反相流动注射化学发光法测定单宁

在碱性介质中 ,单宁对高碘酸钾氧化鲁米诺的化学发光反应有较强的增敏作用 ,据此建立了反相流动注射化学发光测定单宁的新方法 ,并研究了最佳反应条件。该方法快速、准确、线性范围宽 ,测定单宁的检出限为 1 .1 2× 1 0 - 9g/ m L,方法的线性范围为 2 .0× 1 0 - 8～ 6 .0× 1 0 - 6 g/ m L,对于 4.0× 1 0 - 6 g/ m L单宁 1 0次测定的相对标准偏差为 0 .79%。应用于中药五倍子、诃子中单宁的测定 ,结果满意     

μ-氧-双[三(对氟苄基)锡]的合成、表征及晶体结构

The μ-oxygen-bis[tri(p-fluorobenzyl)tin] was synthesized. The structure were characterized by elementary analysis, IR and ¹H NMR and the crystal structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to rhombohedral with space group R, a=1.346 4(4), b=1.346 4(4), c=1.772 9(7) nm, α=90°, β=90°, γ=120°, Z=3, V=2.783 2(15) nm³, D_c=1.625 g·cm^-3, μ(Mo Kα)=1.408 mm^-1, S=1.088, F(000)=1 350, R₁=0.027 5, wR₂=0.065 9. In compound, the tin atom has a distorted tetrahedral coordination configuration. CCDC: 257079.     

稀土高氯酸盐-谷氨酸配合物[Pr2(L-α-Glu)2(ClO4)(H2O)7](ClO4)3•4H2O的低温热容和热化学研究

合成了一种稀土高氯酸盐-谷氨酸配合物. 经TG/DTG、化学和元素分析、FTIR及与相关文献对比, 确定其组成为[Pr₂(L-α-Glu)₂(ClO₄)(H₂O)₇](ClO₄)₃•4H₂O, 纯度为99.0%以上. 利用显微熔点仪分析发现其没有熔点. 在78～370 K温区, 用精密绝热量热仪测量其低温热容, 在285～306 K温区发现一明显吸热峰, 归结为固-固相变过程. 通过相变温区三次重复热容测量, 得到相变温度T_tr、相变焓Δ_trH_m和相变熵Δ_trS_m分别为(297.158±0.280) K, (12.338±0.016) kJ•mol^－1和(41.520±0.156) J•K^－1•mol^－1. 用最小二乘法将非相变温区的热容对温度进行拟合, 得到了热容随温度变化的两个多项式方程. 用此方程进行数值积分, 得到每隔5 K的舒平热容值和相对于273.15 K的热力学函数值. 根据TG/DTG结果, 推测了该配合物的热分解机理. 依据Hess定律, 选择1 mol•dm^－3盐酸为量热溶剂, 利用等温环境溶解-反应量热计, 测定了该配合物的标准摩尔生成焓为: Δ_fH_m⁰＝－(7223.1±2.4) kJ•mol^－1.     

含羧酸配体的鼓形有机锡氧簇合物：六聚苯基锡氧3-吲哚丁酸酯的合成及晶体结构

利用Ph3SnOH和3-吲哚丁酸以1：1摩尔比反应，合成了新型含羧酸配体的鼓形 有机锡氧簇合物：六聚苯基锡氧3-吲哚西酸酯。通过元素分析、红外光谱和X射线 单晶衍射对其结构进行了表征。测试结果表明：该化合物为三斜晶系，空间群P1， a=1.1722(6),b=1.5694（8）nm，c=1.7227(9)nm，α=116.251（8）°，β=100. 854（10）°，γ=95.606（9）°，Z=1，V=2.732(3)nm^3，Dc=1.554g·cm^-3，μ =1.420mm^-1，F(000)=1276，R=0.0630，ωR=0.0762。晶体结构中，六配位的锡原 子呈畸变的八面体构型。     

催化光度法测定痕量对苯二酚

在硫酸介质中，以草酸为活化剂，痕量对苯二酚对碘酸钾氧化天青Ⅱ的褪色反应具有明显的催化作用，据此建立了催化光度法测定痕量对苯二酚的新方法。方法的线性范围是0．04～1．20mg／L，检出限为0．008mg／L。方法操作简便，灵敏度高，选择性好，用于自来水、实验室废水和显影液中对苯二酚的测定，结果满意。     

亲和层析在蛋白质研究中的应用进展

文中介绍了生物、免疫、固定化金属离子拟生物几类常规亲和层析的原理及其在蛋白质分离纯化以及分析鉴定方面的应用（引用文献25篇）。     

具有S…S、S…Cl作用的一维链状有机锡化合物氯代二苄基锡哌啶荒酸酯的合成、表征及晶体结构

The chlorodibenzyltin dithiopiperidylcarbamate was synthesized by the reaction of dibenzyltin dichloride with dithiopiperidylcarbamate and was characterized by elemental analysis， IR and ¹H NMR. The crystal structure was determined by X-ray single crystal diffraction. The crystallographic data are as follows： monoclinic， space group P2₁， a=0.63464(13)nm， b=1.9110(4)nm， c=0.87367(17)nm， β=97.67(3)°， Z=2， V=1.0501(4)nm³，D_c=1.571g·cm^-3， μ=1.546mm^-1， F(000)=500， R=0.0209， wR=0.0381 [I≥ 2σ(I)]. The str- uctures consist of discrete molecules containing five-coordinate tin atoms in a seriously distorted trigonal bipyramidal configuration. The molecules are packed in the unit cell in one-dimensional chain complex through a weak inter-action between the chlorine atom， the sulfur atom and one of the other sulfurs of an adjacent molecule. CCDC： 180034.     

铋配合物[Bi(S2CNC5H10)2(NO3)]·[1，10-Phen]·0.5H2O的合成及晶体结构

The bismuth complex with dithiopiperdylcarbamate [Bi(S₂CNC₅H₁₀)₂(NO₃)]·[1，10-Phen]·0.5H₂O was synthesized. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal belongs to monoiclinic with space group C2/c, a=3.140(2) nm, b=1.176 4(9) nm, c=2.021 6(15) nm, β=103.081(12)°, V=5.713(7) nm³, Z=8, F(000)=3064, D_c=1.815 g·cm^-3, μ=6.502mm^-1. The final R₁=0.0332, wR₂=0.040 3. In the complex, the bismuth atom is eight-coordinated in a capped distorted pentagonal bipyramidal geometry. CCDC: 222655.     

二聚体有机锡配合物{[n-Bu2Sn(O2CCH2CS2NC4H8)]2O}2的合成，表征及晶体结构(英)

The title compound, {[n-Bu₂Sn(O₂CCH₂CS₂NC₄H₈)]₂O}₂, has been synthesized by the reaction of (tetrahydro-pyrrodithiolocarbamoylthio)acetic acid with the di-n-bubyltin oxide in 1∶1 molar ratio. The complex has been characterized by elemental analysis, IR and NMR. The crystal structure of it has been determined by X-ray single crystal diffraction. And the results showed that the crystal belongs to triclinic system with space group P1 and some crystal parameters: a=1.220 2(9) nm, b=1.315 8(10) nm, c=1.380 4(10) nm, α=111.215(9)°， β=99.357(9)°， γ=96.075(10)°, V=2.006(2) nm³, Z=1, F(000)=908, μ=1.489 mm^-1, D_c=1.474 g·cm^-3, R₁=0.037 5, wR₂=0.0839. The complex has a centrosymmetric dimer structure mode with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom which has a distorted octahedron. Each of the endo-cyclic tin atoms exhibits a distorted trigonal bipyramid coordination geometry with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are bidentate and connecting to each of exo-cyclic tin atoms by using both oxygen atoms, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom only. CCDC: 220513.     

考马斯亮蓝-SLS体系共振瑞利散射法测定蛋白质

研究了考马斯亮蓝与蛋白质的结合反应。在十二烷基磺酸钠的存在下,于pH1.6的酸性介质中,蛋白质与考马斯亮蓝可形成复合物,使最大波长351 nm的共振光散射光谱得到加强,据此,用于蛋白质的定量测定。十二烷基磺酸钠的加入,可使灵敏度提高3.2倍。本法测定牛血清白蛋白、人血清白蛋白、卵蛋白、γ-球蛋白的线性范围分别为:0.04~0.8、0.03~0.5、0.04~1.00、.06~1.2 mg/L,检出限分别为:6.3、4.7、7.9、9.2μg/L。已用于人血清、牛奶、豆浆、尿液中蛋白质的测定,所得结果与经典的考马斯亮蓝法一致。