Microwave assisted-semi bionic extraction of lignan compounds from Fructus Forsythiae by orthogonal design

Microwave assisted-semi bionic extraction （MASBE） process for lignans from Fructus Forsythiae was studied. The influences of solvent pH value, microwave power, dosage of solvent and irradiation time were investigated. Optimum extracting parameters were determined by orthogonal experiments as follows： pH value of solvent at first extraction is 5.5-6.0, that at the second extraction is 7-8; microwave power is 700 W, mass ratio ofFructus Forsythiae to water is 1：12; irradiation time is 10 min, and extracting times is two. Under these optimal conditions, the yield of lignans reaches 0.364%. Compared with the conventional extraction methods, the MASBE process has the advantages of high extraction rate, high extraction selectivity.     

Separation of cobalt and nickel by non-equilibrium solvent extraction

Ｓｏｌｖｅｎｔｅｘｔｒａｃｔｉｏｎｉｓｇｅｎｅｒａｌｌｙｂｅｌｉｅｖｅｄｔｏｂｅａｋｉｎｄｏｆｅｑｕｉｌｉｂｒｉｕｍｅｘｔｒａｃｔｉｏｎｏｎｔｈｅｃｏｎｄｉｔｉｏｎｔｈａｔｔｈｅｔｗｏｐｈａｓｅｓａｒｅｍｉｘｅｄｆｏｒｅｎｏｕｇｈｔｉｍｅａｎｄｔｈｅｅｘｔｒａｃｔｉｏｎｐｒｏｃｅｓｓｃａｎｒｅａｃｈｔｈｅｓｔａｔｅｏｆｔｈｅｒ ｍｏｄｙｎａｍｉｃｅｑｕｉｌｉｂｒｉｕｍ .Ｓｏｍｅｔｉｍｅｓ ,ｔｈｉｓｋｉｎｄｏｆｅｑｕｉｌｉｂｒｉｕｍｅｘｔｒａｃｔｉｏｎｃａｎｎｏｔａｃｈｉｅｖｅｓａｔｉｓｆａｃｔｏ…     

Mechanism of crud formation in copper solvent extraction

The authors investigated the mechanism of crud formation in copper solvent extraction. It is indicated that pH value of solution and the phase ratio (O/A) are the main factors affecting crud formation in solvent extraction. The amount of crud extraction increases with aqueous pH value increase, and reduces with the increase of the phase ratio. Fe3 , Mg2 , fine air bubble and suspended particulates in leaching solution contribute to crud formation. One case is that a series of reactions of hydrolization and polymerization occurs for Fe3 , while pH＞2.5, polyhydric complex or Fe-SO4 complex are formed. Then the complex-ions of FeOH2 , Fe2(OH)4 2 cause poly-reaction, which is likely to lead emulsion. The study on Zeta potential indicates the repulsion between electriferous droplets in solvent extraction prevents phase coalescence, which is one of the major reasons for emulsion.     

Kinetic Spectrophotometric Determination of Trace Titanium（IV） Based on Oxidation Discoloration of Acid Chrome Blue K with Hydrogen Peroxide

A simple and sensitive kinetic spectrophotometric method for the determination of trace amounts of titanium（IV）, based upon the catalytic effect of Ti（IV） on the oxidation of acid chrome blue K （ACBK） by hydrogen peroxide in 0.002 mol/L sulfuric acid, is described. The reaction rate is monitored spectrophotometrically by measuring the decrease in absorbance of ACBK at 524 nm. The detection limit of the method is 1.01×10^-9 g/mL, and the linear range is 0-0.048 mg/L The influence of acidity, concentration of reactants, reaction time, reaction temperature and foreign ions is also discussed. The optimum reaction conditions were established and some kinetic parameters determined. The apparent activation energy of the catalytic reaction is 5.32 kJ/mol. The relative standard deviation for the determination of titanium（IV） at the concentration of 0.048 mg/L is calculated to be 1.31% （n = 11）. In combination with solvent extraction separation, the method has been successfully applied to the determination of trace titanium（IV） in human hair, plant matter, tea and rock samples. The results are in good agreement with the certified values with the relative standard deviations （RSD） of 1.4%-3.5%.     

基于颜色和纹理特征的道路网络自动提取研究

提出了一种从高清晰的航拍图像中自动地提取出道路网络的方法,要求的输入仅仅是彩色航拍图像.应用了一项修改过的TPA技术;另外,新的开始点提取方法和基于此的新的评估方法也得以应用.该方案主要由三大模块组成:1,第一次道路检测;2,统计与融合;3第二次道路检测,评估及后期处理.     

超声波辅助法提取玉竹中总黄酮

以玉竹为原料,优化其总黄酮的超声波辅助提取工艺.在单因素试验的基础上,采用正交试验法,考察乙醇浓度、料液比、超声次数、超声时间对提取效果的影响,实验结果表明,玉竹总黄酮的最佳超声提取工艺条件为乙醇浓度40%、料液比1 13、超声2次、超声时间每次25 min,在该条件下玉竹总黄酮的提取率为2.389 mg/g,该提取方法具有操作简单、提取时间短等优点,适用于玉竹总黄酮的提取.     

超声强化提取丹参有效成分的研究

采用超声波技术对丹参酮提取进行强化，选择乙醇浓度、溶剂用量、超声作用时间、浸泡时间因素进行正交实验，得出影响总丹参酮提取率的大小次序先后为：溶剂用量〉乙醇浓度〉超声作用时间〉浸泡时间，优选出超声提取的最佳工艺条件：85%的乙醇，乙醇用量为30mL，超声作用时间为10min，浸泡时间为4h。在这个最佳条件下试验，总丹参酮提取率为81．82％。与常规提取方法相比较，具有溶剂用量少，提取效率高，提取时间短，温度低的优点。     

Study on the method of recovering and separating indium from residue containing indium

A method of recovering indium from complex smelting residue containing indium was investigated. Indium was extracted by technique of low acid leaching and solvent extraction. The conditions of separating iron and indium were studied and the optimal conditions were determined. When the residue is twoclass-countercurrent leached with 2 mol/L H2SO4 and 30-40 g/L NaC1 at 100 ℃, the leaching rate of indium is 80%. The extraction rate of indium is over 98% and that of iron is less than 5% after it is third-class-countercurrent extracted by P204, and when sulfonated kerosene is used as solvent, acidity in aqueous phase remains the same as that of leaching liquid, and phase is for 1 : 3. Using 2 mol/L HC1 as back-extraction agent, with phase ratio being 5 : 1, by third-class-countercurrent back-extraction, the back-extraction rate of indium is over 99%, but that of iron is very low, which can meet the need of separating indium and iron.     

气相色谱-质谱法分析测定甲壳类动物中的大甲基法尼酯

大甲基法尼酯是甲壳类动物体内的一种激素,在早期发育阶段具有改变形态的生物活性,并对繁殖起调控作用.本论文发展了一种基于正相高效液相色谱法纯化、气相色谱-质谱联用仪分析的综合分析方法.以非生物活性异构体反式-顺式-大甲基法尼酯(C-T-MF)作为内标物并用无分流注射法进样,采用电子撞击电离源电离后检测.利用无分流注射模式检测时,气相色谱-质谱联用仪的T-T-MF检出下限为100 pg/(次.柱).若取血淋巴样品4 mL,从最终25μL提取物中注入2μL,此方法的检出下限为0.3 ng/mL.在样品制备第一步(包括溶剂萃取、高效液相色谱纯化、气相色谱-质谱联用仪分析)就加入25 ng T-T-MF的条件下,总回收率为79%(RSD=5%,n=5).这种综合分析方法已被成功地应用于测定甲壳类动物血淋巴中T-T-MF的含量,如龙虾(Homarus americanus)、墨吉尔虾(Fennero peneaus merg-uiensis)、小龙虾(Procambarus clarkii).     

有机溶剂法提取黄粉虫油脂工艺研究

以黄粉虫为原料,研究了有机溶剂法提取黄粉虫油脂的工艺.对影响萃取率的因素:溶剂的选择、同液比、提取温度及时间等条件进行研究,并做正交试验,确定了获得最大提取率的条件,即:以无水乙醚作提取剂,料液比为1:6,温度40℃,时间为3 h.此条件下,萃取率达31.76%.此外对黄粉虫粗油进行精制,得到透明浅黄色、香味纯正的黄粉虫油.     

茶叶生产废料中茶多酚提取工艺研究

采用溶剂萃取法和离子沉淀法(Zn2+)相结合的提取工艺,分别进行单因素实验和正交实验,从乙醇浓度、原料粉碎粒度、浸提温度、浸提次数、料液比、浸提时间等方面探讨了提取工艺的参数。得出提取的最佳条件:乙醇浓度20%、40目、浸提温度70℃、浸提1次、料液比1:20、浸提时间15 min。     

微波萃取草莓中有机磷农药残留量的快速检测

研究了微波辅助萃取气相色谱法测定草莓中五种有机磷农药(乐果、马拉硫磷、敌敌畏、甲基对硫磷、毒死蜱)的快速检测方法。对萃取溶剂的种类进行了选择,并采用正交设计实验优化了溶剂用量、微波辐射时间及微波辐射温度等微波辅助萃取条件。结果表明,当溶剂用量为25 mL、时间为15min、温度为80℃时萃取效果最佳;五种有机磷的检出限为0.0015~0.0072mg/kg,回收率为87.99%~109.3%。     

Extraction process of chlorogenic acid in flos lonicerae by enzymatic treatment

A new method of extracting chlorogenic acid from flos lonicerae, and treating the materials with enzyme before being extracted by ethanol is developed, and the optimum conditions are also investigated in detail. Three important factors, enzyme dosage, treatment time and treatment temperature are adapted to optimize the extraction process. The experimental results show that the extract yield of flos lonicerae and chlorogenic acid can be obviously increased by the cellulase treatment, 61.5 mg chlorogenic acid is obtained from 1.00 g flos lonicerae at most. The optimal temperature of enzymatic treatment is 40-50 ℃. Compared with the use of single cellulase, the combined treatment of cellulase and pectinase increase the extract yield obviously but fail to improve that of chlorogenic acid.     

Solvent extraction of niobium from alkali solution by methyltrioctylammonium chloride

Ｏｆｔｈｅｔｒａｄｉｔｉｏｎａｌｐｒｏｃｅｓｓｅｓｏｆｎｉｏｂｉｕｍｅｘｔｒａｃｔｉｏｎ ,ｔｈｅｈｙｄｒｏｆｌｕｏｒｉｃａｃｉｄｄｉｓｓｏｌｕｔｉｏｎ ｓｏｌｖｅｎｔ (ＭＩＢＫ ,ＴＢＰｅｔｃ .)ｅｘｔｒａｃｔｉｏｎｐｒｏｃｅｓｓｉｓｗｉｄｅｌｙｕｔｉｌｉｚｅｄ[1] .ＢｅｃａｕｓｅｏｆｓｐｅｃｉａｌｐｒｏｐｅｒｔｉｅｓｏｆＨＦ ,ｈｏｗｅｖｅｒ ,ｔｈｉｓｐｒｏｃｅｓｓｇｉｖｅｓｒｉｓｅｔｏｍａｎｙｓｅｒｉｏｕｓｐｒｏｂｌｅｍｓ ,ｆｏｒｅｘａｍｐｌｅ ,ｓｅｒｉｏｕｓｃｏｒｒｏｓｉｏｎｏｆｐｒｏｄｕｃｔｉ…     

Synthesis and adsorption properties for Au（Ⅲ） of alkoxycarbonyl thiourea resin

A novel alkoxycarbonyl thiourea resin（ATR） was synthesized by monomer polymerization of oxydiethane-2,1-diyl dicarbonisothiocyanatidate and polyethylene polyamine, and characterized by FT-IR. The adsorption properties of ATR were investigated by batch test. The adsorption capacities for Au（Ⅲ）, Ag（Ⅰ）, Cu（Ⅱ）, Zn（Ⅱ, Fe（Ⅲ）, Ca（ Ⅱ ） and Mg（ Ⅱ ） are 4.65, 4.40, 0.40, 0.90, 0.86, 0.0080 and 0.016 mmol/g, respectively, when the adsorption condition is as follows： contact time 24 h, temperature 30 ℃, initial concentration of Au（Ⅲ） 5.08 mmol/L and that of other metals 0.10 mol/L, and concentration of acid 1.0 mol/L. The adsorption capacity for Au（Ⅲ） increases with the increase of contact time, temperature and initial concentration of Au（Ⅲ）. The capacity after five adsorption-desorption cycles remains 90% that of the first time, and the separation factors of ATR for binary metal ion solutions are larger than 995, indicating that ATR is of good regeneration property and selectivity. XPS results show that the functional atoms of ATR supply electrons for Au and coordinate with Au during the adsorption.     

Preparation and properties of metal-PVA composite hydrophilic ultrafiltration membranes

1　INTRODUCTIONOrganicmembraneshavegoodflexibilityandse lectivitybutpoormechanicalstrength ,whileinorgan icmembraneshavegoodthermalandchemicalstabili ty ,andimmunetomicroorganism ,butpoorselectivi ty .Thus ,thecombinationofboththeirgoodproper tiesmaymakeanovelmembranewithexcellentprop erties .Metallicfibersinteredmembranehasthechar acteristicsofhighmechanicalstrength ,greatvoidfractionandlittleflowdragoffiltration ,soitiswide lyusedasfiltrationmedium ,butithastoobigholediameterandisdifficu…     

加速溶剂萃取/GC-ECD分析土壤中多氯联苯的研究

为研究加速溶剂萃取土壤中的多氯联苯的方法,以土壤中8种多氯联苯为标样,进行了加速溶剂提取实验,并用佛罗里硅土柱净化,再用GC ECD气相色谱仪测定。实验优化了萃取条件,在20 g土壤样中添加50 ng多氯联苯混标,在实验温度100℃,萃取压力为10.3 MPa,萃取时间为20 min条件下用35 mL丙酮/正己烷混合液提取,并用GCECD测得多氯联苯回收率为95.63%~100.2%;相对标准偏差为0.95%~9.58%;方法检出限为0.089~0.882 ng/g。为进行比较,同时进行了超声波辅助提取和索式提取实验。结果表明:加速溶剂提取时间短,有机溶剂用量少,并且提取回收率高。     

Synthesis and properties of nickel borate acylate as a new rubber-steel cord adhesion promoter

Ａｄｈｅｓｉｏｎｐｒｏｍｏｔｅｒｓ(ＡＰｓ)ａｒｅｕｓｕａｌｌｙａｄｄｅｄｉｎｔｈｅｐｒｏｃｅｓｓｉｎｇａｎｄｍａｎｕｆａｃｔｕｒｉｎｇｏｆｒｕｂｂｅｒｃｏｍｐｏｓｉｔｅｍａｔｅｒｉａｌｓｓｕｃｈａｓｓｔｅｅｌｗｉｒｅｒａｄｉａｌ ｐｌｙｔｙｒｅｓ,ｃｏｎｖｅｙｅｒｂｅｌｔｓ,ａｎｄｒｅｉｎｆｏｒｃｅｄｈｏｓｅｓｉｎｏｒ ｄｅｒｔｏｍａｋｅｔｈｅｃｏｍｂｉｎａｔｉｏｎｏｆｍｅｔａｌｌｉｃｍａｔｅｒｉａｌｓｗｉｔｈｒｕｂｂｅｒｓｔｒｏｎｇｅｒ,ｔｏｉｍｐｒｏｖｅｔｈｅｑｕａｌｉｔｙｏｆｒｕｂｂｅｒｐｒｏ…     

室温离子液体合成过程的优化

用两步法合成离子液体(emim)BF4,以莫尔法测定N-甲基咪唑的转化率.在第一步季铵化反应过程中,不加热不添加任何有机溶剂,可获得高达96.5%的转化率;在第二步离子交换反应中,不加溶剂反应照样进行,转化率可达85.1%.在无惰性气体保护下,合成的产物(emim)BF4为无色透明(或略带黄色)的液体,红外吸收光谱分析未发现杂质吸收峰.结果表明,在简单条件下能得到较高的生产率.     

液相微萃取技术及其发展

样品分析中,以采样、萃取、分离、浓缩为一体的样品前处理技术成为现代样品分析技术发展的新趋向,它同时考虑了萃取溶剂用量以及样品前处理装置的小型化和自动化.液相微萃取技术是近年来发展起来的一种新型的样品前处理技术,该技术集采样、萃取和浓缩为一体,具有萃取溶剂量少、简便快速、萃取效率高、易与其他分析仪器联用等特点,是一种环境友好的萃取技术.本文综述了液相微萃取的萃取模式、取样方式、影响因素和应用.