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建立了催化汽油馏分中各种含氮化合物类型分布的气相色谱-氮化学发光检测分析方法,考察了各种色谱条件对含氮化合物分离的影响。采用化学预处理的方法浓缩了催化汽油中的含氮化合物,并结合气相色谱-质谱检测以及部分含氮化合物标准样品,对某催化汽油中的20多个含氮化合物进行了定性(或归类)。催化汽油中几种主要含氮化合物(苯胺、2-甲基苯胺、二甲基苯胺)含量测定值的相对标准偏差(RSD)均不大于2.5%。当信噪比(S/N)为3时,苯胺氮的检出限为1.0 mg/L。该方法可用于不同来源和不同加工工艺的汽油馏分中各种含氮化合物类型分布的研究。 相似文献
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焦化汽油中硫化物类型分布的气相色谱-硫化学发光检测方法 总被引:2,自引:0,他引:2
建立了焦化汽油中硫化物类型分布的气相色谱-硫化学发光检测分析方法。考察了色谱条件对焦化汽油中各种硫化物分离的影响,定性了某焦化汽油中的74个硫化物。以硫化氢、乙硫醇、正丙硫醇、噻吩、2-甲基噻吩、2-乙基噻吩、2-丙基噻吩、碳四噻吩(tR=40.28 min)、苯并噻吩、甲基苯并噻吩(tR=58.13 min)的保留时间为尺度,计算了焦化汽油中各种硫化物的保留指数,并可推广到其他类型的汽油馏分中各种硫化物保留指数的计算,为仅能提供硫化物信息的仪器提供了可靠的定性依据。焦化汽油中几种主要硫化物(异丙硫醇、正丙硫醇、正丁硫醇、2-甲基噻吩、3-甲基噻吩、2,4-二甲基噻吩、2,3,4-三甲基噻吩)含量测定值的相对标准偏差均小于5%。当信噪比为3时,测得硫的检测限为0.05 mg/L。研究发现:同其他类型的汽油相比,焦化汽油的硫含量较高且所含硫醇比例明显偏高,2-甲基噻吩和3-甲基噻吩的含量差别较大。该法可为加氢脱硫催化剂和工艺的研究提供数据。 相似文献
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催化裂化汽油中硫化物类型分布的气相色谱-硫化学发光检测的方法研究 总被引:18,自引:2,他引:16
采用气相色谱-硫化学发光检测器(GC-SCD),建立了催化裂化汽油(FCC汽油)中各种硫化物类型分布的分析方法。考察了色谱条件对催化裂化汽油中各种硫化物分离的影响,定性了某催化裂化汽油中的58个硫化物。采用该方法,硫化物中的硫在其质量浓度为0.5~800.0 mg/L时,其峰面积与质量浓度呈较好的线性关系,相关系数达0.999,其响应与硫化物的类型无关。FCC汽油中几种主要硫化物(噻吩、正丁硫醇、2-甲基噻吩、3-甲基噻吩、2,4-二甲基噻吩)的浓度测定值的相对标准偏差(RSD)均小于5.0%。当信噪 相似文献
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色谱与色谱/质谱法相结合分析热裂解汽油C9馏分 总被引:3,自引:0,他引:3
采用毛细管气相色谱-氢火焰离子化检测器(CGC-FID)和气相色谱-质谱法(GC/MS)分析了热裂解汽油C9 馏分的组成。实验使用PONA毛细管气相色谱柱(100 m×0.25 mm i.d.×0.5 μm),根据烃类化合物在PONA柱上的保留规律,以正构烷烃标样保留值作为碳数分布依据,定量分析了裂解汽油C9 馏分中烃类化合物的碳数分布和单体烃含量;用GC/MS联用技术和CGC保留值定性法相结合对裂解汽油C9 馏分中相对含量大于0.2%的39种化合物进行了定性。 相似文献
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汽油色谱模拟蒸馏ASTMD-2887的改进以及我国标准蒸馏方法数据的关联 总被引:1,自引:0,他引:1
汽油馏程测定为诸如重整、催化裂化等石油加工工艺提供了指导数据。美国ASTMD-2887气相色谱测定石油产品馏分沸点范围分布标准方法,为馏程测定建立了快速,精确的标准方法。1973年提出以来,在世界上逐渐得到推广。目前我国广泛用于测定 相似文献
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《理化检验(化学分册)》2010,(8)
采用气相色谱-火焰光度检测器对炼油厂碳四烃中硫化物的形态进行了分析,以硫化物保留时间定性。建立了6种硫化物峰面积与其浓度的三次方拟合曲线用于定量。该方法用于测定6种硫化物,测得回收率在90.0%~112.0%之间,相对标准偏差(n=7)均小于4.5%。 相似文献
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用色谱-脉冲火焰光度(GC-PFPD)法分析汽油中的总硫 总被引:6,自引:0,他引:6
实验了脉冲火焰光度检测器(PFPI))对汽油中微量有机硫化物的响应性和重现性,用色谱-脉冲火焰光度检测器法(GC-PFPI))和外标法定量测定了齐鲁和胜华FCC汽油全馏分及其窄馏分中的硫含量,并与微库仑法进行了对比,分析结果表明:(1)脉冲火焰光度(PFPD)检测器能够有效排除烃信号的干扰,只输出硫信号,定性简单,重现性好,是分析汽油中总硫含量的理想检测器。(2)采用色谱-脉冲火焰光度(GC-PFPD)法分析汽油中的总硫,操作简单,分析时间短,分析结果准确可靠,标准偏差小于1%。 相似文献
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This paper reports an analytical method for separating, identifying, and quantifying sulfur-containing compounds in crude oil fraction (IBP-360 degrees C) samples based on comprehensive two-dimensional gas chromatography coupled with a sulfur chemiluminescence detector. Various sulfur-containing compounds and their groups were analyzed with one direct injection. 3620 peaks were detected including 1722 thiols/thioethers/ disulfides/1-ring thiophenes, 953 benzothiophenes, 704 dibenzothiophenes, and 241 benzonaphthothiophenes. The target sulfur compounds and their groups were identified based on the group separation feature and structured retention of comprehensive two-dimensional gas chromatography as well as standard substances. The quantitative analysis of major sulfur-containing compounds and total sulfur was based on the linear response of the sulfur chemiluminescence detector using the internal standard method. The sulfur contents of target sulfur compounds and their groups in 4 crude oil fractions were also determined. The recoveries for standard sulfur-containing compounds were in the range of 90-102%. The quantitative result of total sulfur in the Oman crude oil fraction sample was compared with those from ASTM D 4294 standard method (total S by X-ray fluorescence spectrometry), the relative deviation (RD%) was 4.2% and the precision of the method satisfactory. 相似文献
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Thomas G. Albro Peter A. Dreifuss Richard F. Wormsbecher 《Journal of separation science》1993,16(1):13-17
The identification and quantification of sulfur-containing compounds in gasoline has become an area of interest because of impending legislation regulating total sulfur levels in these fuels. To study the effects of catalyst type and catalytic conditions on gasoline sulfur distribution, a method has been developed employing both the compound-independent and element-specific response of the atomic emission detector (AED). Calibration and quantification can be accomplished even where standards are not available, owing to the nature of the AED response. Compounds were separated on a thick film polydimethylsiloxane column. An external calibration curve was applied to the area responses of individual sulfur components in the sulfur chromatogram, and the concentrations of each were calculated. Summation of these sulfur concentrations over the gasoline range yields the total sulfur content of the gasoline. The method is applicable to the determination of these compounds in raw crude oils, finished gasolines, fluid cracking catalyst (FCC) unit gasolines, and fluid catalytic cracking “model” compound studies. A prefractionating column was employed to remove heavy (>C13) materials; prefractionation is not, however, necessary for distilled or commercial gasoline samples. Detection limits, linearity, detector stability, and accuracy are discussed. 相似文献
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I. P. Afanas’ev T. A. Gorshkova S. A. Arystanbekova M. S. Lapina A. B. Volynskii 《Journal of Analytical Chemistry》2017,72(10):1095-1101
A procedure is developed for the determination of more than 60 individual sulfur-containing compounds (SCC) in liquid hydrocarbon raw materials and in liquid fuels using gas chromatography on a 25-m WCOT column, inner diameter 0.32 mm, with a nonpolar dimethylpolysiloxane stationary phase (layer thickness 5 μm) and chemiluminescence detection. SCC were identified by individual standard substances and published data. Quantitative determination was carried out by the internal standard method. The results of determination of individual SCC in petrol and stable gas condensate are presented. The most high-boiling SCC found in significant amounts (more than 0.005 wt % of sulfur) were C2-benzothiophenes (in petrol) and C4-dibenzothiophenes (in gas condensate). 相似文献
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催化柴油中硫化物的气相-原子发射光谱分析方法及应用 总被引:17,自引:2,他引:17
建立了催化柴油馏分中各种硫化物类型分布的气相 原子发射光谱分析方法,考察了条件对各种硫化物分离的影响,定性(或归类)了催化柴油中的130多个硫化物,计算了程序升温条件下各种硫化物的保留指数,为不同实验室的定性比较和方法的转让提供了依据。硫化物中的硫在2mg/L~1000mg/L时其质量浓度与峰面积呈较好的线性关系,相关系数达0 997。几种硫化物(苯并噻吩、4 甲基苯并噻吩、二苯并噻吩、4 甲基二苯并噻吩、4,6 二甲基二苯并噻吩)6次测定所得峰面积的相对标准偏差均小于5 0%。当信噪比(S/N)为3时,测得苯并噻吩硫的检出限为0 1mg/L。 相似文献
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建立了一种采用填充柱切割-反吹二维气相色谱分析汽油中酯类化合物(包括乙酸乙酯、乙酸仲丁酯、碳酸二甲酯)的方法。利用非极性填充预柱将汽油中沸点低于正辛烷的轻组分保留进入分析柱,重组分反吹放空,轻组分和酯类化合物经一个装填有强极性固定相的色谱柱分离分析。采用外标法定量,3种酯类化合物在50~50000 mg/L范围内线性关系良好,相关系数(r2)分别为0.99999、1.00000和0.99995,标准样品6次重复性测定的相对标准偏差(RSD)均小于1.0%,回收率在98.7%~107.9%之间,方法检出限(S/N=3)为5 mg/L。该方法不需要进行样品前处理,具有操作简单,准确高效的特点,是汽油中酯类化合物测定的理想分析方法。 相似文献
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Rapid determination of total sulfur in fuels using gas chromatography with atomic emission detection 总被引:1,自引:0,他引:1
Link DD Baltrus JP Rothenberger KS Zandhuis P Minus D Striebich RC 《Journal of chromatographic science》2002,40(9):500-504
The purpose of this study is to determine whether gas chromatography (GC)-atomic emission detection (AED) can be used in a low-resolution mode for rapid, accurate determinations of total sulfur in fuels at trace levels to complement other popular methods of total sulfur analysis. A method for the rapid determination of total sulfur in fuels (called "fast GC-AED") is developed. The method is tested on gasoline, jet fuel, kerosene, and diesel fuel with sulfur concentrations ranging from 125 mg/L down to 2.5 mg/L. Fast GC-AED shows better performance than traditional GC-AED for total sulfur determinations, especially for complex mixtures containing many different sulfur-containing compounds at trace levels. This method also shows that GC-AED can be used for both rapid determinations of total sulfur and traditional determinations of speciated sulfur without requiring equipment changes. Fast GC-AED is competitive with other popular methods for sulfur analysis. The 5-min program that is developed for fast GC-AED is comparable with the time scale of other methods, such as wavelength dispersive X-ray fluorescence and UV-fluorescence (2 to 5 min). Fast GC-AED also compares favorably with UV-fluorescence for trace sulfur determinations, demonstrating accuracy down to 2.5-mg/L sulfur. 相似文献