ASTM E777-17a

Designation: E777 − 17aStandard Test Method forCarbon and Hydrogen in the Analysis Sample of Refuse-Derived Fuel1This standard is issued under the fixed designation E777; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (´) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method is for the determination of total carbonand hydrogen in a sample of refuse-derived fuel (RDF). Bothcarbon and hydrogen are determined in one analysis. This testmethod yields the total percentages of carbon and hydrogen inRDF as analyzed and the results include not only carbon andhydrogen in the organic matter, but also the carbon present inmineral carbonates and the hydrogen present in the freemoisture accompanying the analysis sample as well as hydro-gen present as water of hydration.NOTE 1—It is recognized that certain technical applications of the dataderived from this test procedure may justify additional corrections. Thesecorrections could involve compensation for the carbon present ascarbonates, the hydrogen of free moisture accompanying the analysissample, and the calculated hydrogen present as water of hydration.1.2 This test method may be applicable to any wastematerial from which a laboratory analysis sample can beprepared.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific precautionary statements, see Section 8.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD5681 Terminology for Waste and Waste ManagementE790 Test Method for Residual Moisture in Refuse-DerivedFuel Analysis SamplesE791 Test Method for Calculating Refuse-Derived FuelAnalysis Data from As-Determined to Different BasesE829 Practice for Preparing Refuse-Derived Fuel (RDF)Laboratory Samples for Analysis3. Terminology3.1 For definitions of terms used in this test method, refer toTerminology D5681.4. Summary of Test Method4.1 The determination is made by burning the sample toconvert carbon to carbon dioxide and hydrogen to water. Thecombustion is carried out using high-purity oxygen that hasbeen passed through a purifying train. The carbon dioxide andwater are recovered in an absorption train. Combustion tubepacking is used to remove interfering substances. This testmethod gives the total percentage of carbon and hydrogen inthe RDF as analyzed, including the carbon in carbonates andthe hydrogen in water.5. Significance and Use5.1 This standard is intended to provide a method fordetermining the weight percent of carbon and hydrogen in anRDF analysis sample.5.2 Carbon and hydrogen are components of RDF and,when determined, can be used for calculating RDF combustioncharacteristics.6. Apparatus6.1 Oxygen Purifying Train—High-purity oxygen is passedthrough water and carbon dioxide absorbers prior to use for1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.03 on Treatment,Recovery and Reuse.Current edition approved Dec. 1, 2017. Published December 2017. Originallyapproved in 1987. Last previous edition approved in 2017 as E777 – 17. DOI:10.1520/E0777-17A.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at service@astm.org. For Annual Book of ASTMStandards volume information, refer to the standard’s Document Summary page onthe ASTM website.Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1combustion. The oxygen purifying train consists of the follow-ing three components in order of gas passage (see Fig. 1):6.1.1 First Water Absorber—A container constructed suchthat oxygen must pass through a column of water-removingreagent. The container shall have a capacity for at least 45 cm3of solid reagent, and the minimum gas distance traveledthrough the reagent shall be at least 80 mm.6.1.2 Carbon Dioxide Absorber—If solid reagents are usedfor carbon dioxide absorption, the container shall be asdescribed in 6.1.1. If a solution is used, the container shall bea Vanier bulb. It shall provide a column of reagent adequate toremove carbon dioxide below the testing laboratory’s analyticreporting limit.6.1.3 Second Water Absorber—Same as specified in 6.1.1.6.2 Flow Meter, used to permit volumetric measurement ofthe rate of flow of oxygen during the determination. It shall besuitable for measuring flow rates within the range from 50 to100 mL/min. The use of a double-stage pressure-reducingregulator with gage and needle valve is recommended to permiteasy and accurate adjustment to the rate of flow.6.3 Combustion Unit, consisting of three electrically heatedfurnace sections, individually controlled, which may bemounted on rails for easy movement. The upper part of eachfurnace may be hinged so that it can be opened for inspectionof the combustion tube. The three furnace sections shall be asfollows (see Fig. 1):6.3.1 Furnace Section 1—Furnace 1 is nearest the oxygeninlet of the combustion tube, approximately 130 mm long andused to heat the inlet of the combustion tube and the sample. Itshall be capable of rapidly attaining an operating temperatureof 875 6 25 °C.NOTE 2—Combustion tube temperature shall be measured by means ofa thermocouple placed immediately adjacent to the tube near the center ofthe appropriate tube section.6.3.2 Furnace Section 2—Furnace 2 shall be approximately330 mm in length and used to heat that portion of the tube filledwith cupric oxide. The operating temperature shall be 850 620 °C (see Note 2).6.3.3 Furnace Section 3—Furnace 3 shall be approximately230 mm long, and used to heat that portion of the tube filledwith lead chromate or silver. The operating temperature shallbe 500 6 50 °C.6.3.4 Combustion Tube, made of fused quartz, or high-silicaglass and having a nominal inside diameter which may varywithin the limits of 19 to 22 mm and a minimum total lengthof 970 mm. The exit shall be tapered to provide a tubulatedsection for connection to the absorption train. The tubulatedsection shall have a length of 20 to 25 mm, an internal diameterof not less than 3 mm, and an external diameter of approxi-mately 7 mm. The total length of the reduced end shall notexceed 60 mm. If a translucent fused quartz tube is used, atransparent section 190 mm long, located 250 mm from theoxygen inlet end of the tube, will be found convenient (see Fig.2).6.3.5 Combustion Boat, made of glazed porcelain, fusedsilica, or platinum. Boats with internal dimensions of approxi-mately 70 by 8 by 8 mm have been found convenient to use inthis analysis.6.4 Absorption Train, identical to the oxygen absorptiontrain described in 6.1. The absorption train shall consist of thefollowing components arranged as listed which corresponds tothe order of oxygen passage through the apparatus (see Fig. 1):6.4.1 First Water Absorber, as described in 6.1.1.6.4.2 Carbon Dioxide Absorber, as described in 6.1.2.6.4.3 Second Water Absorber, as described in 6.1.3. Thesecond water absorber is also known as a guard tube.A = flowmeter (6.2) E, F, G, H, I = combustion unit (6.3)B, C, D = oxygen purifying train (6.1) E = furnace 1 (6.3.1)B = first water absorber (6.1.1) F = furnace 2 (6.3.2)C = carbon dioxide absorber (6.1.2) G = furnace 3 (6.3.3)D = second water absorber (6.1.3) H = combustion tube (6.3.4)I = combustion boat (6.3.5)J, K, L = absorption train (6.4)J = first water absorber (6.4.1)K = carbon dioxide absorber (6.4.2)L = guard tube (6.4.3)NOTE 1—C and K can substitute a Vanier bulb if liquid absorbent is used.FIG. 1 Construction of Oxygen Purifying ApparatusE777 − 17a27. Reagents7.1 Purity of Reagents—Reagent-grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of theAmericanChemical Society, where such specifications are available.3Other grades may be used, provided it is first determined thatthe reagent is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.7.2 Purity of Water—Unless otherwise indicated, referencesto water shall be understood to mean reagent water, Type III,conforming to Specification D1193.7.3 Oxygen, with minimum acceptable purity 99.5 %.NOTE 3—If the blank tests for flow (see 10.3.2) indicate interferingimpurities in the oxygen supply by consistent weight gain in the absorbers,eliminate these impurities by using a preheater furnace and tube, filledwith cupric oxide. Operate this preheater at 850 6 20 °C and insert inseries between the supply tank of oxygen and the purification train.7.4 Combustion Tube Reagents:7.4.1 Cupric Oxide (CuO), wire form, dust-free.7.4.2 Fused Lead Chromate (PbCrO4), approximately 2.38to 0.84 mm in size.7.4.3 Silver Gauze, 99.9 % silver minimum purity, 0.84 mm,made from approximately No. 27 B wearing NIOSH-approved type dust masks, espe-cially while milling RDF samples; conducting tests under anegative pressure hood; and washing hands with soap andwater after completing the analysis.9. Sampling9.1 RDF products are frequently inhomogeneous. For thisreason, care should be exercised to ensure that a representativelaboratory sample from the RDF lot to be characterized isobtained.9.2 The sampling method for this procedure should be basedon agreement between the involved parties.9.3 The laboratory sample must be air-dried and particlesize reduced to pass through a 0.5-mm screen as described inPractice E829. This procedure must be carefully performed topreserve the sample’s representativeness excepting particle sizewhile preparing the analysis sample for analysis.10. Preparation of Apparatus10.1 Combustion Tube Packing—To ensure complete oxi-dation of combustion products and complete removal ofinterfering substances such as sulfur oxides, the combustiontube shall be packed with cupric oxide and lead chromate orsilver gauze. The configuration and lengths of the tube fillingsand separating plugs shall be as shown in Fig. 2 (see Note 5).It is recommended that the tube be placed in a vertical position3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4Trade names of this reagent are Anhydrone or Dehydrite.A = clear fused quartz section (optional when a translucent quartz tube is used)B = cupric oxide fillingC = lead chromate or silver gauze fillingP1,P2,P3= oxidized copper gauze plugsNOTE 1—When furnace sections longer than those specified in 6.3 are to be used, changes in the above dimensions shall be in accordance withprovisions of Note 5.FIG. 2 Arrangement of Tube Filling for Combustion TubeE777 − 17a3(constricted end downward) for packing. When filling the tubewith lead chromate, any residual reagent adhering to the wallsof the empty portion of the tube must be removed. When silvergauze is used as a tube filling, the required length of filling maybe prepared conveniently from three or four strips 150 to200 mm in length, by rolling each strip into a cylindrical plugand inserting the strips end-to-end in the tube.NOTE 5—Longer furnaces with appropriate lengths of tube packing canbe used.10.2 Purification and Absorption Trains:10.2.1 Water Absorbers—Fill a container, described in6.1.1, with a solid desiccant, as described in 7.5.1, by addingthe required amount in small portions and settling each portionby gently tapping between additions. Place a glass wool plugbetween the reagent and absorber outlet to prevent loss ofreagent dust.10.2.2 Carbon Dioxide Absorbers—If a solid reagent is usedfor the retention of carbon dioxide (7.5.2), fill the absorber(6.1.2) as described in 10.2.1. Place a layer or cap of desiccantin the outlet section of the container; it shall be the same typeof dessicant as that used in the water absorber. This layer shallhave a bulk volume not less than one-fourth nor more thanone-third of the combined volume of both reagents.10.2.2.1 If a liquid absorbent is used, fill the inner tube ofthe Vanier bulb with the same desiccant used in the waterabsorber. If a solid absorbent is used, place a glass wool plugin the outlet section of the container to prevent loss of reagentdust.10.2.3 Guard Tube—Pack a container, as described in 6.1.1,with equal volumes of the water absorbent and a solid carbondioxide absorbent.10.2.4 Connections—To ensure a closed system from theoxygen supply tank to the guard tube at the end of theabsorption train, it is recommended that all connections beglass-to-glass or glass-to-quartz butt joints with short lengthsof flexible tubing as seals. The connection between thepurification train and the combustion tube may be made bymeans of a rubber stopper or other suitable device. Allconnections shall be gastight. No lubricant shall be used formaking tubing connections in the absorption train.10.3 Conditioning of Apparatus:10.3.1 Newly Packed Combustion Tube—Burn a sample ofRDF as described in 11.4 except that the products of combus-tion need not be fixed in a weighed absorption train.10.3.2 Used Combustion Tube—After any extended shut-down (one day or more) test the combustion train under thistest method’s conditions, but without burning a sample, for40 min with weighed absorbers connected. A variation of notmore than 0.5 mg of both water and carbon dioxide absorbersshall be considered satisfactory (see Note 3).10.3.3 Absorption Train—Condition freshly packed absorb-ers and guard tubes by burning a sample of RDF, as describedin 11.4, except that the absorber weights need not be deter-mined.10.3.4 Analyze a control standard frequently, parti