Name: Methane Hydrate Crystallization on Sessile Water Droplets (Video) | JoVE Journal
Uploaded: 2021-05-26T15:00:00.000+00:00
Duration: 8 min 46 s
Description: Learn to form methane hydrate shells on sessile water droplets for studying crystal morphology and biomolecular interactions. This reproducible method enables safe investigation of inhibitors and promoters.

ai_agent_IP

ai_agent

maintenance

instantTrialDurationMinutes

isBiopharma

enableNewMyJoveSectionDesign

educationFeatures

seoMetaApi

ai_copilot_institution_blacklist

ai_chat_institution_blacklist

freeAccessWindow

ssoRoleCapture

scheduledMaintenanceBanner

joveLabsFeatures

disable_autoplay_for_bots

extended_trial_duration

5 minutes

NASA Exobiology grant 80NSSC19K0477 funded this research. We thank William Waite and Nicolas Espinoza for valuable discussions.

<ol><li>Bohrmann, G., Torres, M. E. Gas hydrates in marine sediments. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aBohrmann%2C+G+%22Marine+Geochemistry%22">Marine Geochemistry</a>. Schulz, H. D., Zabel, M. , Springer. Heidelberg, Germany. 481-512 (2006).</li>
<li>Ruppel, C. D., Kessler, J. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((The+interaction+of+climate+change+and+methane+hydrates%5BTitle%5D)+AND+%22Reviews+of+Geophysics%22%5BJournal%5D)">The interaction of climate change and methane hydrates.</a> Reviews of Geophysics. 55 (1), 126-168 (2017).</li>
<li>Hammerschmidt, E. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Formation+of+gas+hydrates+in+natural+gas+transmission+lines%5BTitle%5D)+AND+%22Industrial+and+Engineering+Chemistry%22%5BJournal%5D)">Formation of gas hydrates in natural gas transmission lines.</a> Industrial and Engineering Chemistry. 26, 851-855 (1934).</li>
<li>Ke, W., Kelland, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Kinetic+hydrate+inhibitor+studies+for+gas+hydrate+systems%3A+a+review+of+experimental+equipment+and+test+methods%5BTitle%5D)+AND+%22Energy+%26+Fuels%22%5BJournal%5D)">Kinetic hydrate inhibitor studies for gas hydrate systems: a review of experimental equipment and test methods.</a> Energy & Fuels. 30 (12), 10015-10028 (2016).</li>
<li>Kelland, M. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((A+review+of+kinetic+hydrate+inhibitors+from+an+environmental+perspective%5BTitle%5D)+AND+%22Energy+%26+Fuels%22%5BJournal%5D)">A review of kinetic hydrate inhibitors from an environmental perspective.</a> Energy & Fuels. 32 (12), 12001-12012 (2018).</li>
<li>Walker, V. K., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Antifreeze+proteins+as+gas+hydrate+inhibitors%5BTitle%5D)+AND+%22Canadian+Journal+of+Chemistry%22%5BJournal%5D)">Antifreeze proteins as gas hydrate inhibitors.</a> Canadian Journal of Chemistry. 93 (8), 839-849 (2015).</li>
<li>Bruusgaard, H., Lessard, L. D., Servio, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Morphology+study+of+structure+I+methane+hydrate+formation+and+decomposition+of+water+droplets+in+the+presence+of+biological+and+polymeric+kinetic+inhibitors%5BTitle%5D)+AND+%22Crystal+Growth+%26+Design%22%5BJournal%5D)">Morphology study of structure I methane hydrate formation and decomposition of water droplets in the presence of biological and polymeric kinetic inhibitors.</a> Crystal Growth & Design. 9 (7), 3014-3023 (2009).</li>
<li>Jung, J. W., Espinoza, D. N., Santamarina, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Properties+and+phenomena+relevant+to+CH4-CO2+replacement+in+hydrate-bearing+sediments%5BTitle%5D)+AND+%22Journal+of+Geophysical+Research%22%5BJournal%5D)">Properties and phenomena relevant to CH4-CO2 replacement in hydrate-bearing sediments.</a> Journal of Geophysical Research. 115 (10102), 1-16 (2010).</li>
<li>Chen, X., Espinoza, D. N. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Ostwald+ripening+changes+the+pore+habit+and+spatial+variability+of+clathrate+hydrate%5BTitle%5D)+AND+%22Fuel%22%5BJournal%5D)">Ostwald ripening changes the pore habit and spatial variability of clathrate hydrate.</a> Fuel. 214, 614-622 (2018).</li>
<li>DuQuesnay, J. R., Diaz Posada, M. C., Beltran, J. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Novel+gas+hydrate+reactor+design%3A+3-in-1+assessment+of+phase+equilibria%2C+morphology+and+kinetics%5BTitle%5D)+AND+%22Fluid+Phase+Equilibria%22%5BJournal%5D)">Novel gas hydrate reactor design: 3-in-1 assessment of phase equilibria, morphology and kinetics.</a> Fluid Phase Equilibria. 413, 148-157 (2016).</li>
<li>Udegbunam, L. U., DuQuesnay, J. R., Osorio, L., Walker, V. K., Beltran, J. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Phase+equilibria%2C+kinetics+and+morphology+of+methane+hydrate+inhibited+by+antifreeze+proteins%3A+application+of+a+novel+3-in-1+method%5BTitle%5D)+AND+%22The+Journal+of+Chemical+Thermodynamics%22%5BJournal%5D)">Phase equilibria, kinetics and morphology of methane hydrate inhibited by antifreeze proteins: application of a novel 3-in-1 method.</a> The Journal of Chemical Thermodynamics. 117, 155-163 (2018).</li>
<li>Espinoza, D. N., Santamarina, J. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Water-CO2-mineral+systems%3A+Interfacial+tension%2C+contact+angle%2C+and+diffusion+-+Implications+to+CO2+geological+storage%5BTitle%5D)+AND+%22Water+Resources+Research%22%5BJournal%5D)">Water-CO2-mineral systems: Interfacial tension, contact angle, and diffusion - Implications to CO2 geological storage.</a> Water Resources Research. 46 (7537), 1-10 (2010).</li>
<li>Sloan, E. D., Koh, C. A. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aSloan%2C+ED+%22Clathrate+Hydrates+of+Natural+Gases.+3rd+edn%22">Clathrate Hydrates of Natural Gases. 3rd edn</a>. , CRC Press. (2007).</li>
<li>Makogon, I. F. <a target="_blank" href="http://scholar.google.com/scholar?hl=en&safe=off&q=author%3aMakogon%2C+IF+%22Hydrates+of+natural+gas%22">Hydrates of natural gas</a>. , PennWell Books. Tulsa, Oklahoma, USA. 125(1981).</li>
<li>Johnson, A. M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/pubmed?term=((Mainly+on+the+plane%3A+deep+subsurface+bacterial+proteins+bind+and+alter+clathrate+structure%5BTitle%5D)+AND+%22Crystal+Growth+%26+Design%22%5BJournal%5D)">Mainly on the plane: deep subsurface bacterial proteins bind and alter clathrate structure.</a> Crystal Growth & Design. 20 (10), 6290-6295 (2020).</li>
</ol>

There are no competing financial interests.

We have developed a method to form methane hydrate shells on sessile water droplets safely and share this method to machine and assemble a pressure cell rated to 10 MPa working pressure, as well as the pressurizing and cooling systems. The pressure cell is outfitted with a stage for the droplet containing embedded thermocouples, a sapphire window for visualizing the droplet, and a pressure transducer fixed to the top of the cell. The cooling system includes chilled ethylene glycol circulating through copper coils in a ta...

Gas hydrates are cages of hydrogen-bonded water molecules that trap guest gas molecules via van der Waals interactions. Methane hydrates form under high-pressure and low-temperature conditions, which occur in nature in the subsurface sediment along continental&#160;margins, under Arctic permafrost, and on other planetary bodies in the solar system1. Gas hydrates store several thousand gigatons of carbon, with important implications for climate and energy2. Gas hydrates can also be hazardous in the natural gas industry because conditions favorable for hydrates occur in gas pipelines, which can clog the pipes leading to fatal explosions and oil spills3.
Due to the difficulty of studying gas hydrates in situ, laboratory experiments are often employed to characterize hydrate properties and the influence of inhibitors and substrates4. These laboratory experiments are performed by growing gas hydrate at elevated pressure in cells of various shapes and sizes. Efforts to prevent gas hydrate formation in gas pipelines have led to the discovery of several chemical and biological gas hydrate inhibitors, including antifreeze proteins (AFPs), surfactants, amino acids, and polyvinylpyrrolidone (PVP)5,6. To determine the effects of these compounds on gas hydrate properties, these experiments have employed diverse vessel designs, including autoclaves, crystallizers, stirred reactors, and rocking cells, which support volumes from 0.2 to 106 cubic centimeters4.
The sessile droplet method used here and in previous studies7,8,9,10,11,12 involves forming a gas hydrate film on a sessile droplet of water inside a pressure cell. These vessels are made of stainless steel and sapphire to accommodate pressures up to 10-20 MPa. The cell is connected to a methane gas cylinder. Two of these studies used the droplet method to test AFPs as gas hydrate inhibitors compared to commercial kinetic hydrate inhibitors (KHIs), such as PVP7,11. Bruusgard et al.7 focused on the morphologic influence of inhibitors and found that droplets containing Type I AFPs have a smoother, glassy surface than the dendritic droplet surface without inhibitors at high driving forces.
Udegbunam et al.11 used a method developed to assess KHIs in a previous study10, which allows for the analysis of morphology/growth mechanisms, the hydrate-liquid-vapor equilibrium temperature/pressure, and kinetics as a function of temperature. Jung et al. studied CH4-CO2 replacement by flooding the cell with CO2 after forming a CH4 hydrate shell8. Chen et al. observed Ostwald ripening as the hydrate shell forms9. Espinoza et al. studied CO2 hydrate shells on various mineral substrates12. The droplet method is a relatively simple and cheap method to determine the morphologic effect of various compounds and substrates on gas hydrates and requires small amounts of additives due to the small volume. This paper describes a method for forming such hydrate shells on a droplet of water using a stainless-steel cell with a sapphire window for visualization, rated up to 10 MPa working pressure.

<table><tbody><tr><td>&lt;strong&gt;CAMERA AND LAPTOP&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Camera Body</td><td>Nikon</td><td>D7200</td><td>Name in Protocol: camera</td></tr><tr><td>Camera Control Pro 2 Software</td><td>Nikon</td><td></td><td>Name in Protocol: camera software</td></tr><tr><td>Laptop</td><td>HP Pavilion</td><td>hp-pavilion-laptop-14-ce0068st</td><td>Needs to be PC with plenty of storage (~ 1 Tb)&lt;br/&gt; Name in Protocol: laptop</td></tr><tr><td>Macrophotography Lens</td><td>Nikon</td><td>AF-S MICRO 105mm f/2.8G IF-ED Lens</td><td>Name in Protocol: lens</td></tr><tr><td>&lt;strong&gt;CONSUMABLES&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Deionized water</td><td></td><td></td><td>Name in Protocol: DI water</td></tr><tr><td>Dry Ice</td><td>VWR or grocery store</td><td></td><td>Buy just before nucleation&lt;br/&gt; Name in Protocol: dry ice</td></tr><tr><td>Ethanol</td><td></td><td></td><td>Name in Protocol: ethanol</td></tr><tr><td>Ethylene Glycol</td><td></td><td></td><td>Name in Protocol: ethylene glycol</td></tr><tr><td>&lt;strong&gt;COOLING SYSTEM&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>1/2 in. O.D. x 3/8 in. I.D. x 25 ft. Polyethylene Tubing</td><td>Everbilt</td><td>Model # 301844</td><td>For circulating coolant from chiller to copper coils in aquarium&lt;br/&gt; Name in Protocol: 3/8&amp;rdquo; (inner diameter) plastic tubing</td></tr><tr><td>Circulating chiller</td><td>Polyscience</td><td></td><td>Name in Protocol: chiller</td></tr><tr><td>Economical Flexible Polyethylene Foam Pipe Insulation</td><td>McMaster-Carr</td><td>4530K162</td><td>3/4&quot; thick wall; 1/2&quot; inner diameter; R Value 3; 6&#039; long&lt;br/&gt; Name in Protocol: foam pipe insulation</td></tr><tr><td>Plastic tubing</td><td></td><td></td><td>use any tubing that fits the airline connection in the lab and long enough to travel from the airline connection to the front of the aquarium</td></tr><tr><td>&lt;strong&gt;DATALOGGER&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>Armature Multiplexer Module for 34970A/&lt;br/&gt; 34972A, 20-Channel</td><td>Keysight Technologies</td><td>34901A</td><td>Name in Protocol: datalogger multichannel</td></tr><tr><td>Benchvue or Benchlink software</td><td>Benchvue or Benchlink</td><td></td><td>Name in Protocol: temperature transducer software</td></tr><tr><td>Data Acquisition/Switch Unit. GPIB, RS232</td><td>Keysight Technologies</td><td>34970A</td><td>Name in Protocol: datalogger</td></tr><tr><td>USB/GPIB interface</td><td>Keysight Technologies</td><td>82357B</td><td>Name in Protocol: datalogger USB</td></tr><tr><td>datalogger multichannel</td><td></td><td></td><td></td></tr><tr><td>Schott Fostec -Llc 20510 Ace Fiber Optic Light Source</td><td>Schott Fostec</td><td>A20500</td><td>3115PS-12W-B20 115 V ~AC 50/60Hz 5/4.5 W&lt;br/&gt; Name in Protocol: light source unit</td></tr><tr><td>Schott Fostec light source guide - single bundle</td><td>Schott Fostec</td><td>A08031.40</td><td>Name in Protocol: fiber optic light source cable</td></tr><tr><td>&lt;strong&gt;METHANE GAS AND REGULATOR&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>1/4 OD in. x 20 ft. Copper Soft Refrigeration Coil</td><td>Everbilt</td><td>Model # D 04020PS</td><td>For pressurizing ISCO pressure pump. An additional pack is needed for coolant circulation, as listed below.&lt;br/&gt; Name in Protocol: high pressure-rated 1/4&amp;rdquo; copper pipe</td></tr><tr><td>Methane cylinder regulator</td><td>Airgas</td><td>Y11N114G350-AG</td><td>Name in Protocol: methane cylinder regulator</td></tr><tr><td>Methane gas cylinder</td><td>Airgas</td><td>ME UHP300</td><td>Name in Protocol: methane gas cylinder</td></tr><tr><td>&lt;strong&gt;PRESSURE PUMP&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>1/4 in.&amp;nbsp; flexible tubing, ~ 3 ft.</td><td></td><td></td><td>Connect to pump inlet for leak test&lt;br/&gt; Name in Protocol: 1/4&quot;&amp;nbsp; flexible tubing</td></tr><tr><td>260D Syringe Pump W/Controller</td><td>Teledyne Instruments Inc.</td><td>67-1240-520</td><td>Name in Protocol: pressure pump</td></tr><tr><td>Controller &amp;minus; Ethernet/USB</td><td>Teledyne Instruments Inc.</td><td>62-1240-114</td><td>Purchase if you would like to install Labview onto computer and control pressure pump remotely. We did not do this.</td></tr><tr><td>Smooth-Bore Seamless 316 Stainless Steel Tubing, 1/4&quot; OD, 0.035&quot; Wall Thickness, 1 Foot Long (x5)</td><td>McMaster-Carr</td><td>89785K824</td><td>Name in Protocol: 1/4&quot; pipe</td></tr><tr><td>Smooth-Bore Seamless 316 Stainless Steel Tubing, 1/8&quot; OD, 0.02&quot; Wall Thickness, 1 Foot Long (x4)</td><td>McMaster-Carr</td><td>89785K811</td><td>Name in Protocol: 1/8&quot; pipe</td></tr><tr><td>Stainless Steel Swagelok Tube Fitting, Reducing Union, 1/4 in. x 1/8 in. Tube OD (x4)</td><td>Swagelok</td><td>&amp;nbsp;SS-400-6-2</td><td>Name in Protocol: 1/8&amp;rdquo; to 1/4&amp;rdquo; adapter</td></tr><tr><td>&lt;strong&gt;PRESSURE CELL&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>316 Stainless Steel Nut and Ferrule Set (1 Nut/1 Front Ferrule/1 Back Ferrule) for 1/4 in. Tube Fitting (20)</td><td>Swagelok</td><td>&amp;nbsp;SS-400-NFSET</td><td>Used for fitting connections where necessary&lt;br/&gt; Name in Protocol: ferrule set</td></tr><tr><td>316L Stainless Steel Convoluted (FM) Hose, 1/4 in., 316L Stainless Steel Braid, 1/4 in. Tube Adapters, 60 in. (1.5 m) Length</td><td>Swagelok</td><td>SS-FM4TA4TA4-60</td><td>Connects pressure pump to pressure cell&lt;br/&gt; Name in Protocol: 1/4&quot; braided stainless steel flexible pressure-rated hose</td></tr><tr><td>ABAQUS</td><td>ABAQUS FEA</td><td></td><td>Name in Protocol: simulation software</td></tr><tr><td>Abrasion-Resistant Cushioning Washer for 7/8&quot; Screw Size, 0.875&quot; ID, 2.25&quot; OD, packs of 10 (x1)</td><td>McMaster-Carr</td><td>90131A107</td><td>Name in Protocol: 2.25&quot; rubber washer</td></tr><tr><td>Abrasion-Resistant Sealing Washer, Aramid Fabric/Buna-N Rubber, 3/8&quot; Screw Size, 0.625&quot; OD, packs of 10 (x1)</td><td>McMaster-Carr</td><td>93303A105</td><td>Used for illumination port</td></tr><tr><td>Acrylic Sheet | White 2447 / WRT31&lt;br/&gt; Extruded Paper-Masked (Translucent 55% (0.118 x 12 x 12)</td><td>Interstate Plastics</td><td>ACRW7EPSH</td><td>Machine a circle of acrylic to fit in the inner chamber of the pressure cell to serve as the background for imaging&lt;br/&gt; Name in Protocol: acrylic disc</td></tr><tr><td>AutoCAD</td><td>AutoCAD</td><td></td><td>Name in Protocol: engineering design software</td></tr><tr><td>Conax fitting</td><td>Conax Technologies</td><td>311401-011</td><td>TG(PTM2/)-24-A6-T, OPTIONAL 1/4&quot; NPT&lt;br/&gt; Name in Protocol: pressure seal connector</td></tr><tr><td>High Accuracy Oil Filled Pressure&lt;br/&gt; Transducers/Transmitters for General&lt;br/&gt; industrial applications (x2)</td><td>Omega Engineering, Inc.</td><td>PX409-3.5KGUSBH</td><td>Buy two so there is a backup.&lt;br/&gt; Name in Protocol: pressure transducer</td></tr><tr><td>HIGH PRESSURE CHAMBER&amp;nbsp; PARTS</td><td>Wither Tool, Die and Manufacturing Company</td><td></td><td>Machining for pressure cell parts as listed in CAD drawings (Figure S1)&lt;br/&gt; Name in Protocol: Part B = stainless steel washer</td></tr><tr><td>High-Strength 316 Stainless Steel Socket Head Screw, M5 x 0.80 mm Thread, 14 mm Long (x20)</td><td>McMaster-Carr</td><td>90037A119</td><td>Used for illumination port</td></tr><tr><td>High-Strength 316 Stainless Steel Socket Head Screw, M8 x 1.25 mm Thread, 25 mm Long (x20)</td><td>McMaster-Carr</td><td>90037A133</td><td>Name in Protocol: M8 stainless steel screws</td></tr><tr><td>Oil-Resistant Hard Buna-N O-Ring, 3/32 Fractional Width, Dash Number 120, packs of 50 (x1)</td><td>McMaster-Carr</td><td>5308T178</td><td>Name in Protocol: 1&quot; o-ring</td></tr><tr><td>Oil-Resistant Hard Buna-N O-Ring, 3/32 Fractional Width, Dash Number 128, packs of 50 (x1)</td><td>McMaster-Carr</td><td>5308T186</td><td>Name in Protocol: 1.5&quot; o-ring</td></tr><tr><td>Omega Inc. pressure transducer software</td><td>Omega Engineering, Inc.</td><td></td><td>Name in Protocol: pressure transducer software</td></tr><tr><td>Polycarbonate Disc</td><td>McMaster-Carr</td><td>8571K31</td><td>Listed in CAD drawings for illumination port, Fig. S1 Part E</td></tr><tr><td>Sapphire windows (x3)</td><td>Guild Optical Associates, Inc.</td><td>Optical Grade Sapphire Window, C-Plane&lt;br/&gt; Diameter: 1.811&amp;rdquo; &amp;plusmn;.005&amp;rdquo;&lt;br/&gt; Thickness: .590&amp;rdquo; &amp;plusmn;.005&amp;rdquo;&lt;br/&gt; Surface Quality: 60/40&lt;br/&gt; Edges ground and safety chamfered</td><td>Buy three so there are two backups.&lt;br/&gt; Name in Protocol: sapphire window</td></tr><tr><td>Solid Thermocouple Wire FEP Insulation and Jacket, Type K, 24 Gauge, 50 ft. Length (x1)</td><td>McMaster-Carr</td><td>3870K32</td><td>Name in Protocol: thermocouples</td></tr><tr><td>Stainless Steel Integral Bonnet Needle Valve, 0.37 Cv, 1/4 in. Swagelok Tube Fitting, Regulating Stem (x4)</td><td>Swagelok</td><td>&amp;nbsp;SS-1RS4</td><td>Two will be used for the pressure pump as well.&lt;br/&gt; Name in Protocol: 1/4&quot; needle valves</td></tr><tr><td>Stainless Steel Pipe Fitting, Hex Nipple, 1/4 in. Male NPT (x2)</td><td>Swagelok</td><td>&amp;nbsp;SS-4-HN</td><td>Used for illumination port</td></tr><tr><td>Stainless Steel Swagelok Tube Fitting, Female Branch Tee, 1/4 in. Tube OD x 1/4 in. Tube OD x 1/4 in. Female NPT (x2)</td><td>Swagelok</td><td>&amp;nbsp;SS-400-3-4TTF</td><td>Used with pressure transducer&lt;br/&gt; Name in Protocol: branch tee fitting</td></tr><tr><td>Stainless Steel Swagelok Tube Fitting, Male Connector, 1/4 in. Tube OD x 1/4 in. Male NPT (x4)</td><td>Swagelok</td><td>&amp;nbsp;SS-400-1-4</td><td>Used on top port and side port leading to needle valves&lt;br/&gt; Name in Protocol: NPT screws</td></tr><tr><td>Stainless Steel Swagelok Tube Fitting, Port Connector, 1/4 in. Tube OD (x8)</td><td>Swagelok</td><td>&amp;nbsp;SS-401-PC</td><td>Use as tube connections between NTP and valve connections&lt;br/&gt; Name in Protocol: port connector fitting</td></tr><tr><td>&lt;strong&gt;TANK&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>1/4 OD in. x 20 ft. Copper Soft Refrigeration Coil</td><td>Everbilt</td><td>Model # D 04020PS</td><td>For circulating coolant&lt;br/&gt; Name in Protocol: 1/4&quot; copper pipe</td></tr><tr><td>10 gallon aquarium</td><td>Tetra</td><td></td><td>Name in Protocol: 10 gallon tank</td></tr><tr><td>2 oz. Waterweld</td><td>J-B Weld</td><td>Model # 8277</td><td>Name in Protocol: underwater sealant</td></tr><tr><td>3 in. x 25 ft. Foil Backed Fiberglass Pipe Wrap Insulation</td><td>Frost King</td><td>Model # SP42X/16</td><td>For wrapping around aquarium&lt;br/&gt; Name in Protocol: foil-lined fiberglass</td></tr><tr><td>3/8 7/8 in. Stainless Steel Hose Clamp (10 pack)</td><td>Everbilt</td><td>Model # 670655E</td><td>Name in Protocol: worm drive hose clamps</td></tr><tr><td>Styrofoam</td><td></td><td></td><td>Name in Protocol: insulating material</td></tr><tr><td>&lt;strong&gt;TOOLS&lt;/strong&gt;</td><td></td><td></td><td></td></tr><tr><td>1-1/8 in. Ratcheting Tube Cutter</td><td>Husky</td><td>Model # 86-036-0111</td><td></td></tr><tr><td>1/2 in. to 1 in. Pipe Cutter</td><td>Apollo</td><td>Model # 69PTKC001</td><td></td></tr><tr><td>Adjustable wrench (x2)</td><td>Steel Core</td><td>Model # 31899</td><td>Need two wrenches with jaw at least 1&quot;</td></tr><tr><td>Allen wrench set</td><td>Home Depot</td><td></td><td></td></tr><tr><td>Duct tape</td><td></td><td></td><td>Name in Protocol: duct tape</td></tr><tr><td>Flexible tubing, like an IV line, to fit on the end of grainger probe (canula)</td><td></td><td></td><td>Name in Protocol: IV tube</td></tr><tr><td>Grainger 18 gauge probe</td><td>Grainger</td><td></td><td>For inserting droplet&lt;br/&gt; Name in Protocol: cannula</td></tr><tr><td>High Vacuum Grease</td><td>Dow corning</td><td></td><td>Apply to o-rings before inserting sapphire window&lt;br/&gt; Name in Protocol: vacuum grease</td></tr><tr><td>Klein Tools Professional 90 Degree 4-in-1 Tube Bender</td><td>Klein Tools</td><td>Model # 89030</td><td>Name in Protocol: tube bender</td></tr><tr><td>Snoop liquid leak detector</td><td>Swagelok</td><td>MS-SNOOP-8OZ</td><td>To detect leaks when pressurized when methane&lt;br/&gt; Name in Protocol: liquid leak detector</td></tr><tr><td>Suction cup</td><td>Home Depot</td><td></td><td>For removing tight fitting sapphire window&lt;br/&gt; Name in Protocol: suction cup</td></tr><tr><td>Teflon Tape</td><td></td><td></td><td>Name in Protocol: plumber&#039;s tape</td></tr><tr><td>Temflex 3/4 in. x 60 ft. 1700 Electrical Tape Black</td><td>3M</td><td>Model # 1700-1PK-BB40</td><td>Name in Protocol: electrical tape</td></tr></tbody></table>

methane hydrate crystallization on sessile water droplets

Methane Hydrate Crystallization on Sessile Water Droplets

This paper describes a method to form methane hydrate shells on water droplets. In addition, it provides blueprints for a pressure cell rated to 10 MPa working pressure, containing a stage for sessile droplets, a sapphire window for visualization, and temperature and pressure transducers. A pressure pump connected to a methane gas cylinder is used to pressurize the cell to 5 MPa. The cooling system is a 10 gallon (37.85 L) tank containing a 50% ethanol solution cooled via ethylene glycol through copper coils. This setup enables the observation of the temperature change associated with hydrate formation and dissociation during cooling and depressurization, respectively, as well as visualization and photography of the morphologic changes of the droplet. With this method, rapid hydrate shell formation was observed at ~-6 &#176;C to -9 &#176;C. During depressurization, a 0.2 &#176;C to 0.5 &#176;C temperature drop was observed at the pressure/temperature (P/T) stability curve due to exothermic hydrate dissociation, confirmed by visual observation of melting at the start of the temperature drop. The "memory effect" was observed after repressurizing to 5 MPa from 2 MPa. This experimental design allows the monitoring of pressure, temperature, and morphology of the droplet over time, making this a suitable method for testing various additives and substrates on hydrate morphology.

With this method, a gas hydrate shell on a droplet can be monitored visually through a sapphire window of the pressure cell and via temperature and pressure transducers. To nucleate the hydrate shell after pressurizing to 5 MPa, dry ice can be added to the top of the pressure cell to induce a thermal shock to trigger rapid hydrate crystallization. There is a clear morphologic difference upon dry ice-forced hydrate shell formation. The water droplet transitioned from a smooth, reflective surface (Figu...

We describe a method to form gas hydrate on sessile water droplets to study the effects of various inhibitors, promoters, and substrates on the hydrate crystal morphology.

This paper describes a method to form methane hydrate shells on water droplets. In addition, it provides blueprints for a pressure cell rated to 10 MPa ...

methane-hydrate-crystallization-on-sessile-water-droplets

Research

JoVE Journal

Environment

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

We present a protocol for measuring the thermal properties of synthetic hydrate-bearing sediment samples comprising sand, water, methane, and methane hydrate.

Protocol for Measuring the Thermal Properties of a Supercooled Synthetic Sand-water-gas-methane Hydrate Sample

Here, we present a general protocol to prepare a variety of microhoneycomb monoliths (MHMs) in which fluid can pass through with an extremely low pressure drop. MHMs obtained are expected to be used as filters, catalyst supports, flow-type electrodes, sensors and scaffolds for biomaterials.

Microhoneycomb Monoliths Prepared by the Unidirectional Freeze-drying of Cellulose Nanofiber Based Sols: Method and Extensions

We present a protocol to study the formation of hydrates in the presence of nonionic surfactants on the interface of a water droplet submerged in cyclopentane. The protocol consists of building a low-cost, programmable, temperature regulator. The temperature control system is combined with visualization techniques and internal pressure measurements.

Studying Surfactant Effects on Hydrate Crystallization at Oil-Water Interfaces Using a Low-Cost Integrated Modular Peltier Device

The atmospheric concentrations of weakly bound molecular clusters can be computed from the thermochemical properties of low energy structures found through a multi-step configurational sampling methodology utilizing a genetic algorithm and semi-empirical and ab initio quantum chemistry.

Computation of Atmospheric Concentrations of Molecular Clusters from ab initio Thermochemistry

The present protocol describes the crystallization of microscopic ice crystals and clathrate hydrates in microfluidic devices, enabling liquid exchange around the formed crystals. This provides unparalleled possibilities to examine the crystallization process and binding mechanisms of the inhibitors.

A Microfluidic Approach for the Study of Ice and Clathrate Hydrate Crystallization

Lake eutrophication is a water quality issue worldwide, making the need to identify and control nutrient sources critical. Laboratory determination of phosphorus release rates from sediment cores is a valuable approach for determining the role of internal phosphorus loading and guiding management decisions.

Laboratory-determined Phosphorus Flux from Lake Sediments as a Measure of Internal Phosphorus Loading

EPA Method 1615 uses an electropositive filter to concentrate enteroviruses and noroviruses in environmental and drinking waters. This manuscript describes the procedure for collecting samples for Method 1615 analyses.

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. I. Collection of Virus Samples

Here we present a procedure to quantify enterovirus and norovirus in environmental and drinking waters using reverse transcription-quantitative PCR. Mean virus recovery from groundwater with this standardized procedure from EPA Method 1615 was 20% for poliovirus and 30% for murine norovirus.

EPA Method 1615. Measurement of Enterovirus and Norovirus Occurrence in Water by Culture and RT-qPCR. Part III. Virus Detection by RT-qPCR

The Lysimeter Carbon Dioxide Gradient Facility creates a 250 to 500 µl L-1 linear carbon dioxide gradient in temperature-controlled chambers housing grassland plant communities on clay, silty clay, and sandy soil monoliths. The facility is used to determine how past and future carbon dioxide levels affect grassland carbon cycling.

A CO2 Concentration Gradient Facility for Testing CO2 Enrichment and Soil Effects on Grassland Ecosystem Function

Learn to form methane hydrate shells on sessile water droplets for studying crystal morphology and biomolecular interactions. This reproducible method enables safe investigation of inhibitors and promoters.

Methane Hydrate Crystallization on Sessile Water Droplets

Explore More Videos