移动氢源用铝合金制氢技术研究

铝具有资源丰富、价格低廉、易保存、水解产氢量大(1244mLg-1)等特点,是NaBH4水解产氢的理想替代品[1].本文用机械球磨法制备了系列铝合金,并对其与水反应产氢的性能进行了研究.结果表明:锡和铋能提高铝的活性,其与铝形成的合金能在常温下与水反应.但铝锡合金在常温下与水反应速度缓慢,而铝铋合金能与水迅速反应,产氢率可达80%.     

中成药中铝含量的光度法测定

研究了二溴羟基苯基荧光酮与铝的显色体系。在Tween-80及F-存在下,铝与二溴羟基苯基荧光酮在碱性介质中形成1∶2的玫瑰红色四元配合物,最大吸收波长558 nm,摩尔吸光系数1.5×105L.mol-1.cm-1,铝含量在0~0.24μg/mL符合比尔定律。方法灵敏,选择性好,用于中成药中微量铝的测定取得满意结果。     

酸性媒染紫一示波计时电位法测定天然水不同形态铝

本文报道酸性媒染紫(SVRS)一示波计时电位法测定天然水中不同形态铝.对24个实际水样分别在酸性pH5.2测定了无机单核铝Ali和碱性pH8.8底液中测定总单核铝A1a,有机单核铝Al.=A1a-Ali.同时还应用该法测定了酸化水样中总铝AlT,酸溶态铝Alr=AlT-A1a,从而实现了水样中五种形态铝的电化学测定.测定值与DriSColl方法进行了比较对照,结果基本一致.本法特点为简便快捷,灵敏准确,可以直接测定与铝毒性密切相关的无机单核铝A1i,无需分离步骤,水样用量小,适用于大批量天然水样中Al形态的快速分析.     

铍试剂Ⅲ/钙色素双偶氮染料-示波计时电位法快速测定天然水中不同形态铝

采用铍试剂Ⅲ (简称BER)和钙色素 (简称CAL)双偶氮染料 示波计时电位法快速测定天然水中不同形态铝。实验条件和结果如下 :在pH 5 .0NH4Ac HAc缓冲溶液中 ,BER在dE dt E示波图上出现一个切口 ,Ep1 =-0 .3 5V。加入铝后出现一新切口 ,Ep2 =-0 .70V ,该切口深度与加入铝量在 1 .0× 1 0 - 6 ～ 2 .0× 1 0 - 5mol L浓度范围内呈线性关系 ;检出限为 5 .0× 1 0 - 7mol L ;在 5 .0× 1 0 - 6 mol LAl时相对标准偏差为 5 5 % (n=1 0 )。在pH 8.0NH4Ac NH3·H2 O缓冲溶液中 ,CAL在示波图上出现一个切口 ,EP′1 =-0 .60V。加入铝后出现一新切口 ,EP′2 =-0 .75V ,该切口深度与加入铝量在 1 .0×1 0 - 6 ～ 1 .0× 1 0 - 5mol L浓度范围内呈线性关系 ,检出限为 5 .0× 1 0 - 7mol L ;在 2 .0× 1 0 - 6 mol LAl时 ,相对标准偏差为 5 .5 % (n =1 0 )。分别采用两种试剂在弱酸性和弱碱性条件下测定了天然水样中的铝浓度 ,发现在弱酸性下测定的是无机单核铝 ,而在弱碱性下则是总单核铝 ,据此可以实现对 5种铝形态的区分。测定了实际天然水样 ,与Driscoll方法进行了对照 ,结果基本一致     

吸光光度法测定沸石分子筛中铝

铝是构成沸石分子筛的一种主要元素 ,其含量及其在分子筛骨架中的分布直接影响分子筛的应用及性能 ,因此测定其中铝含量具有十分重要的意义。吸光光度法测定铝具有简便快速等优点 ,有关光度法测铝文献 [1 ]已作综述。偶氮胂 (ASAI)是稀土元素显色剂 ,本文探讨了该试剂与 Al( )的显色反应 ,结果表明 ,在 p H4.4邻苯二甲酸氢钾缓冲介质中 ,ASAI可与 Al3 生成桔红色络合物 ,络合物的最大吸收波长为 560 nm,摩尔吸光系数为 1 .30× 1 0 4。用该法测定某些沸石分了筛中铝 ,结果满意。1　试验部分1 .1　主要试剂与仪器铝标准溶液 :1 0 μg·…     

用左旋多巴-示差脉冲伏安法间接测定生物样品中的铝

人体内摄入过多的铝可能导致或促进阿尔茨海默氏病 ( Alzheimer s disease)、帕金森氏病( Parkinson s disease)及透析脑病 ( Dialysis encephalopathy)的发病 [1] .原子吸收光谱法、能量分布 X射线光谱法、 X射线微探针分析法、激光微探针质量分析法和核显微法曾用于测定脑铝 .这些方法在样品制作过程中易被污染 [2 ,3] ,仪器昂贵 ,灵敏度不高 ,而且均不能用于人体液和脑铝的在体检测 .由于铝的还原电位约 - 1 .7V,易受 H+干扰 ,直接测定铝有困难 .吸附伏安法利用铝与染料的配合物的电化学响应来测定环境和生物制品中的铝 ,检测下限达 1…     

微波消解-环丙沙星荧光光度法测定面制食品中铝

铝在自然界中是一种广泛存在的元素,许多科学家经过研究发现,老年性痴呆症与铝有密切关系.同时还发现,铝对人体的脑、心、肝、肾的功能和免疫功能都有损害[1].因此,世界卫生组织于1989年正式将铝确定为食品污染物而加以控制.     

二溴羟基苯基荧光酮-AI-F!~--Triton X-100四元显色体系的研究与应用

研究了二溴羟基苯基荧光酮与铝的显色体系.在Triton X-100及F~-存在下,铝与二溴羟基苯基荧光酮在碱性介质中形成1∶2的玫瑰红色的四元配合物,最大吸收波长559nm.摩尔吸光系数1.46×10~5,铝含量在0～5μg/25ml符合比耳定律.方法灵敏,选择性高,用于镁合金中微量铝的直接测定,取得满意结果.     

2,4-二羟基苯甲醛缩4-氨基安替比林的合成及与铝的荧光反应

合成了新荧光试剂 2 ,4 二羟基苯甲醛缩 4 氨基安替比林 (2 ,4 DHBAAP) ,并测定其结构。基于铝 (Ⅲ )与 2 ,4 DHBAAP CTMAB形成配合物 ,导致体系荧光增敏的特性 ,提出了一种测定微量铝的新荧光方法。在pH 4 .5～ 6 .0的乙酸铵缓冲溶液及CTMAB存在下 ,铝 (Ⅲ )与DHBAAP形成 1∶1的配合物。在λex λem =385 5 15nm处 ,体系产生的荧光增敏程度最大 ,铝量的线性范围为 0～ 15 0 μg·L-1,检出限为 0 .2 μg·L-1。方法用于水样中铝的测定 ,结果满意     

基于铝氟配位反应的动力学-电位法对铝的测定

以氟离子选择性电极作指示电极,用动力学电位法对铝的测定进行了研究.在低pH条件下,铝氟反应E～t曲线的斜率△E/△t与铝的浓度cAl成正比.实验步骤为:第一步,根据铝的校正溶液与氟反应的△E/△t,作出△E/△t～cAl工作曲线;第二步,根据铝试液与氟反应的△E/△t,求出铝的浓度.合适的实验条件是:pH范围1～2;温度范围288～303 K;铝的浓度范围1×10-3～5×10-2mol/L;加入的氟的浓度范围5×10-4～5×10-2mol/L.此外,对动力学电位法测定铝的计算式进行了理论推导,对该法存在的问题、可以采取的措施及误差的分布进行了讨论.     

SAAQ-CTMAB荧光光度法测定微量铝的研究

某些席夫碱具有一定的刚性平面及富电子的共轭体系 ,从而使其显示出良好的荧光特性 ,导致该类试剂在荧光分析中显出越来越重要的作用[1 ] 。虽然荧光法测定铝已有文献[2～4] 报道 ,但本文所提出的ＳＡＡＱ在ＣＴＭＡＢ存在下与铝产生荧光增敏测定微量铝的方法尚未见报道。研究表明在ｐＨ =4.0～ 5.5的乙酸铵缓冲溶液及ＣＴＭＡＢ存在下 ,铝与ＳＡＡＱ形成 1∶2的络合物。该络合物在λｅχ/λｅｍ=378ｎｍ/490ｎｍ处荧光最强 ,线性范围为 0～ 2 0 0 μｇ·ｄｍ- 3,方法用于人发及茶叶中铝含量的测定 ,结果满意。1　试验部分1 .1　仪器与试剂…     

Selective extraction of gallium from aluminum and indium using tripod phenolic ligands

Solvent extraction of trivalent group 13 metal cations such as aluminum, gallium and indium with tripod quadridentate phenolic ligand, tris(2-hydroxy-3,5-dimethylbenzyl)amine (H(3)tdmba), was investigated as fundamental study for their mutual separation. Gallium was extracted almost quantitatively as Ga(tdmba) (logK(ex)=-6.66+/-0.06 on using chloroform as extraction solvent), whereas aluminum and indium were hardly extracted due to steric hindrance on complexation of them with the ligand. The extracted Ga species was estimated as trigonal bipyramidal complex with one H(2)O molecule. Furthermore, extractability of Ga was increased by changing the ligand to more acidic tris(5-chloro-2-hydroxy-3-methylbenzyl)amine (H(3)tcmba) (logK(ex)=-6.18+/-0.18 on using dichloroethane as extraction solvent).     

Binding of hydroxychromones with Al in methanol

The chelation of 3-hydroxy-, 5-hydroxy- and 5,7-dihydroxychromone with Al³⁺ was studied spectrophotometrically. Both the molar ratio method and method of continuous variation (Job’s method) were used to determine the composition of the complexes. In all cases, complex formation involved 1:1 aluminum ion to hydroxychromone ratios. For the 5-hydroxy and 5,7-dihydroxy derivatives, this composition agrees with that for the corresponding hydroxyflavone. However, 3-hydroxyflavone (flavonol) forms a 2:1 complex with Al³⁺ in methanol in contrast to the results for 3-hydroxychromone in this study. The importance of the cinnamoyl mesomeric form for stabilizing the complex between flavonol and Al³⁺ is invoked to explain this discrepancy.     

A sequential injection method for the fluorimetric determination of aluminum in drinking water using 8-hydroxy-7-(4-sulfo-1-naphthylazo)-5-quinoline sulfonic acid

A robust and simple sequential injection (SI) method for the assay of aluminum ions in drinking water is described. The method is based on the complex formation between aluminum and 8-hydroxy-7-(4-sulfo-1-naphthylazo)-5-quinoline sulfonic acid (HSNQ). The fluorescence of the complex is monitored at an emission wavelength of 492 nm with excitation at 357 nm. The HSNQ concentration, aspirated reagent and sample volumes were optimized simultaneously using 3(3) full factorial design. The optimum operating conditions are aspirated sample and reagent volumes of 90 and 70 microL, respectively, and HSNQ concentration of 20 microM. With these conditions linear calibration curves were obtained from 100 to 800 ppb. The detection limit was 4 ppb. The maximum relative standard deviation of the method was 1.43% (n=5). The method was successfully applied for the determination of aluminum in drinking water samples.     

一种PS给体模型化合物的合成和性能

为了模拟植物光系统的给体部分,设计、合成了配合物2.在该模型化合物中,配体的邻位被2个{[2-羟基-3-(吗啉基-4-甲基)-5-叔丁基-苄基](吡啶-2-甲基)胺基-甲基}取代的苯酚通过酰胺键与光敏体[Ru(bpy)3]2+共价相连.利用ESI-MS和1D,2DNMR(gCOSY,HSQC和HMBC)对化合物结构进行了鉴定,并通过UV-Vis、荧光发射光谱、闪光光解及电化学对其光化学性能和氧化还原特性进行了研究.结果表明,化合物的吸收波长发生红移;激发态寿命长;可螯合双核高价Mn()原子;且Ru3+/Ru2+的氧化电位比Phenol+/Phenol和Mn(,)/Mn()的高,满足自然界PS电子转移的基本要求,可用于PS给体部分的初步研究.     

Spectroscopic and Structural Study of the 1:2 Aluminium(III) Complex of Quercetin

Quercetin (3, 3’, 4’, 5, 7-pentahydroxyflavone) is one of the most common flavonols present in nature. The complexation of Al(III) by various flavonoids has been suggested to reduce the overload of aluminum in the diet, a metal which has been implicated…     

含羟基基团取代的氮氧自由基构筑的三个双核稀土化合物的结构及磁性表征

以三氟乙酰丙酮(tfac)为共配体的稀土配合物分别与5-溴-2-羟基苯取代的自由基配体和5-硝基-2-羟基苯取代的自由基配体进行反应,合成3个稀土-自由基配合物[Ln2(tfac)4(NIT-5Br-2PhO)2](Ln=Gd (1),Dy (2))和[Dy2(tfac)4(NIT-5NO2-2PhO)2](3)(NIT-5Br-2PhOH=2-(2′-hydroxy-5′-bromophenyl)-4,4,5,5-tetramethylimidazoline-1-oxyl-3-oxide,NIT-5NO2-2PhOH=2-(2′-hydroxy-5′-nitrophenyl)-4,4,5,5-tetra-methylimidazoline-1-oxyl-3-oxide)。单晶结构分析表明这3个化合物中的稀土离子均通过自由基配体上的羟基氧基团连接为双核的结构。配合物1的直流磁化率表征揭示了Gd(Ⅲ)离子间的反铁磁耦合对其磁行为起主要作用。     

Langmuir-Blodgett Films from Schiff Base Aluminium (Ⅲ) Complex

The characteristics of the LB films of Schiff base aluminium(Ⅲ), tris(2-hydroxy-5-nitro-N-dodecyl-benzylideneaminato) aluminium(Ⅲ)[Al(TA12)_3], were studied. The surface pressure-area(π-A) isotherm of Al(TA12)_3 in the pure water subphase was investigated. The molecular area, 0.48 nm~2, is one-third of the expected value that indicates the formation of an aggregate. The Langmuir-Blodgett(LB) films of Al(TA12)_3 were transferred and characterized. The UV-Vis spectra and the AFM image both confirmed that the J-aggregates formed. The polarized UV-Vis spectra indicated that the complex plane had to be oriented with an angle of about 30° to the substrate surface. The IR spectra suggested that the complexation took place between aluminium ions and the oxygen atoms of the ligand rather than the nitrogen atom.     

偶氮胂酸型荧光试剂测定铝的研究

比较了５种新试剂及偶氮胂－Ｉ的铝铬合物的荧光性能，讨论了试剂结构与性能之间的关系。试验出７－〔（４－甲基－２－胂酸基苯）偶氮〕－８－羟基喹啉－５－磺酸为铝的优良荧光试剂，并用其测定茶叶、含茶叶饲料，以及大白鼠排泄物中的铝和水样中的铝，结果满意。     

Steric stabilization of a monomeric proalumatrane: experimental and theoretical studies

Treatment of tripodal tris(3-tert-butyl-2-hydroxy-5-methylbenzyl)amine (L) with 1 equiv of trimethylaluminum in toluene gave the stable proalumatrane (AlL) (1) [wherein L = tris(3-tert-butyl-5-methyl-2-oxidobenzyl)amine] featuring a distorted trigonal monopyramidal four-coordinate aluminum geometry. An analogous reaction uses the less sterically congested isomer of L, namely, tris(5-tert-butyl-2-hydroxy-3-methylbenzyl)amine provided dimeric (AlL')2 (2) [wherein L' = tris(5-tert-butyl-3-methyl-2-oxidobenzyl)amine], which contains two bridging alumatrane moieties possessing five-coordinate TBP aluminum geometries. Reaction of AlL with water provided the adduct H2O.AlL (3), a species that is representative of a coordinatively stabilized intermediate in the hydrolysis of an aluminum alkoxide. Theoretical calculations revealed that considerable stabilization energy is obtained by the coordination of a water molecule to the tetracoordinate aluminum in AlL and that this result is consistent with the postulate that the Lewis acidity of AlL exceeds that of boron trifluoride, despite the presence of the transannular N-->Al bond in AlL.