Effects of ion-exchange on the pervaporation performance and microstructure of NaY zeolite membrane

Pervaporation performance of NaY zeolite membranes is improved by ion-exchange with di-valent nitrate salt.Different nitrate salts,including Co(NO_(3))_(2),Mg(NO_(3))_(2),Zn(NO_(3))_(2),Ca(NO_(3))_(2),Cu(NO_(3))_(2),KNO_(3),and AgNO_(3),have great effects on the channel structure and water affinity of the NaY zeolite membrane.When the concentration of nitrate salt,ion-exchange temperature and time are 0.1 mol·L^(-1),50℃and 2 h,the ion-exchange degree order of NaY zeolites is Ag^(+)>K^(+)>Ca^(2+)>Zn^(2+)>>Co^(2+)>Mg^(2+).Especially,Ag^(+)and K^(+)cation exchange degree of NaY zeolites are achieved to 96.54% and 82.77% in this work.BET surface,total pore capacity,pore size distribution and water contact angle of the ion-exchanged NaY zeolites are all disordered by mono-and di-valent cations.Di-valent nitrate salt is favor for increasing the dehydration performance of NaY zeolite membranes by ion-exchange.When the ion-exchange solution is Zn(NO_(3))_(2),the total flux variation and separation factor variation of the NaY membrane(M-5)are -45% and 230% for separation of 10%(mass)H_(2)O/EtOH mixture by pervaporation,and the ion-exchanged membranes showed good reproducibility.

TLC-SERS同时检测降压类保健食品中五种沙坦类违禁添加成分

由于人们不健康的饮食结构和生活作息习惯以及人口老龄化等因素,高血压等慢性病发病率逐渐增高,降压类保健食品逐渐受到人们青睐。但是市场中存在不良商家为了提高保健食品的功效,向保健食品中非法添加降压药,尤其是沙坦类降压药的现象。建立了一种薄层色谱层析技术(TLC)与表面增强拉曼光谱(SERS)联用方法,对降压类保健食品中五种可能添加的沙坦类违禁成分(奥美沙坦酯、厄贝沙坦、氯沙坦钾、替米沙坦、缬沙坦)进行同步检测。对五种药物的SERS检测最佳条件进行探究,并通过比较不同成分及配比的TLC展开剂对于五种药物的分离效果,经过大量配方试验后成功得到环己烷-乙酸乙酯-甲醇-冰醋酸=53∶35∶12∶0.25(v/v/v/v)的分离体系,对五种药物具有良好的分离效果。确定实验条件后利用TLC分离技术对样品溶液分别进行初步分离,在薄层板上不同比移值的斑点原位处滴加金胶进行SERS检测,对样品溶液在斑点原位处的SERS光谱进行采集、比较,确定。研究结果表明,五种沙坦类违禁添加成分可通过TLC明确分离,且其SERS光谱特征峰一致、重复性良好,根据各自的特征峰可快速定性分析,检出限在0.1~1 mg·kg^(-1)之间。研究建立的TLC-SERS方法简单、快速,能够为保健食品中违禁添加成分的现场初步快速筛查提供一定参考。

TLC Identification of Yao Medicine Pileostegia tomentellal and Extraction Technology and Content Determination of Umbelliferone

[Objectives]To establish a TLC and content determination method of Pileostegia tomentellal,with umbelliferone as the indicator component.[Methods]TLC identification was performed by silica gel G thin layer plate with n-hexane-ethyl acetate(4:3)as the developing agent,and the plate was examined by UV lamp(365 nm).The umbelliferone content was determined by HPLC:Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm);mobile phase acetonitrile-0.2%phosphoric acid gradient elution;detection wavelength 320 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The chromatogram of P.tomentellal showed the same color spot in the same position as that of reference medicinal material,and the spot was clear with good specificity.Umbelliferone showed a good linear relationship when the injection volume was 2.63-131.27μg/mL(R^(2)=0.9997).The average recovery of umbelliferone in the low,middle and high adding groups of P.tomentellal was 99.57%and the RSD was 2.15%.[Conclusions]The method can effectively identify Yao medicine P.tomentellal and accurately determine the content of umbelliferone in medicinal materials,which will provide a scientific basis for the development and utilization of medicinal resources of Yao medicine P.tomentellal.

Establishment of a TLC Identification Method for Ensete wilsonii

[Objectives]The paper was to establish a TLC identification method for Ensete wilsonii.[Methods]Usingβ-sitosterol as the reference,the effects of preparation methods of test solutions,developing solvents,developing distances and color developing agents on TLC analysis were investigated,and the best TLC conditions for E.wilsonii were determined.[Results]The test solution prepared with 90%methanol solvent was dotted on TLC silica gel G plate,and developed with dichloromethane-toluene-methanol=10:5:1.5 as the developing solvent.Then the plate was sprayed with 10%sulfuric acid ethanol solution,and dried with hot blast for color development.Finally,the plate was examined under an ultraviolet lamp at 365 nm.The TLC results of E.wilsonii obtained showed good separation and color development effect,and the spots were clear and characteristic.[Conclusions]This method is safe,specific,and easy to operate,and can be used as a TLC identification method for E.wilsonii.

TLC Identification and Extraction Process of Rubiasin-1-methyl Ether from Yao Medicine Chuanlianzhu

[Objectives]To establish a thin-layer chromatography(TLC)method for the determination of rubiadin-1-methyl ether in Yao Medicine Chuanlianzhu(Damnacanthus giganteus).[Methods]A silica gel G thin-layer plate was adopted for TLC.Petroleum ether(60-90℃)-chloroform-methanol-water(7:15:3:1)was used as the developing solvent and inspected under ultraviolet lamp(365 nm).The content was determined by Inertsil ODS-3 C 18 column(4.60 mm×250 mm,5μm),mobile phase:acetonitrile-0.2%phosphoric acid gradient elution,detection wavelength 277 nm,flow rate 1.0 mL/min,column temperature 30℃,injection volume 10μL.[Results]The spots of 10 Chuanlianzhu samples from different origins showed the same color at the same position as the control,and the spots were clear and specific.The injection volume of rubiadin-1-methyl ether showed a good linear relationship in the range of 2.90-145μg(R=0.9996).The average recovery rate of rubiadin-1-methyl ether in the low,medium and high dose groups of Yao Medicine Chuanlianzhu was 98.72%,and RSD=1.78%.[Conclusions]This method can effectively identify Yao Medicine Chuanlianzhu medicinal materials and accurately determine the content of rubiadin-1-methyl ether in the medicinal materials.It provides a scientific basis for the development and utilization of Yao Medicine Chuanlianzhu medicinal resources.

牙膏中三七皂苷TLC定性检测法的改进

目的:寻找、建立一个磷酸氢钙与二氧化硅复配体系牙膏中三七皂苷检测薄层色谱的方法与规程,适用于检测、验证牙膏成品中含有三七根酊、三七花酊、三七总皂苷、三七叶皂苷。方法:以过滤、化学反应、萃取、吸附、洗脱等原理分离出牙膏中存在的三七根、叶、花皂苷,并制成供试样品,通过比较供试样品与对照样品在硅胶板上显现的点位,进行结果判断,确认该成品是否符合配方和生产工艺加工制出。结果:供试品与对照品以三氯甲烷-乙酸乙酯-甲醇-水(15∶40∶22∶10)为展开剂,5℃~10℃展开,喷以10%硫酸乙醇溶液显色,供试品中主要成分的色谱点,与对照品色谱点应显相同位置;置紫外光灯(365nm)下检视,显相同的荧光斑点。结论:通过本次方法学改进,确认符合磷酸氢钙与二氧化硅复配体系牙膏的TLC检测方法。

Tribological Properties of Magnesium Ion-exchanged α-Zirconium Phosphate as a Solid Lubricant Additive in Lithium Grease

Magnesium ion-exchanged a-zirconium phosphates(Mg-α-ZrP) with particle sizes of 600 and 80 nm were prepared through the sealed ion-exchange and one-step hydrothermal synthesis methods, respectively. It was found that larger particles of Mg-α-ZrP had a higher load-carrying capacity than that of smaller particles, whereas smaller Mg-α-ZrP particles had better anti-wear properties than that of larger Mg-α-ZrP particles under mild loads. The correlation between the particle size of the sample and the surface roughness of the friction pair thus seems to be a key factor influencing the performance.

Preparation of Highly Dispersed Antimony-doped Tin Oxide Nano-powder via Ion-exchange Hydrolysis of SnCl_4 and SbCl_3 and Azeotropic Drying

Antimony-doped tin hydroxide colloid precipitates have been synthesized by hydrolysis of SnCl4 and SbCl3 using： （1） an ion-exchange hydrolysis to remove chlorine ions, and （2） isoamyl acetate as an azeotropic solvent to obviate water. The obtained dried powder is of high dispersivity without any need for further grinding. The size and dispersivity of the final particles are investigated with the aid of TG-DTA, BET, XRD and TEM. After having calcined, the antimony-doped tin oxide nanopowder possesses a tetragonal rutile structure with high dispersivity, uniform particles and low hard agglomeration.

Study on Removal of Trace Lead from Nickel Sulphate Solution by Ion-exchange Method

By comparing the adsorption capacity of several kinds of resins, D363 resin is regarded as the most suitable one for removing lead from nickel sulphate electrolyte. The effects of pH, temperature and contact time on exchange adsorption during removing trace lead from industrial nickel sulphate solution with D363 large pore weak alkali anion exchange resin are discussed. Optimum conditions of adsorption of lead from nickel electrolyte by D363 resin are at room temperature, pH 1 2, contact time 30 min.

Effective adsorptive denitrogenation from model fuels over yttrium ion-exchanged Y zeolite

The adsorption removal of indole and quinoline in octane with and without toluene over zeolites NaY and Yttrium Ion-exchanged Y(YY)using batch adsorption experiments was studied at 25℃and 0.1 MPa.YY was prepared by treating NaY with Y(NO3)3 solution twice via liquid ion-exchange method.NaY and YY were both characterized by XRD,SEM,N2 adsorption,XRF,NH3-TPD,and pyridine-FTIR techniques.Adsorption isotherms of indole,quinoline and toluene in octane were conducted at 25.0℃to explain the influence of toluene on nitrogen removal over NaY and YY.The partial destruct of the crystalline structure of NaY was observed after the introduction of yttrium ion,which led to an evident decline in BET surface area and pore volume of YY.Strong Br?nsted acidity and medium Lewis acidity were introduced by yttrium ion-exchange.Though the specific surface area and pore volume of YY were much lower than those of NaY,YY exhibited equivalent adsorption capacities for indole and quinoline as NaY in model fuels without toluene.In the presence of 20 vol%toluene,however,YY exhibited much higher adsorption capacities for indole and quinoline than NaY,especially in the case of quinoline.The improved toluene-tolerant of YY was ascribed to the strong acid–base interaction between YY and quinoline and the decreased adsorption strength between YY and toluene.

Redistributing Cu species in Cu-SSZ-13 zeolite as NH3-SCR catalyst via a simple ion-exchange

The nature and distribution of Cu species in Cu-SSZ-13 play a vital role in selective catalytic reduction of NO by NH3(NH3-SCR),but existing methods for adjusting the Cu distribution are complex and difficult to control.Herein,we report a simple and effective ion-exchange approach to regulate the Cu distribution in the one-pot synthesized Cu-SSZ-13 that possesses sufficient initial Cu species and thus provides a“natural environment”for adjusting Cu distribution precisely.By using this proposed strategy,a series of Cu-SSZ-13x zeolites with different Cu contents and distributions were obtained.It is shown that the dealumination of the as-synthesized Cu-SSZ-13 during the ion-exchange generates abundant vacant sites in the double six-membered-rings of the SSZ-13 zeolite for relocating Cu2+species and thus allows the redistribution of the Cu species.The catalytic results showed that the ion-exchanged Cu-SSZ-13 zeolites exhibit quite different catalytic performance in NH3-SCR reaction but superior to the parent counterpart.The structure–activity relationship analysis indicates that the redistribution of Cu species rather than other factors(e.g.,crystallinity,chemical composition,and porous structure)is responsible for the improved NH3-SCR performance and SO_(2) and H_(2)O resistance.Our work offers an effective method to precisely adjust the Cu distribution in preparing the industrial SCR catalysts.

Synthesis and Characterization of Ion-exchange Sulfonated Poly (ether sulfone)

N,N＇-Bis（3-hydroxyphenyl）-1,8,4,5-naphthalenetetracarboxylic bisimide was prepared from the reaction of 1,8,4,5-naphthalenetetrcarboxylic acid dianhydride and 2-aminophenol in N, N-dimethylformamide. Polymerization of this bisimide with 4,4＇-difluorodiphenylsulfone and disodium 3,3＇-disulfonate4,4＇-difluorodiphenylsulfone gave ion-exchange sulfonated poly（ether sulfone）. The structure of the title compound was characterized with H-NMR and its polymer was characterized with FT-IR.

Research on changes of hydrodynamics and ion-exchange adsorption in Brackish-Water Interface

In light of multiple field experiments in typical tidal areas with active sea-land interaction, corresponding analysis through hydrodynamic simulation and of ion composition evolution all insist on following conclusions. Due to the tide, the groundwater level is basically in line with its level but with a slight lag. Moreover, smaller amplitude of such changes were always accompanied by greater distance from shores. In this paper, two salt-freshwater interfaces were identified, namely, a large wedge-shaped interface and an inverted U-shaped one located at K5 (monitoring point). The critical hydraulic gradient of saltwater intrusion was between 0.0345 and 0.0377. Apart from that, mathematical and physical models were adopted to measure the influence of tides, showing a inverse proportion to the hydraulic gradient In addition, characteristics of ionic components can prove that K^+ was adsorbed and Ca^2+ was displaced during saline intrusion, while a reverse process was witnessed during desalting. In summary, cation exchange adsorption plus other complex physical chemical effects would take place during saltwater intrusion.

小蓟TLC鉴别方法优化及小蓟炭“炒炭存性”内在表征研究

目的优化小蓟TLC鉴别方法并研究小蓟炭“炒炭存性”内在表征。方法对2020年版《中国药典》中“小蓟”项下TLC展开方法中的薄层板和展开剂进行改进,建立小蓟炭的TLC鉴别方法和UPLC指纹图谱,并测定蒙花苷、金合欢素的含量。结果小蓟TLC鉴别建议使用硅胶G板,展开剂建议改为甲苯-丙酮-甲酸-甲醇(6∶3∶0.5∶2.5)。小蓟及不同炒制程度小蓟炭的蒙花苷、金合欢素含量变化与TLC鉴别结果一致。结论与2020年版《中国药典》相比,改进的小蓟TLC鉴别方法较原方法成本低,所用展开剂毒性小。建立的小蓟炭“炒炭存性”的内在表征结合外观性状可用于解决市售小蓟炭的质量问题。

基于茚三酮衍生化TLC-SERS检测血清中的多巴胺

基于茚三酮衍生化薄层色谱法(TLC)与表面增强拉曼光谱法(SERS)联用传感技术建立了一种简便、灵敏度高和选择性高的血清中多巴胺的分离检测方法。多巴胺与茚三酮的橘红色衍生化产物不仅带来可视化效果,而且提供了良好的SERS响应,大大增强了SERS强度。薄层色谱法是一种快速有效的分离方法,表面增强拉曼光谱法具有灵敏度高,能够直接给出分子信息的特点,实现了一种无标记且无损的衍生化TLC-SERS传感检测方法用于检测血清中的多巴胺。

Purification of a Choleragenoid by Ion-exchange Chromatography

Abstract: Choleragenoid was obtained in pure form by ultra-filteration and fractionation on cationexchange resin-phospho-cellulose column. The choleragenoid was highly pure as judged by the electrophoresis of isoelectric focusing,immunization and SDS-gel electrophoresis.The results of test are thesame as that of the standard choleragenoid.Keywoeds:choleragenoid; vibrio cholerae; purification;ion-exchange; chromatography

A RAPID METHOD TO DETERMINE DIFFUSION COEFFICIENTS OF COUNTER-IONS IN AN ION-EXCHANGE MEMBRANE

1 INTRODUCTIONRapid and precise methods to obtain the diffusion coefficients of counter-ions are im-portant for the characterization of ion exchange membranes.Many theoreticaldescriptions of ion transport in ion exchange membranes have been developed by usingthe principles of irreversible thermodynamics,or the Nernst-Planck equations.Fick’s law can also be used for the description of the transport of ions with equaldiffusivity.However,for counter-ions of different diffusivities,Nerst-Planck

Synthesis and Characterization of Ion-exchange Copolyimide

A new diamine, disodium 4, 4-di(4-aminophenoxy)-3, 3-disulfonate-1, 1- diphenyl- ketone, was prepared from the nucleophilic substitution of disodium 4, 4- difluoro-3, 3-di- sulfonate-1, 1-diphenylketone and p-aminophenol. Polymerization of this diamine and 4, 4-diamino-1, 1- diphenyl ether with 3, 3, 4, 4-tetracarboxyl dianhydride-1, 1- diphenyl ketone gave ion-exchange copolyimide. The new diamine and its polyimide were characterized with 1H-NMR and FT-IR.

Soft actuator based on ion-exchange polymer-metal composite

Ion-exchange polymer-metal composite （IPMC） is a new electroactive material. It has large deformation and high force weight ratio in the presence of low voltage （〈1.5 V）. In this study a soft actuator known as artificial muscle based on IPMC was prepared. The IPMC actuator is composed of a perfluorinated ion-exchange membrane and platinum plated on both sides of the membrane by chemical means. Experiences and some key points are introduced in preparation of the IPMC. Electromechanical behaviors of the actuator are investigated, Factors related to the actuator performance are discussed.

TLC-SERS对鸡肉中的氧氟沙星快检研究

采用薄层色谱法与表面增强拉曼光谱联用技术(TLC-SERS)分离和检测鸡肉中的氧氟沙星(OFX)。薄层色谱法(TLC)可以将目标分析物从混合物中快速分离出来,解决了SERS无法准确识别目标分析物的问题,且SERS具有灵敏无损的特点。采用商用硅胶60 F254荧光板作为固定相,无需对样品进行预处理,将含有OFX的鸡肉组织液混合液滴在商用硅胶板上即可实现TLC分离。鸡肉混合样品采用TLC分离后,在OFX对应位置滴加银纳米粒子,采用银纳米粒子作为增强基底,进行SERS检测。TLC-SERS联用技术实现了快速分离检测鸡肉的氧氟沙星,其检出限可达到0.01 ppm。