A Versatile Method for Uniform Dispersion of Nanocarbons in Metal Matrix Based on Electrostatic Interactions

Realizing the uniform dispersion of nanocarbons such as carbon nanotube and graphene in metals, is an essential prerequisite to fully exhibit their enhancement effect in mechanical, thermal, and electrical properties of metal matrix composites(MMCs). In this work, we propose an effective method to achieve uniform distribution of nanocarbons in various metal flakes through a slurry-based method. It relies on the electrostatic interactions between the negatively charged nanocarbons and the positively charged metal flakes when mixed in slurry. For case study, flake metal powders(Al, Mg, Ti,Fe, and Cu) were positively charged in aqueous suspension by spontaneous ionization or cationic surface modification. While nanocarbons, given examples as carboxylic multi-walled carbon nanotubes, pristine single-walled carbon nanotube, and carbon nanotube–graphene oxide hybrid were negatively charged by the ionization of oxygen-containing functional groups or anionic surfactant. It was found that through the electrostatic interaction mechanism, all kinds of nanocarbons can be spontaneously and efficiently adsorbed onto the surface of various metal flakes. The development of such a versatile method would provide us great opportunities to fabricate advanced MMCs with appealing properties.

Matrix Solid-phase Dispersion Extraction of Alkaloids from the Roots of Aconitum kusnezoffii Reichb

Matrix solid-phase dispersion（MSPD） was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid support material, type of the elution solvent and the volume of the elution solvent were tested. Mean recoveries ranged from 93.16% to 102.73%, with relative standard deviations from 0.27% to 4.17%. With the extraction efficiency and time expenditure taken into account, MSPD extraction should be a comparatively good method.

Determination of Tebuconazole Residue in Apples and Vegetables by Matrix Solid Phase Dispersion-Gas Chromatography

[ Objective] The study aimed to determine tebuconazole residue in apples and vegetables using matrix solid phase dispersion-gas chro- matography （MSPD-GC）. [ Method] The effects of extraction and determination conditions on the detection of tebuconazole left in apples and veg- etables were analyzed, and the optimum extraction conditions were determined. [ Result] The recovery rate of tebucenazole was the highest when the ratio of a sample to florisil dispersant was 1 ： 4, and the mixture of hexane and acetone （ 1 ： 1 ） with total volume of 8 ml was as the eluant. Under the optimum conditions, the relative standard deviation （RSD） of the method was 4.9% -7.6%, and the detection limit was 0.1 tJg/g, while the re- covery rate of tebuconazole changed from 86.7% to 95. 2% . [ Conclusion] The method was simple, accurate, sensitive and applicable to the de- termination of tebuconazole in aaricultural Droducts.

Determination of seven active components in Salvia miltiorrhiza herb by matrix solid phase dispersion combined with ion liquid extraction followed by high performance liquid chromatography

A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet detection(UV)is proposed,and it was applied to determine the seven active compounds in Salvia Miltiorrhiza herb.SGSIL and ionic liquid[BMIM]BF4 were used as the adsorbent and the green elution reagent in the MSPD procedure.Several extraction conditions including type of filler and elution solvent,the volume of elution solvent,material liquid ratio were optimized.Under the optimum conditions,the SGSIL-MSPD-HPLC method showed a low limit of detection(LOD,S/N=3)of 0.0122-0.8788μg/mL for standard solution,limit of quantification(LOQ,S/N=10)of 0.0406-2.9292μg/mL for standard solution,wide linear range from 1.56 to 2000μg/mL for all compounds for standard solution,correlation coefficients(r)of more than 0.9990,acceptable reproducibility(relative standard deviations,RSDs<3.54%),and precision of RSDs<3.36%for intra-day,RSDs<3.50%for inter-day.The satisfactory recoveries ranged from 96.4 to 102.5,with RSDs less than 3.45%.The developed SGSIL-MSPD method is easier and more suitable for the determination of the seven active compounds in Salvia Miltiorrhiza herb than the traditional ultrasonic extraction.It was an effective and efficient method for the extraction and quantification of the seven active compounds in traditional Chinese herbal samples.

MSPD-ASE-GC法测定土壤中石油烃(C_(10)-C_(40))

通过优化仪器分析方法和样品前处理条件,建立基质固相分散(MSPD)-加速溶剂萃取(ASE)-气相色谱法(FID检测器)测定土壤中石油烃(C_(10)-C_(40))的分析方法。称取10.0 g冻干处理后的土壤样品与2.0 g硅藻土和5.0 g硅酸镁吸附剂分散均匀,以正己烷为提取剂,经加速溶剂萃取、无水硫酸钠脱水、氮吹浓缩定容至1.0 mL,气相色谱测定,外标法定量。石油烃(C_(10)-C_(40))在0~9300 mg/L浓度范围内线性良好,相关系数可达0.9999,方法检出限为3 mg/kg,对空白石英砂和实际土壤样品进行加标测定,平行分析(n=6)的相对标准偏差在15.0%以内,加标回收率为81.2%~96.0%。该方法实现了土壤样品的同步提取和净化,简化了样品的前处理步骤,提高了样品分析效率,精密度良好、准确度高,可以满足土壤中石油烃(C_(10)-C_(40))测定的要求。

Influence of nano-Al_2O_3-reinforced oxide-dispersion-strengthened Cu on the mechanical and tribological properties of Cu-based composites

The mechanical and tribological properties of Cu-based powder metallurgy （P/M） friction composites containing 10wt%-50wt% oxide-dispersion-strengthened （ODS） Cu reinforced with nano-Al2O3 were investigated. Additionally, the friction and wear behaviors as well as the wear mechanism of the Cu-based composites were characterized by scanning electron microscopy （SEM） in conjunction with energy-dispersive X-ray spectroscopy （EDS） elemental mapping. The results indicated that the Cu-based friction composite containing 30wt% ODS Cu exhibited the highest hardness and shear strength. The average and instantaneous friction coefficient curves of this sample, when operated in a high-speed train at a speed of 300 km/h, were similar to those of a commercial disc brake pad produced by Knorr-Bremse AG （Germany）. Additionally, the lowest linear wear loss of the obtained samples was （0.008 ± 0.001） mm per time per face, which is much lower than that of the Knorr-Bremse pad （（0.01 ± 0.001） mm）. The excellent performance of the developed pad is a consequence of the formation of a dense oxide composite layer and its close combination with the pad body.

High temperature tensile,compression and creep behavior of recycled short carbon fibre reinforced AZ91 magnesium alloy fabricated by a high shearing dispersion technique

The present study seeks the feasibility of using short carbon fibres recycled from polymer matrix composites as alternative to virgin carbon fibres in the reinforcement of magnesium alloys.The microstructures,high temperature mechanical and creep properties of AZ91 alloy and its composites with various recycled carbon fibre contents(2.5 and 5 wt.%)and lengths(100 and 500μm)were investigated in the temperature range of 25-200℃.The microstructural characterization showed that the high shear dispersion technique provided the cast composites with finer grains and relatively homogenous distribution of fibres.The materials tested displayed different behaviour depending on the type of loading.In general,while enhancements in the mechanical properties of composites is attributed to the load bearing and grain refinement effects of fibres,the fluctuations in the properties were discussed on the basis of porosity formation,relatively high reinforcement content leading to fibre clustering and interlayer found between the matrix and reinforcement compared to those of AZ91 alloy.The compressive creep tests revealed similar or higher minimum creep rates in the recycled carbon fibre reinforced AZ91 in comparison to the unreinforced AZ91.

PDRK:A General Kinetic Dispersion Relation Solver for Magnetized Plasma

A general,fast,and effective approach is developed for numerical calculation of kinetic plasma linear dispersion relations.The plasma dispersion function is approximated by J-pole expansion.Subsequently,the dispersion relation is transformed to a standard matrix eigenvalue problem of an equivalent linear system.Numerical solutions for the least damped or fastest growing modes using an 8-pole expansion are generally accurate;more strongly damped modes are less accurate,but are less likely to be of physical interest.In contrast to conventional approaches,such as Newton＇s iterative method,this approach can give either all the solutions in the system or a few solutions around the initial guess.It is also free from convergence problems.The approach is demonstrated for electrostatic dispersion equations with one-dimensional and twodimensional wavevectors,and for electromagnetic kinetic magnetized plasma dispersion relation for bi-Maxwellian distribution with relative parallel velocity flows between species.

Physical dispersion state and fluorescent property of Eu-complex in the Eu-complex/silicon rubber composites

The fluorescent complex Eu（TTA）2（Phen）（MA） （HTTA=2-Thenoyltrifluoroacetone, Phen=1,10-phenanthroline, MA=Maleic an- hydrider） was synthesized and characterized with elemental analysis, infrared spectrum （IR）, scanning electron microscope （SEM）, X-ray Diffraction（XRD）, differential scanning calorimetry（DSC）, and fluorescent measurement. To explore the effect of different physical dispersion state of Eu-complex on the fluorescent property of the Eu-complex/silicon rubber composites, various quantifies of Eu（TTA）2（phen） （MA） were mixed with silicon rubber （SIR） and peroxide to form uncured composites. These composites were vulcanized to obtain cured Eu-complex/SiR composites at 250 ℃, which was higher than the melting-point of Eu-complex. The SEM, XRD, DSC, and the fluorescent measurement of these composites showed that both the complex molecules dispersed in the silicon rubber during the melting process and the parent Eu-complex particles had positive effects on fluorescent property, whereas the re-crystallized Eu-complex particles and the aggregating complexes formed during the melting-process had negative effects on fluorescent property. For the uncured composites, their fluorescent intensities almost did not change with the increasing amount of Eu-complex. Furthermore, for the composites with small content of Eu-complex, their fluorescent intensities decreased significantly after curing, and this difference in fluorescent intensity became smaller as the content of Eu-complex increases.

Formation of composites fabricated by exothermic dispersion reaction in Al-TiO_2-B_2O_3 system

The formation of aluminum matrix composites fabricated by exothermic dispersion reaction in Al-TiO2-B2O3 system was investigated. The thermal analysis results show that the reactions are spontaneous and exothermic. The Gibbs free energy of α-Al2O3 is the lowest among all the combustion products, followed by TiB2 and Al3Ti. It is noted that when the B2O3/TiO2 mole ratio is below 1, the reaction products are composed of particle-like α-Al2O3, TiB2 and rod-like Al3Ti. The α-Al2O3 crystallites, resulting from the reaction between Al and TiO2 or B2O3, are segregated at the grain boundaries due to a lower wettability with the matrix. SEM micrographs show that rod-like Al3Ti phase distributes uniformly in the matrix. When the B2O3/TiO2 mole ratio is around 1, the Al3Ti phase almost disappears in the composites, and the distribution of α-Al2O3 particulates is improved evidently.

A New Approach for Dispersion Parameters

This paper presents a new approach to identify and estimate the dispersion parameters for bivariate, trivariate and multivariate correlated binary data, not only with scalar value but also with matrix values. For this direction, we present some recent studies indicating the impact of over-dispersion on the univariate data analysis and comparing a new approach with these studies. Following the property of McCullagh and Nelder [1] for identifying dispersion parameter in univariate case, we extended this property to analyze the correlated binary data in higher cases. Finally, we used these estimates to modify the correlated binary data, to decrease its over-dispersion, using the Hunua Ranges data as an ecology problem.

基于响应面法的基质固相分散萃取土壤中有机磷阻燃剂

有机磷阻燃剂(OPFRs)被广泛添加于商业品和日用品中,由于具有环境持久性、生物富集性和潜在毒性,已成为一种新兴的持久性有机污染物。因此需要建立能准确定量环境中OPFRs的检测方法。该文基于基质固相分散萃取(MSPD),结合气相色谱-串联质谱(GC-MS/MS)法测定土壤中10种有机磷阻燃剂,筛选对OPFRs具有高选择性的吸附剂,最终确定MSPD最佳萃取条件。该文基于单因素分析法考察了常见吸附剂(C18、PSA、Florisil、石墨化炭黑(GCB)和多壁碳纳米管(MWCNT))及其用量、洗脱溶剂及其体积、研磨时间对OPFRs萃取效率的影响。在此结果基础上,进一步利用响应面法(RSM)考察了3个关键因素(吸附剂用量、洗脱剂用量和研磨时间)以及交互作用对OPFRs萃取效率的影响。最终确定最优条件:吸附剂GCB,用量0.3 g;洗脱溶剂乙酸乙酯,用量10 mL;研磨时间5 min,此时10种OPFR的萃取效率为87.5%。在GC-MS/MS的多反应监测模式(MRM)下,以13C-PCB208为内标物进行定量。10种OPFRs在6个浓度梯度下,获得较好的线性,相关系数大于0.998。该方法的LOD和LOQ分别为0.006~0.161 ng/g和0.020~0.531 ng/g。在最佳条件下,加标土壤中OPFRs的加标回收率为70.4%~115.4%,相对标准偏差(RSD)为0.7%~6.7%。将该方法用于苏州不同功能土壤中OPFRs的含量测定,结果表明电子厂和汽修厂土壤中OPFRs总含量显著高于稻田土和校园土,电子厂和汽修厂土壤中主要污染物为磷酸三(2-氯异丙基)酯(TCIPP)、三苯基氧化膦(TPPO)、磷酸三(2-氯乙基)酯(TCEP)和磷酸三(1,3-二氯-2-丙基)酯(TDCPP),它们在电子厂土壤中含量分别为5.30、4.44、4.54、4.20 ng/g,在汽修厂土壤中的含量分别2.70、3.93、7.60、5.04 ng/g。目前关于TPPO的土壤污染报道较少,该研究在苏州工业区土壤中检出了高浓度TPPO污染。该方法成功用于土壤中10种OPFRs的检测。

水下抗分散水泥土正交试验及配比优化方法研究

水流经过桩基时会形成漩涡侵蚀床面,影响桩基及上部结构的稳定性,冲刷治理是工程界关注的热点问题。为促进固化土技术在桩基冲刷修复中的应用,设计开展了抗分散水泥固化土系列正交试验。针对高岭土和淤泥土,选用PAM、EVA、黄原胶、HPMC四种抗分散剂,采用平均效果分析和极差分析,研究了抗分散剂种类、抗分散剂掺量、含水量和水泥掺量对流动度、浊度、7 d和28 d无侧限抗压强度的影响。结果表明:对于高岭土,抗分散剂掺量从0.25‰增大到1‰,水泥土流动度减小20%,浊度减小25%,抗分散剂掺量对流动性和抗分散性的影响显著。对于淤泥土,对抗分散性影响显著的仍是抗分散剂掺量,而对流动性的影响显著的则是含水量,含水量从1.4倍液限增大到2.0倍液限,水泥土流动度增大45%。基于综合平衡法、矩阵分析法和多元线性回归模型,提出了一种抗分散水泥土配比设计方法,研究得到了高岭土和淤泥土抗分散水泥固化土的推荐配比,其在泥沙起动实验中的抗冲刷特性明显优于原始土样。

基于多元精细复合多尺度波动散布熵和累积欧氏距离矩阵测度的风电机组变桨轴承退化状态评估

针对风电机组变桨轴承服役过程环境噪声干扰严重、退化状态评估精度低的问题,提出一种基于多元精细复合多尺度波动散布熵和累积欧氏距离矩阵测度的退化状态评估模型。该模型将监测数据状态特征获取过程由单通道拓展为多通道进行,通过提出的多元精细复合多尺度波动散布熵算法来获取多通道监测数据的多尺度状态特征,并将累积和检验算法与欧氏距离矩阵测度方法相结合,用于定量衡量基准样本与待分析样本间的差异,从而实现变桨轴承退化状态评估。风电机组变桨轴承全寿命周期加速疲劳实验验证结果表明:该模型能够及时捕捉到变桨轴承的初始退化时刻并且准确跟踪整个退化过程。

牛奶中四环素类药物多残留分析方法研究——MSPD-HPLC-UV

本文建立了牛奶中四环素类药物的MSPD -HPLC -UV分析法。将C18、EDTA—Na2 、草酸和样品研磨混合 ,制成半固态装柱、淋洗、反相HPLC测定。在 0 10～ 0 5 0 μg/ml添加浓度范围内 ,4种四环素类药物的平均回收率为 78 7%～ 90 2 % ,变异系数在 2 4%～ 18 8%之间 ,方法检测限为 0 0 2 μg/ml～ 0 0 5 μg/ml。

MSPD-GPC净化GC-ECD法测定辣椒酱中8种有机氯农药残留分析

建立辣椒酱样品中8种有机氯农药多残留的基质固相分散法-凝胶渗透色谱净化-气相色谱-电子捕获检测器分析方法.辣椒酱样品首先经基质固相分散法除去大部分油脂和色素等大分子干扰基质后,再通过凝胶渗透色谱进一步净化,应用气相色谱-电子捕获检测器进行检测.结果表明：测定辣椒酱中8种有机氯农药的标准曲线相关系数为0.999 1～0.999 6,加标回收率均在74.58％～102.86％之间,日内相对标准偏差均小于5.45％（n=5）,方法检出限为0.40～1.20 μg/kg.该方法具有检出限低、灵敏度高、快速、准确的特点,可适用于辣椒食品中多种有机氯农药残留同时检测.

猪肌肉组织中磺胺类药物的MSPD净化和HPLC测定

本文以基质固相分散（ＭＳＰＤ） 和高效液相色谱为基础，建立了猪肌肉组织中磺胺类药物多残留快速分析法。将０５ｇ 肌肉组织与适量Ｃ１８ 填料混合，研磨，制成半固态装柱，磺胺类药物经二氯甲烷洗脱后直接用反相高效液相色谱测定（ＵＶ２７０ｎｍ） 。在０１ ～０５ｍｇ／ｋｇ 添加浓度范围内７种磺胺类药物的平均回收率为７０６ ％ ±２０３ ％ 。检测限为００１ ～０１ｍｇ／ｋｇ。

不确定转子系统动力学降阶模型构建与模型散度参数辨识

在航空、航天、船舶等领域的实际工程转子系统中,广泛存在高维复杂的非线性系统。在航空发动机转子系统、燃气轮机转子系统等重点研究领域,通常还难以对高维复杂非线性系统进行直接的数据处理和分析统计。针对不确定性转子系统的模型维度较高等问题,提出了一种模型不确定性动力学降阶计算模型构建和模型散度参数辨识方法。首先,根据确定性动力学模型和静态矩阵降阶方法,完善了确定性动力学降阶模型;然后,基于随机矩阵理论和非参数动力学建模方法,提出了不确定性动力学降阶模型;最后,利用系统确定性模型的一阶临界转速、振型和实验数据,对不确定性动力学模型的散度参数进行了辨识;为了验证散度参数辨识方法的有效性,笔者又在转子实验平台上进行了实验验证。研究结果表明:实验结果与降阶之后振动响应均值的差异性较小,且与不确定性动力学模型相差不超过10%,表明所采用的理论模型在描述转子系统行为方面具备了较高的准确性和可靠性,该模型可以为深入研究模型不确定性转子系统提供参考。

MSPD-GC-MS同时测定酱油及调味液中多组分氯丙醇

目的:建立一种快速测定酱油及调味液中多组分氯丙醇的GC-MS测定方法。方法:在样品中加入两种稳定性氘代同位素内标后,样品经过基质固相分散萃取(MSPD)提取与净化,用全扫描定性,选择离子(SIM)定量。结果:各个氯丙醇在进样量在20～400 pg范围内线性良好(r>0.999),3-氯-1,2-丙二醇(3-MCPD)、1,3-二氯丙醇(1,3-DCP)和2,3-二氯丙醇(2,3-DCP)的定量限分别为0.003、0.005和0.005 mg/kg;2种浓度水平下加标重复测定6次,回收率为95%～120%,精密度<10%。结论:方法具有较高的灵敏度、准确度、精密度和特异性,满足了样品中痕量氯丙醇的分析要求。