Chromatography Forum

Hello,
i want to anayze the Anhydrous HCl and free chlorine (Cl2)gas on GC with TCD Detector , is it possible or not and if possible then please suggest the suitable packed column for this kind of analysis.
is there any suitable method is available then please suggest me.


regards
chandresh

Hello,
i want to anayze the Anhydrous HCl and free chlorine (Cl2)gas on GC with TCD Detector , is it possible or not and if possible then please suggest the suitable packed column for this kind of analysis.
is there any suitable method is available then please suggest me.


regards
chandresh

Hi
"is it possible ,but very short "(с) . HCL is very corrosive agent t for iron, copper, aluminum . Especially in the presence of water and oxidizing agents such as chlorine

For the analysis of gaseous HCL used glass gase analyzers. In the Soviet Union used the inticator sobent tubing analizer type АГХ [AGH] http://www.analytpribor.ru/?page=170, now days use ECD end mass-selective analizer such as http://www.analitpribors.ru/OKA.html.
There is no doubt that you have in the country are instruments of similar purpose.

Dear DSP007
Thanks For Your Support.
The Paper is in Russion or any other langeuage if the other leanguage is available then please send me the link.
also i want to use GC so if u know the GC Column then please suggest .

regards
Dr.Chandresh k.Soni

Please be aware that the standard hardware found in a TCD will NOT tolerate long exposures to chlorine gas or HCl.

If you would look at the literature you will find that such analyses have traditionally been performed on packed silica gel columns or on Krytox phases coated onto the carbon based supports.

best wishes,

Rod

I am just wondering if Chandresh has been able to perform this GC analysis yet? We are also trying to analyze HCL in the same manner. Any helpful information would be greatly appreciated.

What additional information do you need?

An actual chromatogram?

Part numbers of the gold plated TCD parts?

Sorry I don't have any specifics for you.

Good luck,

Rod

We are looking for a method that will give us forerun impurities in HCL. We are contemplating on putting cryogenics on a GC, but are worrysome on spending lots of money without knowing if this is even going to work? We have a Krytox column, but the HCL, and HF just come out so fast that there is no time to see anything on the front end.

Use a silica gel column to gain retention.

Go to technical service at Supelco and ask for their recommendations.

They have decades of experience with packed columns.

Glass lined or fused silica lined SS with quartz wool with silica gel should get the job done, and they may have other suggestiions.

I no longer work for Supelco since 2008.

best wishes,

Rod

I don't know if they will work (trace metal contamination is possible) but there are packings called Unibeads 1S, 2S, and 3S.

They are silica - glass based porous beads. I have not heard of anyone using them for HCl or HF but they are not that expensive.

I would try micropacked versions first, maybe a 1 meter 1mm ID, FS coated SS with quartz wool.

Let the Forum know if that works.

Remember that HF will destroy a TCD quickly unless precautions are taken.

best wishes

Rod

I have seen the separation of HCl and Cl2 on a 6Ft Tenax column at 80°C. The HCl came out in just over a minute and the Cl2 in 2.7 minutes. I do not have details on mesh size or column flow, but I would guess that this was done at 30ml/min of Helium. Column should be made from nickel and all tubing should be made from nickel or Hastelloy.

Gasman

Tenax will be destroyed by HF and won't tolerate Cl2 for very long.

If you only have a few samples to test it might be ok if you don't expect exact results from Cl2.

Gasman gave a good suggestion but I don't know how long the column will last? Any info Gasman?

I remember the first time I tried to inject HF on a porous polymer column. It looked like styrene sprayed with acetone in a microwave oven. It wasn't pretty.

best wishes,

Rod

The only copy of the chromatogram that I have is dated August 1992 and was analyzed on a HP5890. This was done by a major German chemical company who I am sure had researched this thoroughly and they had found that Tenax was the best solution for this analysis at that time. I have no data on column life.

Gasman