基于机器人制样和激光诱导击穿光谱分析技术的选煤厂检测系统无人化

目前选煤厂煤质检测过程自动化程度低,采样与制样技术需要大量的人工参与。检测技术的落后直接影响数据的准确性从而对整个选煤厂生产过程控制与产品质量控制产生重要影响,直接关系选煤厂的经济效益。面对产业升级的需要,将先进的自动采制样技术引进煤炭生产经营企业是当务之急。机器人采制样系统包含:机械化采样与初制样技术、机器人精细化制样技术、煤炭快速检测技术、自动快速浮沉技术,为选煤厂提供了一种全自动采制检的新技术方案。     

A study on preparation of glucoamylase by irradiation

A study on preparation of industrial glucoamylase irradiated by ⁶⁰Co gamma-ray showed that an abvious change took place in the extraviolet absorption spectrum and the pH - value of the enzyme solution and the activity of the enzyme preparation was much more resistant to irradiation than that of microbes contained in the preparation. The result indicates that irradiated glucoamylase preparation is not only favourable to activity preservation but also is improved in the hygienic quality of products. A comparison of the various properties of irradiated enzyme preparation with those of unirradiated one has proved that irradiation does not change the normal application of glucoamylase preparation.     

复合乳液乳胶粒样品的制备

报道了利用火棉胶支持膜制取复合乳液乳胶粒样品的技术，不同于传统制作方法，其所其制备的样品具有分散度好，样品边界清晰等优点。     

制样方法对固体粉末X射线光电子能谱测试结果的影响

为了得到准确且分辨率高的X射线光电子能谱(XPS)数据,采用不同制样方法对不同类型的导电、不导电和混合粉末的测试结果进行了研究. 从图谱半峰宽、是否有荷电、真实性、制样效率和数据处理等方面阐述不同制样方法对测试结果的影响. 试验结果表明,对于导电和不导电粉末,粘取制样略优于铟片制样,其中使用碳导电胶带制样效果更好. 对于混合样品,Scotch双面胶带粘样后的测试结果优于其他3种制样方式. 此外,铟片制样可作为数据处理时荷电校正的参考方法.     

Recent progress of microfluidic sample preparation techniques

Sample preparation turns out to be one of the important procedures in complex sample analysis by affecting the accuracy, selectivity, and sensitivity of analytical results. However, the majority of the conventional sample preparation techniques still suffer from time-consuming and labor-intensive operations. These shortcomings can be addressed by reforming the sample preparation process in a microfluidic manner. Inheriting the advantages of rapid, high efficiency, low consumption, and easy integration, microfluidic sample preparation techniques receive increasing attention, including microfluidic phases separation, microfluidic field-assisted extraction, microfluidic membrane separation, and microfluidic chemical conversion. This review overviews the progress of microfluidic sample preparation techniques in the last 3 years based on more than 100 references, we highlight the implementation of typical sample preparation methods in the formats of microfluidics. Furthermore, the challenges and outlooks of the application of microfluidic sample preparation techniques are discussed.     

碳纳米管的最新制备技术及生长机理

结合笔者的工作综述了碳纳米管的制备技术及生长机理的最新研究进展，重点介绍了近两年来碳纳米管制备的进展情况，包括传统制备方法的改进（电弧放电法、化学气相沉积法和激光蒸发法）、新型制备技术、特殊结构的碳纳米管制备；同时探讨了碳纳米管的各种生长机理；最后提出了碳纳米管制备技术和生长机理的发展方向。     

标准气体的制备方法及配制技术

介绍标准气体的制备及杂质去除方法，包括单一组分纯气体的制备方法和混合气体的配制方法，5种常用气体的配制方法及特殊性质的标准气体的配制方法。     

Measurement uncertainty from physical sample preparation: estimation including systematic error

A methodology is proposed, which employs duplicated primary sampling and subsequent duplicated physical preparation coupled with duplicated chemical analyses. Sample preparation duplicates should be prepared under conditions that represent normal variability in routine laboratory practice. The proposed methodology requires duplicated chemical analysis on a minimum of two of the sample preparation duplicates. Data produced from the hierarchical design is treated with robust analysis of variance (ANOVA) to generate uncertainty estimates, as standard uncertainties ('u' expressed as standard deviation), for primary sampling (ssamp), physical sample preparation (sprep) and chemical analysis (sanal). The ANOVA results allow the contribution of the sample preparation process to the overall uncertainty to be assessed. This methodology has been applied for the first time to a case study of pesticide residues in retail strawberry samples. Duplicated sample preparation was performed under ambient conditions on two consecutive days. Multi-residue analysis (quantification by GC-MS) was undertaken for a range of incurred pesticide residues including those suspected of being susceptible to loss during sample preparation procedures. Sampling and analytical uncertainties dominated at low analyte concentrations. The sample preparation process contributed up to 20% to the total variability and had a relative uncertainty (Uprep%) of up to 66% (for bupirimate at 95% confidence). Estimates of systematic errors during physical sample preparation were also made using spike recovery experiments. Four options for the estimation of measurement uncertainty are discussed, which both include and exclude systematic error arising from sample preparation and chemical analysis. A holistic approach to the combination and subsequent expression of uncertainty is advised.     

纳米纤维素的制备*

在纳米尺寸范围操控纤维素分子及其超分子聚集体,结构设计并组装出稳定的多重花样,由此创制出具有优异功能的新纳米精细化工品、新纳米材料,是纤维素科学的前沿领域和热点。为了研究当前制备纳米纤维素的现状和发展方向,简述了纳米纤维素化学基础,介绍了三类纳米纤维素：纳米纤维素晶体（晶须）、纳米纤维素复合物和纳米纤维素纤维,重点综述了纳米纤维素的五种制备方法：化学法制备纳米纤维素晶体和晶须、生物法制备细菌纤维素、物理法制备微纤化纳米纤维素、人工合成纳米纤维素和静电纺丝制备纤维素纤维,讨论了各种制备方法的优点和缺点,指出开展纳米纤维素超分子的可控结构设计、立体与位向选择性控制与制备、分子识别与位点识别等自组装过程机理、多尺度结构效应的形成机理等基础理论性研究是主要研究基础,新型的、绿色、低能耗、快速、高效的制备方法是纳米纤维素制备方法的发展方向。     

alpha-N-benzoylarginine-2-naphthylamide hydrolase (cathepsin B1 ?) from rat skin. II. Purification of the enzyme and demonstration of two inhibitors in the skin.

A thiol-activated, alpha-N-benzoylarginine-2-naph-thylamide (BANA) hydrolyzing enzyme was purified from rat skin by ammonium sulfate precipitation, gel filtration, and DEAE cellulose chromatography. In DEAE cellulose chromatography the enzyme was fractionated into two multiple forms (preparations I and II). The activity of undiluted preparation II, but not that of preparation I, was increased, when the enzyme was preincubated at pH 4, at 55 degrees C. Simultaneously, the isoelectric point of preparation II was shifted to that of preparation I, i.e., from 6.2 to 7.5. Activated preparation II behaved in DEAE cellulose chromatography as preparation I. Molecular weights of the enzymes of both preparations were 27 000, and pH optima were at pH 5.8 and 7.0, for BANA and leucine-2-napthylamide (Leu-NA), respectively. The BANA and Leu-NA hydrolyzing enzymes could not be separated by gel filtration, DEAE, CM, or Amberlite IRC-50 chromatography, isoelectric focusing, or analytical polyacrylamide gel electrophoresis. Two inhibitors of BANA hydrolase were demonstrated by gel filtration in the salt precipitated skin extract. The activities of the BANA hydrolase preparations did not increase linearly with increasing enzyme concentration, with the exceptions of activities of preparation I and acid-activated preparation II. The role of the inhibitors in the nonlinearity of the activity/enzyme concentration curves is discussed.     

Miniaturized sample preparation combined with liquid phase separations

Miniaturized sample preparation methods designed as the sample pretreatment for liquid phase separations, such as liquid chromatography, capillary electrophoresis and capillary electrochromatography, have been reviewed especially for the on-line coupling of the sample preparation process and the separation process. The development of the desorption interfaces for the effective combining of the sample preparation and subsequent liquid phase separations is briefly described along with the applications of the combined analytical systems to the analysis of complex sample mixtures such as biological and environmental matrices. Novel use of fine polymeric filaments as the extraction medium for microscale liquid phase separation methods are investigated and a comparison is made with other sample preparation techniques. Polymer coating onto the fibrous material is also introduced to further develop microscale sample preparation methods with improved extraction performance. Several other microscale sample preparation methods having a potential compatibility to the liquid phase separations are also described for future applications of these techniques.     

介孔氧化铝的制备及应用

本文介绍了介孔氧化铝(MA)的各种制备方法,概括了MA制备的分析表征方法,如TEM、SAED、XRD、LAXRD、气体吸附-脱附、DT-TGA等。通过平均孔径、比表面积、MA形貌等因素,讨论和总结了制备方法、铝源、模板剂、反应物配比、pH值和后处理方法等对MA制备和热稳定性的影响,综述了近年来MA的研究和应用进展,并对今后的研究方向进行了展望。     

直接法制备三乙氧基硅烷催化剂的研究进展

综述了直接法合成三乙氧基硅烷的研究进展,着重对直接法的反应机理和催化剂组分的筛选进行了分析讨论.同时介绍了以三乙氧基硅烷为原料,合成烯丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三乙氧基硅烷、苯乙基三乙氧基硅烷、五乙氧基二硅烷等衍生物的工艺,提出了催化剂制备过程中存在的问题及研究方向.     

自组装单层膜的制备与应用

本文综述了自组装单层膜制备及应用技术的最新发展,分别对有机硅烷/羟基化表面和硫醇/金两种重要的自组装单层膜体系的制备新技术以及在制膜技术和分子电子学等领域的最新应用进行了总结.     

Neue untersuchungen zur prăparativen darstellung von brommonofluorid: Darstellung und eigenschaften des brommonofluorid-pyridin-komplexes.

New investigations on the preparation of bromine monofluoride: preparation and properties of the bromine monofluoride pyridine complex.The reactions of bromine with fluorine, of bromine trifluoride with bromine as well as of the pyridine complexes of bromine trifluoride and bromine will be described. In presence of cesium fluoride bromine trifluoride disproportionates to bromine pentafluoride and bromine monofluoride. Bromine monofluoride may be isolated as its pyridine complex. The preparation and the properties of the bromine monofluoride pyridine complex will be described. In addition, the preparation of a bromine trifluoride pyridine complex will be reported.     

Main stages of gluing technology

The main stages of gluing technology—from surface preparation for gluing to control of the quality of adhesive joints—are considered. Methods of preparation for gluing of surfaces of polymer materials and metals are given. Recommendations for preparation and coating of adhesives are given. The main parameters of the adhesive curing and apparatus used are described.     

Nano-emulsions: New applications and optimization of their preparation

Nano-emulsions, as non-equilibrium systems, present characteristics and properties which depend not only on composition but also on the preparation method. Although interest in nano-emulsions was developed since about 20 years ago, mainly for nanoparticle preparation, it is in the last years that direct applications of nano-emulsions in consumer products are being developed, mainly in pharmacy and cosmetics. These recent applications have made that studies on optimization methods for nano-emulsion preparation be a requirement. This review is focused on the most recent literature on developments of nano-emulsions as final application products and on the optimization of their preparation.     

基于色谱-质谱联用的脂质分析样品前处理技术研究进展

脂质作为细胞膜和亚细胞膜的主要结构成分,在能量来源、细胞信号传导等多种生物学过程中发挥着重要作用。近年来,脂质分析受到越来越多的关注,其中色谱-质谱联用技术在脂质分析中占据主导地位。由于样品基质复杂,样品前处理有富集痕量物质和减少基质干扰的作用,成为脂质分析中的一个关键步骤。该文综述了近年来基于色谱-质谱联用技术的脂质分析中样品前处理技术的研究进展和应用,对各种样品前处理技术进行了阐述和总结。基于液相的萃取方法有液-液萃取和单一有机溶剂萃取。基于固相的萃取方法包括固相萃取和固相微萃取。场辅助萃取方法包括超临界流体萃取、加压流体萃取、微波辅助萃取和超声辅助萃取。此外,还介绍了在线联用样品前处理方法和用于活体分析的样品前处理方法。最后,对基于色谱-质谱联用的脂质分析样品前处理技术存在的问题及发展趋势进行了探讨。样品前处理技术的发展将提高脂质分析的灵敏度、选择性和分析速度。     

高纯橙皮素的制备及HPLC纯度分析

建立了一种基于反相硅胶纯化的高纯橙皮素制备方法,充分优化了上样量、流速及洗脱液极性等因素,采用红外光谱法和核磁共振对纯化后产物进行定性分析,高效液相色谱法检测纯化前后橙皮素的纯度,最终产物的纯度达99.87%。该方法快速简便、制备量大、分离效率高,每天制备效率可达到克级,为制备橙皮素标准物质提供了技术支撑。     

Preparation of thin-sections of painting fragments: Classical and innovative strategies

For more than a century, the analyses of painting fragments have been carried out mainly through the preparation of thick resin-embedded cross-sections. Taking into account the development of innovative micro-analytical imaging techniques, alternatives to this standard preparation method are considered. Consequently, dedicated efforts are required to develop preparation protocols limiting the risks of chemical interferences (solubilisation, reduction/oxidation or other reactions) which modify the sample during its preparation, as well as the risks of analytical interferences (overlap of detected signals coming from the sample and from materials used in the preparation). This study focuses particularly on the preparation of thin-sections (1–20 μm) for single or combined fourier transform infrared (FTIR) spectroscopy and X-ray 2D micro-analysis. A few strategies specially developed for the μFTIR analysis of painting cross-sections have already been reported and their potential extrapolation to the preparation of thin-sections is discussed. In addition, we propose two new specific methods: (i) the first is based on a free-embedding approach, ensuring a complete chemical and analytical neutrality. It is illustrated through application on polymeric design objects corpus; (ii) the second is based on a barrier coating approach which strengthens the sample and avoids the penetration of the resin into the sample. The barrier coating investigated is a silver chloride salt, an infrared transparent material, which remains malleable and soft after pellet compression, enabling microtoming. This last method was successfully applied to the preparation of a fragment from a gilded Chinese sculpture (15th C.) and was used to unravel a unique complex stratigraphy when combining μFTIR and μXRF.