Separation of Dibutyl and Tributyl Phospahte

[praveenpaliwal]

Hellow, every body. We have one serous problem of the separation of Dibutyl phoshate (CAS NO. 107-66-4) and Tributyl Phospahte(CAS No. 126-73-8) . We have tried several columns for this like DB-1 DB-WAX, DB-1701 and DB-624 but both are co-eluted .
We want them separate so which GC stationary phase is suitable for it?
Either any derivatization technique is suitable for the separation

Praveen

[chromatographer1]

Are the two peaks the same size? Do you know the compounds are pure?

DBP should be very difficult, and TBP as well. Poropak P might be a solution but I have doubts.

Carbopack C with a 1% coating of FFAP?

Chromosil 310?

But the issue remains, how will you get the DBP through the detector ?

Rodney George

[praveenpaliwal]

SIr,

We have standard of Aldrich of both samples. OUr R&D expert also confirm that there is possibility of TRibutyl in Dibutyl also.
Now can u suggest us some literature or web site for the separation of these two's

Praveen

[chromatographer1]

My suggestion is to ask Aldrich to tell you the tests they use to determine purity.

I doubt that they use gas chromatography to determine purity, unless it is to revert the DBP and TBP back into the phosphoric acid and alcohol to determine the n-butanol and homolog alcohol content as one might do to determine the fatty content of a triglyceride, for example.

Please let us know if you find any literature on this subject. I would enjoy reviewing it. I would have many questions to propose.

good luck and best wishes,

Rodney George

[praveenpaliwal]

Sir,

I aasked aldrich for the same but they declared titrimetric purity not GC. I also asked them to tell us GC method if possible.
I am also trying to consult the literature and other technical person but I request u to keep in contect.

Praveen

[chromatographer1]

Praveen,

Having worked for Sigma-Aldrich, I will state this much:

If there were a method to determine purity by GC it is quite likely they would employ it.

Since they don't have a method to share with you, I suspect the DBP is too difficult an analyte for GC analysis.

I would also expect that NMR analysis would also be indicative of purity, as well as the titration they mentioned.

Good luck,

Rodney George

[bisnettrj2]

http://www.cdc.gov/niosh/docs/2003-154/pdfs/5017.pdf

Found a CDC paper where it seems they derivatize dibutyl and tributyl phosphate with BSTFA and inject on a "1.2 m x 6-mm OD; 3% OV-101 on 100/120 mesh Chromosorb WHP" packed column and detect via a "phosphorus FPD".

Hope that helps.

[praveenpaliwal]

Sir,

This is NIOSH MOA and we also have it, how we can derrivatized it it is not mention in this note.
CAN u tell us briefly, about derivatization.

IIndly in the monitoring sample this derivatization process is work or not?

Praveen