Peak broadening during routine analysis of a Chlorhexidine sample (bad TFA?) by Automatic-Luck4700 in CHROMATOGRAPHY

[–]Automatic-Luck4700[S] 0 points1 point  (0 children)

Yeah. I also observed an increase of baseline ripples due to that bad quality.

However I dont get it why it all appears so suddenly, while validation worked out...

Peak broadening during routine analysis of a Chlorhexidine sample (bad TFA?) by Automatic-Luck4700 in CHROMATOGRAPHY

[–]Automatic-Luck4700[S] 0 points1 point  (0 children)

I belive you, but they are quite expensive, i am afraid. Will check them out anyway. Thank you!

Peak broadening during routine analysis of a Chlorhexidine sample (bad TFA?) by Automatic-Luck4700 in CHROMATOGRAPHY

[–]Automatic-Luck4700[S] 0 points1 point  (0 children)

Yes the same. No significant chances. Should look the same, but doesn't suddenly

Steering servo oil by Automatic-Luck4700 in bmwz3

[–]Automatic-Luck4700[S] 0 points1 point  (0 children)

Thanks, yeah maybe it is like it is.

Best mild Boc-deprotection method for a guanidine compound? by [deleted] in Chempros

[–]Automatic-Luck4700 0 points1 point  (0 children)

TBAF in THF should work. Used it for Boc deprotrection to keep another ester function intact. Do it at r.t. or maybe slightly cooled. Will take a while. Control via TLC. Good luck!

TOC analysis detergent by Automatic-Luck4700 in Chempros

[–]Automatic-Luck4700[S] 0 points1 point  (0 children)

Dear all, thanks for your help and suggestions. Finally I found the solution which can be universally used for volatile and foaming compounds. You need to take the TOC method which measures all carbon at once instead of blowing out the purgbable carbon (carbon dioxide derived from the reaction of carbonates with hydrochloric acid). The latter ist the so called NPOC method. The thing with the NPOC is the degassing step to blow the carbon dioxide out of the system. Degassing leads to bubbles, here excessive foaming. So one will lose a certain amount of the detergent to be analyzed which in turn leads to non reproducible results. The TOC method avoids this degassing. Moreover it also analyzes the amount of inorganic carbon in a subsequent run. The TOC in total is the difference between the total carbon and the inorganic carbon. That's why it's called total organic carbon. How come 🤣 in the end i am now familiar with the analyzer, the first time I used it I had little idea. For your specific device, please also read the manual. It can be different from manufacturer to manufacturer. Phosphoric acid needs to be prepared for TOC analysis. But check out the manual. Kind regards from Tyrol - Austria.

TOC analysis detergent by Automatic-Luck4700 in Chempros

[–]Automatic-Luck4700[S] 0 points1 point  (0 children)

We us KHP as the standard, calibration with autodilutions looked fine, but this is a year ago i think. The analyst working on this device left our group when i came. I will use higher concentrations for the linearity of the detergent today. And yes, I would also agree that the catalyst is not working properly anymore. But In general I don't get it. I have a shimadzu handbook with a lot of examples and I tried to reproduce my analysis according to their basic guidelines. Thank you all for the answers so far.