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

We thank the H.O.G. group at Arizona State University for developing the initial methodology of these hydrothermal experiments, and in particular, we thank I. Gould, E. Shock, L. Williams, C. Glein, H. Hartnett, K. Fecteau, K. Robinson, and C. Bockisch, for their guidance and helpful assistance. Z. Yang and X. Fu were funded by startup funds from Oakland University to Z. Yang.

1. Prepare the Sample for Hydrothermal Experiment
<ol>
	<li>Choose the size of the quartz or silica glass tubes, e.g., 2 mm inner diameter (ID) x 6 mm outer diameter (OD) or 6 mm ID x 12 mm OD, and determine the amounts of organic compounds and minerals to use. In this work, the amounts of nitrobenzene and magnetite (Fe3O4) to load into the silica tube (e.g., 2 mm ID x 6 mm OD) are 3.0 &#181;L and 13.9 mg, respectively. 
	NOTE: The large diameter tubes allow easier loading o...

<ol>
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In this study, we used nitrobenzene with mineral magnetite as an example to demonstrate how to evaluate mineral effects on hydrothermal organic reactions. Although the experiments are carried out in small silica glass tubes, highly reproducible results are observed in the magnetite experiments, i.e., 30.3 &#177; 1.4% in nitrobenzene conversion, which suggests the effectiveness and the reliability of this hydrothermal protocol. In the no-mineral experiments, the conversion of nitrobenzene is 5.2 &#177; 2.1%, whic...

Hydrothermal environments (i.e., aqueous media at elevated temperatures and pressures) are ubiquitous on Earth. The hydrothermal chemistry of organic compounds plays an essential role in a wide range of geochemical settings, such as organic sedimentary basins, petroleum reservoirs, and the deep biosphere1,2,3. Organic carbon transformations in hydrothermal systems occur not only in pure aqueous medium but also with dissolved or solid inorganic materials, such as Earth-abundant minerals. Minerals have been found to dramatically and selectively influence the hydrothermal reactivity of various organic compounds,1,4,5 but how to identify the mineral effects in complex hydrothermal systems still remains as a challenge. The goal of this study is to provide a relatively simple experimental protocol for studying mineral effects on hydrothermal organic reactions.
The laboratory studies of hydrothermal reactions traditionally use robust reactors that are made of gold, titanium, or stainless steel6,7,8,9. For example, gold bags or capsules have been favorably used, because gold is flexible, and it allows the sample pressure to be controlled by pressurizing water externally, which avoids generating a vapor phase inside the sample. However, these reactors are expensive and could be associated with potential metal catalytic effects10. Hence, it is imperative to find an alternative method with low cost but high reliability for these hydrothermal experiments.
In recent years, reaction tubes made of quartz or fused silica glass have been more frequently applied to hydrothermal experiments11,12,13. Compared to precious gold or titanium, quartz or silica glass is considerably cheaper but also the strong material. More importantly, quartz tubes have shown little catalytic effects and can be as inert as gold for the hydrothermal reactions11,14. In this protocol, we describe a general method for conducting small-scale hydrothermal organic-mineral experiments in thick-walled silica tubes. We present an example experiment using a model compound (i.e., nitrobenzene) in the presence/absence of an iron-oxide mineral (i.e., magnetite) in a 150 &#176;C hydrothermal solution, in order to show the mineral effect, as well as to demonstrate the effectiveness of this method.

<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

Organic-mineral interactions are widely occurring in hydrothermal environments, such as hot springs, geysers on land, and the hydrothermal vents in the deep ocean. Roles of minerals are critical in many hydrothermal organic geochemical processes. Traditional hydrothermal methodology, which includes using reactors made of gold, titanium, platinum, or stainless-steel, is usually associated with the high cost or undesired metal catalytic effects. Recently, there is a growing tendency for using the cost-effective and inert quartz or fused silica glass tubes in hydrothermal experiments. Here, we provide a protocol for carrying out organic-mineral hydrothermal experiments in silica tubes, and we describe the essential steps in the sample preparation, experimental setup, products separation, and quantitative analysis. We also demonstrate an experiment using a model organic compound, nitrobenzene, to show the effect of an iron-containing mineral, magnetite, on its degradation under a specific hydrothermal condition. This technique can be applied to study complex organic-mineral hydrothermal interactions in a relatively simple laboratory system.

To demonstrate how to use this approach to study hydrothermal organic-mineral interactions, a simple experiment using a model compound, nitrobenzene, was conducted with mineral magnetite (Fe3O4) at a hydrothermal condition of 150 &#176;C and 5 bars for 2 h. To show the mineral effect, an experiment of nitrobenzene without mineral was also performed under the same hydrothermal condition. As shown in Figure 1a, two silica tubes were made f...

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

Earth-abundant minerals play important roles in the natural hydrothermal systems. Here, we describe a reliable and cost-effective method for the experimental investigation of organic-mineral interactions under hydrothermal conditions.

Organic-mineral interactions are widely occurring in hydrothermal environments, such as hot springs, geysers on land, and the hydrothermal vents in the ...

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