沸石分子筛对大港减压渣油超临界萃取物的加氢催化

在大港减压渣油超临界萃取物(DVR SFEF)的GC/MS分析检测中,除了第1级超临界萃取分F1以外,其他级分检出的物种和数量均较少。通过沸石分子筛HM对DVR SFEF1~17催化加氢,探索催化产物可检测成分的变化规律。结果表明,用GC/MS检出的主要成分为C11~C34的直链烷烃、C11~C30的支链烷烃、环烷烃(包含饱和环烷烃)、少量的藿烷、降羽扇烷、芳烃及含氧有机化合物等,含量从DVR SFEF1~SFEF16逐步增加。通过大港减压渣油超临界萃取物的加氢催化实验发现,超临界萃取是一种对重质油高效转化利用十分有效的分离方法。     

大港减压渣油超临界萃取物的柱层析分离及GC/MS分析

在大港减压渣油超临界萃取物(DVR SFEF)的GC/MS分析检测中,除了大港减渣1级萃取分F1以外,在其他级分中分析检测出的物种和数量均较少,特别是DVR SFEF 10~SFEF 17的检测结果很不理想。故通过层析柱对DVR SFEF按照标准分析方法进行分离,可以得到饱和分、芳香分、胶质和沥青质在DVR SFEF中的分布规律,以及DVR SFEF所含饱和分、芳香分、胶质和沥青质中链烃、环烷烃和芳烃的含量的变化规律;还检测出了具有高附加值的稀有物质。     

血中非那西丁的GC/MS检测

建立了非那西丁的气相色谱/质谱/质谱(GC/MS/MS)联用检测血中去痛片的主要代谢物非那西丁的新方法。采用液液提取法,用乙醚提取血中非那西丁,提取物水浴浓缩后进行GC/MS和GC/MS/MS分析,检测总离子流色谱(TIC)和一级质谱,并以非那西丁一级质谱基峰为母离子的测定其二级质谱,体内药物用GC/MS全扫描定性分析即用二级质谱结合其总离子流色谱峰的保留时间定性;选择离子扫描定量分析,采用内标曲线法,根据非那西丁和内标SKF525A二级质谱的TIC峰面积比进行定量分析。     

血中非那西丁的GC/MS检测

建立了非那西丁的气相色谱/质谱/质谱(GC/MS/MS)联用检测血中去痛片的主要代谢物非那西丁的新方法。采用液液提取法,用乙醚提取血中非那西丁,提取物水浴浓缩后进行GC/MS和GC/MS/MS分析,检测总离子流色谱(TIC)和一级质谱,并以非那西丁一级质谱基峰为母离子的测定其二级质谱,体内药物用GC/MS全扫描定性分析即用二级质谱结合其总离子流色谱峰的保留时间定性;选择离子扫描定量分析,采用内标曲线法,根据非那西丁和内标SKF525A二级质谱的TIC峰面积比进行定量分析。     

固相萃取GC-MS测定水中16种农药的研究

文章将C18和Sep-pak Porapak Rox固相萃取小柱活化后联用富集水中16种农药,用乙酸乙酯洗脱,浓缩这16种农药,确定各农药的保留时间和定量离子,用气相色谱/质谱联用仪(GC/MS)选择离子模式进行分析测定,分析了各农药的工作曲线线性、回收率和精密度。结果表明,各农药的工作曲线线性、回收率和精密度较好,线性相关系数在0.994～0.999之间,回收率在68.9%～109.2%之间,相对标准偏差小于7.6%。     

分析测试

20011258贸易的工具Zawodny C.P.…;Adhensives Age,1999,42,(6),p .37一42(英)研究人员研究了把热解气相色谱/质谱仪(GC/MS)用于分析粘合剂的效果。热解单元由带一台HP689oGC/MSD单元的CDS 2500 Autosampler接口组成。气相色谱试验在40℃分析样品2分钟,然后以6‘c/分升温直至295℃。Hpehemstation收集所有的质谱数据。结果指出,在分析天然和合成粘合剂时,热解GC/MS消除了制备时间和补充了其它分析技术包括Fourier变换红外法。热解GC/MS在研究粘合剂的派生成份和组成的均匀性方面得到应用。(张桂水)气相色谱法质谱法粘合剂分析 …     

气相色谱/质谱联用分析橡胶制品喷霜析出物

用气相色谱/质谱联用(GC/MS)对汽车门窗密封条、橡胶手套、白胶板、轮胎等喷霜析出物进行分析。从GC/MS总离子流色谱分析得出,橡胶制品喷霜析出物主要为防焦剂、促进剂、防老剂、防护蜡和硬脂酸等。GC/MS分离效果好,测试效率高,可以较准确地分析橡胶制品的喷霜析出物。     

LC MS/MS和GC测定水中乐果的方法比较

目的采用LC MS/MS和GC对比分析了水中乐果含量,并从方法学角度比较两种方法的优劣。方法:水样按照国标GB/T 5750.9-2006萃取浓缩后使用GC分析;同时,采用直接进样方式,用LC MS/MS分析水质中的乐果的含量。结果:GC和LC MS/MS对水中乐果的分析都可以满足国家卫生标准要求,回收率在88.2%~94.7%,精密度在7%以内,两者的回收率与精密度无明显差异。但LC MS/MS的分析时间远低于GC的分析时间,且无需使用有机试剂进行繁琐的前处理,可作为现有国家标准的补充方法。     

呼伦贝尔褐煤溶剂萃取及萃余煤的双氧水氧化产物分析

以CS2、乙醇和丙酮作为溶剂,对呼伦贝尔褐煤进行连续萃取,并利用气相色谱/质谱联用(GC/MS)技术对萃取物进行分析。结果表明:CS2萃取物主要由长链脂肪烃和芳烃组成,而这些脂肪烃存在于3种溶剂萃取物中。在40℃条件下,用H2O2溶液采用恒温水浴和超声两种方式氧化萃余煤,超声条件下氧化剧烈,并用FTIR分析了原煤、萃余煤、氧化煤的化学结构的变化。氧化后的水溶物用乙酸乙酯萃取后,用GC/MS检测萃取物,恒温水浴氧化可以检测到30种化合物,而超声氧化只检测到14种,且都是以酯类为主。     

煤直接液化循环溶剂中饱和烃的分子组成及分布特点

采用全二维气相色谱-飞行时间质谱/氢火焰离子化检测器(GC×GC-TOF MS/FID)从分子水平上对煤直接液化循环溶剂中的饱和烃进行了表征。TOF MS检测器在信噪比(S/N)为200的条件下共检测到599个单体峰,FID检测器在信噪比(S/N)为1000的条件下共检测到458个单体峰。TOF MS的定性结果表明:在GC×GC-TOF MS/FID设定的分析条件下,链烷烃检测到57个单体峰,含有从正戊烷到正三十一烷的完整分布,可达到单体识别;环烷烃共检测到一环烷烃~五环烷烃五种族类,依次检测到104,229,180,28,1个单体峰,可进行每一族类环烷烃中不同碳数的识别。对FID检测器采集的数据进行面积归一化定量,结果表明:链烷烃中主要为正构烷烃,占全部链烷烃的91.86%,一环烷烃中正构烷基环己烷单体的含量比异构烷基环己烷单体的含量大,15种正构烷基环己烷的含量占全部一环烷烃的41.77%;一环烷烃、二环烷烃、三环烷烃、四环烷烃和五环烷烃在煤直接液化循环溶剂中的含量依次为2.11%,14.90%,17.81%,5.30%和0.15%;芳烃组分的总含量为53.64%;含少量含氧杂原子化合物,其含量为0.26%;碳数分布检测结果显示,一环烷烃、二环烷烃、三环烷烃和四环烷烃含量最高的化合物碳数依次为C 13,C 12,C 14和C 16。     

Solubility of Dagang vacuum residue and molecular composition of the soluble fractions in different solvents

Dagang vacuum residue (DVR) was ultrasonically extracted with fifteen organic solvents, respectively, and the soluble fractions (SFs) were analyzed with GC/MS. The results show that DVR tends to dissolve in non-polar solvent and that most of GC/MS-detectable components in the SFs are saturated hydrocarbons.     

An experimental and modeling study of vacuum residue upgrading in supercritical water

Arabian Heavy crude oil was fractionated into distillate and vacuum residue fractions. The vacuum residue fraction was treated with supercritical water (SCW) at 450°C in a batch reactor for 15–90 min. The main products were gas, coke, and upgraded vacuum residue; the upgraded residue consisted of gasoline, diesel, and vacuum gas oil range components. The molecular composition of gas and upgraded vacuum residue was analyzed using gas chromatography (GC, GC × GC). SCW treatment converted higher carbon number aliphatics (≥C₂₁) and long‐chain (≥C₅) alkyl aromatic compounds into C₁?C₂₀ aliphatics, C₁?C₁₀ alkylaromatics, and multiringed species. The concentrations of gasoline and diesel range compounds were greater in the upgraded product, compared to the feed. A first‐order, five lump reaction network was developed to fit the yields of gas, coke, diesel, and gasoline range components obtained from SCW upgrading of vacuum residue. Distillation of crude oil followed by SCW treatment of the heavy fraction approximately doubled the yield of chemicals, gasoline, and diesel, while forming significantly less coke than conventional upgrading methods. © 2018 American Institute of Chemical Engineers AIChE J, 64: 1732–1743, 2018     

Comparison of aroma,aroma-active,and phenolic compounds of crude and refined hazelnut oils

Hazelnut (Corylus avellana L.) is an important shelled nut with its pleasant aroma. The refining process causes significant changes in the quality attributes of hazelnut oil. The aim of this study was to assess the aroma, aroma-active, and phenolic compounds of the crude and refined hazelnut oils by using gas chromatography–mass spectrometry (GC–MS), GC–MS-olfactometry (GC–MS-O), and liquid chromatography–mass spectrometry (LC–MS/MS). The antioxidant capacities were also determined by DPPH and ABTS methods. Results showed that terpenes and aldehydes constituted a significant portion of the aroma profile. Refining process dramatically reduced the numbers (from 63 to 25) and amounts of aroma compounds (from 36,769 to 4461 μg/kg). Similarly, the numbers of aroma-active compounds were reduced from 22 to 8 by the refining process. Their flavor dilution factors ranged from 2 to 1024 for crude oil and from 2 to 32 in the refined oil. As of the phenolics, five and two compounds were quantified in the crude and refined oil samples, respectively. In sum, the refining process had a considerable adverse effect on the aroma, aroma-active, and phenolic constituents of the hazelnut oil; hence, the refining process has to be planned with minimal negative effect on its organoleptic properties.     

Constituents of essential oil from the dried fruits and stems of Akebia quinata (THUNB.) DECNE

The compositions of the essential oil from AKEBIAE FRUCTUS and AKEBIAE CAULIS, the dried fruits and stems of Akebia quinata (THUNB.) DECNE. (Lardizabalaceae), have been investigated by GC and GC/MS. As a result, the fruits oil was revealed the presence of 86 components, representing 98.4% of the total oil. The major compounds of the fruits oil were limonene, eugenol, octanal and p-cymene. The monoterpenoids and saturated short-chain aldehyde (C6 approximately C10) were main volatile fractions of the oil. Ninety components accounting for 90.5% of constituents of stems oil were identified, and the main compounds of the oil were hexanoic acid, palmitic acid, (2E, 4E)-decadienal and hexanol. The oil had high content of saturated fatty acids (C6 approximately C16), and unsaturated short-chain aldehyde (C6 approximately C10).     

Dual Bioactivities of Essential Oil Extracted from the Leaves of Artemisia argyi as an Antimelanogenic versus Antioxidant Agent and Chemical Composition Analysis by GC/MS

The study was aimed at investigating the antimelanogenic and antioxidant properties of essential oil when extracted from the leaves of Artemisia argyi, then analyzing the chemical composition of the essential oil. The inhibitory effect of the essential oil on melanogenesis was evaluated by a mushroom tyrosinase activity assay and B16F10 melanoma cell model. The antioxidant capacity of the essential oil was assayed by spectrophotometric analysis, and the volatile chemical composition of the essential oil was analyzed with gas chromatography-mass spectrometry (GC/MS). The results revealed that the essential oil significantly inhibits mushroom tyrosinase activity (IC₅₀ = 19.16 mg/mL), down-regulates B16F10 intracellular tyrosinase activity and decreases the amount of melanin content in a dose-dependent pattern. Furthermore, the essential oil significantly scavenged 2,2-diphenyl-1-picryl-hydrazyl (DPPH) and 2,2′-azino-bis (3-ethylbenzthiazoline- 6-sulphonic acid) ABTS radicals, showed an apparent reduction power as compared with metal-ion chelating activities. The chemicals constituents in the essential oil are ether (23.66%), alcohols (16.72%), sesquiterpenes (15.21%), esters (11.78%), monoterpenes (11.63%), ketones (6.09%), aromatic compounds (5.01%), and account for a 90.10% analysis of its chemical composition. It is predicted that eucalyptol and the other constituents, except for alcohols, in the essential oil may contribute to its antioxidant activities. The results indicated that essential oil extracted from A. argyi leaves decreased melanin production in B16F10 cells and showed potent antioxidant activity. The essential oil can thereby be applied as an inhibitor of melanogenesis and could also act as a natural antioxidant in skin care products.     

Separation and characterization of bitumen from Athabasca oil sand

Separation and chemical analysis was investigated using bitumen samples from Athabasca oil sand in Alberta. Fractionation according to solubility and polarity has been used to separate bitumen into its fractions. The solvent de-asphaltening was performed by n-pentane solvent (solubility fractionation), and the polarity fractionation using Fuller’s earth allows maltene to separate into SARA components (saturates, aromatics, resins and asphaltenes). The SARA components are analyzed comprehensively using elemental analysis (EA), Fourier-transformed infrared (FTIR), ultraviolet-visible spectroscopy (UV-vis), high performance chromatography (HPLC) and thermogravimetric analysis (TGA). EA (C, H, N, S), heavy metals (Ni, V) concentrations, FT-IR and UV-vis tests provided the explanation of chemical composition. From IR spectra, maltene and saturates/aromatics (sat/aro) contained more aliphatic compounds than resin or asphaltene. Also, IR spectrum of sat/aro was similar to crude oil and VGO (vacuum gas oil). Different UV signal data clearly indicates the contribution of aromatic constituents in the fractions. Using optimized analysis conditions of HPLC, we successfully separated the peaks for bitumen and its fractions. The characteristic peak pattern of SARA (saturates, aromatics, resins, asphaltenes) fractions was observed, and also the peak pattern of sat/aro was similar to that of crude oil and VGO. However, TGA results revealed that thermal behavior for sat/aro was similar to that of crude oil but different from that of VGO. Also, from the comparison between decomposition temperature of TGA and boiling point, their correspondence was found.     

Sulfur specificity in the bench‐scale biological desulfurization of crude oil by Rhodococcus IGTS8

Biological removal of organic sulfur from petroleum feedstocks may offer an attractive alternative to conventional thermochemical treatment due to the mild operating conditions and greater reaction specificity afforded by the nature of biocatalysis. Previous investigations have either reported the desulfurization of model sulfur compounds in organic solvents or gross desulfurization of crude oil without data on which sulfur species were being removed. This study reports initial sulfur speciation data for thiophenic sulfur compounds present in crude oil which may be used as a guide both as to which species are treated by the biocatalyst investigated as well as to where biocatalyst development is needed to improve the extent of biological desulfurization when applied to whole crudes. Biodesulfurization of two different crude oils in the 22–31 ° API specific gravity range with total sulfur contents between 1 and 2% is demonstrated in 1‐dm³ batch stirred reactors using wild type Rhodococcus sp IGTS8. While analysis of the crudes before and after biodesulfurization did not reveal a decrease in total sulfur, GC–MS did reveal significant (43–99%) desulfurization of dibenzothiophenes (DBT) and substituted DBTs. Fractionation of the whole crude, followed by analysis using gas chromatography–sulfur chemiluminescence detection (GC–SCD) of the aromatic fraction of the Van Texas crude oil, demonstrated a reduction of sulfur in this fraction from 3.8% to 3.2%. This research indicates that IGTS8 may be capable of biodesulfurization of refined products such as gasoline and diesel whose predominant sulfur species are dibenzothiophenes. Further biocatalyst development would be needed for effective treatment of the spectrum of sulfur‐bearing compounds present in whole crudes.     

以不同减渣为原料制备大庆油田复合驱用表面活性剂的可行性研究

为扩大大庆油田复合驱用表面活性剂的原料范围,降低表面活性剂的生产成本,研究了利用不同的减渣制备复合驱用表面活性剂的可能性。实验结果表明,利用大庆减渣制备出的OCS表面活性剂具有很好的界面活性,当OCS表面活性剂浓度为0·1%~0·3%,Na2CO3浓度在0·6%~1·2%的范围内,OCS表面活性剂/Na2CO3体系与大庆原油之间的界面张力可达到超低(~10-3mN/m数量级)。大庆减渣适宜作为复合驱用表面活性剂的原料,而大港和石家庄减渣则不适宜。     

Resid Hydroprocessing at Amoco

Future worldwide crude supply projections indicate a shortage of high-quality, low-sulfur crudes. Figure 1 shows that the sulfur, gravity, and l000+°F material will continue to degrade the quality of crude oil for U.S. refiners [1]. The availability of more plentiful, heavier high-sulfur crudes creates several problems for the refiner. First, processing facilities are required to remove sulfur from the various fractions in the crude, and secondly, conversion facilities are required to convert the concentrations of 1000 + °F resid to more valuable products such as gasoline and distillates. In a conventional refinery, the vacuum resid (1000 + °F) is sold either as residual fuel or as asphalt, or it is thermally processed in cokers to produce coker liquids for further processing, and low-value petroleum coke. Because of the reduced markets for residual fuel, asphalt, and coke, refiners have had to install expensive conversion facilities to deal with the larger volumes of vacuum resids from poorer quality crudes.