我国冶金分析定量检测仪器的发展趋势

为了了解我国分析仪器的发展,推动冶金分析领域定量检测技术的进步,文章以北京分析测试学术报告会暨展览会(BCEIA)在国内的展示成果为依托,选择电感耦合等离子体发射光谱(ICP-OES)、电感耦合等离子体质谱(ICP-MS)、X射线荧光光谱(XRF)、激光诱导击穿光谱(LIBS)等基础定量检测仪器为主要分析对象,归纳总结了这些仪器的发展过程、基本原理和主要结构。从分析检测人员的视角,讨论了该检测仪器的优势特点及应用效果;展望了定量分析检测技术的发展趋势;提出了以定量检测仪器为基础的新型高端科学仪器的发展前景。又以激光剥蚀电感耦合等离子体质谱(LA-ICP-MS)、辉光放电质谱(GD-MS)、电子探针X射线显微分析仪(EPMA)等拓展联用检测仪器为例,介绍了设备的主要特点及应用,最终总结出LA-ICP-MS为固体样品中微量元素分析的常用技术,GD-MS技术是痕量元素分析的重要手段,EPMA技术因具有与其他仪器结合包容性高的优点,虽然在使用过程中存在一定的缺陷,但已成为通用的分析手段。而我国定量分析检测技术正朝着现场化、专用化及标准化的方向发展。     

电感耦合等离子体原子发射光谱法测定云南某矿山锑矿选矿流程样品中锑

锑在现代工业体系中占有重要地位,快速准确测定锑矿中锑含量对锑矿的采选具有重要指导意义。云南某矿山锑矿以萤石为主要伴生矿,现有的盐酸、硝酸、氢氟酸和高氯酸混酸体系无法彻底分解样品,而采用碱熔处理流程长且引入大量基体,均无法满足准确快速测定的要求。选择硫酸-氢氟酸混酸体系分解样品,再用酒石酸-盐酸混合溶液加热浸取,锑完全溶解于溶液中,选择Sb 206.833{463}nm为分析谱线,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定锑。结果表明,锑的质量浓度在5.0～80 μg/mL范围内与其发射强度呈良好的线性关系,校准曲线线性相关系数r=0.999 8;方法的检出限为0.012 μg/mL。按照实验方法对锑矿石成分分析标准物质和锑矿选矿流程样品中锑进行测定,结果的相对标准偏差(RSD,n=5)为0.71%～5.7%;标准物质的认定值和测定值相一致;锑矿选矿流程样品中锑的加标回收率为97%～102%,满足国家地质矿产行业标准DZ/T 0130—2006的要求。     

Passivation of Fe-Cr alloys studied with ICP-AES and EQCM

The response of sputter deposited Fe-15Cr and Fe-25Cr alloys to a rapid potential increase in the passive region was studied using two in situ methods: electrochemical quartz crystal microbalance and inductive coupled plasma-atomic emission spectroscopy (ICP-AES). Both methods indicated an increase in the dissolution rate of iron following the potential change; the total amount of material dissolved being higher for the Fe-15Cr alloy. For both alloys, about 10% of the total dissolved material was Cr. This result compared well with experiments on a 430 stainless steel. ICP-AES is shown to be useful for the in situ determination of partial currents of metal dissolution using solution analysis in a flow cell.     

铝合金凝固过程的声发射及氢气析出过程

采用声发射测试技术,对Al-Si和Al-Cu系合金凝固过程进行监测,证实合金在凝固过程中存在声发射现象,表现为两个声发射信号计数率峰,两个峰的总计数都随着合金中气体含量增加而增高。本文对Al-Si,Al-Cu合金系产生声发射现象的机理进行了探讨,同时,借助其它实验手段证实了声发射信号与合金凝固中气体析出有很好的对应性。第一个计数率峰与气泡在枝晶臂间形核相吻合。第二个计数率峰与凝固末期的枝晶间拉裂现象相对应,可能是氢在枝晶间析出和聚集产生高压氢导致的拉裂。     

Monitoring the tensile deformation in real unidirectional Kevlar-epoxy composites

Two acoustic emission (AE) parameters, event count rate (ER) and the skewness of the peak amplitude distribution (PAD), were found to correlate with mechanical and damage mechanisms in unidirectional Kevlar-epoxy composites loaded in tension. The ER of the AE reached a local maximum at about 0.3σ_cu (σ_cu= composite tensile strength), a minimum at about 0.6–0.7σ_cu, and increasing ER rates were noted as failure stress approached, with a peak at final failure.Along with our proposed approach to evaluate the PAD as a tool for characterizing processes, damage mechanisms and failure modes, the third statistical moment of the PAD, the skewness, was found to be able to distinguish between various mechanisms. From the beginning of loading until completion of the fibre straightening process, 0.6–0.7σ_cu, the value of the skewness steadily decreased, and then gradually increased to final failure. This behaviour is explained by a model based on the non-elastic mechanisms which contribute to the monitored AE. At final failure, the PAD's skewness value was affected by macroscopic failure modes. When this mode comprises fibre fracture with little matrix and interface splitting, the skewness decreased; when fibre failure was accompanied by matrix and interface splitting, its value changed slightly or even increased.     

压力容器无损检测 --长管拖车气瓶的无损检测技术

长管拖车是新类型的压力容器,作为一种高效运输工具,在许多领域应用广泛。综述了国内外拖车气瓶在制造和使用过程采用的各种无损检测方法及标准。方法包括超声、磁粉、渗透和声发射检测等。并介绍了各种无损检测方法的特点。     

水泥基复合材料微结构破坏声发射研究

研究不同组分的水泥基复合材料在三点弯曲负荷下,材料内部微结构破坏的声发射特性。结果表明,在加载初期声发射事件发展较为缓慢,且出现的主要是一些低振幅的声发射信号;而在峰值载荷附近,声发射事件数快速增长且开始有大量高振幅声发射信号出现。循环荷载作用下,粗集料水泥砂浆声发射呈现Felicit效应,而结构密实的活性粉末混凝土呈现Kaiser效应。     

Axial characterization of catalytic activity in close-coupled lightoff and underfloor catalytic converters

A exhaust system consisting of a close-coupled Pd technology 32 in³ lightoff converter and Pt/Rh technology 170 in³ underfloor converter was vehicle-aged for 56000 miles on a vehicle equipped with a 3.8 l engine. Following this aging, the converters were taken off the vehicle and cut into 1″ thick sections along their axis and characterized for lightoff and warmed-up activity using a laboratory reactor to simulate vehicle exhaust. Each section was also analyzed for the quantity of oil additive poisons (phosphorus and zinc) deposited. Following this initial characterization, the phosphorus and zinc deposits were removed, and the sections were characterized again for lightoff and warmed-up activity. This procedure was used to qualitatively determine the relative contribution of oil additive poisoning and thermal sintering to the total activity deterioration as a function of axial position in the catalyst monoliths.

Analysis of the lightoff converter as taken from the vehicle showed a dramatic axial gradient in the lean and stoichiometric lightoff and warmed-up (600°C) performance for HC, CO and NO_x, with most of the deterioration having taken place in the forward-most 1″ section of the converter, which was consistent with the gradient in the deposition of phosphorus (P) and zinc (Zn) in this converter. Comparison of these data sets with those obtained after removal of the P and Zn poisons indicates that most of the total deterioration of lean HC and CO activity can be attributed to P and Zn poisoning of the forwardmost 1″ section. When tested under stoichiometric conditions, most of the deterioration of HC activity is attributable to P and Zn poisoning, while most of the deterioration of CO and NO_x activity is attributable to thermal deterioration. A similar activity and poison deposition gradient was detected in the underfloor converter, but to a smaller extent.     

铬盐清洁生产中铬渣的综合利用

利用二氧化碳与液相氧化铬盐清洁生产工艺所产生的铬渣反应 ,得到碳酸氢镁溶液和富铁渣。碳酸氢镁溶液经加热分解得到轻质碳酸镁产品 ,富铁渣可以作为水泥行业原料铁精矿的替代品 ,最终实现了铬铁矿资源的充分利用和铬盐生产的零排放。     

POWER CONSUMPTION WITH ANCHOR MIXERS EFFECT OF BOTTOM CLEARANCE

The effect of bottom clearance on power draw for anchors is investigated. The results suggest that power input decreases as the bottom clearance ratio b/D increases. A new correlation is proposed in which both bottom and wall clearance effects on power input are considered. The dependence of power input on these effects is additive rather than multiplicative. Thus, the total power consumption is the sum of the power inputs generated by the wall and bottom clearance. Power results from 3D-CFD numerical simulations are also presented. These results confirm fairly well the experimental points.