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Gas Chromatography Calibration

I'm sorry. I know I'm suppose to share and write a post about having my article printed in the Yellow Pages Energy Guide. But, I think my recent experience during the GC calibration was very worth sharing.

Brief Introduction of our Gas Chromatography

Our research Chemical Reaction Engineering Group (CREG) have 3 Gas Chromatography (GC) Thermal Conductive Detector (TCD). All of them are HP Agilent 6890 model. We have labeled them as GC 1, GC 2 and GC 3. I have personally used 1 of the older GC-TCD (GC 2) when doing my masters degree 9 years ago. GC 2 is the simplest of our GC-TCD. It can only analyze gasses compound and have only 2 columns inside it which are Molecular sieve and Porapak N column.
GC 1 and GC 3 are far advance then GC 2. Both of the GCs are equipped with Flame Ionization Detector (FID) to analyze liquid product, which in our case are hydrocarbons. That means, GC 1 and 3 can analyze both gasses and liquid compound.

GC 2 and GC 3 (Both Agilent 6890 model) are arranged side by side in one of our research rooms.

On top of the above mentioned GC-TCD, there is also a unit of Gas Chromatography Mass Spectrometry (GC-MS) to power up our analysis capability. This GC-MS is very useful to identify and analyze liquid compound. GC-MS actually combines the features of gas-liquid chromatography and mass spectrometry to identify different substances within a test sample. In our research group we use it to analyze our pyrolysis, biomass, biodiesel liquid fuel and others. I'm not that familiar with GC-MS, but I plan to learn more about it in future. Now, for my ph.D, I'm more focused on using the GC-TCD.

The molecular sieve packed column and Porapak N column in GC 1

Oh yes, we also have one dedicated Perkin Elmer Gas Chromatograph Flame Ionization Detector (GC-FID). This GC-FID is very old, I think it has been around for more than 13 years. It has been used previously to analyze our gas to liquid products. Presently, a master student is using it to analyze her biodiesel from waste vegetable oil research.

Of all the GC brands, we have model from HP and Perkin Elmer but not Shimadzu.

Gas Chromatography Thermal Conductive Detector (GC-TCD) Calibration

All our 3 GC-TCD are in great demand now. The research group population has suddenly increased and all of us need to use this imperative analytical equipment. Unfortunately, the GC-TCDs are not in really good condition. Hence, we've called Agilent engineer to come and help us check on the GCs and calibrate it for us.

I wasn't around on the first part of GC-TCD calibration because I was in Kota Kinabalu with my wife and family for the International Conference on Chemical and Bioprocess Engineering in conjunction with the 23rd Symposium of Malaysian Chemical Engineers (SOMCHE 2009). However, my research colleagues were around for the GC-TCD calibration sessions. Unfortunately, the GC-TCDs could not yet be calibrated due to some problem. It was found that the molecular sieve packed column for GC 1 is not working anymore. So, CREG have to order a new mol sieve column.

Agilent engineer is replacing the mol sieve packed column in GC 1

Luckily we managed to order new mol sieve columns and the second GC-TCD calibration session were carried out last week. This time I was around and we work closely with the Agilent engineer. GC 1 has 5 columns inside it and it took some time to work on the valve switching between the valves. The valve switching is an important feature when there are many columns in a GC. This is because a column can only be suitable for certain chemical compound separation, while the others are suitable for other compounds. We calibrated GC 1 with Agilent natural gas standard and successfully managed to get all peaks in the chromatogram at the end of the day.

The engineer is thinking how to solve the mess in GC 3

The next day, the engineer continue worked with GC 2 and GC 3. However, he only managed to touch GC 3 after lunch. GC 3 has more chronic problem, it has one of its capillary column torn. He discovered this problem together with a ph.D student doing Plasma Reaction Research. However, the engineer has successfully connect the capillary column again.

HP capillary column is torn.

Conclusion of GC-TCD Calibration Session

To conclude the GC-TCD calibration session:

GC 1 - Successfully calibrated with Agilent natural gas standard.
GC 2 - Successfully calibrated with Agilent refinery gas standard.
GC 3 - Need to be further calibrated. Probably need 2 days to complete the job. I have contacted Agilent to come and rectify GC 3. We are still waiting the answer from them. I'll follow up with them again tomorrow.

I look forward to conduct my research as soon as possible... :) wish me luck.

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posted by Kipas Repair JB @ 5:07 PM,


At Saturday, September 05, 2009, Anonymous Mass Spectrometry said...

More info on mass spec is available from IM Publications. Journals and books for all interested in the subject.

At Saturday, September 05, 2009, Blogger Kipas Repair JB said...

Thanks for the information Mass Spectrometry.


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The Author


I’m Zaki. I used to be a project, process and chemical engineer. Few years ago I successfully became a Chartered Engineer (IChemE) and Professional Engineer (BEM). I'm now employed as a chemical engineering educator/researcher/consultant. Hope you like reading my blog. I welcome any feedback from you. My email: zaki.yz[alias]gmail.com. TQ!

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