电化学电极气体氧分析器计量标准不确定度的评定

简述电化学电极气体氧分析器的计量检定方法及过程。给出了检定过程中测量误差的数学模型及电化学电极气体氧分析器计量标准不确定度的来源，并对各不确定度分量进行了评定。电化学电极气体氧分析器计量标准的扩展不确定度小于5％。     

分析方法不确定度评定的通用数学模型

在总结化学实验室常用分析方法共性的基础上,提出了常用分析方法不确定度评定的通用数学模型,介绍了各不确定度分量的计算方法.并通过适当变换,实现了该数学模型在不同分析方法(如滴定法、极谱法、原子吸收光谱法、吸光光度法等)测量结果不确定度评定中的应用.     

几种热量计测量不确定度评定

评定了氧弹热量计、示差扫描热量计、水流型气体热量计的测量不确定度,并分析了各不确定度分量的来源．结果表明,影响热量计测量不确定度的主要因素为测量的重复性。     

氧乙炔焰线烧蚀率测定不确定度的评定

就氧乙炔焰线烧蚀率测定不确定度的评定进行探讨 ,以期提高我们的测试水平。实验按GJB 32 3- 87“氧 -乙炔烧蚀实验方法”进行。     

测定血清中Na 含量不确定度的评定

对血清中Na离子含量的测量不确定度进行评定。不确定度的来源主要包括Na离子标准工作液的配制过程、血清样品的定容消化制备、标准曲线拟合、钠离子各分量不确定度的合成等引入的不确定度计算出各分量的不确定度,通过合成得到测量结果的合成不确定度、扩展不确定度及测试结果的报告形式。     

标准溶液测量不确定度的评定

对标准溶液测量不确定度进行合理评定，充分估计分析不确定度的来源，从量值检验时考虑到影响不确定度的各种因素，测量方法的不确定度．配制时考虑到影响不确定度的各种因素以及标准溶液的不均匀性和在有效期内的变动性所引起的不确定度等方面进行综合分析，得出其扩展不确定度。并以镍标准溶液为例作实际分析。     

塑料中镉的测定不确定度评定

建立了用实验室内精密度和偏差的数据来评定塑料中镉的测定不确定度的方法. 通过研究不同基体和不同含量水平的样品, 考察了方法的精密度和回收率, 分别计算并合并了两者的测量不确定度. 结果表明精密度和回收率的相对不确定度分量分别为0.026和0.068, 合成不确定度为0.072, 扩展不确定度为0.14. 此评定过程为实验室评定测量不确定度提供了一种新的方法, 简单、合理, 计算结果可靠.     

气相色谱-串联质谱法测定灌溉水中啶氧菌酯残留量的不确定度评定

采用气相色谱串联质谱仪(GC-MS/MS)测定水中啶氧菌酯残留量,同时按照测量不确定度的程序,对方法的不确定度进行评价,分析不确定度的来源,并对各分量进行计算与合成.当水中啶氧菌酯的残留量为1.30μg/L时,其扩展不确定度为0.08μg/L.通过分析发现,影响测定的不确定度主要因素为重复性试验和方法准确度等过程.方法可为啶氧菌酯残留量的测量结果准确性和置信度提供理论依据.     

水氯化物的测定不确定度评定方法

根据GB/T 11896-1989《水质氯化物的测定硝酸银滴定法》国标方法对水中氯化物测定的不确定度进行评定。首先对不确定度主要来源进行识别,如测量重复性、标准NaCl的纯度、称量和定容、液体的转移、标准溶液在滴定和标定时滴定管的体积计量、温度等,然后建立数学模型,分别计算各输入量的不确定度分量和相对不确定度分量,合成各相对不确定度分量的方差和合成标准不确定度计算,得到测量结果的最终表示方式。     

芥子气纯度测定不确定度分析与评定

采用酸碱滴定法测定芥子气纯度,对测量结果的不确定度进行评定。分析了测定过程中不确定度来源,包括滴定剂的标定、消耗滴定剂体积、样品称量等引入的不确定度及其计算方法,最后合成得到标准不确定度。当芥子气纯度测定结果为94.78%时,扩展不确定度为0.34%(k=2)。实验结果表明,样品称量引入的不确定度对测量结果的影响最大。     

Low temperature microwave-assisted vs conventional pyrolysis of various biomass feedstocks

A comparison between conventional pyrolysis and a novel developed low-temperature microwave-assisted pyrolysis methodology has been performed for the valorisation of a range of biomass feedstocks including waste residues.Microwave pyrolysis was found to efficiently deliver comparable evolution of bio-gases in the system as compared with conventional pyrolysis at significantly reduced temperatures(120 180 C vs 250 400 C).The gas obtained from microwave-assisted pyrolysis was found to contain CO 2,CH 4 and CO as major components as well as other related chemicals(e.g.acids,aldehydes,alkanes) which were obtained in different proportions depending on the selected feedstock.     

Simulation of the fast pyrolysis of Tunisian biomass feedstocks for bio-fuel production

An optimized model is developed for the production of bio-fuels from biomass using a SuperPro Designer tool. Four types of Tunisian biomass feedstocks including date palm rachis, olive stones, vine stems and almond shells were selected for the fast pyrolysis process simulation. Simulation tests were performed at different temperatures ranging from 450 to 650 °C, and residence times ranging from 0.1 to 10 s and the products yield were determined. The obtained results indicate that a temperature of 575 °C and 0.25 s vapor residence time are the optimum parameters to maximize the bio-oil yield. Comparison between the different feedstocks indicates that a higher bio-oil fraction was obtained from the date palm rachis and vine stem. However, the difference between the samples is not significant and further investigations on the bio-oil properties are requested to select the suitable biomass for bio-oil production in Tunisia.     

Trace determination of oxygen by a potentiometric method

Summary A potentiometric method is proposed for the determination of microamounts of O₂ in inert gases, based on the dependence of the corrosion time of dilute amalgams on the oxygen content in the atmosphere of the cell. The method was tested by analysis of chemically pure argon.

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Zusammenfassung Eine potentiometrische Methode für die Bestimmung von Mikromengen Sauerstoff in inerten Gasen wurde vorgeschlagen, die auf der Abhängigkeit der Korrosionszeit verdünnter Amalgame von dem Sauerstoffgehalt der Atmosphäre in der Zelle beruht. Das Verfahren wurde an chemisch reinem Argon geprüft.

     

Evaluation of high pressure oxygen microwave-assisted wet decomposition for the determination of mercury by CVAAS utilizing UV-induced reduction

The UV-induced cold vapor generation with formic acid coupled to AAS after high pressure oxygen microwave decomposition was developed for determination of total Hg in analytical samples. Certified reference materials were decomposed in 1.5 mol L^{− 1} HNO₃ and 0.6 mol L^{− 1} H₂O₂. Microwave decomposition with oxygen has allowed the use of diluted reagents. The oxygen at a pressure of ca. 15 bar was delivered during the mineralization to the closed vessel. Interference by unused residues of H₂O₂ and HNO₃ was observed. In order to overcome the negative effect of remaining oxidants pre-reduction with hydroxylammonium chloride at a concentration 0.75 mmol L^{− 1} was used. Recovery of mercury in four reference materials containing 0.20–1.99 µg g^{− 1} Hg were 99–104% of certificate values. The limits of detection and quantification in the sample solutions were determined as 0.12 and 0.38 µg L^{− 1}, which corresponds to absolute detection limits of 12 and 38 ng g^{− 1} for total mercury, respectively. The results were in good agreement with the t-test at a 95% confidence level of the certified values in the investigated reference materials. The relative standard deviation was better than 7% for most of the samples.     

Quantitative determination of specific heat by differential scanning calorimetry

The influence of some experimental parameters on the quantitative determination of specific heats by DSC is discussed. Conditions allowing measurement of the specific heat with a maximum relative error of 1.5 % are proposed. The specific heats of NaA zeolite,C _p=0.227±0.003 cal.°C^?1.g^?1, and AgA zeoliteC _p=0.205±0.003 cal.°C^?1.g^?1 have been determined.     

碘量法测定氧载体中的活性氧

氧载体中活性氧气的含量是衡量氧载体实用性的一项重要指标。自行设计了一种改进的碘量法测定混合气体中氧气的装置,完成了混合气体中微量氧气的测定,将该方法用于固相合成氧合氧载体中活性氧的测定,取得很好的结果,为混合气体中氧气的测定提供了新思路。     

New results in oxygen determination by 14-MeV neutrons

New methods of precision analysis for the determination of oxygen, of the thickness of oxide films in the nm range, and of oxygen traces by the use of 14 MeV neutrons are reported. They were tested with success to determine oxygen in ceramics, glass and magnetic materials. Thus, the thickness of oxide films on metal powders has been determined. The methods are recommended as reference methods in trace analysis of non-ferrous materials.     

Developments in the determination of organic oxygen by pyrolysis-gas chromatography

Summary The use of 40% nickel-coated carbon is described in a method for direct determination of organic oxygen, based on instantaneous pyrolysis of the sample in a long quartz capsule, followed by gaschromatographic separation and thermal-conductivity measurement of the CO produced. A short layer of nickelised carbon is used, placed separately from the pyrolysis zone in order to avoid physical and chemical interferences. Carbon coated with 40% of nickel remains active for approximately 20 days when used in a carbon/ carbon dioxide reaction system.

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Zusammenfassung Die Verwendung von 40% Nickel enthaltender Kohle zur direkten Bestimmung von organisch gebundenem Sauerstoff wurde beschrieben. Sie beruht auf der Momentpyrolyse der Probe in einer langen Quarzkapsel und nachfolgender gaschromatographischer Trennung und Messung des entstandenen Kohlenmonoxids durch Wärmeleitfähigkeitsbestimmung. Eine kurze Schicht mit Nickel versehener Kohle wird abseits von der Pyrolysezone verwendet, um physikalische oder chemische Störungen zu vermeiden. Mit 40% Nickel versetzte Kohle bleibt etwa 20 Tage aktiv, wenn sie in einem Kohle/Kohlendioxid-System verwendet wird.