ASTM E778-15(2021)
(Test Method)Standard Test Methods for Nitrogen in Refuse-Derived Fuel Analysis Samples
Standard Test Methods for Nitrogen in Refuse-Derived Fuel Analysis Samples
SIGNIFICANCE AND USE
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 samples.
5.2 Nitrogen is part of the ultimate analysis and can be used for calculation of combustion parameters.
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 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific precautionary statements, see 8.4.1 and Section 9.
1.7 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: E778 − 15 (Reapproved 2021)
Standard Test Methods for
Nitrogen in Refuse-Derived Fuel Analysis Samples
This standard is issued under the fixed designation E778; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2. Referenced Documents
1.1 These test methods cover the determination of total 2.1 ASTM Standards:
Kjeldahl nitrogen in prepared analysis samples of solid forms D1193 Specification for Reagent Water
of refuse-derived fuel (RDF). The procedures measure free D5681 Terminology for Waste and Waste Management
ammonia or ammonia formed from the conversion of organic E180 Practice for Determining the Precision of ASTM
nitrogenous compounds such as amino acids and proteins. Methods for Analysis and Testing of Industrial and Spe-
However, the procedures may not convert the nitrogenous cialty Chemicals (Withdrawn 2009)
compounds of some wastes to ammonia. Examples of such E200 Practice for Preparation, Standardization, and Storage
compounds that may not be measured are nitro compounds, of Standard and Reagent Solutions for ChemicalAnalysis
hydrozones, oxines, nitrates, semicarbazones, pyridines, and E790 Test Method for Residual Moisture in Refuse-Derived
some refractory tertiary amines. Fuel Analysis Samples
E791 Test Method for Calculating Refuse-Derived Fuel
1.2 Two alternatives are described for the final determina-
Analysis Data from As-Determined to Different Bases
tion of the ammonia, the Kjeldahl-Gunning Test Method and
E829 Practice for Preparing Refuse-Derived Fuel (RDF)
the Acid-Titration Test Method.
Laboratory Samples for Analysis
1.3 The analytical data from these test methods are to be
reportedaspartoftheultimateanalysiswhereultimateanalysis
3. Terminology
is requested.
3.1 For definitions of terms used in these test methods, refer
1.4 These test methods may be applicable to any waste to Terminology D5681.
material from which a laboratory analysis sample can be
4. Summary of Test Methods
prepared.
4.1 The determination of nitrogen is made by either the
1.5 The values stated in SI units are to be regarded as
Kjeldahl-Gunning Test Method (Section 11) or the Acid-
standard. No other units of measurement are included in this
Titration Test Method (Section 12). In both these methods, the
standard.
nitrogen in the sample is converted into ammonium salts by
1.6 This standard does not purport to address all of the
destructive digestion of the sample with a hot, catalyzed
safety concerns, if any, associated with its use. It is the
mixture of concentrated sulfuric acid and potassium sulfate.
responsibility of the user of this standard to establish appro-
The salts are subsequently decomposed in a hot alkaline
priate safety, health, and environmental practices and deter-
solution from which the ammonia is recovered by distillation,
mine the applicability of regulatory limitations prior to use.
and finally determined by alkalimetric or acidimetric titration.
For specific precautionary statements, see 8.4.1 and Section 9.
1.7 This international standard was developed in accor-
5. Significance and Use
dance with internationally recognized principles on standard-
5.1 The standard sample is available to producers and users
ization established in the Decision on Principles for the
of RDF as a method for determining the weight percent of
Development of International Standards, Guides and Recom-
nitrogen in the analysis samples.
mendations issued by the World Trade Organization Technical
5.2 Nitrogen is part of the ultimate analysis and can be used
Barriers to Trade (TBT) Committee.
for calculation of combustion parameters.
1 2
These test methods are under the jurisdiction of ASTM Committee D34 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Waste Management and are the direct responsibility of Subcommittee D34.03 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Treatment, Recovery and Reuse. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2021. Published May 2021. Originally the ASTM website.
approved in 1981. Last previous edition approved in 2015 as E778 – 15. DOI: The last approved version of this historical standard is referenced on
10.1520/E0778-15R21. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E778 − 15 (2021)
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 onAnalytical Reagents of theAmerican Chemical Society,
where such specifications are available. Other grades may be
used, provided it is first ascertained that the reagent is of
A = electric heater
sufficiently high purity to permit its use without lessening the
B = Kjeldahl digestion flask
C = Kjeldahl connecting bulb
accuracy of the determination.
D = condenser
8.2 Purity of Water—Unless otherwise indicated, reference
E = connecting tube
F = receiving flask
to water shall be understood to mean reagent water, Type II,
conforming to Specification D1193, prepared by the passage
through an ion-exchange column containing a strongly acid
FIG. 1 Kjeldahl Distillation Apparatus
cation resin in the hydrogen form.
8.3 Potassium Sulfate (K SO ), crystals.
2 4
6. Interferences and Limitations
NOTE 2—Other satisfactory and permissible catalysts for the digestion,
6.1 Because of the nature of RDF, nitrogenous compounds together with the quantities of K SO required in their use, are as follows:
2 4
(1) Five grams of a mixture containing 32 parts by weight of K SO ,
maybepresentwhichwillnotreadilybeconvertedtoammonia 2 4
five parts by weight of mercuric sulfate (HgSO ), and one part by weight
by this test method (see 1.1). Modifications to the digestion of
of selenium.
the waste may enhance the conversion of these nitrogenous
(2) Three-tenths gram of mercuric selenite (HgSeO ) with 7 to 10 g of
compounds to the ammonium salts.
K SO .
2 4
(3) Three-tenthsgramofcupricselenitedihydrate(CuSeO ·2H O)with
2 2
7. Apparatus 7to10gofK SO . When this mixture is used, the addition of a sulfide
2 4
to the alkali solution is not necessary.
7.1 Digestion Unit—An electrical heater of approximately
8.4 Mercury, metal (see Note 2).
500-Wminimumrating,microwavedigester,oragasburnerof
8.4.1 Warning—Appropriate safety precautions should be
comparable capacity. These digestion units shall be provided
used when handling and disposing of mercury and selenium
with adequate means of control to maintain digestion rates as
compounds.
described in 11.1 (Note 1). Commercially made, multiple-unit
digestionracksprovidedwithfumeexhaustductsmaybeused.
8.5 Sulfuric Acid (sp gr 1.84)—Concentrated sulfuric acid
(H SO ).
2 4
NOTE 1—If commercially made electrical heaters are used, auxiliary
voltage control equipment such as an autotransformer may be needed to
8.6 Potassium Permanganate (KMnO ), crystals.
maintain the specified rates of digestion and distillation.
8.7 Zinc, mossy or granular.
7.2 Distillation Unit (Fig. 1)—An electrical heater or gas
8.8 Alkali Solution—Dissolve 8.0 g of potassium sulfide
burner as described in 7.1. Either type shall be provided with
(K S) and 500 g of sodium hydroxide (NaOH) in water and
adequate means of control to maintain rates as described in
dilute to 1 L.The use of appropriate amounts of sodium sulfide
11.2. Commercially made, multiple-unit distillation racks pro-
(Na S) or potassium hydroxide (KOH) may be substituted for
vided with water-cooled glass or block tin condensers may be
the above, if desired (Note 2 (3)).
used.
8.9 Ethyl Alcohol (95 %)—Ethyl alcohol conforming to
7.3 Condenser, glass, water-cooled, having a minimum
Formula No. 30 or 2Aof the U.S. Bureau of Internal Revenue.
jacket length of 500 mm.
Methyl alcohol may be substituted.
7.4 Kjeldahl Digestion Flask, of heat-resistant glass, having
a capacity of 500 or 800 mL. Borosilicate glass has been found
Reagent Chemicals, American Chemical Society Specifications, American
satisfactory for this purpose.
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Kolthoff, I. M. and Stenger, V. A., Volumetric Analysis II, Intersciences and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
Publishers, Inc., New York, NY, pp. 173–176. MD.
E778 − 15 (2021)
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,
weigh approximately1gtothe nearest 1 mg of sample into a
8.11 Reagents Required for Kjeldahl-Gunning Test Method:
weighing scoop.
8.11.1 Methyl Red Indicator Solution (0.4 to 1 g/L)—
11.1.2 Carefully transfer the sample into a 500 or 800-mL
Dissolve 0.04 to 0.1 g of methyl red in 50 mL of 95 % ethyl
Kjeldahl flask containing 7 to 10 g of K SO and 0.6 to 0.8 g
2 4
alcohol or methyl alcohol and add 50 mLof water. Bromcresol
of mercury (see Note 2).
green indicator solution of equal concentration may be used.
11.1.3 Add 30 mL of H SO (sp gr 1.84) to the mixture by
8.11.2 Sodium Hydroxide, Standard Solution (0.1 to 0.2
2 4
pouri
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