浊点萃取-192紫外可见分光光度法测定痕量铝

研究了浊点萃取(CPE)-紫外可见分光光度法测定痕量铝离子的新方法,利用非离子表面活性剂Triton X-114对铝试剂与铝离子形成的络合物进行浊点萃取。探讨了影响浊点萃取及测定灵敏度的因素。在最佳条件下,铝离子的富集倍率为13.5倍,检出限为0.33μg/L,RSD为0.2%(n=6),铝离子含量在10~150μg/L范围内服从比尔定律。本法对实际样品中的铝进行富集和测定,结果令人满意。     

浊点萃取分光光度法测定水样中痕量铁

建立了浊点萃取-分光光度法测定痕量铁的新方法。详细考察了溶液的pH值、螯合剂和表面活性剂浓度、平衡温度和时间等条件对浊点萃取效果的影响。该方法的线性范围为6.0~500μg/L(r=0.9996),检出限为1.58μg/L,加标回收率为98.7%~101.6%,相对标准偏差为1.3%~2.2%。该方法已成功应用于实际水样分析。     

浊点萃取-火焰原子吸收光谱法测定乙醛触媒微量钯含量

建立了以1-（2-吡啶偶氮）-2-萘（PAN）为络合剂,以非离子表面活性剂TritonX-100为萃取剂的浊点萃取分离富集-火焰原子吸收光谱法测定痕量钯的新方法。研究了溶液的酸度、络合剂和表面活性剂浓度、平衡温度和时间、离子强度等条件对浊点萃取效果的影响。该方法对钯的检出限为35．3ng／mL,相对标准偏差（RSD）为3．1％（n=8）,回收率97．6％0～106．7％。可用于乙醛催化剂中微量Pd（Ⅱ）的测定。     

浊点萃取-高效液相法测甘草中甘草次酸和甘草酸含量

采用浊点萃取法萃取甘草药材中甘草次酸和甘草酸,并用高效液相法测定其含量。非离子表面活性剂Triton X-114为萃取剂,观测表面活性剂的浓度、液固比、盐浓度及水浴平衡温度等因素对萃取结果的影响。实验得出萃取条件为Triton X-114的浓度0.03 g/m L,液固比100∶1,水浴平衡温度40℃,平衡时间10 min,Na Cl浓度为1.0 mol/m L。测得甘草酸回归方程:Y=29 465X+13 084 R2=0.999 1;甘草次酸回归方程:Y=21 009X+81014 R~2=0.999 8。本次实验建立研究甘草药材中微量有效成分的新方法,该方法是一种安全有效、灵敏准确的萃取方法,能够应用于药材中的微量成分的富集。     

甘氨酸在痕量铜分析中的应用条件研究

以甘氨酸为络合剂,运用浊点萃取-紫外分光光度法进行铜离子的检测,对影响铜离子浊点萃取效率的相关因素进行研究,确定最佳的铜离子浊点萃取条件为:检测波长230nm,pH值9.0、NaCl溶液用量4.0mL,50.0mgmL-1 Triton X-100溶液用量1.0mL,萃取时间10min.     

聚氧乙烯型非离子表面活性剂的稳定-硫氰酸钻分光光度法

用苯萃取聚氧乙烯型非离子表面活性剂与硫氰酸钴所形成的络合物,然后用紫外分光光度法测定聚氧乙烯型非离子表面活性剂.检测范围为0.1～5mg/L.本法测定速度快,准备度好,灵敏度高,受阴离子表面活性剂扰小.     

浊点萃取法在脱脂月见草子中抗氧化成分提取中的应用

将粉碎后的月见草子以石油醚脱脂,以超声波辅助-浊点萃取法提取和富集活性成分,以提取物的清除DPPH自由基能力为指标,分别考察表面活性剂类型、平衡时间、液固比、离子强度和表面活性剂浓度对提取物的抗氧化活性的影响。结果表明,最佳提取工艺条件为:表面活性剂类型Triton X-100、平衡时间30 min、液固比30∶1 m L/g、氯化钠摩尔浓度3.1 mol/L、表面活性剂质量浓度45 g/L。该条件下提取物的清除DPPH自由基能力IC50值为1.065 mg/m L。表明以本方法从脱脂月见草子中提取的活性物质具有较强的抗氧化活性,且方法简单易行,利于月见草子资源的深入开发。     

浊点萃取-分光光度法测定硫酸阿米卡星

文章建立了硫酸阿米卡星的浊点萃取-紫外可见分光光度检测法。在酸性条件下,以溴麝香草酚蓝(BTB)为显色剂,TritonX-100非离子型表面活性剂浊点萃取硫酸阿米卡星。考察了pH、TritonX-100用量、水浴温度和水浴时间对萃取率的影响,优化了浊点萃取条件。在0.5～3.5μg·mL-1范围内线性关系良好,r=0.9996(n=7),高、中、低三个水平的回收率在92.9%～107.8%之间,大多数离子不干扰测定。本方法用于市售注射剂及人体尿液中硫酸阿米卡星含量的测定,结果令人满意。     

半胱氨酸螯合-浊点萃取-原子吸收光谱法测定痕量金属元素

选用L-半胱氨酸作为螯合剂,聚氧乙烯基壬基苯醚(PONPE 7.5)作为表面活性剂,建立了浊点萃取分离富集痕量过渡金属元素锌、钴、镍、铅的方法。结合火焰原子吸收光谱法,考察了各种实验条件的影响。在优化的实验条件下(样品pH 8.0;螯合剂浓度2.67×10-4mol/L;表面活性剂浓度0.33 g/L;平衡温度30℃;平衡时间20 min),计算了方法的检出限、相对标准偏差。方法对锌、钴、镍、铅的检出限分别为1.2、1.5、1.6、2.8μg/L,相对标准偏差为2.0%~4.3%。将此方法用于环境水样和果汁样品中4种金属元素的测定,回收率80%~106%。     

浊点萃取技术及其应用研究进展

浊点萃取是近年来发展起来的一种样品前处理技术。本文介绍了浊点萃取方法的相分离行为,讨论了关键因素如表面活性剂结构和浓度、平衡温度与时间、添加剂等对萃取效率的影响,总结了操作方法和优化。文章结合近年来的研究成果,对浊点萃取技术在金属离子、蛋白质和有机污染物分离富集中的应用进行了评述。最后探讨了浊点萃取技术的发展前景。     

高效液相色谱法测定愈创木酚甘油醚、福尔可定和马来酸氯苯那敏含量

采用高效液相色谱法同时测定愈创木酚甘油醚、福尔可定和马来酸氯苯那敏的含量.色谱柱为C18 (4.6mm×250 mm,5 μm),流动相为0.05 mol·L-1磷酸二氢钾溶液(每1000 mL加庚烷磺酸钠4.0g、三乙胺1.0 mL,用磷酸调pH值至2.5)—乙腈—甲醇(50∶ 20∶ 30),流速为1.0 mL·m...     

Temperature‐induced surfactant‐ mediated pre‐concentration of uranium assisted by complexation

Cloud‐point extraction (CPE) was used with lipophilic chelating agent to extract uranium(VI) from aqueous solutions. The methodology used is based on the formation of metal complexes soluble in a micellar phase of a non‐ionic surfactant, Triton X‐114. The metal ions complexes are then extracted into the surfactant‐rich phase at a temperature above the cloud‐point temperature. The influence of surfactant concentration on extraction efficiency was studied and the advantage of adding 8‐hydroxyquinoline (8HQ) as lipophilic chelating agent was evidenced. High extraction efficiency was observed, indicating the feasibility of extracting U(VI) using CPE. This study describes a four‐step process—(1) extraction, (2) thermo‐induced phase splitting, (3) back‐extraction and (4) second phase splitting—for the recovery of uranium from water. In our conditions, the extraction yield is quantitative and the concentration factor obtained is superior to 100. After stripping with a diluted nitric acid solution (pH < 1), the system can be recycled through a new four‐step cycle. Copyright © 2006 Society of Chemical Industry     

有机硅表面活性剂对水体中多环芳烃的浊点萃取研究

Cloud point extraction （CPE） processes with two silicone surfactants, Dow Coming DC-190 and DC-193, were studied as preconcentration and treatment for the water polluted by three trace polycyclic aromatic hydrocarbons （PAHs）： anthracene, phenanthrene and pyrene. For all cases, the volumes of surfactant-rich phase obtained by two silicone surfactants were very small, i.e. a lower water content in the surfactant-rich phase was obtained. For example, less than 3% of the initial solution was obtained in a 1% （by mass） surfactant solution, which was much smaller than that of TX-114 in the same surfactant concentration. And TX-114 is known as a high compact surfactant-rich phase among most nonionic surfactants, thus the comparison showed that an excellent enrichment was ensured in the analysis application by the CPE process with the silicone surfactants, and the lower water content obtained in the surfactant-rich phase is also important in the large scale water treatment. The influences of additives and phase separation methodology on the recovery of PAHs were discussed. Comparing with DC-193, DC-190 has a lower cloud point and a higher recovery （near 100%） of all the three PAHs in same surfactant concentration, which was required for application as a preconcentration process prior to HPLC system. However the DC-190 solution is hard to be phase separated only by heating, whereas DC-193 has a relative higher phase separating speed by heating, but a high cloud point （around 360K） limits its application. Due to the phase separation by heating is the only method of CPE suitable to the large scale water treatment, the mixtures of two silicone surfacrants solutions were investigated in this study. A solution containing 1% of mixed DC-190 and DC-193 （in the ratio of 90 ： 10） removed anthracene, phenanthrene and pyrene near 100% with a relative low cloud point and quick phase separating speed.     

Cloud Point Extraction of Acetic Acid from Aqueous Solution

Abstract

A new acetic acid separation method was developed through a successful combination of cloud point extraction and complex extraction technology (CPE-SE), where an acetic acid complex compound formed and was solubilized in a surfactant micelle solution, instead of an organic solvent, and then concentrated into one phase by a phase separation process of the CPE technology. Since no organic solvent diluents were used, the new process was environmentally friendly and with a lower cost; meanwhile, the high selectivity of the complex extraction based on chemical complexation and high efficiency of CPE were also inherited as advantages over conventional solvent extraction process. In consideration of the compatibility and the related CPE characteristics, tributyl phosphate and PEG/PPG-18/18 Dimethicone were selected as complexing agent and surfactant of the CPE-SE system, respectively, and the extraction system was optimized by studying the effect of the main process parameters, including surfactant and complexing agent concentration, temperatures for the stirring and incubation steps, on the recovery and the distribution coefficient. A relative high recovery of 71.4% and a distribution coefficient of 1.4 were achieved simultaneously with the optimized process in the treatment of 0.1 M acetic acid solution. Based on its competitive extractability, high efficiency, low-cost, and environment friendlyness, the CPE-SE process was expected to be a potential separation method for a dilute acetic acid solution.     

一种含氟烷基磷酸酯类氟碳表面活性剂的复配研究

研究了含氟烷基磷酸单酯类表面活性剂[分子式为H(CF2)6CH2OPO(ONa)2,记为DFH-PS]与无机盐和普通碳氢表面活性剂的复配性能,研究结果表明,DFH-PS水溶液最低表面张力为23.73 mN/m;当NaCl浓度为0.2 mol/L时,可使DFH-PS水溶液最低表面张力下降到21.62 mN/m;阴离子碳氢表面活性剂十二烷基硫酸钠(SDS)对该含氟表面活性剂影响显著,当n(DFH-PS)∶n(SDS)=5∶1时,可使水溶液表面张力在很低浓度时降至22.22 mN/m;与非离子表面活性剂辛基酚聚氧乙烯(10)醚(OP-10)混合,当n(DFH-PS)∶n(OP-10)=8∶1时,可使水溶液表面张力降至27.0 mN/m。     

Nafion掺杂多壁碳纳米管固定Ru（bpy）32+的电致化学发光法检测壮观霉素的研究

利用Nafion掺杂多壁碳纳米管形成复合膜将Ru(bpy)32+固定于玻碳电极表面形成Ru(bpy)32+-N-C。基于壮观霉素对该电极电致化学发光信号的增强作用,建立了一种新的壮观霉素电致化学发光检测方法,方法的线性范围为1.0×10-5～2.0×10-4 mol.L-1,检测限为2.5×10-6 mol.L-1。该方法用于尿样中壮观霉素的测定,加标回收率在87.1%～120.2%之间。     

浊点萃取-紫外可见光谱法测定痕量钴

研究了浊点萃取(CPE)-紫外可见光谱法(UV/Vis)测定微量钴的新方法,利用表面活性剂聚乙二醇辛基苯基醚(TritonX-100)和配合剂2[(5-溴-2-吡啶)-偶氮]-5-(二乙氨基)苯酚(5Br-PADAP)对试样中的钴(Ⅱ)进行浊点萃取。探讨了影响浊点萃取及测定灵敏度的因素。在最佳条件下,钴的富集倍率为5,检出限为1.18ng/mL(n=11),RSD为2.8%(n=5,c(Co2+)=0.20μg/mL),钴含量在(0.01～0.5)μg/mL范围内服从比尔定律。本法对实际样品中的钴进行富集和测定,结果令人满意。     

超细二水磷酸铁的制备研究

以六水氯化铁、磷酸为原料,采用沉淀法制备超细二水磷酸铁,用阳离子表面活性剂CTAB控制颗粒生长和防止颗粒团聚。通过实验分析各因素对二水磷酸铁粒径的影响,得出较佳合成工艺条件为：投料比（磷铁物质的量比）为1.50,反应温度为85 ℃,阳离子表面活性剂CTAB用量为铁盐质量的1.5%。在此条件下得到的产物是平均粒径为1.5 μm的单斜晶型二水磷酸铁,其粒度分布均匀,分散性好。     

Cloud Point Extraction and Pre-Concentration of Four Alkaloids in Nelumbo nucifera Leaves by Ultrahigh Pressure-Assisted Extraction

A rapid micellar extraction and pre-concentration method by ultrahigh pressure-assisted was developed for four alkaloids in Nelumbo nucifera leaves. Nonionic surfactant polyoxyethylene octylphenol ether (OP-10) solution was selected as solvent. Various experimental conditions were investigated to optimize the extraction and pre-concentration process. The optimal UPE condition was 5% OP-10 (w/w) solution, 400 MPa of pressure, 1 min of extraction time, and 1:20 (g/mL) of solid/liquid ratio. The pre-concentration of alkaloids was achieved by cloud-point extraction (CPE) and the optimum CPE condition was incubated in a thermostatic water bath at 55°C for 10 min, with 10% OP-10 and 15% sodium chloride added into the solution. The pre-concentration factor (CF) value was 11.6 ± 0.127, and the CPE recoveries for O-nornuciferine, N-nornuciferine, nuciferine, and roemerine were 91.0%, 92.3%, 92.7%, and 94.5%, respectively.     

二氧化氯氧化降解三元采出液技术研究

三元复合驱采出液由于聚合物、碱、表面活性剂的存在,使采出液的粘度增加,乳化严重,油水分离困难,传统的应用于水驱、聚驱采出液的处理技术不能满足三元复合驱采出液的处理要求。本文研究了ClO2氧化降解三元采出液的效果,并且找出了ClO2的最优反应条件,结果表明,反应温度为45℃,采出液中ClO2浓度40mg·L-1,加酸量为0.5%,反应2h以上,采出液粘度可由16.65mPa·s下降到2.9mPa·s,阴离子表面活性剂浓度可由0.16mg·L-1下降到0.10mg·L-1。处理后的三元采出液的腐蚀率在腐蚀三级标准的范围内。