骨质瓷中磷酸三钙含量检测的不确定度评定

按照JJF1059-1999《测量不确定度评定与表示》建立了数学模型,对骨质瓷中磷酸三钙含量的测量不确定度进行了评定;分析不确定度分量及其来源,计算了各分量的不确定度,最后计算出检测结果的合成标准不确定度和扩展不确定度。检测结果和不确定度评定结果为（38．26±0．20）％、k=2,沉淀洗涤造成沉淀损失引起的测量不确定度分量最大。     

微量法测定石油产品中残炭含量的不确定度评价

按照测量不确定度评定的通用规则,建立了数学模型,对微量法测定石油产品中残炭含量的测量不确定度进行了评定,分析了方法中的不确定度分量及其来源,计算了各分量的不确定度,最后计算出了检测结果的合成标准不确定度和扩展不确定度。检测结果和不确定度评定结果为（0．35±0．02）％,k=2。残炭质量称量引起的测量不确定度分量为最大。     

出口金属硅中硅含量检测的测量不确定度评定

按照测量不确定度评定的通用规则,建立了数学模型,对出口金属硅中硅含量检测(容量法)的测量不确定度进行了评定,分析了方法中不确定度分量及其来源,并计算了各分量的不确定度,最后合成标准不确定度和扩展不确定度.检测结果和不确定度评定结果为(99.28±0.01)%,K=2.从各个分量对总不确定度的贡献大小来看,乙二胺四乙酸二钠(Na2EDTA)标准溶液的配制对结果影响最大.     

ICP-MS测定多晶硅基体中金属杂质的不确定度评定

建立ICP-MS测定多晶硅基体中金属杂质Cr、Fe、Ni、Cu、Zn含量的不确定度评定法是多晶硅分析检测行业所迫切需求的。从样品称量、样品溶液的体积变化、仪器测量标准曲线和样品溶液中各杂质元素的浓度、以及整个试验过程中测量重复性引入的不确定度进行分析评定,依次得出分量标准不确定度,以分量标准不确定度计算出合成标准不确定度,并应用A类不确定度评定法计算出测量结果的扩展不确定度,并得出检测结果的置信区间。     

红外碳硫仪测定焊剂中碳、硫含量的不确定度

本文介绍了高频红外碳硫分析仪示值误差测量不确定度的评定。建立了高频红外碳硫分析仪测定焊剂中碳、硫含量测量结果不确定度数学模型,从8个方面评定了不确定度分量的贡献,分别计算其相对标准不确定度,最终得到合成标准不确定度和扩展不确定度。依据《JJF 1059.1-2012测量不确定度评定与表示》,对焊剂中碳硫含量测定结果的不确定度进行评定,为日常检测工作提供指导。结果表明,方法的检测结果可信度较高,适于焊剂中碳、硫含量的测定。     

重量法检测污水中悬浮物含量的不确定度评定

采用重量法对4个不同浓度的实际污水水样的悬浮物含量进行了检测,并根据检测结果进行了测量不确定度的评定。根据实验过程,建立了数学模型,对各个不确定度的来源进行了分析,并计算出各个不同浓度样品的不确定度分量、合成不确定度和扩展不确定度,找到了占支配地位的不确定度分量,从而使检测人员对该方法检测悬浮物含量进行不确定度评定的计算变得简单实用。     

对液相色谱法测定嘧霉胺悬浮剂中嘧霉胺含量不确定度评定

建立了液相色谱法测定嘧霉胺悬浮剂中嘧霉胺含量的数学模型,通过对测定过程中不确定度分量来源的分析,计算了各不确定度分量,并计算出合成不确定度和扩展不确定度。同时,对测定结果进行了描述,达到了对测量不确定度合理评定的目的,反映了实验室的检测技术水平和检测设备水平。     

气相色谱法测定防冻液中乙醇含量的不确定度评定

建立了气相色谱法测定防冻液中乙醇含量的数学模型,通过对测定过程中不确定度分量来源的分析,计算了各不确定度分量,并计算出合成不确定度和扩展不确定度,同时对测定结果进行了描述,达到了对其测量不确定度合理评定的目的,反映了实验室的检测技术水平和检测设备水平。     

冷原子吸收法测定尿中汞的不确定度评定

目的冷原子吸收法测定尿中汞的不确定度进行评定,保证检测工作的准确性。方法结合日常检测,根据测量不确定度的评定理论和检测方法进行评定,确定和计算测量过程中各不确定度分量,并对测定结果进行完整描述。结果合成标准不确定度为0.0410,对于尿汞含量为0.139μg的样品,其扩展不确定度为0.0112μg。结论该法的不确定度主要来源于样品处理、标准溶液配制和曲线线性等方面。     

X-射线荧光光谱法测定石灰石中三种组分含量的不确定度评定

采用压片制样-X射线荧光光谱法测定石灰石中氧化钙、氧化镁和二氧化硅的含量,分析了测量结果的不确定度来源。对测量重复性、标准物质、工作曲线变动性、制样因素、检测环境和仪器稳定性引起的不确定度分量进行评定,计算了合成标准不确定度和扩展不确定度。评定结果表明,工作曲线变动性引入的不确定度分量对总的不确定度影响最大。     

氢化物发生-原子荧光光谱法测定工业磷酸中的铅

采用盐酸处理工业磷酸试样,用氢化物发生-原子荧光光谱法测定工业磷酸中的铅,对仪器条件、盐酸酸度、预还原剂用量、还原剂用量、共存元素干扰进行了试验,方法的检出限为0．028ug／L,测定精密度0．84％,回收率为98．9％-101．4％。建立的氢化物发生-原子荧光光谱法测定工业磷酸中的铅的分析方法具有操作简单,灵敏度高,重现性好等优点,能满足日常检验的要求。     

Removal of Water from Spent Phosphoric Acid Using a Sandwich Silicon Carbide Ceramic Membrane

It is important to develop an energy- and cost-efficient method of concentrating phosphoric acid because it is widely used in several industries. Three different ceramic membranes, namely, a silicon carbide (SiC) membrane, a TiO₂-coated SiC membrane, and a sandwich membrane of TiO₂ between SiC, were successfully applied for the selective separation of water from spent phosphoric acid. SiC was selected as raw material, TiO₂ as supporting material. The membrane was characterized by various instruments to check all parameters. Using the solution diffusion, statistical modeling of these membranes was performed and the membrane parameters, such as membrane diffusivity and mass transfer coefficient, were calculated. By reducing the porosity of the membrane, the desired separation can be improved.     

湿法(浓)磷酸化学法脱氟净化的研究

试验研究了湿法(浓)磷酸两种化学脱氟法，即氟硅酸钾一乙醇沉淀法和氟铝酸钠沉淀法。认为，后者优于前者，比I．M．C真空蒸汽深度脱氟法更经济，更适合于中小企业。文中关键探讨了铝在脱氟过程中的机理，同时对湿法(浓)磷酸(选择性)净化做了综述。     

磷酸快速萃取原理概述

磷矿酸解反应并非是离子间的交换,而是功能基团之间的交换。因此,磷酸萃取过程的P2O5萃取率、磷酸及后继产品性质、磷石膏结晶晶形和过滤性能与磷矿物特性有关。影响装置生产能力的主要因素是泡沫而不是反应时间和温度;磷酸快速萃取技术的核心是提高萃取和料浆过滤系统的温度。     

BESA磷酸工艺─溶剂萃取与原料选择

着重介绍了ＢＥＳＡ湿法磷酸的净化工艺。     

Recovery of Phosphoric Acid from Spent Petrochemical Catalysts

Petrochemical catalysts are widely used in the industry. For the production of cumene, zeolite-based catalysts containing phosphoric acid are applied. Over the time, coking deactivates the surface, and the catalyst has to be exchanged and disposed of. Different process approaches for recycling the phosphoric acid-containing catalysts were investigated. Related preliminary investigations have shown that calcination of the used catalyst is necessary prior to reprocessing. By digesting the catalyst with hydrofluoric acid, ∼96 % phosphate was recovered. However, this process is very costly in terms of process technology. More promising is digestion by basic or acidic routes. Several options are possible here, and digestion with H₃PO₄ proved to be particularly suitable. Here, phosphate yields reached up to 98.8 %, with a positive balance of economic efficiency at the same time. The catalyst can be produced and recycled in the same plant with the same reagents, what constitutes a major breakthrough towards sustainability in industrial catalysis.     

采取有效措施实现磷酸生产水平衡

针对磷酸生产用水的特殊性,总结了大装置磷酸生产用水封闭循环使用存在的问题,并因地制宜地找到了解决此问题的方法。     

Optimization of the Dissolution of Tincal Ore in Phosphoric Acid Solutions at High Temperatures

The aim of the study was to investigate the optimization of the dissolution of tincal ore in phosphoric acid solutions at high temperatures in a batch reactor. The effect of the following parameters on the dissolution process was investigated: the reaction temperature, the phosphoric acid concentration, the particle size, and the solid-to-liquid ratio. The best conditions for the dissolution were determined using the 2⁴ factorial experimental design method. The optimum values of the parameters were experimentally determined. The effective parameters were the reaction temperature, the phosphoric acid concentration, the particle size, and the solid-to-liquid ratio. The optimum conditions resulted in the maximum boron dissolution at an acid concentration of 1 M, reaction temperature of 85°C, particle size of 4.75 mesh, and solid-to-liquid ratio of 1/6 g · mL^?1. Under these optimum conditions, the best dissolution yield was 98.26%.     

Removal of Trace Metal Impurities from Pretreated Phosphoric Acid by Foam Fractionation

Demands for phosphoric acid are growing rapidly in various industries. This has highlighted the importance of optimizing its production and purification methods. Phosphoric acid can be produced by a wet process. However, due to the presence of many organic and inorganic impurities in the wet product, purification of the resulting product is a major concern in this industry. Removal of trace metal impurities (such as magnesium, cadmium, chromium, zinc, etc.) from produced phosphoric acid in a wet process was investigated by foam fractionation in a semi-batch setup using sodium dodecyl sulfate (SDS) as the surfactant. Effects of inlet air velocity, surfactant concentration, and surfactant selectivity were investigated. The optimum air velocity and surfactant concentration were obtained as 0.020 cm/min and 0.7 g/L, respectively. At the optimum condition, the total removal efficiency and enrichment factor reached were 70.2% and 4.39, respectively, while the acid loss was 8.3%. The total metal removal efficiency was increased to 95.3% in a two-stage experimental run.     

湿法磷酸生产用泵密封技术研究进展

综述了磷酸用泵密封技术的研究进展,介绍了填料密封、机械密封、组合密封和动力密封用于磷酸生产用泵的结构和特点,指出了目前磷酸泵密封装置面临的问题以及今后的发展方向。