Although Parr equipment is quite popular, I prefer Autoclave Engineers.

http://www.autoclave.com/
http://www.autoclaveengineers.com/

Dave Lane
Principal
Clavis Technology Development

On 8/28/19 3:15 PM, Yaritza Brinker wrote:
> Hi Jeff,
>
>
>
> I‰??ve purchased and used pressure bombs. The models I‰??ve used are bigger‰?|
> 1L vessels with pressure gauge and temp probe. However, I do know that
> Parr offers PTFE lined small vessels with Safety Blow-Off that can be
> used as hydrothermal reactors.
>
>
>
> https://www.parrinst.com/products/sample-preparation/
>
> https://www.parrinst.com/download/37527/
>
>
>
> Here‰??s what I learned from using the 1L capacity‰?|
>
> * It is safer to spend the extra money and go for a model with a
> Pressure Gauge.
> o `This will help you ensure that‰?|
> + you don‰??t over pressurize the system
> + you don‰??t open the system before it is completely cooled
> * A temperature probe is nice to have.
> o If you intend to heat the system, your heat source should have
> ramp control and temperature readout. If not, then the temp
> probe basically becomes required.
> o For Teflon lined units, you want to keep your system below the
> temp/pressure where Teflon softens.
> * Don‰??t use materials that are known to be incompatible with the
> vessel‰??s interior (goes without saying, but you‰??d be surprised)
> * Look around the area for any other pieces of equipment that could
> cause a larger combined hazard if the vessel fails.
> o i.e. if your pressure vessel has water in it, don‰??t use an oil
> bath as your heat source (you‰??d be surprised here too)
> * Before each use, inspect
> o the seals for any signs of hardening, cracking, or softening.
> o If PTFE lined, inspect that too.
> o the fasteners for any signs of cracking or elongation.
> * Do not over torque it as this can damage the lip seals and cause
> elongation (weakening) of the fasteners
> * Ensure the vessel is back to room temperature before opening.
> o This is where the temperature probe comes in really handy.
> + Also, PTFE is a plastic and as such acts as a thermal
> barrier. Your metal outer may be cool to the touch, but the
> inside can still be hotter that you‰??d think.
> o In the past I‰??ve routinely let the vessel cool down overnight
> and also ensured the pressure gauge was back to ‰??0‰?? before opening.
> * For shielding, we used a latched oven. That particular oven had
> ports we could use to monitor the bomb. We added a containment pan
> at the bottom of the oven just incase of spillage.
> * Cooling and heating rates should always follow the manufacturer‰??s
> recommendations‰?| these are tied to the metal alloys used, the metal
> thickness, and seal design.
> * Always have a lab buddy monitoring from a safe distance when opening
> the unit‰?| just in case it goes south.
>
>
>
>
>
> Hope this helps.
>
>
>
> Yaritza Brinker
>
> 260.827.5402
>
>
>
> *From:* ACS Division of Chemical Health and Safety
> *On Behalf Of *Jeffrey Lewin
> *Sent:* Tuesday, August 27, 2019 12:01 PM
> *To:* DCHAS-L**At_Symbol_Here**PRINCETON.EDU
> *Subject:* [DCHAS-L] Hydrothermal and solvothermal reactor safety
>
>
>
> *** External Email ***
>
> I'm looking for any information on the safe operation of hydrothermal
> and solvothermal reaction chambers. They are sometimes also referred to
> as "autoclaves" (different than what this biologist thinks of) and
> "bombs." which might be the best description having recently viewed
> pictures of one that catastrophically failed (no injuries, plenty of
> damage).
>
>
>
> From what I can find Googling - they've been around commercially for
> some time (10 or more years?); I found very little in written SOP's, but
> the discussion on researc- gate I've seen several comments that if not
> handled correctly, the results can be energetically problematic.
>
>
>
> See https://www.toptionlab.com/Hydrothermal-synthesis-reactor/teflon-lined-hydrothermal-reactor.html
> <https://nam05.safelinks.protection.outlook.com/?url=https%3A%2F%2Fwww.toptionlab.com%2FHydrothermal-synthesis-reactor%2Fteflon-lined-hydrothermal-reactor.html&data=02%7C01%7C%7C39e857f011e24a669c1a08d72b13d78e%7C994c3e8bb42845fb8640593ef0303f7f%7C0%7C0%7C637025236536811653&sdata=zirKpyliQukZGF5xEqq7in3hVXrcQEJ27W8zvwNUB4o%3D&reserved=0> for
> an example of a reactor.
>
>
>
> So questions for the group:
>
>
>
> Does your institution have specific guidance on using these such as
> limiting the size of reaction chambers?
>
>
>
> Do you have minimum engineering controls for containment (blast
> shielding, etc.)?
>
>
>
> Does your institution explicitly prohibit using them?
>
>
>
> Two critical administrative controls I've seen are:
>
>
>
> 1) not overfilling the reaction chamber, allowing headspace for gas
> formation. For hydrothermal reactions, this seems pretty well
> established since water expands about 25% at the temperatures these are
> operating at (190-220C). For solvents, it doesn't seem to be as
> straight forward. For example, I've not been able to find an expansion
> factor for dimethylformamide (DMF).
>
>
>
> 2) not heating and cooling too fast. The instructions I've seen with
> reactors say things like don't heat or cool faster than 5C/min. But
> I've seen instructions that go outside those guidelines (8C/min) and
> several that say "cool naturally" i.e. not at 5C/min (I've also seen
> discussions that specifically advise against quenching them).
>
>
>
> Any insight would be appreciated.
>
>
>
> Jeff
>
>
>
>
>
> --
>
> Jeff Lewin
>
> Chemical Safety Officer
>
> Research Integrity Office
>
> Laboratory Operations
>
> 207 Advanced Technology Development Complex (ATDC)
>
> Michigan Technological University
>
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