Cj. Mason et al., The use of microwaves in the acceleration of digestion and colour development in the determination of total Kjeldahl nitrogen in soil, ANALYST, 124(11), 1999, pp. 1719-1726
An accelerated procedure for the determination of total Kjeldahl nitrogen i
n certified reference Chinese loam soil and real samples has been developed
. This method makes use of open-vessel single-mode microwave technology. Wh
en a direct comparison was made with a fully optimised thermal Kjeldahl dig
estion method an 8-fold decrease in digestion time was observed, reducing t
he time required for the digestion process from 120 min to 15 min for certi
fied reference soil, and a 2-fold decrease for a real soil sample of S.E. E
ngland soil. Extracted nitrogen was determined colorimetrically in a flow i
njection system making use of the Berthelot reaction. A comparison was made
between the use of a heated water bath and a microwave oven for the develo
pment of the indophenol dye. Development times were reduced from 140 s down
to 15 s, resulting in an increase in sample throughput from 36 samples per
hour on the thermally heated system to 60 samples per hour on the microwav
e-heated system. The limit of detection by the 3 sigma method was 14 mu g l
(-1) of nitrogen for the thermally heated system while a limit of detection
of 6 mu g l(-1) was achieved on the microwave-based system. A linear calib
ration of 2 orders of magnitude was achieved for both systems. The combinat
ion of the microwave Kjeldahl and flow injection with microwave-enhanced co
lour development greatly reduced the time required for the determination of
total nitrogen in Chinese loam soil, and recoveries of 100 +/- 2% of the c
ertified value of 640 mg kg(-1) were obtained. Similar recoveries and reduc
ed times to determination were also achieved for real soil samples.