CW diode pumping and FM mode locking of a Nd: KGW laser

We have demonstrated cw diode end pumping of Nd: KGW, a novel solid-state gain medium, with up to 30% conversion efficiency into near-TEM₀₀ (M² < 1.05) output at = 1.067 µm for a pump level of 2.7 W. The slope efficiency was limited by intracavity reflections to 36%; however, direct comparison to a similar Nd:YAG laser indicates the same intrinsic slope efficiency of 60%. FM mode locking of this laser at 200 MHz has produced 12 ps pulses (compared to 16 ps for Nd: YAG), although an intracavity etalon was required. Considerable reduction in pulse width is possible (the line width limit is 0.5 ps) but different techniques may be necessary. Spatial hole burning was evident in both the 120 GHz free-running spectrum and the etalon-limited mode-locked spectrum.     

The nature of the C-defects in nickel and their rôle in the interpretation of radiation damage in metals

In previous Perturbed-Angular-Correlation (PAC) studies of the - emission of ¹¹¹In probe nuclei in cold-worked or particle-irradiated nickel, it has been found that thermal annealing in the temperature regime of recovery stage III leads to the formation of so-called C-defects (Cubic defects). This is indicated by the occurrence of a new frequency of about 80 Mrad/s, in addition to the frequency (200 Mrad/s) that is due to ¹¹¹In on substitutional sites. Obviously, the C-defects are complexes consisting of ¹¹¹In and the intrinsic point-defect species that migrates freely in recovery stage III. Therefore, they have played an important rôle in the long-standing controversy on whether the recovery-stage-III defects are vacancies (one-interstitial model) or self-interstitials (two-interstitial model). The present paper reports on a novel experimental effort to reveal the nature of the C-defects by combining PAC studies on nickel samples differently pretreated in a systematic way, investigations of the Extended X-ray Absorption Fine Structure (EXAFS) on In-doped nickel, and measurements of the decay rate of ¹¹¹In nuclei in the Electron-Capture-Induced Decay (ECID). On the basis of the results of these experiments it is concluded that the defects trapped by substitutional ¹¹¹In atoms (In_s) in recovery stage III are self-interstitials (I), as expected according to the two-interstitial model. Moreover, there is evidence that the C-defects are In interstitials on tetrahedral sites (In_i) that form exclusively in the vicinity of the specimen surface from In_s – I pairs via the reaction In_s+I In_i.     

Syntheses and structural characterizations of Fe_4S_4 cubane-like cluster compounds containing cycloalkylthiolate ligands

In a reaction system consisting of FeCl2,tetrathiometallate and cycloalkylthiolate,two Fe4S4 cubane-like cluster compounds were obtained with the following crystallographic data:(PhCH2NMe32[Fe4S4 (SC5H9)4](Ⅰ),monoclinic space group P21/c,a=1.6327(4),6=1.1229(3),c=2.802 5( 10) nm,β=94.63(2)°,Z=4,and R=0.074; (Et4N)2[Fe4S4(SC6H11)4](Ⅱ),tetragonal space group I42m,a=1.16705(9),b=1.167 06(2),c=2.063 26(5) nm,Z=2,Dabs=1.28 g/cm3,and R=0.078 The participation of cy-cloalkylthiolate ligand does not obviously arouse the change of the Fe4S4 core structure.Meanwhile,the influence of the cation on the structural symmetry of the Fe4S4 cluster dianion is also discussed.     

Spectrophotometric determination of Fe(II) in milligram solid samples

The analytical procedure of determination of Fe(II) in the presence of Fe(III) in milligram samples is proposed. A solid sample is dissolved in hydrochloric acid in argon atmosphere. Subsequently, the pH-value of the solution is fixed and Fe(III) complexed by phosphoric buffer. At the next step Fe(II) is oxidized by -molybdosilicic acid. Finally, the intensity of colouring caused by the reduced form of the acid is measured at the wavelength 770 nm. The proper treatment of the sample during oxidation, and immediately before, is decisive for the accuracy of the analysis. The method was verified by means of the analysis of synthetic magnetite. The theoretical content of Fe(II) was 24.12%, the determined one was 24.02 ± 0.10%. The method was applied to the determination of the homogeneity of an iron catalyst for ammonia synthesis.     

Surface recombination in breakdown time delay experiments: Effect of different cathode materials

The late afterglow in nitrogen with iron electrode is studied by the breakdown time delay method, i.e., by measuring the breakdown time delay t_d as a function of the afterglow time . It is proposed that the cause of the secondary electrons initiating the breakdown is the energy of the surface recombination of nitrogen atoms on the iron electrode. The gas-phase and macrokinetic diffusive models are used to describe the experimental breakdown time delay data. By fitting the theoretical curve to the experimental data: (1) it has been confirmed that the recombination on the molybdenum glass is of the second order and the value of the surface recombination coefficient is determined at 4 mbar; (2) it has been shown that the surface recombination on the iron electrode is of the second order, and the effective recombination coefficients are determined; (3) the analytical form of the recombination coefficient as a function of the adsorption characteristics of surfaces and the pressure of the parent gas has been derived. In addition, the orders of surface recombination on the molybdenum-, aluminum-, and gold-plated electrode were determined by the same method.     

Fe(OH)2悬浮液在EDTA作用下氧气氧化生成δ-FeOOH的机理研究

At room temperature and in the presence of trace EDTA, the formation of δ-FeOOH was studied by the rapid oxidation of Fe(OH)2 suspension with O2. The structural and morphological changes were characterized by various techniques such as XRD, FTIR and TEM. γ-FeOOH and (δ-FeOOH) formed simutaneously in the early period of oxidation. But as the rate of mass transfer was in equilibrium, trace (γ-FeOOH) vanished gradually. Accordingly, pure phase δ-FeOOH was obtained. At the same time, critical amount ratio K of EDTA to Fe2+ was verified. The experiments show that the reactivity, rate of the oxidizing agent and pH of the initial medium were important factors for the formation of pure phase (δ-FeOOH). Under the auxiliary effect of EDTA, the reactivity of O2 was nearly improved to that of H2O2. And the process of the oxidation that Fe(OH)2 suspension was oxidized by O2 under that condition was discussed.     

Multicomponent analysis with a computerized flow injection system using LED photometric detection

An original computer-controlled solid-state photometer has been developed and its potential for simultaneous multicomponent flow-injection analysis of binary and ternary mixtures is demonstrated. The device is simple in construction. Its principle of operation is based on rapid sequential measurements of the absorbance of the complexes formed by the analytes with chromogenic reagents at the wavelengths corresponding to the emission maxima of three light emitting diodes (563, 580 and 638 nm).     

卡尔曼滤波析相光度法同时测定锰铁铜锌镉的研究——5-Br-PADAP—Triton X-100体系

运用卡尔曼滤波递推法,以2-(5-溴-2-吡啶偶氮)—5-二乙氨基苯酚(5-Br-PADAP)为显色剂,建立了同时测定锰、铁、铜、锌、镉析相光度法.在pH9.0硼酸-氢氧化钠介质中,胶束溶液在95℃加热1h,配合物被Triton X-100相完全富集,最大吸收峰分别为锰566nm、铁556nm、铜560nm、锌562nm、镉557nm,工作曲线范围除镉为0～8μg/5ml外,其余均为0～10μg/5ml.应用于大米中锰铁铜锌镉的同时测定,结果满意.     

热解-还原法制备单分散Fe3O4亚微空心球

在用模板法水解FeCl3制备单分散聚(苯乙烯-共-丙烯酸)/Fe2O3[P(St-co-AA)/Fe2O3]核壳粒子的基础上, 于N2环境下热解内核直接得到了单分散的磁性Fe3O4亚微空心球. 用透射电镜(TEM)、场发射扫描电镜(FESEM)、X射线衍射(XRD)、振动样品磁强计(VSM)表征并测试了空心微球的结构形貌、成分以及静磁性能. 结果表明, P(St-co-AA)/Fe2O3核壳粒子在热处理过程中, 由于内核热解生成的有机小分子将Fe2O3 壳层同时还原为Fe3O4, 从而生成了粒径和壁厚均匀的单分散Fe3O4亚微空心球. 该空心微球在室温下的饱和磁化强度、剩余磁化强度和矫顽力分别为50.91 A·m2·kg-1、3.97 A·m2·kg-1和2.33 kA·m-1.     

Solid-phase extraction of iron(III) with an ion-imprinted functionalized silica gel sorbent prepared by a surface imprinting technique

A new Fe(III)-imprinted amino-functionalized silica gel sorbent was prepared by a surface imprinting technique for selective solid-phase extraction (SPE) of Fe(III) prior to its determination by inductively coupled plasma atomic emission spectrometry (ICP-AES). Compared with non-imprinted polymer particles, the ion-imprinted polymers (IIPs) had higher selectivity and adsorption capacity for Fe(III). The maximum static adsorption capacity of the ion-imprinted and non-imprinted sorbent for Fe(III) was 25.21 and 5.10 mg g⁻¹, respectively. The largest selectivity coefficient of the Fe(III)-imprinted sorbent for Fe(III) in the presence of Cr(III) was over 450. The relatively selective factor (α_r) values of Fe(III)/Cr(III) were 49.9 and 42.4, which were greater than 1. The distribution ratio (D) values of Fe(III)-imprinted polymers for Fe(III) were greatly larger than that for Cr(III). The detection limit (3σ) was 0.34 μg L⁻¹. The relative standard deviation of the method was 1.50% for eight replicate determinations. The method was validated by analyzing two certified reference materials (GBW 08301 and GBW 08303), the results obtained is in good agreement with standard values. The developed method was also successfully applied to the determination of trace iron in plants and water samples with satisfactory results.