ASTM E778-87(1996)
(Test Method)Standard Test Methods for Nitrogen in the Analysis Sample of Refuse-Derived Fuel
Standard Test Methods for Nitrogen in the Analysis Sample of Refuse-Derived Fuel
SCOPE
1.1 These test methods cover the determination of total Kjeldahl nitrogen in (prepared analysis) samples of (solid forms) of refuse-derived fuel (RDF). The procedures measure free ammonia or ammonia formed from the conversion of organic nitrogenous compounds such as amino acids and proteins. However, the procedures may not convert the nitrogenous compounds of some wastes to ammonia. Examples of such compounds that may not be measured are nitro compounds, hydrozones, oxines, nitrates, semicarbazones, pyridines, and some refractory tertiary amines.
1.2 Two alternatives are described for the final determination of the ammonia, the Kjeldahl-Gunning Test Method and the Acid-Titration Test Method.
1.3 The analytical data from these test methods are to be reported as part of the ultimate analysis where ultimate analysis is requested.
1.4 These test methods may be applicable to any waste material from which a laboratory analysis sample can be prepared.
1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements see 7.4.1 and Section 8.
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Standards Content (Sample)
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Designation: E 778 – 87 (Reapproved 1996)
Standard Test Methods for
Nitrogen in the Analysis Sample of Refuse-Derived Fuel
This standard is issued under the fixed designation E 778; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope E 790 Test Method for Residual Moisture in Refuse-
Derived Fuel Analysis Sample
1.1 These test methods cover the determination of total
E 791 Test Method for Calculating Refuse-Derived Fuel
Kjeldahl nitrogen in (prepared analysis) samples of (solid
Analysis Data from As-Determined to Different Bases
forms) of refuse-derived fuel (RDF). The procedures measure
E 829 Practice for Preparing Refuse-Derived Fuel (RDF)
free ammonia or ammonia formed from the conversion of
Laboratory Samples for Analysis
organic nitrogenous compounds such as amino acids and
proteins. However, the procedures may not convert the nitrog-
3. Terminology
enous compounds of some wastes to ammonia. Examples of
3.1 Definitions of Terms Specific to This Standard:
such compounds that may not be measured are nitro com-
3.1.1 refuse-derived fuel—solid forms of refuse-derived
pounds, hydrozones, oxines, nitrates, semicarbazones, py-
fuels from which appropriate analytical samples may be
ridines, and some refractory tertiary amines.
prepared are defined as follows in ASTM STP 832:
1.2 Two alternatives are described for the final determina-
RDF-1—Wastes used as a fuel in as-discarded form with
tion of the ammonia, the Kjeldahl-Gunning Test Method and
only bulky wastes removed.
the Acid-Titration Test Method.
RDF-2—Wastes processed to coarse particle size with or
1.3 The analytical data from these test methods are to be
without ferrous metal separation.
reported as part of the ultimate analysis where ultimate analysis
RDF-3—Combustible waste fraction processed to particle
is requested.
sizes, 95 % passing 2-in. square screening.
1.4 These test methods may be applicable to any waste
RDF-4—Combustible waste fraction processed into powder
material from which a laboratory analysis sample can be
form, 95 % passing 10-mesh screening.
prepared.
RDF-5—Combustible waste fraction densified (compressed)
1.5 This standard does not purport to address all of the
into the form of pellets, slugs, cubettes, or briquettes.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
4. Summary of Test Methods
priate safety and health practices and determine the applica-
4.1 The determination of nitrogen is made by either the
bility of regulatory limitations prior to use. For specific
Kjeldahl-Gunning Test Method (Section 11) or the Acid-
precautionary statements see 8.4.1 and Section 9.
Titration Test Method (Section 12). In both these methods the
2. Referenced Documents nitrogen in the sample is converted into ammonium salts by
destructive digestion of the sample with a hot, catalyzed
2.1 ASTM Standards:
2 mixture of concentrated sulfuric acid and potassium sulfate.
D 1193 Specification for Reagent Water
The salts are subsequently decomposed in a hot alkaline
E 180 Practice for Determining the Precision of ASTM
3 solution from which the ammonia is recovered by distillation,
Methods for Analysis and Testing of Industrial Chemicals
and finally determined by alkalimetric or acidimetric titration.
E 200 Practice for Preparation, Standardization, and Stor-
age of Standard and Reagent Solutions for Chemical
5. Significance and Use
Analysis
5.1 The standard sample is available to producers and users
of RDF as a method for determining the weight percent of
nitrogen in the analysis sample.
These test methods are under the jurisdiction of ASTM Committee D34 on
Waste Management and are the direct responsibility of Subcommittee D34.06 on
Recovery and Reuse.
Current edition approved Aug. 28, 1987. Published October 1987. Originally
published as E 778 – 81. Last previous edition E 778 – 81. Annual Book of ASTM Standards, Vol 11.04.
2 5
Annual Book of ASTM Standards, Vol 11.01. Thesaurus on Resource Recovery Terminology, ASTM STP 832, ASTM, 1983,
Annual Book of ASTM Standards, Vol 15.05. p. 72.
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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 778 – 87 (1996)
5.2 Nitrogen is part of the ultimate analysis and can be used 7.4 Kjeldahl Digestion Flask, of heat-resistant glass, having
for calculation of combustion parameters. a capacity of 500 or 800 mL. Borosilicate glass has been found
satisfactory for this purpose.
7.5 Kjeldahl Connecting Bulb, cylindrical type, 45 mm in
diameter by 100 mm long, or larger, with curved inlet and
outlet tubes.
7.6 Receiving Flasks—Erlenmeyer flask having a capacity
of 250 or 300 mL.
7.7 Connecting Tube—Glass tubing approximately 10 mm
in outside diameter by 200 mm in length.
7.8 Pure Gum Rubber Tubing.
8. Reagents
8.1 Purity of Reagents—Reagent grade chemicals shall be
used in all tests. Unless otherwise indicated, it is intended that
all reagents shall conform to the specifications of the Commit-
tee on Analytical Reagents of the American Chemical Society,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
accuracy of the determination.
A = electric heater
8.2 Purity of Water—Unless otherwise indicated, reference
B = Kjeldahl digestion flask
to water shall be understood to mean reagent water, Type II,
C = Kjeldahl connecting bulb
D = condenser
conforming to Specification D 1193, prepared by the passage
E = connecting tube
through an ion-exchange column containing a strongly acid
F = receiving flask
cation resin in the hydrogen form.
FIG. 1 Kjeldahl Distillation Apparatus
8.3 Potassium Sulfate (K SO ), crystals.
2 4
NOTE 2—Other satisfactory and permissible catalysts for the digestion,
together with the quantities of K SO required in their use, are as follows:
6. Interferences and Limitations
2 4
(1) Five grams of a mixture containing 32 parts by weight of K SO ,5
2 4
6.1 Because of the nature of RDF, nitrogenous compounds
parts by weight of mercuric sulfate (HgSO ), and 1 part by weight of
may be present which will not readily be converted to ammonia
selenium.
by this test method (1.1). Modifications to the digestion of the
(2) Three-tenths gram of mercuric selenite (HgSeO )with7to10gof
waste may enhance the conversion of these nitrogenous com- K SO .
2 4
(3) Three-tenths gram of cupric selenite dihydrate (CuSeO ·2H O)
pounds to the ammonium salts. 2 2
with7to10gofK SO . When this mixture is used, the addition of a
2 4
sulfide to the alkali solution is not necessary.
7. Apparatus
8.4 Mercury, metal (see Note 2).
7.1 Digestion Unit—An electrical heater of approximately
8.4.1 Precaution—Appropriate safety precautions should
500-W minimum rating or a gas burner of comparable capacity.
be used when handling and disposing of mercury and selenium
Either type of heater shall be provided with adequate means of
compounds.
control to maintain digestion rates as described in 11.1 (Note
8.5 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
1). Commercially made, multiple-unit digestion racks provided
(H SO ).
2 4
with fume exhaust ducts may be used.
8.6 Potassium Permanganate (KMnO ), crystals.
NOTE 1—If commercially made electrical heaters are used, auxiliary
8.7 Zinc, mossy or granular.
voltage control equipment, such as an autotransformer, may be needed to
8.8 Alkali Solution—Dissolve 8.0 g of potassium sulfide
maintain the specified rates of digestion and distillation.
(K S) and 500 g of sodium hydroxide (NaOH) in water and
7.2 Distillation Unit (Fig. 1)—An electrical heater or gas
dilute to 1 L. The use of appropriate amounts of sodium sulfide
burner as described in 7.1. Either type shall be provided with
(Na S) or potassium hydroxide (KOH) may be substituted for
adequate means of control to maintain rates as described in
the above, if desired (Note 2 (c)).
11.2. Commercially made, multiple-unit distillation racks pro-
8.9 Ethyl Alcohol (95 %)—Ethyl alcohol conforming to
vided with water-cooled glass or block tin condensers may be
Formula No. 30 or 2A of the U.S. Bureau of Internal Revenue.
used.
Methyl alcohol may be substituted.
7.3 Condenser, glass, water-cooled, having a minimum
jacket length of 500 mm.
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by
Kolthoff, I. M., and Stenger, V. A., Volumetric Analysis II, Intersciences the American Chemical Society, see “Analar Standards for Laboratory U.K.
Publishers, Inc., New York, NY, pp. 173–176. Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopoeia”.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
E 778 – 87 (1996)
8.10 Sucrose—National Bureau of Standards primary stan- 11.1.1 After thoroughly mixing the RDF analysis sample to
dard grade. provide the best possible mix of heavy fines with milled fluff,
8.11 Reagents Required for Kjeldahl-Gunning Test Method: weigh approximately1gtothe nearest 1 mg of sample into a
weighing scoop.
8.11.1 Methyl Red Indicator Solution (0.4 to 1 g/L)—
Dissolve 0.04 to 0.1 g of methyl red in 50 mL of 95 % ethyl
11.1.2 Carefully transfer the sample into a 500 or 800-mL
alcohol or methyl alcohol and add 50 mL of water. Bromcresol
Kjeldahl flask containing 7 to 10 g of K SO and 0.6 to 0.8 g
2 4
green indicator solution of equal concentration may be used.
of mercury (see Note 3).
8.11.2 Sodium Hydroxide, Standard Solution (0.1 to 0.2
11.1.3 Add 30 mL of H SO (sp gr 1.84) to the mixture by
2 4
N)—Prepare and standardize a 0.1 to 0.2 N sodium hydroxide
pouri
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