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DETERMINATION OF MAJOR AND TRACE/TOXIC METALS IN COAL SAMPLES BY ATOMIC ABSORPTION SPECTROSCOPY AND NEUTRON ACTIVATION ANALYSIS 原子吸收光谱法和中子活化分析法测定煤样品中主要和痕量/有毒金属
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002463
M. A. Rauf, M. Ikram, N. Ayub
ABSTRACT Twenty mined coal samples obtained from different areas of Pakistan and six wooden coal samples obtained from local market were analyzed for toxic/trace element concentration by two analytical techniques namely atomic absorption spectroscopy and neutron activation analysis. Seven metals, i.e., Ca, Cr, Fe, Mg, Ni, Pb and Zn were determined by AAS whereas 16 elements namely, Ce, Co, Cr, Cs, Eu, Fe, Hf, Mn, Na, Sb, Sc, Rb, Tb, Th, Yb and Zn were determined by NAA in all samples. Significant concentration of toxic elements such as S, Cr, Fe and Na were observed in mined coal samples, which may pose environmental and engineering/operational problems for thermal power plants.
摘要采用原子吸收光谱和中子活化分析两种分析技术,对巴基斯坦不同地区的20个采煤样品和当地市场的6个木煤样品进行了有毒/微量元素浓度分析。原子吸收光谱法测定了Ca、Cr、Fe、Mg、Ni、Pb、Zn等7种金属,NAA法测定了Ce、Co、Cr、Cs、Eu、Fe、Hf、Mn、Na、Sb、Sc、Rb、Tb、Th、Yb、Zn等16种元素。在采煤样品中观察到S、Cr、Fe和Na等有毒元素的显著浓度,这可能给火电厂带来环境和工程/运营问题。
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引用次数: 8
SIMS INVESTIGATIONS OF GETTERING CENTERS IN ION-IMPLANTED AND ANNEALED SILICON 离子注入和退火硅中捕集中心的SIMS研究
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002459
K. Gammer, M. Gritsch, A. Peeva, R. Kögler, H. Hutter
ABSTRACT High-energy ion implantation in silicon leads to the formation of defects around the mean projected ion range R p. These defects are capable of collecting unwanted impurities like metal atoms. A similar effect has been observed in the depth range around half of the projected ion range, R p/2. This gettering ability around R p/2 is supposed to rely on excess vacancies, generated by the implantation process itself. SIMS is a preferential tool in the detection of gettering centres: If copper is applied at the backside of the sample and trapped in the gettering layers during annealing, enrichments of copper in certain areas can be seen in SIMS depth profiles [1]. If the R p/2-effect was caused by excess vacancies, then one attempt to remove these additional gettering centres would be to implant additional Si atoms which could recombine with the vacancies: In order to test this assumption, three Si+ implanted samples were implanted with additional Si+ ions having a projected range that corresponds to R p/2. After application of copper and annealing, the copper distribution was investigated by SIMS. Furthermore a low-energy-He+-implanted silicon wafer was examined, showing that He+ implantation not only leads to an accumulation of metals but also of oxygen in the R p and R p/2 range.
在硅中注入高能离子导致在平均投射离子范围rp附近形成缺陷,这些缺陷能够收集不需要的杂质,如金属原子。在预计离子范围的一半左右的深度范围内,也观察到类似的效应,即rp /2。这种在R / p/2附近的吸收能力应该依赖于植入过程本身产生的多余空位。SIMS是检测吸垢中心的首选工具:如果在样品背面施加铜并在退火过程中被困在吸垢层中,则在SIMS深度剖面中可以看到某些区域的铜富集[1]。如果R p/2效应是由多余的空位引起的,那么去除这些额外的捕集中心的一种尝试是植入额外的硅原子,这些硅原子可以与空位重新结合:为了测试这一假设,三个Si+注入的样品被注入了额外的Si+离子,其投影范围对应于R p/2。在镀铜和退火后,用SIMS对铜的分布进行了研究。此外,对低能He+注入硅片进行了测试,结果表明He+注入不仅导致金属的积累,而且导致R p和R p/2范围内的氧的积累。
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引用次数: 6
RAPID AND SIMULTANEOUS DETERMINATION OF COPPER, CADMIUM, NICKEL, AND COBALT IN ZINC ELECTROLYTE SOLUTIONS BY COMPLEX ADSORPTION WAVE POLAROGRAPHY 复合吸附波极谱法快速同时测定锌电解质溶液中的铜、镉、镍和钴
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002456
Ming-hao Zhang, Yizeng Liang
ABSTRACT Complex adsorption waves of Cu(II), Cd(II), Ni(II) and Co(II) in substrate solution (pH = 9.0) of diacetyldioxime–ammonia–ammonium chloride–sodium citrate–gelatin–ascorbic acid were studied and a new method for determination of trace amounts of Cu, Cd, Ni and Co in aqueous solutions was developed. The results show that there are sensitive complex adsorption waves of Cu(II), Cd(II), Ni(II) and Co(II) complexes at about −0.44, −0.76, −1.07 and −1.24 V, respectively. The method is easy to operate and able to determine Cu, Cd, Ni and Co in aqueous solutions rapidly and simultaneously, and when the signal-to-noise rates equal 3, the detection limits of copper, cadmium, nickel and cobalt are 1.0 × 10−8, 1.3 × 10−8, 2.9 × 10−10 and 3.6 × 10−11 mol/dm3. Good linear relationships exist between the concentrations and the current peaks when those of copper, cadmium, nickel and cobalt are within 2.0 × 10−8 ∼ 10−5, 3.0 × 10−8 ∼ 10−5, 5.4 × 10−10 ∼ 10−7 and 6.8 × 10−11 ∼ 10−8 mol/dm3, respectively. The method has been used in the rapid and simultaneous determination of these metal ions in complex zinc electrolyte solutions with satisfactory results.
研究了二乙酰二肟-氨-氯化铵-柠檬酸钠-明胶-抗坏血酸底液(pH = 9.0)中Cu(II)、Cd(II)、Ni(II)和Co(II)的络合吸附波,建立了测定水溶液中微量Cu、Cd、Ni和Co的新方法。结果表明:Cu(II)、Cd(II)、Ni(II)和Co(II)配合物分别在−0.44、−0.76、−1.07和−1.24 V左右存在敏感的络合物吸附波;该方法操作简便,能快速同时测定水溶液中的Cu、Cd、Ni和Co,当信噪比为3时,铜、镉、镍和钴的检出限分别为1.0 × 10−8、1.3 × 10−8、2.9 × 10−10和3.6 × 10−11 mol/dm3。当铜、镉、镍和钴的浓度分别在2.0 × 10−8 ~ 10−5、3.0 × 10−8 ~ 10−5、5.4 × 10−10 ~ 10−7和6.8 × 10−11 ~ 10−8 mol/dm3范围内时,浓度与电流峰之间存在良好的线性关系。该方法已用于锌电解液中这些金属离子的快速同时测定,结果令人满意。
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引用次数: 23
KINETIC DETERMINATION OF VANADIUM USING THE BROMATE OXIDATIVE COUPLING REACTION OF 4-(METHYLAMINO)PHENOL WITH 2,3,4-TRIHYDROXYBENZOIC ACID AND TARTRATE ACTIVATOR 4-(甲氨基)苯酚与2,3,4-三羟基苯甲酸和酒石酸盐激活剂溴酸盐氧化偶联反应动力学测定钒
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002458
A. Mohamed, Khalid F. Fawy
ABSTRACT A new, simple, sensitive and selective kinetic method is developed for the spectrophotometric determination of VV and/or VIV based on its catalytic effect on the bromate oxidative coupling reaction of 4-(methylamino)phenol (MAP) with 2,3,4-trihydroxybenzoic acid (THBA) in the presence of tartrate as an activator. The reagents: 6.4 mmol l−1 MAP, 2.0 mmol l−1 THBA and 160 mmol l−1 bromate were mixed in the presence of an activator-buffer solution of 10 mmol l−1 tartrate (pH = 3.10) and at 35°C. The rate of formation of the oxidative coupling product was followed at 380 and/or 570 nm for 3 min from the addition of bromate. Linear calibration graphs up to 0.75 ng ml−1 of vanadium were obtained with detection limits, based on the 3S b criterion, of 0.019 and 0.026 ng ml−1 at 380 and 570 nm, respectively. The developed method was conveniently applied to the determination of vanadium in tap and ground waters and in human plasma, serum, and urine. Moreover, the nature of the oxidative coupling product was inferred and the kinetics and mechanism of the activating effects of tartrate were elucidated.
摘要:本文建立了一种新的、简单、灵敏、选择性的动力学方法,利用VIV在酒石酸盐存在下对4-(甲氨基)苯酚(MAP)与2,3,4-三羟基苯甲酸(THBA)的溴酸盐氧化偶联反应的催化作用,测定VIV和/或VIV的含量。试剂:6.4 mmol l−1 MAP, 2.0 mmol l−1 THBA和160 mmol l−1溴酸盐,在10 mmol l−1酒石酸盐(pH = 3.10)的活化剂-缓冲溶液中,在35℃下混合。在380和/或570 nm下,添加溴酸盐3 min,观察氧化偶联产物的形成速率。根据3S b标准,在380 nm和570 nm处,钒的检出限分别为0.019和0.026 ng ml - 1,得到了0.75 ng ml - 1的线性校准图。该方法可方便地用于自来水、地下水和人血浆、血清、尿液中钒的测定。此外,还对氧化偶联产物的性质进行了推断,阐明了酒石酸盐活化作用的动力学和机理。
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引用次数: 7
TRACE LEVEL REMOVAL STUDIES OF CR(III) FROM AQUEOUS SOLUTION 水溶液中cr (iii)的痕量去除研究
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002465
M. Ikram, M. A. Rauf, N. Rauf
ABSTRACT A flame atomic adsorption method was employed to study the removal of Cr(III) from aqueous solution onto bentonite surface, using the batch equilibrium method. Maximum removal (98.7%) was achieved from a solution of pH 2.5. Effect of various parameters like concentration, shaking time and temperature were also examined to achieve the optimized conditions of maximum recovery of Cr(III) from solution by adsorption method. The presence of various anions and cations on the adsorption behavior of Cr(III) were also investigated. The data was also investigated in terms of calculating thermodynamic quantities and also fitted well to Langmuir's equation.
摘要采用火焰原子吸附法,采用间歇平衡法研究了膨润土表面对水溶液中Cr(III)的去除效果。在pH为2.5的溶液中,去除率最高(98.7%)。考察了浓度、振荡时间、温度等参数对溶液中Cr(III)的影响,确定了吸附法最大回收率的最佳条件。研究了各种阴离子和阳离子的存在对Cr(III)吸附行为的影响。这些数据也在计算热力学量方面进行了研究,并很好地符合Langmuir方程。
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引用次数: 11
APPLICATION OF INSTRUMENTAL NEUTRON ACTIVATION ANALYSIS AND MULTIVARIATE STATISTICAL METHODS TO ARCHAEOLOGICAL SYRIAN CERAMICS 仪器中子活化分析和多元统计方法在叙利亚考古陶瓷中的应用
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002460
E. Bakraji, I. Othman, A. Sarhil, N. Alsomel
ABSTRACT Instrumental neutron activation analysis (INAA) has been utilized in the analysis of thirty-seven archaeological ceramics fragment samples from Tal Al-Wardiate site, Missiaf town, Hamma city, Syria. Thirty six chemical elements were determined. These elemental concentrations have been processed using two multivariate statistical methods, cluster and factor analysis in order to determine similarities and correlation between the various samples. Factor analysis confirms that samples were correctly classified by cluster analysis. The results showed that samples can be considered to be manufactured using three different sources of raw material.
利用仪器中子活化分析(INAA)对叙利亚哈马市米西夫镇塔尔阿尔瓦迪特遗址的37块考古陶瓷碎片样品进行了分析。测定了36种化学元素。利用聚类和因子分析两种多元统计方法对这些元素浓度进行了处理,以确定不同样品之间的相似性和相关性。因子分析证实了聚类分析对样本的分类是正确的。结果表明,样品可以认为是用三种不同的原料来源制造的。
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引用次数: 11
AN APPLICATION OF FAB MASS SPECTROMETRY IN ANALYSIS OF A COMPOSITION OF ATMOSPHERIC WATER fab质谱法在大气水成分分析中的应用
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002464
I. A. Korobeinikova, G. Pronchev, A. Yermakov
ABSTRACT The possibilities of FAB mass spectrometry to analyze the composition of the tropospheric cloud droplets are discussed. As a model for atmospheric water, aqueous solutions of sulfuric acid over a wide range of concentrations were used (10−1 ÷ 10−6 M). The parameters examined were: intensity of positive and negative ions sputtered from the working samples and their dependencies on (H2SO4) or pH measured in aqueous phase. A detection limits of (H2SO4)aq was ∼10−5 M (pH ≤ 5). The correlation observed between the mass spectra and thermodynamic properties of the solutions studied supports the applicability of the proposed approach to quantitative determination of sulfuric acid concentration encountered in atmospheric water.
讨论了FAB质谱法分析对流层云滴组成的可能性。作为大气水的模型,使用了广泛浓度范围内的硫酸水溶液(10−1 ÷ 10−6 M)。检测的参数包括:从工作样品溅射的正离子和负离子的强度及其对水相(H2SO4)或pH值的依赖关系。(H2SO4)aq的检出限为~ 10−5 M (pH≤5)。所研究溶液的质谱和热力学性质之间的相关性支持了所提出的方法对大气水中硫酸浓度定量测定的适用性。
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引用次数: 6
ANALYSIS OF TRACE METALS IN INDUSTRIAL FERTILIZERS 工业肥料中微量金属的分析
Pub Date : 2002-02-28 DOI: 10.1081/TMA-120002462
M. A. Rauf, M. Ikram, N. Akhter
ABSTRACT Industrial fertilizers were used to study selected essential and non-essential metals by two analytical techniques, namely atomic absorption spectroscopy and neutron activation analysis. Out of eight metals namely Pb, Cu, Fe, Zn, Ni, Cd, Mn and Cr, which were determined by atomic absorption technique, Fe showed maximum concentration, whereas Cd and Pb showed minimum value. In the case of neutron activation analysis, 16 elements namely Cr, Fe, Zn, Co, Th, Sc, La, Ba, Rb, Cs, Sb, Yb, Ce, Mn, Na and Eu were analyzed. In this group, Na exhibited maximum concentration value, while Sb and Eu showed the minimum value. Cr, Fe, Zn and Mn were the four commonly studied elements by the two techniques. Within this group, Fe showed the highest concentration values, while the lowest was shown in the case of Cr. The comparison of overall data generally showed lower concentrations of trace metals in nitrogenous fertilizers as compared to potash and phosphatic fertilizers.
摘要以工业肥料为研究对象,采用原子吸收光谱和中子活化分析两种分析技术对选定的必需金属和非必需金属进行了研究。在原子吸收法测定的Pb、Cu、Fe、Zn、Ni、Cd、Mn和Cr 8种金属中,Fe的浓度最高,Cd和Pb的浓度最低。在中子活化分析中,分析了Cr、Fe、Zn、Co、Th、Sc、La、Ba、Rb、Cs、Sb、Yb、Ce、Mn、Na和Eu等16种元素。该组Na浓度最大,Sb和Eu浓度最小。Cr、Fe、Zn和Mn是两种技术常用的四种元素。在这一组中,Fe的浓度值最高,Cr的浓度值最低。从总体数据的比较来看,氮肥中微量金属的浓度一般低于钾肥和磷肥。
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引用次数: 19
HIGHLY SENSITIVE N-(9-ACRIDINYL)MALEIMIDE (NAM) FLUOROMETRY TO DETERMINE SULFITE BELOW PPM LEVEL IN ENVIRONMENTAL AND BIOLOGICAL SAMPLES 高灵敏度n -(9-吖啶基)马来酰亚胺(nam)荧光测定法测定环境和生物样品中低于PPM水平的亚硫酸盐
Pub Date : 2002-01-12 DOI: 10.1081/TMA-120015608
H. Meguro, K. Akasaka, H. Ohrui, S. Matsui
ABSTRACT A highly sensitive fluorometric determination of sulfite in biological and environmental samples is described. Sulfite reacted with N-(9-acridinyl)maleimide (NAM), a Michael addition reaction, to give strongly fluorescent derivatives at temperatures ranging from room temperature to 50°C. There was no interference by the inorganic salts, cations and anions nor by the reducing, oxidizing and organic substances present in wine, beer and blood serum. The sensitivities were in the µM range in the batch methods and in the pmol range when using an ODS column in high performance liquid chromatograpy (HPLC).
描述了一种高灵敏度的测定亚硫酸盐的生物和环境样品的荧光法。亚硫酸盐与N-(9-吖啶基)马来酰亚胺(NAM)发生迈克尔加成反应,在室温至50℃的温度范围内生成强荧光衍生物。无机盐、阳离子、阴离子、葡萄酒、啤酒和血清中的还原性、氧化性和有机物均无干扰。批处理法灵敏度在µM范围内,高效液相色谱法ODS柱灵敏度在pmol范围内。
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引用次数: 3
SIMS STUDY OF THE CALCIUM-DEPRIVATION STEP RELATED TO EPIDERMAL MERISTEM PRODUCTION INDUCED IN FLAX BY COLD SHOCK OR RADIATION FROM A GSM TELEPHONE 冷休克或GSM电话辐射诱导亚麻表皮分生组织产生相关的钙剥夺步骤的SIMS研究
Pub Date : 2002-01-12 DOI: 10.1081/TMA-120015622
M. Tafforeau, M. Verdus, V. Norris, G. White, M. Demarty, M. Thellier, C. Ripoll
ABSTRACT Exposing seedlings of the flax, Linum usitatissimum L., to a variety of weak environmental stresses plus a 2-day calcium deprivation triggers the common response of production of epidermal meristems in the hypocotyl. Here, we show that the same response was induced by a 1 min cold shock. Epidermal meristem production was also induced by a single 2-h exposure to radiation emitted at 0.9 GHz at non-thermal levels by a GSM telephone. This flax-based system is therefore well suited to studying the effects of low intensity stimuli, including those of electromagnetic radiation. To begin to determine the underlying mechanisms, in which calcium is implicated, it is desirable to analyse the changes in ions in the tissues affected. We therefore performed a Secondary Ion Mass Spectrometry (SIMS) study of the distribution of the main inorganic cations in the hypocotyl of control and calcium-deprived seedlings. This showed decreases in calcium, sodium and potassium and an increase in magnesium that did not alter substantially the overall ratio of divalent to monovalent cations.
将亚麻(Linum usitatissimum L.)幼苗暴露在各种弱环境胁迫下,再加上2天的钙剥夺,会引发下胚轴表皮分生组织产生的共同反应。在这里,我们发现同样的反应被1分钟冷休克诱导。在GSM电话发出的非热水平的0.9 GHz辐射下单次暴露2小时,也会诱导表皮分生组织的产生。因此,这种基于亚麻的系统非常适合于研究低强度刺激的影响,包括电磁辐射的影响。为了开始确定潜在的机制,其中涉及钙,它是可取的分析在受影响的组织中的离子的变化。因此,我们对对照和缺钙幼苗的下胚轴中主要无机阳离子的分布进行了二次离子质谱(SIMS)研究。这表明钙、钠和钾的减少和镁的增加并没有实质性地改变二价阳离子与一价阳离子的总体比例。
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引用次数: 42
期刊
Journal of Trace and Microprobe Techniques
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