Name: safe use of pressure vessels in chemistry
Uploaded: 2023-04-30T06:59:15.000Z
Duration: 5 min 56 s
Channel: JoVE

K12 Standards

Texas Essential Knowledge and Skills

High School

Chemistry

CHEM.1

CHEM.1.C

operation-of-high-pressure-reactor-vessels

Operation of High-pressure Reactor Vessels

The operation of the high-pressure Parr reactor (or equivalent) can be roughly broken down into 3 steps.
1. Charging
<ol>
	<li>Select an appropriate secondary reaction vessel based on the scale of the reaction. Test tubes, Erlenmeyer flasks, or round-bottom flasks are some examples of appropriate reaction vessels. Make sure to keep enough head space above the solvent level in the flask as the solvent tends to bubble up during pressure venting.</li>
	<li>Place the reactants, along with a stir bar, in the reaction vessel and place it in the high-pressure reactor.</li>
	<li>Place the pressure gauge assembly on the top of the reaction vessel. Make sure the vent valve is completely closed. Turn it clockwise to finger tight. Do not overtighten.</li>
	<li>Assemble the split rings on the vessel.</li>
	<li>Start tightening the diagonally opposite screws on the split rings, but do not tighten them all the way. This is to ensure that the pressure exerted by the gauge is even across the vessel.</li>
	<li>Tighten all screws completely.</li>
	<li>Place the safety ring on the bench, and place the reactor in the ring.</li>
	<li>Slide the ring up to the split rings, and align the screw with the dent on the side of the split ring.</li>
	<li>Finger tighten the safety ring.</li>
	<li>The vessel is now ready for the next stage.</li>
</ol>
2. Purging and Pressurizing
<ol>
	<li>Attach the pressurized gas source to the reactor and turn on the main valve on the regulator.</li>
	<li>Set the pressure to approximately 1/3rd of the final required pressure.</li>
	<li>Slowly open the vent valve on the pressure gauge and pressurize the reactor.</li>
	<li>Now close the main valve on the gas regulator.</li>
	<li>Slowly loosen the pressure line going in to the reactor, so that the pressure in the reactor starts to fall. Make sure the reactor is in a well-ventilated area.</li>
	<li>Once the pressure falls back to zero, tighten the pressure line again, and open the main valve on the gas regulator.</li>
	<li>Adjust the pressure to 2/3 of the final required pressure and repeat steps 3-6 above.</li>
	<li>Now adjust the pressure on the regulator to the final desired value and pressurize the reactor.</li>
	<li>Once the final pressure is reached, close the vent valve on the pressure gauge, and close the main valve on the gas regulator.</li>
	<li>Carefully loosen the pressure line, so that the gas in the line and the regulator is vented.</li>
	<li>Always set the outlet pressure on the gas regulator back to zero (this usually means loosening the pressure control valve). This ensures that gas will not leak, even if the main valve on the regulator is turned on by accident.</li>
	<li>Now place the reactor in a hood and let the reaction run for the desired amount of time. The reactor can be heated if desired. Ensure the temperature is below the rated limit of the vessel.</li>
</ol>
3. Venting
<ol>
	<li>Once the reaction time is over, cool the reactor to room temperature, if necessary.</li>
	<li>Now slowly open the vent valve on the gauge to vent the gas from the reactor. Do this as slowly as possible to prevent the solvent spilling over in the reactor. Crucially, make sure the reactor is in a fume hood.</li>
	<li>Once the pressure in the reactor drops to zero, loosen the safety ring and the screws on the split rings.</li>
	<li>Disassemble the split rings and remove the gauge from the reactor.</li>
	<li>Remove the reaction vessel from the reactor.</li>
	<li>Once the reaction vessel is removed from the reactor, rinse the reactor with water and then acetone and leave it open to dry.</li>
</ol>

The manipulation of gases at high pressure can be done with the use of a Parr reactor (or equivalent) vessel. Proper safety precautions should be observed while operating these vessels as they present an explosion hazard.

operation of high-pressure reactor vessels

Robert M Rioux, Pennsylvania State University, University Park, PA
The use of gases in a synthetic chemistry laboratory is essential for carrying out a variety of highly facile and atom economical transformations. Reactions such as hydrogenation, oxidation, and amination require the use of gases like hydrogen, oxygen, and ammonia. Due to the poor solubility of these gases in typical reactant solutions, high pressures are necessary to achieve a meaningful reaction rate. Not only are these gases highly reactive, the use of high pressures makes these operations fairly hazardous. The biggest challenge in the use of high pressure is the containment of the high-pressure gas for the entire duration of the reaction, with close monitoring of the pressure and temperature, to avoid the formation of explosive mixtures and runaway reactions.
These reactions are typically carried out using thick-walled pressure vessels. The pressurized vessel allows for operation at high pressure with appropriate safety concerns abated. Figure 1 demonstrates the various parts of a typical pressure vessel, used to conduct high-pressure reactions. The following protocol highlights the procedure for the safe operation of these high-pressure reactor vessels.
<img alt="High-pressure reactor setup diagram; features pressure gauge, vent valves, safety ring for experiments." src="/files/ftp_upload/10400/10400fig1.jpg" data-altupdatedat="1761830439000" data-alt="Figure 1"> 
Figure 1. (a) Parts of the high pressure reactor vessel. (b) Assembled high pressure reactor vessel.

Robert M Rioux, Pennsylvania State University, University Park, PA
The use of gases in a synthetic chemistry laboratory is essential for carrying out a ...

The use of gases in the synthetic chemistry laboratory is essential for carrying out a variety of highly facile and atom economical transformations, and often require high pressures to ensure sufficient solubility of gases into the reactant solution.Reactions such as hydrogenation, oxidation, and amination require the use of gases like hydrogen, oxygen, and ammonia, respectively. Due to the poor solubility of these gases in typical reactant solutions, high pressures are necessary to achieve a meaningful reaction rate. Therefore, high-pressure reactor vessels - thick-walled containers, typically made of stainless steel - are used to carry out such reactions. The pressurized vessel allows for operation at high pressure with appropriate safety concerns abated.In this video, we will first review the safety considerations and then learn how to charge, purge, and vent a high-pressure reactor vessel. High-pressure reactor vessels can maintain environments of 3,000 PSI and 500 degrees. Vessels rated for higher pressures require thicker walls, though, making temperature control more difficult.The manufacturer's limits must be maintained during operation, as the gases are highly reactive, as

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safe use of pressure vessels in chemistry

High-pressure reactor vessels are used in synthetic chemistry to handle gases safely during reactions. They help chemists carry out gas-based processes such as hydrogenation, oxidation, and amination. These reactions often use hydrogen, oxygen, or ammonia, which are important reagents in the lab.

These gases usually dissolve poorly in standard reaction mixtures. Because of that, high pressure is needed to make the reaction proceed at a useful rate. The vessel creates a sealed space that keeps the gas inside for the full reaction time.

Working at high pressure brings added safety concerns. The gases are highly reactive, and pressure must be watched closely along with temperature. Careful monitoring helps reduce the risk of explosive mixtures and runaway reactions.

High-pressure reactions are typically done in thick-walled pressure vessels. These vessels are built to contain the gas under pressure while improving safety during the procedure. The protocol shown here focuses on the safe operation of these high-pressure reactor vessels and the main parts of a typical assembled system.

Safe Use of Pressure Vessels in Chemistry

safe-use-of-pressure-vessels-in-chemistry

proper personal protective equipment

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High-pressure reactor vessels are used in synthetic chemistry to handle gases safely during reactions. They help chemists carry out gas-based processes such as hydrogenation, oxidation, and amination. These reactions often use hydrogen, oxygen, or ammonia, which are important reagents in the lab. These gases usually dissolve poorly in standard reaction mixtures. Because of that, high pressure is needed to make the reaction proceed at a useful rate. The vessel creates a sealed space that keeps...

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Learn how high-pressure reactor vessels support gas-based chemistry, including hydrogenation, oxidation, and amination, with safety and pressure control.

Safe Use of Pressure Vessels in Chemistry | JoVE K12

Chemistry and Physics

IPC.1

IPC.1.C

Robert Rioux

Overview

Safety Considerations

Charging the Vessel

Purging and Pressurizing the Vessel

Venting the Vessel

Summary

Scientific Laws and Theories

Scientific Laws

In science, a law is defined as a concise, verbal or mathematical, statement that summarizes a vast number of experimental observations. ...

The Scientific Method

Chemistry is an empirical science. Scientists often pose questions to understand the chemistry in everyday life and seek answers to these questions. To ...

CHEM.1.A

What is an Experiment?

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Study Design in Statistics

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Experimental Designs

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Randomized Experiments

The randomization process involves assigning study participants randomly to experimental or control groups based on their probability of being equally ...

Crossover Experiments

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Controls in Experiments

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CHEM.1.B

Proper Personal Protective Equipment

Robert M. Rioux &#38; William A Elliott, Pennsylvania State University, University Park, PA
Hazards are many and varied in the laboratory, but the right ...

Emergency Eyewash and Shower Stations

Robert M. Rioux, Pennsylvania State University, University Park, PA
The Occupational Safety and Health Administration (OSHA) mandates that an emergency ...

Electrical Safety

Robert M. Rioux &amp; Suprita Jharimune, Pennsylvania State University, University Park, PA
Among the many hazards present in the laboratory, electrical ...

Working with Centrifuges

Source: Robert M. Rioux &amp; Suprita Jharimune, Pennsylvania State University, University Park, PA
Earth's gravitational force is capable of separating ...

Working with Hot and Cold Sources

Source: Robert M. Rioux &amp; Suprita Jharimune, Pennsylvania State University, University Park, PA
Working with extreme temperatures, both high and low, ...

Guidelines in Case of a Laboratory Emergency

Robert M. Rioux &amp; Zhifeng Chen, Pennsylvania State University, University Park, PA
The most common laboratory emergencies include chemical spills, ...

Chemical Storage: Categories, Hazards And Compatibilities

Source: Robert M. Rioux &amp; Taslima A. Zaman, Pennsylvania State University, University Park, PA
While the use of various chemicals in experimental ...

Safe Handling of Mineral Acids

Source: Robert M. Rioux &#38; Taslima A. Zaman, Pennsylvania State University, University Park, PA
A mineral acid (or inorganic acid) is defined as a ...

Handling Chemical Spills

Source: Robert M. Rioux &#38; Taslima Zaman, Pennsylvania State University, University Park, PA
Since chemicals are commonly used for laboratory research ...

Proper Use of Autoclaves

Robert M. Rioux &amp; Zhifeng Chen, Pennsylvania State University, University Park, PA
Autoclaving is one of the most commonly used methods in the ...

Fume Hoods and Laminar Flow Cabinets

Robert M. Rioux &amp; William A. Elliott, Pennsylvania State University, University Park, PA
Fume hoods and laminar flow cabinets are engineering controls ...

Handling Air- and Water-Sensitive Chemicals Using a Schlenk Line

Robert M Rioux, Ajay Sathe, Zhifeng Chen, Pennsylvania State University, University Park, PA
The use of reagents sensitive to oxidation or moisture ...

Proper Operation of Vacuum Based Equipment

Source: Robert M. Rioux, Ajay Sathe &#38; Zhifeng Chen, Pennsylvania State University, University Park, PA
Vacuum is required for a number of laboratory ...

Operating the Glovebox

Robert M Rioux, Ajay Sathe, Zhifeng Chen, Pennsylvania State University, University Park, PA 
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CHEM.1.D

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CHEM.1.E

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Pareto Chart

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CHEM.1.F

Scientific and engineering practices. The student, for at least 40% of instructional time, asks questions, identifies problems, and plans and safely conducts classroom, laboratory, and field investigations to answer questions, explain phenomena, or design solutions using appropriate tools and models. The student is expected to:

Safe Use of Pressure Vessels in Chemistry

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