高压消解-原子荧光光谱法同时测定豆科6种中药材中的砷和汞

采用HNO3+ HC1预消解、HNO3+ H2O2高压消解,硫脲-抗坏血酸预还原等手段,建立了高压消解-双道氢化物发生-原子荧光光谱同时测定豆科中药材中砷和汞含量的分析方法.讨论并优化了分析测定条件,结果表明:砷和汞的线性范围分别为0-150、0-90.0ng·mL-1,相关系数分别为0.9992、0.9981,检出限分别是0.0879ng ·mL-1和0.012ng·mL-1;相对标准偏差(n=6)砷不大于5.17％,汞不大于5.14％.应用于豆科6种中药材砷和汞含量的测定,该方法操作性强、用时短、灵敏度高.     

高压消解-双道氢化物发生-原子荧光光谱法同时测定女贞属苦丁茶中砷与汞

采用HNO3/H2SO4常压预消解,HNO3/H2O2高压消解,硫脲-抗坏血酸溶液预还原等手段,建立了高压消解-双道氢化物发生-原子荧光光谱法同时测定女贞属苦丁茶中砷和汞含量的新方法。考察并优化了分析条件。该方法砷与汞的检出限分别是4.73×10-5 mg.L-1、8.7×10-6 mg.L-1;相对标准偏差(n=10)砷小于2.15%,汞小于3.47%。方法可应用于女贞属六种苦丁茶中砷和汞的测定。     

具有Cl…Cl作用的一维链状有机锡化合物四(2，4-二氯苄基)锡的合成、表征和晶体结构

The tetra(2, 4-dichlorobenzyl)tin was synthesized and characterized by elementary analysis, IR and ¹H NMR. The crystal and molecular structure were determined by X-ray single crystal diffraction. The crystal of the title compound belongs to triclinic, space group P1 with a=1.089 7(3) nm, b=1.050 33(4) nm, c=1.858 5(4) nm, α=96.822(4)°, β=94.477(4)°, γ=94.636(3)°, V=3.001 3(12) nm³, Z=4, D_c=1.679 Mg·m^-3, μ(Mo Kα)=1.582 mm^-1, S=1.005, F(000)=1 496, R₁=0.040 7, wR₂=0.076 3. In compound, the tin atom has a distorted tetrahedral coordination configuration. The molecules are packed in one-dimensional chain polymer through a weak interaction between the chlorine atoms from adjacent molecules, respectively. CCDC: 286106.     

有机锡配合物{[(n-C8H17)2Sn(O2CCH2CS2NC4H8O)]2O}2的合成，表征及晶体结构

The title complex {[(n-C₈H₁₇)₂Sn(O₂CCH₂CS₂NC₄H₈O)]₂O}₂ has been synthesized by the reaction of (morpholinylthiocarbamoylthio)acetic acid with the di-n-octyltin oxide in 1∶1 molar ratio. The complex was characterized by elemental analysis, IR and ¹H NMR. The crystal and molecular structure of complex was determined by X-ray single crystal diffraction. The crystal belongs to triclinic system with space group P1 and unit cell dimensions: a=1.201 5(9) nm, b=1.481 8(11) nm, c=1.894 1(14) nm, α=72.485(10)°, β=88.586(10)°, γ=66.893(9)°, and Z=1, μ=1.034 mm^-1, V=2.941(4) nm³, D_c=1.295 g·cm^-3, F(000)=1 196, R₁=0.058 8, wR₂=0.155 8. The complex is a centrosymmetric structure with a four-membered central endo-cyclic Sn₂O₂ unit in which two bridged oxygen atoms both connect with an exo-cyclic tin atom. The endo-cyclic tin atoms and the exo-cyclic tin atom are all five-coordinate and have coordination geometry of distorted trigonal bipyramid with an additional weak coordination carboxylate oxygen. Four carboxylate ligands are divided into two types. And two of them are monodentate and connecting to each of exo-cyclic tin atoms by using one oxygen atom, whereas the others bridge to each pair of exo-and endo-cyclic tin atoms utilizing one oxygen atom. CCDC: 277048.     

高压消解-双道氢化物发生-原子荧光光谱法同时测定苦丁茶原植物中的砷和汞

采用HNO3/H2SO4预消解、HNO3/H2O2高压消解,硫脲-抗坏血酸预还原等手段,建立了高压消解-双道氢化物发生-原子荧光光谱同时测定苦丁茶原植物中砷和汞含量的分析方法。讨论并优化了分析测定条件,结果表明,砷和汞的线性范围分别为1.0×10-3—11.0×10-3mg.L-1和1.0×10-4—10.0×10-4mg.L-1,相关系数r分别为0.9986、0.9970,检出限分别是4.73×10-5mg.L-1和8.70×10-6mg.L-1;相对标准偏差(n=6)砷不大于4.25%,汞不大于4.92%。应用于5种苦丁茶原植物砷和汞含量的测定,该方法操作性强、用时短、灵敏度高。     

有机锡化合物四对氰苄基锡(p-NCC6H4CH2)4Sn的合成、表征和晶体结构

The organotin(Ⅳ) compound (p-NCC₆H₄CH₂)₄Sn was synthesized by the reaction of p-cyanobenzyl chloride with tin. The compound was characterized by elemental analysis, IR, ¹H NMR, and the crystal structure was determined by X-ray single crystal diffraction. The crystal belongs to triclinic, space group P1 with a=0.894 1(4) nm, b=0.977 9(4) nm, c=1.796 8(8) nm, V=1.386 9(11) nm³, Z=2, D_c=1.397 Mg·m^-3, μ(Mo Kα)=0.948 mm^-1, F(000)=588, R₁=0.046 9, wR₂=0.101 4. The tin atom adopts a distorted tetrahedral coordination geometry. CCDC: 272939.     

催化动力学光度法测定维脑路通片及槐米中维生素P4

在HAc存在下,少量维生素P4可催化KBrO3氧化丙基红的反应,导致丙基红在521 nm处吸光度显著减小,据此建立了测定维生素P4含量的催化动力学新体系.其线性范围为0.01～0.9 mg/L,检出限为8.9×10-3 mg/L,催化反应总速率常数为9.90×10-4/s.该方法可用于维脑路通片剂和槐米中维生素P4含量...