ASTM E775-15(2021)

Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel

SIGNIFICANCE AND USE
5.1 These procedures are used by producers and users of RDF for determining the total sulfur content of the fuel.
SCOPE
1.1 These test methods present two alternative procedures for the determination of total sulfur in prepared analysis samples of solid refuse-derived fuel (RDF). Sulfur is included in the ultimate analysis of RDF.  
1.2 The test methods appear in the following order:    
Test  
Sections  
Eschka Method  
8 – 11  
Bomb Washing Method  
12 and 13  
1.3 These test methods may be applicable to any waste material from which a laboratory analysis sample can be prepared.  
1.4 The values stated in SI units are to be regarded as standard. Inch-pound units are provided for information.  
1.5 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 Section 6.  
1.6 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

• Status: Published
• Publication Date: 30-Apr-2021
• ICS: 75.160.10 - Solid fuels
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.03 - Treatment, Recovery and Reuse

Relations

• Refers: ASTM D5681-23 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Nov-2023
• Refers: ASTM D5681-18 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Nov-2018
• Refers: ASTM D5681-17 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Sep-2017
• Refers: ASTM D5681-16a - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Nov-2016
• Refers: ASTM D5681-16 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Feb-2016
• Refers: ASTM D5681-13 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Feb-2013
• Refers: ASTM D5681-09 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Jul-2009
• Refers: ASTM D5681-08 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Sep-2008
• Refers: ASTM D1193-06 - Standard Specification for Reagent Water
• Effective Date: 01-Mar-2006
• Refers: ASTM D5681-98a(2004)e1 - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Sep-2004
• Refers: ASTM D5681-98a(2004) - Standard Terminology for Waste and Waste Management
• Effective Date: 01-Sep-2004
• Refers: ASTM D1193-99 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D1193-99e1 - Standard Specification for Reagent Water
• Effective Date: 10-Feb-1999
• Refers: ASTM D5681-98ae1 - Standard Terminology for Waste and Waste Management
• Effective Date: 10-Jun-1998
• Refers: ASTM D5681-98a - Standard Terminology for Waste and Waste Management
• Effective Date: 10-Jun-1998

Overview

ASTM E775-15(2021) - Standard Test Methods for Total Sulfur in the Analysis Sample of Refuse-Derived Fuel - is an internationally recognized standard developed by ASTM International. It provides two validated laboratory procedures for determining the total sulfur content in solid refuse-derived fuel (RDF), an essential parameter in the ultimate analysis of waste-derived fuel products. The methods are practical and widely applicable, supporting quality assurance for producers and users of RDF. The standard is compliant with principles established by the World Trade Organization Technical Barriers to Trade (TBT) Committee, underscoring its global credibility and relevance.

Key Topics

• Test Methods for Sulfur Determination:
  The standard presents two alternative analytical procedures:
  • Eschka Method
    Involves ignition of the RDF sample with a specially prepared Eschka mixture, followed by precipitation and gravimetric measurement of sulfur as barium sulfate.
  • Bomb Washing Method
    Utilizes washings from an oxygen-bomb calorimeter, precipitating and weighing sulfur as barium sulfate.
• Sample Preparation:
  Guidance for representative sampling of RDF, air-drying, and particle size reduction in accordance with ASTM E829.
• Units and Safety:
  States SI units as standard and provides inch-pound units for reference. Safety, health, and environmental practices are emphasized, with specific notes on handling heterogeneous waste materials and laboratory best practices.
• Precision and Quality Control:
  Within-laboratory and between-laboratory precision data are provided, supporting reliability and repeatability of results.

Applications

The test methods described in ASTM E775-15(2021) have significant practical value across various sectors:

• Waste-to-Energy Facilities:
  Ensure compliance with emissions regulations by precisely determining sulfur content in RDF before combustion, aiding in environmental impact assessments.
• Fuel Producers:
  Quality control during RDF production, ensuring product consistency and meeting end-user requirements for sulfur limits.
• Research and Analytical Laboratories:
  Standardization of sulfur analysis in waste-derived materials, supporting research, process optimization, and regulatory compliance.
• Municipal Solid Waste Management:
  Assessment and monitoring of RDF generated from municipal and industrial solid wastes to ensure suitability for various energy recovery processes.

By providing robust and internationally recognized procedures, this standard helps organizations improve product quality, safeguard operations, and adhere to environmental policies regarding sulfur emissions from waste-derived fuels.

Related Standards

• ASTM E829 - Practice for Preparing Refuse-Derived Fuel (RDF) Laboratory Samples for Analysis
• ASTM D1193 - Specification for Reagent Water
• ASTM D5681 - Terminology for Waste and Waste Management
• ASTM E180 - Practice for Determining the Precision of ASTM Methods for Analysis and Testing
• Withdrawn Standards:
  • ASTM E711 - Test Method for Gross Calorific Value of Refuse-Derived Fuel by the Bomb Calorimeter

These related documents support proper implementation of ASTM E775-15(2021), ensuring accurate sulfur determination and harmonized RDF analysis workflows.

---

Keywords: ASTM E775, total sulfur analysis, refuse-derived fuel, RDF, Eschka method, bomb washing method, sulfur content testing, waste-to-energy, laboratory procedures, waste fuel analysis, ASTM standards, sulfur emissions compliance.

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: E775 − 15 (Reapproved 2021)
Standard Test Methods for
Total Sulfur in the Analysis Sample of Refuse-Derived Fuel
This standard is issued under the fixed designation E775; 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 cialty Chemicals (Withdrawn 2009)
E711 Test Method for Gross Calorific Value of Refuse-
1.1 These test methods present two alternative procedures
Derived Fuel by the Bomb Calorimeter (Withdrawn
for the determination of total sulfur in prepared analysis
2011)
samples of solid refuse-derived fuel (RDF). Sulfur is included
E829 Practice for Preparing Refuse-Derived Fuel (RDF)
in the ultimate analysis of RDF.
Laboratory Samples for Analysis
1.2 The test methods appear in the following order:
Test Sections 3. Terminology
Eschka Method 8–11
3.1 For definitions of terms used in this standard, refer to
Bomb Washing Method 12 and 13
Terminology D5681.
1.3 These test methods may be applicable to any waste
material from which a laboratory analysis sample can be
4. Summary of Test Methods
prepared.
4.1 EschkaMethod—AweighedsampleandEschkamixture
1.4 The values stated in SI units are to be regarded as
are ignited together and the sulfur is precipitated from the
standard. Inch-pound units are provided for information.
resulting solution as barium sulfate (BaSO ).The precipitate is
1.5 This standard does not purport to address all of the
filtered, ashed, and weighed.
safety concerns, if any, associated with its use. It is the
4.2 BombWashingMethod—SulfurisprecipitatedasBaSO
responsibility of the user of this standard to establish appro-
from oxygen-bomb calorimeter washings and the precipitate is
priate safety, health, and environmental practices and deter-
filtered, ashed, and weighed.
mine the applicability of regulatory limitations prior to use.
For specific precautionary statements see Section 6.
5. Significance and Use
1.6 This international standard was developed in accor-
5.1 These procedures are used by producers and users of
dance with internationally recognized principles on standard-
RDF for determining the total sulfur content of the fuel.
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom-
6. Precautions
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 6.1 Due to the origins of RDF in municipal waste, precau-
tions should be observed when conducting tests on samples.
2. Referenced Documents
Recommended safety practices include use of gloves when
handling RDF; wearing dust masks (NIOSH-approved type),
2.1 ASTM Standards:
especially while milling RDF samples; conducting tests under
D1193 Specification for Reagent Water
negative pressure hood when possible; and washing hands
D5681 Terminology for Waste and Waste Management
upon completion of activity and before eating or smoking.
E180 Practice for Determining the Precision of ASTM
Methods for Analysis and Testing of Industrial and Spe-
7. Sampling
7.1 RDF products are frequently inhomogeneous. For this
These test methods are under the jurisdiction of ASTM Committee D34 on
reason, significant care should be exercised to obtain a repre-
Waste Management and are the direct responsibility of Subcommittee D34.03 on
sentative sample from the RDF lot to be characterized.
Treatment, Recovery and Reuse.
Current edition approved May 1, 2021. Published May 2021. Originally
7.2 Thesamplingmethodforthisprocedureshouldbebased
approved in 1981. Last previous edition approved in 2015 as E775 – 15. DOI:
on agreement between the involved parties.
10.1520/E0775-15R21.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
E775 − 15 (2021)
7.3 The laboratory sample must be air-dried and particle 9.9 Sodium Carbonate (saturated solution)—Dissolve ap-
size reduced to pass through a 0.5-mm screen as described in proximately 60 g of crystallized sodium carbonate
Practice E829. This procedure must be performed carefully to (Na CO ·10H O) or 20 g of anhydrous sodium carbonate
2 3 2
preserve the sample’s representativeness beyond just particle (Na CO ) in 100 mL of water, using a sufficient excess of
2 3
size while preparing the analysis sample to be analyzed Na CO to ensure a saturated solution.
2 3
according to these procedures.
9.10 SodiumHydroxideSolution (100 g/L)—Dissolve 100 g
of sodium hydroxide (NaOH) in 1 L of water. This solution
TEST METHOD A—ESCHKA METHOD
may be used in place of Na CO solution.
2 3
8. Apparatus
10. Procedure
8.1 Gas(Note1)orElectricMuffleFurnaceorBurners, for
10.1 Preparation of Sample and Eschka Mixture—Weigh to
igniting the sample with Eschka mixture and for igniting the
thenearest0.1mgabout1gofmixedair-driedanalysissample
barium sulfate (BaSO ).
and3gof Eschka mixture on glazed paper. Mix thoroughly.
The amount of sample to be taken will depend on the amount
NOTE1—Gasusedcancontainsulfurcompoundsinsufficientquantities
of BaCl solution required (see 10.3.5 and Note 2).
to positively bias the results. The gas may require sulfur compound
removal prior to use.
10.1.1 Quantitatively transfer the mixture to a porcelain
7 capsule or porcelain crucible or platinum crucible, and cover
8.2 Crucibles or Capsules—Porcelain capsules, ⁄8 in.
with about1gof Eschka mixture.
(22 mm) in depth and 1 ⁄4 in. (44 mm) in diameter, or porcelain
crucibles of 30-mL capacity, high or low-form, or platinum
10.2 Ignition—Heat the crucible over a gas flame as de-
crucibles of similar size shall be used for igniting the sample
scribed in 10.2.1, or in a gas or electrically heated muffle
with the Eschka mixture. Porcelain, platinum, Alundum, or
furnace as described in 10.2.2. The use of artificial gas for
silica crucibles of 10 to 15-mL capacity shall be used for the
heating the sample and Eschka mixture is permissible only
final ignition step (see 10.3.8).
when the crucibles are heated in a muffle furnace (see Note 3).
10.2.1 Heat the crucible, placed in a slanting position
9. Reagents
partially covered on a triangle, over a very low flame. This
preventsrapidexpulsionofthevolatilematterandaffordsmore
9.1 Purity of Reagents—Reagent grade chemicals shall be
complete oxidation of the sulfur. After 30 min of low-flame
used in all tests. Unless otherwise indicated, it is intended that
heating, gradually increase the temperature and occasionally
all reagents shall conform to the specifications of theAmerican
stir the mixture until all black particles have disappeared,
Chemical Society, where such specifications are available.
which is an indication of complete combustion.
Other grades may be used, provided it is first ascertained that
10.2.2 Place the crucible in a cold muffle furnace and
the reagent is of sufficiently high purity to permit its use
gradually raise the temperature to 800 6 25 °C in about 1 h.
without impacting the accuracy of the determination.
Maintain this maximum temperature until upon stirring all
9.2 Purity of Water—Unless otherwise indicated, references
black particles have disappeared (about 1 ⁄2 h).
to water shall be understood to mean reagent water, Type III,
10.3 Subsequent Treatment:
conforming to Specification D1193.
10.3.1 Remove the crucible, cool, and empty the contents
9.3 Barium Chloride Solution (100 g/L)—Dissolve 100 g of
quantitativelyintoa200-mLbeaker.Digestwith100mLofhot
barium chloride (BaCl ·2H O) and dilute to 1 L with water.
2 2 1 3
water for ⁄2 to ⁄4 h with occasional stirring.
9.4 Bromine Water (saturated)—Add an excess of bromine
10.3.2 Decant the supernatant liquid through a filter into a
to 1 L of water.
600-mL beaker. Wash the insoluble matter with hot water
several times using 25 mL of water at each washing and filter
9.5 Eschka Mixture—Thoroughly mix two parts by weight
the washings through filter paper into a 600-mL beaker. After
of light calcined magnesium oxide (MgO) with one part of
washing,transfertheinsolublemattertothefilterandwashfive
anhydrous sodium carbonate (Na CO ). Both materials should
2 3
times with hot water, keeping the mixture well agitated,
be as free as possible from sulfur.
collecting the washings in the 600-mL beaker.
9.6 Hydrochloric Acid(1+1)—Mix equal volumes of con-
10.3.3 Treat the filtrate with 10 to 20 mL of saturated
centrated HCl (sp gr 1.19)
...