1、Designation: D5198 09D5198 17Standard Practice forNitric Acid Digestion of Solid Waste1This standard is issued under the fixed designation D5198; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number i
2、n parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This practice describes the partial digestion of solid waste using nitric acid for the subsequent determination of inorganicconstituents by pla
3、sma emission spectroscopy or atomic absorption spectroscopy.the total recoverable content of inorganicconstituents.1.2 The following elements may be solubilized by this practice:aluminum manganeseberyllium mercurycadmium nickelchromium phosphoruscopper vanadiumiron zinclead1.2 This practice is to be
4、 used when the concentrations of total recoverable elements are to be determined from a waste sample.Total recoverable elements may or may not be are often not equivalent to total elements, depending on the element sought andelemental content, because of the solubility of the speciated forms of the
5、element in the sample matrix. Recovery from refractorysample matrices, such as soils, is usually significantly less than total concentrations of the elements present.NOTE 1This practice has been used successfully for oily sludges and a municipal digested sludge standard Environmental Protection Agen
6、cy (EPA)Sample No. 397. The practice may be applicable to some elements not listed above, such as arsenic, barium, selenium, cobalt, magnesium, and calcium.Refractory elements such as silicon, silver, and titanium, as well as organo-mercuryorgano-mercury, are not solubilized by this practice.1.3 Thi
7、s practice has been divided into two methods, A and B, to account for the advent of digestion blocks. Method Autilizeswith Method A utilizing an electric hot plate; plate and Method B utilizesutilizing an electric digestion block.1.4 The values stated in SI units are to be regarded as standard. No o
8、ther units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices an
9、d determine theapplicability of regulatory limitations prior to use.For specific hazard statements, see Section 7.1.6 This international standard was developed in accordance with internationally recognized principles on standardizationestablished in the Decision on Principles for the Development of
10、International Standards, Guides and Recommendations issuedby the World Trade Organization Technical Barriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD5681 Terminology for Waste and Waste Management3. Terminology3.1 DefinitionsFor defin
11、itions of terms used in this standard, refer to Terminology D5681.1 This practice is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on AnalyticalMethods.Current edition approved Feb. 1, 2009Dec. 1, 2017. Published March 200
12、9December 2017. Originally approved in 1992. Last previous edition approved in 20032009 asD5198 92 (2003).D5198 09. DOI: 10.1520/D5198-09.10.1520/D5198-17.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM
13、Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically poss
14、ible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, We
15、st Conshohocken, PA 19428-2959. United States14. Summary of Practice4.1 A weighed portion of the waste sample is mixed with 1 + 1 nitric acid (HNO3) in an Erlenmeyer flask. The flask is heatedon an electric hot plate (Method A) or electric digestion block (Method B) for 2 h at 90 to 95C95 C to disso
16、lve the elements ofinterest.After cooling, the contents of the flask are diluted with reagent water and filtered, and the filtrate is made up to appropriatevolume for subsequent analysis.5. Significance and Use5.1 A knowledge of the inorganic composition of a waste is often required for the selectio
17、n of appropriate waste disposalpractices. Solid waste may exist in a variety of forms and contain a range of organic and inorganic constituents. This practicedescribes a digestion procedure which dissolves many of the toxic inorganic constituents and produces a solution suitable fordetermination of
18、total recoverable contents by such techniques as atomic absorption spectroscopy, atomic emission spectroscopy,and so forth. The relatively large sample size aids representative sampling of heterogenous wastes. The relatively small dilutionfactor allows lower detection limits than most other sample d
19、igestion methods. Volatile metals, such as lead and mercury, are notlost during this digestion procedure, however organo-lead and organo-mercury may not be completely digested. Hydride-formingelements, such as arsenic and selenium, may be partially lost. Samples with total metal contents greater tha
20、n 5 % may give lowresults. The analyst is responsible for determining whether this practice is applicable to the solid waste being tested.METHOD A HOT PLATE6. Apparatus6.1 Analytical Balance, capable of weighing to 0.01 g.6.2 Erlenmeyer Flasks, 125 mL.6.3 Graduated Cylinder, 50 mL.6.4 Electric Hot P
21、late, adjustable, capable of maintaining a temperature of 90 to 95C.95 C.6.5 Watch Glasses.6.6 Thermometer.6.7 Funnels, glass or plastic.6.8 Volumetric Flasks, glass-stoppered, 200 mL.6.9 Filter Paper, quantitative, medium flow rate, Whatman No. 40 or equivalent.6.10 Fume Hood.7. Reagents7.1 Purity
22、of ReagentsReagent grade Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it isintended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American ChemicalSociety, where such specifications are available.3 Other grades
23、 may be used, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening the accuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, reference to water shall be understood to mean reagent water as defined byType II of Spec
24、ification D1193.7.3 Nitric Acid, concentrated, reagent grade.7.4 Nitric Acid (1+1)(1 + 1)Add slowly, with stirring, 200 mL of concentrated nitric acid (HNO3, sp gr 1.42) to 200 mLwater. Cool the mixture and store in a clean pint glass bottle.7. Hazards7.1 Add the nitric acid mixture slowly, with swi
25、rling, to the sample. Samples containing carbonates may foam excessivelyduring acid addition and result in loss of sample. Nitric acid may react violently with some samples containing organic material.7.2 Addition of acid and sample digestion must be conducted in a hood with adequate ventilation and
26、 shielding to avoid contactwith nitrogen oxides, acid fumes, or toxic gases.8. Procedure8.1 Weigh 5 g of a thoroughly mixed waste sample to the nearest 0.01 g into a tared Erlenmeyer flask.3 Reagent Chemicals, American Chemical Society Specifications, , Am. American Chemical Soc.,Society, Washington
27、, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Reagent Chemicals and Standards, by Joseph Rosin, D.D., Van Nostrand Co., Inc., New York, NY, and the United StatesPharmacopeiaPharmacopeia. .D5198 1728.2 With a graduated cylinder, slowly add 25 mL of 1
28、+11 + 1 nitric acid to the flask. Swirl the flask to wet the samplecompletely.8.3 Carry a blank of 25 mL of 1+11 + 1 nitric acid through the procedure.8.4 Place the flask on a cold hot plate, cover with a watch glass, and set the hot plate to maintain a temperature of 90 to95C.95 C.8.5 Heat the flas
29、k and contents for 2 h, occasionally swirling the flask to wash down any sample adhering to the walls. Checkthe solution temperature with the thermometer and adjust the heat if necessary.8.6 After 2 h, remove the flask from the hot plate and cool to room temperature. Add 50 mL of reagent water to th
30、e flask,washing down the flask walls during addition. Swirl the flask to mix the contents.8.7 Filter the contents of the flask into a 200 mL volumetric flask. Rinse the flask and filter paper with several small portionsof reagent water and add the rinsings to the volumetric flask.8.8 Dilute the solu
31、tion in the volumetric flask to the mark with reagent water and mix thoroughly. The solution is now readyfor analysis.METHOD B DIGESTION BLOCK9. Apparatus9.1 Analytical Balance, capable of weighing to 0.01 g.9.2 Fume Hood.9.3 Graduated Digestion Tubes.9.4 Graduated Cylinder, 50 mL.9.5 Digestion Tube
32、 Filters.9.6 Digestion Block, adjustable, capable of maintaining a temperature of 90 to 95C.95 C.10. Reagents10.1 Purity of ReagentsReagent grade Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it isintended that all reagents shall conform to the specifications of the
33、 Committee on Analytical Reagents of the American ChemicalSociety, where such specifications are available.3 Other grades may be used, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening the accuracy of the determination.10.2 Purity of
34、WaterUnless otherwise indicated, reference to water shall be understood to mean reagent water as defined byType II of Specification D1193.10.3 Nitric Acid, concentrated, reagent grade.10.4 Nitric Acid (1 + 1)Add slowly, with stirring, 200 mL of concentrated nitric acid (HNO3, sp gr 1.42) to 200 mL w
35、ater.Cool the mixture and store in a clean pint glass bottle.11. Hazards11.1 Add the nitric acid mixture slowly, with swirling, to the sample. Samples containing carbonites may foam excessivelyduring acid addition and result in loss of sample. Nitric acid may react violently with some samples contai
36、ning organic material.11.2 Addition of acid and sample digestion must be conducted in a hood with adequate ventilation and shielding to avoid contactwith nitrogen oxides, acid fumes, or toxic gases.11. Procedure11.1 Weigh 5 g of a thoroughly mixed waste sample to the nearest 0.01 g and transfer into
37、 a graduated digestion tube.11.2 With a graduated cylinder, slowly add 25 mL of 1 + 1 nitric acid to the digestion tube. Swirl the tube to wet the samplecompletely.11.3 Carry a blank of 25 mL of 1 + 1 nitric acid through the procedure.11.4 Place the digestion tube in a digestion block in a fume hood
38、 and set the digestion block to maintain a temperature of 90to 95C.95 C.11.5 Heat the tube and contents for 2 h, until a volume of approximately 15 mL remains.11.6 After 2 h, remove the tube from the digestion block and cool to room temperature.11.7 Filter the contents of the tube with a digestion t
39、ube filter. Rinse the flask and filter paper with several small portions ofreagent water and add the rinsings to the volumetric flask.D5198 17311.8 Dilute the solution to 50 mL. The solution is now ready for analysis.12. Precision and Bias12.1 No statement is made about either the precision or bias
40、since this practice does not produce a test result. Appendix X1contains representative results obtained with this practice (Method A) and subsequent analysis.13. Keywords13.1 digestion; nitric acid; wasteAPPENDIX(Nonmandatory Information)X1. REPRESENTATIVE ANALYSES OF SAMPLES AFTER NITRIC ACID DIGES
41、TIONX1.1 See Tables X1.1-X1.3.TABLE X1.1 Nitric Acid DigestionAnalysis Digestion Analysisof Standard Sludge Sample (EPA Sample No. 397)Element Concentration, mg/kg PercentRecoveryActual 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
42、1095 1130 103Ni 198 186 94Al 4558 4500 99Ti 2121 95 4.5P 11 573 11 800 102Be 0.28 0.5 179As 17 9 53Ag 81 7.4 9.1Hg 16.3 13.6 83TABLE X1.2 Nitric Acid DigestionReplicate Digestion Replicate Analysis of Used Motor 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
43、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 NDA 0.7 ND 0.7 NDBa 0.6 0.5 0.5Be 0.04 ND 0.04 ND 0.04 NDHg 0.08 ND 0.08 ND 0.08 NDA ND = not detected at the detection limit shown.D5198 174ASTM International takes no position respecting the validity of any patent rights asserted in
44、connection with any item mentioned inthis 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 res
45、ponsible technical committee and must be reviewed every five 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 carefu
46、l consideration at a meeting 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,
47、 100 Barr Harbor Drive, PO 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 AST
48、M 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:/ X1.3 Nitric Acid DigestionRecovery Digestion Recovery of Used Motor Oil Matrix SpikesElement mg/kg PercentRecoveryAdded 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 113D5198 175
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