Embedded Files
Staff Contact: Rachel Alvelais (ralvelais@lbl.gov)
Instrument Location: 67-4203A
Safety Points
Safety Points
The videos provided here offer guidance and are not a replacement for on-the-job training.
You must be authorized to work under two WPC activities: "Work on 4th Floor" (MF-0001) and "Pressure Reactors" (MF-0015).
A completed and approved ISM form is required.
Never use the hydrothermal vessel without a pre-treated, correctly fitting Teflon liner
Only run hydrothermal reactions in the oven in fume hood in 4209 in case of gas venting
Never use perchloric acid or hydrofluoric acid in the hydrothermal reactor
Never combine fats, fatty acids, glycerin, or cellulosic materials with nitric acid in the vessel – these can produce nitro compounds which are highly explosive
Minimize explosion risk by doing the following:
Stay under the maximum temperature (250 C)
Recheck calculations to assure that if your reaction goes to completion the pressure remains below 1800 psig
Never tighten the reactor cap more than 1/8th of a turn beyond hand tight
Replace the two thin metal discs (corrosion and rupture discs) if they are damaged
Replace the Teflon liner if it becomes warped or deformed in any way
Pressure Calculations (Reactor Chemistry)
Pressure Calculations (Reactor Chemistry)
This video describes the chemical, pressure, and temperature requirements when using a 45mL Parr reactor (model #4744). It shows how to evaluate potential reactions by walking the viewer through an example of how to calculate the maximum pressure of a reaction, which assumes that the starting materials go into the gaseous state at the intended temperature. Remember that the Parr reactors used here will vent above 1800psi in an attempt to stop a potential explosion.
Standard Operating Procedure
Standard Operating Procedure
This video explains how to properly assemble the 45mL Parr pressure reactor. It also describes exactly how the spring and cap work to vent any over-pressurized reactions. While you must make every possible effort to ensure that you stay below 1800psi, this ability to vent is a safety feature that offers a layer of protection unavailable in closed systems (which are not allowed at the lab).
COMMON QUESTIONS
COMMON QUESTIONS
Q: The foils I use on the top of the Teflon liner are wrinkled, what do I do?
Q: The foils I use on the top of the Teflon liner are wrinkled, what do I do?
A: There are usually replacement rupture and pressure discs in the box next to the Parr set-up in room 4209 (by the window). If you do not see any unopened packages then reach out to the staff contact listed at the top of this page. DO NOT run using torn or wrinkled discs.
Q: My pressure calculations show that I'll hit 1805psi, is this close enough to run?
Q: My pressure calculations show that I'll hit 1805psi, is this close enough to run?
A: Nope! You absolutely must keep your pressure below 1800psi.
Q: My pressure calculations are too high. What can I do to lower my calculated pressure?
Q: My pressure calculations are too high. What can I do to lower my calculated pressure?
A: There are several things that you can try. Keep in mind the gas law: P=nRT/V. Our volume is fixed at 45mL with this particular reactor type, but you can reduce the temperature or reduce the amount of material you are using in the reactor.
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