羧基化多壁碳纳米管修饰碳糊电极用于溶出伏安法测定铋(Ⅲ)量

将羧基化的多壁碳纳米管滴涂在碳糊电极表面上,应用羧基化的多壁碳纳米管修饰碳糊电极(MWCNT-COOH/CPE)测定铋(Ⅲ)时,将试液在0.1mol.L-1盐酸溶液中在-500mV处预富集120s,使铋(Ⅲ)与1-(4-磺酸基苯基)-3-[4-(苯基偶氮)-苯基]-三氮烯(SPAPT)生成络合物,然后在-500～500mV范围内扫描,使络合物中的铋(Ⅲ)从电极上溶出,实现了铋离子的溶出伏安法测定。在-32mV处可得铋离子的氧化峰电位,其峰电流值与铋(Ⅲ)浓度在1.0×10-9～4.0×10-7 mol.L-1范围内呈线性关系,检出限(3S/N)为3.0×10-10 mol.L-1。     

载铁(Ⅲ)-配位体交换棉纤维素吸附剂对饮用水中砷(Ⅴ)和氟联合去除的研究

使用新型载铁(Ⅲ)-配位体交换棉纤维素吸附剂,通过静态和动态吸附实验,研究了饮用水中砷酸钠[砷(Ⅴ)]和氟化钠(氟)联合去除的效果和浓度因素的影响以及吸附剂经过反复吸附-洗脱再生-再吸附后性能的稳定性.结果表明,该吸附剂能够高效、高选择性地联合去除高砷(Ⅴ)和高氟.吸附柱的饱和吸附容量可高达15mg/g干重,反复使用中饱和体积的相对标准偏差小于0.5%,柱处理出水的各项有关指标均符合我国生活饮用水卫生标准,特别是砷(Ⅴ)的质量浓度低于0.010mg/L,符合世界健康组织(WHO)推荐的饮用水严格砷标准.说明该吸附剂在砷氟共存的地区具有很好的应用前景.     

顺式-二(乙二胺)二硝基合钴(Ⅲ)苹果酸盐的晶体结构及手性识别

合成了标题化合物，并用X-射线衍射法确定了该分子的晶体结构。化合物Δ（λλ），Λ（δδ）－cis－[Co（en）2（NO2）2]2d，l-C4H4O5，Co2C12N12O13H22，Mr=657．94．晶体属单斜晶系，空间群为P21/c，晶胞参数：a=13．969（4），b=6.440（1），c＝14．408（4）A，β=94.37（1）°，V=1292．3A3，Z=2，Dc=1．69g／cm3，μ=105.833cm－1，F（000）=668.最终偏离因子R=0.066，Rw=0．085。结构分析表明晶体存在无序现象，其阴离子C4H4O52-有两种排列方式。R-构型和S-构型的几率各为50％，手性识别是通过Δ构型的阳离子与阴离子R-构型C原子上羟基氧形成氢键相互作用；Λ构型的阳离子与阴离子S-构型C原子上羟基氧形成氢键相互作用而实现的。     

Syntheses and Crystal Structures of Two New Main Group Metal Complexes （M = Al, Bi） with the Substituted p-Hydroquinones

The title complexes [Al(Hcah)(H2O)2]·2H2O (A) and [Bi(Hcah)(H2O)]n (B), where H4cah = 2-[N,N-bis(carboxymethyl)aminomethyl] hydroquinone, have been synthesized and characterized using X-ray single-crystal structure determination, IR and elemental analysis. Both complexes crystallize in the monoclinic system, space group P21/c with a = 7.8660(16), b = 10.096(2), c = 19.053(4) and β = 93.50(3)° for A; and those for B: a = 9.2348(18), b = 7.9061(16), c = 17.141(3) and β = 102.64(3)°. In addition, further investigation revealed that the central Al(III) ion in the mononuclear complex A is in a distorted octahedral coordination geometry, while structural analysis reveals that the Bi(III) ion is in a distorted pentagonal bipyramid, forming a 2-D polymeric complex B, and the coordination network is a 2D 4.82 net. The TG analyses of A indicate two steps of water loss.     

锰、铑原卟啉IX-二甲酯配合物共振拉曼光谱研究

合成了MnPPCl,RhPPCl,RhPPN3,RhPP(CO)Cl四种配合物 (PP =ProtophyrinIXDimethy1Ester) ,用元素分析、红外吸收光谱及紫外吸收光谱确定了配合物的组成 ,测定了它们的共振拉曼光谱 ,对特征谱带进行了归属。分析了拉曼谱带和电子吸收谱带变化的原因 ,提出了谱带频率的变化受金属离子外层d电子和轴配体的影响。     

Crystal Structure Analysis of Tetras[L-tris(ethylenediamine) cobalt(Ⅲ)] tris[hexacyanoruthenate(Ⅱ)]

1 INTRODUCTION The tris(ethylenediamine) cobalt (Ⅲ) complex in which there are L and D configurations is one of the very interest cations due to the chirality among research complexes and the characterization of reaction on the ion-pair charge-transfer transitions. It has been mentioned in a lot of examples on the chirality and the structure, such as [L-Co(en)3]- [?Co(edta)]2Cl?0H2O[1], [(+)DCo(en)3]Cl3稨2O[2], [(+)-Co(en)3?-)-Cr(en)3]Cl?.1H2O[3], [()-Co(en)3] (SCN)3[4], [(+)D…     

双波长双指示剂催化动力学光度法测定痕量Fe(Ⅲ)

研究了在HCl介质中,Fe(Ⅲ)催化H2O2氧化甲基橙和亚甲基蓝褪色的指示反应。通过测量510nm和660nm波长处催化和非催化体系吸光度的变化,基于Fe(Ⅲ)的浓度与两波长处吸光度差值的加和呈线性关系,建立了双波长双指示剂催化动力学光度法测定Fe(Ⅲ)含量的新方法。方法的线性范围为0.008~0.24μg/mL,用该法测定菠菜、紫菜、蛋黄中Fe(Ⅲ)含量,相对标准偏差为1.0%~4.6%,加标回收率为98.9%~104.6%。     

具有双螺旋链结构的3-吡啶丙烯酸镝配合物的水热合成及晶体结构

采用水热法制备了一种新型稀土配位聚合物[Dy(3-PA)3(H2O)]n(3-PA=3-吡啶丙烯酸)(1),并通过X射线单晶衍射结构分析、元素分析、红外光谱、热重分析对配合物1进行了结构表征.结构分析表明,标题配合物属于三斜晶系,Pī空间群,晶胞参数为:a=0.617 16(5)nm,b=1.270 45(11)nm,c=1.564 03(13)nm,α=111.557 0(10)°,β=90.307 0(10)°,γ=95.342 0(10)°,V=1.134 54(16)nm3,Z=2.金属离子Dy(III)通过配体3-AP羧基的桥联作用,链接成为一维双螺旋链状配位聚合物.     

2-十四烷基-DTPA及其钆(Ⅲ)螯合物的合成与表征(英)

Synthesis and characterization of the ligand, [2-tetradecyl-3,6,9-tris(carboxymethyl)-3,6,9-triazaundecan-1,11-dioic acid, H₅L] and its Gd(Ⅲ) chelate are described. Protonation constants for H₅L (lgK_i^H = 10.80, 8.40, 4.30, 2.80, 2.15) and the stability constant for GdL^2- (lgK_GdL^2-= 22.75) were determined by potentiometric titration and are similar with the related values of DTPA and Gd-DTPA respectively. The results obtained show that the basicity of the ligand and the stability constant of its Gd(Ⅲ) chelate are not obviously altered after introduction of a linear chain tetradecyl group at the terminal acetic acid residue of DTPA.     

Highly efficient regioselective ring openings of N-tosylaziridines to haloamines using ferric(Ⅲ) halides

FeX3（X = Cl, Br） were found to be very effective reagents and powerful catalysts for regioselective ring openings of a variety of N-tosylaziridines with them to afford the corresponding b-haloamines in good to excellent yields with high regioselectivity under mild conditions. At the same time, 13 new compounds were obtained firstly. Moreover, the b-bromoamine prepared could be transferred into b-nitroamine with NaNO2 in moderate yield.