抗坏血酸同顺磁离子Mn~(2+)、Gd~(3+)络会的~(13)C NMR研究

该文用顺磁离子对其近邻~(13)C核的NMR吸收增宽效应,系统地研究了抗坏血酸在不同溶剂中对金属离子Mn~(2+)、Gd~(3+)的配合行为.在水溶液中,抗坏血酸可通过两种配合方式与Mn~(2+)作用,但与Gd~(3+)的作用只有一种稳定的结构.在水中抗坏血酸对金属的配位活性部位分别是1位羟基氧,3位离解的羟基氧和6位羟基氧.在DMSO中,3位羟基由于H~+对该基团的静电遮蔽而变得对金属离子Mn~(2+)表现为配位惰性,同时6位羟基配位活性较大增强.对Gd~(3+)来说,此时没有优势配位活性部位存在.文章还讨论了抗坏血酸在H_2O-DMSO混合溶剂中的~(13)C NMR谱及在DMSO中NaOH对其~(13)C NMR谱及其与金属络合结构的影响.     

配合物LaL3.H2O的合成及表征

本文以３－甲基苯甲酸为配体，合成了与三价稀土镧离子的固体配合物ＬａＬ３．Ｈ２Ｏ，并对该配合物进行了元素分析，红外光谱，ＵＶ光谱，ＴＧ－ＤＴＡ，ＨＮＭＲ等的测试与表征。该配合物属螯合双齿配位。     

卡尔曼滤波紫外光度法同时测定酱油、食醋中的山梨酸和苯甲酸

在酸性条件下，采用乙酸乙酯萃取、Na2HPO4溶液反萃取分离酱汪、食醋中的山梨酸、苯甲酸，卡尔曼滤波法计算结果，并与比值导数波谱法进行比较。结果表明，卡尔曼滤波法较地数波谱法有较高准确度和精密度，并能监测干扰物质存在与否。用于实际样品分析有更高的可靠性。     

HPLC法测定阿奇霉素葡萄糖注射液中阿奇霉素的含量

利用高效液相色谱法，以VP-ODS型色谱柱，乙腈-异丙醇-水-氨水（60：25：15：0.1)为流动相，于210nm波长处测定了阿奇霉素葡萄糖注射液中阿奇霉素葡萄糖注射液中阿奇霉素的含量。阿奇霉素的浓度在0.75-1.75mg/mL线性关系良好，线性方程的A=881910.4c-16208.2，相关系数r=0.9999。阿奇霉素的平均回收率为99.59%，测定结果的相对标准偏差为1.31%。     

Structural characterisation of Sb-based heterostructures by X-ray scattering methods

Antimonide-based superlattices dedicated to the elaboration of opto-electronic devices have been studied by X-ray scattering techniques. In particular, specular and non-specular X-ray reflectometry experiments have been performed on two MBE-samples elaborated with different shutter sequences at the interfaces. The results have shown a limitation of the incorporation of Sb species in the subsequent InAs layer for one of the samples, as expected.Then, a study on a InGaAs-cap layer/(InGaAs/AlAsSb)_N superlattice grown on a InGaAs/InP buffer layer by both specular X-ray reflectometry and High resolution X-ray diffraction is reported. In particular, the results have revealed the presence of a highly disturbed thin-layer on top of the MOVPE-made GaInAs, whose presence has been explained by In-concentration modification during the desoxidation procedure at the surface of the MOVPE-made GaInAs.Beside the results on the Sb-based heterostructures, the use of X-ray scattering metrology as a routinely working non-destructive testing method has been emphasized.     

Simultaneous spectrophotometric determination of Zinc(II) and Nickel(II) with 1-(2-pyridylazo)-2-naphthol

A new procedure for the simultaneous spectrophotometric determination of Zn(II) and Ni(II) with 1-(2-pyridylazo)-2-naphthol as chromogenic reagent has been developed. It is based on resolution of the mixed spectrum over the wavelength range 530–590 nm by applying a least-squares fitting program to standard spectra from each component. The spectra are recorded at an apparent pH of 5.0, provided by an acetate buffer in a mixed 6040 v/v 2-ethoxyethanol/water medium. The relative standard deviations for determination of 13.7 g of Ni and 31.0 g of Zn were 1.9 and 1.0%, respectively (8 replications). The method has been applied to the analysis of iron surfaces coated with a Zn-Ni alloy. The results are compared with those obtained by atomic-absorption spectrophotometry.     

X射线荧光光谱滤纸片法测定矿石中的铜

我们用Ｘ射线荧光光谱滤纸片法分析了古今１３铜矿石样品中的铜含量，测量结果与化学法一致。此法不需要铜矿石的标样，而且手续简单，方便，检出限低，灵敏度高，测量结果正确可靠，是分析矿石中单一或几个元素的含量较好的方法之一。     

恒电流吸附计时电位法的研究 Ⅱ.铜、铅的微分吸附计时电位法连测

研究了ＮＨ３／ＮＨ４Ｃｌ底液中，铜、铅与水杨基荧光酮（ＳＡＦ）形成的络合物在悬汞电极上的恒电流吸附计时电位溶出行为。讨论了富集时间，溶液ｐＨ值，溶出恒电流大小及铜、铅浓度比值等对ｄｔ／ｄＥ～Ｅ溶出曲线的影响。并得出了连测铜铅的条件。     

金－钼酸盐－耐尔蓝缔合显色反应的研究

在聚乙烯醇存在下，金与钼酸盐形成络阴离子，继而与耐尔蓝形成离子缔合物，其最大吸收位于５９５ｎｍ，表现摩尔吸光系数ε值为２．７１×１０￣５Ｌ．ｍｏｌ￣（－１）．ｃｍ￣（－１），线性范围０～１６μｇ／２５ｍＬＡｕ，大多数离子不干扰。用于岩矿和冶金产品中金的测定，结果满意。