聚硅氧烷气相色谱固定液的应用与进展

聚硅氧烷是一类非常重要的气相色谱固定液。本文对具有不同化学结构的聚硅氧烷固定液的应用与进展情况作了较详细的评述     

PP-g-PMMA表面性质的反相气相色谱分析

采用反相气相色谱探针技术研究了聚丙烯接枝聚甲基丙烯酸甲酯共聚物的表面物理化学性质,包括探针分子在聚合物表面吸附热力学函数、比保留体积以及分子间相互作用参数。探讨了共聚物中极性链段聚甲基丙烯酸甲酯的含量与其表面性质的关系。结果表明接枝共聚物表面组成中随聚丙烯接枝聚甲基丙烯酸甲酯含量的增加,其表面能增大,表面分子链与探针分子的相互作用增强,表面吸附能力也增强。     

硫酸铬钾结晶水合物用作气相色谱固定相的研究

硫酸铬钾结晶水合物用作气相色谱固定相的特性进行了研究 ,结果表明 ,其色谱性能良好 ,可作固定相使用。     

Dielectric and Chromatographic Characterization of Polyethylene Glycols as Stationary Phases

Abstract

Three types of polyethylene glycols of different molecular weights namely, 600, 4000 and 20000, were evaluated as liquid stationary phases in gas liquid chromatography. Thus, the retention mechanism for the studied polymer stationary phases, 15% by weight on chromosorb PAW and their thermodynamic parameters have been investigated via inverse gas chromatography. The effect of polymer molecular weight on their efficiency as liquid stationary phases for the gas chromatographic separation of different types of hydrocarbons is also studied. The dielectric constant of dilute solutions for the studied polymers as dissolved in solvent chloroform was studied corresponding to their polarities. Two different modes of clusters were determined due to the solute-solute and solute-solvent interaction through hydrogen bonds.

All studied polymers have higher performance for separation of cyclic and aromatic compounds. Good chromatographic separation of n-alcohols is obtained toward polyethylene glycol (PEG20000) of relatively higher molecular weight. The saturated hydrocarbons can be separated very efficiently using low molecular weight polyethylene glycol (PEG600).     

固相萃取-气相色谱法测定水中硝基苯类化合物的含量

建立了固相萃取-气相色谱法测定水中硝基苯类含量的方法。水样经固相萃取柱富集后,进入配有DB-5（30m×320μm×0．25μm）毛细管色谱柱的带ECD检测器的气相色谱中进行测定。测定的方法检出限分别为硝基苯：0．29μg／L,间-硝基氯苯：0．05μg／L,对-硝基氯苯：0．02μg／L,邻～硝基氯苯：0．01恤晷／L,对-二硝基苯：0．03μg／L,间-二硝基苯：0．08μg／L,邻-二硝基苯：O．01μg／L,2,4～二硝基甲苯：0．021μg／L,2,4-二硝基氯苯：0．021μg／L,2,4,6-三硝基甲苯：O．02μg／L,加标回收率在83．O％～118．6％之间,相对标准偏差为2．2％～9．7％。     

气相色谱法测定酒后人体汗液中乙醇含量的方法及研究

在酒后驾车引发的交通肇事案中,对驾驶员进行酒精的定性和定量检验对事故责任的定性有至关重要的作用。对气相色谱法测定酒后人体汗液中乙醇含量的方法进行了研究与探讨。通过对酒后人体分泌的汗液进行实验．利用乙醇易挥发的性质,用火焰离子（FID）检测器,采用顶空-气相色谱法进行分析测定,以峰面积定量,利用两点法测定汗液中的乙醇含量。此方法具有操作简便,快速,测定结果准确等特点。     

商品十八烷基聚氧乙烯醚用于气相色谱固定液

用商品十八烷基聚氧乙烯醚经电渗析制备了气相色谱固定液，用该固定液对环戊酮及环戊醇混合物进行了定性、定量分析，该固定液使用寿命可达１２个月以上。     

Analysis of Physical and Thermodynamic Properties of Poly(2-Phenyl-1,3-Dioxolane-4-Yl-Methyl-Methacrylate-Co-Styrene) Polymer with Inverse Gas Chromatography

In this study, physical and thermodynamic properties of poly(2-phenyl-1,3-dioxolane-4-yl-methyl-methacrylate-co-styrene) (PDMMA-ST) were investigated by using inverse gas chromatography. Two groups of solvents with different chemical natures and polarities were used to obtain information about PDMMA-ST-solvent interactions: alcohols and alkanes. The specific retention volume (V_g ⁰), the sorption enthalpy (ΔH₁ ^S), sorption free energy (ΔG₁ ^S), sorption entropy (ΔS₁ ^S), the weight fraction activity coefficients of solute probes at infinite dilution (Ω ₁ ^∞), and Flory-Huggins interaction parameters (χ ₁₂ ^∞) between polymer and solvents were determined for the interactions of PDMMA-ST with alcohols and alkanes by inverse gas chromatography in the temperature range of 333–473 K. Also, the solubility parameters of PDMMA-ST at infinite dilution were found by plotting the graph of [(δ ₁ ²/RT) - χ ₁₂ ^∞/V₁] versus solubility parameters, δ ₁, of probes.     

Stationary Phases for Complexation Gas Chromatography and Microextraction Methods

The main goal of this review is to provide an overview of the trends in the technological development of complexation gas chromatography. This kind of chromatography, despite the passage of years, continues to offer new opportunities. The authors would like to show how complexation gas chromatography evolved over the years, due to the variety of stationary phases with complexation properties, their ability to separate, very specifically, the structures of the molecules and chemical compounds, improving the quality of the obtained results, and continuously lowering the detection limits of the analysed compounds in very complex matrices, including environmental and medical samples. The work is dedicated to the memory of Professor E. Gil-Av, whose scientific achievements were the inspiration for the improvement and widening of the research on the use of complexing metal ions and coordination metal compounds for selective separation in gas chromatography.     

气相色谱法测定氨触媒升温还原中水汽浓度

样品气经固定相分离H2O、NH3等组分,热导池测定器检测,色谱数据工作站自动求出水汽浓度。     

离子液体作为气相色谱固定相的参数测定

将疏水性离子液体[BMIM]PF6用于气相色谱固定相中,检测分离环己烷、甲苯、邻二甲苯混合有机溶剂,并与邻苯二甲酸二壬酯填充柱对这3种物质的分离效果进行比较。实验结果表明：邻苯二甲酸二壬酯柱虽然也能将这3种物质分开,但各物质出峰太慢、保留时间长、峰高太低,而疏水性离子液体[BMIM]PF6柱对这3种物质有很好的分离效果,各物质保留时间缩短、峰高增强,由此得出离子液体作为气相色谱固定相对分离这类有机物的优势。     

反相气相色谱法表征PVC/纳米碳酸钙复合材料的表面性质

在30～60℃温度下,采用反气相色谱技术分析聚氯乙烯/纳米碳酸钙复合材料(PVC/NC)的表面色散自由能与表面路易斯酸碱性质,得出该材料在此温度区间的表面色散自由能。结果表明,PVC/NC的表面色散自由能随温度的升高而线性降低;PVC/NC为弱碱性路易斯两性聚合物其,路易斯酸常数Ka为0.20碱,常数Kb为0.39。     

气相色谱法测定二硫化碳中甲苯的测量结果不确定度评定

采用气相色谱法对二硫化碳中甲苯含量进行测试,找出影响测量不确定度的因素,通过建立数学模型对影响测量的各不确定度分量进行计算,求出合成不确定度和扩展不确定度,给出了气相色谱法测定二硫化碳中甲苯含量测量的相对扩展不确定度.     

气相色谱在乙苯脱氢实验中的应用

阐明了气相色谱在乙苯脱氢制备苯乙烯实验中的应用,叙述了气相色谱的工作原理、工作程序、数据处理、结果分析。     

2.4-二硝基甲苯的气相色谱分析

建立了以丙酮溶解试样,经OV-225石英毛细管柱分离的2.4-二硝基甲苯气相色谱分析方法.平均回收率为98.92%～104.69%,标准偏差(δ)为0.0020～0.0097,相对标准偏差(RSD)为0.0098%～2.58%,为工业品2.4-二硝基甲苯的质量控制提供了一个简便、准确、快速的分析方法.     

反相微乳聚合制备聚合物纳米粒子

采用正辛烷做连续相,以Span80和Tween60为复合乳化剂,过硫酸铵-亚硫酸氢钠为氧化还原引发剂体系,通过反相微乳聚合制备丙烯酰胺-丙烯酸钠纳米粒子.研究了乳化剂、单体、引发剂配比及用量和温度等因素对聚合的影响.在反应温度为30 ℃,乳化剂浓度为油相质量的12 %～14 %,单体浓度为水相质量的35 %～40 %,引发剂浓度为单体质量的0.05 %～0.07 %时,得到稳定透明的微乳液.经扫描及透射电镜分析,所得共聚物的粒径为40～60 nm之间,粒子均匀分布的规则球形.     

固相萃取-气相色谱法测定水果、蔬菜中的氯丹

建立一种简单、灵敏的用于测定水果、蔬菜中氯丹残留量的气相色谱检测方法.样品用乙腈提取,经Florisil(弗罗里硅土)SPE小柱净化,由配有ECD检测器的气相色谱(GC-ECD)进行测定.该方法对水果、蔬菜中氯丹检出限为0.0002 mg/kg,工作曲线在0.001～0.08 μg/mL范围内呈良好的线性关系.在该线性范围内,苹果、柿子、西红柿和鲜笋中回收率为82.6％ ～93.1％.     

Determination of Thermodynamic Interactions of the Pvc-Pmma Blend System by Inverse gas Chromatography

In this study, the sorption enthalpy (δH^S1), sorption free energy (δ^G1), sorption entropy (δ^S1), enthalpy, and free energy at infinite dilution (δ^H1 and δ^G1) values were calculated for selected probes such as alcohols, ketones, acetates, cyclic ethers, aromatics, and alkanes in the temperature range 403-433 K for poly(methyl methacrylate) (PMMA), poly(vinyl chloride) (PVC) homopolymers, and the PVC-PMMA blend system. The values of the Flory-Huggins interaction parameters χ1(23) have been calculated in this temperature range and show the importance of specific interactions between the polymers and the solvents. The values of the polymer-polymer interaction parameters χ23(for the temperature range 403–433 K) were found to change from +3.57 to +1.16 for alcohols, from +2.99 to +0.52 for ketones, from + 1.60 to ?0.48 for acetates, from +0.96 to ?1.46 for cyclic ethers, from +2.66 to +0.12 for aromatics, and from +8.73 to +1.06 for alkanes.     

毛细管气相色谱柱的选择和使用过程优化

阐述了选择毛细管柱的四个因素：固定相、柱长、内径、膜厚。介绍了大口径毛细管柱的优点及其对填充柱的取代。提出了使用毛细管柱时应注意的事项。     

反气相色谱法研究结晶聚合物的表面性质

采用反相气相色谱法测定了聚乙二醇 (PEG)不同相态结构组成下的色散成分的表面能 Yds,并探讨了 γds 与温度的关系。研究结果表明 :PEG的表面能较低 (32 .39m J- 2 40℃ ) ,在结晶态和熔融非晶态形式下 ,γds 随温度的升高而降低 ;而在 6 7～ 90℃的结晶熔融温度范围内 ,PEG的γds,随温度的升高呈现先降→后升→再下降的趋势 ,特别是当结晶熔融温度达到 6 3℃时 ,PEG的表面能发生明显的转折。