氯甲基苯乙烯包夹硅基单柱强阴离子固定相的制备及应用

用氯甲基苯乙烯包夹硅胶基质制备出一种新型强阴离子色谱柱填料,该填料具有良好的色谱性能,可以较好地分离常见的一些无机阴离子;另外,该填料可以对油田中用作驱油剂的单、双石油磺酸盐进行较好的分离。     

亲水单分散聚合物基质强阴离子色谱固定相的制备及应用

以自合成6.0μm大孔单分散交联聚甲基丙烯酸环氧丙酯微球为基质,采用化学键合法制备了季铵型强阴离子色谱填料,该填料具有良好的色谱性能。选用6.0 mmol/L Na2CO3+5.5 mmol/L NaHCO3混合液作淋洗液,在流速为1.0 mL/min下,可以很好地分离常见的6种无机阴离子(F-、Cl-、NO-2、Br-、NO-3、SO2-4)、4种低碳链酸(甲酸、乙酸、一氯乙酸、草酸)以及甲酸、乙酸和一些无机阴离子的混合物。考察了淋洗液种类、pH值和有机溶剂对6种无机阴离子分离的影响。在最佳色谱条件下,6种无机阴离子在一定浓度范围内具有良好的线性关系和低的检出限。采用该方法对本地自来水进行测定,4种离子可在22 min内完全分离,各离子的加标回收率为96.4%~100.6%。     

窄分布聚苯乙烯—二乙烯苯微球及阴离子色谱柱的制备和应用

报导了制备球径分布较窄的聚苯乙烯—二乙烯苯微球及阴离子色谱柱填料的制备方法和条件以及阴离子色谱柱填料的性能和应用效果。试验了乳悬聚合中影响本乙烯—二乙烯苯球径及其分布的主要因素(分散稳定剂的质和量以及聚合过程降低和防止微球的凝结)。     

直接电导检测-离子色谱法分离测定氟硼酸根及常见无机阴离子

研究了直接电导检测-离子色谱法分离测定BF4-及常见无机阴离子(F-、Cl-、Br-、NO3-、SO24-)。实验采用Shim-pack IC-A3阴离子交换色谱柱,分别选用邻苯二甲酸氢钾、对羟基苯甲酸 三(羟甲基)氨基甲烷 硼酸、邻苯二甲酸 三(羟甲基)氨基甲烷为淋洗液,考察了淋洗液种类、浓度、色谱柱温度、流速对分离测定BF4-及常见无机阴离子的影响。确定最佳色谱条件为:以1.25 mmol/L邻苯二甲酸氢钾为淋洗液,流速1.5 mL/min,柱温45℃。在此条件下可同时基线分离6种阴离子,且色谱峰形对称。所测阴离子的检出限为0.02~0.58 mg/L;峰面积的相对标准偏差(RSD,n=5)小于0.8%。将方法应用于测定离子液体中的BF4-及其它无机阴离子,加标回收率在98.2%~102.7%之间。     

离子转换色谱-紫外检测法测定啤酒中的无机阴离子和有机酸

建立了离子转换色谱与紫外检测器联用检测啤酒中无机阴离子与有机酸的新方法。在传统的离子色谱基础上引入两根离子转换柱,无机阴离子与有机酸经过两步转换,定量转换成有相同紫外响应的碘酸盐,然后用紫外检测器代替电导检测器进行定量分析。在Dionex AS11-HC阴离子色谱柱上,采用KOH梯度淋洗方式实现了12种无机阴离子与有机酸的分离。结果表明,12种无机阴离子和有机酸检出限（S/N=3）与定量限（S/N=10）分别为6.168~29.01 μg/L与20.56~66.30 μg/L;线性关系良好（r在0.9994以上）,回收率为89.0%~117.0%,RSD均小于1.0%,该方法与传统的电导检测器检测结果相当。该方法简单快捷,只需采用少数标准曲线,就可以实现啤酒中无机离子与有机酸的定量测定。     

离子色谱法同时分析啤酒中的有机酸和无机阴离子

建立了以NaOH-甲醇混合淋洗液,离子交换色谱柱,电导检测器检测,分离啤酒中有机酸和无机阴离子的离子色谱法.结果表明：在20 min内分离出啤酒中的11种主要有机酸与无机阴离子,方法回收率和相对标准偏差分别为96.30%～104.8%和0.02%～4.0%.     

季铵型键合硅基单柱离子色谱柱填料的研制

单柱离子色谱法是七十年代末提出的一种快速、简便的离子分析方法。该方法最早使用以苯乙烯-二乙烯基苯聚合物为基体的低交换容量离子交换剂。这类填料具有使用pH值范围宽的优点,在单柱离子色谱分析中应用很广。同树脂型填料相比,硅基型柱填料因具有不溶胀、耐压、渗透性好等优点,在单柱离子色谱分析中也得到重视。程松林等已报道过硅基单柱阳离子色谱柱填料的合成。本文对季铵型键合硅基单柱阴离子色谱柱填料作一介绍。 实验部分     

离子色谱同时分离测定三氟甲烷磺酸根,氟硼酸根及常见无机阴离子

建立了离子色谱-直接电导检测同时测定三氟甲烷磺酸根,氟硼酸根及常见无机阴离子(F-,Cl-,Br-,NO3-,SO24-)的方法。实验采用Shim-pack IC-A3阴离子交换色谱柱,分别选用对羟基苯甲酸-三(羟甲基)氨基甲烷-硼酸,邻苯二甲酸-三(羟甲基)氨基甲烷,邻苯二甲酸氢钾为淋洗液,考察了淋洗液种类,浓度及色谱柱温度对分离测定三氟甲烷磺酸根,氟硼酸根及常见无机阴离子的影响。最佳色谱条件为:以1.2mmol/L邻苯二甲酸氢钾为淋洗液,柱温30℃,流速1.0mL/min。在此条件下,可同时基线分离7种阴离子,且色谱峰形对称。所测阴离子的检出限(S/N=3)为0.02～1.88mg/L,保留时间和峰面积的相对标准偏差(n=5)分别小于0.17%和2.05%。应用本方法测定离子液体中三氟甲烷磺酸根,氟硼酸根及常见无机阴离子,加标回收率在97.0%～102.8%之间。本方法简单,准确,可靠,具有较好的实用性。     

梯度淋洗离子色谱法同时测定西兰花中6种无机阴离子

构建一种利用梯度淋洗离子色谱技术分析西兰花中Cl-、Br-、NO2-、NO3-、PO43-和SO42-6种无机阴离子含量的方法.梯度淋洗色谱离子体系为DIONEX Ion Pac AS11-HC(4 mm×250 mm)色谱柱,流速1.0 mL/min,抑制器电流80 mA,KOH淋洗液梯度淋洗.6种阴离子线性相关系数...     

间接光度高效液相色谱法分析无机阴离子的研究

报导了间接光度高效液相色谱法测定了无机阴离子的新方法，在自己研制的硅基键合阴离子交换柱上，用１．０ｍｍｏｌ／Ｌ苯甲酸钠和０．６ｍｍｏｌ／Ｌ柠檬酸钠为洗脱液，可在１５ｍｉｎ内对Ｈ２ＰＯ４、Ｃｌ，ＮＯ２，ＮＯ３，ＳＯ４等六种阴离子得到较好的分离，对Ｃｌ的最小检测限为４．０ｎｇ。     

Chloromethylstyrene encapsulated and quaternized silica anion exchanger in high performance liquid chromatography

A kind of strong anion exchanger (SAX) was prepared with chloromethylstyrene encapsulated silica. This strong anion silica column has superior ability for the separation of anions, organic acids and also the mixture of them. Using this strong anion exchanger, the sulfonic acids can be separated. With gradient elution, the separation of petroleum mono- and di- sulfonates in Yumen sample can be also well obtained. This anion exchanger’s stability has been studied. After continuous use for three months the carbon and nitrogen contents and the chromatographic behavior of the exchanger were unchanged.     

单一阴离子交换柱同时分离有机酸和无机阴阳离子

研究了用乙二胺四乙酸（ＥＤＴＡ）作淋洗液时，性质迥异的有机酸、无机阴离子和碱土金属离子（Ｃａ＾２＋、Ｍｇ＾２＋）在同一阴离子交换柱上的同时分离以及保留机理，结果表明，在离子交换机理之外，非离子交换机理对有机酸及钙镁的ＥＤＴＡ络阴郭的保留行为起一定的辅助作用，９种有机酸和无机阴阳离子在１０ｍｉｎ内得到了较好的分离。各离子的电导检测灵敏度在１０＾－９至１０＾－１１ｍｏｌ，能满足环境和食吕分析的要求。     

Improvement of the chromatographic separation performance of an imidazolium ionic liquid functionalized silica column by in situ anion‐exchange with dodecyl sulfonate and dodecylbenzene sulfonate anions

The anionic part of ionic liquids can provide additional interactions during chromatographic separations. In this work, the chromatographic separation performance of a silica column functionalized with 1‐propyl‐3‐methylimidazolium chloride ionic liquid was improved by in situ anion‐exchange from chloride anions to dodecyl sulfonate anions and dodecylbenzene sulfonate anions. The separation performances of these ionic liquid functionalized phases were investigated and compared with each other using polycyclic aromatic hydrocarbons, phthalates, parabens, and phenols as model compounds. Results indicated that the new columns presented a better chromatographic separation than the original one. This was ascribed retention mechanism from organic anions. The introduction of dodecyl sulfonate anions increased the hydrophobicity of stationary phase. Furthermore, the phenyl groups of dodecylbenzene sulfonate anions could provide an enhanced selectivity to aromatic compounds such as polycyclic aromatic hydrocarbons by π–π interactions. Analysis repeatability of the new columns was satisfactory (RSD of retention time, 0.10–0.40%; RSD of peak area, 0.66–0.84%).     

Silica based click amino stationary phase for ion chromatography and hydrophilic interaction liquid chromatography

A silica based amino stationary phase was prepared by immobilization of propargylamine on azide-silica via click chemistry. This readily prepared click amino stationary phase demonstrated good selectivity in separation of common inorganic anions under ion chromatography (IC) mode, and the triazole ring in combination with free amino group was observed to play a major role for separation of the anions examined. On the other hand, the stationary phase also showed good hydrophilic interaction liquid chromatography (HILIC) properties in the separation of polar compounds including nucleosides, organic acids and bases. The retention mechanism was found to match well the typical HILIC retention.     

Use of Di(n-butyl) and Di(iso-butyl)dithiophosphoric Acids as Complexing Agents in the TLC Separation of Some d and f Transition Metal Ions

The thin layer chromatographic behavior of U(VI), Th(IV), lanthanides(III), Co(II), Ni(II), and Cu(II) on silica gel H with di(n-butyl) and di(iso-butyl)dithiophosphoric acids as complexing agents in the organic mobile phase has been investigated. The results obtained show that the dithiophosphate anion has a substantial effect on the migration of these metal ions. The presence of electron-donor solvents in the mobile phase increases retention, especially for U(VI), Th(IV), and lanthanides(III). The effect is explained on the basis of greater solubility of the metal chelates of the dithiophosphoric anions in the organic mobile phase, because of a solvation process. Separation was investigated for three groups of metal ions — actinides, lanthanides, and d transition metals. By choice of an appropriate organic mobile phase, separation of the pairs Th(IV)-U(VI), Pr(III)-Sm(III), Sm(III)-Gd(III), and Gd(III)-Er(III) was achieved, as was separation of Co(II), Ni(II), and Cu(II) from each other. A complex separation mechanism based on adsorption-desorption, cation exchange, and extraction is suggested.

     

固相萃取-离子色谱法测定甘蔗糖蜜及糖蜜酒精废液中的非氮有机酸和无机阴离子

建立了固相萃取-离子色谱测定甘蔗糖蜜及糖蜜酒精废液中乙酸、乳酸、琥珀酸、苹果酸、酒石酸、草酸、富马酸、柠檬酸、乌头酸等非氮有机酸和盐酸根、硫酸根、磷酸根等3种无机阴离子的方法。样品稀释液经强阴离子(SAX)固相萃取小柱净化除去糖类和色素等干扰基质,再用稀KOH溶液洗脱,经0.45 μm水膜过滤后,用IonPac AS15阴离子分离柱、KOH溶液梯度淋洗-抑制电导检测分离分析。考察了固相萃取小柱对待测离子的保留和洗脱条件。实验结果表明,除乙酸和乳酸的分离不完全、苹果酸与琥珀酸的组分重叠外,其余组分可达到完全分离,被测组分的浓度与其峰高在一定的范围呈良好的线性关系,检出限均低于0.20 mg/L,相对标准偏差(RSD)小于6.7%。测定了2种甘蔗糖蜜和1种糖蜜酒精废液中有机酸及无机阴离子,结果满足检测的要求,样品中各组分的加标回收率为94%～109%。     

Retention of some glucosinolates in anion exchange chromatography. Part I: Qualitative study on a silica-trialkylammonium exchanger

Summary The retention and separation of glucosinolates, as organic anions, were studied on a silica-based strong anion exchanger under isocratic elution conditions. All glucosinolates carry the same functional ionic group (-OSO ₃ ^– ), however they do not have the same retention in anion exchange chromatography. The plots of capacity factors of organic anions versus the reciprocal of eluent ion concentration show good linearity. From the slope and y-intercept data the major retention mechanisms are interpreted as ion exchange and reversed-phase interactions. The effects of nature and concentration of the eluent ion and the influence of organic modifier addition to the aqueous buffered mobile phase are also investigated. Direct and indirect UV detection were used.Our results open the way for the development of new systems for intact glucosinolate analysis which are easier to use than the present ion-pairing chromatographic method.     

Histidine-functionalized silica and its copper complex as stationary phases for capillary electrochromatography

A histidine-functionalized silica was prepared by covalent bonding of the functional groups to silane-treated silica gel. Conversion of functional groups was confirmed by infrared (IR) spectra, elemental analysis, and potentiometry. The functionality of the silica gel is 0.293 mmol g(-1). The coordination behavior of the histidine-functionalized silica was investigated by metal capacity and electron paramagnetic resonance (EPR). EPR measurements at different copper loadings were made. The results showed that the copper histidine complex might be distorted tetragonal. Both histidine-functionalized silica and its copper complex were employed as stationary phases for packed capillary electrochromatography (CEC). Electrical current was found helpful for evaluating the properties of frit construction and the stationary phase packing. Test samples include neutral compounds, inorganic anions and organic anions. Factors influencing the separation behavior have been studied. With copper-histidine functionalized silica under the condition of citrate buffer (10 mM, pH 4.0) and applied voltage of -20 kV, the separation of benzoic acid, D- and L-mandelic acid, phthalic acid and salicylic acid could be achieved within 12 min. The column efficiency for these acids was more than 1.2 x 10(5) plates m(-1), except salicylic acid.