I am using Freeze-pump-thaw cycle to remove oxygen and moisture from the solvents. Can anyone tell me how to measure the oxygen and moisture level in treated solvents?
I agree with Gabriel that KF ist the best way to determine water.
Due to the fact, that O2 is a common contaminent in aqueous solution, which has to be removed (typically by bubbling N2 through the solution for 10 min -- very efficient) prior to polarographic meassurements. That is done because O2 has two polarographic steps superimposing the step of the actual analyte. The same method might be used to determine O2.
But I'm sorry, I've got no reference for this approach in non aqueous solvents....
KF is indeed often the best method for moisture in solvents. Make sure that the solvent is compatible with the method. I learned first hand that it is not applicable to acetone.
You might try modifying one of the commercially available methodologies for D.O. in water based on either the Indigo Carmine Method or the Rhodazine D™ Method. If your solvent doesn't dissolve the colored product, you might try using say a 1:1 dilution with degassed methanol. An appropriate blank as well as extreme care would be required to get a truly meaningful result. The vendors found via search were Hach Co. and Chemetrics; they may not be the only ones making such kits.
You may determine the water content in (aprotic) solvents also by 1H NMR (if you have direct spectrometer access), this is convenient and reliable despite the fact that you have to do an external calibration (PULCON or similar) for the quantification. References:
G. Wider, L. Dreier, J. Am. Chem. Soc. 2006, 128, 2571-2576.
M. Baseda Krüger, C. Selle, D. Heller, W. Baumann, Journal of Chemical & Engineering Data 2012, 57, 1737-1744.
There are two methods based on the use of Karl Fischer reagents, or Karl
Fischer titration, to measure moisture content.
(1) Volumetric titration
(2) Coulometric titration
The solvent-resistant oxygen probe OXSOLV measures oxygen partial pressure in most polar and nonpolar solvents (except fluorinated and some chlorinated hydrocarbons). It is based on optical detection principles (REDFLASH technology) and can be used for short-term applications in pure and complex organic solvents. A list of tested solvents is available on request.
One important question is: How low a level of water in solvents do you need to determine? I found that a GC with a Thermal Conductivity detector was much more accurate than Karl Fischer at low water concentrations. If you are dealing with very low levels of water, you will also need to make some standards (which will involve making some ultra-low water solvents). Message me if you need some procedures for producing ultra low water solvents.