这项工作是由美国国立卫生研究院（批准号:R00GM106414到FFL）的支持。我们要感谢佛罗里达国际大学的高级质谱设备的支持。

1.低能量水容纳馏分的准备（LEWAF） <ol><li>通过漂洗用二氯甲烷瓶子以除去任何潜在的污染物干净的2升抽吸瓶。 </li><li>灌装瓶用50ml二氯甲烷，将其关闭，并搅拌30秒。沥干他们到合适的废物容器。重复总共洗涤三次。 </li><li>使用一个抽吸瓶照射曝光而另一个瓶作为对照样品（使用重复组，每组如果可能的）。 </li><li>每用于33份每千最后盐度1升的水混合35克海盐混合物准备人工海水。过滤下小的溶液或无负压防止用装有0.45微米或更小的细孔过滤器的过滤装置的挥发性化合物的损失。 </li><li>装满人工海水抽吸瓶，剩下约20％，或400毫升，顶空的。 </li&gt; <li>原油添加到使用气密注射器以1g油/ L的标称浓度预定量的海水。 注:更多的粘性油应该重量递送。 </li><li>在加入油后，在黑暗中（或通过覆盖有铝箔抽吸瓶）利用在低速操作的搅拌盘无涡流（约100rpm）下的产生，以允许混合24小时的解所有的水溶性成分进入溶液，并避免微粒油的包容。 </li></ol> 2. LEWAF光照射，样品采集和处理<ol><li>准备两套瓶的每个光照射实验。 </li><li>盖一组用铝箔抽吸瓶;这将是暗控制。 </li><li>放置抽吸瓶在温度控制的水浴集以保持太阳能照射配备无线的内部，在25℃的温度下的抽吸瓶在765瓦/米2的光强度第一个1500瓦氙弧灯。 </li><li>连续照射的样本的所需时间（在此实验持续115 H）;没有最长时间。 </li><li>后设定的时间，（在此实验15，24，48，和115高）由拔去塞子吸气瓶并打开排水阀收集150毫升水从玻璃抽吸器的底部。 </li><li>利用分液漏斗通过添加二氯甲烷50毫升等分试样，振摇2分钟定期排空漏斗，以避免从吹离塞子的样品进行与二氯甲烷液 - 液萃取。 </li><li>使各相分离，并通过从漏斗除去塞子除去底部的有机相和缓慢打开排水阀。沥干样品到装有填充用100克Na 2 SO 4的漏斗的平底烧瓶中。冲洗用另外的二氯甲烷漏斗为了执行提取3次人口增加Ë提取效率。 注意:多个提取是为了提高该过程的提取效率进行。 </li><li>取下漏斗，添加一个斯奈德列和放置的平坦底部烧瓶在设定为58℃的热水浴中。蒸发直至样品的15毫升保持。 </li><li>将样品转移到集中管使用氮气小心飞溅，避免样品损失吹干干燥样品。 </li></ol> 3.分析试样的制备注意:用于分析样品制备是关键，必须小心，以避免引入外来杂质，特别是通过使用的任何塑料，这将导致浸出进入样品。 <ol><li>制备的1的混合物:利用LC-MS最优级溶剂甲苯:1体积:体积甲醇。 </li><li>使用正位移微量，添加溶剂的玻璃小瓶中，然后以1:1的比例添加样品:100，先加入的溶剂990微升，然后通过添加样品的10μL的。 注:玻璃微量移是为了避免榨取使用，由于二氯甲烷或甲苯。 </li><li>可选:使用混合调谐校准离子迁移。 注:一个API源往往会浸出如果经常作为校准标准使用。 1000稀释:如果校准离子中不存在的光谱，然后混合物可以通过加入一些以1标准溶液到样品的制备。 </li></ol> 4.傅立叶变换离子回旋共振质谱（FT-ICR MS）分析<ol><li>通过点击操作按钮，仪器设置到"操作"模式。 </li><li>加载样品到样品注射器中。 </li><li>根据API源选项卡，设置在200微升/ h的速度输液速度。 </li><li>设置喷雾器压力为1巴，蒸发器温度到300℃。 </li><li>将干气率1.2升/分钟，温度为220℃。 注:此过程同时适用于APPI和APCI。 </li><li>通过单击调按钮设置仪器"调"模式。频谱应该出现在屏幕上。 注意:如果需要，仪器可在顺序通过改变仪器参数，如电压，RF频率，和幅度提高分析物的m / z范围的离子传输和检测进行优化。需要注意的是质谱仪将需要重新校准。 </li><li>通过点击停止按钮停止"调"模式。 </li><li>设定的扫描次数为每质谱20-200扫描之间平均，典型地，按获取按钮获取的质谱。 注:平均多个光谱提高通过降低噪声和增加对低丰度品种14的信号的总体信噪比。 </li></ol> 5.囚禁离子迁移SPECTRometry（TIMS）分析<ol><li>启用了FT-ICR的收购计划"色谱"模式。 </li><li>通过在外部断路器TIMS接通开关使能"TIMS"模式。 注:在TIMS使用的电压从仪器外部控制。第二软件将控制来执行的IMS分析仪器的入口漏斗。 </li><li>打开补充粗抽泵，并使用TIMS的控制阀，调节所述入口和出口压力，以期望的范围（在该实验中，P1被设定为2.8毫巴和P2至1.4毫巴）。 注:外部泵应在几个小时分析之前被接通，以确保所述泵是温暖和性能是IMS分析期间均匀，因为在气体速率的变化会引起光谱的错误。 </li><li>首先确定需要执行所述IMS分析的电压范围;这是一个快速，粗略在宽电压范围（250 V）在搜索完成IMS低解析度（1 V /帧）。 </li><li>如果所用的电压是足以分析整个频谱，然后重复实验，调整TIMS为更高分辨率的分析。这样做，减小V /帧为0.1V和改变帧的数目，以涵盖所有的ΔV 坡道 。 注意:用户可能需要优化的被累加到之前对FT-ICR质谱分析碰撞单元TIMS实验次数。 </li></ol> 6.数据分析<ol><li>在数据分析软件打开MS数据。 </li><li>设置峰值采集标准来选择与上述6的信号与噪声和使用"查找峰"功能。 注意:得到的光谱是使用存在于溶液中的标准内部重新校准。这被用来确定化学系列，然后，为了提高对宽范围的元素分配的准确性再次重新校准。 </li><li>使用公式分配进行元素赋值换货工具或软件。 注:H 1-100ñØ0-2 0-7 0-2小号，奇数和偶数的电子配置，允许的Ç1-100公式的限制，并为0.5ppm M +的质量宽容和[M + H] +离子的形式</li><li>在IMS-MS数据导入到数据分析软件，并为整个分析范围的平均质谱。 </li><li>上述6的信号 - 噪声选择峰。使用在所述超高分辨率MS分析，鉴定系列，在内部重新校准光谱</li><li>从FT-ICR MS分析使用公式标识，生成所有目标M / Z的名单，并在数据文件夹本另存为"Flist.txt"。该列表将在数据处理的第一步骤中使用</li><li>加载并以提取列表中的每个目标M / Z的提取离子色谱（EIC）运行所提供的脚本。 </li><li>修改python脚本输入文件主任y，则启动电压，步长，并在该目标分析11个步骤的数量。 </li><li>运行IMS反褶积脚本。 注意:这将打开每个EIC和迭代高斯拟合确定的峰值。结果将在Excel文件格式输出13。 注:嵌合后，低于一定标准的峰被排除在外，通常基于高度，宽度和峰的面积（一定宽度以下的峰通常从分析中排除，因为随机噪声尖峰的）。 </li><li>利用调谐峰，从电压校准离子迁移率的离子11的流动性。这可以转换为使用梅森 - Schamp方程碰撞截面。 </li></ol>

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作者宣称没有竞争经济利益。

该议定书中的关键步骤 LEWAFs的化学复杂性需要，以便使实验室实验来准确反映自然发生准确制剂。数据的有效评估取决于三个标准:尽量减少引进的文物在整个样品处理（ 例如，准备LEWAF，取样，提取，并准备样品进行分析的），验证实验方案（ 即使用暗控制对于光照射试验），并验证该仪器的性能（ 即，验证MS和IMS性能通过使用标准）。 <p class="jove_cont...

有环境暴露原油的来源众多，无论是从自然原因和人为风险。在释放到环境中，特别是在海洋中，原油可经历分区，与浮油的表面上的形成，挥发性组分到大气中的损失，和沉积。然而，难溶油和确实发生的水，并将该混合物，这是不经典溶解，低能量混合形成什么作为低能量的水容纳部分（LEWAF）简称。在水中的油组分的增溶的油 - 水界面的暴露于太阳辐射中，通常提高。在海洋中的原油的照片增溶可以因此暴露于太阳辐射和/或由于酶促降解1,2经历显著化学变化。理解这些化学变化和<html>他们是如何发生在散装矩阵（ 即，原油）的存在是为了减轻这种曝光，对环境的影响的基础。 以前的研究已经表明，原油经受氧化，特别是多环芳香烃（PAHs），这代表污染一个危害生物，经过生物积累的剧毒源，并且是生物活性3，5，6。因为它们只发生在本体基体的存在理解不同的氧合过程的产物是具有挑战性的。因此，一个单一的标准分析可能不具有代表性的天然存在的变化。该LEWAF的编制必须复制了发生在一个环境背景自然过程。特别感兴趣的是多环芳烃的充氧，发生由于太阳辐射。 T"&gt;在水容纳部分的研究的第二个挑战是在样品中的不同的化学成分的分子鉴定。由于样品的复杂性，所造成的高的质量和氧气的程度，氧化产物是通常不适合于传统的分析用气相色谱法与质谱分析7,8结合进行。另一种方法是通过利用超高质量分辨率质谱技术（ 例如，FT-ICR质谱来表征样品的化学式中的变化），通过耦合TIMS到FT-ICR质谱，除了在MS域中的同量异序的分离，离子迁移光谱（IMS）的尺寸为存在于样品9，10，11中的不同的异构体的分离和特征信息。与大气压力激光组合电离（APLI）源，分析可以是选择性的样品中发现的共轭分子，允许改变该多环芳烃经受是准确特征12,13。 在这项工作中，我们描述了为了研究油成分的变换处理暴露于光照射LEWAFs的制备的协议。我们还说明了在光照射时发生的变化，以及对样品提取的过程。我们也将呈现使用APLI与耦合用FT-ICR质谱表征在LEWAF多环芳烃作为曝光于光的功能TIMS。

<table><tbody><tr><td>&lt;strong&gt;Reagents&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>methylene chloride, Optima</td><td>Fisher Scientific</td><td>DS-151-4</td><td>Used as received</td></tr><tr><td>methanol, Optima LC/MS</td><td>Fisher Scientific</td><td>A456-4</td><td>Used as received</td></tr><tr><td>toluene, Optima</td><td>Fisher Scientific</td><td>T291-4</td><td>Used as received</td></tr><tr><td>Na&lt;sub&gt;2&lt;/sub&gt;SO&lt;sub&gt;4&lt;/sub&gt;, Granular, Anhydrous</td><td>Fisher Scientific</td><td>S415-212</td><td>Combusted at 450&amp;nbsp;&amp;#176;C/Stored at 105&amp;nbsp;&amp;#176;C</td></tr><tr><td>Crude oil</td><td>Various sources</td><td></td><td></td></tr><tr><td>Instant Ocean&amp;reg;</td><td>Aquarium Systems</td><td>SS1200</td><td>33 ppt salinity with 0.45&amp;nbsp;&amp;mu;m pore filtration</td></tr><tr><td>&lt;strong&gt;Name&amp;nbsp;&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Equipment&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Suntext XLS+</td><td>Atlas Chicalo Ill, USA</td><td></td><td>1,500 W xeon arc lamp, light intensity of 765&amp;nbsp;W/m&lt;sup&gt;2&lt;/sup&gt;</td></tr><tr><td>Atmospheric Pressure Laser Ionization</td><td>Bruker Daltonics Inc, MA</td><td></td><td>Note a 266 nm laser is used</td></tr><tr><td>TIMS-FT-ICR MS Instrument</td><td>Bruker Daltonics Inc, MA</td><td></td><td>The set up we had consisted of a 7&amp;nbsp;T magnet with an infinity cell</td></tr><tr><td>&lt;strong&gt;Name&amp;nbsp;&lt;/strong&gt;</td><td>&lt;strong&gt;Company&lt;/strong&gt;</td><td>&lt;strong&gt;Catalog Number&lt;/strong&gt;</td><td>&lt;strong&gt;Comments&lt;/strong&gt;</td></tr><tr><td>&lt;strong&gt;Software&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>DataAnalysis 4.2</td><td>Bruker Daltonics Inc, MA</td><td></td><td></td></tr><tr><td>Python 2.7</td><td></td><td></td><td>Requires Numpy, Scipy, Pandas, glob, oct2py, and os</td></tr><tr><td>Octave 4.0</td><td></td><td></td><td></td></tr></tbody></table>

chemical analysis of water-accommodated fractions of crude oil spills using tims-ft-icr ms

多种化学过程控制石油原油是如何被纳入到海水中，也发生加班的化学反应。研究这种系统需要的样本，以准确的复制出现在自然界的水容纳部分的自然形成的精心准备。低能量水容纳部分（LEWAF）都是严格在设定的比例混合原油和水配制。然后抽吸瓶照射，并在设定的时间点，水进行采样，并使用标准技术提取。第二个挑战是样本，必须考虑到，随时间发生的化学变化的代表特性。可以使用耦合到定制的俘获离子迁移谱傅立叶变换离子回旋共振质谱（TIMS-FT常压激光电离源来执行LEWAF的芳烃馏分的目标分析-ICR MS）。所述TIMS-FT-ICR质谱分析提供的高分辨率离子迁移和超高分辨率MS分析，其中，还允许同分异构组分的鉴定可以通过碰撞截面（CCS）和化学式。结果表明，随着油 - 水混合物被暴露于光，有表面油的显著光溶解到水中。随着时间的推移，溶解的分子的化学转变发生时，在含氮和含硫物种的标识的数量有利于那些具有更大的氧含量比在基础油中典型地观察到的降低。

通过TIMS-FT-ICR MS结果中基于M / Z和TIMS捕获电压的二维频谱LEWAF分析。各样品，在不同时间点拍摄，因此，可以根据特征的改变的化学成分，由化学式的分布和由IMS（ 见图1）所确定的异构体的贡献所观察到的。通常情况下，M / Z信息可以用来为元素式分配给分析峰。使用APLI的允许与芳香双键分子与更高的灵敏度15分析，电离广泛的...

Watch this Scientific Journal Video about Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS at JoVE.com

使用 TIMS-FT-ICR MS 对原油泄漏的含水部分进行化学分析环境 |视频

Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

原油的低能量水容纳部分（LEWAF）是一个具有挑战性的系统来分析，因为随着时间的推移，这种复杂的混合物发生化学转变。这个协议说明了LEWAF样品的准备和用于通过俘获离子迁移谱-FT-ICR质谱进行光照射和化学分析方法。

原油水容纳组分的化学分析泄漏使用TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system ...

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11.1K 次观看.  Florida International University. 原油的低能量水容纳部分（LEWAF）是一个具有挑战性的系统来分析，因为随着时间的推移，这种复杂的混合物发生化学转变。这个协议说明了LEWAF样品的准备和用于通过俘获离子迁移谱-FT-ICR质谱进行光照射和化学分析方法。 

视频: Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

A Whole Cell Bioreporter Approach to Assess Transport and Bioavailability of Organic Contaminants in Water Unsaturated Systems

Bioavailability of contaminants is a prerequisite for their effective biodegradation in soil. The average bulk concentration of a contaminant, however, is not an appropriate measure for its availability; bioavailability rather depends on the dynamic interplay of potential mass transfer (flux) of a compound to a microbial cell and the capacity of the latter to degrade the compound. In water-unsaturated parts of the soil, mycelia have been shown to overcome bioavailability limitations by actively transporting and mobilizing organic compounds over the range of centimeters. Whereas the extent of mycelia-based transport can be quantified easily by chemical means, verification of the contaminant-bioavailability to bacterial cells requires a biological method. Addressing this constraint, we chose the PAH fluorene (FLU) as a model compound and developed a water unsaturated model microcosm linking a spatially separated FLU point source and the FLU degrading bioreporter bacterium Burkholderia sartisoli RP037-mChe by a mycelial network of Pythium ultimum. Since the bioreporter expresses eGFP in response of the PAH flux to the cell, bacterial FLU exposure and degradation could be monitored directly in the microcosms via confocal laser scanning microscopy (CLSM). CLSM and image analyses revealed a significant increase of the eGFP expression in the presence of P. ultimum compared to controls without mycelia or FLU thus indicating FLU bioavailability to bacteria after mycelia-mediated transport. CLSM results were supported by chemical analyses in identical microcosms. The developed microcosm proved suitable to investigate contaminant bioavailability and to concomitantly visualize the involved bacteria-mycelial interactions.

A whole cell bioreporter assay with Burkholderia sartisoli RP037-mChe was developed to detect fractions of an organic contaminant (i.e., fluorene) available for bacterial degradation after active transport by mycelia bridging air-filled pores in a water unsaturated model system.

全细胞Bioreporter方法​​评估交通有机污染物的生物利用度和水饱和系统

Bioavailability of contaminants is a prerequisite for their effective biodegradation in soil. The average bulk concentration of a contaminant, however, is ...

科研

环境科学

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate interferences, a two dimensional column configuration is used, with a Deans switch employed to transfer hydrogen sulfide from the first to the second column (heart-cutting). Liquid crude samples are first separated on a dimethylpolysiloxane column, and light gases are heart-cut and further separated on a bonded porous layer open tubular (PLOT) column that is able to separate hydrogen sulfide from other light sulfur species. Hydrogen sulfide is then detected with a sulfur chemiluminescence detector, adding an additional layer of selectivity. Following separation and detection of hydrogen sulfide, the system is backflushed to remove the high-boiling hydrocarbons present in the crude samples and to preserve chromatographic integrity. Dissolved hydrogen sulfide has been quantified in liquid samples from 1.1 to 500 ppm, demonstrating wide applicability to a range of samples. The method has also been successfully applied for the analysis of gas samples from crude oil headspace and process gas bags, with measurement from 0.7 to 9,700 ppm hydrogen sulfide.

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

A multidimensional gas chromatography method for the analysis of dissolved hydrogen sulfide in liquid crude oil samples is presented. A Deans switch is used to heart-cut light sulfur gases for separation on a secondary column and detection on a sulfur chemiluminescence detector.

h的测量<sub&gt; 2</sub&gt; S在原油和原油顶空用多维气相色谱法，院长交换和选择性硫检测

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate ...

Cellular Lipid Extraction for Targeted Stable Isotope Dilution Liquid Chromatography-Mass Spectrometry Analysis

The metabolism of fatty acids, such as arachidonic acid (AA) and linoleic acid (LA), results in the formation of oxidized bioactive lipids, including numerous stereoisomers1,2. These metabolites can be formed from free or esterified fatty acids. Many of these oxidized metabolites have biological activity and have been implicated in various diseases including cardiovascular and neurodegenerative diseases, asthma, and cancer3-7. Oxidized bioactive lipids can be formed enzymatically or by reactive oxygen species (ROS). Enzymes that metabolize fatty acids include cyclooxygenase (COX), lipoxygenase (LO), and cytochromes P450 (CYPs)1,8. Enzymatic metabolism results in enantioselective formation whereas ROS oxidation results in the racemic formation of products.
While this protocol focuses primarily on the analysis of AA- and some LA-derived bioactive metabolites; it could be easily applied to metabolites of other fatty acids. Bioactive lipids are extracted from cell lysate or media using liquid-liquid (l-l) extraction. At the beginning of the l-l extraction process, stable isotope internal standards are added to account for errors during sample preparation. Stable isotope dilution (SID) also accounts for any differences, such as ion suppression, that metabolites may experience during the mass spectrometry (MS) analysis9. After the extraction, derivatization with an electron capture (EC) reagent, pentafluorylbenzyl bromide (PFB) is employed to increase detection sensitivity10,11. Multiple reaction monitoring (MRM) is used to increase the selectivity of the MS analysis. Before MS analysis, lipids are separated using chiral normal phase high performance liquid chromatography (HPLC). The HPLC conditions are optimized to separate the enantiomers and various stereoisomers of the monitored lipids12. This specific LC-MS method monitors prostaglandins (PGs), isoprostanes (isoPs), hydroxyeicosatetraenoic acids (HETEs), hydroxyoctadecadienoic acids (HODEs), oxoeicosatetraenoic acids (oxoETEs) and oxooctadecadienoic acids (oxoODEs); however, the HPLC and MS parameters can be optimized to include any fatty acid metabolites13.
Most of the currently available bioanalytical methods do not take into account the separate quantification of enantiomers. This is extremely important when trying to deduce whether or not the metabolites were formed enzymatically or by ROS. Additionally, the ratios of the enantiomers may provide evidence for a specific enzymatic pathway of formation. The use of SID allows for accurate quantification of metabolites and accounts for any sample loss during preparation as well as the differences experienced during ionization. Using the PFB electron capture reagent increases the sensitivity of detection by two orders of magnitude over conventional APCI methods. Overall, this method, SID-LC-EC-atmospheric pressure chemical ionization APCI-MRM/MS, is one of the most sensitive, selective, and accurate methods of quantification for bioactive lipids.

This protocol will demonstrate the extraction and analysis of free and esterified bioactive fatty acids from cells. Fatty acids are accurately quantified using stable isotope dilution, chiral liquid chromatography, electron capture atmospheric chemical ionization multiple reaction monitoring mass spectrometry (SID-LC-ECAPCI-MRM/MS).

有针对性的稳定同位素稀释液相色谱 - 质谱法分析细胞脂质提取

The metabolism of fatty acids, such as arachidonic acid (AA) and linoleic acid (LA), results in the formation of oxidized bioactive lipids, including ...

生物工程

Characterization and Application of Passive Samplers for Monitoring of Pesticides in Water

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study provides a protocol for the passive sampler preparation, calibration, extraction method and instrumental analysis. Sampling rates (RS) and passive sampler-water partition coefficients (KPW) were calculated for silicone rubber, polar organic chemical integrative sampler POCIS-A, POCIS-B, SDB-RPS and C18 disk. The uptake of the selected compounds depended on their physicochemical properties, i.e., silicone rubber showed a better uptake for more hydrophobic compounds (log octanol-water partition coefficient (KOW) &#62; 5.3), whereas POCIS-A, POCIS-B and SDB-RPS disk were more suitable for hydrophilic compounds (log KOW &#60; 0.70).

A protocol about the characterization and application of five different passive sampling devices is presented.

表征和被动采样的应用在农药水监测

Five different water passive samplers were calibrated under laboratory conditions for measurement of 124 legacy and current used pesticides. This study ...

Laboratory Production of Biofuels and Biochemicals from a Rapeseed Oil through Catalytic Cracking Conversion

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil (HGO) for production of transportation fuels through a fluid catalytic cracking (FCC) route. Cracking experiments are performed with a fully automated reaction unit at a fixed weight hourly space velocity (WHSV) of 8 hr-1, 490-530 &#176;C, and catalyst/oil ratios of 4-12 g/g. When a feed is in contact with catalyst in the fluid-bed reactor, cracking takes place generating gaseous, liquid, and solid products. The vapor produced is condensed and collected in a liquid receiver at -15 &#176;C. The non-condensable effluent is first directed to a vessel and is sent, after homogenization, to an on-line gas chromatograph (GC) for refinery gas analysis. The coke deposited on the catalyst is determined in situ by burning the spent catalyst in air at high temperatures. Levels of CO2 are measured quantitatively via an infrared (IR) cell, and are converted to coke yield. Liquid samples in the receivers are analyzed by GC for simulated distillation to determine the amounts in different boiling ranges, i.e., IBP-221 &#176;C (gasoline), 221-343 &#176;C (light cycle oil), and 343 &#176;C+ (heavy cycle oil). Cracking of a feed containing canola oil generates water, which appears at the bottom of a liquid receiver and on its inner wall. Recovery of water on the wall is achieved through washing with methanol followed by Karl Fischer titration for water content. Basic results reported include conversion (the portion of the feed converted to gas and liquid product with a boiling point below 221 &#176;C, coke, and water, if present) and yields of dry gas (H2-C2's, CO, and CO2), liquefied petroleum gas (C3-C4), gasoline, light cycle oil, heavy cycle oil, coke, and water, if present.

This paper presents an experimental method to produce biofuels and biochemicals from canola oil mixed with a fossil-based feed in the presence of a catalyst at mild temperatures. Gaseous, liquid, and solid products from a reaction unit are quantified and characterized. Conversion and individual product yields are calculated and reported.

通过催化裂化转换从菜籽油生物燃料和生物化学实验室生产

The work is based on a reported study which investigates the processability of canola oil (bio-feed) in the presence of bitumen-derived heavy gas oil ...

化学

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to visualize the behavior of petroleum samples under process conditions. The experimental setup relies on a custom-built micro-reactor fitted with a sapphire window at the bottom, which is placed over the objective of an inverted microscope equipped with a cross-polarizer module. Using reflection microscopy enables the visualization of opaque samples, such as petroleum vacuum residues, or asphaltenes. The combination of the sapphire window from the micro-reactor with the cross-polarizer module of the microscope on the light path allows high-contrast imaging of isotropic and anisotropic media. While observations are carried out, the micro-reactor can be heated to the temperature range of cracking reactions (up to 450 &#176;C), can be subjected to H2 pressure relevant to hydroconversion reactions (up to 16 MPa), and can stir the sample by magnetic coupling. 
Observations are typically carried out by taking snapshots of the sample under cross-polarized light at regular time intervals. Image analyses may not only provide information on the temperature, pressure, and reactive conditions yielding phase separation, but may also give an estimate of the evolution of the chemical (absorption/reflection spectra) and physical (refractive index) properties of the sample before the onset of phase separation.

In Situ Visualization of the Phase Behavior of Oil Samples Under Refinery Process Conditions

This article describes a setup and method for the in situ visualization of oil samples under a variety of temperature and pressure conditions that aim to emulate refining and upgrading processes. It is primarily used for studying isotropic and anisotropic media involved in the fouling behavior of petroleum feeds.

在油样品的相行为在炼油工艺条件的原位可视化

To help address production issues in refineries caused by the fouling of process units and lines, we have developed a setup as well as a method to ...

工程学

Single-throughput Complementary High-resolution Analytical Techniques for Characterizing Complex Natural Organic Matter Mixtures

Natural organic matter (NOM) is composed of a highly complex mixture of thousands of organic compounds which, historically, proved difficult to characterize. However, to understand the thermodynamic and kinetic controls on greenhouse gas (carbon dioxide [CO2] and methane [CH4]) production resulting from the decomposition of NOM, a molecular-level characterization coupled with microbial proteome analyses is necessary. Further, climate and environmental changes are expected to perturb natural ecosystems, potentially upsetting complex interactions that influence both the supply of organic matter substrates and the microorganisms performing the transformations. A detailed molecular characterization of the organic matter, microbial proteomics, and the pathways and transformations by which organic matter is decomposed will be necessary to predict the direction and magnitude of the effects of environmental changes. This article describes a methodological throughput for comprehensive metabolite characterization in a single sample by direct injection Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS), gas chromatography mass spectrometry (GC-MS), nuclear magnetic resonance (NMR) spectroscopy, liquid chromatography mass spectrometry (LC-MS), and proteomics analysis. This approach results in a fully-paired dataset which improves statistical confidence for inferring pathways of organic matter decomposition, the resulting CO2 and CH4 production rates, and their responses to environmental perturbation. Herein we present results of applying this method to NOM samples collected from peatlands; however, the protocol is applicable to any NOM sample (e.g., peat, forested soils, marine sediments, etc.).

This protocol describes a single throughput for complementary analytical and omics techniques culminating in a fully-paired characterization of natural organic matter and microbial proteomics in different ecosystems. This approach permits robust comparisons for identifying metabolic pathways and transformations important for describing greenhouse gas production and predicting responses to environmental change.

用于表征复杂天然有机物混合物的单吞吐量互补高分辨率分析技术

Natural organic matter (NOM) is composed of a highly complex mixture of thousands of organic compounds which, historically, proved difficult to ...

Experimental Procedure for Laboratory Studies of In Situ Burning : Flammability and Burning Efficiency of Crude Oil

A new method for the simultaneous study of the flammability and burning efficiency of fresh and weathered crude oil through two experimental laboratory setups is presented. The experiments are easily repeatable compared to operational scale experiments (pool diameter &#8805;2 m), while still featuring quite realistic in situ burning conditions of crude oil on water. Experimental conditions include a flowing water sub-layer that cools the oil slick and an external heat flux (up to 50 kW/m2) that simulates the higher heat feedback to the fuel surface in operational scale crude oil pool fires. These conditions enable a controlled laboratory study of the burning efficiency of crude oil pool fires that are equivalent to operational scale experiments. The method also provides quantitative data on the requirements for igniting crude oils in terms of the critical heat flux, ignition delay time as a function of the incident heat flux, the surface temperature upon ignition, and the thermal inertia. This type of data can be used to determine the required strength and duration of an ignition source to ignite a certain type of fresh or weathered crude oil. The main limitation of the method is that the cooling effect of the flowing water sub-layer on the burning crude oil as a function of the external heat flux has not been fully quantified. Experimental results clearly showed that the flowing water sub-layer does improve how representative this setup is of in situ burning conditions, but to what extent this representation is accurate is currently uncertain. The method nevertheless features the most realistic in situ burning laboratory conditions currently available for simultaneously studying the flammability and burning efficiency of crude oil on water.

Experimental Procedure for Laboratory Studies of In Situ Burning : Flammability and Burning Efficiency of Crude Oil

Here, we present a protocol to simultaneously study the flammability and burning efficiency of fresh and weathered crude oil under conditions that simulate in situ burning operations on the sea.

原位燃烧试验方法: 原油可燃性和燃烧效率

A new method for the simultaneous study of the flammability and burning efficiency of fresh and weathered crude oil through two experimental laboratory ...

Enhanced Oil Recovery using a Combination of Biosurfactants

Biosurfactants are surface-active compounds capable of reducing the surface tension between two phases of different polarities. Biosurfactants have been emerging as promising alternatives to chemical surfactants due to less toxicity, high biodegradability, environmental compatibility and tolerance to extreme environmental conditions. Here, we illustrate the methods used for screening of microbes capable of producing biosurfactants. The biosurfactant producing microbes were identified using drop collapse, oil spreading, and emulsion index assays. Biosurfactant production was validated by determining the reduction in surface tension of the media due to growth of the microbial members. We also describe the methods involved in characterization and identification of biosurfactants. Thin layer chromatography of the extracted biosurfactant followed by differential staining of the plates was performed to determine the nature of the biosurfactant. LCMS, 1H NMR, and FT-IR were used to chemically identify the biosurfactant. We further illustrate the methods to evaluate the application of the combination of produced biosurfactants for enhancing residual oil recovery in a simulated sand pack column.

We illustrate the methods involved in screening and identification of the biosurfactant producing microbes. Methods for chromatographic characterization and chemical identification of the biosurfactants, determining the industrial applicability of the biosurfactant&#160;in enhancing residual oil recovery are also presented.

使用生物表面活性剂组合提高石油采收率

Biosurfactants are surface-active compounds capable of reducing the surface tension between two phases of different polarities. Biosurfactants have been ...

Pore-scale Imaging and Characterization of Hydrocarbon Reservoir Rock Wettability at Subsurface Conditions Using X-ray Microtomography

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to characterize the complex wetting conditions of hydrocarbon reservoir rock using pore-scale three-dimensional X-ray imaging at subsurface conditions. In this work, heterogeneous carbonate reservoir rocks, extracted from a very large producing oil field, have been used to demonstrate the protocol. The rocks are saturated with brine and oil and aged over three weeks at subsurface conditions to replicate the wettability conditions that typically exist in hydrocarbon reservoirs (known as mixed-wettability). After the brine injection, high-resolution three-dimensional images (2 &#181;m/voxel) are acquired and then processed and segmented. To calculate the distribution of the contact angle, which defines the wettability, the following steps are performed. First, fluid-fluid and fluid-rock surfaces are meshed. The surfaces are smoothed to remove voxel artefacts, and in situ contact angles are measured at the three-phase contact line throughout the whole image. The main advantage of this method is its ability to characterize in situ wettability accounting for pore-scale rock properties, such as rock surface roughness, rock chemical composition, and pore size. The in situ wettability is determined rapidly at hundreds of thousands of points. 
The method is limited by the segmentation accuracy and X-ray image resolution. This protocol could be used to characterize the wettability of other complex rocks saturated with different fluids and at different conditions for a variety of applications. For example, it could help in determining the optimal wettability that could yield an extra oil recovery (i.e., designing brine salinity accordingly to obtain higher oil recovery) and to find the most efficient wetting conditions to trap more CO2 in subsurface formations.

This protocol is presented to characterize the complex wetting conditions of an opaque porous medium (hydrocarbon reservoir rock) using three-dimensional images obtained by X-ray microtomography at subsurface conditions.

利用 X 射线层析在地下条件下油气储层岩石润湿性的孔隙度成像与表征

In situ wettability measurements in hydrocarbon reservoir rocks have only been possible recently. The purpose of this work is to present a protocol to ...

原油水容纳组分的化学分析泄漏使用TIMS-FT-ICR MS

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利用 X 射线层析在地下条件下油气储层岩石润湿性的孔隙度成像与表征

原油水容纳组分的化学分析泄漏使用TIMS-FT-ICR MS

摘要

探索更多视频

此视频中的章节

全细胞Bioreporter方法​​评估交通有机污染物的生物利用度和水饱和系统

h的测量

有针对性的稳定同位素稀释液相色谱 - 质谱法分析细胞脂质提取

表征和被动采样的应用在农药水监测

通过催化裂化转换从菜籽油生物燃料和生物化学实验室生产

在油样品的相行为在炼油工艺条件的原位可视化

用于表征复杂天然有机物混合物的单吞吐量互补高分辨率分析技术

原位燃烧试验方法: 原油可燃性和燃烧效率

使用生物表面活性剂组合提高石油采收率

利用 X 射线层析在地下条件下油气储层岩石润湿性的孔隙度成像与表征

全细胞Bioreporter方法评估交通有机污染物的生物利用度和水饱和系统