The elimination of matrix effects in the determination of fluorine by proton induced prompt gamma-spectrometry

By measuring the yield of prompt gamma-rays, induced by energetic protons, the ratio of the ranges in sample and standard was used in the average cross-section method to determine fluorine. By spiking the sample with known amounts of a lithium compound, a nonanalyte element (absent from the sample), the appropriate ranges in the samples were determined by measuring the prompt gamma-rays induced in the non-analyte spike. Fluorine was determined in ores and ivory and the method was tested by analyzing the standard reference materials SRM 91, SRM 120c and SRM 694.     

Determination of boron range distribution in ion-implanted silicon by the10B(n, α)7 Li reaction

A measuring technique based on the alpha particles being released from the¹⁰B(n, α) nuclear reaction and using the time-of-flight technique at a periodically pulsing reactor was developed. Non-destructive determination for the range distribution of boron impurities in ion-implanted silicon have been performed. Projected ranges obtained in the energy region 20–80 keV are compared to calculated results and to other experiments. Examples are shown for some typical boron distributions before and after annealing the sample.     

The use of relative deceleration properties in the determination of chromium by PIPPS

Using particle induced prompt photon spectrometry, PIPPS, the ratios of deceleration values of charged particles in samples and standards can be used to determine elemental compositions. Through the spiking of samples and standards with a compound containing a known amount of a non-analyte element (lithium), to which a relative decelaration value is ascribed, appropriate relative deceleration values for samples and standards can be assessed by measuring the prompt -ray yields induced in the spike. Using 5 MeV protons this method was tested for the determination of chromium in a selection of reference standards using pure compounds of chromium as analyte standards. The application of both the average cross section as well as the average stopping power approaches were investigated.     

Determination of boron and lithium in diverse biological matrices using neutron activation-mass spectrometry (NA-MS)

Summary Essential features of the neutron activation-mass Spectrometry (NA-MS) technique are described. Applicability of this technique for the simultaneous determination of boron and lithium is demonstrated for a diverse group of biomaterials. NA-MS is a nondestructive analytical technique, and dynamic in nature since its coverage extends to a broad range of concentration levels. Contamination after the irradiation step, extraneous by natural lithium or boron is inconsequential, since only the activation products are the analyted assayed. Coupling the nuclear activation phenomenon which generates ⁴He and ³He (from ¹⁰B and ⁶Li, respectively), with the high precision potential of mass spectrometry forms the bases of this technique. Under ideal conditions the detection limit is extendable to pg g^–1 concentration ranges and therefore, it is extremely well suited to investigate the natural concentration levels of boron and lithium in biomaterials. The potential of this method for the determination of lithium in biomedical trace element research is of special significance since determination of sub-ppb levels of lithium by other analytical techniques faces serious analytical difficulties mainly due to contamination control and in some cases to insufficiently low detection limits.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定尼日利亚铌钽锂矿石中的铌、钽、锂

经过三种样品前处理实验对比,选择采取氢氟酸-高氯酸-王水溶样,酒石酸-王水浸取,电感耦合等离子体原子发射光谱(ICP-AES)法测定尼日利亚地区铌钽矿石中铌、钽、锂元素。对元素的分析谱线、酒石酸浓度等工作条件进行了优化,选择各元素的最佳分析谱线,并进行加标回收实验,探讨了各元素的加标回收率。选取Nb 269.7 nm、Ta 240.0 nm、Li 670.78 nm作为仪器分析谱线,计算得到的方法检出限分别为:Nb 0.5μg/g、Ta 1.5μg/g、Li 15.0μg/g。对比各种溶样方法,选取一种最简洁方便的样品前处理途径,经国家一级标准物质GBW07153、GBW07155和GBW07185验证,测定值的相对误差为-2.82%~1.77%,方法精密度(RSD,n=6)为0.11%~1.2%,测定尼日利亚地区铌钽锂矿石中的铌、钽、锂元素,结果无显著性差异,方法能够满足尼日利亚铌钽矿石中相关组分的准确测定。     

A density functional treatment of organolithium compounds: Comparison to ab initio,semiempirical, and experimental results

Density functional calculations on several classes of organolithium compounds are described. The compounds studied include lithium bonds to carbon, oxygen, and nitrogen and are representative of most types of organolithium compounds that have appeared in the recent literature. The computational results are compared to those using MNDO, which has been shown to have some serious deficiencies in compounds involving carbon–lithium bonds, and to PM3 results, which offer some improvement over MNDO for many organolithium compounds. Most of the density functional calculations with a large basis set are in good agreement with available ab initio and experimental data. Calculated carbon–lithium bond lengths were slightly shorter than those calculated by other ab initio methods and were substantially longer than those calculated by MNDO, which is known to underestimate carbon–lithium bond lengths severely. Dimerization energies of methyllithium, calculated by DMol, were also in good agreement with those of other ab initio calculations. Lithium–nitrogen bonds in lithium amides were calculated to be slightly shorter by DMol than by MNDO, although the two methods were in qualitative agreement for this type of compound. © 1995 by John Wiley & Sons, Inc.     

Improving the completeness of combustion of boron particles in a solid-fuel ducted rocket owing to distributed air supply to the secondary combustor

A model of combustion of boron particles in ducted rocket using distributed air supply to the secondary combustor was developed for the first time. The completeness of boron combustion in ducted rocket using air supply to the secondary combustor through one outlet or two outlets (distributed air supply) was calculated. It was shown that, in some cases, distributed air supply significantly (by a factor of 1.5–3) decreases the time of complete combustion of boron particles and thereby increases the completeness of fuel combustion in ducted rocket. The modeling results agree with the known experimental data.     

Darstellung und Eigenschaften von Trinorbornylbor-Verbindungen

Synthesis and Properties of Trinorbornyl Boron Compounds Tris(1-norbornyl), Tris(2-norbornyl), and Tris(7-norbornyl) boron were synthesized from boron trifluoride diethylether and 1-norbornyl lithium or 2- and 7-norbornyl magnesium halides respectively. The compounds were characterized by the IR-, ¹³C-, ¹¹B-NMR, and mass spectra. Furthermore 1-norbornyl lithium was isolated in the crystalline state and investigated in detail.     

Etude des possibilites de dosage du lithium par activation au moyen de protons et de deutons de moyenne energie

The determination of lithium by measuring⁷Be, produced by proton or deuteron activation, has been studied. The extent of interference from boron or beryllium, which also form⁷Be, was measured. The calculated sensitivity limits when activating for one hour with 10μA beams of 14 MeV protons or 25 MeV deuterons are, for lithium, 1·10⁻¹ and 2.5·10⁻² ppm and for boron, 2·10⁻¹ and 1·10⁻¹ ppm, respectively.      

Theoretical study of the structure and properties of complexes formed by lithium and a boron α sheet

The ability of lithium to form complexes with a boron α sheet and the occurrence of ionic conduction in the compounds formed were evaluated using quantum-chemical methods. The obtained materials were established to be stable, and the weight fraction of lithium can reach 0.32. It was concluded that a low potential barrier for migration of lithium ions over the surface indicates the presence of ionic conduction.     

The determination of boron in rocks by deuteron activation analysis

The determination of boron in rocks by charged particle activation using the¹⁰B(d, n)¹¹C reaction is studied. A sample holder that allows reproducible irradiation of powdered samples is developed.¹¹C is separated as¹¹CO₂. For boron concentrations between 2.35 and 25.2 μg·g⁻¹, the standard deviations ranges from 7.1 to 22.8%. The results for USGS reference silicate rocks and Moroccan phosphate rock are compared to those obtained by other techniques.     

Ab initio analysis of lithium dimethylaminoborohydride

Ab initio calculations were used to determine the equilibrium geometries and energies of lithium dimethylaminoborohydride. Relative energies of the monomeric and dimeric species were calculated in the gas phase and for the dimethyl ether microsolvated molecules. The most stable structure was a dimer in which the lithium and boron atoms were bridged by two hydrogen atoms, similar to the three-center two-electron bonds in diborane. This hydrogen bridging was maintained in the lithium dimethylaminoborohydride bis(dimethyl ether) microsolvate.     

波长色散X射线荧光光谱法测定铁矿石中铁硅钙铝磷镁锰钛

采用四硼酸锂熔融—X射线荧光光谱法测定铁矿石中铁、硅、钙、铝、磷、镁、锰和钛，以10个铁矿石标准物质建立校准曲线，用Lachance—Trail校正模式进行回归校正。方法准确、快速、简便。     

Polymerization of coordinated monomers. XVII. Alternating copolymerization of methyl methacrylate with styrene by boron compounds

By the use of various boron compounds methyl methacrylate and styrene were copolymerized under photoirradiations at ?20°C. The alternately regulating activities of the boron compounds in the copolymerizations were in the following order: boron trichloride > ethylboron dichloride > boron trifluoride > diethylboron chloride ? triethylboron (?0). Boron trichloride and ethylboron dichloride exhibited such high regulating activities that their presence in 1 mol% in the charged methyl methacrylate was sufficient to complete equimolar alternating copolymerization. The alternating copolymerization proceeded in the steady state. The copolymerization rates decreased in the following order: boron trichloride ? ethylboron dichloride > diethylboron chloride ? triethylboron (?0). The cotacticities of methyl methacrylate-centered triads in the resulting copolymers were identical to those prepared with boron trichloride, ethylboron dichloride, and diethylboron chloride. The mechanism of the alternating copolymerization is discussed.     

电感耦合等离子体原子发射光谱(ICP-AES)法测定钢中硼时样品溶解损失及空白控制研究

用电感耦合等离子体原子发射光谱(ICP-AES)法研究了钢中硼的测定。实验发现,分析线在硼182.64nm处无硼铁基体空白值低于纯试剂(无铁)空白值。样品分析时,应进行无硼铁基空白实验,结果计算只能用此空白值。对普通玻璃烧杯和聚四氟乙烯烧杯的酸溶样品测定结果进行了比较,结果表明,测定结果和空白值相近且都很低,无硼普通玻璃烧杯也能满足钢中低含量硼的测定需要。通过对实验与报道结果比较分析表明,硝酸或王水加热溶解样品得到的溶液中硼没有损失,此溶液可测定钢中酸溶硼;用高氯酸发烟处理后,样品中酸不溶硼可能会溶解,但硼会挥发损失。因此,高氯酸发烟处理不能测定硼。     

Stabilization of Planar Four-Coordinate Boron,Carbon, and Silicon Atoms in Borane Clusters: A Quantum-Chemical Study

Stability of a series of neutral and charged borane clusters containing planar four-coordinate boron centres was predicted by the density functional theory DFT (B3LYP/6-311+G**). The possibility of the modification of these systems to obtain new stable compounds with planar four-coordinate carbon and silicon atoms was examined. The calculations show that the substituted systems should be more stable than the isoelectronic boron analogs.     

Determination of boron in organic compounds by microwave plasma–atomic emission spectrometry

We propose a method for the determination of boron in aliphatic and aromatic trifluoroborates (including perfluorinated ones), ethers, and organoboron compounds containing dioxoborolane fragments, pyridine, and pyrazole rings, and triple bonds. The substances were decomposed by the oxygen flask combustion method. Boron was determined on an Agilent 4100 microwave plasma–atomic emission spectrometer. A number of organic compounds were analyzed, and the mass fraction of boron was determined with an error less than ±0.3 abs. %.     

Entrapment of some compounds into biocompatible nano-sized particles and their releasing properties

Two types of biocompatible nanoparticles with an average diameter of around 200 nm were formed only by mixing hydrolysates of chitosan and carboxymethyl cellulose (CMC). Nanoparticle A was produced from chitosanase hydrolysate of chitosan and cellulase hydrolysate of carboxymethyl cellulose, and nanoparticle B was produced from lysozyme hydrolysate of chitosan and the carboxymethyl cellulose hydrolysate. Negatively charged or amphoteric compounds were first mixed with chitosan hydrolysate and then added to carboxymethyl cellulose hydrolysate to effectively entrap them in the particles. Positively charged compounds could also be effectively entrapped by mixing the hydrolysates and the compound in the reverse order. Negatively charged compounds with high molecular weights were maintained in the particles even at the higher pH levels than the pK(a) of the amino groups of chitosan. Entrapped compounds were gradually released from nanoparticle A by lysozyme treatment. In contrast, there was no release from nanoparticle B. These results indicate that nanoparticle A can be applied to controlled-release drug delivery systems, and that nanoparticle B is stably retained in the body without releasing the entrapped compounds.     

Determination of the effective charge of individual colloidal particles

An optical method is presented that allows simultaneous determination of the diffusion constant and electrophoretic mobility of individual charged particles with radius down to 0.2 mum. By this method the size dependency of the effective charges and zeta potentials of individual particles can be investigated, as well as interparticle interactions and Brownian motion in confined geometries. The diffusion constant and mobility are determined from the power spectrum of the particle speed in a sinusoidal electrical field. The accuracy of the method was tested on PMMA spheres of known size in water. Experiments have been carried out on charged pigment particles with low concentration in a nonaqueous medium containing a charging agent. The mobility is found to be independent of the particle size.     

Determination of organic compounds from wood combustion aerosol nanoparticles by different gas chromatographic systems and by aerosol mass spectrometry

Organic compounds in atmospheric nanoparticles have an effect on human health and the climate. The determination of these particles is challenged by the difficulty of sampling, the complexity of sample composition, and the trace-level concentrations of the compounds. Meeting the challenge requires the development of sophisticated sampling systems for size-resolved particles and the optimization of sensitive, accurate and simple analytical techniques and methods. A new sampling system is proposed where particles are charged with a bipolar charger and size-segregated with a differential mobility analyzer. This system was successfully used to sample particles from wood pyrolysis with particle sizes 30–100 nm. Particles were analyzed by four techniques: comprehensive two-dimensional gas chromatography–time-of-flight mass spectrometry, gas chromatography–time-of-flight mass spectrometry, gas chromatography–quadrupole mass spectrometry, and aerosol mass spectrometry (aerosol MS). In the chromatographic techniques, particles were collected on a filter and analyzed off-line after sample preparation, whereas in the aerosol MS, particle analysis was performed directly from the particle source. Target compounds of the samples were polyaromatic hydrocarbons and n-alkanes. The analytical techniques were compared and their advantages and disadvantages were evaluated. The sampling system operated well and target compounds were identified in low concentrations.