煤间接液化油的毛细管色谱分析

毛细管气相色谱,由于在分辩本领、分析速度及样品量等方面优于传统的填充柱色谱,近年来发展很快。本工作用毛细管色谱法对煤间接液化油的C_3～C_(24)单体烃,进行了分离检定,为煤转化油的工作提供了快速而又可靠的检测方法。实验部分一、色谱条件:仪器:GC—9A气相色谱仪,配有C—R2AX数据处理机;氢火焰离子化检测器;OV—101玻璃毛细管柱,尺     

气相色谱模拟蒸馏在加氢尾油馏程分析中的应用

研究了气相色谱模拟蒸馏测定加氢尾油沸程分布的方法,通过使用正构烷烃校正样进行沸点一保留时间校正分析,用标准参考样进行准确性检查。从而测得样品的百分收率一沸点的馏程数据。同时,考察并探讨了沸点一保留时间校正、基线补偿、色谱柱性能、二硫化碳溶荆及样品洗提时间等主要因素对模拟蒸馏结果的影响。     

沙棘果油不皂化物的色质谱分析

应用柱色谱预分离、色谱质谱联用技术,以NBS标准质谱对照系统为主要定性手段,对中国山西省典型的沙棘果油中的不皂化物进行了系统研究,从中检测出105种化合物、多数成份未有文献报道。     

岗松(精)油质量标准研究

对岗松(精)油质量标准进行研究。采用气相色谱、薄层色谱技术和理化指标对岗松(精)油进行分析。确定其各项指标,并用气相色谱面积归一化法测定特征性组分与代表性组分的相对含量。研究制订岗松(精)油质量标准的技术要求及试验方法,为岗松(精)油的质量控制提供科学基础和方法参考。     

生物油组分分离与化学品提取的研究进展

生物质在高温无氧条件下热解可以生成富含高附加值化学品和燃油成分的生物油。有效分离技术和高效提取手段的发展是生物油质量提升的关键。基于此,本文在介绍生物油性质与生物质快速热解工艺的同时,对目前国内外的生物油分离技术如蒸馏、液-液萃取、柱色谱、超临界萃取、膜分离等进行了较为详细的分析和评述。常规蒸馏和溶剂萃取等技术,工艺成熟、操作简单,但存在生物油的热敏性差、萃取剂回收难度大和污染严重等问题;分子蒸馏技术分离过程安全环保,但工艺复杂,设备成本高;超临界萃取和膜分离等技术安全环保,技术成熟,具有较大的潜力。文章还综述了目前生物油中具有高附加值的组分和单一化学品的分离提取研究进展,为生物油的有效分离和高效利用提供了理论参考,也为未来生物油分离技术的发展提供了研发方向。     

重整生成油C_8馏分中芳烯烃的分析

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(CGC/MS)分析了重整生成油C8馏分中的芳烯烃。实验使用HP-FFAP毛细管色谱柱(50m×0.32mm×0.50μm)和ATTM-WAX毛细管色谱柱(50m×0.32mm×0.30μm),根据烃类化合物在这两种色谱柱上的保留规律,用CGC/MS联用技术和UOP方法744-06以及标准样品相结合的方法对重整生成油C8馏分中的芳烯烃进行了定性定量分析,从12O多种组分中鉴定出18种烯烃,对其中的15种烯烃组分进行了定量分析,对其它3种烯烃组分进行了半定量分析。本法操作简单、重复性好,适用于重整生成油C8馏分和二甲苯塔塔顶液的烯烃检测,也可用于芳烃厂同类产品质量控制分析。     

自动重质油组分分离装置的研制

介绍一种用于测定原油及渣油组分的自动重质油组分分离的装置,该自动重质油组分分离装置按照SH/T0509-2010标准,采用洗脱色谱柱法测量原油及渣油中各组分的含量。应用视觉识别技术和计算机控制,实现原油及渣油组分分离过程中溶剂自动计量、溶剂自动注入色谱层析柱,分离组分自动收集,从而实现原油及渣油组分分离自动操作,提高工作效率和数据检测的准确性,避免有机溶剂对操作者产生危害及环境污染。     

新疆混合原油减三线馏分生产橡胶油工艺研究

利用糠醛、N-甲基吡咯烷酮(NMP)、二甲基亚砜(DMSO)等极性溶剂,正戊烷、正庚烷、石油醚等非极性溶剂对新疆混合原油减三线馏分进行萃取、反萃取,结合Al2O3色谱柱吸附、洗柱等方法,从副产物中生产出主要质量指标合格的高芳烃橡胶油和环保型橡胶油。高芳烃橡胶油芳烃质量分数达80%以上,环保型橡胶油多环芳烃(PCA)质量分数在3%以下。剩余原料的杂质含量降低、碳型分布合理、黏度指数提高,比较适合做润滑油原料。做为催化裂化原料时轻质油收率提高2.9%、焦炭产率下降1.3%。     

煤液化油中酚类化合物分布特征研究

采用气相色谱/质谱联用研究分析了胜利褐煤在0.1t/d直接液化连续实验装置上所得煤液化油中酚类化合物的分布特征.实验通过碱液洗涤法富集煤液化油中混合酚组分,并对该组分进行衍生化处理,以提高色谱柱对混合物的分离性能.以混合衍生物为主要分析对象,共定性出煤液化油中134种个体酚,分属于苯酚、茚满酚、萘满酚和萘酚等四种类型,且绝大多数酚类化合物都带有烷基侧链.苯酚类化合物数量最多,在混合酚组分中含量最大,其次为茚满酚和萘满酚.萘酚类化合物的数量最少,相对含量最小.     

生物油的性质及其分离研究进展

综述了蒸馏、萃取、层析、膜分离、超临界萃取等技术在生物油分离方面的研究进展情况。介绍了常减压蒸馏主要用于生物油的粗分,且受到生物油热敏性的限制;分子蒸馏在生物油的分离方面具有一定的优势。溶剂萃取存在着萃取剂与被萃组分分离困难的缺点,且萃取选择性较差;选择或设计具有特定结构的化合物与生物油中的某种或某些组分作用,进而将其萃取分离是未来的一个研究方向;色谱分离可以高效地将生物油的主要成分分离出来,但吸附量小,适合于生物油成分的定量分析和高附加值化合物的提取与纯化。超临界CO2萃取可有效地克服生物油的热敏性,无需反萃,具有潜在的开发优势。开展生物油分离的基础性研究和多种技术的集成化是未来的重要研究方向。     

毛细管气相色谱法测定洗油中萘含量

洗油萘含量是洗油的主要质量指标,洗油萘含量的测定方法国际标准规定有2种:一是采用蒸馏结晶点法,该法准确度和精密度都较差;二是采用GB/T 24208-2009规定的色谱法,该法虽然采用先进的色谱技术代替结晶点法,但在色谱柱的选择和定量方法的选择方面仍有改进余地。采用毛细管色谱法分析测定洗油中的萘含量。该法分析时间短,操作简单,准确度和精密度都较高,完全可取代以上2种方法。整个试样分析时间只有15min,可直接用于产品质量分析与控制,为现场分析和操作调节提供了便捷。     

Modification of AOCS chromatographic procedure for neutral oil determination

The AOCS chromatographic procedure for neutral oil determination, Ca 9f-57, has been modified through use of a newly designed flask. This modified procedure increases the efficiency and standardization of neutral oil determination by: permitting automatic transfer of weighed crude oil samples onto alumina columns; converting column operation to a semiautomatic level thus reducing cost of operation; and allowing the chromatographic procedure to be performed in laboratories which are not air-conditioned. As a result of collaborative studies the AOCS Fats and Oils Subcommittee for neutral oil investigation has recommended that this procedure be adopted officially by the Uniform Methods Committee.     

毛细管气相色谱法模拟三混油蒸馏

利用毛细管气相色谱测定三混油各组分含量,根据色谱结果和蒸馏结果的线性关系得出三混油的模拟蒸馏数据,测定结果具有良好的准确度和精密度,整个试样分析不超过20min,可代替蒸馏法用于测定三混油的初馏点、干点和萘含量。     

稻壳热解油的特性

利用自行搭建的固定床热反应器对稻壳进行热解实验制备热解油, 采用两种不同极性的石英毛细柱对收油后的二氯甲烷溶液进行GC-MS检测。实验结果表明:热解终温对热解油品的组分种类几乎无影响, 但热解油产率随热解终温增大呈先升高后降低趋势;热解油二氯甲烷溶液的水相部分化合物种类相对较少, 主要物质为甲酸、乙酸和1-羟基-2-丙酮, 油相部分有机物种类极为复杂, 主要物质为糠醛、糠醇以及酚类和酮类物质;可凝结的热解有机气体主要在500～600℃发生二次裂解;对稻壳600℃热解油油相检测时发现:在RTX-5MS柱检测条件下, 组分中前5种化合物是糠醛、2-丁酮、乙酸、苯酚和2-甲氧基苯酚, 而在RTX-WAX 柱检测条件下, 前5种化合物是苯酚、2-甲氧基苯酚、4-乙基苯酚、乙酸和3-甲基苯酚。     

A simplified method for HPLC‐MS analysis of sterols in vegetable oil

We have developed a liquid‐chromatographic method using atmospheric pressure chemical ionization (APCI)‐mass spectrometry (MS) detection in positive mode. This method was used to separate and identify 15 sterols and 2 dihydroxy triterpenes in saponified oils, enabling the analysis of these compounds directly from saponified samples without recourse to thin‐layer chromatography; this fact thus significantly simplifies the process. The analyses were made using a Waters Atlantis 5 µm dC₁₈ 150×2.1 mm column with a gradient of acetonitrile/water (0.01% acetic acid) at a flow rate of 0.5 mL/min and a column temperature of 30 °C. The quantification of several of these compounds in soybean oil, palm oil, seed oil, sunflower oil, olive‐pomace oil and virgin olive oil was carried out using their commercial standards, and the results were compared satisfactorily with the official method.     

Isolation and identification of the causative factors responsible for color fixation in rice bran oil

To understand the chemical nature of the dark coloring constituents responsible for color fixation in rice bran oil, crude and dewaxed rice bran oils of 6.8% free fatty acids were fractionated on a silica gel column to get a dark-colored material (0.57% of the oil). Thin-layer chromatographic analysis of the material showed a spot corresponding to monoglycerides, but there were no spots corresponding to other glycerides. It contained traces of phosphorus (<0.1 ppm, which is equivalent to 2.5 ppm phospholipids) and iron (1.3 ppm) that could not be attributed to phospholipids or to any iron-complex. Upon saponification it yielded 12% nonsaponifiable matter. Gas-liquid chromatographic analysis of the saponifiable matter (after acidification and methylation of fatty acids) showed the presence of palamitic, oleic and linoleic acids. Further, on the basis of comparison with spectroscopic data of synthetic monoglyceride, the constituent was characterized to be a mixture of monoglycerides with side chains of oxidized unsaturated fatty acids.     

高效液相色谱法测定食用植物油中的游离棉酚

研究采用高效液相色谱法测定食用植物油中游离棉酚的方法,最佳色谱条件:色谱柱C18柱,流动相为甲醇-磷酸溶液(1%)=84+16,波长240 nm,流速为1.0 mL/min,柱温30℃。曲线方程y=3.1033×10-5x,相关系数r=0.999871,线性关系良好。检出限为2.5 mg/kg,回收率为98.0%～100.2%。该法简便,快速,准确性高,重现性好。     

Analysis of vegetable oil volatiles by multiple headspace extraction

Quantitative determination of the volatiles produced from oxidized vegetable oils is an important indicator of oil quality. Five vegetable oils, low-erucic acid rapeseed, corn, soybean, sunflower and high oleic sunflower, were stored at 60°C for four and eight days to yield oils with several levels of oxidation. Peroxide values of the fresh oils ranged from 0.6 to 1.8 while those of the oxidized oils were from 1.6 to 42. Volatile analysis by the multiple headspace extraction (MHE) technique, which includes a pressure and time controlled injection onto the gas chromatography (GC) column (a chemically bonded capillary column), was compared with that obtained by static headspace gas chromatography (SHS-GC). Several volatile compounds indicative of the oxidation of polyunsaturated fatty acids from the vegetable oils were identified and measured by MHE; pure compounds of twelve major volatiles also were measured by MHE, and peak area was determined. Multiple extractions of the oil headspace provided a more reproducible measure of volatile compounds than was obtained by SHS-GC. Concentration of all volatiles increased with increased oxidation as measured by peroxide value of the oil. Presented at the Annual American Oil Chemists' Society Meeting, May 8–12, 1988, Phoenix, AZ.     

油标对红外光度法测定水中油的影响

油标准物质的选择是红外分光光度法测定水中油的重要环节,选择了两种不同的油标,采用红外分光光度法对水中油进行了分析,结果表明,油标不同,测量结果不同。理想的油标是从待测水样中提取,这样的油标的组成才能与被测水样中油的组分相同,红外光谱图基本相同,测定结果才准确可靠。     

气相色谱法模拟蒸馏实验测定三混油、蒽油组分及其初点、干点技术的开发与应用

近年来随着色谱技术的发展,利用色谱仪器模拟蒸馏试验已在化工企业得到了应用,我公司已开始利用气相色谱模拟蒸馏试验测定三混油、蒽油馏分的初点、干点、及230℃、270℃、300℃、360℃前的馏出量,通过大量的试验对比,利用色谱数据和蒸馏数据的相关性,求出的关于色谱值和蒸馏值的线性公式,已成功地应用到生产工艺的调节。