Use of 2, 3-Butanedione Monoxime for Homogeneous Precipitation of Nickel (II)

Abstract

The solid monoxime of 2, 3-butanedione is a more convenient material than liquid dione for the homogenous generation of DMG. 2, 3-butanedione dioxime. Determinations of Ni in steels and in pure Ni(II) solutions have shown the optimum pH and order of adding reagents. Gravimetric and/or an EDTA titrimetric finish are possible for a method of reliability within ± 0.2 mg of Ni in 50–150 mg Ni. The solid has the same character and filterability as that from the 1960 dione method of Salesin and Gordon¹.     

Electron Capture Determination of Propoxyphene from Human Plasma

Abstract

A procedure for the determination of propoxyphene (α-d-dimethylamino-1, 2 -diphenyl-3 -methyl-2 -propionoxybutane) in plasma is reported. The method is based on the electron capture characteristics of propoxyphene. The plasma is rendered basic to generate the free amine and extracted with ether. The extract is analyzed by gas chromatography using a 4 foot OV-225 column. An internal standard of imipramine hydrochloride is used to quantitate the propoxyphene. This internal standard is carried through the entire procedure. The ratio of the peak heights of propoxyphene to imipramine is compared to ratios obtained from standards placed in plasma and treated in the same manner as the samples. Six subjects were given propoxyphene at different time intervals, and the data are presented concerning these subjects.     

Cd(0.2)-Sn-Zn三元合金高压垂直截面相图的测定

 采用高压DTA方法，测定了Cd-Sn-Zn三元系中x_Cd=20 at.%截面的高压垂直截面相图，实验压力为0，0.5，1.0，1.5 GPa。所得高压相图与常压相图比较，在p=1.5 GPa时低共晶点上移了大约35 K，共析组成在加压过程中几乎不变。这种变化趋势与理论计算的结果相图，所得高压相图的液相线与计算相图的一致。     

快速测定氧化还原酶活力的一次性介体电极

以葡萄糖氧化酶（GOD）为模型酶,用一次性丝网印刷电极检测氧化还原酶活力,选用具有较低氧化还原电位的单羟基二茂铁（HMF）作为电子传递介体,以电流法测定氧化酶的活力,所需时间仅为60s,线性响应范围为0～40U/mL.将电极用于检测黑曲酶发酵产生的葡萄糖氧化酶（GOD）的活力,测定结果与传统的方法相对照,具有较好的一致性,相关系数为0.9813.     

Selection of response measurement locations to improve inverse force determination

The forces obtained by inverse methods are prone to errors. These arise due to a combination of errors in the measurements and high condition numbers in the matrix of transfer functions to be inverted. Ill-conditioning of the frequency response function matrix causes measurement errors to be magnified significantly. When the condition numbers are small, the measurement errors simply propagate without much amplification. Due to modal behaviour of the structure, the condition numbers can vary significantly over the frequency range and with the spatial location of the response measurements. The spatial variation can be quite considerable across the structure. The potential for using this characteristic to improve force determination is explored in this paper as an alternative to matrix regularization methods. The aim is to reduce error magnification in inverse methods by an ‘optimal’ spatial distribution of response locations. A method is proposed which is based on the minimization of the average condition number across the frequency range. If many possible locations are available, however, this can involve excessive calculation. An approximate method is therefore proposed which results in consistently good location selection for use in inverse force determination but involves much less computational effort. The error reduction in reconstructed forces is found to be significant in numerical simulations on a simply supported plate and in validation experiments.     

吸光度比值-导数光谱法同时测定铜(Ⅱ)和铬(Ⅲ)的研究

提出了运用吸光度比值-导数光谱法同时测定Cr(Ⅲ)与Cu(Ⅱ)含量的新方法。在pH 5.7的HAc-NaAc的缓冲溶液中,Cr3+,Cu2+与铬天青S(CAS)和溴化十六烷基三甲胺(CTMAB)可分别形成蓝色三元络合物。其摩尔吸光系数分别为2.52×105 L·mol-1·cm-1和1.01×105 L·mol-1·cm-1。Cu2+和Cr3+的浓度分别在0.08～1.2 μg·mL-1和0.05～0.52 μg·mL-1范围内符合比尔定律,其检测限分别为0.014和0.013 μg·mL-1。此方法应用于环境水中Cr(Ⅲ),Cu(Ⅱ)的同时测定,取得了满意的结果。     

一种用于土壤非金属养分测试的光纤探头式分光光度计

针对测土配方施肥技术中要求快速、便捷、高效地进行土壤养分测试的需求,文章基于浸入式光纤探头、平场凹面全息光栅、二极管线阵检测器开发了一种光纤探头式分光光度计用于土壤养分中非金属元素的快速、准确测试。基于国家计量检定规程JJG 178—2007对紫外、可见、近红外分光光度计的性能检测方法测试的该仪器的波长最大允许误差与波长重复性、基线平直度、透射比最大允许误差与透射比重复性均达到了国标第Ⅲ级别标准,其最小光谱带宽、噪声与漂移、杂散光基本达到了国标第Ⅳ级别标准。基于该仪器测试的土壤硝态氮、铵态氮、有效磷、有效硫、有效硼、和有机质含量与基于商用的国产单光束和进口双光束分光光度计测试的结果呈极显著的线性相关关系,其回归方程的斜率接近于1,且对比数据之间无显著性差异。因此,该光纤探头式分光光度计可用于土壤非金属养分的快速、准确测试。     

甲基异丁酮萃取-原子荧光光谱法间接测定碘

在硝酸浓度为0.1mol.L-1介质中,I-和Hg2+能生成稳定的化合物,被甲基异丁酮萃取,原子荧光光谱法测定有机相中的汞,间接得到碘的含量。工作考察了萃取条件以及其他影响因素。在优化的实验条件下,碘的含量在0～12μg.L-1范围内呈良好的线性关系,方法的检出限是0.14μg.L-1,相对标准偏差3.3%,对蛋类样品加标回收率为101.8%～110.4%。     

Backbone-only restraints for fast determination of the protein fold: the role of paramagnetism-based restraints. Cytochrome b562 as an example

CH(alpha) residual dipolar couplings (Deltardc's) were measured for the oxidized cytochrome b562 from Escherichia coli as a result of its partial self-orientation in high magnetic fields due to the anisotropy of the overall magnetic susceptibility tensor. Both the low spin iron (III) heme and the four-helix bundle fold contribute to the magnetic anisotropy tensor. CH(alpha) Deltardc's, which span a larger range than the analogous NH values (already available in the literature) sample large space variations at variance with NH Deltardc's, which are largely isooriented within alpha helices. The whole structure is now significantly refined with the chemical shift index and CH(alpha) Deltardc's. The latter are particularly useful also in defining the molecular magnetic anisotropy parameters. It is shown here that the backbone folding can be conveniently and accurately determined using backbone restraints only, which include NOEs, hydrogen bonds, residual dipolar couplings, pseudocontact shifts, and chemical shift index. All these restraints are easily and quickly determined from the backbone assignment. The calculated backbone structure is comparable to that obtained by using also side chain restraint. Furthermore, the structure obtained with backbone only restraints is, in its whole, very similar to that obtained with the complete set of restraints. The paramagnetism based restraints are shown to be absolutely relevant, especially for Deltardc's.