1、Designation: D 5198 92 (Reapproved 2003)Standard Practice forNitric Acid Digestion of Solid Waste1This standard is issued under the fixed designation D 5198; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision
2、. 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 This practice describes the digestion of solid wasteusing nitric acid for the subsequent determination of inorganicconstituents by
3、 argon plasma emission spectroscopy or atomicabsorption spectroscopy.1.2 The following elements may be solubilized by thispractice:aluminum manganeseberyllium mercurycadmium nickelchromium phosphoruscopper vanadiumiron zinclead1.3 This practice is to be used when the concentrations oftotal recoverab
4、le elements are to be determined from a wastesample. Total recoverable elements may or may not be equiva-lent to total elements, depending on the element sought and thesample matrix. Recovery from refractory sample matrices,such as soils, is usually significantly less than total concentra-tions of t
5、he elements present.NOTE 1This practice has been used successfully for oily sludges anda municipal digested sludge standard Environmental Protection Agency(EPA) Sample No. 397. The practice may be applicable to some elementsnot listed above, such as arsenic, barium, selenium, cobalt, magnesium,and c
6、alcium. Refractory elements such as silicon, silver, and titanium arenot solubilized by this practice.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 he
7、alth practices and determine the applica-bility of regulatory limitations prior to use. For specific hazardstatements, see Section 7.2. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for Reagent WaterD 2777 Practice for Determination of Precision and Bias ofApplicable Methods of Commit
8、tee D19 on WaterD 3223 Test Method for Total Mercury in WaterD 3682 Test Method for Major and Minor Elements inCombustion Residues from Coal Utilization ProcessesD 3919 Practice for Measuring Trace Elements in Water byGraphite Furnace Atomic Absorption SpectrophotometryD 4503 Practice for Dissolutio
9、n of Solid Waste by LithiumMetaborate FusionD 4698 Practice for Total Digestion of Sediment Samplesfor Chemical Analysis of Various MetalsE 50 Practices for Apparatus, Reagents, and Safety Consid-erations for Chemical Analysis of Metals, Ores, andRelated Materials3. Summary of Practice3.1 A weighed
10、portion of the waste sample is mixed with1 + 1 nitric acid (HNO3) in an Erlenmeyer flask. The flask isheated for2hat90to95C to dissolve the elements of interest.After cooling, the contents of the flask are diluted with reagentwater and filtered, and the filtrate is made up to appropriatevolume for s
11、ubsequent analysis.4. Significance and Use4.1 A knowledge of the inorganic composition of a waste isoften required for the selection of appropriate waste disposalpractices. Solid waste may exist in a variety of forms andcontain a range of organic and inorganic constituents. Thispractice describes a
12、digestion procedure which dissolves manyof the toxic inorganic constituents and produces a solutionsuitable for determination by such techniques as atomic ab-sorption spectroscopy, atomic emission spectroscopy, and soforth. The relatively large sample size aids representativesampling of heterogenous
13、 wastes. The relatively small dilutionfactor allows lower detection limits than most other sampledigestion methods. Volatile metals, such as lead and mercury,are not lost during this digestion procedure. Hydride-formingelements, such as arsenic and selenium, may be partially lost.Samples with total
14、metal contents greater than 5 % may givelow results. The analyst is responsible for determining whetherthis practice is applicable to the solid waste being tested.1This practice is under the jurisdiction of ASTM Committee D34 on WasteManagement and is the direct responsibility of Subcommittee D34.01
15、.06 onAnalytical Methods.Current edition approved Apr. 10, 2003. Published June 2003. Originallyapproved in 1992. Last previous edition approved in 1997 as D 5198 92 (1997).2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For A
16、nnual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Apparatus5.1 Analytical Balance, capable of weighing to 0.01 g.5.2 Erl
17、enmeyer Flasks, 125 mL.5.3 Graduated Cylinder,50mL.5.4 Electric Hot Plate, adjustable, capable of maintaining atemperature of 90 to 95C.5.5 Watch Glasses.5.6 Thermometer.5.7 Funnels, glass or plastic.5.8 Volumetric Flasks, glass-stoppered, 200 mL.5.9 Filter Paper, quantitative, medium flow rate, Wha
18、tmanNo. 40 or equivalent.6. Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specificat
19、ions are available.3Other grades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated, referenceto water shall be understood to mean reagent water
20、 as definedby Type II of Specification D 1193.6.3 Nitric Acid, concentrated, reagent grade.6.4 Nitric Acid (1+1)Add slowly, with stirring, 200 mL ofconcentrated nitric acid (HNO3, sp gr 1.42) to 200 mL water.Cool the mixture and store in a clean pint glass bottle.7. Hazards7.1 Add the nitric acid mi
21、xture slowly, with swirling, to thesample. Samples containing carbonates may foam excessivelyduring acid addition and result in loss of sample. Nitric acidmay react violently with some samples containing organicmaterial.7.2 Addition of acid and sample digestion must be con-ducted in a hood with adeq
22、uate ventilation and shielding toavoid contact with nitrogen oxides, acid fumes, or toxic gases.8. Procedure8.1Weigh5gofathoroughly mixed waste sample to thenearest 0.01 g into a tared Erlenmeyer flask.8.2 With a graduated cylinder, slowly add 25 mL of 1+1nitric acid to the flask. Swirl the flask to
23、 wet the samplecompletely.8.3 Carry a blank of 25 mL of 1+1 nitric acid through theprocedure.8.4 Place the flask on a cold hot plate, cover with a watchglass, and set the hot plate to maintain a temperature of 90 to95C.8.5 Heat the flask and contents for 2 h, occasionally swirlingthe flask to wash d
24、own any sample adhering to the walls.Check the solution temperature with the thermometer andadjust the heat if necessary.8.6 After 2 h, remove the flask from the hot plate and coolto room temperature. Add 50 mL of reagent water to the flask,washing down the flask walls during addition. Swirl the fla
25、sk tomix the contents.8.7 Filter the contents of the flask into a 200 mL volumetricflask. Rinse the flask and filter paper with several smallportions of reagent water and add the rinsings to the volumetricflask.8.8 Dilute the solution in the volumetric flask to the markwith reagent water and mix tho
26、roughly. The solution is nowready for analysis.9. Precision and Bias9.1 No statement is made about either the precision or biassince this practice does not produce a test result. Appendix X1contains representative results obtained with this practice andsubsequent analysis.10. Keywords10.1 digestion;
27、 nitric acid; wasteAPPENDIX(Nonmandatory Information)X1. REPRESENTATIVE ANALYSES OF SAMPLES AFTER NITRIC ACID DIGESTION3Reagent Chemicals, American Chemical Society Specifications, Am. ChemicalSoc., Washington, DC. For suggestions on the testing of reagents not listed by theAmerican Chemical Society
28、, see Reagent Chemicals and Standards, by JosephRosin, D. Van Nostrand Co., Inc., New York, NY, and the United States Pharma-copeia.D 5198 92 (2003)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
29、 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 committee and must be reviewed every f
30、ive years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
31、 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 Box C700, West Conshohocken,
32、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).TABLE X1.1 Nitric Acid Digestion
33、Analysis of Standard SludgeSample (EPA Sample No. 397)ElementConcentration, mg/kgPercentRecoveryActual FoundZn 1323 1300 98Mn 205 235 115Pb 519 500 96Cd 20.8 24.1 116Cr 204 218 107Fe 16 155 16 400 102V 13.0 12.7 98Cu 1095 1130 103Ni 198 186 94Al 4558 4500 99Ti 2121 95 4.5P 11 573 11 800 102Be 0.28 0
34、.5 179As 17 9 53Ag 81 7.4 9.1Hg 16.3 13.6 83TABLE X1.2 Nitric Acid DigestionReplicate Analysis of UsedMotor Oil, mg/kgElement Run 1 Run 2 Run 3Zn 1170 1150 1170Mn 2.5 2.1 2.1Pb 43 40 35Cd 0.6 0.5 0.4Cr 2.8 2.1 2.3Fe 74 66 66V 1.32 1.04 0.92Cu 3.8 3.6 3.6Ni 0.7 NDA0.7 ND 0.7 NDBa 0.6 0.5 0.5Be 0.04 N
35、D 0.04 ND 0.04 NDHg 0.08 ND 0.08 ND 0.08 NDAND = not detected at the detection limit shown.TABLE X1.3 Nitric Acid DigestionRecovery of Used Motor OilMatrix SpikesElementmg/kgPercentRecoveryAdded FoundMn 3.2 3.3 103Pb 3.4 3.0 88Cd 2.0 1.6 80Cr 2.0 2.4 120V 2.6 1.0 38Cu 2.2 4.2 191Ni 2.8 2.75 98Ba 2.3 2.1 91Be 1.6 1.3 81Hg 0.08 0.09 113D 5198 92 (2003)3
