Sciencemadness Discussion Board - Did I Install This Column Right?

Did I Install This Column Right?

Kavion123 - 13-5-2015 at 13:39

I don't have any instruction manual or anything... Can't find any pictures on the internet of an installed column on this machine (Finnigan Surveyor HPLC w/ MS Pump).

Thanks.

Kavion123 - 13-5-2015 at 14:30

I know the mobile phase goes through the top and the eluent comes out of the bottom of the column, but I'm just so messed up right now...

smaerd - 13-5-2015 at 15:00

It's pretty hard to tell without knowing which way the rheodyne goes. Looks like there's lots of air bubbles in the line though, gonna have to prime it. Maybe ask a TA or who owns the instrument.

phlogiston - 14-5-2015 at 05:22

The heating symbol and the door suggests that this is a column oven, so that would be the right place to install it.

However, I am not sure about the connections.

The thing that the bottom of the column is connected to doesn't look like an MS to me, rather like a pump, suggesting the flow would be from bottom to top.
Yet, the top of the column seems to be connected via a rather long (and thick) tube to a valve with a sample loop, suggesting the flow to be from top to bottom. Also, however, it looks like the thin tube has just been slid into a thicker tube to connect the two, but such a connection which will never ever work with typical HPLC pre-column pressures, which is in agreement with the pump being on the bottom.

I would expect the following connections:
Pump to the valve with the sample loop, then to the column (via short and thin tubing), and then out from the column to the MS ion source.

Some columns need to be installed in a specific direction, look if it is marked (arrow, tekst) to indicate this.

[Edited on 14-5-2015 by phlogiston]

[Edited on 14-5-2015 by phlogiston]

Kavion123 - 14-5-2015 at 07:30

But with all the loops they shipped with the machine, only two of them screw into the pump and have another end that screws into the valve. But they only reach from the pump to the bottom of the column, not to the valve. I looked at the pictures online, and all the machines are stacked this way. I couldn't locate any arrows or anything on the machine.

DutchChemistryBox - 14-5-2015 at 07:32

The module on the bottom is a quaternary pump. Inside this module you see a metal block, this is the pump itself. Below this block you those 4 'things', which are gradient proportion valves. This is the point at which the tubes which leads to the solvent bottles has to be connected. To avoid introducing air into the system, make sure you have a solvent on each line. After connecting the solvent lines, prime/purge the system with the purge valve opened (the wing nut left of the metal block). For about 5 minutes for every channel at 5ml/min.

In your photo, it looks like you've attached the column to the gradient proportion valves, this is not where it belongs.

The tube you connected to the upper side of the column, looks like the waste line to me. You don't want to use this tubing with high pressures, and even then, the tube is way to thick to get small peaks. As smaerd told you, it is really hard to tell without knowing which way the rheodyne goes. But it looks like you want the beginning of the column connected to the 'hole' with the red nut inside of it. You can test this just by turning on the flow and check if the fluid flows out of that port.

The end of the column has to go to the upper module of the system, where the detector is located.

Maybe it is smart to invite someone which is experienced with HPLC to connect everything for you. He can also tell you something about maintenance, which is crucial for a HPLC system.

[Edited on 14-5-2015 by DutchChemistryBox]

Kavion123 - 14-5-2015 at 08:02

Ok so once the solvent reservoirs and serial cable arrive, I'm gonna start the pump and see if any mobile phase comes out of that empty port in the valve. If it does, I'll connect a loop from that port to the bottom of the column. Then I have to figure out how to connect it to the PDA detector.

blogfast25 - 14-5-2015 at 08:43

Kavion123:

May I ask how you obtained this machine?

Kavion123 - 14-5-2015 at 08:45

Haha "The important thing is to not stop questioning." ~ Einstein

DutchChemistryBox - 14-5-2015 at 09:07

Quote: Originally posted by blogfast25

Kavion123:

May I ask how you obtained this machine?

I was wondering the same thing. To be honest, I'm a little jealous

Kavion123 - 14-5-2015 at 09:08

Lies, this machine is old school. Dionex Ultimate 3000 or whatever it's called is way more user friendly.

blogfast25 - 14-5-2015 at 09:35

Quote: Originally posted by Kavion123

Lies, this machine is old school. Dionex Ultimate 3000 or whatever it's called is way more user friendly.

"Lies"???

Not going to answer the question then?

Kavion123 - 14-5-2015 at 09:42

eBay.

blogfast25 - 14-5-2015 at 10:41

And you buy a piece of kit like that without the manual??

Kavion123 - 14-5-2015 at 10:43

We got it without a lot of things, waste jar, solvent reservoirs, serial cable to attach the pump to the computer. Something tells me I'm missing loops as well seeing that none of them are long enough to reach the valve from the pump. We also ordered another column and it came without the plugs for the ends. eBay is turning into Craigslist. A rapist will come with the gas chromatograph we want to get.

DutchChemistryBox - 15-5-2015 at 00:03

Quote: Originally posted by Kavion123

We got it without a lot of things, waste jar, solvent reservoirs, serial cable to attach the pump to the computer. Something tells me I'm missing loops as well seeing that none of them are long enough to reach the valve from the pump. We also ordered another column and it came without the plugs for the ends. eBay is turning into Craigslist. A rapist will come with the gas chromatograph we want to get.

You know what a loop is?

Do you have someone near who can help you with installing the system? Maybe it is smart to let someone come over, it would be regrettable if something goes wrong.

If I understand it correctly, the system has stand still for some time. I really advise you to (let someone) perform some (small) maintenance to system.

[Edited on 15-5-2015 by DutchChemistryBox]

Kavion123 - 15-5-2015 at 13:20

I'm sorry I meant tubes, not loops. I'm close to figuring it all out. I'm just missing a tube that lead from the column to the inlet of the PDA detector, and a tube that leads from the outlet out. I need a tube to connect the pump to the injection valve. But thanks for y'alls help.