By R. B. Bradstreet
Sm 4to, Hardcover, Burgundy textile, Gilt Lettered, 1965, Pp.239,
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Additional resources for The Kjeldahl Method for Organic Nitrogen
Example text
O n samples of t o b a c c o , linseed c a k e , leather, and wool, C a r t i a u x (64) treated 0 . 7 - 3 . 0 gm of sample with 5 ml of c o n c e n t r a t e d sulfuric acid and allowed the mixture to stand for 15 minutes at r o o m t e m p e r a t u r e before heating for several minutes. After cooling, 1 0 - 2 0 ml of peroxide are a d d e d in small portions, avoiding a large evolution of gas. After heating to expel t h e gas, the digest is boiled for 5 minutes and the p r o c e s s r e p e a t e d until a clear solution results.
Since with this high salt:acid ratio, both time a n d t e m p e r a t u r e a r e critical, a n d t h e digestion (at full heat) c a n n o t b e p r o longed after clearing. 3 gm of p o t a s s i u m sulfate p e r milliliter of acid, a n d digesting with full heat until clearing. A v e r a g e results of duplicate determinations a r e s h o w n in T a b l e X V I . 5 gm of m e r c u r y . W h e r e p o s sible, full heat w a s applied at o n c e . H o w e v e r , m a n y of the amino acids h a v e a t e n d e n c y t o foam, so that low heat a n d frequent shaking a r e THE BOILING PERIOD AFTER DIGESTION TABLE 47 XVI RECOVERY OF NITROGEN FROM AMINO ACIDS WITHOUT THE BOIL PERIOD Compound /-Lysine monohydrochloride /-Cystine Methionine Phenylalanine /-Histidine monohydrochloride ^/-Valine Arginine monohydrochloride Glycine Hydroxyproline Leucine b Alanine Glutamic acid Aspartic acid Tyrosine a b Gm K2SO4/ ml H S 0 Digestion time (min) Found Calc.
I y s s 90-10 y 340 320 300, 0 Grams K S 0 1 0 2 2 0 3 0 4 FIG. 8. Boiling points of H S O - H P O - K S 0 digestion mixtures. 2 4 3 4 2 4 indices of 8 0 % - 2 0 % and 7 0 % - 3 0 % mixtures b a s e d on the total volume of acid are s h o w n in Fig. 10. Although it c a n b e s o m e w h a t a m a t t e r of preference in selecting a combination of mixed acids, mixtures of 7 0 % - 3 0 % , a n d 8 0 % - 2 0 % sulfuric acid-phosphoric acid with p o t a s s i u m sulfate h a v e b e e n arbitrarily selected for r e a s o n s of high t e m p e r a t u r e s , liquid digests, and only slight differences in oxidation time of sample as c o m p a r e d with sulfuric acid-potassium sulfate mixtures.