Modified iron oxide nanoparticles as solid phase extractor for spectrophotometeric determination and separation of basic fuchsin

This study presents a novel separation, preconcentration and determination of basic fuchsin (BF) in an aqueous solution by sodium dodecyl sulfate (SDS)-bounded iron oxide nanoparticles (S-IONPs). It is shown that the novel magnetic nano-adsorbent is quite efficient for the adsorption and desorption of BF at 25 °C. Different parameters such as pH, temperature, ionic strength and composition of desorbent solvent were optimized. The effect of some co-existing ions on the determination was investigated. The nanoparticles were analyzed by transmission electron microscopy (TEM) and the sizes of S-IONPs were in the range of 20-100 nm. The method showed good linearity for the determination of BF in the range of 10-300 ng mL⁻¹ with a regression coefficient of 0.9989. The limit of detection (LOD) (signal-to-noise ratio of 3:1) was 0.0073 μg L⁻¹ and the relative standard deviation (RSD) for 0.03 μg mL⁻¹ and 0.2 μg mL⁻¹ of BF were 4.53% and 4.73%, respectively. The BF was determined successfully in spiked samples of Karoon River water.     

混合稀土储氢合金中氧和氮的测定

研究了混合稀土储氢合金中氧和氮的测定方法。针对稀土金属高温易挥发、分解的特点，选择适宜的加热温度，使用镍浴，选择高温座坩埚进行试验：选择出了合适的助熔剂的预处理方法。方法已用于实际样品。对含氧0．43％、含氮0.018％的试样，分析精密度为氧4．3％，氮5.9％，加标回收率氧为93％～104％，氮为92％～110％。     

Atom interferometry gravity-gradiometer for the determination of the Newtonian gravitational constant G

We developed a gravity-gradiometer based on atom interferometry for the determination of the Newtonian gravitational constant G. The apparatus, combining a Rb fountain, Raman interferometry and a juggling scheme for fast launch of two atomic clouds, was specifically designed to reduce possible systematic effects. We present instrument performances and preliminary results for the measurement of G with a relative uncertainty of 1%. A discussion of projected accuracy for G measurement using this new scheme shows that the results of the experiment will be significant to discriminate between previous inconsistent values.     

Intramolecular Alkylation of Aromatic Compounds XXXVI [1]. Stereoselective Synthesis of C/D-cis-Configured Ergolines

Summary.  The stereoselective synthesis of cis-ergoline is presented. Starting from rac-N-benzoyl tryptophan methyl ester, the key compound indolinylmethylpyridin-3-one was prepared via a seven-step reaction in good yield. Since its cyclization to the desired ergolinone failed, the key compound was reduced to yield the two diastereomeric pyridin-3-ols; only one of them cyclized in trifluoromethanesulfonic acid, affording cis-ergoline. Catalytic hydrogenation of the latter gave N,N′-dimethyldihydroergoline, the X-ray crystallography of which revealed both the correct structure and identical relative configurations at C-5a and C-6a (SS or RR). Hydroboration and subsequent perruthenate oxidation of the Δ⁹-ergoline provided access to the regioisomeric ergolinols and ergolinones. Received December 27, 2001. Accepted January 15, 2002     

Modified Newton method in circular interval arithmetic

The modified Newton method for multiple roots is organized in an interval method to include simultaneously the distinct roots of a given polynomialP in complex circular interval arithmetic. A condition on the starting disks which ensures convergence is given, and convergence is shown to be quadratic. As a consequence, a simple parallel algorithm to approach all the distinct roots ofP is derived from the modified Newton method.The research reported in this paper has been made possible through the support and the sponsorship of the Italian Government through the Ministero per l'Universitá e la Ricerca Scientifica under Contract MURST 60%, 1990 at the Universitá di L'Aquila.     

原子吸收光谱法测定气样中一氧化碳的研究

本文研究了用自制Ｎｉ（ＣＯ）４发生管和电加热石英管原子化器间接测定一氧化碳的条件，探讨了Ｎｉ（ＣＯ）４的产生和在石英管中原子化效率及干扰消除。     

旋光法测定注射用盐酸阿糖胞苷的含量

对注射用盐酸阿糖胞苷采用旋光法进行测定,测定管长为1 cm。当盐酸阿糖胞苷浓度在1~9.000 0 g.L-1之间时,旋光度与浓度呈线性关系,回归方程为α=0.130 1C+0.000 1,相关系数为0.999 9,平均回收率为99.93%,RSD为0.47%。方法简便、快速、准确,适合于药厂、医院对产品及制剂的快速分析。     

On‐line Liquid‐liquid Extraction Coupled to a Reversed Micellar‐mediated Chemiluminescence Detection System: Application to the Determination of Amino/Nitroaromatic Compounds

A simple and fast flow method for the trace level determination of p‐toluidine, 2‐methyl‐5‐nitroaniline, and 2,4‐dinitroaniline in aqueous samples is reported. These amino/nitroaromatics are related to trinitrotoluene (TNT) and appear during the degradation process of the explosive. The chemical principles of ion‐pair formation and liquid‐liquid extraction are applied: In aqueous acidic medium, the protonated analyte [HA]⁺ makes an ion‐pair with the tetrachloroaurate(III) ion, followed by on‐line ion‐pair extraction into the dichloromethane carrier used. After membrane separation, the CH₂Cl₂ containing the ion‐pair, [HA]⁺[AuCl₄]⁻, is mixed with the reversed micellar luminescent reagent of luminol (in 0.3 M Na₂CO₃) prepared from cetyl‐trimethylammonium chloride in CH₂Cl₂‐cyclohexane and the [AuCl₄⁻‐luminol chemiluminescence (CL) output is recorded. The detection limits (S/N> 3) are: p‐toluidine, 1.0 × 10⁻⁴M; 2‐methyl‐5‐nitroaniline, 1.0 × 10⁻⁷ M; 2,4‐dinitroaniline, 1.0 × 10⁻⁷ M, while the calibration curves are linear between 1.0 × 10⁻⁴ — 1.0 × 10⁻² M for all the compounds. Although spectral studies indicated the formation and extraction of a very small amount of the ion‐pair species, the reversed micellar‐mediated CL detection system provides an alternative procedure for the determination of degradation products of the explosive TNT in environmental aqueous samples.     

环境光对PE塑料薄膜近红外激光拉曼光谱的影响

探讨了环境光自然光和室内荧光灯光的存在,对PE透明塑料薄膜的近红外激光拉曼光谱的影响.研究表明不同的环境光,会对近红外拉曼光谱产生不同的明显特征峰.自然光干扰产生的是以倒峰群形式为主,而室内荧光灯光造成的干扰主要以尖锐的脉冲峰形式.虽干扰表现形式不同,但都有严重地影响,在测定时一定要引起重视,不能忽略.建议在进行透明塑料近红外拉曼光谱检测时,须在暗室或暗罩遮光保护中进行,以完全隔离环境光的影响.     

原子吸收光谱间接测定色氨酸的研究

色氨酸(Tryptophan,Trp)在碱性条件下与新生成的ZnS悬浮液反应,生成可溶性碱式色氨酸锌配合物,再用塞曼原子吸收光谱测定溶液中的总锌浓度即可间接的得到色氨酸的含量.优化了测定的最佳条件,在pH 9.10的2%硼砂底液中于室温下,使色氨酸试液与新生成的ZnS悬浮液反应22min,离心分离后测定上层清液的FAAS响应.在所选定的条件下色氨酸测定的线性浓度范围为0-18.5mg·mL-1,特征浓度为0.219mg·mL-1,检出限为1.414mg·mL-1.该法用于样品中的色氨酸测定,其相对标准偏差RSD为4.12%,方法的回收率在70.1%-120.3%之间.并对测定机理进行了探讨.