倒置实验法测定了高吸水树脂形成凝胶的临界浓度(凝胶点)。 结果表明,这6种商用聚丙烯酸类高吸水树脂吸水后的粒子的尺寸大小对其形成凝胶的临界浓度的影响不符合理论预测,这是由于粒子尺寸分布宽度不均一造成的。 在选择粒子大小分布占优的均一范围内,样品的凝胶浓度随着粒子尺寸的增大而降低。     

Measuring Bismuth Oxide Particle Size and Morphology in Film-Coated Tablets

The assessment of active pharmaceutical ingredient (API) particle size and morphology is of great importance for the pharmaceutical industry since it is expected to significantly affect physicochemical properties. However, very few methods are published for the determination of API morphology and particle size of film-coated (FC) tablets. In the current study we provide a methodology for the measurement of API particle size and morphology which could be applied in several final products. Bismuth Oxide 120 mg FC Tabs were used for our method development, which contain bismuth oxide (as tripotassium dicitratobismuthate (bismuth subcitrate)) as the active substance. The sample preparation consists of partial excipient dissolution in different solvents. Following this procedure, the API particles were successfully extracted from the granules. Particle size and morphology identification in Bismuth Oxide 120 mg FC Tabs was conducted using micro-Raman mapping spectroscopy and ImageJ software. The proposed methodology was repeated for the raw API material and against a reference listed drug (RLD) for comparative purposes. The API particle size was found to have decreased compared to the raw API, while the API morphology was also affected from the formulation manufacturing process. Comparison with the RLD product also revealed differences, mainly in the API particle size and secondarily in the crystal morphology.     

Preparation of Small Particle Sized ZnAl-Hydrotalcite-Like Compounds by Ultrasonic Crystallization

Ultrasonic technology has been intensively studied recently due to its special features. In this paper, an ultrasonic crystallization method was introduced for the preparation of ZnAl-Hydrotalcite-Like compounds (ZnAl-HTLcs). Samples with high crystallinity, small particle size and narrow particle size distribution were obtained and fully characterized using conventional techniques of XRD, FT-IR and TGDTA. The results prove that both ultrasonic frequency and ultrasonic power have effects on the sizes of the product particles. By varying the ultrasonic power from 250 W to 88 W, with the ultrasonic frequency fixed at 59 kHz, the median particle size of the samples increased from 0.37 μm to 0.82 μm. By altering the hydrothermal treatment time from 1 h to 5 h at 110℃, the median particle size of ZnAl-HTLcs synthesized via ultrasonic crystallization increased from 0.88 μm to 1.11 μm.     

用动态激光散射法测定悬浮液中颗粒尺寸分布的一些经验

介绍了用动态激光散射仪测定用炸药爆炸法制备的纳米金刚石粉在水悬浮液中的颗粒尺寸分布时,取得的一些经验和教训.指出,在悬浮液样品制备和测定条件选择上的一些重要因素,必须认真对待,才能得到重复性良好的结果.可供从事此项工作的人士参考.     

Some Observations on Particle Size and Velocity Measurements Using Phase Doppler Anemometry in Plasma Spray

Applications of Phase-Doppler anemometry to the measurements of metal (nickel) particle size and velocity in the plasma spray process have been studied and analyzed with the aid of Mie scattering theory. The optimum optical settings used in two PDA systems were determined and tested experimentally. Measurements at cross-sectional planes 5 and 10 cm below the SG-100 (Miller) plasma gun were obtained and discussed. In this study, only one particle injection port was used. It is noticed that the variation of the percentage of the diameter validation rate would affect the volume flux results considerably. If the diameter validation rate can be maintained above 65%, the integrated volume flux would be close to the results obtained from the total volume deposited on a substrate or from the estimation based on the mass balance in the powder feeder (measured before and after spraying). The PDA measurement may also provide some predictions on the deposition area and the corresponding maximum height of the coating at a specific stand-off distance from the nozzle.     

T形微反应器共沉淀法制备Mg-Al层状双金属氢氧化物及其粒径可控性

采用T形微反应器通过共沉淀法制备了Mg-Al层状双金属氢氧化物(LDHs)纳米颗粒, 考察了流速、混合盐溶液浓度和温度等对产物粒径及其分布的影响. 实验结果表明, 所制备的LDHs样品的形貌和晶体结构与传统共沉淀法结果一致, 但本方法制备的样品粒径小、分布窄. 随着流速增大, 温度升高, 所合成的LDHs样品平均粒径减小, 分布变窄; 而随着混合盐溶液浓度的增大, 所得LDHs样品粒径增大, 分布变宽.