GC with FID

Feb 2013
2
0
Hello everyone!

I'm new here and I really need some technical/mechanical help on a project I'm working on here at Texas A&M.
I decided for my senior project to build a GC with an FID. After deciding this I realized the difficulty in finding a good publication or paper as a reference on how to do this. What I'm asking is if anyone can run down the steps and basic procedures on how to accomplish this task (or point me in the direction of a paper/publication/book/website on the matter). I have access to an electronics lab to add any sort of electrical parts to our detector. In addition, I will have the funds to order a column, injection port, and any and all other supplies I may or may not need, including chemicals. I have taken both an analytical chemistry class and lab, so I know all the background information on the subject of gas chromatography as well as flame-ionized detectors. As for carrier gas, we have access to all of the standard gasses, and the analyte will be various hydrocarbons, which, from my understanding, are the compounds to be used with an FID.

Thanks in advance for any and all help!

Note: I'm not looking for an undergraduate university lab procedure to build a very simplistic GC. For example, I've run across procedures to build a GC using laundry detergent as a mobile phase and some that don't make their own FID; this is not what I'm wanting. I really need someone with a mechanical/technical background to help me actually construct a GC with a working FID (since I will have access to facilities to accommodate any construction and expense); granted, it will be basic, but not so amateur that I could construct one at home.
 
Last edited:

Unknown008

CHF Hall of Fame
May 2010
1,658
37
Mauritius
Hello dek442! Welcome to CHF! :)

I would have liked to help you but unfortunately, I don't know much about the technical part of setting up a GC with FID, and since there are not many people on this site, I'm afraid you might not get the help you want. I however, hope that you manage to get the proper help. Maybe you could then share a little of what you learned on here so that others who will stumble on the same problem can in turn use it as reference. Also, I'd sure be curious to learn more about it myself :)
 
Feb 2013
2
0
Current Progress

Here is what I found out thus far, with a listing of everything I would need.


1) PARTS – Four main parts: Carrier gas w/pressure reg., Injection site w/ oven, Column, and the detector.
a) Carrier gas w/pressure regulator
i) Carrier gas – H¬2 because we are using an FID, it will be easier with a flammable gas.
ii)Pressure Regualator – Provided in the lab, they have plenty
iii)Also using a molecular sieve which we can make in the lab with glass ware and CaCl2, will remove moisture and anything else that could interfere with our results
b) Injection site w/oven
i)Oven - Three parts: The box, heating element, and temperature sensor.
(1)Metal box – will cover the injection port, column, and the FID. It will be insulated with either glass wool or something from home depot. Also need med temp rubber tubing to use as fittings for the openings
(2)Heating element – Something like this: http://www.omega.com/ppt/pptsc.asp?ref=SRT_heaters
(3)Temperature sensor – either a thermometer, or by this: http://www.vernier.com/products/sensors/temperature-sensors/go-temp/
ii)Injection site – Two option that I see, can come up with more. I like the first
(1)http://www.chemglass.com/product_view.asp?pnr=CG-4022
(2)http://chemglass.com/product_view.asp?pnr=CG-132
c)Column – Fused silica capillary column, suggested for hydrocarbons
i)http://www.restek.com/catalog/view/7718 column
ii)http://www.sisweb.com/lc/sge/siltite-fingertite-gc-ferrules.htm for connecting the column to the injector port and the FID
d)Detector – FID using this style: Hughes, D. E. P J. Chem. Ed. 1965, 42, 450. http://pubs.acs.org/doi/pdf/10.1021/ed042p450
i)Need to have connector for end of GC that turns up
ii)I can provide a Sterican long needle or we can use the shorter ones that the lab has as the cathode
iii)The flame doesn’t need to be strong and the anode needs to be fairly close
iv)The amplifier: http://www.vernier.com/products/sensors/ina-bta/


List of Items:
1) H2 gas cylinder
2) Pressure regulator
3) Molecular sieve - http://chemglass.com/product_view.asp?pnr=CG-1012 , http://chemglass.com/product_view.asp?pnr=CG-1013 , with glass wool at each end, and CaCl2 beads as the sieve in the open space in between.
4) Keck clamp(s)
5) Med temp rubber tubing, small diameter
6) Three way glass: http://www.chemglass.com/product_view.asp?pnr=CG-4022
7) Metal box: made by us
8) Insulation: probably a bunch of glass wool
9) Heating element: http://www.omega.com/ppt/pptsc.asp?ref=SRT_heaters
10) Temp sensor: Thermometer or this http://www.vernier.com/products/sensors/temperature-sensors/go-temp/
11) Really small rubber septum for the three way glass injection side
12) Heat shrink? Possibly
13) Column: http://www.restek.com/catalog/view/7718
14) Ferrules for column connection: http://www.sisweb.com/lc/sge/siltite-fingertite-gc-ferrules.htm
15) Sterican long needle or short needle for Cathode
16) Wiring to connect amplifier and use as Anode
17) Amplifier: http://www.vernier.com/products/sensors/ina-bta/
18) Vernier connection for computer
19) Small metal clamps and screwdriver for those
20) Razor blade for cutting tubing
21) Heat gun possible



I will keep you updated with progress!
 

Unknown008

CHF Hall of Fame
May 2010
1,658
37
Mauritius
Awesome! It sounds like it's going well ^^