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Author: Subject: Christmas Comes Early This Year
Sauron
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[*] posted on 4-11-2008 at 21:49
Christmas Comes Early This Year


FINALLY the last shipment of my lab equipment has arrived from the warehouse in SF Ca where it was idling. Thai Customs hit me for about $600 and the customs broker abother $300, freight was prepaid, another $700. But worth it. As usual it came by ocean cargo. A few weeks on the water and a week in Customs.

My Parr 4521 1 liter heated & stirred pressure reactor and 4843 Controller

And Parr 4833 temperature controller for the mantle to shaker hydrogenator 3911 already here

and Aldrich Kugelrohr (current model) plus an old model air oven that takes up to 4 liter flasks. I can use this with the motor for the new model.

and Ace Hanovia 450 W power supply for med pressure Hg arc lamp

and Sequoia Turner 340 UV-Vis spectrophotometer

and a bunch of Buchi rotavap hardware, trhree motor heads, a couple water baths, and four or five stands or jackstands. Along with the Buchi spares I have here I can assemble 2-3 more Model R, R110 and EL-130 sets in addition to the R110 I have on hand.

I will have to take some pics and post them once I get everything situated.

I am going to look into upgrading the Parr to 4522, 2 liter, which just involves changing the mantle, reactor body (heads are same) and a few internal reactor parts that need to be longer. That would give it a working volume of about 1325 ml. The thing is rated at 1900 psig and 325 C. with the stainless steel vessel.

The only item still on other side of the pond is a Cole Parmer Masterflex peristaltic pump drive with a PTFE diaphragm pump head suitable for pumping really corrosive, aggressive liquids and there's damned little it can't handle.

The warehouse is closed down so I have to change the way I deal with US purchases in the future.

[Edited on 5-11-2008 by Sauron]




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[*] posted on 4-11-2008 at 21:54


Thats very nice! Please get some pictures up, I'm excited to see how nice they all look! :D
What are some of the experiments you hope to do with all this new equipment?

Oh yeah, Doesn't hydrogen cause problems with Stainless steal?

[Edited on 4-11-2008 by kclo4]
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[*] posted on 4-11-2008 at 23:00


Not that I am aware, but if it does, Parr makes vessels out of lots of other alloys, like hastalloy, monel, and refractory metals like titanium and tantalum. I shudder to think of prices. A new vessel body may well cost more than the $2000 I paid for this whole unit, used. And the more exotic materials will certainly cost more than SS 316.

The main concern when using an autoclave for more than a single purpose it to avoid using it for anything involving catalytic poisons or it will never be useful for catalytic hydrogenation again.




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[*] posted on 4-11-2008 at 23:48


Oh you lucky person! I would have liked to witness the reception :D

Now that my dream of having a rotavap is fullfilled, next one on the list is a Parr!Gonna take a while though...

Well hope to hear you doing some work with all that!




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[*] posted on 5-11-2008 at 00:06


Major money pit is next stop: fume hood. $7000 including the exhaust scrubber That goes outdoors with vent stack over the roof. It's a big hood (2 m wide, 90 cm deep, 1 m height, cabinets under.) Should have been installed already but various financial snags ensued.

Maybe I will sell off a few spare rotavaps.




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[*] posted on 6-11-2008 at 04:53


T spebt 4-5 hours unboxing and sorting out the shipment. Thus far no bad new. The Parr pressure reactor came in sections: the vessel, very heavy, the base, the heater assy with its three legs, the motor and stirrer overarm, which turns out to mount to the shell of the mantle and couples to the packed-gland stirrer assy. And the controller, which is modular. This one has the mantle controller unit and a digital tachometer. There;s two more bays available for a t/c and a transduce to display internal temperature and pressure. There's also an option for PC interface and control. The normal pressure display is a gauge, the one that came with this is a 0-600 psi but I can change that out to one that goes to 2000 psi.

The new model Kugelrohr came with safety guard, which I was not expecting. That's nice. Looks immaculate. Aldrich sells these now for 7X what I paid for this one. Plus I got an old model coffee-urn type air bath and an old model air motor of the windshield-wiper type which, unlike the air bath, I probably will never use.

Pleasant surprises in the assorted Buchi rotavap bits. Three Model R bases with jacks. Two Model R110 jackstands, two RE-111 jackstands. One freestanding waterbath for Model R, one for R110. Two EL-130 motor heads (the variant of R110 that is for reflux and descending condenser setups mostly.) One R110 motor head built into a custom plexiglass shell that is airtight, with provision for inert atmosphere or purge, intended for use in a flammable environment (explosion proof.) Probably out of a refinery lab. One diagonal style Buchi double coil condenser. That one was properly packed (padding between coils) so intact.

Once I consolidate these with the surplus Buchi stands etc and motors I have already, I may have some rotavaps for sale.

A Kipp + Zonen chart recorder.

And Ace Hanovia 450 W power supply for medium pressure Hg vapor UV lamp.

In a day or two I will take some photos. First lots of boxes to inspect for little bits I may have missed, then trash. Lots pf bubblepack and plastic peanuts to police up. Must keep busy so as not to dwell on how much this all just cost me for freight, duty, VAT, and broker fees.




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[*] posted on 6-11-2008 at 15:09


Geez, that's alot of heavy duty artillery.

I hope you got a project that is worth it. I don't see any chemistry related projects right now that could possibly give any worthwhile investment returns.
But then of course I don't see this area being a good hedge right now either except for acquiring distressed inventory.

You may be able to get more cheap(er) items soon as values are still deflating

good luck with the project(s)




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[*] posted on 6-11-2008 at 15:23


Investment recovery has never been my concern. I just want to have fun doing my chemistry. Not out to make a buck, been there, done that. I have projects backed up for years that are awaiting the last big acquisition (hood).

This little shipment is nothing comapred to what I have ties up in HPLC kit (Waters). A lot of other big ticket purchases were made for now defunct liquor project, like 20 liter Buchi rotavap w/glass, and a pair of 72 liter Glas Col TM mantles and four matchine flasks. Bought the mantles and two of the flasks new, other two used. Someday I'll find a use for these.

Here's a photo of Sequoia Turner 340 UV-Vis spectrophotometer, this is off the net but exactly the one I have. I need a manual for this thing. If anyone has one to scan or knows where I can get one, scan, xerox, anything, I'll be grateful.


[Edited on 7-11-2008 by Sauron]

ST340.jpg - 29kB




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[*] posted on 7-11-2008 at 00:47
Buchi Rotavapors Galore!


After consolidating the old pile of Buchi bits with the new pile of Buchi bits here is what shakes out:

1 R110 w/waterbath and glass - my workhorse.
1 more R110 with custom gas-tight containment for motor head
2 EL-130 (rotating seal) version of R110, 1 w/ bath
1 RE-111 series jackstand only plus a second that needs a little work and a spare stripped baseplate

3 Model R on V-style jackstands, 1 water bath matching
3 alt style stands for built in bath, adjustable track for upright,, no motor heads or baths
1 spare V stand w/jack

That's seven working rotavaps w/jackstands, and I recon I can sell off the 3 Model R's while keeping the 2 R110s and 2 EL130s. Photos shortly.

The nice thing about the R and EL, R110 and EL130 is that they are dead simple, no electronics apart from the capacitor for motor. They last a long LONG time. Whereas the later models all have pcbs supporting digital displays and once Buchi stops supporting spares for those models, the user is s.o.l.

[Edited on 8-11-2008 by Sauron]




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[*] posted on 7-11-2008 at 18:51


What's holding up the pics is that the auto focus on my video camera is on the fritz. I have tom sort this out.

Very annoying.

Well, I took the pics with an unfamiliar Sony digital, and now am having trouble getting XP to recognize the USB card reader that is supposed to move the jpgs from the SD-card to the hard disk. Grrrrr.

One damned thing after another!

[Edited on 8-11-2008 by Sauron]




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[*] posted on 9-11-2008 at 08:14


AT LONG LAST

Photos of Recent Shipment from USA

Parr 4521 Pressure reactor Stainless Steel 316, 1 liter, rated 1900 psi @325 C, w/bottom drain. The 4843 controller is also shown.

[Edited on 9-11-2008 by Sauron]

Parr.jpg - 66kB




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[*] posted on 9-11-2008 at 08:19


Just the vessel w/head and assorted kit atop

[Edited on 9-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 08:23


Another view The two units alongside are Buchi EL-130 Rotavaps which resemble one armed bandits with their jack handles in a Hitler salute.

[Edited on 9-11-2008 by Sauron]

[Edited on 9-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 08:25


Nice equipment. Just one thing, has the parr reactor been tested recently? I would hate to see it fail filled with hydrogen gas and some catalyst. Testing with some compressed air first might be a good idea.



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[*] posted on 9-11-2008 at 08:31


Three Model R Buchi rotavaps, one with matching waterbath, all on jackstands. The closest two are early models, the third is the transitional variant just before change to R-110 late 1960s I think. I had one of these in my lab at university mid 70s.

[Edited on 9-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 08:40


Nestled in a corner of my master bedroom, more of the loot.

L to R and back to front:

Kugelrohr new model motor, air bath, old model air bath
Kipp + Zonel chart recorder, Sequoia Turner 340 UV-Vis spec, Parr 4833 temperature controller for 3911 shaker hydrogenator's mantles; Kugelrohr air motor for old model, automotive windshield wiper reciprocating type; very nice costly airtight Halliburton type instrument case that Buchi stuff came in; jackstand for Re-111 Buchi; B-461 waterbath for R-11o/EL-130 Buchis.

The Kugelrohrs deserve better photos. I will do tomorrow.


[Edited on 10-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 08:44


Ace Hanovia power supply (lamp ballast) for 450 watt Hg medium pressure UV vapor arc lamp - standard photochemical research tool.

[Edited on 9-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 08:53


R-110 head interchangeable on the jackstands with EL-130. I have two of these, but only one in this interesting airtight enclosure with gasketing and a threaded vent for I guess positive overpressure. My best guess if petrochem industry use in volatile environments demanding EX-proof equipment. I doubt that U/L ever saw this one though.

I already found that this rig is incompatible with the standard Buchi diagonal double coil condensers, so I guess it has to be used with a distributor head and vertical conder, which I like better anyway as they take up less bench space.

[Edited on 10-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 08:58


From an earlier shipment, Thermolyne 2" x 12" 1100 C tube furnace.

[Edited on 9-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 09:05


Lastly for tonight, a few items outside my lab equipment storage room door waiting for me to make room.

The drun is 25 Kg TCCA.

Lurking behind the mini-drill press is a Waters 715 Ultra WISP autosampler for HPLC w/controlled temperature carousel. Still on its skid.

In upper RH corner a Waters fraction Collector (first model), a PrepLC 25mm Radial Compression Module for 1,2, or 3 x 100mm prep HPLC column segments.

Most of what is taking up the space in next room is HPLC equipment.

[Edited on 10-11-2008 by Sauron]

[Edited on 10-11-2008 by Sauron]

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[*] posted on 9-11-2008 at 09:17


Oh, and @eliteforum, how would you like your entree of crow?

Southern fried?

or Tartar?

Cornish game crow?

Or Crow a l'orange?

You've been as much as calling me a liar for about a year, so now, take what is coming to you.

[Edited on 10-11-2008 by Sauron]




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[*] posted on 9-11-2008 at 11:25


Beautifull, very impressive equipement! Chemporn at it's best ;)

Funny, the 2 old Buchis look alot like the model I recently aquired, it is said to be a Buchi KRV 65/45, although the stand isn't the same (it's one with a integrated place for the water bath). The motor look identical though. I am always lost with all the Buchi models...

I must agree with the comment about how tought they are, the one I got is from the mid 60's,a nd in perfect conditions (motor works fine, it's just the old electric plugs). The second one another frecnh member aquired, from the same place, also from mid 60's worked perfect also, although it was very dusty. That last one is indentical to the two first old Buchis you have.. What model type are they?

I guess you are going to have some fun with all that! The Parr is surely going to appear in a dream of mine tonight :)

[Edited on 9-11-2008 by Klute]




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[*] posted on 9-11-2008 at 11:58


Sauron, are you planning something huge ? ;]
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[*] posted on 9-11-2008 at 14:59


@Maja: Global domination! (insane tittering, similar to Richard Widmark as Tommy Udo in "Kiss of Death")

Seriously, not one huge project, just lots and lots of smaller ones.

@Klute: Extremisn in the pursuit of chemistry is no vice. (Paraphrase of half of Barry Goldwater's famous 1964 campaign remark.)

I have two of those stabds for the integral bath, with support rod but no jacks or baths, plus another without even support rod or the clamp assy to mount it. I had one complete a few years ago that I bought on LabX from Oregon State University, but sold it off. These older Buchis seem to last forever. I think Buchi later got into planned obsolescence.


That long model number sounds like something off the motor plate rather than the Model of the Rotavap proper. I have lots of Buchi brochures and parts lists extorted from their former Thai agent and they just refer to the models R and EL for the original Rotavaps, R being stationary seal, rotating vapor duct, EL being rotating seal, stationary vapor duct.

The next were R-110 and EL-130 which were very similar to R and EL in terms of motor head, but the "one armed bandid" jackstand with fat tubular column was a departure.

After that c.1980 the RE-111 series and EL-131 and variants, the motor head was now mounted not on a rod or column but directly on a spring loaded housing and elevated when released by gripping the handle - no jack handle. The introduction of electronics and digital displays allowed for control of variables like RPM and temperature (on some models) but at the expense of complexity and maintenance problems. The bath for these models interfaces to the base plate and will not stand alone.

In the 1990s the 124/134/144 models were bundles with vacuum systems and their controllers. Most of that stuff was not actually made by Buchi, the recirculating aspirator pumps were made by Sibata (Japan) for example. Modularity allowed changeover from R to EL seals and glassware configurations.

The present 200-series models were introduced in the early 21st century and feature even more intergarion with vacuum control, remote operation, solvent trap (secondary condenser) and powered jack Glassware redesigned and some of the nicer variants of glassware eliminated, a development I disapprove. For example the descending condenser setup is great for foaming and bumping solvents like toluene. I have this setup on my 20 liter industrial model Buchi R-151.

[Edited on 10-11-2008 by Sauron]




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[*] posted on 9-11-2008 at 16:32


Vulture,

Initial testing of a high-pressure vessel, is most safely carried out by hydro-testing.

Fill the vessel with water, purge all gases. Raise the internal pressure by means of an airless sprayer, or pressure washer unit. Many of these units can produce pressures of several thousand psi.

If the vessel fails at room temperature, under water pressure, it usually merely warps, or at worst, goes....sploosh.

Under hydro-test conditions, distortion of the vessel can be measured mechanically.

Too much distortion, indicates the vessel should no longer be used for high pressure applications.

If a pressure vessel fails under air/gas pressure, rather than water pressure, more spectacular effects may be observed.

Parr reports testing procedures they use, somewhere on their website. Possibly in their on-line manuals. For a price, you can periodically send in your vessels for factory testing.

Also note. To me, the stirrer unit on the above pictured Parr pressure vessel, appears to be the more expensive magnetically-coupled drive. The Parr packed-gland drives that I am familiar with, are considerably smaller in size.

[Edited on 9-11-2008 by zed]

[Edited on 9-11-2008 by zed]
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