Section 32: KJELDAHL DIGESTION PROCEDURE
1. Select an appropriate volume of sample to be placed in the 500 to 800 mL Kjeldahl digestion flask.
expected TKN mL of sample
concentration (mg/L) to use
0 to 1 500 (use 800 mL flask)
1 to 10 250
10 to 20 100
20 to 50 50
50 to 00 25
Dilute if necessary to 300 mL with ammonia free distilled water.
2. CAREFULLY add 50 mL of digestion reagent. If large amounts of organic matter are present, an additional 50 mL of reagent must be added per gram of organic matter. (This may be estimated from volatile solids information).
3. Mix thoroughly. (Incomplete mixing can cause bumping during the digestion and may result in glassware breaking or loss of sample).
4. Add several glass beads of boiling chips to the flask.
5. Place flask on digestion apparatus and heat to boiling and continue boiling until you see the formation of dense white fumes (SO2).
6. Continue to digest the sample for 30 minutes more. As the digestion continues, colored or turbid samples will turn clear or straw colored.
7. Cool the flask and dilute the sample with 300 mL of ammonia free distilled water. Mix.
8. Add 0.5 mL phenolphthalein indicator.
9. Tilt the digestion flask and CAREFULLY add a sufficient amount of sodium hydroxide - thiosulfate reagent to form an alkaline layer (pink zone) in the bottom of the flask. Usually 50 mL of reagent is needed for every 50 mL of digestion reagent used.
10. Connect the flask to the distillation apparatus, mix thoroughly and distill 200 mL of distillate into a boric acid absorbing solution. (See Section 11 for the distillation procedure.)
11. Determine Total Kjeldahl Nitrogen as ammonia using one of the methods outlined in Sections 12, 13, and 14.
NOTE: For the spectrophotometric method, the blank and standards must be treated by the digestion procedure.)