离子镀渗铝

本文论述了离子镀渗铝的基本原理、工艺过程,从实验结果中获得了最佳工艺参数。并对试件进行了耐蚀试验、疲劳试验。对镀膜进行了结构分析、成份分析。     

石墨炉原子吸收法测定食品中镍的研究

建立了测定食品中镍的石墨炉原子吸收法，方法的最低检出限为１．６０μｇ／Ｌ，标准参考物牡蛎镍的测定值怀保证值偏差小于５％，回收率在８６．０％￣１０３．０％之间，并对我国八大类食品中镍含量本底值作了调查。     

电阻炉温度微机控制系统的研制

以个人计算机为基础，以Ａ／Ｄ转换器为核心，并配以适当的外围接口电路，实现对电阻炉温度自动控制．设计了一种过零检测电路，将ＰＩＤ控制增量转换成占空比，并由数字电路输出有一定占空比的矩形波，利用硬件方法实现普通双向可控硅的同步过零触发从而实现功率可调     

竖炉散料层热交换公式的简化计算及应用讨论

在竖炉内散料层的逆流换热系统中存在这样一个炉气与炉料温度实际相等的区域，据炉气与炉料水当量的变化特征，本文在Ｂ．Ｈ基塔耶夫建立的逆流换热模型公式的基础上、整理出更为简单，清晰的竖炉散料层热交换的简化计算式，并进行了应用讨论。     

精细小件化学热处理滚筒炉的研制

研制了适于精细小零件大批量化学热处理的滚筒炉,有效地解决了薄片状小零件在其它类型炉中散料处理时,由于零件相互堆叠、不能更位而导致加热和与活性气氛接触不均匀所带来的质量问题。为照相机、仪表、标准件等行业提供了一种新型工艺装备。     

Determination of lead, copper and manganese by graphite furnace atomic absorption spectrometry after separation/concentration using a water-soluble polymer

In this study, a water-soluble polymer, polyvinylpyrrolidinone (PVP) having chelating functionalities was used for the preconcentration and separation of traces of Pb, Cu, Ve and Mn prior to their determination by graphite furnace atomic absorption spectrometry. For this purpose, the sample and the PVP solutions were mixed and the metal bound polymer was precipitated by adding the mixture onto acetone. The precipitate was separated by decantation and dissolved with water. By increasing the ratio of the volumes of sample to water used in dissolving the precipitate, the analyte elements were concentrated as needed. The concentration of trace elements was determined using graphite furnace atomic absorption spectrometry. The analyte elements in matrix free aqueous solutions were quantitatively recovered. The validity of the proposed method was checked with a standard reference material (NIST SRM 1577b bovine liver) and spiked fruit juice, sea water and mineral water samples. The analytical results were found to be in good agreement with certified and added values. Detection limits (3δ) were 1.7, 3.6 and 4.1 μg l⁻¹ for Pb, Cu and Mn, respectively, using 10 μl of sample volume. The method is novel and can be characterized by rapidity, simplicity, quantitative recovery and high reproducibility.     

Beam-injection flame furnace AAS: comparison of different nozzle types for beam generation and application of sub-critical liquid carbon dioxide as carrier and gas pressure pump

In beam injection flame furnace AAS (BIFF-AAS) the sample is introduced as a free-flying high-speed liquid beam into an AAS flame-heated nickel tube, resulting in a considerable improvement in the power of detection. For optimization of beam generation different nozzle types (smooth jet nozzles, turbulent working nozzles) have been compared at different pressures. It was found that the type of the nozzle hardly influences the analytical signal. However, the flow rates resulting from the different inner diameters of the nozzles and the applied pressures led to drastic changes in the analytical signal. For these investigations a recently developed 0.6 MPa (84 psig) diaphragm pump system was used. Furthermore, for the first time ever sub-critical liquid carbon dioxide has been used simultaneously as a liquid gas-pressure pump, as carrier in a flow-injection system (FIA), and for the beam generation. Transport of the carrier takes place as a result of the head pressure (6 MPa) of the liquid CO₂ in the gas cylinder. For volatile elements (e.g. Cd, Hg, Pb, and Tl) detection limits between 0.2 µg L^–1 (Cd) and 28 µg L^–1 (Hg) were found, the standard deviation was from 0.6% to 3.2% depending on the element, concentration, and sample volume used. The use of liquid CO₂ as a carrier in FIA systems opens up new possibilities for online sample pretreatment and trace preconcentration.     

Method development for the determination of iron in milligram amounts of rice plants (Oryza sativa L.) from cultivation experiments using graphite furnace atomic absorption spectrometry

The amount of sample that is available for analysis in laboratory plant cultivation experiments is usually very limited. Highly sensitive analytical techniques are therefore required, even for elements that are present in the plants at mg g^–1 concentrations, and graphite furnace atomic absorption spectrometry (GFAAS) was chosen in this work because of its micro-sampling capability, and its relatively simple operation. Four micro-methods were investigated for the determination of iron in roots and leaves of rice plants: i) a micro-digestion with nitric and hydrochloric acids, ii) a slurry procedure using tetramethylammonium hydroxide (TMAH) tissue solubilizer, iii) a slurry prepared in 1.4 mol L^–1 nitric acid, and treated in an ultrasonic bath, and iv) the direct analysis of solid samples. The micro-digestion was suffering from high blank values and contamination problems, so that it could not be recommended for routine purposes. The TMAH method exhibited poor precision and occasional low recoveries, particularly for real samples. Direct solid sampling analysis gave results similar to those obtained with the slurry technique with ultrasonic agitation for the determination of iron in certified reference materials with iron content up to about 100 g g^–1, but was too sensitive for the investigated rice plants, which had an iron content up to several mg g^–1. The slurry technique with ultrasonic treatment of the samples, suspended in dilute nitric acid, was finally adopted as the method of choice.The method was then applied for the determination of iron in the leaves and in different compartments of the roots of two rice cultivars, one sensitive to iron toxicity, an important nutritional disorder, and the other one resistant to iron toxicity. The results suggest that the higher resistance to iron toxicity of the second cultivar is due to a smaller uptake of iron from the soil, resulting in lower iron levels in all compartments of the plant.     

Method of Eliminating Systematic Errors of Atomic Absorption Analysis in Atomization of a Material in a Graphite Furnace

By taking as an example the obtaining of the spectra of the gas phase over alkali metal iodides and calcium fluoride, we show the possibility of eliminating systematic errors of atomic absorption analysis which are due to nonselective absorption of light. It is been suggested that it makes sense to create a database that would contain molecular absorption spectra of the most abundant substances and would be intended for use by chemistsanalysts.     

燃烧过程中铅颗粒粒径分布的实验研究

使用高3.4m、内径0.15m的一维炉实验台,对燃烧中铅颗粒的粒径分布进行了实验研究。铅元素以醋酸铅溶液的形式通过空气雾化引入到燃烧液化石油气的炉膛中。使用切割粒径从0.48～12.63μm的8级Andersen撞击器和切割粒径从0.030～10.0μm的12级静电低压撞击器(ELPI)进行采样,同时对铅颗粒物的质量浓度粒径分布和数量浓度粒径分布进行了测量。使用场发射扫描电镜(FESEM)对铅颗粒微观形貌进行了观察。结果表明,在质量方面,铅颗粒主要集中在亚微米区间,质量浓度的峰值在0.2～0.6μm之间;在数量方面,铅颗粒主要集中在0.03～0.4μm区间,数量浓度的峰值在0.2～0.3μm之间。