Neutron activation analysis of petroleum feeds and products of a catalytic cracking unit

Na, Al, S, Cl, V, Mn, Ni, As, Br, I, La, Eu and Dy were determined in 2 feeds and 5 products of a catalytic cracking unit. Catalysts used in this unit were also analyzed and 18 elements were measured in this matrix. The overall mass balance of the unit was calculated and it was shown that the concentrations of most elements are reduced during cracking but the concentrations of some others (Al, Dy, Eu and La) are increased.     

Determination of 18 trace elements in petroleum and its derivatives by neutron activation with a small nuclear reactor

Non-destructive neutron activation has been used to analyze 6 different samples of crude oil and heating oil, from Western Canada and Venezuela. These samples were irradiated with thermal neutrons for 2, 30 and 240 min in the SLOWPOKE reactor and the concentrations of 18 trace and minor elements (Al, As, Br, Cl, Co, Dy, Eu, Fe, I, La, Mn, Mo, Ni, Na, S, Se, Sm and V) ranging from 0.6 ppb to 2.24% have been measured. Eleven elements (As, Br, Co, Cl, Fe, Mo, Mn, Na, Ni, S and V) were determined in the fuel oil (SRM-1634) obtained from the National Bureau of Standards and were found to be in good agreement with the values certified by NBS     

电感耦合等离子体-发射光谱分析中硫酸基体效应及抑制

研究了电感耦合等离子体-发射光谱分析中的硫酸基体效应及克服干扰的有效方法。对2%~20%范围内4种不同体积分数H2SO4溶液中30种元素的基体效应进行了观察,发现H2SO4对各元素的谱线发射强度均存在明显的抑制作用。实验证实体积分数5%乙酸可有效抑制H2SO4的基体效应,并建立了H2SO4溶液中痕量元素的电感耦合等离子体-发射光谱分析法。     

Nuclear Activation Methods in the Estimation of Environmental Pollution and the Assessment of the Industrial Plant Impact on the Citizens of Gdansk (Poland)

Neutron Activation Analysis (NAA) is a sensitive analytical technique useful for performing both qualitative and quantitative multi-element analysis of major, minor, and trace elements in samples from almost every conceivable field of scientific or technical interest. The NAA method was applied to estimate the atmospheric air quality assessment based on the analytical investigation of rainwater composition in comparison to a moss biomonitoring study performed in selected urban areas of Gdańsk, Poland, during the half-year of exposure. The main objectives of this project were: comparison of dry and alive moss abilities to bioaccumulate inorganic pollutants; and, detection and identification of natural and anthropogenic pollutant sources in this region. An impact of Gdansk Phosphatic Fertilizer Plant “Fosfory,” Poland, on occupational staff and citizens living near the plant has also been examined. The elements, Al, As, Au, Br, Ca, Cl, Cu, Dy, I, In, K, La, Mg, Mn, Mo, Na, S, Sb, Sm, U, V, and Zn, have been determined by instrumental neutron activation analysis (INAA) in the indoor workplace air; in urine, hair, and toenails collected from workers and persons living in a neighborhood near the plant; and from people from the control group not connected with the plant in any way. Analyses of hair and nails was performed at the Interfaculty Reactor Institute in Delft, The Neatherlands, at a 2MW swimming-pool nuclear reactor and at the Joint Institute for Nuclear Research, Dubna, Russia. The essential differences in concentrations of elements for workers and control group were evaluated using non-parametric Mann-Whitney U-tests. Significant differences between workers/citizens of the factory neighborhood and the control group were found for some elements (i.e., Mg, Sb, S, and V), but in the base of these differences, it is hard to define if the factory impact exists. An impact of Federeal-Mogul BIMET S.A. in Gdansk, the biggest manufacturer of slide bearings in Poland, on occupational staff has been also examined. The concentrations of Cu and Pb are much higher in samples taken from workers then from the control group. These results also indicated that hair and toenail samples are useful in the evaluation of that impact. Workers of the slide bearing factory are occupationally exposed to elements, which can be harmful to their health.     

Trace element determinations in shale oil products by neutron activation

Neutron activation offers some important advantages for the determination of selected trace elements in shale oil products. This paper gives techniques and results of a study of crude shale oil and naphtha, heavy distillate, and wax products of shale oil. The elements determined were Al, As, Au, Br, Ce, Cl, Co, Cr, Fe, Hg, I, K, Mn. Mo, Na, S, Sb, Se, V, and Zn. Some elements (Mn, Na, As) tend to accumulate in heavier fractions, whereas chlorine and iodine are concentrated in the more volatile fractions. The volatility of sulphur compounds in the shale oil products appears to be essentially uniform, with some tendency toward accumulation in distillation residues. The tendency for the trace elements to accumulate in the waxes that precipitated from cooled heavy distillates was very low.     

Cluster analysis of elemental constituents of individual atmospheric aerosol particles from the volcanic plume of Lonquimay eruption in 1989

Aerosol samples collected around the Chilean site Lonquimay during major volcanic activities in January 1989 have been subjected to microPIXE measurements of 1 mm lateral resolution in the Debrecen Institute. Elemental concentrations relative to calcium have been determined for Al, Si, P, S, K, Sc, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, and Ba in 187 individual aerosol particles with the particle sizes between 15 mm and 1 mm. On the basis of a cluster analysis performed on the data set we defined eight clusters. Scatter plots for selected pairs of elements as Si/Al, K/Si, S/Cl, and Al/S elemental ratios that are considered as signatures characterizing types and mechanisms in volcanic eruption - have been compared with published data available in the literature for various volcanic sites.     

Aluminum orthovanadate (AlVO4): synthesis and characterization by (27)Al and 51V MAS and MQMAS NMR spectroscopy

Polycrystalline samples of AlVO(4) have been prepared by two methods of synthesis and characterized by (27)Al and (51)V MAS NMR spectroscopy at 14.1 T. The MAS NMR spectra clearly reveal that essentially pure samples with minor impurities of V(2)O(5) and alumina have been obtained. From these samples, (27)Al quadrupole coupling parameters and isotropic chemical shifts as well as the magnitudes and relative orientations of the (51)V quadrupole coupling and chemical shift tensors have been determined with high precision for AlVO(4). These data have been obtained from a combined analysis of multiple-quantum (MQ) MAS NMR spectra and MAS NMR spectra of the central and satellite transitions. The (27)Al and (51)V NMR data show that the asymmetric unit for AlVO(4) contains three isolated VO(4) tetrahedra, one pentacoordinated Al site, and two AlO(6) octahedra. This is in agreement with the supposition that AlVO(4) is isostructural with FeVO(4) and with a recent structure refinement for AlVO(4) based on powder X-ray diffraction (XRD) data. The favorable agreement between the refined crystal structure from powder XRD and the NMR parameters is apparent from a convincing correlation between experimental (51)V quadrupole tensor elements and calculated (51)V electric field gradient tensor elements obtained by the point-monopole approach. An assignment of the (27)Al NMR data is obtained from similar calculations of the (27)Al electric field gradients and by estimation of the distortion of the AlO(6) octahedra.     

Redistribution of Metal Concentrations in the Products of Microwave Discharge in Liquid Residues of Heavy Petroleum Feedstock

Microwave discharges in liquids represent a new direction in plasma physics and chemistry. Results of experiments on the recovery of metals from a liquid residue after vacuum distillation of the hydroconversion product of vacuum tower bottoms by treating the residue with microwave discharge initiated in its bulk at atmospheric pressure are presented. It has been found for the first time that the concentrations of Al, Co, Cu, Fe, Mo, Ni, V, and Zn metals in a treelike structure deposited on a microwave antenna are 10–20 times their concentrations in the substrate.     

由特殊相互作用导致的高分子间的络合Ⅸ.聚(苯乙烯-co-4-乙烯基苯酚)/聚(苯乙烯-co-4-乙烯基吡啶)在本体中的相容-络合行为

采用结合物理老化技术的示差扫描量热法（ Ｄ Ｓ Ｃ） 以及非辐射能量转移荧光光谱法（ Ｎ Ｒ Ｅ Ｔ） 研究了聚（ 苯乙烯 ｃｏ ４ 乙烯基苯酚） （ Ｓ Ｔ Ｖ Ｐｈ） 与聚（ 苯乙烯 ｃｏ ４ 乙烯基吡啶）（ Ｓ Ｔ Ｖ Ｐｙ） 共混体系在本体中的相容与络合行为．当 Ｓ Ｔ Ｖ Ｐｈ 中 Ｏ Ｈ 含量为３ ,６ ,９ ｍ ｏｌ ％ 时,可以分别与吡啶基含量是２５ ,５０ ,７５ ｍｏｌ ％ 的 Ｓ Ｔ Ｖ Ｐｙ 实现相容, Ｏ Ｈ 含量更高时还可进一步形成络合,表现为远较 Ｆｏｘ 方程预示值高的 Ｔｇ 和窄的转变温度区间．此外,还讨论了浇膜溶剂对相容与络合的影响     

Elemental characterization of TSP and two size fractions of airborne particulate matter from Tehran by INAA and AAS

Airborne particulate matter has been collected by a high volume and a Gent-type stacked filter unit (SFU) low volume sampler during the 2000-2001 period. The high volume sampler used S&S cellulosic and the SFU two Nuclepore polycarbonate filters to collect fine and coarse size fractions. The elemental analysis of the collected TSP, fine and coarse particles has been performed using instrumental neutron activation analysis and atomic absorption spectrometry. Twenty-two trace elements on Nuclepore and twenty-four elements on S&S filters have been measured. The collected data have been compared with the previous data of Tehran air and with other cities in the world. This revised version was published online in July 2006 with corrections to the Cover Date.     

Elemental analysis of airborne fine particles collected at the roadside of an arterial road

Airborne particulate matter was collected at the intersection of Industrial Road in Kawasaki-city, Kanagawa, Japan using a 12-stage low-pressure impactor. High concentrations of airborne particulate matter have been observed in this area. The collected samples were analyzed for 34 elements by instrumental neutron activation analysis (INAA), and data on the elemental concentrations were obtained. High concentrations of fine particles of As, Br, Sb, V, and Zn were observed. It was further observed that these fine particles were originated predominantly from the wear of tires and brakes, and not from automobile exhaust emissions.     

Heavy metals content in rain water collected in three different locations in Italy during 1999

Rain water samples collected at three different locations in Italy during 1999 were analysed for heavy metals determination. Results for V, Cr, Mn, Co, Cu, Cd, Sb, Pb, Al and Ni are reported in this paper. For most of the elements higher concentration values have been measured in the samples from Alpe Gera (rural site): only for Cd and V were the concentrations higher at Pisa. The total annual deposition (microg m(-2) y(-1)) shows a similar behaviour, with Alpe Gera being the location with highest total annual input for Cr, Mn, Co, and in particular for Cu, Sb, Pb and Al. The reason of the higher deposition at a rural site in comparison to a urban one (Milan) is not known: further experimental work and investigations are needed. Generally, no evident seasonal trends have been observed for the measured concentrations, while few correlations have been found among elements within the same station. Crustal contribution to total concentration varies from about 20% for V to less than 1% for Cu, Cd, Sb, Pb and Ni.     

Modeling and analysis of vacuum membrane distillation for the recovery of volatile aroma compounds from black currant juice

A vacuum membrane distillation (VMD) model has been developed and validated with experimental data. The model consists of an extended transport model for the VMD process and is able to predict the effects of concentration and temperature polarization on the overall process performance. To validate the model, first it was tested with few experimental case studies from literature [S. Bandini, G.G. Sarti, Heat and mass transport resistances in vacuum membrane distillation per drop, AIChE J. 45 (7) (1999) 1422–1433; K.W. Lawson, D.R. Lloyd, Membrane distillation. I. Module design and performance evaluation using vacuum membrane distillation, J. Membr. Sci. 120 (1996) 111–121; A.M. Urtiaga, G. Ruiz, I. Ortiz, Kinetic analysis of the vacuum membrane distillation of chloroform from aqueous solutions, J. Membr. Sci. 165 (2000) 99–110]. Then the VMD model has been validated with experimental data collected from the recovery of aroma compounds from black currant [R.B. Jørgensen, A.S. Meyer, C. Varming, G. Jonsson, Recovery of volatile aroma compounds from black currant juice by vacuum membrane distillation, J. Food Eng. 64 (2004) 23–31]. In this work, recovery of 12 characteristic volatile aroma compounds from black currant juice has been studied. The simulated results from the VMD model, in terms of aroma concentration in the permeate have been compared with those obtained from laboratory experiments. The validated model has been used to study the effects of various process and membrane parameters on the concentration factor. The physical properties of various aroma compounds have been predicted using group contribution method as a function of temperature.     

Methode de mesure de la periode d'un corps radioactif et applications

The authors propose a function describing a curve taken on a multiple-stage instrument. This function depends on three parameters; the time, the half-life, and the initial dead-time. The latter has been measured accurately on an electronic unit developed for this purpose. The half-lives of certain elements (Hf, Ag, Se, Na, V, Sc, Al) have been determined and the differences in the half-lives of an element and its salt have been pointed out.      

Short-term and spatial variation of selected metals in the atmosphere of Niterói City, Brazil

In this work, the atmospheric concentration of selected trace elements (Cd, Fe, Mn, Pb, V and Zn) was determined in total suspended material (TSP) from three sampling sites located at Niterói, an urban medium city of Rio de Janeiro, Brazil. TSP samples were collected with a high volume air sampler and glass fibber filters. The determinations of Cd, Pb and Zn were performed by ICP-AES while V was determined by ETA-AAS and Fe and Mn were measured by FAAS. Among all elements, Fe showed the highest concentrations (0.5-12.5 μg/m³) during the study but the concentrations of all elements varied along the week. The maximum levels of TSP, Fe, Mn, Cd and V were observed on Wednesday which was characterised by the highest winds frequency with higher speeds coming from the North quadrant, mainly from the Northeast direction. Enrichment factors showed that Cd, Pb and Zn are enriched in all sites suggesting that anthropogenic sources play important roles for those elements. Statistical analysis has been carried out to evaluate the effect of meteorological parameters and characterisation of sampling sites.     

Rapid determination of sulfide in waste waters by continuous flow analysis and gas diffusion and a potentiometric detector

The continuous-flow system is based on a flow-through gas diffusion unit and a potentiometric detection with sulfide-selective electrode. The sampling rate is about 15 h^?1. In the 0.5–600 mg l^?1 sulfide range, the mean slope of the response is 30.2 ± 0.3 mV per decade. The percentage transference of H₂S across the teflon membrane is 48 ± 1%. Up to sample concentrations of 50 mg l^?1 sulfide, results agree well with those obtained by a distillation method. Sample storage is discussed.     

Effects of combined substitution of Dy and Mo or Si on the crystal structures and magnetic properties of Nd_(1-y)Dy_yFe_(11-x)TiM_x(M=Mo,Si) compounds

A series of Nd1-yDyyFe11-xTiMx(M=Mo,Si) alloys have been prepared by arc melting and studied by X-ray diffraction and neutron diffraction.All samples are found to crystallize in the ThMn12-type structure.The lattice parameters a and c and unit cell volume V of Nd0.5Dy0.5Fe11-xTiMox alloys increase linearly with increasing content of Mo(x),while the lattice parameters a and c and unit cell volume V of Nd0.5Dy0.5Fe11-xTiSix alloys decrease linearly with increasing content of Si(x).In NdyDy1-yFe11-xTiMx(M=Mo,S...     

出生缺陷高发区人发元素含量分析研究

目的:寻找出生缺陷高发区病人体内含量异常的元素,为出生缺陷的干预和治疗提供理论依据。方法:在病区分别采集有出生缺陷儿童和健康儿童头发样品,经预处理后,采用ICP-电感耦合等离子发射光谱法,对16种元素进行了测定,所得数据采用SPSS 10.0进行非参数检验和多元回归分析。结果:与健康儿童头发样品相比,患儿发中Mo,Zn,Sr,Fe,Mg,Ca等含量显著偏低,V偏高;以病情为因变量,发中16种元素含量为自变量经逐步回归分析,有Mo,Zn,Ni等进入方程。提示该区病人体内Mo,Zn等含量低、Ni含量高与病情有关。结论:Mo,Zn等在人体内的缺乏可能是出生缺陷发生的重要因素,Sr,K,Cu,Sn,Mg,Se,Fe,Ca等含量偏低及V含量偏高可能与Mo,Zn,Ni等共同起到协同致病的作用。     

广州市夏、冬季室内外PM2.5中元素组分的特征与来源

通过采集广州市9个居民住宅室内、外的PM2.5样品,测定分析PM2.5中18个元素组分的质量浓度,分析讨论其污染、分布特征并解析其污染来源。经过比较得知,广州市PM2.5中元素污染较严重;不同类型住宅PM2.5中元素浓度存在空间分布特征;大部分元素浓度具有夏季比冬季低的变化特征;室内与室外元素浓度比值介于0.4974～2.0497之间;元素浓度的室内、室外相关拟合结果说明冬季室内空气受室外空气影响比夏季时情况更明显;基于富集因子分析,Se、As、S、Pb、Br、Zn和Cl元素高度富集;Ni、V、Cu元素中等富集,主要来自人为源,而Cr、Sr、K、Mn、Ca和Ti元素不富集,主要来自自然源。     

Comparative instrumental multi-element analysis I: Comparison of ICP source mass spectrometry with ICP atomic emission spectrometry, ICP atomic fluorescence spectrometry and atomic absorption spectrometry for the analysis of natural waters from a granite region

Summary Multi-element analysis by ICP source mass spectrometry for practically matrix-free natural waters, coming from a granitic area and, therefore, rich in trace elements, has been compared with ICP-atomic emission, ICP atomic fluorescence and atomic absorption spectrometry. The following elements have been investigated and their concentrations are in the decreasing order: Ca, Si, Na, Mg, K, Al; Sr, Mn, Ba, Fe, Rb, Zn, B, U, Y, Li, La, Be, Cs, Co, Cr, V, Sb, Bi, Th, Cu, Cd, Ni, Se, Pb, As, Hg, Mo, Tl, Sn. The concentration ranges were between 10 ppm and <0.01 ppb.As a measure of agreement between the different methods under investigation, two criteria have been used (a) the relative variation coefficient VK (%) of the mean element concentration of an element, determined by different methods in all the 98 water samples and (b) the linear, logarithmic and Spearman rank correlation coefficients between ICP-MS and each of the other methods. Detection limits are given from literature for about 32 elements using different methods.The elements Ca, Na, Mg, K, Mn, Sr, Zn, Fe, Li, Cu have been determined with ICP-MS, ICP-AES and AAS; Al, Ba with ICP-MS and ICP-AES; Si only with ICP-AES, whereas B, Be, Bi, Co, Cr, Cs, Hg, La, Mo, Ni, Pb, Rb, Sb, Sn, Th, Tl, U, V, Y only with ICP-MS. In all 34 of the investigated 36 elements could be analysed by ICP-MS, 14 (from about 20 possible) by AAS, 13 by ICP-AES and 12 by ICP-AFS.The agreement between ICP-MS and ICP-AES as well as between ICP-MS and AAS in most cases is remarkably good according to (a). VK (%) for each element in 98 water samples is in the range from ±2.6 to 10% for Na, Mg, Ca, K, Fe, Sr, Ba, Cu, Li (increasing order). Cd and Zn have unexpectedly higher values (±17.3 and ±20.5%); Cd concentrations are, however, near the detection limit.Comparing the different methods on the basis of correlation coefficients according to (b), gives for the Spearman rank correlation coefficient over the whole range of concentrations, respectively for ICP-MS/ICP-AES, AAS, ICP-AFS in case of Ca: 0.998; 0.984; 0.899; Na: 0.993; 0.991; 0.978; Mg: 0.997; 0.993; 0.959; K: 0.986; 0.942; 0.677; Al: 0.987; -; -; Fe: 0.864; 0.974; 0.701; Mn: 0.989; 0.990; 0.198; Sr: 0.988; 0.992; -; Zn: 0.894; 0.819; 0.300; Cu: -; 0.977; 0.202; Li: -; 0.907; 0.586.It is evident from these trace element concentrations as well as the electrical conductivities, that only about three fourths of the investigated samples are typical granitic waters and the remaining ones are associated with different geological background. The samples have been mainly radon waters with more than 18 nCi/l of Rn-222.

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Vergleichende Instrumentelle Multielementanalyse I: Vergleich von ICP-Massenspektrometrie mit ICP-Atomemissionsspektrometrie, ICP-Atomfluorescenzspektrometrie und Atomabsorptionsspektrometrie zur Analyse natürlicher Wässer aus einem Granitgebiet

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6th Contribution to the principles of trace analysis of elements and radionuclides

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Dedicated to Professor Dr. H. Kelker, Frankfurt, on the occasion of his 65th birthday