Analytical Solution required

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G.A.Raman
G.A.Raman's picture
Analytical Solution required

Dear Members,
I need a reliable method for estimation of Triflic acid content in the Triflic anhydride samples.
I tried with a GC method in vain; I got distinct peak for triflic anhydride whereas the triflic acid gave either offset of background or noisy chromatogram with no peak.
I am also trying out some titration methods by derivatisation but its in vain.
Kindly help me with your knowledge.

tsragu
tsragu's picture
Can it be tested by the

Can it be tested by the procedure used for acetic anhydride.

mallesh.jubburu
mallesh.jubburu's picture
titrate it agaist methanolic

titrate it agaist methanolic Morpholine solution

G.A.Raman
G.A.Raman's picture
Dear Mr.Mallesh,

Dear Mr.Mallesh,

Quite interesting to understand that morpholine will involve in titrating triflic anhydride. A little more info such as a suitable indicator and titration procedure would really help me.

Thank you Mallesh for your kind interest and awaitng for your earnest reply.

mallesh.jubburu
mallesh.jubburu's picture
Dear Raman,

Dear Raman,

Were you able to get any method for  determining % of triflic acid in triflic anhydride.
i am having the same problem with GC method.
If you got any solution please provide me

technologist
technologist's picture
 Interesting to note this.

 Interesting to note this.
Have you tried the method used for analysis of trifluoroacetic anhydride.
I think same can work.

G.A.Raman
G.A.Raman's picture
Except NMR no method works

Except NMR no method works for this if you could provide any suggestion. what method of trifluoroacetic anhydride do you say? I tried titration by derivatization also but not fruitfull.

mallesh.jubburu
mallesh.jubburu's picture
 we are analysing

 we are analysing trifluoroacetic anhydride by gc also,using 100% Dimethylpolysiloxan gc capillary colimn,dimensions are 0.32mm I.D  ,5.0 nicron film thickness, 30m length .
Inj port temp -100ºC
Detector temp-150ºC
Column temp prog : at 0 min 80ºC to120ºC in 5 min  and hold for 10 min
Detector:FID
Column flow :0.5mL/min
Split ration 1:50
Inj volume:2 uL neat

technologist
technologist's picture
 That is my point. When we

 That is my point. When we follow The same method for trfilic anhydride it is giving many humps (No clear peaks) is it because of hydrates, fuming etc or what. I am not an expert in analyticals but a process development engineer.

So any suggestion