SYNTHESIS AND STRUCTURE OF α''''-ACE-TYL-α-THIENYL PHENYLACETYLENEDI-COBALT HEXACARBONYL AND α''''-ACE-TYL-α-THIENYL P-ACETYLPHENYLACE-TYLENEDICOBALT HEXACARBONYL

Friedel-Crafts acylation of α-thienyl phenylacetylenedicobalt hexacarbonyl with acetyl chlo-ride has been investigated. The results showed thiophene nucleus to be somewhat more reactivein the electrophilic acylation than benzene nucleus and benzene nucleus in turn to be morereactive than acylated thiophene nucleus. Through the acylation two new cobalt- carbon clustercomplexes, i. e. α'-acetyl-α -thienyl phenylacetylenedicobalt hexacarbonyl Ⅰ and α'- acetyl-α-thienyl P- acetylphenylacetylenedicobalt hexacarbonyl Ⅱ, were synthesized. The single crystalstructure of Ⅱ was determined as well as the structures of Ⅰ and Ⅱ were elucidated in termsof combustion analysis, IR and ~1HNMR spectroscopy. The crystal structure of Ⅱ belongsto the monoclinic system, space group Pz_1/n; cell parameters a = 8 .037(2), b = 16 .347(3),c = 17.823(2)A, β= 102.68(2)°, D_c = 1.61g·cm~(-3), Z = 4, and the final factor R = 0.040.     

三苯膦铁硫原子簇配合物(μ-cy-C_6H_(11)S)(μ-n-C_5H_(11)S)Fe_2(CO)_5PPh_3的合成和晶体结构

通过(μ-cy-C_6H_(11)S)(μ-n-C_5H_(11)S)Fe_2(CO)_6同PPh_3在苯中,80℃下反应5小时,制得了三苯膦单取代产物(μ-cy-C_6H_(11)S)(μ-n-C_5H_(11)S)Fe_2(CO)_5PPh_3(1),并用X衍射技术测得其单晶结构.晶体属正交晶系,空间群为.Pbca,α=12.940(2)A,b=23.170(7)A,c=23.294(2)A,D_=1.25g·cm~(-3) Z=8.采用直接法(RANTAN)测得其初结构,以SHELX-76程序经全矩阵最小二乘法分块修正,最后偏离因子R=0.043,R_w=0.058.单晶X射线分析表明,三苯膦取代反应发生在配合物Fe—Fe键的反位上;两个硫桥以不等性方式同两个铁原子相连;硫桥上的取代基cy-C_6H_(11)及n-C_5H_(11)同处于e,e键,且弯向Fe_2原子一边.重要的键长有Fe(1)—Fe(2)=2.527(1)A,Fe(1)—S=2.287(1)及2.281(1)A,Fe(1)—p=2.271(1)A,Fe(2)—S=2.267(1)及2.275(1)A.五个Fe—C键长在1.757(7)～1.810(6)A范围内。     

MWCNTs-rGO/PDDA-AuNPs复合膜修饰电极对莱克多巴胺的灵敏检测

采用自组装方法,将聚二烯丙基二甲基氯化铵(PDDA)功能化的金纳米颗粒(Au NPs)负载于多壁碳纳米管(MWCNTs)-还原型氧化石墨烯(r GO)夹层,再涂覆于玻碳电极(GCE)上,制备了纳米复合膜修饰电极MWCNTs-r GO/PDDA-Au NPs/GCE.采用透射电子显微镜(TEM)和紫外-可见光谱(UV-Vis)对修饰膜的形貌及结构进行表征.探讨了其对莱克多巴胺(Rac)的循环伏安行为,结果表明MWCNTs-r GO/PDDA-Au NPs纳米复合物对Rac表现出显著的电催化氧化特性.采用差分脉冲伏安法测得该复合膜修饰电极对Rac检测的线性范围为0.036~4.5μmol/L,检出限为6.35 nmol/L(S/N≥3),且显示出良好的抗干扰能力、稳定性及重现性.采用该方法检测猪血清及猪尿样中的Rac,回收率达95.4%~105.9%,表明该复合膜修饰电极对实际样品中Rac的检测具有潜在应用价值.     

仪器参数对烟叶淀粉测定值的影响

研究了跳动取样、取样时间、泵速3个参数对自动化学分析仪测定烟叶淀粉含量的影响,结果表明,3个参数均显著影响淀粉测定值,而且跳动取样与取样时间、取样时间与泵速以及三者间存在显著的交互作用。样品测定时选择跳动取样关闭、泵速35、采样时间30较为合适。     

127°径向位置灵敏柱形静电离子能谱仪

针对高电荷态离子与表面作用产生的溅射离子能谱测量,研制了一台127°径向位置灵敏柱形静电离子能谱仪。利用能量为800 keV的Ar8+离子轰击金属铍靶产生的溅射离子测试了本谱仪。 测试结果表明,该谱仪克服了传统静电谱仪通过扫描工作电压单能量点取谱的缺点, 实现分段取谱——在单个工作电压下可同时获取一段0.85Ec≤E≤1.15Ec范围的能谱, 从而提高测量效率。 A 127° electrostatic coaxial cylindrical energy spectrometer with a radial position sensitive MCP detector is designed for sputtering ions measurement. It has been tested by measuring the energy spectrum of the sputtering ions in the collision of 800 keV Ar8+ bombarding beryllium target. A segment of the energy spectrum (0.85Ec≤E≤1.15Ec) can be obtained at one working voltage (U), which is much efficient than the traditional point to point voltage scanning method.     

Resonator insensitive investigation to thermal lens for end-pumped lasers

Optical pumping of solid-state lasers induces a thermal lens effect in the laser crystal; this thermal effect determines the beam properties. In this paper, the focal length of the thermal lens is calculated, and resonator parameter (g_1 g_2) is obtained, which is insensitive to thermal distortions when the product of the resonator parameters (g_1, g_2) equals 1/2. By using our calculated results, we get the fundamental transverse mode laser output with optic－optic conversion of 48.6%, and slope efficiency of 56.3%.     

RE(ClO4)3.nH2O与丙氨酸、 咪唑配合物的合成、表征及生物活性

研究了9种RE(ClO     

星点设计-效应面法优化化香树果序酚类物质的提取工艺及抗氧化分析

本研究以单因素实验为基础,没食子酸、鞣花酸、咖啡酸3种酚酸类成分的总含量为质控指标,利用星点设计-效应面法优化乙醇浸提化香树果序酚类物质的最佳工艺;采用DPPH和Fetion法考察其抗氧化性。结果表明,醇提一体化的最佳工艺为料液比14.28,提取时间114.43min,乙醇浓度73.71%,提取温度89.04℃,提取3次,提取量10.68mg·g^-1。化香树果序酚类物质在梯度浓度内,DPPH自由基、羟基自由基的清除率呈上升趋势。该工艺简便可行,为化香树果序的提取生产及抗氧化组分利用提供了依据。     

苯乙烯—环氧乙烷嵌段共聚物的阴离子聚合与表征

用二苯甲烷钾为引发剂,阴离子聚合法合成了苯乙烯（Ｓｔ）－环氧乙烷（ＥＯ）嵌段共聚物,并用ＦＴＩＲ,＾１Ｈ－ＮＭＲ,ＳＥＣ,ＷＡＸＤ和动态粘弹谱对共聚物进行了表征。结果表明所得聚合物为分子量可控,窄分布的两嵌段共聚物。