2－（2－噻唑偶氮）－5－〔N，N－二羧基甲基）氨基〕苯酚的分析特性和钴测定的研究

研究了新显色剂２－（２－噻唑偶氮）－５－［（Ｎ，Ｎ－２羧基甲基）氨基］苯酚（ＴＡＤＣＡＰ）与金属离子的显色反应，着重探讨了试剂与Ｆｅ￣（３＋）、Ｃｏ￣（２＋）、Ｎｉ￣（２＋）、Ｃｕ￣（２＋）、Ｚｎ￣（２＋）、Ｍｎ￣（２＋）显色反应的最佳条件，测定了这些络合物的络合比和稳定常数等，同时建立了钴的分析方法，并用于维生素Ｂ＿（１２）注射液中Ｃｏ￣（２＋）的测定。     

以磷酸三丁脂为载体的乳状液膜迁移、分离稀土元素的研究──Sm（Ⅲ）与常见阳离子的分离

用磷酸三丁酯－Ｓｐａｎ８０－二甲苯乳状液膜体系迁移Ｓｍ（Ⅲ）的研究表明，在确定的条件下，可以快速并完全迁移Ｓｍ（Ⅲ）。许多常见离子不能在此条件下通过液膜迁移，故可从含有Ｆｅ￣（２＋）、Ｃｏ￣（２＋）、Ｎｉ￣（２＋）、Ｃｕ￣（２＋）Ｚｎ￣（２＋）、Ｃｄ￣（２＋）、Ｍｎ￣（２＋）等离子混合液中分离出Ｓｍ（Ⅲ），分离效率高。     

铁（Ⅱ、Ⅲ）、钴（Ⅱ）、镍（Ⅱ）、铜（Ⅱ）－MBTAE配合物的反相高效液相色谱分离和测定

本文报道了以２－（６－甲基－２－苯并噻唑偶氮）－５－二乙氨基酚（ＭＢＴＡＥ）作柱前衍生化试剂，在ＳｐｈｅｒｉｓｏｒｂＣ＿８柱上，以甲醇：水＝８０：２０（Ｖ／Ｖ），含２ｍｍｏｌ／ＬＬｉ＿２ＳＯ＿４和１０ｍｍｏｌ／ＬｐＨ５．０醋酸盐缓冲溶液作流动相，反相高效液相色谱分离和测定了Ｆｅ￣（２＋）、Ｃｏ￣（２＋）、Ｎｉ￣（２＋）和Ｃｕ￣（２＋）。各金属离子的检出限（Ｓ／Ｎ＝３）分别为（ｐｇ）：Ｆｅ￣（２＋）６．４０，Ｃｏ￣（２－）１．３８，Ｎｉ￣（２＋）４．４７，Ｃｕ￣（２＋）７．２８。方法用于欧洲标准局，黑麦草标样的分析，所得结果与标准值相符。     

喹啉基氮杂大环铜,镍配合物的结构和性质差异

喹啉基氮杂大环铜、镍配合物的结构和性质差异安道利，卜显和，李金亮，陈荣悌（南开大学化学系，天津３０００７１）二氧四胺大环配体是Ｃｕ￣（２＋）、Ｎｉ￣（２＋）、Ｃｏ￣（２＋）、Ｐｔ￣（２＋）等金属离子的优良配体，它们同时具有饱和大环多胺和寡聚肽的结构特...     

含硫脲基开链冠醚的合成（Ⅲ）

含硫脲基开链冠醚的合成（Ⅲ）韩江华，白宝林，赵明根（山西省忻州师范专科学校，忻州，０３４０００）关键词：合成，硫脲，开链冠醚，络合剂文献￣［１］报道类化合物可以络合：等１８种阴离子，在不同条件下也可以络合Ｎｉ￣（２＋）、Ｃｏ￣（２＋）、Ｃｕ￣（２＋）...     

离子色谱法快速同时测定营养药物中微量铜、锰、锌

在ＨＰＬＣ－ＣＳ５阳离子分离柱上选用５．０×１０￣（－２）ｍｏｌ／Ｌ草酸（ｐＮ为５．２４）作淋洗液分离了微量Ｃｕ￣２＋、Ｍｎ￣２＋和Ｚｎ￣２＋离子,用４－（２－吡啶偶氮基）间苯二酚作显色剂在５２０ｎｍ处连续检测,方法快速、简便、准确。本法用于施尔康片中微量Ｃｕ￣２＋、Ｍｎ￣２＋和Ｚｎ￣２＋离子的测定,结果令人满意。     

新试剂N－烯丙基－N′－（氨基对苯磺酸钠）硫脲（ASATu）的合成、表征及其反应性能的研究

本文报道了新试剂Ｎ－烯丙基－Ｎ′－（氨基对苯磺醚钠）硫脲（ＡＳＡＴｕ）的合成并确定了结构。该试剂与４５种元素在不同介质中反应，仅有Ｃｕ￣（２＋）、Ａｇ￣＋、Ｂｉ￣（３＋）、Ｈｇ￣（２＋）和Ｆｅ￣（３＋）等离子产生特征性反应。实验证明，它可作为Ｃｕ￣（２＋）、Ａｇ￣＋等新的鉴定试剂；在酸性和近中性介质中测定了该试剂与稀土元素等四十多种金属元素反应的摩尔吸光系数。     

铜（Ⅱ）－聚丙烯酰胺和铜（Ⅱ）－聚乙烯醇配位聚合物的配位数

配位聚合物ＰＡＡｍ－ＣｕＣｌ＿２和ｃｕＣｌ＿２·２Ｈ＿２Ｏ的Ｃｕ￣（２＋）２ｐＸＰＳ谱上都有Ｓｈａｋｅ－ｕｐ峰，其与各自的Ｃｕ￣（２＋）２ｐ３／２肩峰或主峰距离ΔＥｓ２或ΔＥｓ分别为８．７和８．６ｅＶ；但配位聚合物Ｃｕ（Ⅱ）－ＰＶＡ却无此峰．由此推定，前者的Ｃｕ￣（２＋）是以ｓｐ￣３杂化轨道接受ＰＡＡｍ４个链节单元Ｃ－Ｎ上Ｎ的孤对电子部分转移形成配位键；而Ｃｕ（Ⅱ）－ＰＶＡ配位聚合物中的Ｃｕ￣（２＋）却以ｄｓｐ￣２杂化轨道接受ＰＶＡ４个链节单元侧基Ｏ的孤对电子部分转移，产生配位键，即Ｃｕ￣（２＋）与ＰＡＡｍ或ＰＶＡ的链节单元配位比均是１：４，此结果与电导率法测定ＰＡＡｍ－ＣｕＣｌ＿２的配位比相同．     

过渡元素三取代钨锗杂多酸盐异构体的氧化还原性质

用电化学方法研究了过渡元素三取代钨锗杂多酸盐Ｍ＇＿ｘＨ＿ｙ［ＧｅＷ＿９Ｍ＿３（Ｈ＿２Ｏ）＿３Ｏ＿（３７）］·ｎＨ＿２Ｏ（Ｍ＇＝Ｂｕ＿４Ｎ￣＋，Ｋ￣＋；Ｍ＝Ｃｒ￣３＋，Ｍｎ￣２＋，Ｃｏ￣２＋，Ｎｉ￣２＋，Ｃｕ￣２＋）的α－，β－异构体在水溶液中的氧化还原质，提出了它们的还原机理，讨论了取代的过渡元素和杂多阴离子的结构对氧化还原性质的影响，比较了两种异构体的氧化能力。     

氮杂冠醚研究X．双偶氮基开链有色冠醚与过渡金属离子选择配位作用的研究

本文研究了双偶氮基开链有色冠醚１和２与过渡金属离子反应后的紫外可见光谱。实验结果表明：化合物１对Ａｇ￣＋Ｒｄ￣２＋、Ｐｔ￣４＋、Ｎｉ￣２＋和Ｃｒ￣２＋，化合物２对Ｐｄ￣２＋和Ｐｔ￣４＋有明显的选择配位作用，其中２对Ｌｉ￣＋生成配合物时△λ＿（ｍａｘ）很大（１０５ｎｍ），溶液有根明显的变色现象，故２可能用作Ｌｉ￣＋的分光光度显色剂。     

Thermal decomposition behavior of the rare-earth ammonium sulfate R2(SO4)3·(NH4)2SO4

Rare-earth ammonium sulfate octahydrates of R₂(SO₄)₃·(NH₄)₂SO₄·8H₂O (R=Pr, Nd, Sm, and Eu) were synthesized by a wet process, and the stable temperature region for the anhydrous R₂(SO₄)₃·(NH₄)₂SO₄ form was clarified by thermogravimetry/differential thermal analysis, infrared, Raman, and electrical conductivity measurements. Detailed characterization of these double salts demonstrated that the thermal stability of anhydrous R₂(SO₄)₃·(NH₄)₂SO₄ is different between the Pr, Nd salts and the Sm, Eu salts, and the thermal decomposition behavior of these salts was quite different from the previous reports.     

UPLC-MS/MS detection of disaccharides derived from glycosaminoglycans as biomarkers of mucopolysaccharidoses

Mucopolysaccharidoses (MPSs) are a group of disorders resulting from primary defects in lysosomal enzymes involved in the degradation of glycosaminoglycans (GAGs). Depending on the specific enzyme defect, the catabolism of one or more GAGs is blocked leading to accumulation in tissues and biological fluids. GAG measurements are important for high-risk screening, diagnosis, monitoring treatment efficacy, and patient follow up. The dimethylmethylene blue (DMB) spectrophotometric method commonly used in most biochemical genetics laboratories relies on a non-specific total GAG analysis which has led to false positive results, and even false negative results (mainly for MPS III and IV patients). The main objective of our project was to devise and validate a reliable tandem mass spectrometry multiplex analysis for the urine quantitation of four GAGs (dermatan sulfate (DS), heparan sulfate (HS), keratan sulfate (KS), and chondroitin sulfate (CS)) for an eventual technological transfer to the clinic. The developed methodology is rapid (7 min) and our results showed good intraday and interday precision (RSDs ≤ 8.7%) and accuracy (Biases range: −12.0%–18.4%). Linearity was good (r² > 0.995) for DS, HS, CS, and KS calibration curves. In comparison with the DMB spectrophotometric method, this multiplex tandem mass spectrometry method allows GAG fractionation, thus a differentiation of MPS types, except for MPS I and II which are characterized by the same GAG profile. The devised method is a useful and reliable tool for diagnosis of MPS patients, as well as their monitoring and follow up, as shown by longitudinal studies.     

聚硅硫酸亚铁的混凝特性及影响因素

混凝剂;聚合硫酸铁;水处理;聚硅硫酸亚铁的混凝特性及影响因素     

用炼锌厂废泥制取硫酸铜、海绵镉和硫酸锌

研究了以炼锌厂废泥为原料,经氧化、酸浸、中和沉淀、稀硫酸溶解、置换等步骤制取硫酸铜、海绵镉和硫酸锌的工艺.     

Aqueous solubilities of praseodymium,europium, and lutetium sulfates

The aqueous solubilities of finely divided Pr₂(SO₄)₃·8H₂O(cr), Eu₂(SO₄)₃·8H₂O(cr), and Lu₂(SO₄)₃·8H₂O(cr) have been measured as a function of time at 25°C using isothermal saturation. Solubilities of the latter two salts showed a steady decrease with time, whereas Pr₂(SO₄)₃·8H₂O(cr) showed no such variation within the accuracy of the determinations. The turbidities of these filtered saturated solutions also decreased with time, and indicate that some colloidal rare earth sulfates were present. These colloidal particles (<0.2 m) have a large surface area, which contributes to the Gibbs energy of the solid phase, thus giving rise to enhanced solubilities. The micro-particles also grow with time, thereby reducing the surface area contribution to the Gibbs energy and also leaving fewer particles to pass through the filters. Extrapolation of solubilities to infinite time gives the solubilities of macrocurstalline Eu₂(SO₄)₃·8H₂O and Lu₂(SO₄)₃·8H₂O. Previous solubility data for Lu₂(SO₄)₃, at 20 and 40°C, yield an interpolated value at 25°C that is about 30% low. Densities were also measured at several concentrations of each salt.     

Capillary electrophoresis and enzyme solid phase assay for examining the purity of a synthetic heparin proteoglycan-like conjugate and identifying binding to basic fibroblast growth factor

Interaction of basic fibroblast growth factor (bFGF) with heparin/heparan sulfate proteoglycans protects the growth factor against proteolytic degradation and is essential for its cellular activity. Although the structural requirements of heparin and heparan sulfate for the high-affinity binding to bFGF have been extensively examined, studies on intact heparin proteoglycans are limited. In this report, the purity and the binding ability of a heparin proteoglycan-like molecule-the heparin-bovine serum albumin (heparin-BSA) conjugate-was examined using capillary zone electrophoresis (CZE). Furthermore, the affinity of bFGF binding to the heparin-BSA conjugate was studied using an enzyme solid-phase assay. Chondroitin sulfate, dermatan sulfate, hyaluronan, heparan sulfate and variously sulfated disaccharides derived from heparin and heparan sulfate were also studied for their ability to compete with the binding of bFGF to heparin. Heparin-BSA conjugate was synthesized by reductive amination and, following precipitation with 1.5 vols of ethanol-sodium acetate, it was obtained free of contaminating heparin. Heparin-BSA-bFGF conjugate was obtained following incubation of heparin-BSA with bFGF for 2 h at 37 degrees C. Intact heparin, heparin-BSA and heparin-BSA-bFGF conjugates were completely resolved by CZE using 50 mM phosphate, pH 3.5, as operating buffer, reversed polarity (30 kV) and detection at 232 nm. Competitive solid phase assay showed that, among the glycosaminoglycans tested, heparin exhibits the highest affinity binding to bFGF (IC(50) = 6.4 nM). Heparan sulfate showed a lower affinity as compared with that of heparin, whereas all other glycosaminoglycans and heparin/heparan sulfate-derived disaccharides tested showed minute effects. The developed CZE method is rapid and accurate and can be easily used to identify bFGF-interacting heparin preparations of biopharmaceutical importance.     

Ce(SO4)2·xH2O复合CuSO4·yH2O催化剂的制备及其酯化催化性能

硫酸铈;硫酸铜;复合催化剂;酯化反应;Ce(SO4)2·xH2O复合CuSO4·yH2O催化剂的制备及其酯化催化性能     

无机高分子聚合铁盐类混凝剂制备方法评述(英文)

综述了无机高分子聚合铁盐类混凝剂的几种生产制备方法.对用硫酸亚铁经催化氧化法和直接氧化法制备聚合硫酸铁,用各种含铁工业废渣制备复合聚铁,以及采用生物和电化学方法制备聚铁类混凝剂等方法的优缺点等作了较全面评述.还对固体聚合铁的生产及液体聚合铁混凝剂的稳定性进行了讨论,对目前聚合铁生产中存在的问题及发展方向提出了建议.     

Ein neues Lithiumhydrogensulfat,Li2(HSO4)2(H2SO4) – Synthese und Kristallstruktur

A New Lithium Hydrogen Sulfate, Li₂(HSO₄)₂(H₂SO₄) – Synthesis and Crystal Structure The title compound crystallizes in good shaped single crystals from the system lithium sulfate/sulfuric acid in the orthorhombic space group Pccn, unit cell parameters a = 17.645(4), b = 5.378(1), c = 10.667(3) Å. V = 1 012.2 ų, Z = 4, D_x = 2.009 g cm^?3. There are two types of SO₄ tetrahedra, SO₃(OH) and SO₂(OH)₂, connected via hydrogen bonds forming layers parallel to the xy-plane. The layers are linked by Li atoms, which are tetrahedral coordinated by O atoms coming two by two from neighboured layers.