选矿产品矿物自动分析的光片制备

基于扫描电子显微镜的矿物自动分析仪(Quantitative Evaluation of Minerals by Scanning Electronic Microscopy)、MLA (Mineral Liberation Analyser)和AMICS(Advanced Mineral Identification and Characterization System)可用于测定选矿产品中目的矿物的粒度和单体解离度,为确定合理的磨矿细度以及优化选矿工艺流程提供依据。环氧树脂光片的制备是矿物自动识别和测量的最关键的一环,其代表性直接关系到后续数据测量的准确性和真实性。对于金属矿产品来说,由于选矿产品中矿物颗粒粗细不均、密度差异较大,在环氧树脂胶结固化过程中矿物颗粒会产生明显的分异作用并互相黏连,造成分析结果失真。实验证明,把样品与晶质石墨混均,然后加入环氧树脂以及固化剂搅拌混合倒入圆柱状模具进行冷镶嵌,待样品固化后再沿圆柱体的纵向进行切割,并对其切割面进行粗磨、细磨、精磨以及抛光,就可以制备出样品分散性好、分布均匀、表面光滑平整的具有代表性的环氧树脂光片。     

基于扫描电子显微镜-X射线能谱的矿物自动分析系统(BPMA)测定高纯石英砂中杂质矿物

杂质矿物作为高纯石英中杂质元素主要载体之一,是高纯石英砂产品中严格限定的成分,也是影响高纯石英提纯方案的关键因素,对其组成、含量及赋存特征进行准确分析测定对高纯石英砂产品质量评价、原料选择合理性判断及提纯方案制定均有重要意义。采用基于扫描电子显微镜（SEM）和X射线能谱（EDS）的工艺矿物学参数自动分析系统（BPMA）测定了SiO2纯度≥99.998 %（4N8）的高纯石英砂中杂质矿物的组成、含量及嵌布特征,建立了高纯石英砂中杂质矿物的分析测定方法。结果表明：样品中石英的重量百分比为99.9988 %,与高纯石英砂产品质量指标对应的SiO2纯度化学分析结果基本一致;杂质矿物主要为辉石和锆石,偶见极其微量的方解石、磷钇矿、独居石和方铅矿;石英粒度均匀,主要分布在0.020～0.208 mm之间;杂质矿物嵌布粒度较细,绝大多数杂质矿物粒度在43 μm以下,主要以微细粒矿物包裹体的形式嵌布在石英颗粒内。方法简捷高效、测量结果准确可靠,适用于高纯石英砂中杂质矿物组成、含量及赋存特征分析测定,也可以为其它高纯物料中微量杂质矿物检测提供技术借鉴。     

岩石矿物分析

评述了2004年6月～2006年6月期间国内在岩石矿物分析领域的现状及进展概况。内容包括综述与会议、试样的前处理、重量法和容量法、光度法、原子光谱法、电化学分析法、X射线荧光光谱法、色谱、质谱及中子活化分析法、化学物相分析及形态分析、联用技术、质量控制及标准方法等。收集文献352篇。     

岩石矿物分析

评述了2006年6月-2008年5月期间国内在岩石矿物分析领域的研究与应用现状及进展概况。内容包括综述与会议、试样的前处理、滴定法和重量法、光度法、原子光谱法、电化学分析法、X射线荧光光谱法、电感耦合等离子体质谱法及联用技术、化学物相分析及形态分析、质量控制及标准方法等。收集文献462篇。     

岩石矿物分析

评述了2012年6月至2014年5月期间国内在岩石矿物分析领域的研究与应用现状及进展概况。内容包括综述与会议、试样的前处理、X射线荧光光谱法、原子光谱分析法、光度分析法、电感耦合等离子体质谱法、滴定法和重量法、电化学分析法、化学物相分析及形态分析、质量控制及标准物质、标准方法等。收集文献648篇。     

岩石矿物分析

评述了2008年6月~2010年5月期间国内在岩石矿物分析领域的研究与应用现状及进展概况。内容包括综述与会议、试样的前处理、容量法和重量法、光度法、原子光谱法、X射线荧光光谱法、电感耦合等离子体质谱法、电化学分析法、化学物相分析及形态分析、质量控制及标准物质、标准方法等。收集文献429篇。     

岩石矿物分析

评述了2010年6月～2012年5月期间国内在岩石矿物分析领域的研究与应用现状及进展概况。内容包括综述与会议、试样的前处理、滴定法和重量法、光度法、原子光谱法、X射线荧光光谱法、电感耦合等离子体质谱法、电化学分析法、化学物相分析及形态分析、质量控制及标准物质、标准方法等。收集文献582篇。     

矿物分析技术及进展

评述了2001年11月至2003年10月期间国内有关矿物分析技术的现状及进展概况。内容包括综述与会议、重量法与滴定法、光度法、电化学分析法、原子光谱分析法、X射线荧光光谱法、电感耦合等离子体质谱法、联用技术、国家标准方法及其它。     

水中矿物元素的ICP-MS分析

用ICP－MS对地下水、地表水和饮用水中的矿物元素进行了分析测定，实验证明用ICP－MS可以同时测定地下水，地表水和饮用水中矿物元素；该法灵敏度、精密度和准确度都能满足有关标准的要求，具有多元素同时分析，样品前处理简单，干扰少，测定快速，省事省力等优点。     

A flow-batch analyzer with piston propulsion applied to automatic preparation of calibration solutions for Mn determination in mineral waters by ET AAS

The increasing development of miniaturized flow systems and the continuous monitoring of chemical processes require dramatically simplified and cheap flow schemes and instrumentation with large potential for miniaturization and consequent portability. For these purposes, the development of systems based on flow and batch technologies may be a good alternative. Flow-batch analyzers (FBA) have been successfully applied to implement analytical procedures, such as: titrations, sample pre-treatment, analyte addition and screening analysis. In spite of its favourable characteristics, the previously proposed FBA uses peristaltic pumps to propel the fluids and this kind of propulsion presents high cost and large dimension, making unfeasible its miniaturization and portability. To overcome these drawbacks, a low cost, robust, compact and non-propelled by peristaltic pump FBA is proposed. It makes use of a lab-made piston coupled to a mixing chamber and a step motor controlled by a microcomputer. The piston-propelled FBA (PFBA) was applied for automatic preparation of calibration solutions for manganese determination in mineral waters by electrothermal atomic-absorption spectrometry (ET AAS). Comparing the results obtained with two sets of calibration curves (five by manual and five by PFBA preparations), no significant statistical differences at a 95% confidence level were observed by applying the paired t-test. The standard deviation of manual and PFBA procedures were always smaller than 0.2 and 0.1 μg L⁻¹, respectively. By using PFBA it was possible to prepare about 80 calibration solutions per hour.     

Comparison of sample preparation methods for analysis of isoflavones in foodstuffs

Due to the lack of one universally applicable and commonly used reference method, sample preparation in isoflavone (IF) analysis has been performed by many different methods which renders comparison and quality assessment of published IF contents in foodstuffs difficult.In the present work, the impact of different experimental parameters on the IF concentrations determined in soybeans, tofu, soy drink and textured vegetable protein by different extraction and hydrolysis methods was assessed and IF contents obtained by optimized orthogonal methods were compared. Chromatographic analysis was performed by HPLC-UV-ESI-MS. If possible sources of error - which are also pointed out in this work - are avoided, IF contents obtained by extraction, acid-, base- and enzymatic hydrolysis are similar. However, these sample preparation methods differ in the amount of time, standard compounds and instruments required, ruggedness, and in their applicability to analysis of complex composite samples containing soy as minor ingredient. Enzymatic hydrolysis with Helix pomatia juice after extraction by sonication with first 50, then 80% aqueous acetonitrile in the presence of zinc sulfate heptahydrate and after adjustment to ≤10% organic solvent turned out to be the method of choice if only aglucone equivalent contents are required. The advantages of this method are short chromatographic run times, smallest danger of coelution, lowest achievable limits of quantitation and therefore best suitability for work-up of complex composite samples and that only aglucone standards are needed for quantitation.     

水产品中有害物质分析样品前处理技术研究进展

水产品含有丰富的蛋白、维生素和多种微量元素,是人们摄取动物性蛋白质的重要来源之一,我国是世界上最大的水产品消费国,其质量安全问题一直备受关注。但水产样品基质复杂,有害物质的含量低,须对其进行分离富集后才能进行检测,传统的液-液萃取、固相萃取和快速固相分散萃取等样品前处理技术在水产品分析中得到广泛应用,同时针对一些挥发性和超痕量有害物质检测时,固相微萃取同样体现出巨大优势。这些样品前处理技术可以有效去除基体对分析对象的干扰,提高检测方法的灵敏度和准确度。根据目标分析物性质的不同,选择合适的样品前处理技术,是水产品中有害物质分析的关键步骤。该文以水产品中有害物的来源不同,将其分为3类:(1)水产品中环境污染物的分析;(2)养殖运输和加工过程中有害物的分析;(3)水产品中生物毒素的分析。以这3类有害物质的分析为主线,综述了近10年水产品中有害物质分析的样品前处理技术,包括液-液萃取、固相萃取、固相微萃取、快速固相分散萃取和磁性固相萃取等。此外,还对各种技术的优缺点进行了探讨,并对其未来发展方向进行了展望。     

Trends in the sample preparation and analysis of nanomaterials as environmental contaminants

Much research on the use of nanomaterials in different applications is being conducted in areas such as water treatment, catalysis, oil processing, medicine, food, sensors, energy storage, building materials, constructions, and others. Nanoparticles are ultra-small particles with exceptional properties, but some nanoparticles and nanomaterials may exhibit harmful properties when leaked into the environment. Due to the lack of analytical methods for the detection and analysis of nanoparticles in complex matrices, not much is known about the potential risks associated with nanomaterials. Therefore, more knowledge is needed of the sampling and analysis of nanomaterials (NMs) as environmental contaminants. This review is undertaken to identify and assess key characteristics in potential sampling and analysis methods for identifying and quantifying the occurrence of NMs in numerous types of environmental media. To select suitable sampling and analysis methods, information on NM sources and transformation in environmental media is essential and thus is also discussed. This provides more information about the negative impacts of NMs on the environment. Challenges and future perspectives on the determination of NMs are also discussed.     

Feasibility study for the preparation of certified reference materials part I – mineral oil contaminated soils

The international joint project HYCREF (Contract No. G6RD-CT-2002-00854), funded by the European Commission in the 5th Framework programme, aimed to develop methods to prepare homogeneous and stable reference materials of water, soil, and waste contaminated with mineral oil hydrocarbons and to certify the mineral oil content by gas chromatographic methods. The results of a feasibility study for the preparation of three soil reference materials are discussed in this paper, and for the preparation of three waste reference materials in the second part (Koch et al., Accred Qual Assur submitted for publication). The soil materials were selected to represent different soil types and contamination levels. The project plan set three requirements for these reference materials: uncertainty in the mineral oil content resulting from the certification exercise <5%, a sample inhomogeneity of <3% and a minimum long-term stability of 5 years. For the most part, these requirements were met within this project.     

食用植物油中矿物油掺假的确证检测方法研究

应用气相色谱 质谱技术,建立了植物油中是否掺加矿物油的确证分析方法。本文报道的方法,简便、快速、准确、灵敏,方法最低检出浓度为1.2g L,经大量样品测定。     

用FTIR定量研究环氧树脂固化反应动力学制样方法的确定

利用FTIR进行环氧树脂固化反应的动力学研究需要精确的样品制备方法,摸索到一套合适的样品制备方法。将KBr研成细粉,通过孔径为0.074mm筛子使粒子均匀,在120~150℃下加热24h后,取0.25g,放入红外压片模具,在压力为800MPa条件下加压时间5~10min,压制成厚度为0.08mm的透明均匀KBr盐片。将环氧树脂均匀涂在这种KBr盐片上,放入微型反应器中反应,之后一同放入FTIR仪中进行扫描,实验证明这种制样方法可以保证红外定量分析的可靠性。     

Evaluation of sample preparation protocols for proteomic analysis of sunflower leaves

Six protocols for extraction of proteins from sunflower (Helianthus annuus L.) leaves were evaluated for their abilities in both removing interferents and attaining the best resolution in two-dimensional gel electrophoresis. “Classical” phenol extraction followed by precipitation with ammonium acetate in methanol displayed the most efficient protocol, which allowed the detection of 244 protein spots with ca. 485 μg of protein in gel electrophoresis. Tandem mass spectrometry was performed to identify proteins in 61 spots, and cross species identification was used for this task. Proteins from twenty two spots were identified, and 12 of these proteins are up to now not included into the ExPASy sunflower protein databank.     

Remarks on the sample preparation of oxidic materials for X-ray analysis

Summary The universal method which is established in practice and has the best reproducibility is indicated in a critical comparison of different techniques for producing melting fusion tablets for the X-ray analysis. By studying fusion tablets with methods of local analysis, users of the tablet technique shall be made critical. The different objectives of analytical problems with the analysis of oxides are discussed.

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Bemerkungen zur Probenvorbereitung oxidischer Materialien für die Röntgenfluorescenzanalyse

Zusammenfassung Ausgehend von einem kritischen Vergleich verschiedener Techniken zur Herstellung von Schmelzaufschluß-Tabletten für die RFA wird auf die in der Praxis bewährte Universalmethode mit der besten Reproduzierbarkeit hingewiesen. Durch die Untersuchung von Schmelztabletten mit Hilfe lokalanalytischer Methoden sollen Anwender der Tablettentechnik zur Kritik angeregt werden. Die unterschiedlichen Zielsetzungen analytischer Aufgaben bei der Untersuchung von Oxiden werden diskutiert.