Varian 300-MS GC-MS-MS Turbo Pump

Discussions about GC-MS, LC-MS, LC-FTIR, and other "coupled" analytical techniques.

20 posts Page 1 of 2
This a new to me instrument, but was bought in used/tested good condition and there was a tune report with a date a few weeks back in the box with it. I'm wondering if I'm doing something wrong with it.

In any case, though, I have the instrument set up, pumped down, and currently have a blank ferrule on the transfer line. I think I'm running MS workstation v. 6.9.3 or something along those lines.

When I execute a pump-down command from the software(or just let the instrument decide to do it on its own) the turbo pump will start spinning. I can see it starting to spin before it spins so fast that the top blade can't be seen(top of pump can be seen through glass on top of instrument), I hear a high pitched whine and other characteristic noises of a starting turbo, and the software reports that the pump is "starting up." As it's spinning up over the course of ~3 minutes or so, I will see the pump power climb from a few watts to around 160W(a bit under, but close) before it reaches a steady speed and the power drops to ~10W.

In all of this, though, the software does not report a pump speed, and even after it has "settled down" the instrument is reporting the speed at 0%. Interestingly enough, right under that, Q2 temperature is listed at 68ºC, a value which never changes.

Since the software doesn't see the pump spinning, it also locks out doing things like checking ion gauges to see what the actual vacuum level in the chamber is. I SUSPECT it's in the ballpark of where it should be, but of course can't confirm that.

Has anyone seen this sort of issue before, and if so is there anything simple and obvious I can do to resolve it?
do you have the software configured correctly for that versionof the instrument?
So, here's the thing:

The computer shipped with the instrument, and in the control window for the instrument I see a tune with a Nov. 21st date(which is the same date as the printed copy shipped in the box with me).

So, it certainly looks/seems to me that 3 weeks ago, the instrument MS was operating correctly with this very computer, and the computer has not operated any others in the interim(otherwise, it would seem to me that the last tune report would be different from what was printed out/shipped, and the one shipped matches the SN of the instrument).

With that said, when it initially connects to the instrument I get an error that tells me a match in the configuration of the input board. I'm given a listing of a bunch of things that were "checked" and most have a green check-this shows a red X. I'm also instructed to click "override" to fix it, but that is grayed out.

I'm thinking I need to call the seller tomorrow(esp. since it has a 3 month warranty), but I'm hoping to resolve it without doing that.
you’re in the right screen, you just have to pick the right configuration for your hardware. I have the 1200 version of this beast with the same software, so some similarities exist.
if the cable was bad, you probably wouldn’t be able to pump down. is it possible a cable got loose in shipping?
There are some former varian service folks on this board, hopefully they will see your post soon. it weird you lost turbo readback and manifold/quad temperature readout.
you’re in the right screen, you just have to pick the right configuration for your hardware. I have the 1200 version of this beast with the same software, so some similarities exist.
if the cable was bad, you probably wouldn’t be able to pump down. is it possible a cable got loose in shipping?
There are some former varian service folks on this board, hopefully they will see your post soon. it weird you lost turbo readback and manifold/quad temperature readout.
Okay, I THINK we're going.

When I left on Friday, communication had deteriorated even further and I wasn't even able to start the pump.

With a fresh perspective on it today, I popped the top/side and rear covers off and gave everything a good looking over.

Finally, I spotted a likely problem-the largish(main board?) at the rear has two multi-pin connectors(they look like old Mac NuBus connectors, although I have no idea whether or not they're the same thing) that plug into another board. They appeared to not be fully seated. I pushed and they seated probably 1/2" or so.

So, I powered it back up and launched the software again. This time, it launched with no errors. As I sit here now, the turbo pump speed has disappeared, although the last I looked(with it still spinning up and drawing ~150W) it was at around 85%. I can see that the filament in one of the vac gauges is on, and I'm getting pressure and logical temperature readouts all over the instrument. I'm getting an overall vacuum of 1.9x10^-6 torr, which seems reasonable to me.

Now, the only error I'm seeing is "manifold temperature not at 40º" but all other temperatures are coming up-i.e. the source is now reading 35º and the transfer line is 52º.

So, I think that was the issue, and it most likely did happen in shipping.

Now I just have to sort out that work of the devil known as 10base2 to get the GC talking to the computer. I'll tackle that once I'm satisified with how the MS is running.

Thanks again for the help!

EDIT:

Went to the instrument parameters screen and turbo speed is at 99%. I'll take it!
This is certainly turning into a ton of fun...

I tried to get it to calibrate the CID pressure, but that fails because it claims the "manifold pressure is too high." I don't know what it wants to see. When I was trying to do it, the pressure was running in the ~1.4x10^-5 range. I started a bakeout cycle before I left for the day, and after a half hour of baking out it had dropped to ~1.2x10^-5. There again, I don't know exactly what it wants to see-if this is what it's pulling with a blank ferrule, I can't imagine that it will do better with a column installed. Granted I've also had the chamber open several times over the past few days, so perhaps it does just need a good bake-out.

Also, the filament either broke in shipping or during its initial power-up. When I powered it on, the source pressure read as ~.15 millitorr, which should be plenty low for a filament to power up. I actually pulled it out twice and looked at it then went looking for other problems because it didn't LOOK broken, but finally checked it with a VOM and indeed it was open. I have two more on the way, and I'll send this one off to SIS as ~$350 each from Agilent is going to kill me. I also can't figure out how to even access any of the source beyond the ion volume, as the manual I have shows a totally different design than what's in my instrument(I have an email in to Scion to see if they can supply a more current user manual).

The good news, though, is that I did get the GC talking to the computer. It came to me set up with the computer's on board ethernet connected to a hub that also had a BNC port, and that port running to the GC. The BNC port on the hub never seemed to work, so at first I tried bypassing it by putting a 3Com BNC NIC in the computer(I have a small stash of them bought up in a failed attempt to get a Finnigan LC-MS working-that MS needs a specific revision of a specific P/N of 3Com card to work). I went GC-computer, but even though the computer reported network activity I never could get them talking. Finally, I dug in and figured out that the NIC needed a specific static IP address which the manual does give. For whatever reason, it also doesn't seem to want to assign an IP address to the GC, but once I told the GC to use a static address and typed in the one that was given in the software(one higher than the computer's address) it worked fine.
Woohoo!!!
Now give it some time to get the vacuum down. Thats a huge chamber and its been vented for a while, don’t be afraid to let it pump down for a week or two. Crank the manifold temperature up to 55 and heat up the source and transfer line. It would be a good time to get some He flowing in as well. When all settles in, you should be operating in the 3x10-7 range.
Good luck!
Woohoo!!!
Now give it some time to get the vacuum down. Thats a huge chamber and its been vented for a while, don’t be afraid to let it pump down for a week or two. Crank the manifold temperature up to 55 and heat up the source and transfer line. It would be a good time to get some He flowing in as well. When all settles in, you should be operating in the 3x10-7 range.
Good luck!
Thanks!

The bakeout got me into the high 10^-6 torr range, so I'll leave it alone and see what happens.

This is my last week before I'm off for two weeks before Christmas, so I'll leave it running and pumping while I'm off.

I'm wondering if-when I pop it open tomorrow to change the filament-I should put a small amount of Alpezion L on the gasket. I know Agilent suggests doing that for similar type seals on their MSs.

Also, I'd used a "short" Agilent blanking ferrule. I did find a tray of Varian-supplied blanks that came with our since-retired Saturn, so I may try one of those. I wonder if the one on it isn't sealing as well as it should.

One last thing-by "helium flowing" are you suggesting installing a column and flowing helium in through the GC at a low flow rate, or just letting it run through the purge port at the rear of the MS?
Alright, I'm officially an idiot.

It seems as though I'd capped it not with a blank ferrule, but rather with a "used" ferrule that had been cinched down on a .25mm ID column(I'd put the nut with the blank on the inlet).

The fact that it could pull down into the high 10^-6 range with that is impressive to me.

I now have it pumping down with a column installed and a low flow of helium. When I left it, it was in the mid 10^-6 range, and I have no doubt that it will continue to go down.
benhutcherson wrote:
Alright, I'm officially an idiot.

It seems as though I'd capped it not with a blank ferrule, but rather with a "used" ferrule that had been cinched down on a .25mm ID column(I'd put the nut with the blank on the inlet).

The fact that it could pull down into the high 10^-6 range with that is impressive to me.

I now have it pumping down with a column installed and a low flow of helium. When I left it, it was in the mid 10^-6 range, and I have no doubt that it will continue to go down.


Before you send off those filaments, I will let you know I heard SIS was sold to another company and the SIS name is gone. The person that let me know said the new company is still doing the same work but the filament repair went up a little in price, but still much less expensive than the Agilent prices. The new name is Adaptas Solutions.
The past is there to guide us into the future, not to dwell in.
James_Ball wrote:
benhutcherson wrote:
Alright, I'm officially an idiot.

It seems as though I'd capped it not with a blank ferrule, but rather with a "used" ferrule that had been cinched down on a .25mm ID column(I'd put the nut with the blank on the inlet).

The fact that it could pull down into the high 10^-6 range with that is impressive to me.

I now have it pumping down with a column installed and a low flow of helium. When I left it, it was in the mid 10^-6 range, and I have no doubt that it will continue to go down.


Before you send off those filaments, I will let you know I heard SIS was sold to another company and the SIS name is gone. The person that let me know said the new company is still doing the same work but the filament repair went up a little in price, but still much less expensive than the Agilent prices. The new name is Adaptas Solutions.


They caught me off guard when I called a few weeks ago and answered with that-and made me make sure I'd actually dialed the correct number.

In any case, the price I have is ~$50 for a 1200/300 filament, which doesn't seem terrible to me especially given that they're over $300 from Agilent.

Also, the instrument was at 1.6x10^-6 when I left for today. I was able to successfully do a CID calibration.
At 8x10^-7 torr today, so we're getting there!
Also, another couple of questions for those who use these instruments(including tdgcuser)-

1. Do CI and EI use the same ion volume? I realize that's probably a stupid question, but at the same time none of the documentation I have(Scion Instruments was nice enough to send me a BIG volume of internal service/training documents that I'm still wading through) shows the difference between the two even though the software prompts you to change volumes when switching modes.

Going on that, is there a tell-tale way to ID which volume is which-assuming that they are in fact different?

2. In the absence of the insertion/removal tool, have you ever installed and removed volumes by venting, taking off the glass top, and manually inserting/removing? If so, are there any tricks to ensure proper alignment? I'm assuming that the large hole gets aligned toward the top in line with the filament and the smaller hole 90º apart with the column, but would appreciate confirmation on this.
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