Introduction:
This
method is adapted for use on AIM600 Block Digestion
System following US EPA Office of Ground Water and Drinking Water
methodology.
Scope & Application:
This is an
acid digestion procedure to prepare ground waters, surface waters,
drinking waters andindustrial or domestic wastewaters for the subsequent
determination of TKN (Total Kjeldahl Nitrogen) and TP (Total Phosphorus)
by colorimetric methods. The range for the method is 0.1-20 mg/l as N
and P respectively. Samples can be diluted to increase the range.
Note: the
digestion procedure may not convert some nitrogen containing compounds
sometimes found in industrial waste such amines, nitro compounds,
hydrazones, oximes, semicarbazones and some refractory tertiary amines.
Apparatus:
DG-U-A013*
AIM600 50 place Block Digestion System. Consists of
the DG-U-A002-240V 50 place AIM600 digestion
block, DG-U-A003-AIM600 Controller, 8028114 - 50 place tube rack/draftshield,
4003036 - 50 x 100 ml straight tubes, and 5001511 Cooling Stand.
Reagents:
8032173
PTFE boiling chips, 450g
Catalyst Kjeltabs M/1.5 (1.5 g
K2SO4+ 7.5 mg HgO)
or
Catalyst Kjeltabs Cu/1,5 (1.5 g
K2SO4+ 0.15 g
CuSO4x
5
H20)
(alternative catalyst for mercury free digestion solution)
6N Sulphuric Acid - Dilute 167ml of concentrated sulphuric acid to 1 liter
with reagent grade water
Reagent
Grade Water
Control Program:
STEP to
160 C
HOLD for 60 minutes
RAMP to 380 C at 5 C/min
HOLD for 30 minutes
End
Procedure:
1. Shake
sample and transfer 25ml of well mixed sample into a clean dry digestion
tube.
2. For
mercury catalyst: Carefully add 6ml of 6N sulphuric acid and 1 x Kjeltab
MQ and mix
thoroughly. or For copper catalyst: Carefully add 8ml of 6N sulphuric
acid and 1 x Kjeltab CQ and mix thoroughly.
3. Add 4 -
8 PTFE boiling chips to each tube.
4. RUN the
control program above on the AIM600 Control Module.
5. At the
completion of the digestion, raise the digestion tubes in the tube rack
to the elevated
position on the cooling stand to facilitate rapid cooling.
6. When
cool, dilute to 25ml with reagent grade water.
The sample
is now ready for
colorimetric FIA analysis of
Total Kjeldahl
Nitrogen and
Total Phosphorus.
Safety Notes:
The AIM600
Digestion Block should be located inside a ventilated acid-resistant
fume hood. It is recommended that the AIM600 Program Controller be
located outside the fume hood.
Great care
should be taken when handling acids. Always add acid to water unless
otherwise directed. Protective clothing should be worn including gloves
and face mask. If acids are spilled on the skin, immediately wash with
copious amounts of water.
Neutralize any acid spills with sodium carbonate (Na2CO3) or sodium
bicarbonate (NaHCO3).
Digests
must be cool before dilution water is added to avoid a violent reaction
during which the acid can shoot out of the flask.
References:
(1) US EPA
Method 351.2, "Determination of Total Kjeldahl Nitrogen by
Semi-Automated Colorimetry", EPA/600/R-93/100, Methods for the
Determination of Inorganic Substances in Environmental Substances,
Revision 2, August 1993
(2) US EPA
Method 351.4, Potentiometric Ion Selective Electrode Method for
determining Total Kjeldahl Nitrogen, EPA/600/4-79/020, Methods for
Chemical Analysis of Water and Wastes, March 1983.
(3) US EPA
Method 365.4, Colorimetric, Automated, Block Digestor method for
determining Total Phosphorus, EPA/600/4-79/020, Methods for Chemical
Analysis of Water and Wastes, March 1983.
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