Quantitative gas chromatographic analysis of lipids: Comparison of gas density balance and flame ionization detector

Accuracy of available detectors for gas chromatography is a subject of continuing research in analytical chemistry. The quantitative deficiency of the flame ionization detector, as well as of other detectors, has been widely recognized, and empirical correction factors have been required. By contrast, the gas density balance, the forgotten ideal detector, should not require calibration. A gas density balance, now available in a commercial chromatograph, and a flame ionization detector were compared for quantitative analyses of lipids. Wt percents of known methyl ester mixtures were determined, as well as mole percents of aldehyde fragments from certain ozonized octadecenoate isomers. Percentages were calculated from area response without correction factors for the gas density balance and with correction factors, based upon the number of ionizable carbon-atoms, for the flame ionization detector. Accuracy, as measured by percentage deviation from either known or theoretical values, was better for gas density balance data than for flame ionization detector data. Aldehyde and aldehydic ester fragments formed by reductive ozonolysis of octadecenoate isomers from partially hydrogenated methyl linolenate also were determined with each detector. Theoretically, ozonolysis of these monoenes should yield an aldehyde and an aldehydic ester in equal mole percents. Experimentally, the average of the ratios of aldehyde to aldehydic ester from each of the Δ5-Δ13 monoenes was 1.29 for the FID data (corrected) and 1.01 for GDB data (uncorrected). This difference in averages approaches significance at the 95% confidence level. For the Δ14 and Δ15 monoenes from which C₄ and C₃ aldehydes are formed, ionizable carbon-atom corrections proved even less adequate. Presented at the AOCS Fall Meeting, Chicago, September 1973. ARS, USDA.     

碳四烃催化裂解制丙烯反应过程中尾气分析

采用2阀2柱HP6890气相色谱运行系统,通过HPPLOT/Al2O3"S"毛细管柱分析有机烃类,并用FID检测,13 X分子筛填充柱分析氢气,用TCD检测,建立了碳四烃催化裂解制丙烯反应尾气分析方法。结果表明:标准样品的分析结果标准偏差不大于4%,实际样品测试结果可保障物料平衡在98%以上。     

常规氢火焰离子化检测器用于便携式气相色谱仪的可行性讨论

讨论并优化建立了满足便携式气相色谱仪要求的常规氢火焰离子化检测器的相关操作参数。基于实验室气相色谱仪使用的常规氢火焰离子化检测器,考察氢气、空气、辅助气和检测器温度对它性能的影响。在优化后的便携式操作参数下,检测器的线性范围可达107,检出限低至1.4×10-12g/s,以115μg/m L n-C12H26为样品,其峰面积重现性优于0.4%(n=8);相对于常规操作参数,FID的气体消耗降低了75%以上,仅需氢气和空气两种气体;无需额外研制微电流放大装置,易于直接集成于第三方便携式气相色谱仪。     

气相色谱检测器进展

热导检测器（ＴＣＤ）、火焰电离检测器（ＦＩＤ）、电子俘获检测器（ＥＣＤ）、氮磷检测器（ＮＰＤ）、光电离检测器（ＰＩＤ）和火焰光度检测器（ＦＰＤ）是气相色谱常用的六种检测器。本文对近年来这些检测器在其结构、体积和电路等方面的改进,以及在灵敏度、选择性和线性范围等方面的提高,作了综述。     

气相色谱法测定饲料香味剂中香味成分的含量

用气相色谱氢火焰离子化检测器，SE－52毛细管柱对四甲苯做内标，分别饲料香味剂中NB－68200香精液组分的含量，分离效果好。     

丙环唑含量分析方法的研究

丙环唑含量分析用气相色谱法，FID检测器，三氯甲烷溶解，以邻苯二甲酸二环己酯为内标物，使用5％SE—30/Cromosorb W AW—DMCS(80—100目)为填充物的不锈钢柱和氢火焰检测器，对丙环唑进行气相色谱分离和测定。该方法定量准确，精密度较好，对丙环唑原药同一样品进行10次重复测定，方法标准偏差0．28，变异系数为0．29％，回收率为98．9％～101．2％。     

粗苯中三苯含量快速定量分析方法的研究

通过气质联用仪(GC-MS)对粗苯中的有机组分进行定性分析,使用配有氢火焰离子检测器(FID)的气相色谱仪对苯、甲苯、二甲苯(三苯)进行定量的研究。     

电石反应法测定气体中微量水分

介绍了一种测定气体中水含量的方法:依据电石吸收气体中水分并生成乙炔气的原理,采用氢火焰离子检测器气相色谱分析乙炔含量,从而计算出气体中水含量。指出该方法具有精确、方便的特点。     

气相色谱法测定蒽醌和磷酸三辛酯的含量

用大口径毛细管柱气相色谱法、氢火焰离子化(FID)检测器测定了双氧水工作液组分中的2-乙基蒽醌(2-EAQ)、四氢2-乙基蒽醌(H4EAQ)和磷酸三辛酯(TOP)的含量。     

毛细管气相色谱法分析双丙酮丙烯酰胺的含量

用毛细管气相色谱，FID检测器，内标法定量，分离测定了双丙酮丙烯酰胺及其主要杂质丙烯酰胺的含量，其相对标准偏差分别为0．19和0．014；变异系数分别为0．19％和4．71％。     

A specific detector for nitrogen and halogen compounds in TLC on coated quartz rods

A new detector has been developed for use with the Iatroscan TH-10 TLC/FID instrument-a “solid-phase” chromatographic system (SPC). This new detection system contains a unique stage of detection that is called a flame thermionic ionization detector or FTID. The FTID evolved from a similar device that recently has been used in gas chromatography. The basic concept of an FTID is that organic sample compounds are first decomposed by combustion in an H₂-air flame. The FTID does not sense any of the ionization produced directly in the flame but, instead, re-ionizes the combustion products by means of a unique thermionic transducer placed in the downstream effluent of the flame. The thermionic transducer ionizes specifically only those combustion products which are acidic or electronegative in chemical activity. In particular, organic samples containing nitrogen (N) or halogen atoms combust to products which are especially well detected with high sensitivity. Hence, the FTID adds to the Iatroscan a state-of-the-art detection stage which produces large signals for nitrogen and halogen compounds and negligible signals for hydrocarbon compounds.     

多维气相色谱法分析复杂组分高温气体

采用多维气相色谱法,用岛津GC 14C气相色谱仪,采用自动阀切换技术,完成丙烯酸(MMA)合成过程中高温气体组分在线分析。采用1根填充柱做为预柱,分离无机气体及有机组分。2根填充柱测定永久气体。1根聚乙二醇毛细柱分离有机酸及醛类组分。用氢火焰离子化检测器及热导检测器分别检测有机类及无机气体。采用外标面积归一化法进行定量计算。整个系统具有分析结果重复性好、准确度高、省时、操作方便等特点。     

气相色谱法测定丙烯酸树脂中的残余单体含量

乙酸丁酯稀释丙烯酸树脂后,用气相色谱法使丙烯酸树脂中的各种残余单体得到较好分离,再采用氢火焰离子化检测器(FID)定量测定。该方法灵敏度高,重现性好,应用于丙烯酸树脂的科研与生产中,取得满意效果。     

Monitoring the products and kinetics of oil shale pyrolysis using simultaneous nitrogen specific and flame ionization detection

The use of the thermionic nitrogen specific detector (TSD) and flame ionization detector (FID), in conjunction with gas sampling and capillary column g.c. is described as a means of following the thermal degradation of involatile substances containing organically bound nitrogen. The response of the TSD to a range of nitrogen compounds is shown to be approximately proportional to nitrogen content in most instances. Application of this method to a study of oil shale pyrolysis reveals that nitrogen compounds are evolved more rapidly than hydrocarbons.     

毛细管柱气相色谱法测定77.5%敌敌畏乳油的含量

采用DB-1701毛细管柱和FID氢火焰离子化检测器,在选定的色谱条件下对77.5%敌敌畏乳油的含量进行气相色谱测定。结果表明:敌敌畏的线性相关系数为0.9998,标准偏差为0.0738,变异系数为0.0958%,平均回收率为99.93%。     

气相色谱法测定十五内脂

十五内酯是一种具有珍贵的麝香香气的大环麝香类化合物 ,是配制名贵香水的重要香料。由于十五内酯在氢焰离子化检测器中有强烈的信号响应 ,故十五内酯的含量可用气相色谱法进行测定。采用十六酸甲酯作为内标物 ,用气相色谱法的内标法进行定量测定十五内酯 ,方法简单、快速 ,测定结果准确、可靠     

光离子化气相色谱法对空气中挥发性有机物的测定研究

采用光离子化气相色谱仪新技术测定了室内空气中典型的挥发性有机化合物。研究了气相色谱仪柱温、载气压力对色谱峰的分辨率、保留时间和强度的影响,确定了光离子化气相色谱法测试苯系物的最佳条件,通过与传统FID气相色谱法的比对,结果表明:光离子化气相色谱法测定苯系物的灵敏度(检出限)比氢火焰离子化气相色谱法优于100倍以上,前者的分辨率也比后者的高。     

3-溴-4-氟苯甲醛的气相色谱分析方法

采用气相色谱法,氢火焰离子化检测器,选用3%OV-17填充柱,正十三烷为内标,气化室和检测器温度为180℃,柱温120℃,对3溴4氟苯甲醛进行定量测定。该方法简单、快速、准确、适用,标准偏差0.26%,变异系数0.27%,平均回收率100.1%。     

大口径三氧化二铝毛细柱在乙烯生产分析中的应用

介绍了以大口径PLOT/AL2O3石英毛细管柱为分析柱,氢火焰离子化检测器在测定高纯度乙烯、丙烯微量烃类杂质及裂解C4、液化气组成气相色谱分析中的应用,解决了以往采用3根填充柱、2台仪器操作的繁琐,大大降低了分析成本,提高了工作效率,操作简便、分析速度快、准确度高、重复性好。     

六甲基二硅氧烷中三甲基硅醇含量的定量分析

利用气相色谱和1H NMR核磁共振分析了六甲基二硅氧烷(MM)中三甲基硅醇的含量。配备氢火焰离子化检测器(FID)的气相色谱进行准确定量。结果表明:采用FID气相色谱测定样品中三甲基硅醇的含量为53.15%;采用TCD气相色谱检测样品中三甲基硅醇的含量为55.27%;核磁共振检测出三甲基硅醇的质量分数为51.59%。