From: Jonas Nilsson (jonni$##$ifm.liu.se)
Date: Tue Feb 22 2000 - 07:33:57 EST
Hello
I've just got som new analysis results on my troublesome amidines.
After drying for 3 hours at 90 deg centigrade in vacuum a new analysis
was made.
This is the results:
Theory : First result : Rigourus drying result
C 64.0%:51.7%:59.9%
H 6.4%:5.3%:5.7%
N 13.4%:11.4%:11.4%
Ash content 900 deg centigrade in air overnight:8.9%
The new analysis results are now within publicable (0.26% from theory)
limits if i use the following contaminants:
13.2288% CH3COOH (1.066eq)
8.1516% CO2 (0.896eq)
However this does not seem very good... The total amount of base
(CHCOOH/CO2) should not be much above one equivalent. There shoult also
be some water and it is not possible to match against CH3COOH/H2CO3 for
instance.
Maybe the different values is due to degradation at 90 deg.
There is also the ash content. 8.9%! This much cannot be inorganic
contamininant. Remember I have run RP-HPLC with MeOH/H2O/CH3COOH just
before. I have no explanation of this.
Does anybody know any compound containing only CHNO that will not
evaporate off at 900 deg. in air? Could some of my sample be left in the
elemental analysis apparatus?
What is wrong with theese amidines?
/jN
-- _____________________ _____________________ | Jonas Nilsson | | | |Linkoping University | | Telephone | | IFM | | --------- | | Dept. of Chemistry | | work: +46-13-285690 | | 581 83 Linkoping | | fax: +46-13-281399 | | Sweden | | home: +46-13-130294 | |_____________________| |_____________________|__________________
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