ASTM D5830-22

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it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D5830 − 14 D5830 − 22
Standard Test Method for
Solvents Analysis in Hazardous Waste Using Gas
Chromatography
This standard is issued under the fixed designation D5830; 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 test method is used to determine qualitatively and quantitatively the presence of the following compounds in waste
samples using gas chromatography. This test method is designedintended for use as a screening method with a typical reporting
level of 0.1 %.
Dichodifluoromethane Tetrahydrofuran
Trichlorofluoromethane Acetone
1,1,2-Trichloro-1,2,2- Methyl Ethyl Ketone
trifluoroethane MIBK
Methanol Cyclohexanone
Ethanol Ethyl Acetate
Isopropanol Propyl Acetate
n-Propanol Butyl Acetate
Isobutanol Benzene
n-Butanol Toluene
tert-Butanol Ethylbenzene
Methylene Chloride Xylenes
Chloroform Styrene
Carbon Tetrachloride Chlorobenzene
1,1-Dichloroethane Dichlorobenzenes
1,2-Dichloroethane Nitrobenzene
1,2-Dichloropropane Fluorobenzene
1,1-Dichloroethylene n-Propyl Benzene
1,2-Dichloroethene Isopropyl Benzene
1,1,1-Trichloroethane Isobutyl Benzene
Tetrachloroethylene n-Butyl Benzene
Trichloroethylene 2-Ethoxyethanol
Tetrachloroethane 2-Butoxyethanol
Cyclopentane 2-Ethoxyethanol Acetate
Pentane 2-Methoxyethanol
Hexane Bromoform
Heptane Carbitol
Cyclohexane Ethyl Ether
Isooctane 1,4-Dioxane
Nitropropane Diacetone Alcohol
Ethanolamine Acetonitrile
Nitromethane Pyridine
Ethylene Chloride Toluidine
Benzyl Chloride Ethylene Glycol
Propylene Glycol
This test method 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 May 1, 2014March 1, 2022. Published June 2014March 2022. Originally approved in 1995. Last previous edition approved in 20062014 as
D5830 – 95D5830 – 14.(2006). DOI: 10.1520/D5830-14.10.1520/D5830-22.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D5830 − 22
Dichodifluoromethane Tetrahydrofuran
Trichlorofluoromethane Acetone
1,1,2-Trichloro-1,2,2- Methyl Ethyl Ketone
trifluoroethane MIBK
Methanol Cyclohexanone
Ethanol Ethyl Acetate
Isopropanol Propyl Acetate
n-Propanol Butyl Acetate
Isobutanol Benzene
n-Butanol Toluene
tert-Butanol Ethylbenzene
Methylene Chloride Xylenes
Chloroform Styrene
Carbon Tetrachloride Chlorobenzene
1,1-Dichloroethane Dichlorobenzenes
1,2-Dichloroethane Nitrobenzene
1,2-Dichloropropane Fluorobenzene
1,1-Dichloroethylene n-Propyl Benzene
1,2-Dichloroethene Isopropyl Benzene
1,1,1-Trichloroethane Isobutyl Benzene
Tetrachloroethylene n-Butyl Benzene
Trichloroethylene 2-Ethoxyethanol
Tetrachloroethane 2-Butoxyethanol
Cyclopentane 2-Ethoxyethanol Acetate
Pentane 2-Methoxyethanol
Hexane Bromoform
Heptane Carbitol
Cyclohexane Ethyl Ether
Isooctane 1,4-Dioxane
Nitropropane Diacetone Alcohol
Ethanolamine Acetonitrile
Nitromethane Pyridine
Ethylene Chloride Toluidine
Benzyl Chloride Ethylene Glycol
Propylene Glycol
1.1.1 This compound list is a compilation of hazardous solvents and other constituents that are routinelycommonly seen in
hazardous waste samples.
1.2 The scope of this test method may be expanded to include other volatile and semivolatile organic constituents.constituents
such as but not limited to those described below, provided the intended use data quality objectives including sampling, recovery,
and analytic data quality are demonstrated as satisfied by the user.
1.2.1 Hydrocarbon mixtures such as kerosene and mineral spirits.
1.2.2 High-boiling organics, defined here as compounds which boil above n-Hexadecane.
1.2.3 Other organics that the analyst is able to identify, either through retention time data or gas chromatography/mass
spectrometric (GC/MS) analysis.
1.3 Gas chromatographic methods are recommended for use only by, or under close supervision of, an experienced analyst.
1.3 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.
1.4 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
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.
D5830 − 22
D4547 Guide for Sampling Waste and Soils for Volatile Organic Compounds
D4687 Guide for General Planning of Waste Sampling
D5013 Practices for Sampling Wastes from Pipes and Other Point Discharges
D5681 Terminology for Waste and Waste Management
D5743 Practice for Sampling Single or Multilayered Liquids, with or Without Solids, in Drums or Similar Containers
2.2 EPA Document:Documents:
Test Method 8000D Determinative Chromatographic Separations, SW-846, Revision 5, 2018
Test Method 8015D Nonhalogenated Organics Using GC/FID, SW-846, Revision 4, 2003
Test Method 8021B Aromatic and Halogenated Volatiles By Gas Chromatography Using Photoionization and/or Electrolytic
Conductivity Detectors, SW-846, Revision 3, 2014
Gas Chromatography/Mass Spectrometry Method 8260,Test Method 8260D Test Methods for Evaluating Solid Waste
Physical/Chemical Methods, SW-846, Third Edition, Final Update 1, July 1992Volatile Organic Compounds by Gas
Chromatography/Mass Spectrometry (GC/MS), SW-846, Revision 4, 2018
3. Terminology
3.1 Definitions—For definitions of terms used in this standard, refer to Terminology D5681.
4. Summary of Test Method
4.1 Waste samples are analyzed by direct injection, or by carbon disulfide, M-Pyrol, or other suitable solvent extraction and
injection of the extract into a gas chromatograph. Detection is achieved using a detector which is specific for the needed
application, for example, flame ionization detector (FID), electron capture detector (ECD), thermal conductivity detector (TCD),
photoionization detector (PID), or mass selective detector (MSD). This test method may be expanded to utilize other detector types
not previously mentioned.
5. Significance and Use
5.1 This test method is useful in identifying the majorcommon solvent constituents in hazardous waste samples. This test method
is designed to support field or site assessments, recycling operations, plant operations, or pollution control programs.
6. Interferences
6.1 Interferences may be encountered from any number of organic compounds that respond in the detector. to which a specific
detector responds. Also, closely eluting components may complicate identification based solely on retention time. When these
types of interferences are encountered, the analyst must rely on other sources of information for positive identification, such as:
6.1.1 Gas chromatography/mass spectrometric (GC/MS) confirmation, GC/MS confirmation; see EPA Method 8260,
Method 8260D, direct injection technique; technique.
6.1.2 Gas chromatography with an analyte class selective detector such as PID or electrolytic conductivity (ELCD) detectors or
both; see EPA Method 8021B.
6.1.3 Use of confirmation column, or confirmatory detector; detector.
6.1.3.1 This method identifies one column (DB1701)(DB-1701) and one detector (FID) and utilizes three solvent standards and
one QC daily check. Use of confirmatory columns or detectors, or both, will also require the use of the three solvent standards (see
Note 2, 8.19.1) and QC daily check, one for each confirmatory column or detector, or both. EPA Method 8000D provides useful
guidance on calibration and QC requirements applicable to this activity.
6.1.4 Use of varying temperature programs or standard comparison, or both;both.
6.1.4.1 Use of varying analytical programs will also require the use of three solvent standards and QC daily check for each
variation.
Available from the Superintendent of Documents, U.S. Government Printing Office, Washington, DC 20402.United States Environmental Protection Agency (EPA),
William Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460, http://www.epa.gov.
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FIG. 1 Daily QC Standard FID/DB-1701
6.1.5 Sample history, for example, any information available from the waste generator; and,generator.
6.1.6 Physical characteristics, for example, flammability, specific gravity, or miscibility with water.
6.2 Interferences may also be encountered from syringe carryover. Immediately following each injection, the syringe should be
is thoroughly rinsed with carbon disulfide,disulfide or M-Pyrol. Other solvents such as methanol may be used as rinse solvents if
sample types necessitate their use, but be aware that carryover and possible interferences may occur if the rinse solvent is not
completely cleaned from still present in the syringe beforeat reuse. Before each injection the syringe must be thoroughly is rinsed
with the sample to be injected, where the first two pumps are flushed into a separate waste receptacle.
6.3 When carbon disulfide (CS ) is used to extract solids or sludges that contain significant amounts of water, low recovery of the
water miscible water-miscible solvents may result.
6.4 Some grades of CS may contain trace amounts of benzene.
6.5 M-Pyrol seems to degrade slowly degrades with time. The low-level degradation products interfere with some late eluting
compounds on some columns (approximately five small peaks).
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6.6 Interference from the CS solvent peak may occur if using a TCD.
6.7 When using a TCD, be aware that water, water as well as oxygenated compounds, for example,compounds such as MEK,
MIBK, or both, may suppress detector response.
6.8 If an electrolytic conductivity detector (ELCD) or electron capture detector (ECD) must be used, be aware that ELCD or ECD
is used, CS , M-Pyrol (required for an ELCD), and high concentrations of halogenated compounds may overload and possibly
damage boththese detectors. It is recommended that these detectors be used only when very low detection levels of halogenated
compounds are expected and direct injection of the sample is possible.
7. Apparatus
7.1 Gas Chromatograph System—Equipped with capillary or packed column injection ports, or both, detector, and data system.
7.2 RecommendedSuggested Chromatographic Columns:
7.2.1 Capillary; Microbore or Megabore. Capillary, microbore or megabore.
7.2.1.1 DB-1701, 30M × 0.25-mm30M by 0.25 mm inside diameter, 0.25-μm0.25 μm film thickness.
7.2.1.2 DB-624, 30M × 0.3-mm 30M by 0.3 mm inside diameter, 1.8-μm 1.8 μm film thickness.
7.2.2 Packed: Stainless Steel or Glass.
7.2.2.1 1 % SP-1000, 60/80 Carbopak B, 8-ft 8 ft by ⁄8-in. in. inside diameter.
7.2.2.2 10 % SP-2100, 100/120 Chromosorb WHP, 2M × 2 mm 2M by 2 mm ID.
NOTE 1—These columns are recommended and have shown to give good results. as they have demonstrated acceptable results in many applications.
Operating conditions for each isare listed in Section 1011. Equivalent or alternative columns, or both, columns may be used depending on when they are
demonstrated as fulfilling the needs of a particular application.
7.3 Glass Screw-Cap Vials or Equivalent—To collect samples and store standards. Polytetrafluoroethylene or other inert material
should be used for the cap liner.
7.4 Microsyringes, 1.0, 10, and 100 μL.
7.5 Analytical Balance, accurate to 0.0001 g.
7.6 Pipettes, glass, disposable, or volumetric micropipettor or equivalent.
7.7 Microdisk Filters, 0.45, 1.0, or 5.0 μm, optional.
7.8 Centrifuge, optional.
7.9 Vortex-Type Mixer.
8. Reagents and Materials
8.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society, where such
D5830 − 22
specifications are available. Other grades may be used, provided it is first ascertained determined that the reagent is of sufficiently
high purity to permit its use without lessening the accuracy ofretain an acceptable accuracy for the determination.
8.2 Purity of Water—Unless otherwise indicated, references to water shall be understood to mean reagent water as defined by Type
II of Specification D1193.
8.3 Nitrogen or Helium (High Purity)—(UHP)—For carrier and makeup gases. Air and hydrogen (high purity) (UHP) for fuel
gases. Gases may be obtained from a gas generator if available, through purification of a lower grade, or from a high-purity tank
supply.providing gases of sufficient purity, or from commercially available high-purity gas cylinders.
8.4 Carbon Disulfide, CS —Chromatography grade.
8.5 M-Pyrol, C H NO—Available through several chemical suppliers and sources as 1-methyl-2-pyrrolidone.
5 9
8.6 Individual Standards for Each Component of Interest—99 % purity, available from many vendors.
9. Standard Preparation
9.1 Stock Standard Solutions—Stock standards are prepared from pure standard materials. It is recommended that the standards
be prepared so that each component is 5 to 10 % by weight. The stock standards must be prepared by directly weighing each
component. For extremely volatile components,components such as ether and freons, it is recommended that a new stock standard
be prepared daily or as needed. If a dilution solvent is needed when preparing the stock standards, use the same solvent used for
sample extraction or dilution in Section 711.
NOTE 2—Due to the incompatibility of some standard compounds, that is, some compounds are not miscible with each other, and also because of the such
as immiscible substances, or when a large number of compounds typically looked for in a single chromatographic run, are determined, it is advisable to
prepare 3three or 4four standard solutions each composed of 10ten to 15 compounds. A compatible compounds. In addition, a set of standard
chromatograms and a retention timetable should be available for reference.are typically retained as references.
9.2 Secondary Working Standards—These are prepared from stock standard solutions using the appropriate solvent. Secondary
standards should encompass the linear range of the GC system.
NOTE 3—Linear response and range mustshall be established with all detectors and chromatography systems used for quantitation. All calibration and
sample analysis mustshall be done within the established linear range.
9.3 Calibration Check Standard—A calibration check standard should be is prepared. The standard mixture should provide a good
overall check of the GC/detector system. The compounds system with respect to analytic accuracy and precision. These criteria
are established prior to commencing sample analysis and are based upon the data quality needs of the investigation. The
compounds selected should cover the major compound types, for example, alcohols, aromatics, aliphatics, ketones, and
halogenates. A typical calibration check standard flame ionization detector (FID) FID chromatogram is shown in Fig. 1.
10. Sample Collection, Preservation, and Handling
10.1 Sample collect
...