ASTM D5198-17

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Designation: D5198 − 09 D5198 − 17
Standard Practice for
Nitric Acid Digestion of Solid Waste
This standard is issued under the fixed designation D5198; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This practice describes the partial digestion of solid waste using nitric acid for the subsequent determination of inorganic
constituents by plasma emission spectroscopy or atomic absorption spectroscopy.the total recoverable content of inorganic
constituents.
1.2 The following elements may be solubilized by this practice:
aluminum manganese
beryllium mercury
cadmium nickel
chromium phosphorus
copper vanadium
iron zinc
lead
1.2 This practice is to be 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 and
elemental content, because of the solubility of the speciated forms of the element in the sample matrix. Recovery from refractory
sample matrices, such as soils, is usually significantly less than total concentrations of the elements present.
NOTE 1—This practice has been used successfully for oily sludges and a municipal digested sludge standard [Environmental Protection Agency (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 This practice has been divided into two methods, A and B, to account for the advent of digestion blocks. Method A
utilizeswith 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 other 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 responsibility
of the user of this standard to establish appropriate safety safety, health, and healthenvironmental practices and determine the
applicability 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 standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
D5681 Terminology for Waste and Waste Management
3. Terminology
3.1 Definitions—For definitions of terms used in this standard, refer to Terminology D5681.
This practice is under the jurisdiction of ASTM Committee D34 on Waste Management and is the direct responsibility of Subcommittee D34.01.06 on Analytical
Methods.
Current edition approved Feb. 1, 2009Dec. 1, 2017. Published March 2009December 2017. Originally approved in 1992. Last previous edition approved in 20032009 as
D5198 – 92 (2003).D5198 – 09. DOI: 10.1520/D5198-09.10.1520/D5198-17.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
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D5198 − 17
4. Summary of Practice
4.1 A weighed portion of the waste sample is mixed with 1 + 1 nitric acid (HNO ) in an Erlenmeyer flask. The flask is heated
on an electric hot plate (Method A) or electric digestion block (Method B) for 2 h at 90 to 95°C95 °C to dissolve the elements of
interest. After cooling, the contents of the flask are diluted with reagent water and filtered, and the filtrate is made up to appropriate
volume for subsequent analysis.
5. Significance and Use
5.1 A knowledge of the inorganic composition of a waste is often required for the selection of appropriate waste disposal
practices. Solid waste may exist in a variety of forms and contain a range of organic and inorganic constituents. This practice
describes a digestion procedure which dissolves many of the toxic inorganic constituents and produces a solution suitable for
determination of 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 dilution
factor allows lower detection limits than most other sample digestion methods. Volatile metals, such as lead and mercury, are not
lost during this digestion procedure, however organo-lead and organo-mercury may not be completely digested. Hydride-forming
elements, such as arsenic and selenium, may be partially lost. Samples with total metal contents greater than 5 % may give low
results. The analyst is responsible for determining whether this practice is applicable to the solid waste being tested.
METHOD A – HOT PLATE
6. Apparatus
6.1 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 Plate, adjustable, capable of maintaining a temperature of 90 to 95°C.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. Reagents
7.1 Purity of Reagents—Reagent grade Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it is
intended that all reagents shall conform to the specifications of the Committee on Analytical Reagents of the American Chemical
Society, where such specifications are available. Other grades may be used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the accuracy of the determination.
7.2 Purity of Water—Unless otherwise indicated, reference to water shall be understood to mean reagent water as defined by
Type II of Specification 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 (HNO , sp gr 1.42) to 200 mL
water. Cool the mixture and store in a clean pint glass bottle.
7. Hazards
7.1 Add the nitric acid mixture slowly, with swirling, to the sample. Samples containing carbonates may foam excessively
during acid addition and result in loss of sample. Nitric acid may react violently with some samples containing
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