1、Designation: D4978 16Standard Test Methods forScreening of Reactive Sulfides in Waste1This standard is issued under the fixed designation D4978; 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
2、 parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods are applicable to the screening ofreactive sulfides in wastes, liquids, sludges, semisolids, andsolids by using the following
3、 methods:SectionsTest Method ALead Acetate Paper 914Test Method BGas Detector Tube 15191.2 These test methods are not applicable in determining thetype and concentration of reactive sulfides.1.3 These test methods are designed and intended as apreliminary test to complement the more sophisticated qu
4、anti-tative analytical techniques that may be used to determinesulfide concentration. These test methods offer, to the user, theoption and the ability to screen waste for potentially hazardouslevels of reactive sulfide when the sophisticated techniques arenot available and the total waste compositio
5、n is unknown.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 and health practices and determine the applica-bility of regulatory limitations prior to use. S
6、pecific hazardinformation is given in Section 7 and 11.3.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent Water3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 reactive sulfidea compound containing sulfide thatreadily forms hydrogen sulfide gas upon re
7、action with acid.3.1.2 screening analysisa preliminary qualitative or semi-quantitative test developed from classical qualitative andquantitative techniques that is designed to efficiently give theuser parameters about a waste that will aid in determiningwaste identification, process compatibility,
8、and safety in han-dling.4. Summary of Test Methods4.1 Method A: Lead Acetate PaperA sample of wastematerial is acidified. If sulfides are present in the waste,hydrogen sulfide (H2S) is evolved. In the presence of hydrogensulfide, lead acetate paper changes color to silvery brown orblack.4.2 Method B
9、: Gas Detector TubeA portion of the sampleis acidified in a beaker to release sulfide as hydrogen sulfidegas. The gas is funneled through a detector tube creating acolor stain in the tube proportionate to the concentration ofsulfide gas in the vapor. A definite color change in the detectortube indic
10、ates a positive presence of sulfide.5. Significance and Use5.1 These test methods are intended for use by wastetreatment, storage, disposal, and remedial facilities, in order toshow the presence of potentially hazardous sulfide.5.2 Method B: Gas Detector TubeThis proposed testmethod was designed to
11、measure gases migrating into an airspace at a height of 10 units (for example, 10 ft) from areceiving or mixing pit of 10 units square (for example, 100ft2). In essence, the total volume of the atmosphere is approxi-mately 10 times the surface area of the sample and testsolution.6. Reagents6.1 Purit
12、y of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.3Other grades may be used1These tes
13、t methods are under the jurisdiction of ASTM Committee D34 onWaste Management and is the direct responsibility of Subcommittee D34.01.05 onScreening Methods.Current edition approved May 1, 2016. Published May 2016. Originallyapproved in 1989. Last previous edition approved in 2007 as D4978 95(2007)w
14、hich was withdrawn January 2016 and reinstated in May 2016. DOI: 10.1520/D4978-16.2For 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 Summary pag
15、e onthe ASTM website.3Reagent Chemicals, American Chemical Society Specifications , AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the Un
16、ited States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1provided it is first ascertained that the reagent is of sufficientlyhigh purity t
17、o permit its use without lessening the accuracy ofthe determination.6.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type III of Specification D1193.7. Hazards7.1 These tests should be conducted under a fume hood.7.2 Avoid inhal
18、ation and skin or eye contact, or both, withall hazardous material.8. Sampling8.1 Collect a representative sample of the waste in a sealedcontainer.8.2 Store the sample in an operating fume hood.8.3 The sample should be analyzed as soon as possible.TEST METHOD ALEAD ACETATE PAPER9. Interferences9.1
19、Compounds evolving gases or vapors upon acidificationthat react with lead may interfere causing false positives.NOTE 1All positives should be followed up by a more detailedmethod, that is, distillation for total sulfides.10. Reagents and Materials10.1 Beakers or Test Tubes.10.2 Stirring Rod.10.3 Hyd
20、rochloric Acid (1+1)Add 1 volume of hydro-chloric acid (HCl, sp gr 1.19) to 1 volume water.10.4 Lead Acetate Paper.10.5 Sodium Sulfide, Standard Solution (1 mL = 1 mgNa2S)Dissolve 1.00 g sodium sulfide (Na2S) in water anddilute to 1 L. Make this solution fresh daily.10.6 Quality Control Check Standa
21、rdDilute an appropri-ate volume of sodium sufide standard solution with water toproduce a solution with the desired action level. Make thissolution fresh daily.11. Procedure11.1 Place 5 to 10 g of sample into the beaker (slurry withapproximately 15 mL water if the material is solid).11.2 Wet a strip
22、 of lead acetate paper and let it adhere to theside of beaker above the sample.11.3 Slowly and carefully adjust the pH to less than 2.0 withHCl solution 1 + 1.NOTE 2Warning: The addition of HCl to waste materials may causeviolent reaction or highly toxic vapors, or both.11.4 Stir the solution.11.5 A
23、silvery brown to black color on the lead acetate paperindicates the presence of sulfides and shall be recorded aspositive. Compare the color observed to a blank and standardsolution.11.6 No color change to the lead acetate paper will bereported as negative.12. Report12.1 Report the following informa
24、tion:12.1.1 Sample identification,12.1.2 Date of test,12.1.3 Test procedure performed, and12.1.4 Sample classification: positive or negative.13. Quality Control13.1 A quality control check sample shall be tested witheach batch of samples. The concentration of this sample shouldreflect the action lev
25、el required by the laboratory. Method orreagent blanks, duplications, and fortification (spikes), shouldbe performed at an action level specified by the laboratory at anappropriate frequency.13.2 Method detection limits should be determined by eachlaboratory using the standard and at the appropriate
26、 actionlevel.14. Precision and Bias14.1 No statement is made about either the precision or biasof Test Method A for measuring sulfides in wastes since theresult merely states whether there is conformance to the criteriafor success specified in the procedure.TEST METHOD BGAS DETECTOR TUBE15. Reagents
27、 and Materials15.1 Buffer SolutionDissolve 740 g trisodium phosphate(Na3PO4) in 3.5 L of water. Add carefully 500 mL ofphosphoric acid (H3PO4, 85 %) and mix. Adjust the pH to 2with H3PO4if necessary.15.2 pH Indicator Paper, range: 0 to 14.15.3 Disposable Beaker, 400-mL.15.4 Plastic Funnel, 8-cm.15.5
28、 Jack Stand.15.6 Ring Stand and Clamps.15.7 Gas Detector Pump with a volume range of 0 to 100cc.15.8 Gas Detector Tube for hydrogen sulfide.15.9 Magnetic Stirrer.15.10 Magnetic Stirring Bar.15.11 See Fig. 1 for suggested equipment setup.16. Procedure16.1 Place approximately 20 g of the material to b
29、e testedinto a beaker with a magnetic stirring bar. Solid samples shallbe crushed into small particles 9.5 mm in size (38-in. meshscreen).16.2 Add approximately 50 mL of the buffer solution to thesample.16.3 With a lab jack, raise the beaker and magnetic stirrer toa point at which the funnel fits do
30、wn inside the beaker opening.D4978 16216.4 The gas detector tube with the pump attached shouldbe directly positioned through the small opening of the funnel,with the tip of the tube about midway in the funnel area.16.5 Begin stirring the sample.16.6 Activate the pump by pulling out the handle to dra
31、w in100 cm3of atmosphere from the apparatus.16.7 A positive sulfide is determined by a color stain in thedetector tube.16.8 Allow at least a 1-min reaction time before readingresults.17. Report17.1 Report the following information:17.1.1 Sample identification,17.1.2 Date of test,17.1.3 Test procedur
32、e performed, and17.1.4 Sample classification: positive or negative.18. Quality Control18.1 A quality control check sample shall be tested witheach batch of samples. The concentration of this sample shouldreflect the action level required by the laboratory. Method orreagent blanks, duplications, and
33、fortification (spikes), shouldbe performed at an action level specified by the laboratory at anappropriate frequency.18.2 Method detection limits should be determined by eachlaboratory using the standard and at the appropriate actionlevel.19. Precision and Bias19.1 No statement is made about either
34、the precision or biasof Method B for measuring sulfides in wastes since the resultmerely states whether there is conformance to the criteria forsuccess specified in the procedure.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item me
35、ntionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committe
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37、ng of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO
38、 Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1 Method B, Sulfide Test ApparatusD4978 163
