钯镁基体改进剂对铅,铋,锗在石墨炉中原子化影响的研究

通过原子吸收和X-射线衍射分析证明,加入钯镁基体改进剂在预热处理后对Pb、Bi和Ge三个元素分别生成金属间化合物PbPd_3、BiPd_3、Ge_9Pd_(23)和其他化合物,从而提高了最高允许灰化温度,改变了原子化机理。在原子化阶段这些金属间化合物直接分解为金属原子,结果提高测定灵敏度。     

Sequential determination of platinum, ruthenium, and molybdenum in carbon-supported Pt, PtRu, and PtMo catalysts by atomic absorption spectrometry

A simple accurate and precise analytical method for the determination of platinum, ruthenium, and molybdenum in Pt, PtRu, and PtMo nanoparticles catalysts deposited on high-surface area carbon by flame atomic absorption spectrometry (FAAS) and graphite furnace atomic absorption spectrometry (GFAAS) is described. The complete digestion of samples (0.010-0.020 g), which contain noble metals (NMs) in the range between 0 and 30% in combination among them or with other non-NMs, is obtained under mild conditions using both concentrated HCl and HCl+HNO₃ (1+1 (v/v)) mixture to boiling for 30 min in an open vessel. Carbon is separated from the solution by filtering it. Under optimized conditions of the flame, the poor sensitivity of platinum is enhanced 50-fold in presence of 1% (m V⁻¹) ascorbic acid, whereas the analytical signal of ruthenium increased by the presence of co-existing platinum. Any kind of interference is observed on the analytical signal of molybdenum. Recovery test obtained by analyzing commercial powder catalysts ranged from 99 to 101%. The precision, expressed as relative standard deviation of five measurements, is better than 1%. Electrode catalysts, made by using the carbon-supported platinum-based powder catalysts, have been analyzed for the metal loadings onto the electrode by GFAAS after dissolution under the same conditions used for the powder catalysts. The precision, expressed as relative standard deviation of three measurements, is better than 2%.     

Speciation of Antimony in Leaching Solution in Contact with Plastic by Novel Liquid-Liquid Microextraction and Graphite Furnace Atomic Absorption Spectrometry

A novel, simple, sensitive, and efficient method for the speciation of inorganic antimony by dispersive liquid–liquid microextraction (DLLME) combined with graphite furnace atomic absorption spectrometry (GF-AAS) is reported. The method uses a hydrophobic complex of antimony(III) with a new chelating agent, 1,2,6-hexanetriol trithioglycolate, at neutral pH. The complex was extracted into the organic phase, whereas antimony(V) remained in aqueous solution. The concentration of antimony(V) was obtained by subtracting the antimony(III) concentration from the total antimony concentration following the reduction of antimony(V) to antimony(III) by L-cysteine. The pH, extraction and dispersive solvents and volumes, and concentration of 1,2,6 -hexanetriol trithioglycolate were optimized. Under the optimized conditions, the analytical curve was linear from 0.26 to 3.2 micrograms per liter with a limit of detection of 27.0 nanograms per liter for antimony(III). The relative standard deviation was 6.8 percent at 0.52 microgram per liter antimony(III) with an enrichment factor of twenty-six. The method was employed for the speciation of antimony in leaching solution in contact with plastic; and the recoveries in fortified samples were between 94.2 and 118.0 percent.     

The Determination Of Thallium In Human Hair By Graphite Furnace Atomic Absorption Spectrophotometry

Abstract

An atomic absorption spectrophotometric procedure is des-scribed for the rapid determination of thallium in human hair. Samples of 500 μg are dissolved in nitric acid and treated with hydrogen peroxide. Aliquots of 10 μL are then analyzed using electrothermal atomization in a graphite tube furnace. The characteristic concentration for the method is 1 mg Tl kg^?1 which is adequate for forensic investigation. The relative standard deviation for a series of signals from a hair sample spiked to contain 32 mg Tl^?1 kg was 3 per cent.     

A Simple and Fast Method for Manganese Determination in Antihypertensive Drugs by Slurry Sampling Graphite Furnace Atomic Absorption Spectrometry

Abstract

A simple and rapid procedure for the determination of manganese in anti‐hypertensive drugs is proposed. The samples were treated with dilute nitric acid (1.2% v/v) with stirring using a vortex stirrer to yield a slurry. To determine the best conditions for analysis by graphite furnace atomic absorption spectrometry (GF AAS), a planning factorial was initially employed that demonstrated that the non‐use of chemical modifiers and the use of lower pyrolysis temperatures were more appropriate. Next, the pyrolysis and atomization temperature curves were obtained. The best pyrolysis and atomization temperatures encountered were 500 and 2200°C, respectively. Calibration was performed by matrix matching. The characteristic mass was 0.70±0.14 pg (the recommended mass was 0.60 pg); the limits of detection and quantification were 0.23 and 0.77 µg l^?1, respectively. The precision obtained in the intra‐ and inter‐assay studies of the drug spiked with 0.5, 1.0 and 1.5 µg l^?1 of Mn did not exceed 11% (n=7). Recovery studies of the drug spiked with three levels (n=7) of Mn yielded results between 101.0±4.5 and 116.3±9.7%. The results of an analysis of a certified urine sample (two levels of Mn) agreed at a 95% level of confidence. Forty‐eight antihypertensive drug samples were analyzed, and the results varied from 2.9 ng to 1.9 µg of Mn per capsule^?1.     

Thermal Analysis in Examination of Reduction of Blast Furnace Pellets

This paper presents applications of thermal analysis to observe the course of reduction of acidic pellets, metallurgical substances whose reducibility and strength are basic parameters of use in blast furnace processes. Both parameters depend on the mineral composition of the samples. The investigations included determination of the chemical and phase compositions of the initial samples and reduction products. Research was conducted on acidic pellets from Połtawa (Poland), applied in the T. Sendzimir Steelworks (Poland), in comparison with pellets from Brazil, Canada and Lebedyn (Russia). This revised version was published online in August 2006 with corrections to the Cover Date.     

固相萃取-石墨炉原子吸收法光谱分析铝合金中痕量铍的研究

建立了固相萃取-石墨炉原子吸收光谱法测定铝合金中铍的方法。利用偶氮砷酸类试剂7-(2′-胂酸基-5′-羧酸)苯偶氮-8-羟基喹啉-5-磺酸(H2L)与Be2+形成螯合物,该螯合物可用C18固相萃取柱富集,而Al3+则不被保留。采用石墨炉原子吸收光谱法(GF-AAS)测定C18柱洗脱液中的Be2+的螯合物,从而实现铝合金中铍的分离检测。最佳实验条件为:采用pH=3.0的5%H2L水溶液螯合Be2+,水相上柱,用2mL体积比为50%的甲醇/水溶液作为洗脱液。结果表明:经过C18柱固相萃取可以去除Al3+的干扰,Be2+的测定范围为0.05～16μg/L,检出限为0.025μg/L,加标回收率为92%～108%。应用该法于铝合金标样中铍的测定,结果与认定值相符。     

配煤燃烧过程中煤灰熔融性研究

采用灰熔点较低的神华煤和较高的准格尔煤以及这两种煤组成的混煤在沉降炉内进行实验,模拟实际电站锅炉内结渣的形成过程。采用SEM、XRD技术对煤粉和灰渣的微观形貌和晶相成分进行分析。结果表明,准格尔煤粉中包含的大量高岭石和勃姆石为莫来石的大量生成提供了条件,神华煤中不含勃姆石,高岭石的含量也不多,莫来石的生成量很少。莫来石在高温下遇到石灰石的分解产物CaO,要与之反应生成钙长石,这是神华煤灰渣中没有检测到莫来石衍射峰的主要原因。莫来石是一种高熔点矿物（1850℃）,能显著改善煤灰的熔融温度,神华煤灰渣中不含莫来石,灰渣中缺少大量能在其熔融过程中发挥“骨架”作用的成分,这是导致神华煤灰熔融温度较低的一个重要原因。     

浊点萃取-石墨炉原子吸收光谱法测定环境样品中的镉

建立了浊点萃取分离富集石墨炉原子吸收光谱法测定环境样品中痕量镉的方法.浊点萃取选择8-羟基喹啉为螯合剂,Triton X-100为表面活性剂.在pH 8～9、0.01%8-羟基喹啉和0.2%-Triton X-100、80 ℃水浴20 min的优化条件下,所建立方法的检出限为2.5 ng/L; 加标回收率为94.6%～106.2%; 对样品溶液进行富集的富集因子为17.利用该方法分别测定了2个实际水样和2个国家标准参考物质中的总镉含量,结果令人满意.     

Factors affecting the combustion toxicity of polymeric materials

Fire gas toxicity is an essential component of any fire hazard analysis. However, fire toxicity, like flammability, is both scenario and material dependent. A number of different methods exist to assess the fire toxicity, but many of them fail to relate this to a particular fire scenario. Sample thickness alone, in a closed box test such as the NBS Smoke Chamber, is shown to change the fire scenario from well-ventilated to under-ventilated. Data from two flow-through tests, the static tube furnace (NF X 70-100) and the steady state tube furnace (the Purser furnace, BS 7990 and ISO TS 19700) show that there are different patterns of behaviour for different polymers (LDPE, polystyrene, rigid PVC and Nylon 6.6). The predicted toxicities show variation of up to two orders of magnitude with change in fire scenario. They also show change of at least one order of magnitude for different materials in the same fire scenario. Finally, they show that in many cases CO, which is often assumed to be the most, or even the only toxicologically significant fire gas, is of less importance than either HCl, or HCN, when present, and in some cases less important than organo-irritants. Nylon 6.6 shows the highest predicted toxicity, the greatest scenario dependence, and the least sensitivity to different apparatuses, while polystyrene shows the highest sensitivity to the different apparatuses, but the lowest to different fire scenarios. PVC shows high toxicity, mostly due to HCl in the fire effluent, under all fire conditions, and LDPE shows a more progressive increase in toxicity from well-ventilated flaming to both smouldering and under-ventilated flaming.