BIS监测与镇静-躁动评分在预防ICU患者非计划性气管拔管中的应用研究

目的探讨脑电双频指数(BIS)监测在预防ICU患者非计划性气管拔管中的应用价值。方法选择123例神志清醒的气管插管患者作为研究对象,采用随机数字法将患者分为实验组62例与对照组61例,实验组采用BIS监测对照组采用镇静-躁动评分(SAS评分)进行镇静管理,对2组患者气管插管期间非计划性拔管发生率进行比较。结果实验组非计划性拔管发生率显著低于对照组。结论 BIS监测比SAS镇静评分法更适合于气管插管患者的镇静管理。

PO_(4)^(3-)掺杂Bi_(2)O_(2)CO_(3)/Bi^(0)的制备及其可见光催化性能

构建氧空位以及附着金属单质Bi(Bi^(0))是增强半导体材料光吸收性能、促进半导体光生载流子分离的有效方法。通过简单的共沉淀法及氢气热还原成功制备了PO_(4)^(3-)掺杂Bi_(2)O_(2)CO_(3)附着Bi^(0)(Bi-P-BOC)的可见光催化剂,并对其在可见光下催化降解氧氟沙星(OFX)的性能及机理进行了研究。材料表征结果表明BOC随着PO_(4)^(3-)的均匀掺杂,可见光吸收能力增强,表面缺陷增多,比表面积增大。而随着氢气热还原,BOC表面形成Bi^(0)的同时也原位构建了大量的氧空位。可见光催化性能测试表明,Bi-P-BOC可以在180 min内降解约85%的OFX,降解速率为0.013 0 min^(-1),是BOC降解速率的8倍。Bi-P-BOC光催化降解机理表明其具有更好的可见光吸收能力,Bi^(0)以及氧空位的存在促进了光生载流子的分离,h+是其光催化降解过程中的主要的活性氧物种(ROS),此外,^(1)O_(2)和·O_(2)-也对降解有一定贡献。

Synthesis, Crystal Structure and Properties of a New Zn(II) Coordination Polymer Constructed from 2,3-Pyridine Dicarboxylic Acid and 1,1′-(1,4-Butanediyl)bis(imidazole)

A new coordination polymer, namely [Zn（pdc）（bbi）]n {H2 pdc = 2,3-pyridine dicar- boxylic acid, bbi = 1,1-（1,4-butanediyl）bis（imidazole）}, has been prepared under hydrothermal conditions and characterized by elemental analysis, IR, and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group P21 /n with a = 8.436（3）, b = 16.988（5）, c = 12.106（4）, β = 92.204（5）°, V = 1733.6（9）3, Z = 4, C17 H17 N5 O4 Zn, Mr = 420.73, Dc = 1.612 g/cm3, F（000） = 864, μ（MoKa） = 0.452 mm-1, the R = 0.0672 and wR = 0.1645. In the mononuclear complex, each Zn（II） is five-coordinated by one carboxylate O and one pyridyl N atoms from one pdc anion, one carboxylate O atom from another pdc anion, and two N atoms from two bib ligands. The Zn（II） ions are connected by pdc ligands to form skeleton chains, and bbi ligands further link them to construct a 2D framework. The thermal and luminescence properties of the complex were also investigated.

Bi掺杂对溶胶-凝胶法制备Cu_(2)ZnSnS_(4)薄膜性能影响的研究

Cu_(2)ZnSnS_(4)(CZTS)薄膜太阳电池因其具有较佳带隙、组成元素丰富、理论转换效率高等优点,而被广泛研究。采用溶胶-凝胶法制备了Bi掺杂的CZTS薄膜,研究了Bi掺杂量对薄膜的微观形貌、物相结构和光电性能的影响。研究结果表明,所制备的薄膜为锌黄锡矿结构的CZTS。Bi元素的掺入对薄膜形貌影响很大,晶粒尺寸先增大后减小,薄膜更致密、更均匀。随着Bi掺杂含量增加,CZTS薄膜的光学带隙呈上升趋势,光电流响应先增大后减小。当Bi掺杂浓度为1%时,CZTS薄膜综合性能最佳。

Synthesis,Structural Characterization and Properties of Bis(1,5-diamino-1Htetrazolium)3,3'-bis(nitramino)-4,4'-azofurazan

An energetic salt of bis（l,5-diamino-lH-tetrazolium）3,3＂-bis（nitramino）-4, 4x-azo- furazan （C6H10N2206） was synthesized with the total yield of 61.7% by using 3,4-diaminofurazan （DAF） as the starting material. The structure of the title compound was confirmed by NMR, IR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in orthorhombic, space group P21/c with a = 10.739（2）, b = 6.4765（12）, c = 14.138（3） A, fl= 108.787（3）°, V= 930.9（3） A3, Z = 1, Mr= 486.36, Dc = 1.735 g.cm3, μ= 0.15 mm-1, F（000） = 496, R = 0.042 and wR = 0.121. The thermal stability was analyzed by subsequently differential scanning calorimetry （DSC）. And the enthalpy of formation and detonation was calculated theoretically, showing the first decomposition temperature was 142.1℃, the enthalpy of formation was 1614.23 kJ.mol1 and the detonation velocity and detonation pressure were 8.781 km.s-1 and 30.7 GPa, respectively.

A One-dimensional Pseudo-helical Coordination Polymer with 4,4′-(Hexafluoroisopropylidene)bis(benzoic acid)

The title complex [Zn2（hfipbb）2（2,2′-bpy）2], 1 has been hydrothermally synthesized from Zn（NO3）2·6H2O, 4,4′-（hexafluoroisopropylidene）bis（benzoic acid） and 2,2′-bipyridine. Singlecrystal X-ray analysis reveals that 1 presents a one-dimensional coordination polymer with pseudo-helical chain structure. Two Zn（Ⅱ） atoms in an unsymmetrical unit of 1 adopt distorted octahedral and square-pyramidal coordination geometries, respectively. The packing of parallel chains gives a three-dimensional supramolecular network supported by π-π stacking interactions. Crystal data： C54H32F12N4O8Zn2, Mr = 1223.58, monoclinic, space group P2 1/c, a = 27.557（6）, b = 16.751（3）, c = 11.350（2） A, β= 99.21（3）°, V= 5171.5（18） A^3, Z= 4, Dc = 1.572 g/cm^3, F（000） = 2464, μ= 1.030 mm^-1, the final R = 0.0552 and wR = 0.1070 for 6631 observed reflections （I〉 2σ（I））.

Use of Ultrasound and Microwave Irradiation for Clean and Efficient Synthesis of 3,3’-(Arylmethylene)bis (2-hydroxynaphthalene-1,4-dione) Derivatives

Nine 3,3’-(arylmethylene)bis(2-hydroxynaphthalene-1,4-dione) derivatives were synthesized through the reaction between 2-hydroxy-1,4-naphthalen-1,4-dione and different aromatic alde-hydes in water applying ultrasonic irradiation for 5 min at room temperature and microwave irradiation for 15 min at 70°;C. Two of the nine derivatives, compounds 3-e and 3-i, obtained from 3-bromo-hydroxybenzaldehyde and 5-methylfuran-2-carbaldehyde, respectively, are previously unpublished. The structures of all compounds were established on the basis of their spectral data and mass analysis. The attractive features of this synthesis protocol include mild conditions, high atom-economy and excellent yields with the elimination of water as the only by-product.

STRUCTURE AND PROPERTIES OF PHOSPHROUS-CONTAINING POLY(ARYLETHER KETONE)WITH BISPHENOL-A MOIETY

A phosphrous-containing poly（aryl ether ketone） was synthesized derived from bisphenol-A and bis[4-（4- fluorobenzoyl）phenyl] phenyl phosphine oxide （FPPPO） by nucleophilic substitution reaction. The structure of the polymer was characterized by FT-IR, ^1H-NMR and ^31p-NMR. The thermal property of the PAEK was measured by DSC and TGA. The glass transition temperature （Tg） of the polymer was 205℃, and the 5% weight loss temperature under nitrogen was 475℃. Good solubility of the polymer in organic solvents, such as N-methylpyrrolidone, dimethylformamide, dimethylacetamide, dimethylsulfoxide and chloroalkanes was observed, flexible film was obtained from the polymer＇s CH2Cl2 solution. The limiting oxygen index （LOI） of the PAEK was 40, which indicated that organic phosphorus moiety can offer good flame retardant property to the polymer.

Synthesis of Racemic Bis[2-(6-fluoro-2-chromanyl)-2-hydroxyethyl]-amine Methanesulfonic Acid Salt Using Lithium Aluminum Amide as a Promoter in Regioselective Ring Opening of Epoxide

Lithium aluminium amide [LiAI（NHR）4] 5 obtained by treating the primary amine 4 with LiAlH4 could promote the ring opening of epoxide 2 and led to high regioselective product of racemic bis[2-（6-fluoro-2-chromanyl）-2-hydroxyethyl]amine methanesulfonic acid salt 7.

Synthesis and Crystal Structure of 4,4'-(4-(1-Naphthyl)-4-phenyl-1,3-butadienylidene)-bis[N,N-diethylbenzenamine]

The title compound （C40H42N2） has been synthesized by the reaction of l-（l- naphthyl）-l-phenyl-3-chloropropylene and bis（4-（diethylamino） phenyl）methanone, and characterized by IR, ^1H NMR, MS and X-ray diffraction analysis. The crystal belongs to the monoclinic system, space group P21/c with a = 17.047（3）, b = 10.807（2）, c = 18.494（4） A, β = 105.727（4）°, V= 3279.4（11） A^3, Mr = 550.76, Z = 4, Dc = 1.115 g/cm^3,μ（MoKa） = 0.085 mm^-1, F（000） = 1184, the final R = 0.0625 and wR = 0.1384 for 2276 observed reflections （1 〉 2σ（I））. X-ray analysis reveals that the butadiene fragment adopts a planar cisiod conformation and makes a dihedral angel of 69.4（2）° with the naphthalene ring.

A SENSITIZED PHOTOINITIATION SYSTEM ——BIS (7-DIETHYLAMINO COUMARIN ) KETONE-3 AND DIPHENYLIODONIUM SALT COMBINATION

Bis (7- diethylaminocoumarin) ketone- 3(DACK) and diphenyliodonium salt (DPIO)combination as an effective photoinitiation system for radical polymerization has been investigated. The sensitized photolysis of DACK/DPIO leads to bleaching of DACK and decomposition of DPIO to generate initiating radical species. The electron transfer sensitization occurs mainly from the triplet state of DACK. The photobleaching obeyed a second-order kinetics and the rate constant was evaluated to be 31.3mol^(-1)·1·s^(-1) Photopolymerization of MMA initiated by DACK/DPIO was carried out in acetonitrile solution. The polymerization rate was found to be proportional to the concentration of DACK, DPIO and MMA with the exponents of 0.34, 0.40 and 1.0 respectively. The initiated efficiency is comparable to those of small molecular ketones.The sensitized photoinitiation mechanism has been discussed.

Photoluminescence and Electroluminescence Properties of 2,5-Bis[2,2′-bis(5-phenyl)-1,3,4-oxadiazole] Thiophene(T-OXD) and T-OXD/Poly(9-vinylcarbazole) Blends

The photoluminescence(PL) and the electroluminescence(EL) properties of a novel organic compound, 2,5-bis(2,2′-bis(5-phenyl)-1,3,4-oxadiazole(T-OXD), were studied in chloroform and in a solid thin film. The PL and the EL properties of T-OXD/poly(9-vinylcarbazole)(PVK) blends were also studied, which contained various contents of T-OXD. The PL maximum emission peaks of T-OXD/PVK blends show gradual bathochromtic-shift with the increase of the T-OXD content. The EL spectra of T-OXD/PVK devices are similar to their PL spectra, and all the EL maximum emission peaks show bathochromtic-shift compared with the corresponding PL spectra, which is ascribed to the formation of electroplex. The turn-on voltages for ITO/T-OXD:PVK/Al devices decreased from 13.5 V of the device cotaining 0.1% T-OXD(mass fraction) to 5 V of the device containing 5% T-OXD, which suggests that T-OXD improves the energy level match between T-OXD and PVK and enhances the emission efficiency. The experimental results indicate that T-OXD can be used as a good electron transporting material.

Synthesis and Crystal Structure of 1,4-Bis-(benztriazol-1-ylmethyl)-2,3,5,6-tetramethylbenzene

The title compound 1,4-bis(benztriazol-1-ylmethyl)-2,4,5,6-trimethylbenzene crys- tallizes in the monoclinic system, space group Pbca with a = 9.842(5), b = 9.455(5), c = 22.165(12) ?, V = 2062.6(18) ?3, Dc = 1.277 g/cm3, Z = 4, C24H24N6, Mr = 396.49, μ(MoKa) = 0.079 mm-1 and F(000) = 840. The structure was refined to R = 0.0662 and wR = 0.1891 for 1163 observed reflections (I > 2σ(I)). The title molecule has trans-conformation about the central phenyl ring. The zigzag-like molecules are connected by face-to-face π…π stacking to form an infinite 2D layer.

Identification of N-Methyl Bis(2-(Alkyloxy-Alkylphosphoryloxy)Ethyl) Amines by LC-HRMS/MS

N-Methyl bis(2-(alkyloxy-alkylphosphoryloxy)ethyl)amines, which are abbreviated as PNPs, are a series of new skeleton chemicals belonging to schedule 2.B.04 chemicals of Chemical Weapons Convention (CWC). PNPs are important markers of chemical warfare agents because they are structurally relative to both nerve agents and N-mustards. In this study, fragmentation pathways of the most characteristic fragment ions in Q-TOF mass spectrometry were proposed based on the information from accurate mass and secondary fragmentations of product ions scan experiments. Results indicated that the base ion in LC/HRMS was the quasi-molecular ion [M+H]+. In LC-HRMS/MS, it was [M+H-CnH2n+1P(O)(OH)CmH2m+1O]+ fragment ion which was formed by losing an alkyloxy alkylphosphoryloxy group from the quasi-molecular ion. The diagnostic ion m/z84.0814 was identified as [C5H10N]+, which was the group of (CH2=CH)2N+(H)CH3. PNPs have two protonated centers. One is on the N atom, the other is on the O atom (P=O). O-n-propyl PNPs generally exhibited two fragmentation pathways. Firstly, the quasi-molecular ion [M+H]+ lost a propoxy alkylphosphoryloxy group to produce [R1P(OH+)(O-n-C3H7)OCH2CH2N(CH3)CH=CH2]+, which could be fragmented further to produce [C5H10N]+ ion. Secondly, [R1P(OH+)(O-n-C3H7) OCH=CH2]+ ions were produced from [M+H]+ and fragmented further to produce the abundant ions [R1P(OH+)(OH)OCH =CH2]. However, O-isopropyl PNPs characteristically produced weak fragment ions [M+H-C3H6]+, which were presumably formed via loss of CH3CH=CH2 from [M+H]+. Other PNPs showed similar fragmentation pathways as O-n-propyl PNPs. On the summarization of the MS fragmentation pathways of PNPs, LC-HRMS/MS quantitative and qualitative methods were developed and applied to analyze N-Methyl bis(2-(butoxy-methylphosphoryloxy)ethyl]amine in high background organic samples. The analytical results had successfully supported the sample preparation for the 33rd official proficiency test of Organization for Prohibition of Chemical Weapons (OPCW).

Synthesis, Reactions and Characterization of 1,1’-(1,4-Phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(ethan-1-one)

Reaction of 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-thioxo-1,2-dihydropyridine-3-carbonitrile) (1) with methyl iodide afforded the 4,4’-(1,4-phenylene)bis(5-acetyl-6-methyl-2-(methylthio)nicotinonitrile) (2). The reaction of 2 with hydrazine hydrate followed by diazotization reaction af-forded the 1,1’-(1,4-phenylenebis(3-amino-6-methyl-1H-pyrazolo[3,4-b]pyridine-4,5-diyl))bis(e-than-1-one) (3) and 1,1’-(1,4-phenylenebis(3-(chlorodiazenyl)-6-methyl-1H-pyrazolo[3,4-b]-pyridine-4,5-diyl))bis(ethan-1-one) (4) respectively. On the other hand, reaction of 4 with malononitrile, 2-cyanoethanethioamide, ethyl acetoacetate, acetyl acetone, ethyl benzoylacetate, diethylmalonate, ethyl cyanoacetate and phenacylbromide aiming to build up pyrazolotriazine or pyrazole ring on the ring system of 4. Structures of all newly synthesized heterocyclic compounds in the present study were confirmed by considering the data of IR, 1H NMR, mass spectra as well as that of elemental analyses.

动态增强MRI结合DWI对乳腺疾病BI-RADS分类诊断的价值

目的探讨动态增强MRI结合DWI在乳腺疾病BI-RADS分类诊断中的应用价值。方法回顾性分析215例经手术或穿刺病理证实的乳腺疾病患者的MRI资料,均行动态增强扫描及DWI(b=1 000 s/mm2),其中良性46例,恶性169例。分析病灶时间-信号强度曲线、ADC值及两者结合的MRI BI-RADS分类诊断乳腺病变的灵敏度、特异度及诊断符合率。结果 ROC曲线确定的ADC诊断阈值为1.177×10-3mm2/s,时间-信号强度曲线、ADC值及两者结合的MRI BI-RADS分类诊断乳腺癌的灵敏度分别为94.7%、89.3%、97.0%,特异度分别为39.1%、87.0%、80.4%,诊断符合率分别为82.8%、88.8%、93.5%。结论结合时间-信号强度曲线及ADC值,MRI BI-RADS分类能显著提高乳腺疾病的诊断水平。

溶胶-凝胶法制备Bi_2WO_6微纳米材料及其光催化性能

为了开发可见光响应型光催化剂,以柠檬酸为络合剂,采用溶胶-凝胶法制备前驱体,通过煅烧得到了Bi2WO6微纳米材料。采用X-射线衍射(XRD)、场发射扫描电镜(FESEM)、紫外-可见光漫反射谱(UV-vis DRS)等技术对其进行表征,考察了制备条件对样品晶相结构的影响。结果表明,在煅烧温度450℃、煅烧时间3 h、柠檬酸与Bi3+的物质的量比为3∶1、前驱液的pH=1、分散剂为PEG-4000的条件下制备的Bi2WO6样品为斜方晶系Bi2WO6结构,由粒径为50 nm左右的小薄片堆积而成。所得的Bi2WO6样品具有优良的光催化性能,在可见光照射(200 W点钨灯)及H2O2助剂的存在下,对10 mg/L罗丹明B溶液的光降解率可达82.0%。研究结果可为高效Bi2WO6光催化材料的制备提供新的思路。

Bi2WO6量子点(QDs)修饰Bi2MoO6-xF2x异质结的构筑及其催化活性增强机理

采用简单沉积-沉淀法合成了Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)(BWO/BMO_(6-x)F_(2x))异质结,借助XRD、XPS、TEM、SEM、EDS、UV-Vis-DRS、PC和EIS等测试技术对其组成、形貌、光吸收特性和光电化学性能等进行系统表征,并以模型污染物罗丹明B(Rh B)的光催化降解作为探针反应来评价Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)异质结的光催化活性增强机制。形貌分析表明,所得Bi_2MoO_6微球由大量厚度为20~50 nm的纳米片组成;FE-SEM和HR-TEM分析表明,尺寸约为10 nm的Bi_2WO_6量子点均匀沉积在Bi_2MoO_(6-x)F_(2x)微球表面,形成新颖的Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)异质结;与纯Bi_2MoO_6或者Bi_2WO_6相比,1∶1Bi_2WO_6@Bi_2MoO_(6-x)F_(2x)异质结表现出更好的光催化活性和光电流性质,其对RhB光催化降解的表观速率常数分别为纯BMO和BWO的6.4和11.6倍。PC和EIS图谱分析表明,Bi_2WO_6量子点表面沉积显著提高Bi_2MoO_(6-x)F_(2x)光生电子/空穴的分离效率和迁移速率;活性物种捕获实验证明了·O_2^-和h^+是主要的活性物种。根据实验结果,探讨了F-掺杂和Bi_2WO_6量子点之间的协同效应对Bi_2MoO_6的光催化活性的影响机制。

(Bi,Pb)-2223相分解-再形成过程中超导相的演变

研究了低氧分压气氛中，不同熔化处理温度下单芯银包套带材（Bi，Pb）-2223（以下称Bi-2223）芯部熔化分解及随后的缓慢冷却阶段，淬火试样中Bi-2223，Bi-2201和Bi-2212相之间的演变关系。结果显示，在Tp=855℃-865℃范围内，随着熔化处理温度（Tp）的升高，淬火带材中Bi-2223相相对含量逐渐减少，而Bi-2201相含量则明显增加。Tp=855℃-860℃时，Bi-2223相发生部分分解，其淬火后的主要产物为Bi-2201，（Sr,Ca）2CuO3（2：1AEC）和（Sr,Ca）14Cu24O41（14：24AEC）。经过随后的缓慢冷却，部分分解的Bi-2223相可以直接从液相中再形成。在所有熔化试样及部分熔化后慢冷所得的试样中均未发现Bi-2212相。当Tp=865℃时，Bi-2223相则全部分解，在同样冷却条件下，其回复过程经历了两个不同的途径，一是少量Bi-2223相直接从液相中生成，二是先从液相中析出Bi-2212相，在随后继续冷却过程中再转变为Bi-2223相。由于Bi-2212转变为Bi-2223所固有的迟缓特性，以致在本实验的冷却条件下，完全分解的Bi-2223相只能部分得到回复。