1、Designation: E 775 87 (Reapproved 2004)Standard Test Methods forTotal Sulfur in the Analysis Sample of Refuse-Derived Fuel1This standard is issued under the fixed designation E 775; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover two alternative procedures forthe determination of total sulfur in prepared analy
3、sis samplesof solid forms of refuse-derived fuel (RDF). Sulfur is includedin the ultimate analysis of RDF.1.2 The test methods appear in the following order:Test SectionsEschka Method 8-11Bomb Washing Method 12 and 131.3 These test methods may be applicable to any wastematerial from which a laborato
4、ry analysis sample can beprepared.1.4 The values stated in inch-pound units are to be regardedas standard. The values given in parentheses are for informa-tion only.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of th
5、e user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificprecautionary statements see Section 6.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterE 180 Practice fo
6、r Determining the Precision of ASTMMethods for Analysis and Testing of Industrial ChemicalsE711 Test Method for Gross Calorific Value of Refuse-Derived Fuel by the Bomb CalorimeterE 829 Practice for Preparing Refuse-Derived Fuels (RDF)Laboratory Samples for Analysis3. Terminology3.1 Definitions of T
7、erm Specific to This Standard:3.1.1 refuse-derived fuelssolid forms of refuse-derivedfuels from which appropriate analytical samples may beprepared are defined as follows in ASTM STP 832:3RDF-1Wastes used as a fuel in as-discarded form withonly bulky wastes removed.RDF-2Wastes processed to coarse pa
8、rticle size with orwithout ferrous metal separation.RDF-3Combustible waste fraction processed to particlesizes, 95 % passing 2-in. square screening.RDF-4Combustible waste fraction processed into powderform, 95 % passing 10-mesh screening.RDF-5Combustible waste fraction densified (compressed)into the
9、 form of pellets, slugs, cubettes, or briquettes.4. Summary of Test Methods4.1 Eschka Method A weighed sample and Eschka mix-ture are ignited together and the sulfur is precipitated from theresulting solution as barium sulfate (BaSO4). The precipitate isfiltered, ashed, and weighed.4.2 Bomb Washing
10、MethodSulfur is precipitated asBaSO4from the oxygen-bomb calorimeter washings and theprecipitate is filtered, ashed, and weighed.5. Significance and Use5.1 The standards are available to producers and users ofRDF for determining the total sulfur content of the fuel.6. Precautions6.1 Due to the origi
11、ns of RDF in municipal waste, commonsense dictates that some precautions should be observed whenconducting tests on the samples. Recommended hygienicpractices include use of gloves when handling RDF; wearingdust masks (NIOSH-approved type), especially while millingRDF samples; conducting tests under
12、 negative pressure hoodwhen possible; and washing hands before eating or smoking.1These test methods are under the jurisdiction of ASTM Committee D34 onWaste Management and is the direct responsibility of Subcommittee D34.03.02 onIndustrial Recovery and Reuse.Current edition approved Aug. 28, 1987.
13、Published October 1987. Originallypublished as E 775 81. Last previous edition E 775 81.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summa
14、ry page onthe ASTM website.3Thesaurus on Resource Recovery Terminology, ASTM STP 832, ASTM, 1983,p.72.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7. Sampling7.1 RDF products are frequently nonhomogeneous. For thisreason significa
15、nt care should be exercised to obtain a repre-sentative laboratory sample from the RDF lot to be character-ized.7.2 The sampling method for this procedure should be basedon agreement between the involved parties.7.3 The laboratory sample must be air-dried and particlesize reduced to pass a 0.5-mm sc
16、reen as described in PracticeE 829. This procedure must be performed carefully to preservethe samples representative characteristics (other than particlesize) while preparing the analysis sample to be used in theprocedures.TEST METHOD AESCHKA METHOD8. Apparatus8.1 Gas (Note 1) or Electric Muffle Fur
17、nace or Burners, forigniting the sample with Eschka mixture and for igniting thebarium sulfate (BaSO4).NOTE 1Gas may contain sulfur compounds in sufficient quantities toaffect the results.8.2 Crucibles or CapsulesPorcelain capsules,78 in. (22mm) in depth and 134 in. (44 mm) in diameter, or porcelain
18、crucibles of 30-mL capacity, high or low-form, or platinumcrucibles of similar size shall be used for igniting the samplewith the Eschka mixture. Porcelain, platinum, Alundum, orsilica crucibles of 10 to 15-mL capacity shall be used for thefinal ignition step (see 10.3.8).9. Reagents9.1 Purity of Re
19、agentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the AmericanChemical Society, where such specifications are available.Other grades4may be used, provided it is first ascertained thatthe reagent
20、 is of sufficiently high purity to permit its usewithout lessening the accuracy of the determination.9.2 Purity of Water Unless otherwise indicated, refer-ences to water shall be understood to mean reagent water, TypeIII conforming to Specification D 1193.9.3 Barium Chloride Solution (100 g/L)Dissol
21、ve 100 g ofbarium chloride (BaCl22H2O) and dilute to 1 L with water.9.4 Bromine Water (saturated)Add an excess of bromineto 1 L of water.9.5 Eschka Mixture Thoroughly mix 2 parts by weight oflight calcined magnesium oxide (MgO) with 1 part of anhy-drous sodium carbonate (Na2CO3). Both materials shou
22、ld be asfree as possible from sulfur.9.6 Hydrochloric Acid (1 + 1)Mix equal volumes of con-centrated HCl (sp gr 1.19) and water.9.7 Hydrochloric Acid (1 + 9)Mix 1 volume of concen-trated HCl (sp gr 1.19) with 9 volumes of water.9.8 Methyl Orange Indicator Solution (0.2 g/L)Dissolve0.2 g of methyl or
23、ange in 1000 mL of hot water and filter.9.9 Sodium Carbonate (saturated solution)Dissolve ap-proximately 60 g of crystallized sodium carbonate(Na2CO310H2O) or 20 g of anhydrous sodium carbonate(Na2CO3) in 100 mL of water, using a sufficient excess ofNa2CO3to ensure a saturated solution.9.10 Sodium H
24、ydroxide Solution (100 g/L)Dissolve 100 gof sodium hydroxide (NaOH) in 1 L of water. This solutionmay be used in place of Na2CO3solution.10. Procedure10.1 Preparation of Sample and Eschka MixtureWeigh tothe nearest 0.1 mg about1gofmixed air-dried analysis sampleand3gofEschka mixture on glazed paper.
25、 Mix thoroughly.The amount of sample to be taken will depend on the amountof BaCl2solution required (see 10.3.5 and Note 2).10.1.1 Quantitatively transfer the mixture to a porcelaincapsule or porcelain crucible or platinum crucible, and coverwith about1gofEschka mixture.10.2 IgnitionHeat the crucibl
26、e over a gas flame as de-scribed in 10.2.1, or in a gas- or electrically heated mufflefurnace as described in 10.2.2. The use of artificial gas forheating the sample and Eschka mixture is permissible onlywhen the crucibles are heated in a muffle (see Note 2).10.2.1 Heat the crucible, placed in a sla
27、nting positionpartially covered on a triangle, over a very low flame. Thisprevents rapid expulsion of the volatile matter and affords morecomplete oxidation of the sulfur. After 30 min of low flameheating, gradually increase the temperature and occasionallystir the mixture until all black particles
28、have disappeared,which is an indication of complete combustion.10.2.2 Place the crucible in a cold muffle furnace andgradually raise the temperature to 800 6 25C in about 1 h.Maintain this maximum temperature until upon stirring allblack particles have disappeared (about 112 h).10.3 Subsequent Treat
29、ment:10.3.1 Remove the crucible, cool, and empty the contentsquantitatively into a 200-mL beaker. Digest with 100 mL of hotwater for12 to34 h with occasional stirring.10.3.2 Decant the supernatant liquid through a filter into a600-mL beaker. Wash the insoluble matter with hot waterseveral times usin
30、g 25 mL of water at each washing and filterthe washings through the filter paper into the 600-mL beaker.After washing, transfer the insoluble matter to the filter andwash five times with hot water, keeping the mixture wellagitated, collecting the wash waters in the 600-mL beaker.10.3.3 Treat the fil
31、trate with 10 to 20 mL of saturatedbromine water. Make slightly acid with HCl and boil to expelthe liberated bromine.10.3.4 Neutralize using methyl orange indicator with NaOHor Na2CO3solution; then add 1 mL of HCl solution (1 + 9).10.3.5 Boil again and then, while stirring constantly, addslowly from
32、 a pipet 10 mL or more of BaCl2solution.NOTE 2Barium chloride solution must be added in excess. If morethan 10 mL of BaCl2solution is required, reduce the weight of sample toabout 0.5 g and repeat the ignition and digestion.4“Reagent Chemicals, American Chemical Society Specification,” AmericanChemi
33、cal Society, Washington, DC. For suggestions on testing of reagents not listedby the American Chemical Society, see “Analar Standards for Laboratory U. K.Chemicals,” BDH Ltd., Poole, Dorset, and the “United States Pharmacopeia.”E 775 87 (2004)210.3.6 Continue boiling for 15 min and allow to stand fo
34、r atleast 2 h, or preferrably overnight, at a temperature just belowboiling.NOTE 3When standing overnight at a temperature slightly less thanboiling, cover the flask with a watchglass to prevent the solution fromevaporating to dryness and to protect it from external contamination.10.3.7 Filter the s
35、olution and the precipitate of bariumsulfate (BaSO4) through an ashless paper and wash the BaSO4 residue with hot water until 1 drop of silver nitrate (AgNO3)solution produces no more than a slight opalescence whenadded to 8 to 10 mL of filtrate.10.3.8 Place the wet filter containing the precipitate
36、 ofbarium sulfate (BaSO4) in a preweighed platinum, porcelain,silica, or Alundum crucible, allowing a free access of air byfolding the paper over the precipitate loosely to preventspattering.10.3.9 Smoke the paper off gradually over a gas burner or ina gas or electrically heated muffle furnace. At n
37、o time allow itto burn with a flame (see Note 4). After charring of the paper,raise the temperature to approximately 925C and heat toconstant weight.NOTE 4Partially covering the crucible while smoking and smolderingwill aid in the prevention of the flaming of the paper.10.3.10 Transfer the crucibles
38、 to a desiccator and weighwhen cooled to room temperature.10.4 Blanks and CorrectionsIn all cases a correction mustbe applied. Either a reagent blank may be run exactly asdescribed above, using the same amount of all reagents thatwere employed in the routine determination, or a more accuratecorrecti
39、on may be made by analyzing a weighed portion of astandard sulfate using the prescribed reagents and operations.NOTE 5If the latter procedure is carried out once a week, or whenevera new supply of a reagent is used for a series of solutions covering theapproximate range of sulfur concentrations in t
40、he samples, it is onlynecessary to add or subtract from the weight of BaSO4determined for thesample the deficiency or excess found by the appropriate “check”determination. This procedure is more accurate than the simple reagentblank because, for the amounts of sulfur in question and condition ofprec
41、ipitation prescribed, the solubility error for BaSO4is probably thelargest one considered. Barium sulfate is soluble in acids5and in purewater, and the solubility limit is reached almost immediately on contactwith the solvent. Hence, if very high-purity reagents are used or extraprecaution is exerci
42、sed, there may be no sulfate apparent in the “blank.”In other words, the solubility limit for BaSO4has not been reached or atany rate not exceeded; consequently, some sulfate in the sample mayremain in solution or has redissolved.11. Calculation11.1 Calculate the sulfur content as follows:Sulfur, %
43、5 A 2 B! 3 13.738/W (1)where:A = grams of BaSO4precipitated,B = grams of BaSO4correction,W = grams of sample used, and13.738 = percentage of sulfur in BaSO4.TEST METHOD BBOMB WASHING METHOD612. Reagents12.1 Purity of Reagentssee 9.1.12.2 Purity of Water see 9.2.12.3 Ammonium Hydroxide (sp gr 0.90)Co
44、ncentrated am-monium hydroxide (NH4OH).12.4 Bromine Water (saturated)see 9.4.12.5 Hydrochloric Acid (1 + 1)see 9.6.12.6 Sodium Carbonate SolutionDissolve 18.02 g ofanhydrous sodium carbonate (Na2CO3) in water and dilute to 1L. The Na2CO3should be previously dried for 24 h at 105C.NOTE 6Other concent
45、rations of sodium carbonate solution may beused.12.7 Wash Solution Dilute 1 mL of a saturated solution ofmethyl orange to 1 L of water.13. Procedure13.1 IgnitionSulfur is determined in the washings fromthe oxygen-bomb calorimeter following calorimetric determi-nation in accordance with Test Method E
46、711. The type ofbomb, amount of water in the bomb, oxygen pressure, andamount of sample taken shall be the same as specified underthe calorimetric determination. The bomb shall stand in thecalorimeter water for not less than 5 min after firing.13.2 Subsequent Treatment:13.2.1 Remove the bomb from th
47、e calorimeter water andopen the valve carefully so as to allow the gases to escape at anapproximately even rate so the pressure is reduced to atmo-spheric in not less than 1 min. Bombs equipped with valvesother than needle valves, such as compression valves, shall beprovided with a device so the val
48、ve can be controlled to permita slow and uniform release of the gases.13.2.2 Open the bomb and examine the inside for traces ofunburned material or sooty deposit. If these are found, discardthe determination. Wash carefully all parts of the interior of thebomb, including the capsule with a fine jet
49、of water containingmethyl orange (12.7) until no acid reaction is observed. It isessential to wash through the valve opening in the case ofbombs equipped with compression valves, or other types ofvalves with large openings, as considerable spray may collectin such valve openings.13.2.3 Collect the washings in a 250-mL beaker and titratewith standard sodium carbonate solution (12.6) to obtain theacid correction for the heating value, as specified in thecalorimetric determination of Test Method E711.13.2.4 Adjust the pH to between 5.5
