Father, want to show my 10yo chemistry. Just bought a 5890

[JLMarcus321]

Hi everyone, I'm in the middle of a neat sort of puzzle, and I'd like your help. I've always been interested in Chem (even had it briefly as my major back in college, before I moved into math) and I've got a 10 year old (though a mentoring program like Big Brothers/Big Sisters) that I'd like to get interested in science.

I had the opportunity to buy a GC-FID used from a lab that was closing for cheap, and after doing as much due diligence as possible I decided to bite the bullet and try to make this a hobby and a learning tool... But now that I've done it, well... I'm a teansy bit in over my head, and I would greatly appreciate your help!

Details so far... and please bear with me, I've really attempted to do my research ahead of time before coming to you all.

my equipment
HP 5890 Series II with dual FID
7673 autosampler injector, controller and tray
A computer running windows XP with chemstation Rev a.10.02 [1757]
Cost me 4k for everything, and the only thing that appears to be wrong is that the front FID temp is giving an error (DETA temp rdg) but detb is showing accurate temp

What I still need, as far as I can tell
1. (and I know this is a biggie) instructions on how to run the damn thing... Remember this is just for a hobby, so even getting poor separation and lack of quantitative data isn't that big a deal

2) I'm aware I need research grade helium, hydrogen, and air. Luckily there's an airgas just a few blocks from me, but when I went in they only wanted to sell me their largest tank of helium, which was going to be in the ~1500 range. It would be nice to call their hotline and negotiate delivery of a smaller tank, if possible. Any tips?

3. Also, I'm not 100% on the hookup locations of the various gasses, makeup gasses, etc. Also since this is laboratory surplus, I'm not sure if it has the "usual" internal set of regulators or pressure control, etc.

4. other things like the column, ferrules, regulators, gas plumbing, syringe/septum for the autosampler, etc etc. Any help would be appreciated.

I'm aware I've bit off a big project, but I read up for 2 months beforehand and 4k for a computer/gc/autosampler didn't seem like a bad deal. It was this or a 3d printer anyway, and I just found this to be more interesting. Would you mind helping out?

Thanks, in advance.

[Peter Apps]

About the only thing that I can help you with over the internet is that you do not need helium. Use nitrogen as carrier gas - the only drawback is that separations take twice as long and the detection limits will be higher. You can also use hydrogen as carrier, but I would pracise a bit first.

For the rest, by far the best way will be to find a friendly chromatographer who lives close to you and buy a couple of cases of beer !!

Peter

[James_Ball]

I agree with Peter, don't worry about helium, just stay with nitrogen or hydrogen. If you use hydrogen then you only need two tanks, one for carrier and fuel the other zero air for the FID. Do you have capillary columns or packed? Split/Splitless injection ports or Direct Injection ports?

Also you dont need to use the expensive Research grade gasses, you will save a ton using 4.5 or 5.0 grade gasses and using simple gas purifiers to clean up any contaminates, but actually if you are not doing quantative work you probably won't even need the purifiers. It isn't like you will be doing trace analysis running 24/7 and hundreds of samples per day.

Just don't do as one lab I helped out one time and purchase red tank generic hydrogen and use rubber air brake lines for the gas plumbing(it was on an ECD even), most horrible setup I have ever seen.

For supplies check here http://www.restek.com/Supplies-Accessor ... ccessories

Copper tubing will work, don't need stainless steel. You will need a two stage regulator for the gas tanks if you don't already have them, that will keep you from sending 2500psi straight to the instrument which would be very dangerous.

You may want to let us know where you are located, someone here might be near by to be able to help.

Ask any questions as you go, always someone here to give advice.

[rb6banjo]

I certainly admire your ambition!

That detector temperature error might be as simple as the thermocouple isn't seated in the heating block correctly. I get those types of errors now and then on a 5890 Series II that I have but I get it on the injector side. Usually, I am able to correct it if I take it apart and jostle the thermocouple leads around a little and then reassemble. If there is insulation, make sure the insulation gets packed in between the leads so they don't short each other out.

Do you have 2 injectors or just one? What type of inlet(s) do you have? Split/splitless are the most common. My Series II has 2 split/splitless inlets and on the front panel of the GC they say "split programmable pressure". The total-flow controllers help you adjust the split ratio. You set the head pressure on the column with the Chemstation software. Series II was the first Agilent instrument with electronic pressure control (EPC).

Will you be injecting liquids or gases? This will help you figure out how you want to configure your inlets (right type of insert, septa, etc.). For illustration purposes, liquids are easiest.

Once you get that error cleared you set your column flows based on:

1) what type of carrier gas you have (I recommend helium or nitrogen for you). Hydrogen would work but it's a little trickier to work with than those other 2.
2) what size inner diameter and length column you have.

In the iTunes store, there's an app that you can get for free that will help you adjust your pressures so that the flows are what you want/need.

Agilent has a number of helpful videos on column installation on youtube. You should check them out.

Good detector flows for my FID in my series II are 30:300:25 H2:Air:He makeup gas.

Light-her up and go!

If you need supplies (ferrules, column nuts, syringes, septa, etc.) there are a number of good supply houses (Restek, Sigma-Aldrich, Fisher Scientific. VWR Scientific, etc.). The nuts for the Series II are pretty universal but you'll need ferrules that fit whatever column you have.

Again, I really admire your ambition. I hope your little experiment works out for you.

[KM-USA]

Unless you're doing sensitive work, I think helium like for balloons would suffice.

You could use front inlet and route the column back to the working back FID, just tell the software to use those, we've done similar.

I'm laughing, as our remaining 5890 is running Windows NT and A.06, older than yours.

[JLMarcus321]

Hi everyone, thanks for your encouragement so far!

Posting my location is a good idea, I'm in LA. Trying to get the advice of a local chromatographer is a great idea, I posted a job request to the UCLA job board but haven't had any responses yet. A grad student would go a long way towards helping me get this up and running, I think.

If I were to go with helium, which I'm still thinking of doing... Well, I'm not 100% sure on exactly where the hookups are. Just confirming, I'd need a tank of helium, hydrogen for the fid, and either a compressor or another tank for the air? Does the air need to be of any particular quality, or have a filter/trap on it? And FID makeup gas can be run off the helium tank too, right? Would I use some sort of plumbing to split the helium after the 2 stage regulator, so I don't need a separate tank?

I'm a bit wary about parts, quality etc. I do want this to be relatively accurate chromatography so I'm trying to avoid making too many compromises, but I'm not sure on the level or quality of components I need. For example, would a "normal" airgas 2 stage regulator suffice or are those known to insert impurities? Same for piping, etc.

I was planning on picking up a MXT-5 column (was advised on that), as it appears to be more or less general purpose.

At this point I think I need about 15 minutes of someone to look over the machine and say "you hook the helium up here, this is how you properly ignite the FID" and then an hour or two of chemstation. Anyone know a hungry grad student who would be interested in a couple cases of good beer and a pizza in LA?

Thanks everyone

[rb6banjo]

On the back of my Series II, there are 2 swage-nut fittings for the inlet gases. I put a tee in my helium line to feed both injectors:

http://i1285.photobucket.com/albums/a59 ... bafe92.jpg

I put an extra tee in the line to feed the makeup gas (I use helium for that as well). One helium tank feeds it all for multiple GC's in my lab. The makeup gas control is a needle valve (see the set screw inside the knob on the front of the instrument). You adjust it with a screwdriver and set the flow how you want it. Chemstation should allow you to adjust the head pressure on your columns.

I have one air and hydrogen cylinder that feeds the FID's in my lab. So, I use these inexpensive single-stage regulators (I think I got these from Restek) to step the pressure down and adjust the flows to the detector(s) from the main 2-stage regulators on my tanks.

http://i1285.photobucket.com/albums/a59 ... 697e50.jpg

I have been doing it for years and haven't had any trouble. The FID support gas connections are made through the side door of the instrument and go into the on/off valves on the front of the instrument.

For a flame detector, the cleanliness of your gas will have a direct bearing on your sensitivity. Bad gas will give lots of noise. If you don't need "gnat's hind end" sensitivity, then the air won't matter too much. If you want a quiet baseline, the cleaner the air the better.

5-phase columns are good ones for general purposes. I use Rtx-5 from Restek, HP-5 from Agilent Technologies, and SPB-5 from Supelco. All are good columns.

[dblux_]

"The older man, the more expensive toys"

Good luck and much fan with chromatography.

PS - have you considered HPLC instead of GC ? (no troubles with gases)

[James_Ball]

Hi everyone, thanks for your encouragement so far!

Posting my location is a good idea, I'm in LA. Trying to get the advice of a local chromatographer is a great idea, I posted a job request to the UCLA job board but haven't had any responses yet. A grad student would go a long way towards helping me get this up and running, I think.

If I were to go with helium, which I'm still thinking of doing... Well, I'm not 100% sure on exactly where the hookups are. Just confirming, I'd need a tank of helium, hydrogen for the fid, and either a compressor or another tank for the air? Does the air need to be of any particular quality, or have a filter/trap on it? And FID makeup gas can be run off the helium tank too, right? Would I use some sort of plumbing to split the helium after the 2 stage regulator, so I don't need a separate tank?

I'm a bit wary about parts, quality etc. I do want this to be relatively accurate chromatography so I'm trying to avoid making too many compromises, but I'm not sure on the level or quality of components I need. For example, would a "normal" airgas 2 stage regulator suffice or are those known to insert impurities? Same for piping, etc.

I was planning on picking up a MXT-5 column (was advised on that), as it appears to be more or less general purpose.

At this point I think I need about 15 minutes of someone to look over the machine and say "you hook the helium up here, this is how you properly ignite the FID" and then an hour or two of chemstation. Anyone know a hungry grad student who would be interested in a couple cases of good beer and a pizza in LA?

Thanks everyone

I have set up one here in the lab before just using the house compressed air and an activated charcoal Hydrocarbon Trap from Restek to clean the air. You would probably also want to add a moisture trap just in case, I a sure there are times it can get humid out there. If you get one of the small oil free compressors then the hydrocarbon trap would last a long time.

I wish I wasn't so far away here in Ky, I do love me some pizza!

[osp001]

I run a 5890/FID on hydrogen + compressed air. You need to tinker a bit to find the sweet spot for the gases, and you might sacrifice some sensitivity, but it works fine- no helium, no nitrogen. Hydrogen gas plus an air compressor and gas line filters. I'm still ringing the bell with a nice signal:noise ratio on a capillary column and microliter injections with tiny sample concentrations, so by "sacrificing sensitivity," I'm still WELL into the high sensitivity range. Running hydrogen may help a little with that.

However- you may want to check your homeowner's or renter's insurance. Most will disown you for compressed gases in the house, particularly flammable gases. A hydrogen generator will be an option.

What do you have for software?

[Bigbear]

Good for you. I would also say to use nitrogen for carrier.
Wish you had posted earlier as I just recycled 3 sets of 5890 manuals a few weeks ago!

A source for older Agilent instrument parts is Alpha Omega Tech, though they are on the east coast (NJ).

[JLMarcus321]

Hi everyone, sorry for taking a long time to respond, but this is a hobby and real life got in the way

I've hit a couple problems that should be pretty easy to solve, hopefully. Number one, there are a lot of utilities and programs that I don't have access to anymore, like to reprogram the autosampler controller, etc.

I'm unfortunately in a middle zone, where the manuals are written for commercial purposes with, how was it put earlier? "gnat's hind end" sensitivity, when we're looking for something way less accurate and simple. Thus I don't think we really need 3 different types of traps and filters before plumbing the gas, etc.

Also, I've really tried to do my due diligence, but the practical "how EXACTLY do I hook this up" is escaping me. I spoke with Restek, and they were about as condescending and dismissive as they could have been. I was planning on just grabbing some inexpensive 2 stage regulators, some swagelock connectors (although those are surprisingly expensive), and a multipurpose column (mxt-5?) and see what we get.

I'm being a bit facetious with that, I'm aware its more complicated. Actually, I've contacted a couple labs who are willing to put me in touch with an installer, but how much will that cost? I've got some money to put into this, but I could use some encouragement to keep me motivated. I'm super interested in the science here, and ready to geek out.

And does anyone have access to the 7673 autosampler/controller reprogramming utility? It's be cool just to see it move around, at least

[mrussell]

http://ipes.us/used/58901.pdf

http://ipes.us/used/58904.pdf

http://www.meadowshplc.com/pdfs/5890.pdf

I agree,use nitrogen for your carrier gas. You will need hydrogen for your FID though. One thing to remember is,heating your column when there is oxygen in it will damage it. So when you start it up,let the carrier gas flow for 15 or 20 minutes,with the oven cool. The detectors should be heating up during this time,and by the time that part is done they should have lit. The signal will be high at first,and should come down. If it stays high, then it means you probably have a leak somewhere. Get all that going good before you heat your oven up.

[osp001]

I'm unfortunately in a middle zone, where the manuals are written for commercial purposes with, how was it put earlier? "gnat's hind end" sensitivity, when we're looking for something way less accurate and simple. Thus I don't think we really need 3 different types of traps and filters before plumbing the gas, etc.

Fair enough- but give eBay a peek. Sometimes you'll luck out and find the right traps for $20 each, new-in-box old stock.

Also, I've really tried to do my due diligence, but the practical "how EXACTLY do I hook this up" is escaping me. I spoke with Restek, and they were about as condescending and dismissive as they could have been. I was planning on just grabbing some inexpensive 2 stage regulators, some swagelock connectors (although those are surprisingly expensive), and a multipurpose column (mxt-5?) and see what we get.

Swages aren't cheap, but- again: eBay for Swagelok and a lightly used column will save you a few hundred bucks easy.

Which part of the connection were you seeking help for? Cylinder-to-GC?

1) Nice, clean regulators. Connect to cylinders with face of gauges either perpendicular to the ground, or at a slight "up" angle for visibility. Teflon tape is not appropriate for CGA fittings. Wrench on, leak test (methanol is best- soap solution is strongly discouraged), tighten as appropriate.

2) You should have cleaned copper tubing specific to GC work; typically tubing is drawn with wax, which causes problems. Solvent cleaning yourself is a PITA, so buy the pre-cleaned stuff. I think Alpha Omega will sell you less than the 50' lengths sold by most suppliers. You will probably have to clean up the ends after cutting in order to accept the Swagelok fittings, so- pipe cutter (for 1/8" tubing), then file the shoulder carefully to remove any burr. You'll know when you have it right because you'll be able to fit the back ferrule on.

3) Install nut, then back ferrule, then front ferrule. See also: http://www.ecs.umass.edu/eve/facilities ... ctions.pdf

I always put a pen mark on one of the flat faces of the nut, so once you go finger-tight, it's easier to figure how many turns you've gone through to get that Swage to seat correctly. When finished, leak test with methanol.

You will need to connect the tubing on the other end- carrier gas, fuel gas, makeup gas. Post an image or two of what you have (image with the left side off, showing the existing plumbing that you can) and perhaps we can help you sort out which goes where. However, I have used FID with hydrogen for all three, then compressed air for the combustion in the FID, and it works with very high sensitivity although it's a bit of a trick to tweak it in: gotta make sure your air pressure and hydrogen pressure are in just the right zone- also true of nitrogen/hydrogen/air systems, but with hydrogen/air only the zone is harder to find.

So- hydrogen plumbed through a dryer, then hydrocarbon filter, and compressed air, plumbed through a dryer and a hydrocarbon filter. Each filter has Swagelok fittings on either end, so- lots of cutting and de-burring (there's a special tool for that, but if you don't do much of it a file is fine). In your case, if you are determined to leave out the drying and filtering steps, do so.

The usual caveats apply: hydrogen is one sneaky bastard, and compressed cylinders of hydrogen is just askin' for it.

As for your column- I personally prefer capillary GC, and would suggest an RTX-5. There are at least half a dozen on eBay right now, including a used one for under $100. I think I have 2-3 extra if that doesn't pan out. Post some images inside the GC showing the connectors, so that we may advise as to any parts you may need there. For example, the two cylinders at the top of this image:

[mrussell]

Do a search for 5890 site setup and installation guide.