铂制品中的铂含量的无损方法——能量色散X射线荧光光谱法

本文叙述了采用能量色散Ｘ射线荧光光谱法对铂制品中的铂含量作无损检测的方法，我们运用多次熔炼的方法制作工作标样，根据Ｘ射线荧光光谱分析方法的基本原理，对样品进行检测及数据比对，并对方法进行了必要的修正，以提高测量方法的精度。本方法可测量多元素铂合金，其测量范围为Ｐｔ含量９９．９＾￣８５％，测量误差定为０．３％。     

铂制品中铂含量的无损方法──能量色散X射线荧光光谱法

本文叙述了采用能量色散X射线荧光光谱法对钳制品中的钥含量作无损检测的方法。我们运用多次熔炼的方法制作工作标样,根据X射线荧光光谱分析方法的基本原理,对样品进行检测及数据比对,并对方法进行了必要的修正,以提高测量方法的精度。本方法可测量多元素铂合金,其测量范围为Pt含量99．9％～85％,测量误差定为0．3％。     

铂首饰镍含量的X荧光法无损检测

应用能量色散X射线荧光光谱法对铂首饰镍含量(范围0．2％～10％)进行无损检测，利用沈阳冶炼厂制作的国家标准物质：Johnson Mattey Public Limited Company的标样以及我们自行研制的工作标样建立工作曲线，采用Lucas-Tooth和Price强度修正模式，有效消除可能的元素干扰，降低背景干扰提高方法分析精度。对样品的检测结果与其它方法结果     

铂、钯材料ICP分析方法的研究

由于铂、钯材料被广泛应用于多种精密行业,其材料含量也越来越受到重视,目前采用的方法不是操作复杂就是范围太窄而不符合日常检测要求,因此急需建立一种简捷快速的、适用于铂、钯材料含量为95．0％-99．99％的化学分析方法。该文用电感耦合等离子发射光谱分析,测定铂、钯材料中铂（钯）、铑、铱、钌、金、银、铜、铁、镍、铝、铅、锰、铬、镁、锡、硅、锌及铋等杂质元素的方法,达到了检出限低、重复性好、回收率在88．3％-100％的检测目标。     

XRF测定铂制品中Pt、Au、Pd、Ag、Cu、Ni等6种元素含量

本文利用XRF金标样的多元素回归方程,对Pt、Pd的荧光强度进行修正,修正后的荧光强度当作Au、Ag的荧光强度代入回归方程中,利用计算机编程计算铂制品中的Pt、Au、Pd、Ag、Cu、Ni等6种元素的含量。该法测定的准确度优于0.5％,适用于Pt的测定范围为85％～99.92％.具有无损、快速、准确、可靠等优点。     

能量色散X射线荧光光谱法测定贵金属首饰中的铅、汞

采用能量色散X射线荧光光谱法对金首饰和铂首饰中的有害元素铅和汞进行检测。在能量色散X射线荧光光谱仪上对金首饰和铂首饰的空白标样进行检测,得出铅和汞的检出限。然后以同样的方法对金首饰和铂首饰的标样进行检测。结合检出限和其他判定规则对金首饰和铂首饰样品中铅、汞元素的测试结果给出合格与否的判定。该测定方法与ICP法的实验比对结果表明了该方法的可行性。     

氯铂酸铵重量法测定铂合金首饰中的铂含量测量不确定度评定

本文根据GB/T19720-2005对首饰中铂含量进行测定,根据实验过程分析重量法测定铂首饰中铂含量不确定度的来源,对样品称量、杂质元素等不确定度分量进行分析,依据JJF1059.1-2012《测量不确定度评定与表示》对不确定度分量进行计算,并计算出合成不确定度及扩展不确定度。     

镀铂溶液中铂的快速测定

镀铂是装饰性电镀的重要镀种,铂是镀铂溶液中的主成分,检测和控制其含量对获得最佳的镀层质量十分重要.以氯化亚锡作显色剂,用分光光度法测定镀铂溶液中的铂,优选出最佳的测量波长,并研究了酸度、显色剂浓度及干扰元素对测定的影响.结果表明,铂的质量浓度介于0～10 μg/mL范围内遵守比尔定律,本方法简便快捷,并具有良好的选择性.     

X射线荧光光谱法检测银首饰合金中的铅含量

阐述应用X射线荧光光谱法(XRF法)检测银首饰合金中的铅元素。针对不同纯度银合金的工作标样,分别利用波长色散X荧光光谱仪和能量色散X荧光光谱仪对银合金空白工作标样进行实验,从而获得铅元素的检出限。在同等条件下,对各种银合金样品进行铅含量的分析测试以获得检测值。结合仪器检出限,评估检测值的校正系数,给出判定结果,与ICP法验证实验分析判定结果进行比较,证明XRF方法可行。分析讨论可能影响检测的因素。     

X射线荧光光谱法测定铂首饰中铂

X射线荧光光谱法测定铂首饰中铂,现有的国家铂标准物质中只含有Pt、Pd,而实际铂首饰样品的主成分是Pt,时常伴有Cu、Pd、Ag、Au.本文开展了铂首饰中铂、铜、钯、金、银化学成份标准样品的研制,主要内容包括制备标准物质候选物;对标准物质候选物进行均匀性检验;采用多家有资质的实验室协作定值的方式对标准样品进行定值;并对...     

Investigation of the interpolation relations for a platinum resistance thermometer over narrow temperature ranges

The systematic difference between the Callendar—Van Dusen function and the ITS-90 polynomial for working platinum resistance thermometers with different values of W(100) is analyzed and it is shown that this difference is not related to the purity of the platinum over a wide range of values of W(100), and depends considerably on the temperature range. A method of calculating the standard relations for platinum resistance thermometers is proposed based on a quadratic approximation of the ITS-90 function, and a method of constructing individual functions for platinum resistance thermometers in the 0–230°C range using a single calibrated point in addition to 0°C is described.Translated from Izmeritelnaya Tekhnika, No. 11, pp. 39–43, November, 2004.This is the last of the series of papers (of which the first was published in Izmeritelnaya Tekhnika No. 9, 2004), prepared from the proceedings of the Second All-Russia Conference on Problems of Thermometry Temperatura-2004, held in Obninsk in March 2004.     

高活性Pt／TiO2纳米管的制备及其光催化性能

采用电化学阳极氧化法和浸渍一提拉法成功制备了高度有序的Pt改性TiO2纳米管（Pt／TNT）阵列电极,并运用场发射扫描电子显微镜（FESEM）、X射线衍射（XRD）、x射线光电子能谱分析（XPS）、紫外可见漫反射光谱（UV—VisDRS）等手段对其进行表征,考察了其光电化学性质,并研究了该电极光电催化降解甲基橙染料废水的催化性能及其稳定性．结果表明,Pt的均匀负载成功地将TNT阵列电极的光响应范围拓宽到可见光区域,光电流密度达到负载前TNT阵列电极的18倍;Pt／TNT阵列电极对甲基橙的降解符合拟一级动力学,其反应速率常数为TNT阵列电极的3倍,这主要归结于Pt与TiO：间的肖特基势垒和纳米管阵列结构带来的较大比表面积、有效的光生电子和空穴的分离与传输和宽的光响应范围．     

A lamellar ceria structure with encapsulated platinum nanoparticles

A novel lamellar feather-like CeO₂ structure has been fabricated by using a triblock copolymer as the structure-directing agent. This material was characterized in detail by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, X-ray photoelectron spectroscopy, and BET surface area measurements. Compared with conventional spherical shaped ceria prepared by ammonia gelation, the ceria feathers have superior ability to support nanosized platinum particles due to their special structure. The “skeletons” of ceria feathers can serve as an ideal host matrix to anchor the platinum particles. Furthermore, the inter-crossing pattern of the “skeletons” also acts as a partition to separate platinum particles, allowing the Pt nanoparticles (average diameter ∼6 nm) to be highly dispersed in the structure. The Pt/feather-like CeO₂ catalyst exhibits high activity in the water gas shift reaction.      

The applicability of the ITS-90 method to platinum resistance thermometers of different purity

The static characteristics of platinum resistance thermometers with different platinum purities were measured. It is shown that in the 0–420°C range the ITS-90 method gives an error of less than 0.01°C, while in the 0–230°C range the error is less than 0.006°C. __________ Translated from Izmeritel’naya Tekhnika, No. 12, pp. 33–36, December, 2006.     

Point-defect formation and temperature coefficient of electrical resistivity of platinum and platinum-(10 wt%) rhodium alloy in the range 1100–1900 K

Measurement of the temperature coefficient of electrical resistivity of platinum and platinum-(10 wt%) rhodium alloy was performed by the modulation method in the temperature range 1100–1900 K. Nonlinear change in the temperature coefficient of resistivity of metals at high temperatures can be explained by the formation of equilibrium point defects. The enthalpy of point-defect formation in platinum md platinum-rhodium alloy has been determined to be 1.6±0.3 and 1.8±0.3 eV, respectively. The modulation frequency was 0.2 Hz; the amplitude of the temperature oscillation was about 10 K. The accuracy of the temperature coefficient of resistivity measurements was about 1%.     

硫酸铁铵滴定法测定高钛型高炉渣中的钛

针对高炉渣反应活性差、熔样困难等特点,采用将炉渣粒度球磨至120目以下,硼酸和碳酸钠(2+1)作熔剂,900℃下熔融20 min,在瓷坩埚中铺垫石墨的方式来代替铂坩埚熔融样品,然后用硫酸(φ=10%)加热浸取熔块,铝还原Fe3+消除干扰,最后用硫酸铁铵滴定法测定钛含量。该方法用于高炉渣中钛的测定,相对标准偏差RSD(n=5)为0.41%~0.75%,加料回收率为98.6%~101.5%,能满足测定要求。     

Biomimetic synthesis of platinum nanoparticles utilizing a terrestrial weed Antigonon leptopus

In this work, we report for the first time a new bio-inspired method for platinum nanoparticle (PtNP) synthesis utilizing a highly invasive terrestrial weed coral vine (Antigonon leptopus) as the main bioagent. Extracts of all three basic components of the plant – leaves, stem and root – were explored and were found to be suitable in effecting the PtNP synthesis. The electron micrographs of the synthesized PtNPs revealed the presence of particles of monodispersed spherical and polydispersed shapes in sizes ranging from 5 to 190?nm. The presence of Pt atoms was confirmed from the energy dispersive X-ray (EDAX) and X-ray diffraction (XRD) studies. The FTIR spectral study indicated that the polysaccharides and proteins in the plant extract could have been responsible for the reduction of Pt ions to PtNPs and the latter’s stabilization.     

精密铂电阻温度计的校准方法

介绍了精密铂电阻温度计的特性及0~660.323℃温度范围内精密铂电阻温度计的校准方法。提出对测量上限温度高于450℃的精密铂电阻温度计可参考使用说明书要求进行上限温度退火,进行定点法校准时,可采用熔化点温坪替代凝固点温坪,对于无法进行定点法校准的精密铂电阻温度计,可采用比较法校准及采用简化公式计算各项参数的可行性,同时指出自热效应对测量的影响。     

基于VBA的工业铂电阻半自动校准系统

介绍一种在Excel内嵌的VBA平台上开发的工业铂电阻半自动校准系统,对系统的工作原理及软件流程进行了论述,通过程序实现了判断恒温槽温场变化、自动记录铂电阻阻值数据、在校准(检定)完成后对铂电阻进行自动等级判定、自动生成原始记录和证书等功能,解决了以往工业铂电阻的校准(检定)工作中遇到的数据量大,后期处理繁琐的问题,具有推广价值。