薄层色谱在高分子研究中的应用

本文综述了薄层色谱的高分子研究中的应用概况，着重介绍发薄层色谱在高分子的分离、分子量分布、组成分布、溶解度参数、官能度分布和高分子材料中助剂的测定等的应用。     

合成高分子作为手性固定相在高效液相色谱中的应用

具有旋光活性的合成高分子基于它的手性结构而具有广泛的应用,其中最实际和广泛的应用是在高效液相色谱中作为手性固定相来拆分对映异构体,目前已成为合成化学、分析化学以及制药化学领域必不可少的分离材料.本文简要介绍了高效液相色谱手性固定相拆分法,综述了合成高分子,包括加聚物特别是聚甲基丙烯酸酯类和聚甲基丙烯酰胺类聚合物、聚酰胺...     

书刊征订

色谱在材料分析中的应用(ISBN 978-7-122-10567-7)该书为《色谱技术丛书》之一,系统介绍了各种色谱方法与技术,包括气相色谱、高效液相色谱、离子色谱、凝胶渗透色谱、毛细管电泳等方法以及一些联用技术在无机材料中的金属元素和非金属元素的分析、无机材料和高分子材料结构     

体积排除色谱技术在高分子表征中的应用

体积排除色谱(SEC)也称为凝胶渗透色谱(GPC),是利用多孔填料色谱柱将溶液中的高分子按照流体力学体积大小进行分离的一种液相色谱技术,主要用于测定各种天然和合成高分子的平均分子量及分子量分布.多检测SEC技术可同时获得经色谱柱分离后高分子各级分的含量、分子量、均方根回转半径、流体力学半径、特性黏数等参数,进而推断高分...     

聚甲基异丙烯基酮和聚异亚丙基丙酮的不对称硅氢化反应

光活性高分子的合成具有重要意义，它在生物活性高分子、用于不对称合成的高分子试剂或催化剂以及不对称选择性色谱柱填料等领域具有潜在的应用价值．研究表明，不对称选择性聚合反应难以获得高光学活性的高分子［１］，而手性过渡金属络合物催化的高分子不对称反应是获得...     

凝胶渗透色谱异常问题系列讲座（4）液相基线噪声

在合成高分子材料过程中，我们应用凝胶渗透色谱（GPC）对高分子材料进行分子量的表征，应用LC高效液相色谱对原材料进行质量控制，在进行色谱实验的时候经常会碰到液相噪声异常情况，这些异常噪声如何引起，如何解决，使实验顺利进行，通过对这些异常现象的分析我们找到了一些规律，找到了一些解决方法，并汇成下表，供大家参考。     

小分子在高分子膜中无限稀释扩散系数的测定

随着高分子材料研究和应用的日益广泛,小分子在高分子中迁移规律的研究显示出其重要的理论和现实意义．小分子在高分子中的扩散系数是衡量其在高分子中迁移速率的一个重要物理量,其测定方法有多种,其中反相气相色谱法具有简便、迅速的特点且能适用于无限稀的浓度范围,反相气相色谱法早期所采用的模型是VanDeemter方程’‘·”,但此模型往往受柱子条件限制,且得出的扩散系数由于包含了小分子在气相中的扩散而其值偏大．最近R0mdhane和＂anner”‘提出了新的数学模型来描述填充柱的色谱过程,并采用矩分析法处理色谱流出峰,修正了流…     

聚二乙烯苯多孔微球液相色谱性能的研究

本文是在研究成孔性与孔结构的基础上进一步探讨高交联度聚二乙烯苯多孔微球在色谱过程中的吸附和溶解对保留的贡献。实验证明,无论在极性或非极性淋洗剂条件下、许多种有机化合物在分离过程中均以溶解的贡献为主;因此认为研究淋洗剂的改性对高分子固定相选择性的影响较与对硅胶类固定相更富有实际意义。实验中并建立了评价高分子本体对色谱峰展宽贡献的方法。最后介绍了在择优条件下得到的液相色谱应用实例。     

用高分子冠醚和高分子液晶混合物作毛细管气相色谱固定液的研究

作为毛细管气相色谱固定液,对高分子液晶和高分子冠醚的共混物和含冠醚的高分子液晶单一固定液进行了比较,结果表明它们具有大致相同的保留性能。     

《功能高分子材料》

全书共分17章，结合功能高分子材料的结构开发性能，制备方法及领域，对离子交换树脂，吸附树脂，离子交换纤维和活性碳纤维，高分子膜分离材料，高分子色谱固定相，高分子试剂。     

Effect of viscosity on stationary phase stability in capillary column gas chromatography

With recent advances in column technology it is now possible to prepare highly efficient, very inert, and thermally stable capillary columns coated with nonpolar polysiloxane stationary phases. Unfortunately, the same degree of success has not been achieved for some of the more polar polysiloxane phases. A parameter that has been studied little in the past in relation to stationary phase film stability is the viscosity of the stationary phase. In this paper the efficiency and stability of coated columns are correlated to the viscosity of the phase. Due to their structure, the viscosity of the phenyl-containing polysiloxanes change rapidly with temperature and hence, thin-film coatings are not stable at elevated temperatures. By using high viscosity phenyl-containing methylphenylpolysiloxanes which were recently synthesized, efficient and stable columns have been prepared.     

Comparison and characterization of reversed phases

Summary A pragmatic test procedure for comparison and evaluation of reversed phases is described. The differences in retention between RP8 and RP18 can be compensated for by adjustment of the eluent composition. A 10% increase in the water content doubles the k values, as does the exchange of an RP8 with an RP18 column. It is possible to differentiate between the two columns with the pair ethylbenzoate and toluene. Under stand-ard conditions (methanol-water, 55–45, v/v; 49–51, w/w) with RP8 ethylbenzoate is always eluted together or after toluene, whereas with RP18 it is always eluted in front of toluene.With the same eluent composition the suitability of stationary phases for the separation of basic solutes can be evaluated. With good phases—symmetrical peaks for basic solutes—aniline is always eluted before phenol and the peak asymmetry relationship of the aniline and phenol peak is less than 1.3. With such good stationary phases the retention of bases is independent of sample size if the linear capacity of 0.1 mg sample/g stationary phase is not exceeded. The test can also be used to study column stability towards hydrolysis.     

The preparation of analytically stable,immobilized stationary phase coatings on colums packing materials

Summary A coating of silicone SE-54 on Chromosorb W has been converted to an analytically stable, immobilized stationary phase layer by cross-linking with an organic peroxide. Up to 10% by weight has been applied in this manner. Excellent high temperature qualities are exhibited, such as low bleeding and good base line stability, during typical analyses.Poly (2,6-dimethyl-p-phenylene oxide) has also been crosslinked as a surface coating on Chromosorb W with an organic peroxide. From 3 to 4% by weight has been immobilized in this way. The resultant packing material, following high temperature conditioning, has been examined for use as an adsorbent of trace substances, similar to the applications to which such adsorbents as Tenax GC have commonly been applied, e.g. trace analysis of air. It appears to exhibit satisfactory properties for this analytical purpose.     

Porous graphitic carbon: A versatile stationary phase for liquid chromatography

Chromatographic stationary phases based on porous graphitic carbon were invented 30 years ago, while columns have been commercially available for 20 years. This special occasion deserved a complete review on this material. In this paper, we describe current knowledge on graphitic carbon stationary phases, based on over 400 fundamental studies and applications.     

Capillary electrochromatography of methylated benzo[a]pyrene isomers. II. Effect of stationary phase tuning

For Part II of our ongoing study, we present a strategy for stationary phase optimization for the capillary electrochromatographic (CEC) separation of the 12 methylated benzo[a]pyrene (MBAP) isomers. Utilizing the optimum mobile phase conditions from Part I of our study as a guide, seven commercially available stationary phases have been evaluated for their ability to separate highly hydrophobic MBAP isomers. Ranging in design from high-performance liquid chromatography (HPLC) to CEC application, each phase was slurry packed in house and tested for CEC suitability and performance. Several stationary phase parameters were investigated for their effects on MBAP separation including bonding type (monomeric or polymeric, % carbon loading, surface coverage), pore size, particle size, and type of alkyl substituent. In this manner, the present state of commercially available packings has been assessed in our laboratory. Utilizing the optimum polymeric C18-5 microm-100 A-PAH stationary phase, the effects of CEC packed bed length and capillary inside diameter (I.D.) were also evaluated. A 50 microm I.D. capillary, 25 cm packed bed length and 75% (v/v) acetonitrile, 12.5 mM Tris, pH 8.0, 20 degrees C at 30 kV, provided resolution of 11 out of 12 MBAP isomers thus showing the effectiveness of CEC for analysis of structurally similar methylated polyaromatic hydrocarbons.     

Donor-acceptor complex chromatography (DACC) part II. Review of papers

Summary Liquid chromatographic separations by the formation of donor-acceptor complexes (DAC) are reviewed. The article treats these examples, where donor or acceptor compounds are coated on or chemically bonded to a matrix. The effect of chemical structure of donors and acceptors, the effect of temperature and solvent composition of the mobile phase on retention is discussed.     

Short polystyrene monolith-fritted micro-liquid chromatography columns for rapid isocratic analysis of pharmaceuticals direct from plasma

The manufacture of micro-HPLC columns with combined stationary phases, a body of 3.5-μm XTerra-C₁₈ particles, and poly(styrene–divinylbenzene) (PS–DVB) frits is described in detail. The efficiency of the columns was assessed by rapid separation of neutral and acid compound mixtures. Direct analysis of some pharmaceuticals in plasma resulted in lower limits of detection (LOD) for salmeterol xinofate of 12.5 nanograms on-column.     

十二烯基丁二酸改性氧化锆色谱固定相性能研究

本文用十二烯基丁二酸（DSA）改性氧化锆得到一种新的锆基质色谱固定相。改性前后的红外光谱的差异表明，DSA以两个羧基与氧化锆结合，由于多位点结合方式提高了固定相的稳定性，因此固定相可以在碱性（pH8．5）条件下稳定使用。锆基质色谱固定相具有较强的疏水性，用于中性及碱性化合物的分离取得了满意的结果。     

新型杯[4]芳烃气相色谱固定相的研究

合成了上缘特丁基脱去的杯[4]芳烃25，27-二丁氧基-26，28-二（ω-十一碳烯氧基）杯[4]芳烃（p-H-C[4]B)及其相应的聚硅氧烷化高分子（PSO-p-H-C[4]B)，以有上缘用N，N-二乙基氨甲基取代的杯[4]芳烃5，11，17，23-四（N，N-二乙基氨甲基）-25，26，27，28-四（ω-十一碳烯氧基）杯[4]芳烃（p-DEAM-C[4]U），并首次将它们用作毛细管柱气相色谱固定液，涂制成色谱柱，考察了这些杯[4]芳烃色谱柱的性能。结果表明，研制的杯[4]芳烃柱对芳香位置异构体均有良好的分离能力。     

窄分布聚合物微球的制备及其在氨基酸分析上的应用

采用PVA和DBS-Na复合分散剂,在高速搅拌下(1500～2000转/min),用悬浮聚合法合成了粒度分布较窄的聚合物微球(3～10μm),并考查了聚合反应条件对聚合微球粒度及其分布的影响。最后,对所得磺化微球在氨基酸分析方面的应用进行了试验。