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941.
高效液相色谱-电感耦合等离子质谱法分析海洋沉积物中有机锡的形态 总被引:4,自引:0,他引:4
建立了高效液相色谱-电感耦合等离子质谱(HPLC-ICP-MS)测定海洋沉积物中二丁基锡(DBT)、三丁基锡(TBT)、二苯基锡(DPhT)及三苯基锡(TPhT)的形态分析方法。通过改变流动相组分比例,使4种有机锡达到基线分离。比较不同提取方法对标准参考物质PACA-2中有机锡的提取效率。以V(乙腈)∶V(H2O)∶V(乙酸)=55∶33∶12(含5%三乙胺,pH 3.0)为提取剂时,超声提取效率最高(>91.5%),其加标回收率均大于96%。本方法对DBT,TBT,DPhT和TPhT的检出限分别达到0.7,0.75,0.45和0.4μg/kg。对浓度范围为0.5~100μg/kg有机锡混合标准溶液进行测定,4种有机锡回归系数均大于0.998。利用本方法对几种海洋沉积物样品和海产品中的有机锡进行测定,在部分沉积物样品中检测到了DBT和TBT,部分海产品中测到了少量TBT和TPhT。 相似文献
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944.
建立了基于微波辅助-顶空液相微萃取在线联用、高效液相色谱法测定水样中邻硝基苯酚的分析方法。采用L16(45)正交实验设计对影响萃取的各种因素,如萃取有机溶剂、微波辐射功率、萃取时间、离子强度、样品液体积,进行了优化。优化后萃取条件为,以乙酸丁酯作为萃取溶剂,功率和时间分别为100W和12min条件下,离子强度为0的样品溶液体积为20mL。在优化萃取条件下,邻硝基苯酚的检出限LOD(S/N=3)为0.94μg/L,萃取富集倍数为30,实际水样的加标回收率为85.2%。理论分析和实验结果表明,微波辅助-顶空液相微萃取在线联用方法具有简便、快速、高效、节省溶剂、选择性好、应用范围广的特点。 相似文献
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Perez AA Sánchez CC Patino JM Rubiolo AC Santiago LG 《Colloids and surfaces. B, Biointerfaces》2011,85(2):50-315
Milk whey proteins (MWP) and pectins (Ps) are biopolymer ingredients commonly used in the manufacture of colloidal food products. Therefore, knowledge of the interfacial characteristics of these biopolymers and their mixtures is very important for the design of food dispersion formulations (foams and/or emulsions). In this paper, we examine the adsorption and surface dilatational behaviour of MWP/Ps systems under conditions in which biopolymers can saturate the air-water interface on their own. Experiments were performed at constant temperature (20 °C), pH 7 and ionic strength 0.05 M. Two MWP samples, β-lactoglobulin (β-LG) and whey protein concentrate (WPC), and two Ps samples, low-methoxyl pectin (LMP) and high-methoxyl pectin (HMP) were evaluated. The contribution of biopolymers (MWP and Ps) to the interfacial properties of mixed systems was evaluated on the basis of their individual surface molecular characteristics. Biopolymer bulk concentration capable of saturating the air-water interface was estimated from surface pressure isotherms. Under conditions of interfacial saturation, dynamic adsorption behaviour (surface pressure and dilatational rheological characteristics) of MWP/Ps systems was discussed from a kinetic point of view, in terms of molecular diffusion, penetration and configurational rearrangement at the air-water interface. The main adsorption mechanism in MWP/LMP mixtures might be the MWP interfacial segregation due to the thermodynamic incompatibility between MWP and LMP (synergistic mechanism); while the interfacial adsorption in MWP/HMP mixtures could be characterized by a competitive mechanism between MWP and HMP at the air-water interface (antagonistic mechanism). The magnitude of these phenomena could be closely related to differences in molecular composition and/or aggregation state of MWP (β-LG and WPC). 相似文献
947.
The thermal and dielectric properties of high performance cyanate ester resins/microcapsules composites 总被引:3,自引:0,他引:3
Novel high performance bisphenol A dicyanate ester (BADCy) resins/poly(urea-formaldehyde) microcapsules filled with epoxy resins (MCEs) composites have been prepared. The effects of different contents of MCEs on the thermal and dielectric properties of cured BADCy were investigated using dynamic mechanical analyzer (DMA), thermalgravimetric analyzer (TGA) and broadband dielectric analyzer. The dielectric properties of BADCy/MCEs treated in hot water and hot air were also discussed. The morphologies of BADCy/MCEs composites were characterized by scanning electron microscopy (SEM). Results indicate that the appropriate content of MCEs can improve or maintain the thermal stability, the low dielectric constant and dielectric loss of cured BADCy mainly owing to higher conversion of cyanate ester (-OCN) groups. After aged in hot water and hot air, respectively, BADCy/MCEs composites with small content of MCEs can retain the low dielectric constant and dielectric loss. 相似文献
948.
Hong Liu Mengyang Wang Yuguang Liang Weiran Cao 《Journal of solid state chemistry》2011,184(3):509-515
Mesoporous silicas and Fe-SiO2 with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 °C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 °C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 °C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO2 has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 °C for 12 d or steam-treated at 600 °C for 6 h. 相似文献
949.
Carrier-mediated three-phase hollow fiber microextraction combined with high-performance liquid chromatography-ultra violet detection (HPLC-UV) was applied for the extraction and determination of propylthiouracil in biological samples. Propylthiouracil (PTU) was extracted from 7.5 mL of the basic solution (the source phase) with pH 12 into an organic phase (n-octanol containing 6% (w/v) of Aliquat 336 as the carrier) impregnated in the pores of a hollow fiber, and finally was back extracted into 24 μL of the acidic solution located inside the lumen of the hollow fiber (the receiving phase). The extraction was performed through the gradient of counter ion from the source to the receiving phase. The effects of different variables on the extraction efficiency were studied simultaneously using an experimental design. A half-fractional factorial design was employed for screening to determine the variables significantly affecting the extraction efficiency. Then, the factors with significant effect were optimized using a central composite design (CCD) and the response surface equations were developed. The optimal experimental conditions obtained from this statistical evaluation included: source phase, pH 12; temperature, 25 °C; extraction time, 40 min; counter ion concentration, 2 mol L−1 of NaClO4; organic solvent 6% of Aliquat in octanol and without salt addition in the source phase. Under the optimized conditions, the preconcentration factors were between 125 and 198 and also the limit of detections (LODs) ranged from 0.1 μg L−1 to 0.4 μg L−1 in different biological samples. The calibration curve was linear (r2 = 0.998) in the concentration range of 0.5-1000 μg L−1. Finally, the feasibility of the proposed method was successfully confirmed by extraction and determination of PTU in human plasma and urine as well as the bovine milk and meat samples in microgram per liter, and suitable results were obtained (RSDs < 6.3%). 相似文献
950.
A simple, stable and sensitive electrogenerated chemiluminescence (ECL) detector was developed. It was based on tris(2,2-bipyridyl)ruthenium(II) (Ru(bpy)32+) immobilized on the surface of a Pt wire with Nepem-105D ion exchange solution. The detector was prepared by inserting a Pt wire with immobilized Ru(bpy)32+ (working electrode) into a capillary tube, followed by inserting another Pt wire (counter electrode) in this tube and sealing. ECL behavior was investigated using ofloxacin as an analyte. Under optimal conditions, stable ECL intensity was obtained. This detector has been used in HPLC-ECL for the determination of multiple target fluoroquinolone residues in milk. There is no post column reagent addition, which would dilute the analytes, potentially leading to chromatographic band-broadening. The system is very simple with low dead volume, low baseline and background noise, together with high sensitivity and stability. The as-prepared ECL detector, when was used for the determination of ofloxacin, pefloxacin, enrofloxacin and difloxacin in milk, demonstrated adequate sensitivity to allow quantification of trace FQ levels in commercial milk samples. One or more of the target FQ analytes were present at levels above the LOD of the new ECL detector in each and every one of the 22 milk samples analysed. 相似文献