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。     

光电隔离技术在PLC上的应用

光电耦合技术主要是为了解决模拟电路和数字电路的集成、交叉应用时的相互干扰问题,同时具有信号整形、降低误操作等功能。本文就光电隔离抗干扰技术的特性在PLC的接口、功率驱动、远距离传送、过零检测电路中的应用做了介绍。     

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.     

异形坯连铸坯壳应力与鼓肚变形分析

坯壳应力引起的鼓肚变形是影响铸坯质量的重要因素,为防止过大的鼓肚变形,依据湍动能理论、热流传递理论和粘弹性理论,建立了异形坯三维热-力耦合模型,开发了鼓肚分析软件,从而避免了漏钢事故的发生.该模型将温度场和应力场的计算相互耦合,交替进行.结果表明:异形坯截面最危险点位于腹板中部,其次为翼板中点,在两者相结合的圆角部,由于凝固坯壳比较薄,其应力值也比较大;当坯壳厚度小于20 mm时,两点的鼓肚变形量将分别超过其极限变形量,铸坯出结晶器时必然发生漏钢事故.该模型通过预测坯壳应力和鼓肚变形量为现场安全生产提供了理论依据.     

Quantification of trace amounts of impurities in high purity cobalt by high resolution inductively coupled plasma mass spectrometry

An analytical method using high resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid simultaneous determination of 24 elements (Be, Mg, Al, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Ga, Ge, As, Se, Mo, Ag, Cd, Sn, Sb, Ba, Pt, Au, and Pb) in high purity cobalt was described. Sample digestions were performed in closed microwave vessels using HNO3 and HCl. The matrix effects because of the presence of excess HCl and Co were evaluated. The usefulness of high mass resolution for overcoming some spectral interference was demonstrated. The optimum conditions for the deter- mination were tested and discussed. The standard addition method was employed for quantitative analysis. The detection limits were 0.016-1.50 μg?g?1, the recovery ratios were 92.2%-111.2%, and the RSD was less than 3.6%. The method was accurate, quick, and convenient. It was applied to the determination of trace impurities in high purity cobalt with satisfactory results.     

厌氧膜生物反应器在废水处理中的研究进展

厌氧膜生物反应器是一种处理高浓度有机废水的有效工艺.综述了厌氧膜生物反应器的特征,在工业废水处理中的应用以及低温下厌氧处理低浓度废水的效果,并展望了厌氧膜生物反应器的应用前景.     

水电站进水塔动水压力研究和探讨

基于理想流体,将进水塔简化成水中悬臂梁体系,推导了其受迫振动时的动力响应方程,给出了进水塔内外表面动水压力的解析表达式。与有限元法、水工抗震规范公式计算结果进行了对比,分析验证了该方法在进水塔结构上的适用性及准确性。结果表明:动水压力表达式与结构振型密切相关。该方法的动水压力曲线趋势与有限元方法相似,均在水面以下某深度处迅速变大及达到最大值后曲线值减小弯回,两者最终在塔体底部收于相近的值;最大值大于有限元法,其最大值处曲线折回明显,幅度较大。弹性模量和进水塔高度对动水压力的曲线形态和数值有重要影响。同时,输入激励荷载的频率对动水压力影响巨大,尤其频率与进水塔某阶频率相近时会导致动水压力的异常增大。该方法对分析进水塔动水压力具有参考价值。     

Energy Efficiency of an Indirect Thermally Coupled Distillation Sequence

Several thermally coupled distillation sequences have been proposed to improve the thermal inefficiency of conventional distillation sequences. Particularly, for the separation of ternary mixtures, structures that perform a lateral extraction in one of the columns of the integrated arrangement have been shown to provide significant energy savings. The structure of existing sequences, based on conventional distillation columns, might provide the basis for alternate thermally coupled designs. In this paper, it is shown how a thermally coupled system derived from an indirect conventional sequence can provide energy savings through a proper optimization of the interconnecting streams.     

纳米氧化锆/氧化锌光催化降解酸性红B的研究

以醋酸锌和氯氧化锆为原料，采用化学沉淀法制备了纳米氧化锆／氧化锌光催化剂。在中性条件下研究了催化剂煅烧温度，锆复合量，催化剂用量，染料初始质量浓度，过氧化氢质量浓度，各种阴、阳离子等条件对酸性红B脱色反应的影响。结果表明，该催化剂最佳制备条件为煅烧温度350℃，锆复合量2．5％（物质的量分数）。催化剂最佳用量0．9g／L。提高染料初始质量浓度会降低反应脱色率。适量过氧化氢可提高反应脱色率，当其质量浓度超过300mg／L会起负作用。NO3^-对反应影响不大；Fe^3＋和Ag^＋对反应起促进作用；SO4^2-，Cl^-，NO2^-等阴离子和Fe^2＋，Mn^2＋等阳离子对反应起抑制作用。