NMR法测定重油中碳、氢的质量百分含量

用高分辨的1H-NMR和13C-NMR法对重油中的氢、碳的质量百分含量进行测定.采用标准化合物考察了本方法的准确性,以实际油样考察了方法的重复性,则本方法具有良好的准确性、重复性.然后测定了30个重油油样的氢、碳的质量百分含量,测定结果与元素分析法(ASTM D5291)有很好的一致性.核磁共振法可以用于测定重油中碳、氢含量.     

EDXRF测定土壤元素含量及其在有机碳垂直分布特征研究中的应用

针对X射线荧光光谱(XRF)法不确定度计算和测定地质样品中硫的准确度、精密度与可靠性不高的难点,研究了提高土壤中硫分析准确度的途径,建立了土壤中S的XRF分析方法,完善了偏振能量色散XRF测定土壤中主、次、痕量元素的方法,利用不确定度评价、证实了所见方法的有效性和可靠性。测定、获得了研究区土壤元素剖面,通过对短期植被更替土壤剖面的土壤有机碳含量(TOC)、有机碳稳定碳同位素((13C)特征及其与元素垂直分布的关系研究,发现土壤中元素含量与有机碳含量和有机碳稳定碳同位素存在显著相关性。     

红外碳硫分析仪分析生铁、矿石和焦炭中碳和硫

建立了红外碳硫仪分析生铁、矿石、焦炭中的碳和硫的测定方法 ,该法可用于样品中碳和硫测定 ,结果令人满意     

地球化学样品中有机碳的光谱分析

有机碳已成为多目标地球化学调查、土地质量地球化学调查等项目研究的必测指标,对有机碳的准确定量是地球化学调查工作的重要内容,准确测定有机碳含量具有重要意义。然而传统的重量法、容量法流程长、速度慢,已经不能满足大批量及快速测定地球化学样品的要求。采用稀盐酸去除样品中的无机碳,应用高频红外碳硫分析仪对不同类型地球化学样品中有机碳的测定进行了研究,着重从称样量、酸的选择、最佳浓度及用量、助熔剂的选择和最佳加入量进行对比实验,优化出适合分析地球化学样品中有机碳含量的条件,并采用国家一级地球化学标准物质建立校准曲线,建立盐酸预处理-红外吸收光谱法测定地球化学样品中有机碳含量的分析方法。结果表明：陶瓷坩埚经1 200 ℃灼烧处理可以有效降低碳空白,减小对分析结果的影响;选择50.0～70.0 mg称样量,测试准确度高且样品熔融时不易喷溅;0.40～0.60 mL稀盐酸（1+7）除尽样品中的无机碳同时减少有机碳流失损失;0.40～0.50 g纯铁屑和1.50～1.70 g钨粒作为助熔剂,助熔效果稳定;采用国家一级地球化学标准物质建立校准曲线,校准曲线线性良好（R2=0.998 5）。该方法的检出限为69 μg·g-1,测定结果的相对标准偏差（RSD,n=12）均小于8%。经63个不同类型国家一级地球化学标准物质（土壤、岩石、水系沉积物）验证,测定结果与标准值相符。本方法操作简便,检出限低,灵敏度高,结果准确可靠,适用于地球化学样品中有机碳含量的测定。     

高频-红外吸收光谱法测定煤中全硫

介绍了用 ELTRA CS- 80 0红外碳硫分析仪测定煤中硫的方法 ,确定了最佳分析条件 ,例如助熔剂、称样量等条件。本法操作简单、分析时间短 ,测定结果令人满意。     

预烧－碱熔－分光光度法测定中碳石墨中二氧化硅

本文研究了预烧－碱熔－光度法测定中碳石墨中二氧化硅的条件，确定了高温灼烧排除主体成份碳的时间，在草－硫混酸介质中，用硫酸亚铁铵还原硅钼黄，波长８１０ｎｍ处，二氧化硅含量在０．０１－０．３２ｍｇ／１００ｍＬ范围内呈良好线性，用于测定中碳石墨中二氧化硅含量，结果满意。     

X射线荧光光谱研究粮食中生命有机碳与碳化学循环

采用X射线荧光光谱(XRF)方法测定六种粮食:稻谷(大米)、小麦(面粉)、黄豆、小米、高粱和玉米中生命有机碳含量和化学元素组成,建立一种新方法测定它们的蛋白质含量.粮食中生命有机碳平均含量约为44%.黄豆中的蛋白质含量最高(42.74%),小米蛋白质含量28.56%,麦子蛋白质含量27.57%,玉米蛋白质含量24.99...     

端视ICP-AES法测定水中的有机碳

本文建立了利用端视ＩＣＰ－ＡＥＳ技术测定水中有机碳的方法。本法检出限为０．６ｍｇ／Ｌ,灵敏度比国外同类方法提高了大约八倍,方法精密度好,其相对标准偏差０．４％￣３．２％（ｎ＝６）,回收率在８３．６％￣１０９．０％之间,本法前处理简单,测定速度快,灵敏度高,适合天然水中有机碳的测定。     

结晶紫内酯开环机理的13C NMR研究

报道了结晶紫内酯开环机理研究。通过测定开环前后及平衡混合物的¹³C NMR谱,对结晶紫内酯开环形成的正碳离子结构及影响正碳离子稳定性因素进行了分析。利用开环前后及平衡体系的化学位移数据求得了平衡混合物中内酯态和正碳离子之间的平衡常数.对不同条件下结晶紫内酯开、闭环机制进行了讨论。     

用迈克耳孙干涉仪测量杨氏模量

提出用迈克耳孙干涉仪测金属杨氏模量的新方法,并从实验上测定了碳钢丝的杨氏模量。     

ICP-AES法测定钛合金中的6种元素

用ＨＣｌ分解钛合金样品,直接用ＩＣＰ－ＡＥＳ法测定其中的Ｃｒ、Ｍｏ、Ｆｅ、Ｓｉ、Ａｌ及Ｚｒ６种元素,方法简便、快速、测定各元素含量范围为０．２８％－６．５１％,相对标准偏差为０．７２％－５．０７％,回收率为９７．４％－１０２％。     

Formation of titanium carbide coating with micro-porous structure

Micro-porous titanium carbide coating was successfully synthesized in a vacuum gas carburizing furnace by using a sequential diffusion technology. The composition and structure of the as-synthesized TiC were examined by X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and glow discharge mass spectrometry (GDMS), and scanning electron microscopy (SEM). All of the XRD, XPS and GDMS analysis results indicate that carbon atoms effectively diffused into the titanium alloys and formed a uniform acicular TiC coating with micro-porous structure.     

Structure–property correlation of a boron and carbon modified as cast β titanium alloy

Beta titanium alloys, Ti-15V-3Cr-3Al-3Sn, with minor additions of boron and carbon were prepared by consumable vacuum arc melting. Detailed microstructural characterizations were carried out using optical, scanning electron microscopes and transmission electron microscopes. Addition of boron resulted in refinement of the as cast beta grain while carbon addition resulted in the precipitation of extremely fine α phase during ageing. Formation of boride and carbide particles due to addition of boron and carbon, respectively, and refinement of the aged microstructure increased the hardness and strength as compared to the base alloy but reduced elongation to failure considerably, especially in the carbon-containing alloy where no measurable plasticity was observed. Fracture toughness values, however, were comparable for the boron- and carbon-containing alloys but these were lower than that of the base alloy.     

Investigation of the influence of the conditions during recrystallization annealing on the plasticity of molybdenum-base alloys with low concentrations of additives

An investigation was made of the conditions during recrystallization annealing on the plasticity and the nature of fracture of Mo-base alloys containing zirconium or titanium (TSM-4, TsM-6, Mo-Ti-C) and alloys free of active oxide-forming elements (TSM-3). Annealing at T > T_recr took place under traditional conditions employed in heat treatments (in 10^–4–10^–6 torr vacuum, in hydrogen-filled furnaces) or under conditions ensuring minimal saturation of the alloys with oxygen during heat treatments (this involved preliminary outgassing vacuum furnaces and wrapping of the samples in molybdenum foil) or under conditions of controlled partial oxygen pressure (in the presence of the Al₂O₃ powder in the annealing zone). The degree of saturation of the alloys with oxygen was deduced from the appearance of zirconium or titanium oxide in the surface layers of the alloys containing these elements. The results indicated that the conditions during heat treatment and alloying of molybdenum with zirconium and titanium had an important influence on the plasticity and fracture of the Mo-base alloys. The results obtained were analyzed on the basis of the ideas on intergranular brittleness in bcc materials because of segregation of oxygen at grain boundaries and a refining influence of zirconium and titanium on the Mo alloys saturated with oxygen, involving binding of the oxygen in oxides and thus preventing its segregation at grain boundaries.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 8, pp. 93–99, August, 1980.     

Microstructure effect on microtopography of chemically etched α + β Ti alloys

Microstructure effect on chemical etching behavior of the annealed Ti-6Al-4V and Ti-3Al-2.5V titanium (Ti) alloys was compared with that of unalloyed commercially pure titanium. The microstructural evolution of structure phases after annealing the titanium and its alloys at temperature near and above β transus and followed by furnace cooling to room temperature was studied using optical microscope, scanning electron microscope and X-ray diffraction techniques. The microstructure study illustrates that the heat treatment enhanced partitioning effect allows extensive formation of hemispherical and near spherical pits roughened surface to be readily acquired by chemically etching the annealed α + β titanium alloys. The kinetics of the chemical etching reaction process show a linear dependence on time. The annealed α + β titanium alloys that exhibit relatively lower weight loss and thickness reduction rate illustrate less chemical activity than the annealed unalloyed titanium.     

Titanium as an endogenous grain-refining nucleus

Several studies have confirmed the applicability of the inverse growth restriction theory for predicting grain size in titanium alloy systems. However, until now, no work has identified nuclei particles that could be used to refine the β-grain size of titanium alloys during solidification. This work investigated whether titanium powder can be used to nucleate β-grains during solidification. A novel technique was used to introduce titanium powder to a series of titanium alloys, which results in significant grain refinement with an order of magnitude increase in grain density. Electron back-scattered diffraction (EBSD) was used to prove that titanium substrates can epitaxially nucleate titanium during solidification, and although a number of other potential mechanisms were investigated, it was concluded that the titanium particles heterogeneously nucleate β-grains.     

Structural defects in Ni-Ti alloys in the region of B2-phase homogeneity

A comparison is made of the x-ray and pycnometric densities of Ti-Ni alloys, with a high nickel content relative to the equiatomic composition, when the alloys are quenched outside the region of -phase homogeneity. An analysis is made of the possibility of the formation of vacancies, interstitial atoms, triple defects, and substitutional defects in the alloys. It is concluded that substitutional defects are formed: nickel atoms which are excess atoms relative to those found at the lattice points in the CsCl superstructure are located in the titanium sublattice. An evaluation showed that in the formation of alloys near the equiatomic composition of TiNi, the atomic volumes of titanium and nickel are about 1.8 and 7.4% smaller than for the pure components, respectively.Translated from Izvestiya Vysshikh Uchebnykh Zavedenii, Fizika, No. 11, pp. 45–50, November, 1987.     

Formation of titanium carbide layer by laser alloying with a light-transmitting resin

The weight reduction of mechanical components is becoming increasingly important, especially in the transportation industry, as fuel efficiency continues to improve. Titanium and titanium alloys are recognized for their outstanding potential as lightweight materials with high specific strength. Yet they also have poor tribological properties that preclude their use for sliding parts. Improved tribological properties of titanium would expand the application of titanium into different fields.Laser alloying is an effective process for improving surface properties such as wear resistance. The process has numerous advantages over conventional surface modification techniques. Many researchers have reported the usefulness of laser alloying as a technique to improve the wear resistance of titanium. The process has an important flaw, however, as defects such as cracks or voids tend to appear in the laser-alloyed zone.Our group performed a novel laser-alloying process using a light-transmitting resin as a source for the carbon element. We laser alloyed a surface layer of pure titanium pre-coated with polymethyl methacrylate (PMMA) and investigated the microstructure and wear properties. A laser-alloyed zone was formed by a reaction between the molten titanium and thermal decomposition products of PMMA at the interface between the substrate and PMMA. The cracks could be eliminated from the laser-alloyed zone by optimizing the laser alloying conditions. The surface of the laser-alloyed zone was covered with a titanium carbide layer and exhibited a superior sliding property and wear resistance against WC-Co.     

Characterization of in situ mechanically worked PVD Mg–Ti alloys

Mg–Ti alloys with up to 46?wt%?Ti in solid solution were produced by physical vapour deposition (PVD) with in situ mechanical working. All the alloys exhibited compositional inhomogeneity, columnar microstructures and typical PVD defects. The thermal stability of the solid solutions decreased with increasing Ti content, with the most stable solid solution breaking up above 566?K. The in situ mechanical working reduced porosity by closing pores and flattened surface asperities. The oxide film on the surface of the Mg–8?wt%?Ti alloy was Ti-free. The air formed oxide film on the alloys with a Ti content above 8?wt% was identiffied as a mixture of MgO and TiO₂ covered by Mg(OH)₂ and hydromagnesite at the outermost surface. Magnesium oxide and titanium oxide were also formed at the columnar boundaries that were not affected by the in situ mechanical working. The oxide chemistry was studied using Auger parameter analysis.     

ICP-AES测定钛合金中铝、钼和锆的不确定度评定

对钛合金中铝、钼和锆含量测定过程中的不确定度来源进行了辨别,并在此基础上评定了分析结果的不确定度.测量不确定度主要来源于试样称量、标准溶液配制、校准曲线拟合、各种玻璃量器的使用及测量重复性.依据不确定度评定的步骤,计算得到了各分量标准不确定度及合成标准不确定度.