苯乙烯与D—120共聚物的性能研究

合成了侧基含有过氧键的苯乙烯－Ｄ－１２０共聚物（Ｐｏｌｙ（Ｓｒ－ｃｏ－Ｄ－１２０）ＰＳＤ）。用ＩＲ、ＧＰＣ进行了表征。用ＤＳＣ、ＧＰＣ、ＴＧＡ探讨了共聚物的热稳定性及分解机理，并对其就地增容ＰＳ／ＬＤＰＥ共混体系进行了初步研究。结果表明：共聚物中过氧键浓度越大，其起始分解温度越低，降解越严重，该共聚物可作为ＰＥ／ＰＳ共混体系的就地增容剂。     

甲基睾酮人体代谢物的选择反应监控检测法

采用ＧＣ／ＭＳ／ＭＳ的选择反应监控（ＳＲＭ）法检测尿中甲基睾酮的人体代谢物，与ＧＣ／ＭＳ的选择离子检测（ＳＩＭ）法比较，ＳＲＭ法有更高的选择性和确证能力。该种检测方法的建立，可以更有效地判定阳性尿。     

气相色谱/质谱/质谱法分析石油基引燃物

应用Ｖａｒｉａｎ ３８００ ＧＣ／Ｓａｔｕｒｎ ２０００ ＭＳ 气相色谱／质谱联用分析仪（简称ＧＣ／ＭＳ／ＭＳ）对以汽油、煤渍和紫油为引燃物，燃烧聚丙稀化纤地毯和土壤时的模拟现场物品进行了引燃物的检出。发现采用ＧＣ／ＭＳ／ＭＳ方法比用ＧＣ／ＭＳ方法可以较彻底地排队由于柱注失、地毯燃物分解产物、土壤背景产物和地毯增塑剂等引起的干扰，而且可以提高检测灵敏度。详细考察了以不同质荷比的离子作母离子时对ＧＣ     

曼氏血吸虫谷胱甘肽S—转移酶Sm26／2抗原肽研究

在计算机辅助下，应用Ｇｏｌｄｋｅｙ和ＰＣ－Ｇｅｎｅ程序，根据新报道的曼氏血吸虫谷胱甘肽Ｓ－转移酶Ｓｍ２６／２的氨基酸序列，进行亲水性、柔韧性、可接近性、电荷分布和二级结构分析，预测出６个抗原肽，并用固相法进行了合成。经Ｄｏｔ－ＥＬＩＳＡ法测定，其中的２个对抗日本血吸虫免疫球蛋白多克隆抗体（抗－Ｓｉ－ＩｇＧ－ＰｃＡｂ）显示出较好的抗原性，１个对抗血吸虫表膜单克隆抗体（Ａ６ＭｃＡｂ）显示出较好的抗原性     

田菁胶、羟丙基田菁胶和瓜胶的分子量及其分布研究

用凝胶色谱（ＧＰＣ）法测定了羟丙基田菁胶（ＨＰＳ）、田菁胶（ＳＧ）和瓜胶原粉（ＧＧ）三种样品的分子量,其重均分子量顺序Ｍ＿（ＷＨＰＳ）＞Ｍ＿（ＷＧＧ）＞Ｍ＿（ＷＳＧ）,分子量范围为２．３×１０￣５～３．４×１０￣５,分散系数关系为Ｄ＿（ＨＰＳ）＝Ｄ＿（ＳＧ）＞Ｄ＿（ＧＧ）,并讨论了聚糖的多分散性与产品性能的关系。     

PC/ABS及PC/ABS/PE-g-MAH共混体系相容性的研究

研究了聚碳酸酯与ＡＢＳ（ＰＣ／ＡＢＳ）及ＰＣ／ＡＢＳ与马来酸酐接枝聚乙烯共聚物（ＰＣ／ＡＢＳ／ＰＥ－ｇ－ＭＡＨ）共混体系的力学性能和应力开裂性能。用ＤＳＣ和ＳＥＭ研究了共混体系的相容性。结果表明：ＡＢＳ的加入能提高ＰＣ的冲击强度,ＡＢＳ的含量及品种影响ＰＣ／ＡＢＳ合金的力学性能,ＡＢＳ能提高ＰＣ的耐溶剂应力开裂性能。ＰＣ／ＡＢＳ／ＰＥ－ｇ－ＭＡＨ共混体系的力学性能和相容性优于ＰＣ／ＡＢＳ共混体系,     

GC／MS检测信息的综合利用

从充分利用气相色谱／质谱（ＧＣ／ＭＳ）提供的信息来鉴定ＧＣ流出组分的目的出发，并以脂肪醇分析为例讨论了ＧＣ保留指数在ＭＳ谱图解析及ＭＳ鉴定结果的合理性检验方面的作用。总结了ＧＣ保留的同系物规律、极性规律、加和规律及异构物规律来指导ＭＳ谱图解析。提出了含氧化合物官能团相对于－ＣＨ２－质量数的保留指数附加贡献值辅助ＭＳ确定化合物的类别。同时采用了ＧＣ／ＭＳ中选择离子检测方法（ＳＩＭ）在分子离子峰受噪音干扰或太弱以至完全未观测到时来进一步佐证其相对分子质量。     

用多维色谱—稳定同位素稀释质谱联用技术测定酒中氨基甲酸乙酯

建立了一个用多维色谱／质谱方法（ＧＣ／ＧＣ／ＭＳ），结合同位素稀释技术（ＩＤＭＳ），测量酒中致癌物质－氨基甲酸乙酯（ＥＣ）的准确方法，主要步骤如下：向精确称取的样品中，加入精确称取为，以＾１３Ｃ，＾１５Ｎ标记的氨基甲酸乙酯（ＬＥＣ）内标溶液，试样经调节，ｐＨ萃取，浓缩等化学前处理步骤后，进行ＧＣ／ＧＣ／ＣＩＭＳ测定。测量以ＧＣ／ＧＣ的中心切割技术排除复杂基体的干扰。以化学电离（ＣＩ）和选择性子检测     

HPLC／CoPC修饰电极安培检测大鼠心肌线粒体中谷胱甘肽的研究

研究了钴酞菁修饰电极的修饰方法及其电化学性质。它可以催化氧化谷胱甘肽,降低ＧＳＨ的过电位。以ＣｏＰＣ何尝修饰电极为工作电极的安培薄层化学检测器,与高压认相色谱联用,在工作电极电位为＋０．８Ｖ时,ＧＳＨ的浓度在３．０＊１０＾－６ｍｏｌ／Ｌ－１．０＊１０＾－３ｍｏｌ／Ｌ浓度范围内与峰电流呈良好的线性关系,线性相关系数为０．９９９１,检出限为１．０＊１０＾－３ｍｏｌ／Ｌ浓度范围内与峰电流呈良好的线性关系     

弹性体型聚氨酯和聚碳酸酯共混物的形态结构

用ＤＳＣ、ＷＡＸＤ和ＳＡＸＳ研究了溶液共混的弹性体型聚氨酯（ＰＵ）／聚碳酸酯（ＰＣ）共混物的结构。结果表明，ＰＵ／ＰＣ为部分相容体系；共混过程中，溶剂ＤＭＦ的诱导作用使ＰＣ形成结晶，其长周期与ＰＵ硬段形成微相的长周期相近     

Characterizing property distributions of polymeric nanogels by size-exclusion chromatography

Nanogels are highly branched, swellable polymer structures with average diameters between 1 and 100nm. Size-exclusion chromatography (SEC) fractionates materials in this size range, and it is commonly used to measure nanogel molar mass distributions. For many nanogel applications, it may be more important to calculate the particle size distribution from the SEC data than it is to calculate the molar mass distribution. Other useful nanogel property distributions include particle shape, area, and volume, as well as polymer volume fraction per particle. All can be obtained from multi-detector SEC data with proper calibration and data analysis methods. This work develops the basic equations for calculating several of these differential and cumulative property distributions and applies them to SEC data from the analysis of polymeric nanogels. The methods are analogous to those used to calculate the more familiar SEC molar mass distributions. Calibration methods and characteristics of the distributions are discussed, and the effects of detector noise and mismatched concentration and molar mass sensitive detector signals are examined.     

Size exclusion chromatography of branched polymers: Star and comb polymers

Monte Carlo simulations were conducted to estimate the elution curve of size exclusion chromatography (SEC). The present simulation can be applied to various types of branched polymers, as long as the kinetic mechanism of nonlinear polymer formation is given. We considered two types of detector systems, (1) a detector that measures the polymer concentration in the elution volume to determine the calibrated molecular weights, such as by using the differential refractive index detector (RI), and (2) a detector that determines the weight‐average molecular weight of polymers within the elution volume directly, such as a light scattering photometer (LS). For polydisperse star polymers, both detector systems tend to give a reasonable estimate of the true molecular weight distribution (MWD). On the other hand, for comb‐branched polymers, the RI detector underestimates the molecular weight of branched polymers significantly. The LS detector system improves the measured MWD, but still is not exact. The present simulation technique promises to establish various types of complicated reaction mechanisms for nonlinear polymer formation by using the SEC data quantitatively. In addition, the present technique could be used to reinvestigate a large amount of SEC data obtained up to the present to estimate the true MWD.     

Quantitative interpretation of Fourier-transform infrared spectoscopic data from a size--exlusion chromatorgraphy solvent- evaporation interface

Quantitative evaluation of polymer composition across the SEC chromatogram can provide more accurate characterization of heterogeneous polymer samples for problem solving and for material specification. To this end Fourier-transform infrared spectroscopy (FTIR) with solvent-evaporation interfaces has become a very powerful detector for size-exclusion chromatography (SEC). The solvent-evaporation interface removes the mobile phase at the exit of the chromatograph and deposits the separated molecular sizes as polymer films on infrared transparent substrates. Quantitative interpretation of the FTIR spectra obtained from these films has recently been found to be best accomplished by using partial least squares. In this paper, polystyrene and poly(methylmethacrylate), alone, as blends, and a copolymer were analyzed in a SEC equipped with an evaporative interface. Molecular weight effects, wavelength selection, the effect of averaging spectra on results, and selection of the best data preprocessing method were investigated. General methods of evaluating these variables were developed to arrive at conditions for this particular "model" situation in order to provide a basis for the analysis of more complex polymers.     

Composition determination of binary polymer mixtures by size exclusion chromatography with light scattering detection

<正>Base on the principle of absolute quantification of size exclusion chromatography(SEC),a light scattering(LS) detector coupled with a concentration detector(refractive index detector) is utilized to determine the compositions of complicated binary mixtures.A theoretical analysis predicts that the response factors for both LS and RI detectors are linear functions with the composition of any specified polymer mixtures in the binary polymer mixtures.Two pairs of complicated binary mixtures were used to test the theory mentioned in the present paper,and the experimental results show an excellent accordance with the theory.     

An Eluent Pressure Detector for Aqueous Size Exclusion Chrohatography

Abstract

An on-line viscometer which measures the eluent pressure drop across a long capillary was developed for use in aqueous size exclusion chromatography (SEC). Intrinsic viscosities of several polymer standards were calculated from data collected by the viscometer. These viscosities agree well with the measurements made with a Ubbelohde four-bulb shear dilution viscometer. The on-line viscometer becomes more sensitive as polymer hydro-dynamic volume increases. Therefore, it can be more effective than a refractive index detector for SEC analysis of high molecular weight, water soluble polymers.     

Online Coupling of Size‐Exclusion Chromatography and IR Spectroscopy to Correlate Molecular Weight with Chemical Composition

The determination of molecular weight and correlated chemical composition is of major interest for the advanced analysis of copolymers, blends, or unknown samples. In this work, we present a new way of online coupling IR spectroscopy and SEC to achieve a chemically sensitive, universally applicable SEC detector. Our method overcomes the limitations of existing spectroscopy–SEC combinations. We solved the major problems, like huge intensity of solvent signals (polymer concentration in detector <1 g L⁻¹) and short measuring time (<30 s), by recording the IR spectra with fully optimized sensitivity and by following mathematical solvent suppression. The measuring time for a certain S/N was reduced in several optimization steps by a factor of more than 70 000. The resulting sensitivity allows online coupled IR–SEC measurements.     

Size exclusion chromatography with Corona charged aerosol detector for the analysis of polyethylene glycol polymer

A technique of using size exclusion chromatography (SEC) with the Corona charged aerosol detector (CAD) was developed and evaluated in comparison with refractive index (RI) and evaporative light scattering detection (ELSD) for fast screening of polyethylene glycol (PEG), a polymer used in preparing pegylated pharmaceutical compounds. These detection techniques were used in the analysis of multiple lots of PEG reagents. CAD was found to provide more accurate impurity and polydispersity profiles of PEG reagents that better differentiate their quality, while RI was not suitable for this application due to its low sensitivity and ELSD led to underestimation of the impurity and polydispersity. The accuracy of polydispersity determination by SEC-CAD was validated against a commercial reference standard of known polydispersity. The SEC-CAD technique and the observed differences between the three detectors can also be applied to polymer analysis in general.     

One‐pot synthesis of soluble and fluorescent aliphatic hyperbranched poly(amide‐imide) with solvent‐dependent emission

Aliphatic hyperbranched poly(amide‐imide) was facilely prepared by employing a functional thiolactone‐maleimide monomer. Highly efficient, selective and quantitative properties of amine‐maleimide Michael addition and aminolysis of a thiolactone guaranteed the generation of an ABB' thiol‐yne intermediate without side products, followed by consecutive thiol‐yne click reaction in one‐pot. The hyperbranched structure of the poly(amide‐imide) was confirmed by NMR spectroscopy and triple‐detector GPC/SEC analysis. Additionally, due to the presence of aminosuccinimide fluorophores and intrinsic physical property of hyperbranched polymers, this aliphatic hyperbranched poly(amide‐imide) possessed solvent‐dependent emission and presented good solubility in various organic solvents. © 2017 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2017 , 55, 2053–2060     

Data processing method for the determination of accurate molecular weight distribution of polymers by SEC/MALDI-MS.

A novel data processing method for a hyphenated technique, size exclusion chromatography/matrix-assisted laser desorption/ionization-mass spectrometry (SEC/MALDI-MS), has been proposed to determine accurate molecular weight distributions on the basis of the individual oligomer species of a polymer. This method is based on the concept that the individual peak intensities of MALDI mass spectrum observed for every SEC fraction with narrow molecular weight distribution could be adjusted to the quantified values to reveal the accurate molecular weight distribution using the signal intensity of the corresponding fraction on the SEC chromatogram observed with a refractive index detector. At first, the theory of the proposed date processing is described in detail. Then, experimental verification of the method is described. This was performed through the characterization of mixtures of three kinds of monodispersed polystyrene reference materials (weight average molecular weight = ca. 6000, 10000, and 18000) as model samples. An accurate trimodal molecular weight distribution for the individual oligomer species of the sample was obtained without any influence of the chromatographic band broadening observed in the original SEC chromatogram. Moreover, the method for depicting the elution profiles of individual oligomer species during SEC separation was also obtained as a "mass chromatogram" using the data processing procedure.