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Gas Chromotograpy as a hobby
Posted: Fri Mar 09, 2007 2:44 pm
by zetron
Hello: My name is David Roach. I worked in Chemical QA at several companies before retiring in 1998. When I started GC work at Magnafux we were cutting and weighing, using MECHANICAL integrators and estimating areas with triangles.
I have acquired a Carle Instruments Basic GC and several packed columns. The older Carle Engineering GC which I also bought on Ebay I have taken apart. I plan to place the oven from the latter into the Portable Basic GC. The oven that the portable basic GC came with only has room for columns that have been bent into an ellipse instead of a normal circular column.
I have a Helium cylinder, VWR regulator, SS tubing and fittings, Matheson GAS MISER and a filter. The columns: six foot 80% Porapak N + 20% Porapak Q 50/80, seven foot LMS13X 40/60, three foot PTA (either first or last column), eighteen foot 27% BEEA and others, four foot Durapak OPN Porasil 50/100.,10% Carbowax 20M 80/100 Chromosorb,Carbowax 20M.
The setup for the GC I will end up with will have the hot wire detector from the Carle Basic and the detectors from the older GC (they are in a block and consist of two gold plated electrodes a few millimeters apart?). With this old and portable equipment I will only be able to do ISOTHERMAL runs.
I am initially interested in water samples and ethanol. Any guidance would be appricated.
DR Roach
Posted: Fri Mar 09, 2007 3:36 pm
by chromatographer1
Your Porapak column is probably used to perform ethylene analysis (it will separate CO2 from methane, ethane and acetylene from ethylene).
The mole sieve 13X is used to separate oxygen carbon monoxide, and methane from nitrogen.
The BEEA and Durapak columns are used to separate propane and propylene and butane from its olefin and diolefin homologs.
The Carbowax columns on Chromosorb {P?} or {W} would be good for ethanol analysis except isopropanol will elute very close to ethanol.
I hope this information will be helpful.
Rod
GC as hobby
Posted: Fri Mar 09, 2007 4:16 pm
by zetron
Rod: Thanks, that information will be very helpful. It appears most of the columns I have would not be useful for water analysis?
I want to investigate H2O and some unusual Platinium group complexes that are soluble at pH 3 or so and precipitate out at pH 8.8. The term used is Orbitally Rearranged Monoatomic Elements ORMEs.
I have a DataQ DI-194RS starter pack which I want to use to send the data from the GC detectors to a computer. I have a program that is suppose to quantify the areas under curves (have not tried it yet). Are there any programs out there for this purpose that are free?
I have a couple Hamilton syringes (undoubtable will need more). I also have 'slide in modules' for a Varian 3200 GC, one allows RAMPING. But, there are 36 connector strips on the back. I would not know how to INTERFACE this module with the Carle Basic GC oven?
DR Roach
Posted: Fri Mar 09, 2007 5:31 pm
by GOM
David,
Your mixed Porapak N and Q column will be good for water and ethanol
Regards,
Ralph
Posted: Fri Mar 09, 2007 7:36 pm
by zetron
Thanks Ralph. I found another column; a short one, six inches LM513X 80ing/100.
I also found a heating "slug" with SS tubing wraped around it and controllable with a variac and with an analog temp meter.
Are most "portable GCs" ISOTHERMAL only"?
David
David's Hobby
Posted: Fri Mar 09, 2007 7:44 pm
by chromatographer1
David,
The hardware you describe is a methanizer. It is a catalyst column used with hydrogen carrier to convert ppm levels of carbon monoxide and carbon dioxide to methane. The methane is then sent to a FID for measurement.
Usually a portable GC does not have the energy resources to conduct anything but isothermal and low temperature analyses.
It takes a lot of battery power to heat an oven above 100°C, much less above 300°C.
Your analysis of ethanol and water using a Porapak column will require temperatures above 120°C. Molecules larger than 6 carbons will not be feasible with that column. Your carbowax 20M column will handle molecules up to 20? carbons.
Your hobby GC is really that, a hobby instrument, not a business instrument, unless your business or hobby is quite limited.
Enjoy !
Rod
Posted: Fri Mar 09, 2007 7:56 pm
by GOM
Hi David
Your LM513X is probably LMS13X i.e. mol sieve 13X.
As Rod said, your portable one will be isothermal. A trick for water at a lower temperature is to drop a pellet of calcium carbide in the injection port. Water injected reacts to form acetylene (the old carbide lamps).
Cutting and weighing? -----luxury!! (to be said in a Yorkshire accent

)
Regards,
Ralph
David's hobby
Posted: Fri Mar 09, 2007 8:15 pm
by chromatographer1
Yes, the LMS 13X stands for Linde Molecular Sieve 13X.
The Durapak is no longer available.
The numbers involved indicate mesh size, the size of the particles of the packing. 40/60 or 80/100
Are you measuring water content of samples or measuring impurities found in water? I am confused (but it's not the first time).
best wishes,
Rod
Posted: Fri Mar 09, 2007 8:26 pm
by zetron
Thanks Rod, thanks Ralph: i suppose my GC setup could be used for a Moonshine whistey maker to tell him if his distillate will cause him to go blind or cause him to have a hangover??
Rod: I am puzzled that the methanelizer was in this GC as it has no FIDs. At least there were no Hydrogen lines. It has labelled lines for Helium and Nitrogen. I knew that the portable GC would be limited in power, if it were a REAL portable. The one I have runs on AC. One that I bid on AND LOST at Ebay HNU GC311 also had an AC powre cord visable. I REALLY wanted to win that GC. It was such a nice looking compact one!
I had someone from a Yahoo group phone me about my putting together a GC. He suggested that people would want their BATCHES of ORMUS (ORMEs) tested. It seems no one is sure that the Ormes would show a elution peak. The Home Brew Ormus people have claimed LOTS OF THINGS for this mixture of elements.
It is said by some that water containing Ormes when distilled still contains these Ormes, that these substances boil over with water. They also claim that "ordinary" water is not really a pure substance; water made from burning Hydrogen in Oxygen is very different in properties and LACK of content.to me All this has yet to be deminstrated .
Ralph I like the calcium carbide idea.
David
Posted: Fri Mar 09, 2007 8:47 pm
by zetron
Rod: I am hoping to show that there are some hither to unknown substances in water; even distilled water.
But who would be stupid enough to try chromatography on DISTILLED WATER?
So I guess I am looking for IMPURITIES in water. What I hope to find, at least in my "Batches of ORMUS are unknown peaks for the Orme elements. I was reseaching Nanoparticle gold sols when I came across this ORMUS thing. A very long read from David Radius Hudson who supposedly discovered this material on his farm in Arizona. It was a white powder (ghost gold) that did not assey as anything when examined by US Chemists in the 1970s. With a semiquant type (circa 1940's) carbon arc spectroscope in Soviet Russia they found the white powder contained the platinium group elements .
The Soviets used Argon around the arc and ran behond 300 seconds which is why they discovered these Ormes. The whole Hudson ORME thing went up in smoke when he had a dangerous chemical spill at his piliot plant in AZ. The Vitamin Freak Crowd has taken this over and ORME is selling for $50.00 for half ounce.
I want to try and find out if this material is real. The Orme elements are mono or diatomic supposedly with copper paired electrons. They are like ceramics rather than metals. You can read about this on Yahoo group "ORMUS".
I want to use Gas Chromatography on water samples of ormes
Sounds crazy, no;
David
Posted: Sat Mar 10, 2007 1:31 pm
by GOM
yes
Posted: Mon Mar 12, 2007 7:12 am
by Peter Apps
This reminds me of a prospective customer who wanted me to analyse water for previously unknown silicon compounds.. He had been all around the country (SA) taking samples from natural water sources. I don't recall the exact details of his sampling protocol but it involved plastic tubing and an aquarium pump. I also do not recall whether the compounds were elixirs of eternal life or deadly toxins about to wipe the human race off the face of mother Earth.
Despite my best efforts to put him off he insisted on paying to have samples run by GC-MS, and although I never got feedback on the report he was probably delighted to find that there were some "unknowns" among the peaks.
And of course there is still red mercury ................
Peter
Posted: Mon Mar 12, 2007 4:15 pm
by zetron
Peter: I guess there are a lot of people out there looking for this "elixer of life"? I will not bother a compentent Scientist with this sort of stuff, I WILL TRY AND DO IT MYSELF.
After my reseach into gold colloids and ORME and ORMUS I have QUESTIONS and a little more respect for Alchemists. Although I am not going to mess with Hg or HF!!! Their techniques leave much to be desired.
The gold colloid sells for $110.00 or so for a quart. I think there is only $1.00 worth of gold in it. ORMUS is much more expensive.
Oh well, shooting various "ORMUS samples" into my (GC?) will be part of the hobby. There are undoubtable more suitable and interesting substances to experiment with.
David
Posted: Mon Mar 12, 2007 4:55 pm
by GOM
David,
With respect, please read
http://www.answers.com/topic/pathological-science. (I worked in the lab that was involved with Polywater)
I wish you well in getting your GC to work.
Regards,
Ralph
Posted: Mon Mar 12, 2007 7:36 pm
by zetron
Ralph: Thanks, I know what Pseudo-Science and CargoCult Science are. I don't think I have heard of 'poly water".
The individual who first started the ORME thing weaved a very complex tale that covered a great range. If it was all hucksterism I would be very supprised!
The idea expressed in the article you referenced, about Psedo-Science continuing to be "believed" by people even after it has been proven false simply reinforces the idea in "What the Bleep Do We Know". We each choose our (QUANTUM) reality.
I think my GC will end up more like a STILL. For my analysis of this UNKNOWN I also need more information from the people making the substance. These people are not interested in proper technique, even with using a pH meter.
There are undoubtably old methods like the Calcium Carbide idea that I do not know about.
David