RAPID KJELDAHL

BENCHNOTES
Rapid Kjeldahl Straight, Pkg. of 5 (Model 23040-05)
Straight, Pkg. of 25 (Model 23040-25)
Methodology for the 5. Two 25 ml Class A burets
Determination of Nitrogen
6. 500 ml Erlenmeyer flasks
in Paper Products with the
Rapid Digestor and the Reagents

RapidStill II (All reagents should be reagent grade and nitrogen-free.)

1. Sodium hydroxide 45% (w/v) pellets or beads for

Principle: This method covers the nitrogen determination: Dissolve 450 g sodium
determination of organic nitrogen in hydroxide (NaOH) in deionized water. Cool.
Dilute to one liter with deionized water.
paper products including those
containing glue, adhesives and other 2. Methyl red/methylene blue indicator: Dissolve
collagenous material. 200 mg (0.2 g) methyl red in 100 ml ethyl alcohol.
In a separate beaker, dissolve 200 mg methylene
blue in 100 ml ethyl alcohol. Combine two parts
Apparatus methyl red with one part methylene blue solution
and mix.
1. Labconco Rapid Digestor:
Rapid Digestor 4 (Model 23080) 3. Boric acid/indicator solution 2% (w/v): Dissolve
Rapid Digestor 25 (Model 23012) 20 g boric acid (H3BO3) in 800 ml of deionized
water. Add 10 ml methyl red/methylene blue
2. Labconco Fume Removal System: indicator solution and dilute to one liter with
Fume Removal System-4 place (Model 23540) deionized water.
Fume Removal System-25 place (Model 23500-25)
4. Sulfuric acid (H2SO4) - concentrated
3. Labconco Rapid Distillation Unit:
RapidStill II (Model 65200) 5. Red mercuric oxide (HgO) or cupric sulfate (CuSO4
or CuSO4 • 5 H2O)
4. Labconco 250 ml Digestion Tubes:
Volumetric, Pkg. of 5 (Model 23030-05) 6. Potassium sulfate (K2SO4) suitable for nitrogen
Volumetric, Pkg. of 25 (Model 23030-25) determination

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7. 0.2N sulfuric acid (H2SO4) solution 11. When distillation is complete, fill a class A buret to
the mark with 0.2N sulfuric acid (H2SO4) and titrate
8. Alundum boiling stones to the purple endpoint. Correct for reagent blank.

Procedure %N = (ml std. H2SO4 - ml H2SO4 blank)(N H2SO4)(1.4007)

gram sample weight

1. Cut paper samples into pieces (approximately 1" x

Example:
1/2"). Weigh samples and place in digestion tubes.
blank = 1 ml sample = 1 gram
A one gram sample works best for paper containing acid added = 11 ml
3% nitrogen.
%N = (11 ml - 1 ml)(0.2N H2SO4)(1.400)
2. Place weighed sample in 250 ml digestion tube with 1 gram
0.42 g HgO, 9.0 g K2SO4, and 15 ml H2SO4.
%N = 2.8%
3. Place digestion tubes in Rapid Digestor which has %Protein = 17.5%
been preheated to 410° C.
Notes
4. Digest for 45 minutes. When digestion is complete,
remove tubes. Make sure digestion sample is clear. 1. Run a blank sample (reagents only, no sample) and
If necessary, digest longer until sample is clear and subtract the milliliters of H2SO4 consumed by the
then cool for ten minutes. blank from that consumed by the sample as
indicated in the calculation.
5. Add 50 ml deionized water to each tube, dissolving
all crystallized material. It may be necessary to
place tubes back in the Rapid Digestor, to expedite 2. When titrating, titrate to the purple endpoint. Do
dissolving the crystallized material. Allow to cool. not titrate all the way back to red.
Cooling times depend on the temperature and
circulation of air around the tubes and may require 3. With careful technique, this equipment will give
adjustment depending on your conditions. Do not results with a relative standard deviation of no
allow hard cakes to form. greater than 1.5%.

6. After the sample has cooled, attach digestion tube to 4. All testing done at our laboratory was performed
the distillation head and twist securely in place. with a Kjeldahl digestion mixture containing
K2SO4/TiO2/CuSO4 in the ratio 10/0.3/0.3.
7. Place delivery tube in 500 ml Erlenmeyer flask
which contains 50 ml boric acid/indicator solution. Reference
The tip must be below the surface of the boric
acid/indicator solution. Official Methods of Analysis AOAC. 15th ed.
Arlington, VA: (1990) • 7.032, 24.038 - 24.040.
8. Add approximately 80 ml sodium hydroxide
solution to the digestion tube. This methodology is for reference only. It is not a
citable document. It is based on data we believe to be
9. Set the RapidStill II for 8 minutes. reliable. It is offered in good faith but without
guarantee.
10. Start the distillation process and steam vigorously
until 125 ml of distillate collects.
 RAPID KJELDAHL
BENCHNOTES
Rapid Kjeldahl 4. Labconco 250 ml Digestion Tubes:
Volumetric, Pkg. of 5 (Model 23030-05)
Methodology for the Volumetric, Pkg. of 25 (Model 23030-25)
Straight, Pkg. of 5 (Model 23040-05)
Determination of Total Straight, Pkg. of 25 (Model 23040-25)

Kjeldahl Nitrogen in Water 5. 250 ml Erlenmeyer flasks or flat bottomed

Florence flasks
with the Rapid Digestor
and the RapidStill II 6. Spectrophotometer with sensitiviy less than 5 ppm

Reagents

Principle: This method covers the (All solutions must be made with ammonia-free water)
determination of free ammonia and
1. Mercuric sulfate solution: Dissolve 8 g mercuric
organic nitrogen in drinking water, oxide (HgO) in 50 ml 1:4 sulfuric acid (10 ml
surface and saline water, and domestic H2SO4: 40 ml deionized water) and dilute to
100 ml with deionized water.
and industrial wastes.
2. Sulfuric acid-mercuric sulfate solution (digestion
Apparatus solution): Dissolve 267 g potassium sulfate
(K2SO4) in 1300 ml deionized water and 400 ml
1. Labconco Rapid Digestor: concentrated H2SO4. Add 50 ml mercuric sulfate
Rapid Digestor 4 (Model 23080) solution in step 1 and dilute to two liters with
Rapid Digestor 25 (Model 23000, 23006, 23012) deionized water.

2. Labconco Fume Removal System: 3. Sodium hydroxide/potassium sulfide solution: Add

Fume Removal System-4 place (Model 23540) 500 g sodium hydroxide (NaOH) and 10 g potas-
Fume Removal System-25 place (Model 23500-25) sium sulfide (K2S) to 700 ml water in a one liter
container on a magnetic stirrer in a well-ventilated
3. Labconco Rapid Distillation Unit: area. Agitate until dissolved, then dilute to one liter
RapidStill II (Model 65200) with deionized water. Cool before using.

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4. Boric acid/indicator solution: Add 20 g boric acid evaporation is complete) without using the Fume
(H3BO3) to 800 ml of water, dissolve and dilute Removal System. After sulfur trioxide (SO3) gas
with deionized water to one liter. Keep covered to evolves, conduct the digestion phase for 30 minutes
prevent carbon dioxide (CO2) contamination. with the Fume Removal System in place.
Premix two volumes of .2% methyl red in 95%
ethanol with one volume of .2% methylene blue 6. Make sure digestion sample is clear. If sample is
(prepare fresh every 30 days). Add 10 ml of the not a clear liquid, digest longer unitl sample is clear.
indicator solution to boric acid solution if perform-
ing titrimetrically. 7. Allow to cool. Cooling times depend on the
temperature and circulation of air around the tubes
5. 0.02N standard sulfuric acid. and may require adjustment depending on your
conditions. Do not allow hard cakes to form.
6. Nessler reagent: In deionized water, dissolve 100 g
mercuric iodide (HgI) and 70 g potassium iodide 8. Add 50 ml of deionized water to each digestion tube
(KI). Add this slowly to a cooled solution contain- and keep covered.
ing 160 g NaOH diluted in 500 ml of deionized
water and dilute with deionized water to one liter. 9. Determine the nitrogen content titrimetrically or
colorimetrically.
7. Ammonium chloride (stock solution): 1.0 ml =
1.0 mg NH3-N. Dissolve 3.819 g NH4Cl in deion-
ized water and dilute to 1 liter in a volumetric flask.
Titrimetric Method

8. Ammonium chloride (standard solution): 1.0 ml = 1. Add approximately 50 ml of 2% boric

0.01 mg NH3-N. Dilute 10.0 ml of the stock acid/indicator solution to each receiving flask.
solution in step 7 to one liter with deionized water .
2. Twist the distillation tube securely in place on the
RapidStill II. Place an Erlenmeyer flask containing
Procedure the receiving solution (Reagent step 4) at the
receiving end with the delivery tube submerged
1. Place the Rapid Digestor under a fume hood near a in it.
water source, aspirator and a cup sink. Preheat to
200° C. 3. Add 40 ml of NaOH for every 20 ml of digestion
solution used. You will be collecting approximately
2. Place an identifying label or mark on each 250 ml 100-125 ml of distillate.
digestion tube.
4. Set the RapidStill II timer for 8 minutes.
3. Place tubes in the digestion rack.
5. Start the distillation process. Collect approxi-
4. To each tube add 4-5 alundum boiling stones and mately 125 ml of distillate.
the volume recommended below:
TKN in Sample(mg/l) Sample(ml) Volume of 6. When the distillation is complete, fill a class A
Digestion(ml) buret to the mark with 0.02N H2SO4 and titrate to
the purple endpoint.
0-20 100 20
20-50 50 10
ppm N = (ml acid - ml acid of blank)(N H2SO4)(14.007)
50-500 25 10
Liters of sample

5. Place the rack containing the tubes on the preheated ppm ammonia = (ml acid ml acid blank)(N H2SO4)(17.03)
digestion block. Attach heat shields. Pre-evaporate Liters of sample
at 110° C for 30 minutes to avoid splashing. Turn
the temperature control knob to 380° C. Conduct
the evaporation phase for 60 minutes (or until
Colorimetric Method Notes

1. When distillation is complete: 1. It is a good practice to regularly check procedural

Prepare Nessler tubes from a standard ammonium accuracy with standards such as those supplied by
solution. the EPA.
a. Stock solution: Dissolve 3.819 g anhydrous
NH4Cl in water and dilute to one liter with 2. Twenty ml of digestion reagent solution appears to
deionized water. work well for levels of nitrogen up to about
b. Standard solution: Dilute 10.0 ml of the stock 150 ppm.
ammonia solution to one liter with deionized
water. 3. When titrating, titrate to purple endpoint. Do not
titrate all the way back to red.
2. From the standard solution, prepare a series of
Nessler standards by diluting the volumes given in 4. Run a blank sample (reagents only, no sample) and
the following chart to 50 ml in ammonia-free water subtract the milliliters of H2SO4 consumed by the
and adding one ml of Nessler reagent. blank from that consumed by the sample.

ml Sample mg NH3-N/50 ml 5. With careful technique, this equipment will give

results with a relative standard deviation of no
0 0 greater than 1.5%.
0.5 0.005
1.0 0.010
2.0 0.020 6. The Nessler reagent is stable for at least a year if
4.0 0.040 stored in a rubber stoppered brown bottle.
5.0 0.050
8.0 0.080 7. Use reagent blank to zero spectrophotometer.
10.0 0.10
8. If splashing occurs during digestion (Step 5)
3. Mix thoroughly. pre-evaporate for 30 minutes at 100° C.

4. After 30 minutes, read the absorbance at 420 nm References

against a blank.
EPA Methods for Chemical Analysis of Water and
5. Place a blank in spectrophotometer. Read
Wastes. Cincinnati, OH: (1983) • pp 351.3-1 to
absobance. Adjust absorbance to read zero.
351.3-6.
Alternate samples and blanks, readjusting blank to
zero each time.
Official Methods of Analysis AOAC. 15th ed. Arlington,
VA: (1990) • 7.026, 7.031, 7.032, 24.038-24.040, and
6. Plot a calibration curve of absorbance vs
47.023.
mg NH3-N.
Standard Methods for the Examination of Water and
7. Measure the volume of the distillateand reveiving
Wastewater. 16th ed. Washington, D.C.: (1985) • pp
solution and record it. Pipet 50 ml of the distillate
358-410.
and add one ml of the Nessler reagent to develop
the color. Measure the absorbance after 30 minutes,
This method is for reference only. It is not a citable
and from the calibration curve, read the mg NH3-N.
document. It is based on data we believe to be reliable.
It is offered in good faith but without guarantee.
TKN, mg/L = A x 1000 x B
ml sample C

where:
A = mg NH3-N read from curve
B = ml total distillate measured
C = ml of original sample
 RAPID KJELDAHL
BENCHNOTES
5. Hand chopper, food processor, or blender
Rapid Kjeldahl
Methodology for the 6. 500 ml Erlenmeyer flasks

Determination of Nitrogen Reagents

in Meat Products With the (All reagents should be reagent grade and nitrogen-free.)
Rapid Digestor and the
1. Red mercuric oxide (HgO) or cupric sulfate (CuSO4
RapidStill II or CuSO4 • 5H2O)

2. Potassium sulfate (K2SO4) suitable for nitrogen

determination
Principle: This method covers the
determination of organic nitrogen and 3. Sulfuric acid (H2SO4) - concentrated

protein in meats. 4. Sodium hydroxide/potassium sulfide: Dissolve

450 g solid sodium hydroxide (NaOH) in deionized
Apparatus water. While still warm, dissolve 10 g potassium
sulfide (K2S) in the sodium hydroxide solution.
1. Labconco Rapid Digestor:
Rapid Digestor 4 (Model 23080)
5. Methyl red/methylene blue indicator: Dissolve
Rapid Digestor 25 (Model 23012)
200 mg methyl red in 100 ml ethyl alcohol. In a
separate beaker, dissolve 200 mg methylene blue in
2. Labconco Fume Removal System:
100 ml ethyl alcohol. Mix 2 volumes of methyl red
Fume Removal System-4 place (Model 23540)
with 1 volume methylene blue solution.
Fume Removal System-25 place (Model 23500-25)
6. Boric acid/indicator solution: Dissolve 20 g boric
3. Labconco Rapid Distillation Unit:
acid (H3BO3) in 800 ml of deionized water. Add
RapidStill II (Model 65200)
10 ml of the indicator solution in step 5 and dilute
to one liter with deionized water. NOTE: potassium
4. Labconco 250 ml Digestion Tubes:
sulfide is only required with mercury catalyst.
Volumetric, Pkg. of 5 (Model 23030-05)
Volumetric, Pkg. of 25 (Model 23030-25)
Straight, Pkg. of 5 (Model 23040-05)
Straight, Pkg. of 25 (Model 23040-25)

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7. 0.2N Sulfuric acid standard solution (volume Example:
depends on % N expected) blank = 1 ml sample weight = 1 gram
acid added = 11 ml
8. Alundum boiling stones
%N = (11 ml - 1 ml)(0.2N H2SO4)(1.400)
1 gram
Procedure
%N = 2.8%
%Protein = 17.5%
1. Preheat the Rapid Digestor to 410° C.

2. Place preweighed (up to 2 g), finely ground Notes

homogenous samples into digestion tubes.
1. Samples with high moisture content may need to be
3. Add 0.42 g HgO, 9.0 g K2SO4, 15 ml H2SO4 and preheated to a lower temperature (200° C) for 15
10-12 boiling stones to the digestion tubes. minutes to boil off the moisture and then taken to
410° C.
4. Place samples in the Rapid Digestor and digest for
45 minutes. Make sure digestion sample is clear. If 2. When titrating, titrate to the purple endpoint. Do not
sample is not a clear liquid, digest longer until titrate all the way back to red.
sample is clear.
Reference
5. Remove tubes from the Rapid Digestor and cool for
10 minutes. Do not allow hard cakes to form.
Official Methods of Analysis AOAC. 15th ed.
6. Add 50 ml deionized water and dissolve all Arlington, VA: (1990).
crystallized material.
This method is for reference only. It is not a citable
7. After the sample has cooled, attach digestion tube to document. It is based on data we believe to be reliable.
the distillation head of the RapidStill II. It is offered in good faith but without guarantee.

8. Place distillation outlet tube in 500 ml Erlenmeyer

flask which contains 100 ml boric acid/indicator
solution. The tip must be below the surface of the
boric acid/indicator solution.

9. Add 60 ml sodium hydroxide solution to the

digestion tube.

10. Set the RapidStill II timer for 8 minutes.

11. Start distillation and steam distill vigorously until

125 ml of distillate is collected or a total volume of
225 ml is in receiving flask.

12. When distillation is complete, fill a class A buret to

the mark with .2N sulfuric acid (H2SO4) standard
solution and titrate to the purple endpoint. Correct
for reagent blank.

%N = (ml std. H2SO4- ml H2SO4blank)(N •H2SO4)(1.4007)

gram sample weight

%Protein = %N x 6.25
 RAPID KJELDAHL
BENCHNOTES
4. Labconco 250 ml Digestion Tubes:
Rapid Kjeldahl Volumetric, Pkg. of 5 (Model 23030-05)
Methodology for the Volumetric, Pkg. of 25 (Model 23030-25)
Straight, Pkg. of 5 (Model 23040-05)
Determination of Nitrogen Straight, Pkg. of 25 (Model 23040-25)

in Feeds, Foods, Grains, 5. 25 ml Class A buret

Cereals, and Grasses with 6. 500 ml Erlenmeyer flasks

the Rapid Digestor and
Reagents
RapidStill II
(All reagents should be reagent grade and nitrogen-free)

1. Red mercuric oxide (HgO) or cupric sulfate

Principle: This method covers the (CuSO4 or CuSO4 • 5H2O)
determination of organic nitrogen in
2. Potassium sulfate (K2SO4) - suitable for nitrogen
feeds, foods, grains, cereals, and determination.
grasses.
3. Sulfuric Acid (H2SO4) - concentrated, 95-98%.
Apparatus
4. Sodium hydroxide/potassium sulfide solution:
Dissolve 450 g solid sodium hydroxide (NaOH) in
1. Labconco Rapid Digestor: deionized water. While still warm, dissolve 10 g
Rapid Digestor 4 (Model 23080) potassium sulfide (K2S) in the sodium hydroxide
Rapid Digestor 25 (Model 23012) solution. Cool and dilute with deionized water to
one liter. NOTE: Potassium sulfide is only
2. Labconco Fume Removal System required with mercury catalyst.
Fume Removal System-4 place (Model 23540)
Fume Removal System-25 place (Model 23500-25) 5. Methyl red/methylene blue indicator: Dissolve
200 mg methyl red in 100 ml ethyl alcohol. In a
3. Labconco Rapid Distillation Unit: separate beaker, dissolve 200 mg methylene blue in
RapidStill II (Model 65200) 100 ml ethyl alcohol. Mix 2 volumes methyl red
with 1 volume methylene blue.

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6. Boric acid/indicator solution: Dissolve 20 g boric 12. Start the distillation process. Distill until 125 ml of
acid (H3BO3) in 800 ml deionized water. Add 10 ml distillate collects.
methyl red/methylene blue indicator solution and
dilute to one liter with deionized water. 13. When distillation is complete, fill a class A buret to
the mark with .2N sulfuric acid standard solution
7. 0.2 N sulfuric acid standard solution (volume and titrate to the purple endpoint. Correct for
depends on % N expected). reagent blank.

8. Alundum boiling stones. %N = (ml std. H2SO4 - ml H2SO4 blank)(N H2SO4)(1.4007)

gram sample weight
Procedure Example:
blank = 1 ml sample weight = 1 gram
1. Preheat Rapid Digestor to 410° C. acid added = 11 ml

2. Place weighed (approximately 1 g) finely ground %N = (11 ml - 1 ml)(0.2N H2SO4)(1.400)

1 gram
homogeneous samples into digestion tubes.
%N = 2.8%
3. Add 0.42 g HgO, 9.0 g K2SO4, 15 ml H2SO4 to the %Protein = 17.5%
digestion tubes.

4. Place samples in Rapid Digestor and digest for 45 Notes

minutes or until white smoke comes off.
1. Run a blank sample (reagents only, no sample) and
5. Make sure digestion sample is clear. If necessary, subtract the milliliters of H2SO4 consumed by the
digest longer until sample is a clear liquid. blank from that consumed by the sample.

6. Remove tubes from Rapid Digestor and cool for 10 2. When titrating, titrate to purple endpoint. Do not
minutes. Do not allow hard cakes to form. If cakes titrate all the way back to red.
form, reheat samples until cakes are dissolved.
3. With careful technique, this equipment will give
7. Add 50 ml deionized water and dissolve all results with a relative standard deviation of no
crystallized material. greater than 1.5%.

8. After the sample has cooled, attach digestion tube to Reference

the distillation head and twist tightly in place.
Official Methods of Analysis AOAC. 15th ed.
9. Place delivery tube in 500 ml Erlenmeyer flask
Arlington, VA: (1990).
which contains 100 ml boric acid/indicator solution.
The tip must be below the surface of the boric
This method is for reference only. It is not a citable
acid/indicator solution.
document. It is based on data we believe to be reliable.
It is offered in good faith but without guarantee.
10. Add 60 ml sodium hydroxide solution to the
digestion tube. (Total volume in the Erlenmeyer
flask will be 225 ml.)

11. Set the RapidStill II timer for 8 minutes.

 RAPID KJELDAHL
BENCHNOTES
Rapid Kjeldahl 5. One 25 ml class A buret

Methodology for the 6. 500 ml Erlenmeyer flasks

Determination of Protein Reagents:

Content in Milk with the (All reagents should be reagent grade and nitrogen-free.)
Rapid Digestor and the
1. Sulfuric acid (H2SO4) - concentrated
RapidStill II
2. Red mercuric oxide (HgO) or cupric sulfate(CuSO4
or CuSO4 • 5H2O)
Principle: This method covers the
determination of organic nitrogen in 3. Potassium sulfate (K2SO4) suitable for nitrogen
fluid and dry milk. determination

4. 45% sodium hydroxide: Add 450 g sodium

Apparatus hydroxide (NaOH) to 700 ml deionized water. Add
10 g potassium sulfide (K2S), dissolve, and dilute to
1. Labconco Rapid Digestor: one liter with deionized water. NOTE: Potassium
Rapid Digestor 4 (Model 23080) sulfide is only required with mercury catalyst.
Rapid Digestor 25 (Model 23012)
5. Methyl red/methylene blue indicator: Dissolve 200
2. Labconco Fume Removal System: mg (0.2 g) methyl red in 100 ml ethyl alcohol. In a
Fume Removal System-4 place (Model 23540) separate beaker, dissolve 200 mg methylene blue in
Fume Removal System-25 place (Model 23500-25) 100 ml ethyl alcohol. Combine two parts methyl
red with one part methylene blue solution and mix.
3. Labconco Rapid Distillation Unit:
RapidStill II (Model 65200) 6. Boric acid/indicator solution 1%: Dissolve 10 g
boric acid (H3BO3) in 800 ml deionized water. Add
4. Labconco 250 ml Digestion Tubes: 10 ml methyl red/methylene blue indicator solution
Volumetric, Pkg. of 5 (Model 23030-05) and dilute to one liter with deionized water.
Volumetric, Pkg. of 25 (Model 23030-25)
Straight, Pkg. of 5 (Model 23040-05) 7. 0.1N sulfuric acid (H2SO4) solution.
Straight, Pkg. of 25 (Model 23040-25)

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3-48-A-5/96-100-R3
Procedure 11. Set the RapidStill II timer for 8 minutes.

1. Place the Rapid Digestor under a fume hood near a 12. Start the distillation process.
water source, aspirator and a cup sink. Preheat to
410° C. 13. Steam distill until approximately 125 ml distillate
collects, or a total of 225 ml is collected.
2. First weigh the weigh boat and then weigh the
samples. AOAC recommends 5 ±0.1 ml for 14. When distillation is complete, fill a class A buret to
liquid milk or approximately 1 g for dry milk. the mark with 0.1N sulfuric acid (H2SO4). Titrate
Transfer the sample from the weigh boat into the drop by drop to the purple endpoint. Correct for
digestion tube. reagent blank.

%N = (ml H2SO4 - ml H2SO4of blank)(N H2SO4)(1.4007)

3. Place the tubes in the digestion rack of the Rapid gram sample weight
Digestor.
Example:
4. To each tube add 0.42 g HgO, 9 g K2SO4, 15 ml For a 5.0 g sample of milk containing 3.0% protein,
H2SO4 and 3-4 alundum boiling stones. 16.78 ml 0.1N H2SO4 will be required for titration.

5. When the light on the Rapid Digestor begins Notes

blinking, place the rack containing the digestion
tubes on the Rapid Digestor block. Attach heat
1. Run a blank sample (reagents only, no sample) and
shields. On the top of the tubes, place the Fume
subtract the milliliters of H2SO4 consumed by the
Removal System and connect to the water aspirator.
blank from that consumed by the sample.
Turn on the water to the water aspirator and digest
for 45 minutes.
2. When titrating, titrate to the purple endpoint. Do
6. After 45 minutes, remove the tubes from the block. not titrate all the way back to red.
Make sure digestion sample is clear. If sample is
not a clear liquid, digest longer until sample is clear. 3. With careful technique, this equipment will give
results with a relative standard deviation of no
7. With the Fume Removal System still in place, set greater than 1.5%.
the tube-filled rack on a hard, dry, heat-resistant
surface. Remove the heat shields and cool for ten Reference
minutes. Cooling times depend on the temperature
and circulation of air around the tubes and may Official Methods of Analysis AOAC. 15th ed.
require adjustment depending on conditions. Arlington, VA: (1990) • 16.036, 7.025 - 7.032, 24.038 -
Do not allow hard cakes to form. 24.040.

8. Add 50 ml deionized water to each tube, dissolving This method is for reference only. It is not a citable
all crystallized material. It may be necessary to document. It is based on data we believe to be reliable.
place tubes back in the Rapid Digestor, to expedite It is offered in good faith but without guarantee.
dissolving the crystallized material. Cover to
prevent contamination.

9. After the sample has cooled, attach digestion tube to

the RapidStill II and twist securely in place.

10. Place delivery tube in 500 ml Erlenmeyer flask

which contains approximately 100 ml boric
acid/indicator solution. The tip must be below the
surface of the boric acid/indicator solution.