Determination of boron in amorphous and nanostructured soft magnetic alloys,ribbons and layered materials by ICP atomic emission spectrometry

Optimum conditions for the accurate determination of B in amorphous or nanocrystalline soft magnetic Fe and Co base alloys (ribbons), boride coated powders and other materials by ICP atomic emission spectrometry are worked out. The spectral interferences of the 3 most prominent B emission lines caused by the matrix elements Fe, Co and Ni and the enhancement of the B blank values by a memory effect are investigated. Using a well-suited line fitted to the sample matrix and a special measuring regime including frequent recalibrations by an external standard, the total error of the analytical method could be reduced to 0.02% at B contents of 1 to 5% (w/w).     

电感耦合等离子体原子发射光谱(ICP-AES)法测定NiCrAlYSi合金中铝、硅、铁、钴、钛

用盐酸、硝酸及氢氟酸溶解样品,采用基体匹配法配制标准溶液系列以消除基体效应的影响,选择Al 394.401nm、Si 251.611nm、Fe 259.940nm、Co 238.892nm、Ti 337.280nm为分析线,使用电感耦合等离子体原子发射光谱(ICP-AES)法测定NiCrAlYSi合金中的铝、硅、铁、钴、钛。Al的质量分数在0.10%~15%、Si的质量分数在0.01%~6.0%、Fe、Co、Ti的质量分数在0.005%~0.50%时,各元素质量分数与对应的发射强度呈线性,线性相关系数不小于0.999 5;方法中各元素检出限为0.0005%~0.0020%;结果的相对标准偏差为0.46%~3.7%;加标回收率为90.0%~104%。方法简单、快速,结果令人满意。     

马氏珠母贝各部位及其插核珍珠层微量元素的含量及分布

用电感耦合等离子体发射光谱仪检测了马氏珠母贝5个部位及其人工插核珍珠层中的11种微量元素的含量。结果表明,人工插核珍珠层中Se、Si、Zn含量,角质层中B、Co、Fe、Mn含量,内脏囊中P含量,闭壳肌中Cu、Cd含量,人工插核珍珠层、角质层、闭壳肌中V含量较其他部位高;各部位w(Cu)/w(Zn)均小于0.50,其中人工插核珍珠层的w(Cu)/w(Zn)特别小,为0.05。为进一步加工利用和揭示其药用价值提供基础信息。     

Synthesis of Nano-catalysts by Induction Suspension Plasma Technology (SPS) for Fischer–Tropsch Reaction

Nanometric catalysts were synthesized through induction suspension plasma technology (SPS) for application in the Fischer–Tropsch synthesis (FTS). Carbon-supported single metal catalysts (Co/C, Fe/C), bimetallic formulations (Co–Fe/C), and ternary (Co–Fe–Mo and Co–Fe–Ni) systems have been considered in this work. SPS has been selected because it simultaneously allows for: (1) atomizing and generating metallic nanoparticles; (2) creating particularly Fe carbides, which are important in Fe-based FTS reaction mechanism; (3) in situ production of the nanometric graphitic-carbon matrix; and (4) saving time in catalyst synthesis, limiting sample preparation steps and eliminating post synthesis treatment before use. Porosity measurements by the Brunauer–Emmett–Teller method indicate that the samples are essentially non-porous. The synthesized catalysts characterized by X-ray Diffraction analysis show the presence of both metallic and carbidic species. The graphitic-carbon matrix has substantial structural defects that make it partly amorphous. Scanning Electron Microscopy analysis coupled with Energy Dispersive X-ray Spectroscopy mapping shows uniform dispersion of the metal moieties in the carbon support. Analysis by Transmission Electron Microscopy imaging displays metal nanoparticles with mean particle size within the 9–15 nm range enveloped in the carbon matrix.     

Effects of the host matrix on the 57Fe-species produced through EC-decay in 57Co-labelled tris(phenanthroline) cobalt (II) perchlorate.

Emission M?ssbauer spectroscopic studies of 57Co-labelled [Co(phen)3]clO4)2 in host matrices [M(II)(phen)3](ClO4)2(M=Co, Fe, and Ni) indicate that the relative intensities of the anomalous species produced through the EC-decay depend on the kind of the host matrix. The largest intensity was observed with the cobalt (II) matrix, and the smallest with the iron (II) matrix. Emission spectra of 57Co-labelled [Co(2-CH3-phen)3](ClO4)2 2H2O in the matrix of [Fe(2-CH3-phen)3](ClO4)2 were also studied. The high-spin state (5T2) was predominantly observed at 4.2 K in the emission spectrum, while the low-spin state (1A1) was mainly observed in the absorption spectrum at 78 K. The results are discussed in terms of the stability of the lattice.     

仙人掌果汁红色素含量测定与微量元素分析

用可见分光光度法与等离子体发射光谱法对仙人掌果汁色素及其微量元素的含量进行了测定，仙人掌果汁色素含量达２．１％￣３．３％，成熟果的果汁色素含量比预成熟果大。在２７种被测定的元素中，除Ａｓ、Ｂｅ、Ｃｄ、Ｃｏ、Ｍｏ、Ｐｂ，Ｓｂ，Ｔｌ等未被检出外，其余Ａｇ，Ａｌ，Ｂ，Ｂａ，Ｃａ，Ｃｒ，Ｃｕ，Ｆｅ，Ｍｇ，Ｍｎ，Ｎａ，Ｎｉ，Ｓｅ，Ｖ，Ｚｎ，Ｋ，Ｐ，Ｓ等均有准确测定值。成熟果与预成熟果的果汁微量元素含量无明显     

An integrated approach to the complete chemical analysis of magnesium or sodium diuranate (yellow cake) sample

A procedure for the complete chemical analysis of magnesium or sodium diuranate (yellow cake) sample is reported. Uranium is determined gravimetrically after peroxide precipitation. Optimum parameters, such as pH, quantity of hydrogen peroxide, volume of sample, temperature and complexing agent for quantitave precipitation of uranium, and effective separation of other elements were studied. Aluminum, Ca, Cd, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni, Pb, and Zn were determined by flame atomic absorption spectrometer and B, Mo, SO₄, REEs and Y by inductively coupled plasma atomic emission spectrometer in the filtrates of hydroxide and peroxide precipitation separation. The proposed method is accurate and the precision is characterized by an RSD of ~0.2% for U; 2 to 6% for Mg, Na, K, Ca, Fe, SiO₂, Al, Cd, Co, Cr, Fe, Mn, Ni, Pb, and Zn and 3 to7% for REEs, Y, Mo and B     

Preparation of poly(acrylonitrile-co-methyl acrylate)/cellulose composite membranes and their application in wastewater treatment

In this study, new poly(acrylonitrile-co-methyl acrylate)/cellulose composite membranes were prepared firstly and then characterized. Then they were used in the removal of Fe(III) and Co(II) ions from wastewater with a stirred ultrafiltration cell. Also, alginic acid polymer was used as complexing agent to enhance the retention. In the filtration of Fe(III) and Co(II) solutions, the effects of pH, concentration of solutions, and pressure on the retention percentage were examined. Aqueous solutions of Fe(III) and Co(II) were filtrated at the stirred velocity of 400?rpm. The maximum retention percentage was found as 78.66% for Fe(III) solution at the pH of 3.3, concentration of 0.3?×?10^?4 M Fe(III) solution, pressure of 40?psi by using 2.5 (w/v)% Poly(acrylonitrile-co-methyl acrylate)/cellulose composite membranes. For Co(II) solutions the maximum retention percentage was found as 77% at the pH of 6, concentration of 0.3?×?10^?4 M Co(II) solution, pressure of 50?psi by using 2.5 (w/v)%Poly(acrylonitrile-co-methyl acrylate)/cellulose composite membranes.     

Isotachophoretic separation behavior of rare-earth EDTA chelates and analysis of minor rare-earth elements in an iron ore by bidirectional isotachophoresis-particle-induced X-ray emission.

Mobilities of 16 anions of rare-earth-EDTA 1:1 chelate (RE-EDTAs) were isotachophoretically measured by using two leading electrolytes (pH 3.6 and 6.0) in order to assess their separation behavior. The leading electrolyte was 20 mM hydrochloric acid. The pH of the solution was adjusted to 3.6 by adding beta-alanine and to 6.0 by adding histidine. The obtained mobilities were very close to each other in the range 20.1x10(-5)-21.9x10(-5) cm2 V(-1) s(-1) with the minimum mobilities for Pr-EDTA and Nd-EDTA for pH 3.6 and 6.0, respectively, and pH dependence was hardly observed. On the basis of the above knowledge. minor rare-earth elements in a standard iron ore sample were determined as RE-EDTAs by bidirectional isotachophoresis-particle-induced X-ray emission (PIXE), where the Fe(II) matrix digested by alkali fusion was separated as Fe(II)Phen3(2+) (phen = 1,10-phenanthroline). Since 5% of the total iron was still detected as Fe(III)EDTA- and might disturb PIXE analysis of RE-EDTA-, itaconic acid was used as the spacer for Fe(III)EDTA- and RE-EDTA-. The fractions of RE-EDTA- were successfully analyzed off-line by a multielemental analytical method, PIXE [analytical result (3.62% (w/w) as RE2O3]; the nominal value was 3.37% (w/w) as RExOy.     

The application of butanol as dilution agent for the inductively coupled plasma-atomic emission spectrometric determination of boron and phosphorus in lubricating oils

An evaluation of butanol-1 as dilution solvent for the determination of boron (B) and phosphorus (P) in lubricating oils by inductively coupled plasma-atomic emission spectrometry (ICP-AES) has been performed. Standard solutions of boric acid and tri-n-butyl phosphate (TBP) in butanol were employed as calibrants for B and P, respectively. Solutions of phosphoric acid and tris(2-ethylhexyl)phosphate (TEHP) in butanol were also tested as possible P standards. Increased concentrations of oil in the sample in the range of 0 to 20% showed no significant effects on B and P emission intensities indicating that matrix matching is not required for lubricating oils of about 2–15 cPoise. Detection limits in absence of spectral interferences were 0.06 μg B/g oil and 2 μg P/g oil. Overall estimated precision was 2.5% for B concentrations above 4 μg/g oil, and 6.5% for P concentrations above 20 μg/g oil. We evaluated the performance of a high resolution scanning spectrometer for mitigating the effects of overlapping spectral interferences from iron (Fe) and copper (Cu) on B and P emission lines. An interference from Fe 249.782 nm on the primary B line at 249.773 nm is observed for Fe concentrations higher than 100 μg/g oil, but a secondary B line at 249.678 nm is completely resolved from Fe 249.653 nm. In the case of P 213.618 nm, a contribution of the right wing of a Cu line at 213.598 nm generates a signal equivalent to P 18 μg/g oil for Cu 1000 μg/g oil. Received: 25 June 1997 / Revised: 16 September 1997 / Accepted: 7 October 1997     

The application of butanol as dilution agent for the inductively coupled plasma-atomic emission spectrometric determination of boron and phosphorus in lubricating oils

An evaluation of butanol-1 as dilution solvent for the determination of boron (B) and phosphorus (P) in lubricating oils by inductively coupled plasma-atomic emission spectrometry (ICP-AES) has been performed. Standard solutions of boric acid and tri-n-butyl phosphate (TBP) in butanol were employed as calibrants for B and P, respectively. Solutions of phosphoric acid and tris(2-ethylhexyl)phosphate (TEHP) in butanol were also tested as possible P standards. Increased concentrations of oil in the sample in the range of 0 to 20% showed no significant effects on B and P emission intensities indicating that matrix matching is not required for lubricating oils of about 2–15 cPoise. Detection limits in absence of spectral interferences were 0.06 μg B/g oil and 2 μg P/g oil. Overall estimated precision was 2.5% for B concentrations above 4 μg/g oil, and 6.5% for P concentrations above 20 μg/g oil. We evaluated the performance of a high resolution scanning spectrometer for mitigating the effects of overlapping spectral interferences from iron (Fe) and copper (Cu) on B and P emission lines. An interference from Fe 249.782 nm on the primary B line at 249.773 nm is observed for Fe concentrations higher than 100 μg/g oil, but a secondary B line at 249.678 nm is completely resolved from Fe 249.653 nm. In the case of P 213.618 nm, a contribution of the right wing of a Cu line at 213.598 nm generates a signal equivalent to P 18 μg/g oil for Cu 1000 μg/g oil. Received: 25 June 1997 / Revised: 16 September 1997 / Accepted: 7 October 1997     

Simultaneous determination of traces of impurities in high-purity molybdenum and molybdenum trioxide by coprecipitation and inductively coupled plasma-atomic emission spectrometry

Summary Inductively coupled plasma-atomic emission spectrometry (ICP-AES) has been developed for a simultaneous determination of traces of non-hydride-forming elements in high-purity Mo and molybdenum trioxide. Coprecipitation of diverse elements with lanthanum hydroxide is used to separate them from the Mo matrix and for concentration. Effects of pH and amount of La on the recoveries of diverse elements are discussed. Ten elements (Co, Cr, Cu, Fe, Mn, Ni, Ti, V, Zn, and Zr) are quantitatively recovered and determined. Matrix-matched calibration solutions are used for the determination.     

Determination of impurities in high-purity gold, with a gas-stabilized low-temperature arc

A gas-stabilized arc with aerosol supply has been used for emission spectrometric determination of Al, B, Be, Co, Cr, Fe, Ga, In, Mg, Mn, Ni, Pd, Rh and Zn, as impurities in high-purity gold. Two analytical procedures were compared: (a) direct aspiration of dissolved samples containing 2% of gold and 0.25M KCl as buffer, and (b) separation of impurities by ether extraction of gold from 1M HCl followed by impurity determination with a stabilized arc. Limits of detection, precision and recovery of the extraction procedure are given.     

Co-B/γ-Al2O3非晶态催化剂的制备及其催化乳酸乙酯液相加氢性能

采用浸渍-还原法制备了负载型Co-B/γ-Al₂O₃非晶态合金催化剂, 并将其应用于乳酸乙酯液相加氢制备1,2-丙二醇(1,2-PDO)反应中, 研究了其催化加氢性能. 采用电感耦合等离子体(ICP)发射光谱仪、X射线衍射(XRD)仪、透射电子显微镜(TEM)、差示扫描量热(DSC)、X射线光电子能谱(XPS)等手段对催化剂的性能进行了表征, 考察了制备条件对催化剂性能的影响. 结果表明, 新鲜的Co-B/γ-Al₂O₃催化剂具有非晶态结构, Co-B均匀地分散在载体γ-Al₂O₃上. 随着Co负载量的增加, 催化剂的热稳定性提高, 催化剂表面Co/B原子比增加. 当金属Co理论负载量为30%(质量分数, w)时, Co-B/γ-Al₂O₃催化剂表现出最高的加氢催化性能, 在160 ℃, 氢气压力为6.0 MPa条件下反应9 h, 乳酸乙酯的转化频率(TOF)为1.41 h^-1, 转化率达到93.63%, 1,2-丙二醇的选择性达到96.10%. 催化剂的加氢性能取决于其分散均匀的Co-B纳米粒子、较高的表面Co/B原子比及Co和B之间的电子转移效应.     

Role of Transition Metals in UV‐B‐Induced Damage to Bacteria

The purpose of this study was to explore the possible link between metals and UV‐B‐induced damage in bacteria. The effect of growth in the presence of enhanced concentrations of different transition metals (Co, Cu, Fe, Mn and Zn) on the UV‐B sensitivity of a set of bacterial isolates was explored in terms of survival, activity and oxidative stress biomarkers (ROS generation, damage to DNA, lipid and proteins and activity of antioxidant enzymes). Metal amendment, particularly Fe, Cu and Mn, enhanced bacterial inactivation during irradiation by up to 35.8%. Amendment with Fe increased ROS generation during irradiation by 1.2–13.3%, DNA damage by 10.8–37.4% and lipid oxidative damage by 9.6–68.7%. Lipid damage during irradiation also increased after incubation with Cu and Co by up to 66.8% and 56.5% respectively. Mn amendment decreased protein carbonylation during irradiation by up to 44.2%. These results suggest a role of Fe, Co, Cu and Mn in UV‐B‐induced bacterial inactivation and the importance of metal homeostasis to limit the detrimental effects of ROS generated during irradiation.     

Binuclear cyclopentadienylcobalt carbonyls: comparison with binuclear iron carbonyls

The binuclear cyclopentadienylcobalt carbonyls Cp2Co2(CO)n (n = 3, 2, 1; Cp = eta5-C5H5) are studied by density functional theory using the B3LYP and BP86 functionals. The experimentally known monobridged isomer Cp2Co2(CO)2(mu-CO) and the tribridged isomer Cp2Co2(mu-CO)3 of Cp2Co2(CO)3 with formal Co-Co single bonds are found to be similar in energy, with the precise relative energies of the two isomers depending on the functional chosen. For Cp2Co2(CO)2, the experimentally known coaxial isomer Cp2Co2(mu-CO)2 with two bridging CO groups and a formal Co=Co double bond (2.360 angstroms by B3LYP or 2.346 angstroms by BP86) is found to lie 38.2 (B3LYP) or 34.9 kcal/mol (BP86) below a perpendicular isomer perpendicular-Cp2Co2(CO)2. Similarly, for Cp2Co2(CO), the coaxial isomer Cp2Co2(mu-CO) with one bridging CO group and a formal CoCo triple bond (2.021 angstroms by B3LYP or 2.050 angstroms by BP86) is found to lie 9.36 (B3LYP) or 9.62 kcal/mol (BP86) below the corresponding perpendicular isomer perpendicular-Cp2Co2(CO). This coaxial isomer Cp2Co2(mu-CO) is a possible intermediate in the known pyrolysis of the trimer (eta5-C5H5)3Co3(mu-CO)3 to give the tetranuclear complex (eta5-C5H5)4Co4(mu3-CO)2. These optimized Cp2Co2(CO)n (n = 3, 2, 1) structures can be compared with the corresponding Fe2(CO)6+n structures since the CpCo and Fe(CO)3 groups are isolobal. In general, the metal-metal bonds are 0.09-0.22 angstroms shorter for the Cp2Co2(CO)n (n = 3, 2, 1) complexes than for the corresponding Fe2(CO)6+n complexes. For Fe2(CO)9, the experimentally well-known Fe2(CO)6(mu-CO)3 isomer is shown to be very close in energy to the unknown Fe2(CO)8(mu-CO) isomer, with the precise relative energies depending on the basis set used.     

Optimized microwave-assisted decomposition method for multi-element analysis of glass standard reference material and ancient glass specimens by inductively coupled plasma atomic emission spectrometry

A novel microwave-assisted wet-acid decomposition method for the multi-element analysis of glass samples using inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed and optimized. The SRM 621 standard reference glass material was used for this purpose, because it has similar composition with either archaeological glass specimens or common modern glasses. For the main constituents of SRM 621 (Ca, Na, Al, Fe, Mg, Ba and Ti), quality control data are given for all the examined procedures. The chemical and instrumental parameters of the method were thoroughly optimized. Thirteen acid mixtures of hydrochloric, nitric, and hydrofluoric acids in relation to two different microwave programs were examined in order to establish the most efficient protocol for the determination of metals in glass matrix. For both microwave programs, an intermediate step was employed with addition of H₃BO₃ in order to compensate the effect of HF, which was used in all protocols. The suitability of the investigated protocols was evaluated for major (Ca, Na, Al), and minor (Fe, Mg, Ba, Ti, Mn, Cu, Sb, Co, Pb) glass constituents. The analytes were determined using multi-element matrix matched standard solutions. The analytical data matrix was processed chemometrically in order to evaluate the examined protocols in terms of their accuracy, precision and sensitivity, and eventually select the most efficient method for ancient glass. ICP-AES parameters such as spectral line, RF power and sample flow rate were optimized using the proposed protocol. Finally, the optimum method was successfully applied to the analysis of a number of ancient glass fragments.     

Principal component analysis: a chemometric aid for classification of polluted and unpolluted mussels

Ten trace elements (Al, Cr, Mn, Fe, Co, Ni, Cu, Zn, Cd and Pb) were determined in the dissolved ash of the edible part of wild mussels (28 samples) from a polluted site by electrothermal atomic absorption spectrometry. The distribution of the concentration of each element in the mussels was first investigated by means of a test of normality. The correlation matrix around the mean was used as a starting matrix for principal component analysis (PCA). Ten variables were reduced to two principal components, accounting for 77% of the total variance; Al, Cr, Mn, Fe, Zn, Cd and Pb are all positively associated with the first principal component and form a cluster of variables, indicating a common terrigenous origin. Comparison with 43 samples of unpolluted mussels from a nearby hatchery, on the basis of eight common variables (concentration of Mn, Fe, Co, Ni, Cu, Zn, Cd and Pb; 71 samples) by using a two-dimensional plot of PC scores, allows the mussels from the two sites to be differentiated.     

Direct determination of trace elements in niobium,tantalum and their oxides by inductively coupled plasma atomic emission spectrometry after microwave dissolution

Analytical schemes for the determination of trace elements in high-purity niobium, tantalum and their oxides are proposed. The schemes are based on microwave dissolution of the metals and oxides followed by inductively coupled plasma atomic emission spectrometry (ICP-AES) determination of impurities in the solutions. The possibilities of interelement and off-peak background corrections in ICP-AES analysis are discussed. The accuracy of the results obtained is confirmed by the determination of trace elements after a matrix sorption separation procedure. For a number of elements, a comparison of the results obtained by ICP-AES without and with the matrix separation procedure and by electrothermal atomic absorption spectrometry (ETAAS) shows good agreement. The limits of detection for direct ICP-AES determination are in the range 0.4*1.0 μg g⁻¹ for Ba, Ca, Fe, Mg, Mn, Y and La; between 2.0 and 10.0 μ g⁻¹ for B, Cd, Co, Cr, Cu, Hf, Mo, Na, Nb, Ni, Pb, Sr, Ti, Zr and Ta; and for K, Sb and W a detection limit of 20 μ g⁻¹ is achieved. The schemes proposed are intended for rapid routine analysis.     

Iminoimidazole‐based Co(II) and Fe(II) complexes: Syntheses,characterization, and catalytic behaviors for isoprene polymerization

A stereoselectivity switchable polymerization of isoprene has been developed, which is catalyzed by iminoimidazole‐Co(II) and ‐Fe(II) complexes. The influence of substituents ranging from electron donating to the electron withdrawing on the iminoimidazole‐Co(II) and ‐Fe(II) catalysts is investigated for isoprene polymerization. Two sets of iminoimidazole‐Co(II) and ‐Fe(II) complexes have been prepared and fully characterized. X‐ray crystallography analysis reveals that the complexes Co1 and Fe1 adopt distorted tetrahedral geometries. In the presence of AlEt₂Cl as co‐catalyst, all the Co(II) complexes are active and the catalytic activity is highly dependent on the molar ratio of Al/Co. All the Co(II) complexes exhibit higher activities at low Al/Co ratio. Compared with the Co(II) complexes, the Fe(II) complexes are essentially inactive under the identical condition. However, on activation with combination of AlEtCl₂ and [Ph₃C][B(C₆F₅)₄], both Co(II) and Fe(II) complexes display high activities with good conversions of isoprene (up to >99%). Additionally, low molecular weight and high trans‐1,4‐unit (>96%) selectivity are characteristics of the resultant polyisoprene. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019 , 57, 767–775