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建立了用盐酸乙醇标准溶液非水滴定γ-氨丙基三乙氧基硅烷(APS)偶联剂及其修饰的二氧化硅纳米颗粒表面氨基的方法,探讨了滴定溶剂、指示剂对滴定结果的影响,并用电位滴定法对指示剂的终点进行了确定。实验表明:以乙醇作溶剂、百里酚兰作指示剂时,其准确度较高、精密度较好,对APS偶联剂工业样品(A)的回收率为99.40%~100.8%,RSD为0.1%;对APS修饰的二氧化硅纳米颗粒(B),其回收率为99.45%~102.2%,RSD为0.66%。该方法简便、快速,可作为APS含量及其二氧化硅纳米颗粒表面修饰的氨基含量测定的基本方法和企业生产控制与质量检测的方法,具有良好的应用前景。 相似文献
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硅烷化与乙酰化联合衍生化法定性定量分析摇头丸 总被引:1,自引:0,他引:1
在摇头丸片剂中 ,有效成分为安非他明( amphetamine)类药物。此毒品除了掺假剂 ,多数还含有糖类作为稀释成分。这些成分的定性定量分析对于确立毒品特性、建立毒品间的区别与关联、进而追踪毒品的来源与走私路线具有重要的法庭科学意义。这一类毒品中 NH基团与 OH基团通常是共存的。在气相色谱分析中 ,为了提高检测灵敏度和改善色谱行为 ,衍生化是十分重要的。而对于这两类基团 ,硅烷化与乙酰化是常用的衍生化方法。本文采用 N-甲基 - N-三甲基硅烷基三氟乙酰胺( MSTFA)和 N-甲基 -双三氟乙酰胺 ( MBTFA)为这两类衍生化试剂的代表 ,… 相似文献
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利用溶胶-凝胶法在非水体系中合成出ZnO量子点,并用3-氨丙基三乙氧基硅烷(APTES)对其进行包覆,制得水溶性ZnO/氨丙基-硅氧烷量子点(ZnO-ASQDs)。通过实验确定最佳包覆条件:t=60℃,T=30min,nSi:nZn=1:1,VPEG/Vtotal=1/9。合成的ZnO量子点分别在348与512nm处有2个荧光发射峰,且激发区域较宽(220~360nm)。经过APTES包覆,ZnO量子点荧光发射强度明显增强,同时具有良好的水溶性与荧光稳定性,稳定时间可达60d之久。由Brus公式计算表明,包覆层对ZnO量子点不但改性还起到保护作用,抑制其团聚。经XRD与TEM证实,ZnO-ASQDs具有核壳结构,ZnO核平均粒径为6nm,整体粒径约为20nm。此外,通过调整ZnO核的粒径可制备出不同荧光颜色的ZnO-ASQDs。 相似文献
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在镍电极表面制备了γ-氨丙基三甲摒在硅烷膜并对其形成和结构进行了研究 。镍电极表面有机官能团硅烷膜的X射线光电子能谱(XPS)结果表明氮、硅等元素 在电极表面的存在,并且氨基在膜中有若干种存在方式,包括自由氨基和质子化的 氨基。通过对表面增强拉曼散射光谱(SERS)谱图的分析,发现与电极表面作用的 吸附基团硅醇羟基和氨基发生了竞争吸附,它们及其邻近基团的拉曼谱几随着电位 的负称除了相对强度发生变化以外,还发生了一定的位移,这缘于吸咐基团吸附的 量和吸附取向随电极电位发生了变化并形成的更为复杂的界面结构;氨基不同存在 方式之间也会随之发生转变,这一结果与X射线光电子能谱分析的结果相符合。原 子力显微镜(AFM)结果表明镍电极表面的有机官能团硅烷膜呈现为一种较规则的 多孔结构。 相似文献
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沿S0I0路径,以十六胺为模板剂,以3-氨丙基三乙氧基硅烷为有机硅源,通过与TEOS共水解沉淀合成了氨丙基官能化HMS介孔分子筛.采用粉末X-射线衍射分析、N2吸/脱附、扫描电镜分析、高分辨透射电镜分析、傅立叶变换红外分析以及元素分析等表征手段,对所合成的材料进行表征.氨丙基官能化HMS介孔分子筛具有worm-like孔道结构,且较为均一的孔径分布.研究了前体硅源中3-氨丙基三乙氧基硅烷含量的变化对氨丙基官能化HMS介孔分子筛的相结构及织构性能的影响.傅立叶变换红外分析表明,NH2-CH2-CH2-CH2有机基团分布在杂化HMS介孔孔道中. 相似文献
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阳离子和两性表面活性剂对石英表面润湿性的影响 总被引:3,自引:0,他引:3
利用座滴法研究了阳离子表面活性剂十六烷基醚羟丙基季铵盐(C16PC)和两性离子表面活性剂十六烷基醚羟丙基羧酸甜菜碱(C16PB)溶液在石英表面上的润湿性质, 考察了表面活性剂类型及浓度对接触角的影响趋势, 讨论了黏附张力和黏附功的变化规律. 研究发现, 两种表面活性剂在高能的石英表面的吸附造成石英-水的界面自由能(γsl)增大. C16PB通过弱相互作用随机吸附到石英表面, 其增大γsl的能力与降低表面张力(γ1g)的能力相当, 接触角(θ)随浓度变化不大. C16PC 随体相浓度增大能够在石英表面通过静电作用形成定向排列的单分子层, 而后在临界胶束浓度(cmc)附近形成双层结构, 接触角随浓度变化的趋势可分为4个区域, 并通过一个极大值. 相似文献
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In the solution adsorption experiment, different adsorption mode has been observed for aqueous ethanol and aqueous n-butanol, respectively. However, it is difficult to make an adjustment by the profiles of σ-c relationship. Choosing the experimental conditions improperly will give wrong results. Since there is no consistency between the Gibbs adsorption isotherm and Langmuir adsorption isotherm, the experimental data should not be fitted by using any algebraic equations or physical models. The data fitting for this experiment should be carried out according to the following steps:fitting the σ-lnc curve manually, making it monotonic and smooth; retrieving more data from this fitting curve, and re-plotting the σ-lnc curve; calculating the first derivatives at these data points (i.e., (∂σ/∂lnc)T); calculating surface adsorptions by Gibbs adsorption isotherm, Γ=-(∂σ/∂lnc)T/RT. As for the calculation of the cross-section area for the solute molecule, the effect of concentration of bulk solution (i.e., c) on the surface molecular density should be taken into account. 相似文献
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An adsorption isotherm that generalizes the Langmuir equation for the cluster adsorption of several interacting molecules
at one center is proposed. In the case of the adsorption of water molecules at surface hydroxyl groups on modified silica
it was shown that the energy and structure characteristics of such a system, determined by the ab initio method, agree with
the experimental data and lead to satisfactory agreement with the parameters of the proposed isotherm.
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Translated from Teoreticheskaya i Eksperimental'naya Khimiya, Vol. 41, No. 5, pp. 283–289, September–October, 2005. 相似文献
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利用等离子体技术研究聚苯乙烯表面的接枝聚合反应 总被引:2,自引:0,他引:2
用O2等离子体对聚苯乙烯(PS)进行预处理, 再用Ar等离子体引发N-乙烯基吡咯烷酮(NVP)在其表面接枝聚合. 通过接触角(CA)及表面自由能(SE)分析, 探讨了O2等离子体预处理条件对PS表面自由能的影响, 确定了预处理的最佳条件. 通过衰减全反射红外光谱(ATR-FTIR)、X射线光电子能谱(XPS)和动态接触角(DCA)分析, 比较了O2等离子体预处理前后和接枝聚合前后PS的表面组成及表面性能, 实验结果表明, 利用等离子体技术能成功地将NVP接枝聚合于PS表面, 接枝聚合后的PS表面由于极性高分子链和粗糙度的增加, 亲水性增强, 水滴易在其表面铺展. 由于接枝聚合后PS表面的高分子链在水中发生重构, 使后退角降低幅度较大, 接触角滞后现象明显. 相似文献
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氨基功能化纳米Fe3O4磁性高分子吸附剂对废水中Cr(VI)的吸附研究 总被引:3,自引:0,他引:3
采用分散聚合法通过共聚、开环反应, 对纳米Fe3O4进行表面功能化修饰, 得到富含NH2官能团的纳米磁性高分子复合材料. 通过透射电镜(TEM)、振动样品磁强计(VSM)、热重差热分析(TGA)、X射线衍射(XRD)、红外光谱(IR)等对其进行表征, 着重研究了其作为吸附剂对Cr(VI)的吸附性能. 结果表明: 该吸附剂对Cr(VI)的吸附能在10 min内达到平衡; 废水溶液pH值能显著影响吸附剂对Cr(VI)的吸附效果, pH为2.5时效果最佳. 废水中Cr(VI)的初始浓度、吸附时间、温度等因素对吸附效果均有不同程度的影响. 结合相应pH值下Cr(VI)的形态分布, 探讨了这种新型材料对Cr(VI)的吸附机理. 结果表明: 其吸附机理及吸附容量与废水中Cr(VI)的离子形式有关; 吸附过程以离子交换与静电引力为主. 等温吸附数据符合Langmuir模型, T=308 K, pH=2.5, V=40 mL时, 吸附剂的饱和吸附容量qm=25.58 mg/g. 吸附为吸热过程, 焓变ΔH=8.64 kJ/mol. 相似文献
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《Journal of Dispersion Science and Technology》2013,34(5):567-574
Abstract Scanning confocal microscopy was used for contact angle measurement of individual microspheres. The measurements were carried out by using different laser‐scanned layers of the particle floating on the air–water interface. The ratio of the diameter for the cross‐section of the protruded area of the particle at the air–water interface to the actual diameter of the particle is used for contact angle measurements. Two systems, i.e., glass and polystyrene microspheres with diameters of 3–10 and 6 µm, respectively, with water were used for this investigation (this size range of particles are most relevant to inhalation applications). Using the developed methodology, contact angles of 27° and 41° were measured (with water) for glass and polystyrene particles, respectively. The theoretical error in contact angle measurement for the developed methodology is determined to be generally about 1° with a maximum of 3° for contact angle of particles ranging from 2 to 24 µm in size; the experimental error was 4–6°. The contact angles of glass and polystyrene particles were compared to those obtained from pendant drop method and confirmed. 相似文献
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The adsorption of SO2 on alumina used in the aluminium industry, the so-called smelter-grade alumina, was studied in the temperature range 15–120°C.
It was found that at temperatures lower than 40°C, sulphur dioxide was bonded to alumina reversibly by physical forces, and
the adsorption could be described satisfactorily by the Langmuir adsorption isotherm. The heat of adsorption was estimated
to be −33 kJ mol−1. At temperatures ranging from 80°C to 120°C, which prevail in dry scrubbers in the aluminium industry, the heat of adsorption
was determined to be −56 kJ mol−1. When SO2 was adsorbed at temperatures higher than 80°C, about 30 % of the SO2 could not be desorbed even if the samples were heated up to 250°C. In the presence of SO2 and oxygen, the formation of sulphate was observed at temperatures above 90°C. 相似文献
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低温等离子体处理聚酯(PET)表面润湿性与表面结构的研究 总被引:11,自引:0,他引:11
陈杰瑢 《高等学校化学学报》1997,18(3):466-471
研究了O2、N2、He、Ar、H2和CH4气体低温等离子体改性聚酯(PET)的表面润湿性与表面结构的关系.用已知表面张力的液体测定接触角,作Zisman曲线,求得试样的临界表面张力γc;并按扩展的Fowkes式计算试样的表面张力γs及其三组分值γsa(色散力)、γsc(偶极矩力)和γ(氢键力),发现经O2、N2、He和Ar等离子体短时间处理的聚酯表面自由能显著增大,表面润湿性增强,主要是聚酯表面张力的氢键力成分的贡献,X射线光电子能谱分析表明,这是由于聚酯表面含氧或含氮极性基团增加所致. 相似文献
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High Pressure Adsorption Data of Methane, Nitrogen, Carbon Dioxide and their Binary and Ternary Mixtures on Activated Carbon 总被引:2,自引:0,他引:2
Adsorption equilibria of the gases CH4, N2, and CO2 and their binary and ternary mixtures on activated carbon Norit R1 Extra have been measured in the pressure range 0 P 6 MPa at T = 298 K. Pure gas adsorption equilibria were measured gravimetrically. Coadsorption data of the three binary mixtures CH4/N2, CH4/CO2, and CO2/N2 were obtained by the volume-gravimetric method. Isotherms of five ternary mixtures CH4/CO2/N2 were measured using the volumetric-chromatographic method. First, we present in a short overview the method and procedure of measurement. In a second part, the measured data of pressures, surface excess amounts adsorbed and absolute amounts adsorbed are presented and analyzed. In the last part of the paper the resulting pure gas adsorption data are correlated using a generalized dual-site Langmuir isotherm. Mixture adsorption can be predicted by this model using only pure component parameters with fair accuracy. Results are presented and discussed in several tables and figures. 相似文献