The determination of manganese by electrothermal atomic absorption spectrometry with a graphite furnace at constant temperature

Many of the interferences reported earlier for the determination of manganese in a graphite furnace were not found when a modern graphite furnace was used. At high levels of chloride matrix, an interference which was observed in the modern furnace was reduced when manganese was determined under constant temperature conditions. In this work, the sample was introduced on a tungsten wire after the graphite furnace had reached a constant, preset temperature. Drying and ashing were accomplished outside the atomization furnace, reducing contamination from matrix materials.     

The clay wall of an ancient iron smelting furnace studied by Mössbauer spectroscopy

For an investigation of the ancient iron manufacturing technique, a modern simulation experiment was carried out. The smelting furnaces were built with clay. Charcoal and raw materials were installed from the top of the furnace. Magnetite was used as the raw material. In the furnace, iron oxide was reduced to metallic iron. The reduction reaction was mainly controlled by temperature and oxygen fugacity in the furnace. In order to investigate the possibility for the estimation of these parameters, ⁵⁷Fe Mössbauer spectra were recorded of the furnace wall at room temperature.     

Temporal Variations in Gas Temperature in an Atomization Stage of Cadmium and Tellurium Evaluated by Using the Two-line Method in Graphite Furnace Atomic Absorption Spectrometry

In order to discuss the atomization process of an analyte element occurring in a graphite furnace for atomic absorption spectrometry, we measured variations in the characteristic temperature with the progress of an atomization stage, by using a two-line method under the assumption of a Boltzmann distribution. For this purpose, iron was chosen as the analyte element. Also, the atomic absorption of two iron atomic lines, Fe I 372.0 nm and Fe I 373.7 nm, was simultaneously monitored as a probe for the temperature determination. This method enables variations in the gas temperature to be directly traced, yielding a temperature distribution closely related to the diffusion behavior of the probe element in the furnace. This temperature variation was very different from the furnace wall temperatures, which were monitored in conventional temperature control for atomic absorption spectrometry. Correlations between the gas temperature and the charring/atomizing temperatures in the heating program of the furnace were investigated. The atomization of cadmium and tellurium was also investigated by a comparison between the gas temperature with the wall temperature of the furnace. The atomic absorption of cadmium or tellurium appeared to be apart from the absorption of iron while the gas temperature was still low. Therefore, the analyte atoms could be atomized through direct contact with the wall of the graphite furnace, which has a much higher temperature compared to the gas atmosphere during atomization. Their atomization would be caused by conductive heating from the furnace wall rather than by radiant heating in the furnace.     

The gas temperature inside graphite furnaces used for atomic absorption spectrometry

A simplified model for heat transfer is used to calculate the gas temperature inside graphite furnaces used for atomic absorption spectrometry. In the absence of a convective flow through the furnace, the gas temperature follows the wall temperature of the heated furnace to within a few degrees. When a significant flow of protective cold gas is forced through the furnace, the gas temperature varies greatly along the furnace and its average value can be several hundred degrees lower than the wall temperature. These predictions are confirmed by the vapour temperatures which were measured experimentally by means of the two-line absorption technique. The results also demonstrate that analyte species volatilized in the furnace have the same temperature as the inert gas. The advantages of preheating the protective gas are indicated.     

On-line and in situ monitoring of oxygen concentration and gas temperature in a reheating furnace utilizing tunable diode-laser spectroscopy

Increased demands on energy savings and quality control in metallurgical processes have created incentives for new methods to monitor and control the process. In this paper we will present a field trial that shows the potential of tunable diode-laser spectroscopy (TDLS) for simultaneous contact free measuring and monitoring of the oxygen concentration as well as the gas temperature in a reheating furnace during production. The field trials were carried out at an oil-fueled reheating furnace during 7 weeks of production. The tunable diode-laser spectrometer was measuring in situ across the preheating zone and the soaking zone in the furnace. During the campaign the oxygen concentration and the gas temperature in the furnace environment were simultaneously monitored and instantaneous variations in these parameters could easily be recorded and subsequently correlated to actual changes in the process. Furthermore, the much shorter response-time of the TDLS technique compared with conventional measurement methods such as thermocouples and extractive gas analyzers was also demonstrated during the trials. The results show the potential for the TDLS technique to be used for energy savings as well as product quality improvements by controlling the burners in the reheating furnace. The results show that it would be possible to control and optimize the oxygen concentration with TDLS in the control loop of the reheating furnace.     

Environmental and chemical grounds for the utilization of blast furnace slag in the production of binders

Mineralogical, elemental, and oxide compositions and morphological surface characteristics of different grain-size fractions of blast furnace slag were determined. The hydraulic activity of blast furnace slag was found to be sufficient for its utilization in the manufacture of binders.     

乙烯装置裂解炉管焦炭燃烧特性的研究

齐鲁石化公司乙烯厂是我国最先引进计算机控制下蒸汽 空气在线烧焦技术的乙烯厂 ,在线烧焦使其过程自动化程度大大提高 ,裂解炉没有升降温过程 ,延长了裂解炉管的使用年限[1～ 5] 。但裂解气盘管管径较小 ,易于堵塞 ,烧焦时间稍短 ,管壁上的焦炭就燃烧不完全 ,目前在线烧焦时间还需 70ｈ～ 80ｈ。为了进一步缩短烧焦时间 ,节约能源 ,提高炉子运行周期 ,必须对乙烯装置裂解炉管焦炭的微观结构及燃烧过程进行深入研究 ,以提出进一步加快烧焦速度的办法 ,满足工业生产的需要。本研究采用国内某乙烯厂裂解炉管焦炭为实验原料 ,研究了焦炭的微观…     

Temperature of a W ribbon furnace in electrothermal atomic absorption spectrometry

Temperatures of the surface of a W ribbon furnace were measured using a pyrometer. The accuracy of the indicated temperatures was ascertained by a method based on the melting points of some metals, and it was demonstrated that the furnace temperature can be obtained with the pyrometer within an error of ± 15 K in a range from 1000 to 2000 K.A mathematical model for predicting the temperature was also proposed. The model is based on the power balance during atomization in the furnace. Two terms are essential: the power supplied to the furnace and the power lost by convection of sheath gas. Temperatures calculated by this model agreed well with those measured with the pyrometer.     

Transport of benzene and methyl‐substituted benzenes through carbon black‐filled epoxidized natural rubber

Sorption and diffusion of benzene and methyl‐substituted benzenes were investigated through epoxidized natural rubber (ENR) reinforced with four types of carbon black: superabrasion furnace (SAF), intermediate superabrasion furnace (ISAF), high‐abrasion furnace (HAF), and semireinforcing furnace (SRF). Kraus equation has been used to investigate the extent of reinforcement for the different types of carbon black used in the experiments. Effect of the type and concentration of the carbon black on solvent uptake and mechanism of diffusion were studied in detail. The rate constant for diffusion of the solvents in epoxidized natural rubber vulcanizate based on different carbon black type, and loading was investigated. Diffusion constant was found to decrease with increase in the degree of reinforcement. The interaction constant values were experimentally determined. The sorption data were used to determine the activation energy for the diffusion process and the enthalpy and entropy of the sorption process. The experimental results were compared with theoretical predictions. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 415–427, 1999     

Effects of growth behaviors on chemical and physical properties of sol–gel derived ZnO:Ga films

In this study, we investigated the effects of different heating processes on the structural, electrical and chemical properties of ZnO:Ga (GZO) films from the viewpoint of nucleation and growth behaviors. An infrared heating furnace and a traditional tube furnace were employed for the homogeneous and heterogeneous nucleation of GZO films. XRD patterns demonstrated that the preferential growth orientation of both kinds of GZO films is still the (002) direction. XPS data implied that the infrared heating process enables more uniform distribution of the dopant material and retards the oxidization of gallium in grain boundary areas. At the same time, the textured crystallite might provide a free tunnel for oxygen diffusion. Thus, the activation of free charge carriers could be more efficient when the GZO films were annealed under vacuum. As a result, the samples annealed by the infrared heating furnace had a noticeably high carrier concentration. Although the mobility was slightly smaller than that of the samples annealed by the tube furnace, film resistivity dropped obviously in general.     

New method for vapor pressure measurement applicable to potassium over coal slag

A constant-temperature graphite furnace for vapor pressure measurements at high temperatures is described. The capability of the furnace for measurements of potassium vapor pressures over coal slags is evaluated, and a series of measurements are presented and analyzed. Vapor loss mechanisms which are of general interest for graphite furnace spectroscopy are discussed.     

Application of Solid Sampling for the Determination of Total Fluorine in Fish and Seafood by High-Resolution Continuum Source Graphite Furnace Molecular Absorption Spectrometry

Total fluorine concentrations in some fish species and seafood such as mussels, squid (calamary), and shrimp were determined using the molecular absorption of calcium monofluoride (CaF) generated in a graphite furnace using a high-resolution continuum source atomic absorption spectrometer and direct solid sampling. The fish fillets and seafood were dried at 110°C, minced finely, put on the platform using masses less than 1.2?mg, and introduced to the graphite furnace with 20?µg of calcium by a solid sampling accessory. The effects of CaF wavelength, graphite furnace program, amount of sample introduced to the furnace, the use of modifier on the determination of fluorine were investigated and optimized. The absolute limit of detection and characteristic mass of the method were 0.28 and 0.14?ng of fluorine, respectively. By applying the optimized parameters, the concentrations of fluorine in various fish species and seafood were determined.     

Determination of bismuth in nickel-base alloys by atomic absorption spectrometry with introduction of solid samples into an induction furnace

Atomic absorption spectrometry with an induction furnace is applicable'to the determination of bismuth at 0.02–10 μg g^-1 levels in 1–30-mg samples of nickel-base alloys dropped into the furnace. Calibration graphs of peak absorbance versus mass of bismuth are constructed by use of standardised alloys. Samples of alloys can be added to the furnace at 2.5-min intervals. Calibration graphs, accuracy, precision and limits of detection of the method are discussed for 26 alloys. Accuracy is assessed by comparing the induction furnace results with results supplied with the alloys, and with results obtained for solutions of the alloys by atomic absorption spectrometry in association with hydride generation or a mini-Massmann furnace. With alloys containing more than 0.1 μg Bi g^-1, relative standard deviations by the induction furnace method are usually < 15%. The limit of detection for bismuth is 0.02 μg g^-1     

用ETV-ICP-MS研究Cr、Ni、Zr、Nb、Yb在石墨炉中的蒸发/原子化机理

本文以电热蒸发电感耦合等离子体质谱（ETV-ICP-MS）为手段,探讨了Cr、Ni、Zr、Nb和Yb在石墨炉中的蒸发/原子化机理;比较了不同化学改进剂存在条件下,Cr、Ni、Zr、Nb和Yb的蒸发行为和在石墨炉原子吸收（GFAAS）中的原子化行为;考察了石墨炉温度和ICP功率等实验参数对上述元素发射强度及轮廓的影响.结果表明,Pd和Mg化合物的存在对Cr、Ni、Zr、Nb和Yb的蒸发/原子化行为没有明显的化学改进作用;然而,以聚四氟乙烯（PTFE）为化学改进剂时,可显著改善Cr、Ni、Zr、Nb和Yb的蒸发行为,避免难熔碳化物的形成,降低待测物的蒸发温度;对Cr和Ni的GFAAS信号强度略有增强;但是,由于Yb、Nb和Zr氟化物的离解键能很高,难以离解/原子化,PTFE的存在反而降低了Yb、Nb和Zr在GFAAS中的信号强度.     

Determination of mercury in environmental samples by cold vapour generation and atomic-absorption spectrometry with a gold-coated graphite furnace

Mercury is determined at below the pg/ml level by a combination of cold vapour generation, trapping in a gold-coated graphite furnace and atomic-absorption detection. The mercury is reduced to the element by stannous chloride, stripped from solution by a stream of nitrogen and collected on a gold-coated porous graphite disk in a graphite furnace. It is then atomized by increasing the graphite furnace temperature and detected by an atomic-absorption spectrophotometer. The absolute detection limit and the characteristic mass were found to be 5 and 20 pg for 0.0044 absorbance, respectively. The concentration limit of detection was 0.1 pg/ml for a 50-ml sample, and the linear dynamic range covered three orders of magnitude. The precisions of the measurements were 2.7% for 0.1 ng and 2.6% for 2 ng of mercury. Analyses of NBS and NIES reference materials showed quantitative recovery. Analytical results obtained by the technique are presented for natural waters, marine biota and sediments.     

Capacitive Discharge Graphite Furnace Laser-Excited Atomic Fluorescence of Thallium

For the first time, an anisotropic graphite furnace heated by capacitive discharge was used for laser-excited atomic fluorescence spectrometry. A detection limit of 5 fg for thallium was obtained with a laser repetition rate of 500 Hz and a peak integration time of 80 ms. The use of a capacitive discharge furnace allows for a shorter integration time, which in turn should allow for integration of less background noise, and improved detection limits. Theoretically, the magnitude of the shot noise should be proportional to the square root of the integration time, and inversely proportional to the square root of the laser repetition rate. Experimental data illustrated the effect of laser repetition rate, but were inconclusive with respect to integration time. The linear dynamic range of the calibration curve was six orders of magnitude, which was comparable to that normally obtained for laser-excited atomic fluorescence in modern commercial graphite furnaces. Thallium was accurately determined in NIST biological samples at levels one to two orders of magnitude below the detection limit of electrothermal atomic absorption spectrometry, with an analytical precision between 8 and 20%. The interference effects of calcium, sodium chloride, and potassium chloride on the thallium signal were investigated and shown to be similar to both laser-excited atomic fluorescence in a conventional furnace and capacitive discharge furnace atomic absorption results reported in the literature.     

含钛高炉渣对水中氨氮的吸附特性

选用含钛高炉渣作为吸附剂,研究渣的投加量、粒径大小、温度以及溶液初始pH等因素对含钛高炉渣吸附水中氨氮的影响及吸附特性。动力学数据分析表明,准二级动力学模型能更好地描述含钛高炉渣对氨氮的吸附;颗粒内扩散方程拟合结果发现,含钛高炉渣对氨氮的吸附包括表面吸附和颗粒内扩散两个阶段。吸附等温线拟合表明Langmiur方程能够更好地模拟含钛高炉渣对氨氮的吸附过程。在20℃、反应时间4h的条件下,对于100mL浓度为100mg/L的氨氮溶液,8g粒径为80~120目的含钛高炉渣对氨氮的去除率可以达到32%;随着温度的升高,去除率基本呈上升趋势;溶液初始pH对氨氮的去除有一定的影响,在碱性条件下有较好的去除效果。     

Determination of silver in irons and steels by atomic-absorption spectrometry with an induction furnace: Direct analysis of solid samples

The silver contents of 17 irons and steels have been determined by dropping 0.5-20mg of millings or turnings of the metals into an induction furnace situated within an atomic-absorption spectrophotometer. The limit of detection was 0.005 mug/g and the relative standard deviations were 12% or better for silver contents of not less than 0.05 mug/g. Samples are added to the furnace at 4-5 min intervals.     

A graphite-tube furnace for use in laser-excited atomic-fluorescence spectrometry

The construction and performance of a graphite-tube furnace for use in laser-excited atomic-fluorescence spectrometry are evaluated. The graphite-tube furnace gives better detection limits than a cup-furnace does for the non-volatile elements.     

Anregung von Spektren durch niederenergetischen Elektronenstoβ mit Anwendung als Lichtquelle für Spektralanalyse

Detection limits of atomic absorption spectroscopy (AAS) and atomic fluorescence spectroscopy (AFS) have been improved by the use of a King furnace. In atomic emission spectroscopy, however, the King furnace was hitherto used only in connection with thermal or RF excitation.The object of this work was to combine the advantages of the King furnace and the advantages of excitation by electron impact for AES. A light source based on a work by Ritschl in 1932 was built. The device consists of a King furnace for sample evaporation. Excitation of atoms is achieved by separate production and acceleration of electrons.The spectrochemical application of this excitation method was tested with Cd, Mg, Hg and B. Detection limits were measured and compared with those attained by other methods. Detection limits are better than those of comparable AES methods using thermal light sources. They compete favourably with those of AAS and AFS using a graphite crucible. The detection limit of Cd, for example, is 3·10^?13 g.The source was applied to determine traces in spectral graphite and to study the transport of material between the electrodes in high-voltage spark.