title: A simultaneous, direct microwave/ultrasound-assisted digestion procedure for the determination of total Kjeldahl nitrogen.
abstract: Simultaneous direct irradiation with microwaves and ultrasound was used to determine total Kjeldahl nitrogen. The method involves chemical digestion in two steps, mineralization with sulfuric acid and oxidation with H(2)O(2). The most influential variables for the microwave/ultrasound (MW/US)-assisted digestion were optimized using tryptophan as the model substance. The optimum conditions were: H(2)SO(4) volume, 10 mL; H(2)O(2) volume, 5 mL; weight of sample, 0.05 g; MW power, 500 W; US power, 50 W; digestion time, 7 min (i.e., 5 min mineralization and 2 min oxidation). A modification of the classical Kjeldahl (Hach) method and an US-assisted digestion method were used for comparison. The latter was also optimized; the optimum conditions were: H(2)SO(4) volume, 10 mL; H(2)O(2) volume, 5 mL; sonication time with H(2)SO(4), 15 min; sonication time with H(2)O(2),10 min; US power, 50 W; weight of sample, 0.05 g. Five pure amino acids and two certified reference materials (NIST standard reference materials 1547 (peach leaves), and soil, NCS DC 73322) were analyzed to assess the accuracy of our new MW/US-assisted digestion method, that was successfully applied to five real samples. The significant reduction in digestion time (being 30 min and 25 min for classical Kjeldahl and US-assisted digestion methods, respectively) and consumption of reagents show that simultaneous and direct MW/US irradiation is a powerful and promising tool for low-pressure digestion of solid and liquid samples.
authors.affiliation: Departamento de Química, Universidad Nacional del Sur, Av. Alem 1253, 8000 Bahía Blanca, Argentina.
authors.forename: Claudia
authors.initials: C
authors.lastname: Domini
authors.forename: Lorena
authors.initials: L
authors.lastname: Vidal
authors.forename: Giancarlo
authors.initials: G
authors.lastname: Cravotto
authors.forename: Antonio
authors.initials: A
authors.lastname: Canals
mesh_terms: D000596:Amino Acids / Q000737:chemistry; D008872:Microwaves; D009584:Nitrogen / Q000032:analysis* / Q000737:chemistry*; D014465:Ultrasonics
chemical_list: D000596:Amino Acids; D009584:Nitrogen