1/9/97


Dear Fellow Microscopists:

We are considering of installing an Automatic Liquid Nitrogen

Filling System for our SEM. The only source we came across is VBS

Industries, Inc. I wonder if any of you would like to share with me your

experience with any automatic LN2 filling system. Are they dependable? Are

there other sources that sell similar type system? Any feed back will be

greatly appreciated.

Pearl W. Yip

Rome Lab

yip@maxwell.rl.plh.af.mil


There was a long thread on this subject in the early days of the listserver.

Perhaps it resides in Nestor's or the Florida archives??

I put in my comment that I would never have auto LN fillers again.

We had them on TEMs and SEMs in the 70s and early 80s and they all

failed catastrophically. (I guess there is no simple, benign failure

mode when the possibility of emptying a large LN cow over an

instrument and into an unoccupied room exists)!

Long term reliability under extreme temperature excursions seemed

to be the problem.

However, to be fair, we are talking 20+ year old technology. This is

the wonderful 90s...

ron-anderson@vnet.ibm.comRon


I agree with Ron and Bill, they are not dependable. Anything that has

moving parts or electronics is not dependable. If you must keep something

cold all the time (much better than temp cycling, IMHO), I recommend that

you design and build a large LN dewar that keeps the thing cold that you

periodically refill every few days or so - much like a dewar for an EDS

detector. There are companies out there that will work with you on this

if you don't have the facilities to build your own.

Good Luck!

John Posthill

jbp@es.rti.org


Dear Pearl,

Our automatic LN2 controllers are from Torr Vacuum, Inc. We have

had several disasters: 1) The LN2 source--a very large tank about 200 m

from our lab--would occasionally run dry; then the solenoid would over-

heat. Usually it would open, but occasionally it would fuse and draw

current until someone noticed (see #3). 2) The filler shut-off failed

on the system attached to our EDS detector. LN2 poured into and over

the dewar until the outer bottle deformed and ice formed all over the in-

side and outside of the system. We had to warm up everything, dry every-

thing out and re-form the outer bottle--it had a concave bottom originally,

but was convex after the disaster. Luckily, everything worked out well,

and the detector is still functioning a decade later with its specified

resolution. 3) For some reason--not an empty LN2 tank--the solenoid on

the line on the 200 kV TEM fused and heated the plastic foam insulation

starting a fire. The fire was, fortunately self-limiting; the event

occurred after hours on a Friday before a holiday weekend and was not

discovered until the next Tuesday.

We have not lost any expensive equipment, but there was certainly

the potential for such losses. I don't think our problems were the fault

of Torr Vacuum; they seem to be inherent in automatic LN2 systems. If you

can avoid such systems, I would reccommend you do so. Good luck--especi-

ally if you must use them.

Yours,

Bill Tivol

tivol@wadsworth.org


Pearl,

As others have said, these systems do seem to unreliable and considering

the value of the equipment they are attached to, I would not trust them. I

would even be wary about LN2 level alarms - they seem to be reliable, but

do you really want to have the safety of perhaps 500k dollars or more of

equipment depending on one?

Anyway, what is the problem with a regular manual schedule of re-filling?

You don't actually say what you are filling with LN2.

If it is an EDX detector, I would suggest that if you are really concerned,

you should have a routine for users to disconnect the HT from the detector.

Then if the detector should run dry, there is no risk of damage (although,

to be honest, I have, more than once, had an EDX detector go dry while the

HT was on and survive apparently unharmed, but I don't recommend anyone

trying it). However, this might require that you allow the detector to

restabilise following reconnection of the HT.

If you are filling LN2 traps on the vacuum system, then I would caution you

about running them continuosly anyway - over a period of time this will

actually degrade your vacuum. All cold traps should be allowed to warm to

room temperature at least once a week and the vacuum stabilise. If not, you

will gradually get a build up of ice and other contaminants on the traps

which, eventually will outgas at a sufficient rate to contaminate your

system.

Regards,

Larry Stoter

LPS@teknesis.demon.co.uk


I certainly wouldn't suggest anyone try warming up EDX detectors, on or off

the microscope, without first talking to the manufacturer regarding

warming/cooling procedures. However, from personal experience of Be window

detectors, they can survive warming up while on a TEM column, so if it does

happen to you (and you are responsible), try cooling it down again, before

you cut your throat :)

With UTW detectors, you probably won'tt be so lucky.

Regards,

Larry Stoter

Dr L. P. Stoter Technical Editor, MICROSCOPY & ANALYSIS

Technesis

17, Rocks Park Road email: LPS@teknesis.demon.co.uk

Uckfield, E. Sussex Phone: +44 (0)1825 766911

TN22 2AT Fax: +44 (0)1825 766911

United Kingdom


VBS is the only automatic LN2 filling system I have seen commercially,

although there may be others. However, you might want to design your own

system, using cryogenic solenoid valves and sensors, and providing LN2 from

cylinders. It is fairly inexpensive to do this. I can send you information

on a system we built and used in our lab for some time, if you are

interested. I presented a poster on this system at the 1994 MSA meeting and

the description in included in the Proceedings from that meeting.

One problem we ran into with our system is that we did not have a failsafe

mechanism to shut the system off when the cylinder ran out of liquid. The

result was that nitrogen gas would continue to fill the dewar and eventually

would blow out the remaining liquid. I think this can be remedied by making

some changes to the system.

Regards,

Melanie A. Behrens

Texaco, Inc.

P.O. Box 509

Beacon, NY 12508

914-838-7261

behrema @ Texaco.com or MelanieOwl @ aol.com


Our disaster story:

The filler for an LN trap over the DP on our JEOL 2000FX TEM malfunctioned,

and a tank of LN2 emptied out all over the diffusion pump. The microscope

shut down, luckily valving the column off from the DP. The water lines

froze, including the water in the baffle at the top of the pump. This

caused the baffle to crack, and when it warmed up again, the pump and

reservoir tank flooded with water. The next morning the microscope was

found in the OFF condition, and, no problem being evident, was simply

restarted. This caused an emulsion of DP oil and water to be sucked into

the rough pump, which *was* evident, and the machine was immediately turned

off. The damage was done however, and a complete teardown and cleaning was

necessary, taking a couple of weeks.

So if you use a filler system, be sure to provide a way to funnel LN away

from the microscope, in the event that the solenoid fails to close properly

and the tank empties.

allardlfjr@ornl.gov

Larry Allard


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