灰铸铁石墨形态的自动分类

在所提取的纹理特征的基础上,使用误差后向传播神经网络构建了一种优化的人工神经网络人顺。实现了灰铸铁石墨态的自动分类。用于描述石墨形态特征由分形维,粗细参数和二维自回归系数共同组成。该法成功地将人工神经网络引入了对灰铸铁石墨形态的分类,相对于传统人工目测法是一种很大的进步,而神经网络分类器的优化方法对其它神经网络模型的构也具有一定参考价值。     

Automatic classification of graphite in cast iron.

A method for automatic classification of the shape of graphite particles in cast iron is proposed. In a typical supervised classification procedure, the standard charts from the ISO-945 standard are used as a training and validation population. Several shape and size parameters are described and used as discriminants. A new parameter, the average internal angle, is proposed and is shown to be relevant for accurate classification. The ideal parameter sets are determined, leading to validation success rates above 90%. The classifier is then applied to real cast iron samples and provides results that are consistent with visual examination. The method provides classification results per particle, different from the traditional per field chart comparison methods. The full procedure can run automatically without user interference.     

Direct identification of organic inclusions in graphite on the basis of field desorption mass spectrometry

A method for the direct identification of organic inclusions in graphite on the basis of field desorption mass spectrometry is proposed, based on the possibility of using a fractured graphite sample as a field emitter. Under such circumstances, the organic inclusions adsorbed on the surface of the microcrystallites of modified graphites may be directly field desorbed and identified by their mass spectra without any pretreatment of the sample. Two differently modified types of graphite were analysed by this method and the nature of the admixtures was established: one sample appeared to contain a mixture of polymethylsiloxanes and the other and blend of dyes. For the latter sample, temperature fractionation of admixed substances was performed and the presence of three individual dyes was established. Such features of field desorption as the production of abundant molecular ions with negligible fragmentation and the possibility of obtaining of mass thermograms greatly facilitate the identification of individual components of mixture inclusions.     

Structures and Properties of Cast Irons Reinforced by Trace Addition of Modified SiC Nanopowders

"To improve the performance of traditional cast iron, trance amount of surface modified nanometer SiC powders were added into the melted iron. The microstructures, the mechanical properties, as well as the wear resistance were investigated. The trace addition of SiC nano-powders were active due to the presence of structural defects arising from the treatment, they were eoient in affecting not only the generation and growth of crystals but also change the morphology of graphite. On the other hand, the addition of SiC nanopowders as heterogeneous seedings in the crystallization of liquid metals lead to the changing of supercooling temperature, so the ratio of ferrite and pearlite was changed. The mechanical characteristics and wear resistance were enhanced as a result of the improved graphite shape and changed matrix composition caused by the trace addition of SiC nanopowders (in amounts of about 0.01% mass). The strengthening mechanism and the free gap between powders were also discussed. It is suggested that the tensile strength, toughness, as well as the wear resistance can be improved simultaneously, which indicates the novel strengthening technology by trace addition of nanopowders is promising to extend to large-scale industrial production."     

自动石墨消解–电感耦合等离子体质谱法同时测定左氧氟沙星胶囊中7种金属元素

建立自动石墨消解-电感耦合等离子体质谱法(ICP-MS)同时测定左氧氟沙星胶囊中铅、铬、砷、镉、锡、铝、铁7种金属元素含量的方法。以HNO3-H2O2()体积比为1∶1为消解体系,采用自动石墨消解法消解左氧氟沙星胶囊样品,消解液除酸后,用5%硝酸溶液定容至50 mL,采用电感耦合等离子体质谱法对消解液进行测定,以内标法定量。铅、铬、砷、镉、锡、铝、铁的质量浓度在0.05~20.0μg/mL范围内与质谱响应值成良好的线性关系,相关系数均大于0.998,方法检出限为0.119~1.323μg/kg。样品加标回收率为91.2%~105.5%,测定结果的相对标准偏差为1.67%~3.46%(n=6)。该方法样品前处理简单,检出限低,测定结果准确,适用于左氧氟沙星胶囊等沙星类抗生素中多种金属元素残留的测定。     

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for spatially resolved trace analysis of early-medieval archaeological iron finds

The suitability of laser ablation ICP-MS for minor and trace analysis of archaeological iron finds, produced by a direct reduction process in a ‘bloomery’ furnace, is reported. The analysis of elemental impurities in the iron can provide useful archaeometallurgical information on the production process and the provenance of the iron. Since, even after refinement, the iron resulting from this process may contain many inclusions (slag, charcoal, holes, etc.), a method should be used with sufficient spatial resolution to preclude the inclusions from the analysis. The ablation parameters are selected such that ablation craters of approx. 100 μm in diameter are obtained. The method is validated with low alloy steel and cast iron standard reference materials and by a comparative analysis with electron probe microanalysis (EPMA). The precision is limited mainly by the homogeneity of the iron, rather than by instrumental reproducibility. The advantages and drawbacks of the method are briefly compared with EPMA. Preliminary results from the analysis of archaeological iron samples from excavations at Develier-Courtételle (Canton Jura, CH), Neftenbach (Canton Zurich, CH), Wartau (Canton St Gallen, CH) and Mont Chemin (Canton Valais, CH) are given.     

Laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) for spatially resolved trace analysis of early-medieval archaeological iron finds

The suitability of laser ablation ICP-MS for minor and trace analysis of archaeological iron finds, produced by a direct reduction process in a 'bloomery' furnace, is reported. The analysis of elemental impurities in the iron can provide useful archaeometallurgical information on the production process and the provenance of the iron. Since, even after refinement, the iron resulting from this process may contain many inclusions (slag, charcoal, holes, etc.), a method should be used with sufficient spatial resolution to preclude the inclusions from the analysis. The ablation parameters are selected such that ablation craters of approx. 100 microm in diameter are obtained. The method is validated with low alloy steel and cast iron standard reference materials and by a comparative analysis with electron probe microanalysis (EPMA). The precision is limited mainly by the homogeneity of the iron, rather than by instrumental reproducibility. The advantages and drawbacks of the method are briefly compared with EPMA. Preliminary results from the analysis of archaeological iron samples from excavations at Develier-Courtetelle (Canton Jura, CH), Neftenbach (Canton Zurich, CH), Wartau (Canton St Gallen, CH) and Mont Chemin (Canton Valais, CH) are given.     

稀土奥贝蠕铁制取工艺及其性能的研究

稀土奥贝蠕铁可用含稀土的蠕化剂及等温淬火工艺稳定地制取,藉助高温扫描电子显微镜,观察并研究了稀土蠕铁奥氏体化过程及稀土奥贝蠕铁随温度升高时组织的变化。用带有加热装置的万能材料试验等土奥贝蠕铁的各种性能进行了系统测定了如抗拉强度、延伸率、冲吉韧性、热膨胀系数及伸长百分率,结果表明,稀土奥贝蠕铁在室温和高温下均有良好的性能。     

Removal of graphite by oxidation with perchloric acid plus periodic acid Inapplicability to the spectrophotometric determination of manganese in steel

An attempt has been made to improve the Willard and Greathouse periodate method for the determination of manganese in high-carbon steel and cast iron by oxidizing the graphite with periodic acid in the presence of perchloric acid and phosphoric acid. Graphite is rapidly oxidized at 150 degrees by this mixture but manganese is lost by volatilization as the heptoxide and decomposition of the latter on hot surfaces to manganese dioxide. No way was found for either the quantitative removal and recovery of manganese by volatilization or for quantitative return to the main solution. The spectrophotometric determination of manganese in the supernatant liquid after allowing graphite to settle yields imprecise but not wholly unacceptable results; for the highest accuracy, graphite should be removed along with silica following dehydration of the latter with perchloric acid.     

Removal of graphite by oxidation with perchloric acid plus periodic acid: Inapplicability to the spectrophotometric determination of manganese in steel

An attempt has been made to improve the Willard and Greathouse periodate method for the determination of manganese in high-carbon steel and cast iron by oxidizing the graphite with periodic acid in the presence of perchloric acid and phosphoric acid. Graphite is rapidly oxidized at 150° by this mixture but manganese is lost by volatilization as the heptoxide and decomposition of the latter on hot surfaces to manganese dioxide. No way was found for either the quantitative removal and recovery of manganese by volatilization or for quantitative return to the main solution. The spectrophotometric determination of manganese in the supernatant liquid after allowing graphite to settle yields imprecise but not wholly unacceptable results; for the highest accuracy, graphite should be removed along with silica following dehydration of the latter with perchloric acid.     

Fabrication of a Novel Polymeric Scaffold for Amperometric Laccase Biosensor

Present work displays the preparation of an electrochemical biosensor using a conjugated polymer and laccase enzyme for catechol quantification in samples. The biosensing system is based on an enzyme immobilization on polymer modified graphite transducer surface. For that purpose, a random conjugated polymer, thienothiophene‐benzoxadiazole‐alt‐benzodithiophene (BOTT), was coated onto a graphite electrode surface via drop casting method followed by immobilization of a biomolecule (laccase) for sensing experiments. Herein, for the first time, we proposed a BOTT polymer as an inexpensive and effective way to fabricate highly sensitive and fast response biosensors. The proposed sensing system possessed superior properties with 0.38 μM limit of detection and 110.81 μA mM^?1 sensitivity. Furthermore, cyclic voltammetry and scanning electron microscopy techniques were used to examine the surface modifications. The proposed system could be useful for many future studies for catechol quantification in environmental samples.© 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 2333–2339     

稀土变质及热处理对耐磨铸铁冲击疲劳性能的影响

采用金相显微镜、扫描电镜观察了经冲击疲劳试验后耐磨铸铁中碳化物的形貌、疲劳裂纹的萌生与扩展,测定了稀土含量及加热温度与裂纹的长度和裂纹扩展之间的关系曲线,在此基础上探讨了稀土变质及热处理对耐磨铸铁冲击疲劳性能的影响.结果表明: 稀土能推迟裂纹萌生的时间,降低裂纹扩展速率,提高其冲击疲劳抗力.当稀土与热处理共同作用时,效果更显著.其原因主要归于网状共晶碳化物形态与分布的改变.     

稀土—氮复合孕育剂对灰铸铁石墨组织的影响

采用主碳当量灰铸铁作为试验材料，以孕育处理的方式加入稀土和氮，研究了稀土，氮及二者复合能对石墨数量和石墨表面形貌的影响。试验结果表明，稀土和氮，特别是它们复合加入，使石墨百分含量减少；氮和氮与稀土复合孕育使灰铸铁的石墨表面变粗糙，且端部有钝化现象。     

一种模式分类降维策略及其在复杂化学信息处理中的应用

采用分类相关分析方法处理复杂化学信息的模式分类问题。从高维模式中提取的分类相关成分,它们相互独立,并集中了原有模式的分类信息。提出由相关量份额选择分类相关成分,计算简便,用以替代原模式,可以显著地降维,使问题简化,分类效果良好。该方法应用于天然留兰香油多类判别,结果良好。     

Determination of fluoxetine enantiomers in pharmaceutical formulations by electrokinetic chromatography–counter current technique

In this work, an electrokinetic chromatography–counter current procedure for the separation of fluoxetine enantiomers using highly sulfated β‐cyclodextrin was optimized and applied to the determination of the enantiomers in three pharmaceutical formulations according to the matrix features. Quality criteria were applied to facilitate its transferability to testing laboratories. Fluoxetine was used therapeutically as the racemate, although a stereospecificity associated with its interactions with the neuronal serotonin‐uptake carrier was demonstrated. In this context, the development of enantioselective methods for the chiral analysis of pharmaceuticals allowing stereoisomer ratio estimations has increasing interest in pharmaceutical industry. The proposed method allows the quantification of both enantiomers in less than 2 min with high resolution (R_s = 2.4). Copyright © 2012 John Wiley & Sons, Ltd.     

Validation of a Simple HPLC-Based Method for Lysine Quantification for Ruminant Nutrition

Robust and selective quantification methods are required to better analyze feed supplementation effectiveness with specific amino acids. In this work, a reversed-phase high-performance liquid chromatography method with fluorescence detection is proposed and validated for lysine quantification, one of the most limiting amino acids in ruminant nutrition and essential towards milk production. To assess and widen method applicability, different matrices were considered: namely Li₂CO₃ buffer (the chosen standard reaction buffer), phosphate buffer solution (to mimic media in cellular studies), and rumen inoculum. The method was validated for all three matrices and found to be selective, accurate (92% ± 2%), and precise at both the inter- and intra-day levels in concentrations up to 225 µM, with detection and quantification limits lower than 1.24 and 4.14 µM, respectively. Sample stability was evaluated when stored at room temperature, 4 °C, and −20 °C, showing consistency for up to 48 h regardless of the matrix. Finally, the developed method was applied in the quantification of lysine on real samples. The results presented indicate that the proposed method can be applied towards free lysine quantification in ruminant feeding studies and potentially be of great benefit to dairy cow nutrition supplementation and optimization.     

Acylation d'aromatiques sous irradiation micro-onde en présence de graphite

Acylation of aromatics under microwaves in the presence of graphite. Under microwave irradiation, acylations of aromatic compounds could be achieved in the presence of graphite powder, used either to support the reagents (dry medium), or in small amount (solid-liquid medium). The process takes advantage both of the interaction of the graphite with the electromagnetic field and with the organic compounds. Acylations were achieved in an open reactor and at temperatures notably higher than the boiling point of the reagents. A catalytic effect of metallic inclusions present on the graphite surface, in particular iron ones (magnetite), has been established.     

Automatic identification of novel bacteria using Raman spectroscopy and Gaussian processes

Raman spectroscopy is successfully used for the reliable classification of complex biological samples. Much effort concentrates on the accurate prediction of known categories for highly relevant tasks in a wide area of applications such as cancer detection and bacteria recognition. However, the resulting recognition systems cannot always be directly used in practice since unseen samples might not belong to classes present in the training set. Our work aims to tackle this problem of novelty detection using a recently proposed approach based on Gaussian processes. By learning novelty scores for a large bacteria Raman dataset comprising 50 different strains, we analyze the behavior of this method on an independent dataset which includes known as well as unknown categories. Our experiment reveals that non-parametric methods such as Gaussian processes can be successfully applied to the task of finding unknown bacterial strains, leading to encouraging results motivating their further utilization in this area.     

Solid phase extraction and HPLC determination of veterinary pharmaceuticals in wastewater

This work focuses on the application of SPE-HPLC analysis of important veterinary pharmaceuticals from different classes in highly complex wastewater matrix. The pharmaceutical investigated included three sulfonamides (sulfamethazine, sulfadiazine and sulfaguanidine), a sulfonamide synergist (trimethoprim), a tetracycline (oxytetracycline), a fluoroquinolone (enrofloxacine) and a β-lactame (penicillin G/procaine). The method involves pre-concentration and clean-up by solid phase extraction (SPE) using Oasis HLB extraction catridges. Final analysis of the selected pharmaceutical compounds was carried out by high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD). Recoveries were ranged from 68.3 to 97.9% with relative standard deviation below 8.4%. Only for sulfaguanidine low recovery was obtained. Limits of quantification were in the range 1.5-100 μg/L depending on pharmaceutical. The described method was applied to the determination of pharmaceuticals in wastewater samples from pharmaceutical industry.     

Low-Cost Detection of Methane Gas in Rice Cultivation by Gas Chromatography-Flame Ionization Detector Based on Manual Injection and Split Pattern

Rice cultivation is one of the most significant human-created sources of methane gas. How to accurately measure the methane concentration produced by rice cultivation has become a major problem. The price of the automatic gas sampler used as a national standard for methane detection (HJ 38-2017) is higher than that of gas chromatography, which greatly increases the difficulty of methane detection in the laboratory. This study established a novel methane detection method based on manual injection and split pattern by changing the parameters of the national standard method without adding any additional automatic gas samplers. The standard curve and correlation coefficient obtained from the parallel determination of methane standard gas were y = 2.4192x + 0.1294 and 0.9998, respectively. Relative standard deviation (RSD, <2.82%), recycle rate (99.67–102.02%), limit of detection (LOD, 0.0567 ppm) and limit of quantification (LOQ, 0.189 ppm) of this manual injection method are satisfying, demonstrating that a gas chromatography-flame ionization detector (GC-FID), based on manual injection at a split ratio (SR) of 5:1, could be an effective and accurate method for methane detection. Methane gases produced by three kinds of low-methane rice treated with oxantel pamoate acid, fumaric acid and alcohol, were also collected and detected using the proposed manual injection approach Good peak shapes were obtained, indicating that this approach could also be used for quantification of methane concentration.