Name: an experimental protocol for studying mineral effects on organic hydrothermal transformations
Uploaded: 2018-08-08T15:00:00
Description: Watch this Scientific Journal Video about An Experimental Protocol for Studying Mineral Effects on Organic Hydrothermal Transformations at JoVE.com

我们感谢亚利桑那州立大学的 H.O.G. 小组制定了这些热液实验的初步方法, 特别是感谢我. 古尔德、e. 休克、l. 威廉斯、c. Glein、h. Hartnett、k. 费克图、鲁滨逊和 c. Bockisch, 他们指导和帮助。从奥克兰大学到 z 杨的创业基金资助了他和 x。

1. 制备热液试验样品
<ol><li>选择石英或石英玻璃管的尺寸,如2 毫米内径 (ID) x 6 毫米外径 (外径) 或6毫米 x 12 毫米外径, 并确定使用的有机化合物和矿物质的数量。在这项工作中, 硝基苯和磁铁矿的数量 (Fe3O4) 加载到二氧化硅管 (如2 毫米 ID x 6 毫米外径) 分别为3.0 µL 和13.9 毫克。 注: 大口径管允许材料更容易加载, 但需要更多的管道密封工作。</li>
	<li>用管子切割机?...

<ol>
	<li>Yang, Z., Gould, I. R., Williams, L. B., Hartnett, H. E., Shock, E. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effects+of+iron-containing+minerals+on+hydrothermal+reactions+of+ketones.">Effects of iron-containing minerals on hydrothermal reactions of ketones.</a> Geochimica et Cosmochimica Acta. 223, 107-126 (2018).</li><li>Seewald, J. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Organic-inorganic+interactions+in+petroleum-producing+sedimentary+basins.">Organic-inorganic interactions in petroleum-producing sedimentary basins.</a> Nature. 426 (6964), 327-333 (2003).</li><li>Sogin, M. L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microbial+diversity+in+the+deep+sea+and+the+underexplored+"rare+biosphere".">Microbial diversity in the deep sea and the underexplored "rare biosphere".</a> Proceedings of the National Academy of Sciences. 103 (32), 12115 (2006).</li><li>McCollom, T. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Laboratory+Simulations+of+Abiotic+Hydrocarbon+Formation+in+Earth's+Deep+Subsurface.">Laboratory Simulations of Abiotic Hydrocarbon Formation in Earth's Deep Subsurface.</a> Reviews in Mineralogy and Geochemistry. 75 (1), 467-494 (2013).</li><li>Foustoukos, D. I., Seyfried, W. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrocarbons+in+Hydrothermal+Vent+Fluids:+The+Role+of+Chromium-Bearing+Catalysts.">Hydrocarbons in Hydrothermal Vent Fluids: The Role of Chromium-Bearing Catalysts.</a> Science. 304 (5673), 1002 (2004).</li><li>Bell, J. L. S., Palmer, D. A., Pittman, E. D., Lewan, M. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=10.1007/978-3-642-78356-2_9.">10.1007/978-3-642-78356-2_9.</a> Organic Acids in Geological Processes. , 226-269 (1994).</li><li>Palmer, D. A., Drummond, S. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+decarboxylation+of+acetate.+Part+I.+The+kinetics+and+mechanism+of+reaction+in+aqueous+solution.">Thermal decarboxylation of acetate. Part I. The kinetics and mechanism of reaction in aqueous solution.</a> Geochimica et Cosmochimica Acta. 50 (5), 813-823 (1986).</li><li>Yang, Z., Gould, I. R., Williams, L. B., Hartnett, H. E., Shock, E. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+central+role+of+ketones+in+reversible+and+irreversible+hydrothermal+organic+functional+group+transformations.">The central role of ketones in reversible and irreversible hydrothermal organic functional group transformations.</a> Geochimica et Cosmochimica Acta. 98, 48-65 (2012).</li><li>McCollom, T. M., Ritter, G., Simoneit, B. R. T. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Lipid+Synthesis+Under+Hydrothermal+Conditions+by+Fischer-+Tropsch-Type+Reactions.">Lipid Synthesis Under Hydrothermal Conditions by Fischer- Tropsch-Type Reactions.</a> Origins of life and evolution of the biosphere. 29 (2), 153-166 (1999).</li><li>Bell, J. L. S., Palmer, D. A., Barnes, H. L., Drummond, S. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Thermal+decomposition+of+acetate:+III.+Catalysis+by+mineral+surfaces.">Thermal decomposition of acetate: III. Catalysis by mineral surfaces.</a> Geochimica et Cosmochimica Acta. 58 (19), 4155-4177 (1994).</li><li>Yang, Z., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrothermal+Photochemistry+as+a+Mechanistic+Tool+in+Organic+Geochemistry:+The+Chemistry+of+Dibenzyl+Ketone.">Hydrothermal Photochemistry as a Mechanistic Tool in Organic Geochemistry: The Chemistry of Dibenzyl Ketone.</a> The Journal of Organic Chemistry. 79 (17), 7861-7871 (2014).</li><li>Yang, Z., Hartnett, H. E., Shock, E. L., Gould, I. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Organic+Oxidations+Using+Geomimicry.">Organic Oxidations Using Geomimicry.</a> The Journal of Organic Chemistry. 80 (24), 12159-12165 (2015).</li><li>Venturi, S., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Mineral-assisted+production+of+benzene+under+hydrothermal+conditions:+Insights+from+experimental+studies+on+C6+cyclic+hydrocarbons.">Mineral-assisted production of benzene under hydrothermal conditions: Insights from experimental studies on C6 cyclic hydrocarbons.</a> Journal of Volcanology and Geothermal Research. 346, 21-27 (2017).</li><li>Lemke, K. H., Rosenbauer, R. J., Bird, D. K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Peptide+Synthesis+in+Early+Earth+Hydrothermal+Systems.">Peptide Synthesis in Early Earth Hydrothermal Systems.</a> Astrobiology. 9 (2), 141-146 (2009).</li><li>Byrappa, K., Yoshimura, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Handbook of Hydrothermal Technology. , (2001).</li><li>Johnson, J. W., Oelkers, E. H., Helgeson, H. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=SUPCRT92:+A+software+package+for+calculating+the+standard+molal+thermodynamic+properties+of+minerals,+gases,+aqueous+species,+and+reactions+from+1+to+5000+bar+and+0+to+1000&#176;C.">SUPCRT92: A software package for calculating the standard molal thermodynamic properties of minerals, gases, aqueous species, and reactions from 1 to 5000 bar and 0 to 1000&#176;C.</a> Computers &amp; Geosciences. 18 (7), 899-947 (1992).</li></ol>

本研究以硝基苯为矿物磁铁矿为例, 说明如何评价矿物对热液有机反应的影响。虽然在小型石英玻璃管中进行了实验, 但在磁铁矿实验中观察到了高重现性的结果,即30.3 1.4% 的硝基苯转化, 表明了该热液协议。在无矿物实验中, 硝基苯的转化率为 5.2, 为 2.1%, 表现出的重现性比矿物试验低。在无矿物实验中, 相对较高的不确定性可能是由于起始材料的低转换, 考虑到小管中所用样品的µL (或 mg)。?...

水热环境 (即高温和高压下的水介质) 在地球上无处不在。有机化合物的热液化学在多种地球化学环境中起着重要作用, 如有机沉积盆地、油气藏和深生物圈1、2、3。热液系统中的有机碳转化不仅发生在纯净的水介质中, 而且还与溶解或固体无机材料 (如富含地球的矿物) 相结合。矿物被发现对各种有机化合物的水热反应性有显著的选择性影响,1、4、5 , 但如何识别复杂的热液体系中的矿物效应仍然是一个挑战。本研究的目的是为研究矿物对热液有机反应的影响提供一个相对简单的实验协议。
水热反应的实验室研究传统上使用的是由金, 钛, 或不锈钢6,7,8,9制成的坚固的反应堆。例如, 金袋或胶囊已经得到了良好的使用, 因为黄金是灵活的, 它允许样品压力由外部加压水控制, 从而避免在样品内产生汽相。然而, 这些反应堆是昂贵的, 可能会与潜在的金属催化效应10。因此, 为这些热液实验寻找一种成本低但可靠性高的替代方法势在必行。
近年来, 石英或熔融石英玻璃的反应管越来越多地应用于水热实验11,12,13。与贵重的金或钛相比, 石英或二氧化硅玻璃的价格要便宜得多, 而且材料也很结实。更重要的是, 石英管显示的催化效果很少, 并且可以像金一样惰性的热液反应11,14。在本协议中, 我们描述了在厚壁石英管中进行小规模热液有机矿物实验的一般方法。我们提出一个例子实验使用模型化合物 (即硝基苯) 在存在/没有铁氧化物矿物 (即磁铁矿) 在150°c 热液溶液, 为了显示矿物作用, 并且证明此方法的有效性。

<table>
	<tbody>
		<tr>
			<td>Chemicals:</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Dichloromethane</td>
			<td>VWR</td>
			<td>BDH23373.400</td>
			<td></td>
		</tr>
		<tr>
			<td>Dodecane</td>
			<td>Sigma-Aldrich</td>
			<td>297879</td>
			<td></td>
		</tr>
		<tr>
			<td>Nitrobenzene</td>
			<td>Sigma-Aldrich</td>
			<td>252379</td>
			<td></td>
		</tr>
		<tr>
			<td>Fe2O3</td>
			<td>Sigma-Aldrich</td>
			<td>310050</td>
			<td></td>
		</tr>
		<tr>
			<td>Fe3O4</td>
			<td>Sigma-Aldrich</td>
			<td>637106</td>
			<td></td>
		</tr>
		<tr>
			<td>Supplies:</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Silica tube</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Vacuum pump</td>
			<td>WELCH</td>
			<td>2546B-01</td>
			<td></td>
		</tr>
		<tr>
			<td>Vacuum line</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Oven</td>
			<td>Hewlett Packard</td>
			<td>5890</td>
			<td></td>
		</tr>
		<tr>
			<td>Thermocouple</td>
			<td>BENETECH</td>
			<td>GM1312</td>
			<td></td>
		</tr>
		<tr>
			<td>Gas chromatography</td>
			<td>Agilent</td>
			<td>7820A</td>
			<td></td>
		</tr>
	</tbody>
</table>

an experimental protocol for studying mineral effects on organic hydrothermal transformations

有机-矿物相互作用在热液环境中广泛发生, 如温泉、陆地间歇泉和深海热液喷口。矿物在许多热液有机地球化学过程中的作用是至关重要的。传统的热液方法, 包括使用由金、钛、铂或不锈钢制成的反应堆, 通常与高成本或不想要的金属催化效应有关。近年来, 在水热实验中使用经济高效、惰性石英或熔融二氧化硅玻璃管的趋势越来越大。在此, 我们提供了一种在石英管中进行有机矿物热液实验的协议, 并描述了样品制备、实验装置、产品分离和定量分析的基本步骤。我们还演示了一个实验使用的一个模型有机化合物, 硝基苯, 以显示的影响, 含铁矿物, 磁铁矿, 对其降解在特定的水热条件下。该技术可应用于比较简单的实验室系统中复杂的有机矿物热液相互作用的研究。

为了演示如何使用这种方法来研究热液有机矿物相互作用, 一个简单的实验使用了一个模型化合物, 硝基苯, 用矿物磁铁矿 (Fe3O4) 在热液条件150°c 和52小时的酒吧。为了显示矿物效应, 在同一热液条件下, 还进行了无矿物硝基苯的实验。如图 1a所示, 在热液实验之前, 两个硅胶管是按照协议进行的。没有矿物的密封管是明确的, 与磁铁矿?...

Watch this Scientific Journal Video about An Experimental Protocol for Studying Mineral Effects on Organic Hydrothermal Transformations at JoVE.com

An Experimental Protocol for Studying Mineral Effects on Organic Hydrothermal Transformations

地球丰富的矿物在天然热液系统中起着重要的作用。本文介绍了水热条件下有机矿物相互作用实验研究的一种可靠、经济有效的方法。

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