舰船用无溶剂环氧涂料常温释放物及高温热解物分析与评价

涂料作为舰船舱室及其部件的内部防护装饰材料已广泛地应用于舰船舱室,科技的发展使得涂料更新换代的步伐加快。舰船舱室经常处于全封闭状态,为减少舱室空气污染对船员的身心健康和战术技术发挥的不良影响,故对舰船舱室大气环境质量提出了更高更新的要求,因此舰船用涂料的筛选尤为重要。涂料作为常用的一种非金属材料其挥发物具有一定的毒性,尤其是对一些新的、毒性不明的涂料,必须先对其进行使用条件下的安全性评价,以便确定其可否应用于舰船舱室之中。本实验根据有关标准对舰船用低毒无溶剂环氧涂料常温释放物及高温热解物进行分析,并对其作卫生学评价,从而为舰船设计、建造部门在筛选艇用涂料方面提供可靠的科学依据。     

GC-MS技术在舰船复合板毒性评价中的应用

海军舰船舱室多为密闭环境,其舱室狭小,设备庞杂,人员密集。舱室内部的防护装饰多系非金属材料,随着现代各种复合、聚合材料的迅速发展和广泛使用,周围环境特别是密闭舱室空气污染的问题也更为突出。本文根据有关军用标准和规程[1],应用GC-MS技术对2种舰船复合板常温释放物和高     

舰船用3种特殊胶粘剂常温释放物及高温热解物的定性分析

舰船特殊胶粘剂不仅能把各种造舰材料紧密粘合,还具有某些特殊的性能,如绝缘、防水、防火、防磁、防震等.这些特殊胶粘剂在用于海军舰船之前必须进行使用环境下的毒性评价.模拟使用环境条件下对其常温释放物及高温热解物的定性分析是毒性评价的主要内容.     

GC-MS技术在舰船胶粘材料毒性评价中的应用

胶粘材料简称胶粘剂、粘合剂、粘结剂、接着剂。因其能把各种材料紧密地粘合在一起,并具有各种良好的性能,因而广泛地应用于海军舰船的制造及维修中。应用GC-MS技术对在使用环境及条件下其释放物及高温热解物的定性分析是对其进行使用过程中毒性评价的重要步骤。1实验部分1.1仪器与材料仪器:JMS-D300(日本JEOL);PIATFORMⅡGC-MS。     

基于纳米金星的层析试纸条用于检测HIV-DNA（英文）

构建了基于纳米金星(AuNSs)的快速、简单且可视化的横向流层析试纸条(LFTS),并用于检测人类免疫缺陷病毒的DNA。采用一步法合成AuNSs,并对其进行生物功能化,目标物与DNA修饰的AuNSs结合。该复合物通过碱基互补配对原则被捕获在测试线上,依据测试线上纳米金星颜色的变化进行定性和半定量分析,使用便携式读条器在最佳实验条件下进行定量分析。该方法的线性范围为0.2～50 nmol/L,检出限为0.14 nmol/L。相同条件下,该方法比传统纳米金试纸条的灵敏度约高5倍。该方法可用于人血清中HIV DNA的检测,结果良好。     

基于纳米金星的层析试纸条用于检测HIV-DNA

构建了基于纳米金星(AuNSs)的快速、简单且可视化的横向流层析试纸条(LFTS),并用于检测人类免疫缺陷病毒的DNA。采用一步法合成AuNSs,并对其进行生物功能化,目标物与DNA修饰的AuNSs结合。该复合物通过碱基互补配对原则被捕获在测试线上,依据测试线上纳米金星颜色的变化进行定性和半定量分析,使用便携式读条器在最佳实验条件下进行定量分析。该方法的线性范围为0.2~50 nmol/L,检出限为0.14 nmol/L。相同条件下,该方法比传统纳米金试纸条的灵敏度约高5倍。该方法可用于人血清中HIV DNA的检测,结果良好。     

新型导弹驱逐舰舱室大气组分的定性定量分析

新型导弹驱逐舰是我海军主要战斗舰船,因其"全封闭"的环境特点,对舱室空气质量产生不同影响,致使舱室大气组份复杂,浓度差异,只有对其进行全面的定性定量测定,才能正确给予卫生学的分析与评价.     

近三年来气相色谱法的新进展（下）

定性和定量分析 随着毛细管色谱柱工艺的发展,对定性和定量分析都提出了更高的要求。在定性方面要求滞留值准确可靠,检测灵敏度高和选择性好。在定量方面要求仪器性能稳定,样品的预处理要准确无误,进样量要准确和不失真(包括柱子和仪器的气路部件对样品不     

3,4-二巯基甲苯衍生化法结合SPME/GC-MS技术分析尿样中超痕量氯乙烯基胂酸

选取氯乙烯基胂酸(CVAOA)为生物标志物,建立了路易氏剂染毒尿样中超痕量CVAOA的分析方法。采用正交试验,优化了CVAOA的巯基化衍生方法,选取3,4-二巯基甲苯(DMT)作为衍生试剂,CVAOA与DMT的用量摩尔比为1∶1 000,常温衍生5 min,可达到最高的衍生效率;之后在优化的顶空-固相微萃取(HS-SPME)条件下富集纯化衍生产物CVAOA-DMT;使用气相色谱-质谱/选择离子监测模式(GC-MS/SIM)进行定性定量分析。该方法在50.0 pg/m L~500 ng/m L浓度范围内呈良好的线性(r2=0.998 5),相对标准偏差(RSD)小于10%,检出限可达7.6 pg/m L,定量下限为23 pg/m L。对低、中、高3种浓度的路易氏剂染毒尿样进行检测,回收率为97.6%~105%,RSD为4.4%~7.1%。该方法分析灵敏度高,具有良好的准确度、精密度和普及性,可被广泛推广和使用。     

气相色谱-质谱法测定聚氯乙烯包装材料和食品模拟物中的46种增塑剂

建立了46种增塑剂在聚氯乙烯(PVC)食品包装材料中的含量及其在水、3%乙酸、10%乙醇和橄榄油4种食品模拟物中迁移量的气相色谱-质谱(GC-MS)测定方法。食品包装材料、水质模拟物和橄榄油中增塑剂分别采用溶解-沉淀法、正己烷液-液萃取和凝胶渗透色谱(GPC)法提取。采用GC-MS法,在选择离子监测模式(SIM)下对46种增塑剂进行定性,采用外标法进行定量测定。各种增塑剂在0.1～2.0 mg/L质量浓度范围内呈线性,相关系数为0.9910～0.9999,各组分检出限均在0.005～0.05 mg/kg之间。在2种食品模拟物中,3个浓度添加水平下46种增塑剂的加标回收率在69.51%～107.21%之间,精密度(RSD, n=6)为3.53%～18.95%。该方法可满足PVC食品接触制品及4种不同性质的食品模拟物中多种类增塑剂的快速筛查和准确定性、定量测定要求。     

功能型单层石墨烯的热剥离法制备及其超电容性能

以氧化石墨(GO)作为前驱体,在两种不同热剥离温度下制备了两类功能型单层石墨烯.其中第一类功能型单层石墨烯通过在较低温度及空气气氛下热剥离GO制备;第二类功能型单层石墨烯通过在氮气保护下高温热剥离GO得到;利用氮气吸附-脱附方法测定了两类样品的比表面积,利用电化学测试方法分析了其超电容性能.结果表明,通过低温热剥离的方式即可以有效剥离GO;两类样品均具有较高的BET比表面积.低温热剥离GO所制备的功能型单层石墨烯在2 mol/L KOH体系中的最大比电容值约为220 F/g;而通过高温热剥离GO所制备的功能型单层石墨烯虽然同样具有较高的BET比表面积,但其最大比电容值下降至约150 F/g.这表明通过低温热剥离GO所制备的功能型单层石墨烯具有更优异的超电容性能.     

Photocatalytic degradation and adsorption of 2-naphthol on suspended TiO2 surface in a dynamic reactor

The photocatalytic oxidation of 2-naphthol has been investigated at room temperature in a dynamic photoreactor with system UV/O2 (air) and aqueous suspension of titanium dioxide TiO2 irradiated under a variety of conditions. The kinetics of disappearance of pollutant were affected by several operating parameters such as TiO2 mass, concentration of the substrate and reaction pH. The experiments were measured by high performance liquid chromatography. A Langmuir-Hinshelwood model was found to be accurate for photocatalytic degradation and indicates that adsorption of the solute on the surface of semiconductor particles plays a role in photocatalytic reaction.     

苯基键合高比表面积活性炭的制备及其对挥发性有机化合物的吸附性能研究

以核桃壳为原料,经过碳化、KOH活化, 制备了高比表面积活性炭,通过三甲基氧基苯基硅烷对活性炭表面进行改性,制得苯基键合高比表面积活性炭吸附材料.通过氮气吸附法测定了苯基键合活性炭的比表面积及孔径分布;采用红外光谱、X射线光电子能谱、X射线粉末衍射技术对苯基键合活性炭的有机官能团、表面元素的化学环境及晶体结构进行了表征.将该吸附材料制成采样管,吸附空气中的挥发性有机物,二硫化碳解吸后使用气相色谱进行分析.考察了苯基键合活性炭对乙醇、丙酮、正己烷、乙酸乙酯、四氢呋喃、1,2-二氯乙烷和苯共7种挥发性有机化合物(VOCs)的吸附性能,饱和吸附量在129~216 mg/g之间;在0.05~ 2.50 mg/mL范围内,7种组分的峰高与浓度呈良好的线性关系,检出限在0.92~3.60 mg/m3之间.     

Thermal Decomposition Studies of Organoplatinum Films

 This study examines the thermal decomposition of 1,5-cyclooctadiene platinum (II) chloride organometallic films, deposited by thermal evaporation. The thin film samples were annealed both in air and hydrogen with well-controlled temperature regimes. After annealing, the decomposed thin films were examined by AFM and STM scanning probe, XPS and TEM microbeam analytical techniques. The experimental results confirm that the thermal decomposition products on silicon substrates are composed predominantly of metallic platinum. Annealing in hydrogen can reduce substantially the decomposition temperature of the material from around 250 to 160 °C but the surface morphology of the decomposed films is significantly different to those annealed in air. The metallic nature of the thermally decomposed films was confirmed by bonding configuration recognition, electronic property probing and microstructure analysis.     

Principles of methane adsorption and natural gas storage

The adsorption amount of methane on 16 different kinds of materials at 3.5 MPa and 298 K holds a linear relation with the specific surface area. The linear relationship implies that gases are adsorbed monolayerly on the surface of adsorbents at above-critical temperatures. Determination of surface area and calculation of storage capacity of a material are explicitly discussed. It is indicated that methane storage is different from natural gas storage and the difference affects the development of storage material. Natural gas is a mixture and all components other than methane cannot be desorbed when the tank pressure released to atmospheric at ambient temperature, therefore, a storage mechanism other than adsorption might be more suitable.     

Identification and quantification of diesel fuel components derived from off-shore drilling operation discharges

A GC/MS technique that provides quantitative and qualitative information on diesel fuel components in drilling muds is described. Several low molecular mass aromatic components of diesel fuel are identified as indicators of diesel fuel. The presence and relative concentration of these indicators is used to identify diesel fuel contamination. This information can be used to approximate the amount of diesel fuel contamination in off-shore drilling discharges.     

Metal@COFs: Covalent Organic Frameworks as Templates for Pd Nanoparticles and Hydrogen Storage Properties of Pd@COF-102 Hybrid Material

Three-dimensional covalent organic frameworks (COFs) have been demonstrated as a new class of templates for nanoparticles. Photodecomposition of the [Pd(η(3) -C(3) H(5) )(η(5) -C(5) H(5) )]@COF-102 inclusion compound (synthesized by a gas-phase infiltration method) led to the formation of the Pd@COF-102 hybrid material. Advanced electron microscopy techniques (including high-angle annular dark-field scanning transmission electron microscopy and electron tomography) along with other conventional characterization techniques unambiguously showed that highly monodisperse Pd nanoparticles ((2.4±0.5)?nm) were evenly distributed inside the COF-102 framework. The Pd@COF-102 hybrid material is a rare example of a metal-nanoparticle-loaded porous crystalline material with a very narrow size distribution without any larger agglomerates even at high loadings (30?wt?%). Two samples with moderate Pd content (3.5 and 9.5?wt?%) were used to study the hydrogen storage properties of the metal-decorated COF surface. The uptakes at room temperature from these samples were higher than those of similar systems such as Pd@metal-organic frameworks (MOFs). The studies show that the H(2) capacities were enhanced by a factor of 2-3 through Pd impregnation on COF-102 at room temperature and 20?bar. This remarkable enhancement is not just due to Pd hydride formation and can be mainly ascribed to hydrogenation of residual organic compounds, such as bicyclopentadiene. The significantly higher reversible hydrogen storage capacity that comes from decomposed products of the employed organometallic Pd precursor suggests that this discovery may be relevant to the discussion of the spillover phenomenon in metal/MOFs and related systems.