氢化物发生-原子荧光光谱法测定铬矿中砷

铬矿中砷的测定方法对完善铬矿检测方法和质量评价手段有重要意义。在0.5 g样品中加入2 g过氧化钠,于650 ℃熔融20 min,熔融物经盐酸酸化溶解,以10%盐酸为载流,15 g/L硼氢化钾溶液为还原剂,采用氢化物发生-原子荧光光谱法(HG-AFS)进行测定,建立了铬矿中砷测定的新方法。实验表明,砷质量浓度在0.025～100 μg/L范围内与荧光强度呈线性关系,相关系数为1.000 0,方法检出限为0.05 μg/g,定量限为0.17 μg/g。对产地为南非、土耳其、巴基斯坦等19个国家共2 649个铬矿样品的成分进行统计,发现铬矿主要成分为铬、铁、镁、铝和硅;干扰试验表明,这些样品中的共存元素均不干扰测定。按照实验方法对3个不同砷含量的铬矿样品进行精密度和加标回收试验,结果的相对标准偏差(RSD,n=11)为1.4%～6.0%,回收率为96%~109%。将实验方法应用于与铬矿基体近似的铁矿标准物质中砷的测定,测定值与认定值基本一致。     

高温熔融-电感耦合等离子体原子发射光谱法测定含铁尘泥中5种有害元素

准确、快速地测定含铁尘泥中有害元素,对含铁尘泥节能降废项目研究及综合利用有着重要的指导意义。实验针对含铁尘泥试样因含碳量高,导致常规酸溶解方法如果不增加除碳步骤则很难完全分解试样的问题,采用高温熔融法将试样制成熔融液后倾倒于稀酸中溶解的方法,解决了碳含量高难溶解的问题。采用四硼酸锂-碳酸锂混合熔剂在高温下将试样熔融,熔融液高温倾倒于稀酸中制成澄清溶液,由于骤冷,试样炸裂成微小玻璃珠,无迸溅,操作简单,使得后续溶解过程快速完成,从而建立了电感耦合等离子体原子发射光谱(ICP-AES)测定P、Pb、K、Na、Zn共5种有害元素的方法。按照实验方法测定含铁尘泥中P、Pb、K、Na、Zn,测定值的相对标准偏差(RSD,n=9)在1.4%～5.7%之间,加标回收率在96%～110%之间。研究结果表明方法能够满足含铁尘泥样品中5种元素的定量分析要求。     

高压粉末制样-X射线荧光光谱法测定海洋沉积物中28种组分

常规粉末压片制样是一种简单、高效的绿色环保制样技术,但是应用于某些沉积物样品制备存在样片表面粗糙和粉末容易脱落的问题。实验采用高于常规的压力进行样品制备,建立了X射线荧光光谱法(XRF)分析海洋沉积物样品中包括硫、氧化钠、氧化镁、三氧化二铝、二氧化硅、五氧化二磷、氧化钾、氧化钙、二氧化钛、氧化锰、三氧化二铁、钴、镍、铜、锌、钒、铬、镓、铌、锆、钇、锶、铷、铅、钡、镧、钕和铪在内的28种主、微量组分的方法。探讨了压力为300 kN和1 600 kN时的制样效果,并尝试引入BP神经网络模型利用其非线性拟合能力校正主量组分的基体效应。结果表明,采用1 600 kN压力制备的样片,表面致密、光滑、不龟裂和不掉粉,制样重复性和测试精密度也有较大提高。以55个有证标准物质中17种组分的数据集为训练样本,建立了海洋沉积物样品中主、微量组分的遗传算法-BP神经网络预测模型。按照实验方法对各组分含量相对较低的实际样品连续测试12次,计算得方法的检出限在 0.63～634 μg/g之间;精密度试验结果表明,各组分测定值的相对标准偏差(RSD, n=7)为0.16%～25.1%。方法用于海洋沉积物实际样品分析,其分析结果与国标法的测定结果吻合,能够满足海洋沉积物样品中多种组分准确分析的要求。     

Formation of the Fe(II)-Fe(III) hydroxysulphate green rust during marine corrosion of steel

Rust layers formed on steel sheet piles immersed 1 m above the mud line for 25 years were analysed by Raman spectroscopy, scanning electron microscopy and elemental X-ray mappings (Fe, S, O). They consist of three main strata, the inner one mainly composed of magnetite, the intermediate one of iron(III) oxyhydroxides and the outer one of hydroxysulphate green rust GR(SO₄²⁻). Simulations of GRs formation in solutions having large [Cl⁻]/[SO₄²⁻] ratios revealed that the hydroxysulphate GR(SO₄²⁻) was obtained instead of the hydroxychloride GR(Cl⁻), as demonstrated by X-ray diffraction and transmission Mössbauer spectroscopy analyses. Measurements of the [S], [Fe] and [Cl] concentrations allowed us to establish that GR(SO₄²⁻) formed along with a drastic impoverishment of the solution in sulphate ions; the [Cl⁻]/[SO₄²⁻] ratio increased from 12 to 240. The GR, acting like a “sulphate pump”, may favour the colonisation of the rust layers by sulphate reducing bacteria.     

Thermal stability behaviors of Cr(N,O)/CrN double-layered coatings by TGA/DTA analysis

In this study, Cr(N,O)/CrN double-layered coatings were synthesized using the cathodic arc deposition (CAD) process. CrN film was first deposited onto a substrate as an interlayer to ensure better adhesion, and Cr(N,O) film was subsequently deposited on top of the CrN layer as the surface layer. Variation in the Cr(N,O) coating composition was achieved through changing the O₂/N₂ flow ratio during the last stage of processing. Phase structure, chemical composition, and morphology of the resulting coatings were analyzed and observed using the X-ray diffractometer, Auger electron spectrometer and SEM. In addition, oxidation behavior of the coatings was investigated using TGA/DTA methods. The tests were carried out by increasing temperature up to 1000 °C in ambient air. With the introduction of oxygen gas during the CAD process, a superficial layer was produced in the Cr(N,O) constituent containing CrN and Cr₂O₃ phases. The formation of the oxide phase attributed to the reaction of chromium and oxygen was more favorable than that of chromium and nitrogen. The results also showed that Cr(N,O)/CrN double-layered coatings exhibited superior oxidation resistance at elevated temperature than that of CrN single-layer coated specimen (870 °C vs. 750 °C).     

矢功率谱与RBF网络结合在旋转机械故障诊断中的应用

与传统功率谱相比,矢功率谱融合了多通道的能量信息,反映的信息更全面.径向基函数网络具有良好的推广能力和分类能力.基于此,本文结合矢功率谱和径向基函数网络,提出了一种新的故障识别方法,该方法以矢功率谱为特征向量,径向基函数网络为分类器.并以转子裂纹、转子不对中、油膜涡动为例进行实验研究,实验结果表明,该方法是有效的.     

Mn,Zr对Mg-Gd-Y合金组织与力学性能的影响

研究了微量Mn、Zr对Mg-13%Gd和Mg-9%Gd-4%Y合金铸态和挤压后的微观组织及力学性能的影响.结果表明:在铸态,含Zr合金的晶粒明显小于不含Zr的合金,而Mn对合金的铸态显微组织影响不大;将Mg-9%Gd-4%Y-0.6%Mn和Mg-9%Gd-4%Y-0.6%Zr合金挤压后,都可以得到非常细小均匀的等轴晶,晶粒尺寸约14 μm;这两个合金在挤压时效态(T5)的力学性能都明显优于WE54合金的,且Mg-9%Gd-4%Y-0.6%Zr合金比Mg-9%Gd-4%Y-0.6%Mn合金性能更好.     

Process Requirements for Cost-Effective Precision Grinding

Costs in precision cylindrical grinding are compared for different abrasives, machines and grinding conditions. The analysis is for repeated batch production. Account is taken of machine cost and abrasive cost. Cost comparisons were based on extensive trials to assess re-dress life against workpiece quality requirements. Experiments show that different workpiece materials require different strategies to reduce costs. Easy-to-grind AISI 52100 and difficult-to-grind Inconel 718 materials were ground at conventional speeds and at high speeds. It is shown that wheel speed affects production rate through acceptable values of re-dress life, removal rate and dwell time. Advantages were gained using vitrified CBN at conventional speed and at high speed. For both materials, vitrified CBN wheels used at high speed, gave better quality at lower cost than conventional abrasives. Wheel costs became negligible and labour costs greatly reduced. Re-dress life trials, usually neglected, are shown to be essential to reduce costs and maintain quality [1].     

基于SolidWorks/COM的压铸型计算机辅助设计

文章结合压铸型计算机辅助设计系统中标准件模块与压铸型零件注释模块的开发 ,提出并介绍了基于Solid Works/COM的应用程序开发思想与具体实现过程     

1.4%C超高碳钢显微组织与疲劳性能的研究

对1．4％C超高碳钢试样热处理后的疲劳极限与断裂韧性进行测定，观察了显微组织与试样断口。结果表明，经950℃淬火700℃回火热处理后，又经860℃正火处理，试验用钢的组织结构超细化且碳化物弥散均匀分布，获得良好的综合强度与韧性及较高的疲劳极限，断裂强度较40CrNiMo调质态提高48％，屈服强度提高15％，延性指标相当，是一种优良的结构钢材料。