Na2O-B2O3-Ta2O5系统玻璃红外光谱的研究

本文首次系统地研究了Na₂O—B₂O₃—Ta₂O₅。三元新系统的红外光谱,分析了B₂O₃、Ta₂O₅含量的变化对玻璃结构的影响。结果表明:随着Na₂O/B₂O₃比值的减小,结构中:[BO₄]四面体减小,[BO₃]三角体增加。随着Ta₂O₅含量的增加,[BO₄]四面体的数量增多,非桥氧的数量减少,表明Ta⁵⁺可以连结非桥氧,形成网络。     

Nb2O5-B2O3-K2O系统玻璃的结构与性质

本工作用大功率转靶 X 射线衍射仪研究铌硼酸盐玻璃结构;根据 B·E·War-ren 方程,建立了一种计算玻璃原子径向分布函数(RDF)的解析方法。因其涉及因素少,计算简便,适用于多元系统玻璃结构分析。应用本方法,已获得了 Nb-B-K 系统玻璃的比较完整的三维结构模型。模型表明,这种玻璃结构松散,克分子体积比较大,并具有较高的自激发极化率。于是铌硼酸盐玻璃的低密度、低折射率和相对高的色散,以及较高的电导率等特殊性质的结构因素得到了证实。     

Ta2O5对B2O3-La2O3-CaO系统玻璃生成范围的影响

本文研究了在B₂O₃—La₂O—CaO三元系统中,当Ta₂0₅的含量分别为5、10、15、20wt%时,该系统的玻璃生成范围.结果表明,随着Ta₂O₅含量的增加,系统的玻璃生成范围向贫B₂O₃,富La₂O₃边界扩充.当Ta₂O₅的含量为10wt%时,玻璃的生成区域最大.通过差热分析确定了玻璃析晶温度,并用X射线衍射进行了物相鉴定.结果表明,随Ta₂O₅取代La₂₃其主结晶相的放热峰或吸热峰的位置变化不同,所析出的结晶物质亦不同.     

SiO2-BaO-La2O3-RmOn系统玻璃的光吸收

本文系统地研究了,SiO₂-BaO-La₂O₃-R_mO_n系统玻璃的光吸收。通过选用不同硅硼比值及引入适宜的Nb₂O₅含量获得了紫外区透过率好,抗析晶性能好的玻璃。     

Al2O3-TiB2-ZrO2三元复合陶瓷刀具的性能研究

对Al     

BaO-Nd2O3-PbO-TiO2微波介质陶瓷的研制

本文介绍了BaO－Nd2O3－PbO－TiO2微波介质陶瓷的研制结果,εr＝90,Q＝2000（2GHz）,τf＝0ppn／℃。此材料有一非常高的介电常数,它适用于频率小于1GHz的应用。另外,我们对此材料作了电镜和X衍射等结构分析,证明此材料生晶相为（Ba、Pb）Nd2Ti5O14。     

Nb2O5-B2O3-K2O三元系统玻璃分相与电导的跃变

本文报导了Nb₂O₅-B₂O₃-K₂O三元系统玻璃分相导致的电导突跃现象。从“界面效应”出发,阐明了这一现象的实质,并进一步说明了同成份物质的非晶态比晶态有较高电导的可能原因。     

化学镀Ni-P-MoS2/Al2O3复合镀层制备及其性能

通过化学沉积法在MoS2颗粒表面形成一层氧化铝,采用化学复合镀覆的方法制备Ni-P-MoS2/Al2O3复合镀层。研究复合镀液中MoS2颗粒含量和搅拌速度对复合镀层显微硬度及摩擦磨损特性的影响,比较由MoS2改性方式和添加分散剂方式获得镀层的性能,分析复合镀层的横截面及表面形貌。结果表明:随着MoS2颗粒含量和搅拌速度增加,镀层显微硬度、摩擦因数、耐磨性均先减小后增大。与添加分散剂制备的Ni-P-MoS2复合镀层相比,改性颗粒获得的Ni-P-MoS2复合镀层的自润滑性、显微硬度、耐磨性均有所提高。     

B2O3—La2O3—BaO—Nb2O5系统的玻璃生成范围及其性质

本文研究了在B₂O₃-La₂O₃-BaO-Nb₂O₅四元系统中当B₂O₃含量分别为25、30、35wt%时,该系统的玻璃生成范围和它们的光性、密度等变化规律。结果表明,随着B₂O₃含量的增加,系统的玻璃生成范围向贫Nb₂O₅边界扩充,富Nb₂O₅边表现收缩。工作中得出了该系统分别以SiO₂代B₂O₃、Al₂O₃代BaO后的析晶、折射率、色散及密度等性质的变化规律。最后应用该系统研制定型了713/538玻璃。     

微波消解-电感耦合等离子体质谱测定口红中的铅

An analytical method based on microwave digestion and ICP-MS detection was developed for the determination of lead in lipsticks. The conditions of the digestion were optimized by different mix-acid and sample weight, 0.2 g sample and a mixture of HNO₃＋HF＋H₂O₂ was found available. Its accuracy and precision were evaluated by GBW(E)090028 and two lipsticks. The results indicated that microwave-ICP-MS is accurate, sensitive and short of analytical cycle, which can meet the demand for the determining lead in lipsticks.     

植物样品中稳定碳同位素的EA-IRMS系统分析方法

通过多组实验对比,分析并讨论了利用元素分析仪-稳定同位素比率质谱仪（EA-IRMS）联用技术测定植物样品中碳同位素比值的实验条件。初步建立了植物样品中稳定碳同位素组成的分析方法,同时对系统分析的稳定性和精密度等进行了检验分析。结果表明：当IRMS真空度为7×10^-8kPa,高压3.0 kV,EA系统Carrier-He载气流量在90～100 mL•min-1,Conflo-He载气压力为80 kPa,氧喷条件为110 mL•min^-1时,使用Cr₂O₃/Co₃O₄作为EA氧化柱氧化剂填料,在严格控制样品残余和本底空白的条件下,植物样品的测定精密度为±0.20‰,测定值与给定值值偏离0.01‰。     

电感耦合等离子体质谱测定人肝中48种微量元素

Human liver samples were obtained in autopsy from 16 subjects died suddenly, who were healthy, normal before death and lived in 4 different areas with different dietary types in China. To determine 48 micro quantity elements in human liver by inductively coupled plasma mass Spectrometry (ICP-MS),samples were microwave digested using HNO₃ and H₂O₂ . Rhenium was used as an internal standard element standard. Reference materials of GBW(E) 080193 bovine liver and GBW09101 human hair were analysed by the described method. The analytical values of two standard reference materials showed close agreement with the reference values. The method is simple ,rapid, sensitive and accurate.     

LC/MS研究有机金属钌抗肿瘤化合物与蛋白酪氨酸磷酸酶模型化合物的相互作用

Protein tyrosine phosphatase 1B(PTP 1B) which contains a catalytic cysteine plays important role in the negative regulating of insulin signaling, and it has been investigated as a therapeutic target in type II diabetes and obesity. In the present work, the reactions of ruthenium anticancer complex[(ŋ⁶-cymene)Ru(en)Cl]PF₆ with the model compound(2-mercaptobenzanilide) were studied under physiologically relevant conditions. Then we treated the mono- and di-ruthenium product with GSH and H₂O₂ to mimic the inactivation and activation of PTP1B whilst [(ŋ⁶-cym)Ru(en)Cl]PF₆ binds to the active site of PTP1B. HPLC-ESI-MS time courses suggest that organometallic ruthenium complexes may inhibit the enzymatic activity of PTP1B by coordinating to the thiol in the active site, which may have important biological and pharmacologic significances in the treatment of diabetes and obesity.     

质谱学方法研究H＋(H2O)n(n＝4~16)团簇的解离过程

The forms of water vapor in the atomspheric circumstance were observed using a triple quadrupole mass spectromter. There was not any single H₂O, which were detected, and H^＋(H₂O)_n , n＝3-37 were the main forms of water in gas phase. The collisional induced dissociation (CID) mass spectrometry was studied, which showed that the main dissociation products of H^＋(H₂O)_n (n＝4-16) were H^＋(H₂O)₄ and/or H^＋(H₂O)₅.     

Mg(OH)2中的硼同位素测定与同位素分馏

We experimented with the incorporation of boron into Mg(OH)₂ during its deposition in magnesium-free artificial seawater with pH values ranging from 9.5 to 13.0. The results indicate that the ¹¹B values of the deposited Mg(OH)₂ were higher than those of the associated artificial seawater. The isotopic fractionation characteristics of boron are distinct from those of inorganic carbonate deposition, and indicate that the mechanism for boron incorporation into Mg(OH)₂ also differs from that of inorganic carbonates.     

6种他汀类药物的电喷雾离子阱质谱分析

采用电喷雾离子阱多级质谱技术对6种他汀类药物进行系统研究,总结了该类化合物的电喷雾质谱断裂规律。根据主要药效基团存在形式的不同,分两类解析。第一类:辛伐他汀和洛伐他汀在正离子模式下发生β,δ-二羟基戊内酯开环断裂,生成中性丢失H2O、CO、CH3COOH的碎片离子;第二类:普伐他汀和阿托伐他汀在负离子模式下产生脱去104 u(3-羟基-1,4-丁內酯和H2)和160 u(3,5-二羟基-1,7-庚内酯)的碎片离子;氟伐他汀和瑞舒伐他汀在负离子模式下产生脱去62 u(CO2和H2O)的碎片离子,对该二级碎片离子进行三级全扫描质谱分析,产生脱去42 u(CH2=C=O)和96 u(环已烯-3-酮)的碎片离子。这些质谱特征有助于他汀类药物的结构分析和鉴定。     

苯撑肼基二硫代碳酸甲酯质子化离子双氢协同迁移的裂解机理研究

使用碰撞诱导裂解质谱（CID-MS）和泛密函数（DFT）理论计算研究了苯甲撑肼基二硫代碳酸甲酯质子化离子的气相裂解行为。丢失H₂S,CH₃SH 和（NSC）SCH₃是其主要裂解途径。量子化学计算表明,分子中脲基S最容易接受外加质子,形成质子化离子MH-a;该外加质子很容易迁移到亚胺N上,形成异构体MH-b。在碰撞活化下,前驱离子MH-b发生N—N键断裂,伴随着酰胺氢迁移到亚胺氮上,发生（NSC）SCH₃丢失裂解反应;若酰胺氢直接迁移到甲基硫上,则发生CH₃SH丢失反应。若前驱离子MH-a的外加质子迁移到到甲基硫上,则发生CH₃SH丢失反应;若酰胺氢经过甲硫基迁移到脲基S上,则发生H₂S丢失。上述结果证实了该化合物质子化离子的碎裂反应是外加质子和酰胺氢协同迁移的结果。     

鸟嘌呤自由基阳离子的碰撞诱导解离实验和理论研究

An electrosprayed water/methanol of Guanosine and Cu(NO₃)₂ was observed to give rise to gas-phase guanine radical ion. The Collision-Induced Dissociation (CID) of guanine radical cation generates five competing dissociation channels to lose NH₃, HCN, CN₂H, H₂NCN and HNCO, respectively. At the same time, the DFT theory was also used to simulate the HCN lost channel. It was turned out that through the three complicated structure changes a [ 4. 1. 0] bicyclic ion intermediate was formed before kicking off the HCN.     

EA-MS测试过程中添加助燃剂的影响效应研究

利用元素分析-质谱仪(EA-MS)联用系统,探讨对高C/N植物样品测试过程中添加助燃剂对样品氮同位素比值、氮含量和仪器本底的影响。在植物样品中添加CuO或者V₂O₅,测定的氮同位素组成结果表明：添加助燃剂导致样品测试的结果偏差更小,这与测试过程中植物样品能够完全燃烧有关;添加助燃剂使测试的氮含量高于不添加助燃剂的情况,同时仪器本底也能迅速降低,说明助燃剂的添加有助于样品在瞬间燃烧,因此使测试结果更为精确;不同助燃剂的添加对植物氮同位素比值结果的影响程度不同,与不添加助燃剂的情况相比,CuO的添加使得同位素比值偏正,而V₂O₅的添加结果不具有规律性;在样品中添加CuO助燃剂（和植物样品以4∶1的质量比混合）,样品测试的同位素值偏差最小,测试结果也更加可信,样品本底可以达到连续做样而不影响测定下一样品的氮同位素组成。该方法简单、有效、投入较少,可以用于难以反应的样品分析中。