D34.01.06 - Analytical Methods

SIGNIFICANCE AND USE
4.1 The analysis of trace elements is often a regulatory and process-specific requirement for facilities utilizing LHWF. With proper instrument standardization, set-up, and quality control, this test method provides the user an accurate, rapid, nondestructive method for trace element determinations.
SCOPE
1.1 This test method applies to the determination of trace element concentrations by energy-dispersive X-ray fluorescence (EDXRF) spectrometry in typical liquid hazardous waste fuels (LHWF) used by industrial furnaces.  
1.2 This test method has been used successfully on numerous samples of LHWF that are mixtures of solvents, oils, paints, and pigments for the determination of the following elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.  
1.3 This test method also may be applicable to elements not listed above and to the analysis of trace metals in organic liquids other than those used as LHWF.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFAS have been detected in soils, sludges, and surface and drinking waters. Hence, there is a need for a quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure.  
5.3 This method has been used to determine selected PFAS in sand (Table 4) and four ASTM reference soils (Table 5).
SCOPE
1.1 This procedure covers the determination of selected polyfluorinated alkyl substances (PFAS) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFAS in difficult soil matrices. An exhaustive extraction procedure for PFAS, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFAS. The approach from this standard was utilized to screen laboratory coats (textiles) to identify if PFAS would be leached from the materials.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The method of detection limit3 and reporting range4 for the target analytes are listed in Table 1.    
1.3.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for the PFAS after taking into account a 2 g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered, leaving the solid and any residual solvent behind. It is raised above the Level 1 calibration concentration for PFOS, PFHxA, FHEA, and FOEA; these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 The elemental analysis of liquid hazardous waste is often important for regulatory and process-specific requirements. This test method provides the user an accurate, rapid method for trace and major element determinations.
SCOPE
1.1 This test method covers the determination of trace and major element concentrations by energy-dispersive X-ray fluorescence spectrometry (EDXRF) in liquid hazardous waste (LHW).  
1.2 This test method has been used successfully on numerous samples of aqueous and organic-based LHW for the determination of the following elements: Ag, As, Ba, Br, Cd, Cl, Cr, Cu, Fe, Hg, I, K, Ni, P, Pb, S, Sb, Se, Sn, Tl, V, and Zn.  
1.3 This test method is applicable for other elements (Si-U) not listed in 1.2.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 PFAS are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFAS have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. PFAS have been detected in soils, sludges, surface, and drinking waters. This is a quick, easy, and robust method to quantitatively determine these compounds at trace levels in soil/biosolid matrices.  
5.2 This test method has been validated using four ASTM reference soils (CH-1, ML-1, CL-1, and SP-1). ASTM reference soil CH-1 is Fat Clay (CH)—Vicksburg Buckshot Clay; ASTM reference soil ML-1 is silt (ML)—Vicksburg silt; ASTM reference soil CL-1 is lean clay (CL)—Annapolis clay; and ASTM reference soil SP-1 is sand (SP)—Frederick sand and four biosolids (Missouri, California, Idaho, and Georgia). Refer to the Precision and Bias (Section 17).
SCOPE
1.1 This test method covers the determination of per- and polyfluoroalkyl substances (PFAS) in soil/biosolid matrices by solvent extraction, filtering, separation using liquid chromatography (LC), and detection with tandem mass spectrometry (MS/MS). These analytes are extracted from soil/biosolids with basic water and methanol then qualitatively and quantitatively determined by this test method. Quantitation is by selected reaction monitoring (SRM), sometimes referred to as multiple reaction monitoring (MRM).  
1.2 The reporting limit (RL) and reporting range (see Note 2) for the target analytes are listed in Table 1. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 5 for the PFAS after taking into account a 2 g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered, leaving the solid and any residual solvent behind. Sporadic PFAS hits due to PFAS contamination in consumables/collection tools used during sample collection and preparation is possible while executing this standard and must be monitored. All samples should be taken at a minimum as duplicates in order to compare the precision between the two prepared samples to help ensure the concentration/positive result is reliable.
Note 1: This standard only includes the determination of the analytes listed in Table 1 and is only applicable to soil and biosolid matrices; any added compost or soil additives may contain PFAS that may be bound and not able to be determined by this method. Analysis of packaging materials and polymeric PFAS moieties are not amenable to this standard.
Note 2: Injection volume variations and sensitivity of the instrument used will change the reporting limit and ranges.  
1.2.1 Recognizing continual advancements in the sensitivity of instrumentation, advancements in column chromatography, and other processes not recognized here, the reporting limit may be lowered assuming the minimum performance requirements of this test method at the lower concentrations are met.  
1.2.2 Depending on data usage, you may modify this test method but limit to modifications that improve performance while still meeting or exceeding the method quality acceptance criteria. Modifications to the solvents, ratio of solvent to sample, or shortening the chromatographic run simply to save time are not allowed. Use Practice E2935 or similar statistical tests to confirm that modifications produce equivalent results on non-interfering samples. In addition, use Guide E2857 or equivalent statistics to revalidate the modified test.  
1.2.3 Analyte detections under the reporting limit are estimated concentrations. If results are to be reported below the RL using this standard and following the method detection limit procedure in 40 CFR Part 136 Appen...

SIGNIFICANCE AND USE
5.1 The determination of total moisture is important for assessing the fuel quality. Water content will affect the heating value of fuels directly and can contribute to instability in the operation of an industrial furnace or adversely impact performance in other applications. Additionally, high water content can present material handling and storage problems during winter months or in cold environments.
SCOPE
1.1 This test method covers the determination by Karl Fischer (KF) titrimetry of total moisture in solid or liquid hazardous waste fuels used by industrial furnaces.  
1.2 This test method has been used successfully on numerous samples of hazardous waste fuel composed of solvents, spent oils, inks, paints, and pigments. The range of applicability for this test method is between 1.0 and 100 %; however, this evaluation was limited to samples containing approximately 5 to 50 % water.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 The U.S. Environmental Protection Agency Regulations, 40 CFR 266, require that boilers, cement kilns, and other industrial furnaces utilizing waste-derived fuel adhere to specific guidelines in assessing potential metals emissions. A common approach for estimating potential emissions is performing total metals analysis on all feed stream materials. This practice describes a multi-stage microwave-assisted digestion procedure that solubilizes trace elements for spectroscopic analyses.
SCOPE
1.1 This practice describes the multi-stage microwave digestion of typical industrial furnace feed stream materials using nitric, hydrofluoric, hydrochloric, and boric acids for the subsequent determination of trace metals.  
1.2 This practice has been used successfully on samples of coal, coke, cement raw feed materials, and waste-derived fuels composed primarily of waste paint-related material in preparation for measuring the following trace elements: Ag, As, Ba, Be, Cd, Cr, Hg, Pb, Sb, and Tl. This practice may be applicable to elements not listed above.  
1.3 This practice is also effective for other waste materials (for example, fly ash, foundry sand, alum process residue, cement kiln dust, etc.).  
1.4 The values stated in SI units are to be regarded as standard. Other units of measurement in parentheses in this standard are informational.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 8.  
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.

SIGNIFICANCE AND USE
5.1 This test method is useful in identifying the common 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.
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 intended 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-
trifluoroethane  
Methyl Ethyl Ketone
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 commonly seen in hazardous waste samples.  
1.2 The scope of this test method may be expanded to include other volatile and semivolatile organic 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 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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents, or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. TDG is both a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.5  
5.2 This method has been investigated for use with soil.
SCOPE
1.1 This procedure covers the determination of thiodiglycol (TDG) in soil using pressurized fluid extraction (PFE). A commercially available PFE system2 is used, followed by analysis using liquid chromatography (LC), and detected with tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The method detection limit (MDL) and reporting range for TDG are listed in Table 1.  
1.2.1 The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.  
1.2.2 The reporting limit (RL) is calculated from the concentration of the Level 1 calibration standard as shown in Table 4. The RL for this method is 200 ppb. Reporting range concentrations are calculated from Table 4 concentrations assuming a 5 μL injection of the lowest level calibration standard, 5 g sample, and a 2 mL final extract volume.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 A high percentage of insoluble, suspended solid material can create pumping, filtering, or grinding difficulties in the off-loading of bulk shipments of OLHW and can contribute to excessive wear on processing equipment. High solids can also decrease the quality and consistency of commingled solutions by decreasing the effectiveness of agitation in storage tanks. These issues are of concern to the recycling industries (solvents, paints, and other materials handled in significant quantities) in addition to those activities that propose to use the waste as a fuel.
SCOPE
1.1 This test method covers the determination of the approximate amount of insoluble, suspended solid material in organic liquid hazardous waste (OLHW).  
1.2 This test method is intended to be used in approximating the amount of insoluble, suspended solids in determining the material-handling characteristics and fuel quality of OLHW. It is not intended to replace more sophisticated procedures for the determination of total solids.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This is a performance-based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this standard are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 Organophosphate pesticides affect the nervous system by disrupting the enzyme that regulates acetylcholine, a neurotransmitter. They were developed during the early 19th century, but their effects on insects, which were similar to their effects on humans, were discovered in 1932. Some are poisonous and were used as chemical weapon agents. Organophosphate pesticides are usually not persistent in the environment.7,8  
5.3 This test method is for the analysis of selected organophosphorous based pesticide degradation products.  
5.4 This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Diisopropyl Methylphosphonate (DIMP), Ethyl Methylphosphonic Acid (EMPA), Isopropyl Methylphosphonic Acid (IMPA), Methylphosphonic Acid (MPA), and Pinacolyl Methylphosphonic Acid (PMPA), referred to collectively as organophosphonates (OPs) in this test method, in soil. This method is based upon solvent extraction of a soil by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). OPs are qualitatively and quantitatively determined by this method.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The method detection limit2 (MDL), electrospray ionization (ESI) mode, and reporting range3 for the OPs are listed in Table 1.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This is a performance-based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this standard are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC).6 Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents, or have a number of other non-military commercial uses. Schedule 2 chemicals can also be found in applications unrelated to chemical weapons. These chemicals are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. TDG is a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.  
5.3 This method has been investigated for use on surface wipes. TDG is also a human metabolite resulting from sulfur mustard exposure but this method has not been investigated for such determinations.
SCOPE
1.1 This procedure details the determination of thiodiglycol (TDG), also known as 2,2’-thiobis-ethanol, on wipes with 3,3’-thiodipropanol (TDP) as the surrogate. This method is based upon solvent extraction of wipes by either sonication or a pressurized fluid extraction (PFE) technique as an alternative option. The extract is filtered, concentrated, and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). TDG is qualitatively and quantitatively determined.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The method detection limit (MDL)2 and reporting range3 for TDG are listed in Table 1.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This test method developed for the analysis of TPs in soil and sediment samples is based upon an LC/MS/MS analysis. Any type of coupled liquid chromatography/mass spectrometry system may be used that meets the study objectives of the individual project. These may include, but are not limited to: trap, single quadrupoles, time-of-flight, high resolution, and others not mentioned here.  
5.2 The MDL and reporting range for TPs are listed in Table 1. This SOP has been tested on Ottawa sand, four ASTM soil types, biosolid sample, and one commercial soil. The P&A QC acceptance criteria are listed in Table 3. Tables 4-17 display the TC and surrogate recoveries in the various soil types. 40 CFR Part 136, Appendix B was used as a guide to determine the MDLs. The 40 CFR Part 136 MDL criteria were not met for NP2EO; this does not affect the method because the SOP only reports to the RL and is not a regulatory method. All site sample results are not reported below the RL using this method. RLCS concentrations may be reported below the RL because they are spiked at or near the RL. (A) Uncertainty calculation based upon 95 % confidence interval and a two-tailed Student t distribution.
Uncertainty = Student t Value [(standard deviation) / (number of LCS)1/2].            (A) P&A values are after subtraction of average of MB if ≥RL.   (A) P&A values are after subtraction of average of MB if ≥RL.  (A)    
5.3 The RL for a specific soil sample may differ from that listed depending on the nature of the interferences in the sample matrix. Variability in historical LCS spike recovery may be used to estimate uncertainty. The estimate of minimum laboratory contribution to measurement uncertainty of this test method for each analyte is listed in Table 3. These values are derived from P&A samples from the initial IDOC study for this test method. The uncertainty will be greater near the RL and much greater near the DL. Also, uncertainty estimated based on variability in LCS recov...
SCOPE
1.1 This test method covers analysis of nonylphenol (NP), nonylphenol monoethoxylate (NP1EO), nonylphenol diethoxylate (NP2EO), octylphenol (OP), and bisphenol A (BPA), referred to collectively as target phenols (TPs), in soil, sediments, and biosolids by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TPs have an affinity for surfaces and particles that is more pronounced at lower concentrations. The range of applicability of the test method is shown in Table 1. The method may be extended outside of these ranges depending on additional performance studies not undertaken here.  
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.  
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, health, and environmental 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.

SIGNIFICANCE AND USE
5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 TTPC may be used in various industrial and commercial products for use as a biocide. Products containing TTPC have been approved for controlling algal, bacterial, and fungal slimes in industrial water systems.2 TTPC should not be persistent in water but may be deposited in sediments at concentrations of concern. Hence, there is a need for quick, easy, and robust method to determine TTPC concentration at trace levels in various soil matrices for understanding the sources and concentration levels in affected soils and sediments.  
5.3 This method has been used to determine TTPC in sand, a commercial top soil, and four ASTM reference soils (Table 4).
SCOPE
1.1 This procedure covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil matrix by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. TTPC is a biocide that strongly adsorbs to soils.2 The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 250 to 10 000 ng/kg. This analyte is qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The method detection limit (Note 1) (MDL) and reporting range (Note 2) for the target analyte are listed in Table 1.  
Note 1: The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B, as a guide utilizing solvent extraction of soil. Two-gram sample of Ottawa sand was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this standard to be explained here.
Note 2: Reporting range concentration is calculated from Table 2 concentrations assuming a 50-μL injection of the Level 1 calibration standard for TTPC, and the highest level calibration standard with a 20-mL final extract volume of a 2-g soil sample. Volume variations will change the reporting limit and ranges.  
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for TTPC after taking into account a 2-g sample weight and a final extract volume of 20 mL in 75 % acetone/25 % water. The final extract volume is 20 mL because a 15-mL volume of acetone is added to each soil sample and only the liquid layer after extraction is filtered leaving the solid behind followed by the addition of 5 mL of water to the acetone extract.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This practice will identify waste materials that are potentially unstable when they come in contact with other materials at a waste treatment or disposal site.  
5.2 This practice will serve to determine the miscibility of waste materials with various media, including other wastes.  
5.3 This practice may not be applicable to all wastes. The appropriateness of these tests depends upon the proposed management of the waste.  
5.4 Since the initiation of some chemical reactions are slow to take place, the user may wish to establish reagent-to-waste contact times prior to observing the mixes for any reactions.
SCOPE
1.1 This practice is designed to determine whether a waste material reacts when it is mixed with air, water, strong acid, strong base, an oil/solvent mixture, other waste mixtures, or solid media such as a geological formation or solidification agents.  
1.2 The miscibility of the waste material with the above media can also be defined.  
Note 1: The following ASTM standards provide supplemental information: Test Methods D4978, D4980, D4982, D5049, and D5057 and Practices D4979, D4981, and D5058.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This is a performance-based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this test method are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this test method shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.7 BPA has become an important high-volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products, including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings, and many other products.8  
5.3 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency and will biodegrade. BPA has been reported to have adverse effects in aquatic organisms and may be released into environmental waters directly at trace levels through landfill leachate and sewage treatment plant effluents. This method has been investigated for use with soil, sludge, and biosolids.  
5.4 The land application of biosolids has raised concerns over the fate of BPA in the environment, and a standard method is needed to monitor concentrations. This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Bisphenol A (BPA) in soil, sludge, and biosolids. This test method is based upon solvent extraction of a soil matrix by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). BPA is qualitatively and quantitatively determined by this test method.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The method detection limit (MDL),2 electrospray ionization (ESI) mode, and reporting range3 for BPA are listed in Table 1.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This procedure is intended to be used to evaluate the ignitability of liquid wastes.  
5.2 Flash point measures the response of the subsample to heat and an ignition source under controlled laboratory conditions. It is only one of a number of properties that shall be considered in assessing the overall flammability hazard of a liquid waste material.  
5.3 Flash point can indicate the possible presence of highly volatile and flammable materials in a relatively nonvolatile or nonflammable material.  
5.4 This test method uses a small sample volume (2 mL) and short test time (1 min).
SCOPE
1.1 This test method covers the procedure for a flash point test, within the range of –20 to 70 °C, of liquid wastes using a small-scale closed cup tester.
Note 1: Some apparatus are not designed for subambient temperature tests, so the testing range would be between 20 °C and 70 °C.
Note 2: This test method is not applicable for liquid waste that forms a surface film (see Test Method D8175 for Finite Flash Point Determination of Wastes by Pensky-Martens Closed Cup Tester).  
1.2 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in this standard.  
1.3 This standard measures the ignitability properties of liquid wastes (which may be any discarded material), which may include secondary materials, off-specification products, and materials containing free liquids recovered during emergency response actions. Results from this test method may be used as part of a fire risk assessment of the material, but it is the responsibility of the user to perform any additional characterization needed for determination of storage, transport, treatment, or disposal per current regulations.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Warning statements appear throughout. See applicable Safety Data Sheets (SDS) for information about certified reference materials (CRMs) or secondary working standards (SWSs) that may be used in this test method. SDS may also be useful if some components of the waste sample are known.  
1.5 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.

SIGNIFICANCE AND USE
5.1 This procedure is intended to be used to evaluate the ignitability of liquid wastes.  
5.2 Flash point measures the response of the subsample to applied heat and an ignition source under controlled laboratory conditions. It is only one of a number of properties that must be considered in assessing the overall flammability hazard of a liquid waste material.  
5.3 Flash point can indicate the possible presence of highly volatile and flammable materials in a relatively nonvolatile or nonflammable material.
SCOPE
1.1 This test method covers the procedure for a finite flash point test, within the range of 20 to 70 °C, of liquid wastes using a manual or automated Pensky-Martens closed cup tester.  
1.2 This test method contains two procedures and is applicable to liquid waste, liquid phase(s) of multi-phase waste, liquid waste with suspended solids, or liquid waste that tends to form a surface film under test conditions.
Note 1: If the liquid waste is of a viscosity such that the subsample volume will not be uniformly heated under the test conditions even with the increased stir rate of Procedure B, then use the small-scale method (Test Method D8174 for Finite Flash Point Determination of Liquid Wastes by Small-Scale Closed Cup Tester).  
1.3 Procedure A is applicable to non-viscous liquids that are without suspended solids. Procedure B is applicable to viscous liquids, liquids with suspended solids, or liquids that form films.
Note 2: This test method is not applicable for corrosive liquid wastes (see Test Method D8174).  
1.4 Units—The values given in SI units are to be regarded as the 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Warning statements appear throughout. Also see applicable Safety Data Sheets (SDS) for information about certified reference materials (CRMs) or secondary working standards (SWSs) that may be used in the analysis. SDS may also be useful if some components of the waste sample are known.  
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.

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.
SCOPE
1.1 This practice describes the partial digestion of solid waste using nitric acid for the subsequent determination of the total recoverable content of inorganic constituents.  
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 are often not equivalent to total 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-mercury, are not solubilized by this practice.  
1.3 This practice has been divided into two methods, A and B, with Method A utilizing an electric hot plate and Method B utilizing 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
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.

SIGNIFICANCE AND USE
5.1 Elemental species such as Cr, Ni, As, Cd, Hg, and Pb are widely used in many industrial processes. These elements have been identified in many former industrial sites driving the need for a quick, easy method for testing on-site at trace levels in soil and solid waste matrices.  
5.2 This method may be used for quantitative determinations of Cr, Ni, As, Cd, Hg, and Pb in soil matrices and solid waste. Typical test time is 90 seconds to 15 minutes.
SCOPE
1.1 This test method is based upon energy-dispersive X-ray Fluorescence (EDXRF) spectrometry using multiple monochromatic excitation beams for detection and quantification of selected heavy metal elements in soil and related solid waste.  
1.2 This test method is also known as High Definition X-ray Fluorescence (HDXRF) or Multiple Monochromatic Beam EDXRF (MMB-EDXRF).  
1.3 This test method is applicable to various soil matrices for the determination of Cr, Ni, As, Cd, Hg, and Pb in the range of 1 to 5000 mg/kg, as specified in Table 1 and determined by a ruggedness study using representative samples. The limit of detection (LOD) for each element is listed in Table 1. The LOD is estimated by measuring a SiO2 blank sample (see Table X1.1 in Appendix X1).  
1.4 This test method is applicable to other elements: Sb, Cu, Se, Ag, Tl, Zn, Ba, Au, Co, V, Fe, Mn, Mo, K, Rb, Sn, Sr, and Ti.  
1.5 X-ray Nomenclature—This standard names X-ray lines using the Siegbahn convention.2  
1.6 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.7 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
3.1 This test method is intended for the evaluation of the wetting and drying resistance of monolithic, solid, solidified/stabilized wastes under the testing conditions of this test method.  
3.2 This test method may be used for the comparison of wetting and drying resistance of wastes.  
3.3 Data tabulated in Table 1, Table 2, and Table 3 may be used to observe irregularities caused by inhomogeneity of specimens, or comparison of mass loss-cycle relations of different wastes, or both, as well as to measure method-related mass losses such as matrix dissolution.
SCOPE
1.1 This test method covers procedures for determining material losses produced by repeated wetting and drying of solid waste specimens. It also covers the visual observation of the disintegration of solid specimens.  
1.2 This test method intends that the material used in the procedure be physically, chemically, and biologically representative; hence it does not address problems as a result of the inhomogeneity of specimens.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 PFCs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFCs have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFCs have been detected in soils, sludges, and surface and drinking waters. Hence, there is a need for a quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure.  
5.3 This method has been used to determine selected polyfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).
TABLE 4 Single-Laboratory Recovery Data in Ottawa Sand    
Sample  
Measured ng/kg from Ottawa Sand P&A Data (400 ng/kg spike for all PFCs except 2000 ng/kg for PFBA and PFPeA and 8000 ng/kg spike for FHEA, FDEA, and FOEA)  
PFTreA  
PFTriA  
PFDoA  
PFUnA  
PFDA  
PFNA  
PFOA  
PFHpA  
PFHxA  
PFPeA  
PFBA  
Unspiked 1  
Unspiked 2  
P&A 1  
389.6  
394.3  
384.7  
376.7  
362.1  
347.6  
345.8  
232.9  
222.2  
1614.9  
1344.5  
P&A 2  
462.1  
424.6  
397.2  
379.1  
378.4  
376.9  
365.9  
247.9  
229.8  
1710.1  
1388  
P&A 3  
402.7  
387.7  
383.1  
365.9  
374.7  
363.3  
347.1  
242.4  
222.9  
1658.9  
1376  
P&A 4  
403.9  
397.1  
395.4  
381.5  
379  
359.4  
342.7  
246.8  
225.8  
1693.6  
1401.9  
P&A 5  
467.2  
445.8  
412.6  
388.5  
376.8  
370.3  
369.7  
249.3  
231.4  
1716.5  
1433.4  
P&A 6  
392.1  
385.3  
374.2  
370.9  
353.2  
351.7  
340.3  
236.7  
220.5  
1659  
1366.4  
Mean R...
SCOPE
1.1 This procedure covers the determination of selected polyfluorinated compounds (PFCs) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFCs in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFCs.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The Method of Detection Limit3 and Reporting Range4 for the target analytes are listed in Table 1.
TABLE 1 Method Detection Limit and Reporting RangeA    
Analyte  
MDL
(ng/kg)  
Reporting Limit
(ng/kg)  
PFTreA  
6.76  
25–1000  
PFTriA  
5.26  
25–1000  
PFDoA  
3.56  
25–1000  
PFUnA  
2.45  
25–1000  
PFDA  
5.54  
25–1000  
PFOS  
18.83  
50–1000  
PFNA  
2.82  
25–1000  
PFecHS  
2.41  
25–1000  
PFOA  
6.24  
25–1000  
PFHxS  
7.75  
25–1000  
PFHpA  
5.80  
25–1000  
PFHxA  
15.44  
50–1000  
PFBS  
6.49  
25–1000  
PFPeA  
20.93  
125–5000  
PFBA  
22.01  
125–5000  
FHEA  
199.04  
600–20 000  
FOEA  
258.37  
750–20 000  
FDEA  
137.46  
500–20 000  
FOUEA  
4.85  
25–1000  
FhpPa  
5.09  
25–1000  
FHUEA  
3.50  
25–1000(A) Abbreviations are defined in 3.2.  
TABLE 2 Concentrations of Calibration Standards (ng/L)    
Analyte/Surrogate  
LV1  
LV2  
LV3  
LV4  
LV5  
LV6  
LV7  
LV8  
LV9  
PFPeA, PFBA  
25  
50  
100  
200  
300  
400  
500  
750  
1000  ...

SIGNIFICANCE AND USE
5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 PFCs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFCs have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFCs have been detected in soils, sludges, and surface and drinking waters. Hence, there is a need for a quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure.  
5.3 This method has been used to determine selected polyfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).
SCOPE
1.1 This procedure covers the determination of selected polyfluorinated compounds (PFCs) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFCs in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances, such as published by Washington et al.,2 for difficult matrices should be considered when analyzing PFCs.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The Method of Detection Limit3 and Reporting Range4 for the target analytes are listed in Table 1. (A) Abbreviations are defined in 3.2.    
1.3.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for the polyfluorinated compounds after taking into account a 2-g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered, leaving the solid and any residual solvent behind. It is raised above the Level 1 calibration concentration for PFOS, PFHxA, FHEA, and FOEA; these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.  
1.5 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.

SIGNIFICANCE AND USE
4.1 The elemental analysis of liquid hazardous waste is often important for regulatory and process specific requirements. This test method provides the user an accurate, rapid method for trace and major element determinations.
SCOPE
1.1 This test method covers the determination of trace and major element concentrations by energy-dispersive X-ray fluorescence spectrometry (EDXRF) in liquid hazardous waste (LHW).  
1.2 This test method has been used successfully on numerous samples of aqueous and organic-based LHW for the determination of the following elements: Ag, As, Ba, Br, Cd, Cl, Cr, Cu, Fe, Hg, I, K, Ni, P, Pb, S, Sb, Se, Sn, Tl, V, and Zn.  
1.3 This test method is applicable for other elements (Si-U) not listed in 1.2.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC). Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents or have a number of other commercial uses. They are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. Schedule 2 chemicals can be found in applications unrelated to chemical weapons. TDG is both a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.5  
5.2 This method has been investigated for use with soil.
SCOPE
1.1 This procedure covers the determination of thiodiglycol (TDG) in soil using pressurized fluid extraction (PFE). A commercially available PFE system2 was used, followed by analysis using liquid chromatography (LC), and detected with tandem mass spectrometry (MS/MS). TDG is qualitatively and quantitatively determined by this method. This method adheres to single reaction monitoring (SRM) mass spectrometry.  
1.2 The Method Detection Limit (MDL) and Reporting Range for TDG are listed in Table 1.  
1.2.1 The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B.  
1.2.2 The reporting limit (RL) is calculated from the concentration of the Level 1 calibration standard as shown in Table 4. The RL for this method is 200 ppb. Reporting range concentrations are calculated from Table 4 concentrations assuming a 5 μL injection of the lowest level calibration standard, 5 g sample, and a 2 mL final extract volume.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 This is a performance based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this standard are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this Standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 Organophosphate pesticides affect the nervous system by disrupting the enzyme that regulates acetylcholine, a neurotransmitter. They were developed during the early 19th century, but their effects on insects, which were similar to their effects on humans, were discovered in 1932. Some are poisonous and were used as chemical weapon agents. Organophosphate pesticides are usually not persistent in the environment.7,8  
5.3 This test method is for the analysis of selected organophosphorous based pesticide degradation products.  
5.4 This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Diisopropyl Methylphosphonate (DIMP), Ethyl Methylphosphonic Acid (EMPA), Isopropyl Methylphosphonic Acid (IMPA), Methylphosphonic Acid (MPA) and Pinacolyl Methylphosphonic Acid (PMPA), referred to collectively as organophosphonates (OPs) in this test method, in soil. This method is based upon solvent extraction of a soil by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). OPs are qualitatively and quantitatively determined by this method.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The Method Detection Limit2 (MDL), electrospray ionization (ESI) mode and Reporting Range3 for the OPs are listed in Table 1.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 This is a performance based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries changes to the analysis described in this standard are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this Standard shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 TDG is a Schedule 2 compound under the Chemical Weapons Convention (CWC).6 Schedule 2 chemicals include those that are precursors to chemical weapons, chemical weapons agents or have a number of other non-military commercial uses. Schedule 2 chemicals can also be found in applications unrelated to chemical weapons. These chemicals are used as ingredients to produce insecticides, herbicides, lubricants, and some pharmaceutical products. TDG is a mustard gas precursor and a degradant as well as an ingredient in water-based inks, ballpoint pen inks, dyes, and some pesticides.  
5.3 This method has been investigated for use on surface wipes. TDG is also a human metabolite resulting from sulfur mustard exposure but this method has not been investigated for such determinations.
SCOPE
1.1 This procedure details the determination of thiodiglycol (TDG), also known as 2,2’-thiobis-ethanol, on wipes with 3,3’-thiodipropanol (TDP) as the surrogate. This method is based upon solvent extraction of wipes by either sonication or a pressurized fluid extraction (PFE) technique as an alternative option. The extract is filtered, concentrated and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). TDG is qualitatively and quantitatively determined.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The Method Detection Limit (MDL)2 and Reporting Range3 for TDG are listed in Table 1.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. (A) Chemical Abstract Service (CAS), A division of the American Chemical Society, 2540 Olentangy River Road, Columbus, OH, 43202, USA.

SIGNIFICANCE AND USE
4.1 A high percentage of insoluble, suspended solid material can create pumping, filtering, or grinding difficulties in the off-loading of bulk shipments of OLHW and can contribute to excessive wear on processing equipment. High solids can also decrease the quality and consistency of commingled solutions by decreasing the effectiveness of agitation in storage tanks. These issues are of concern to the recycling industries (solvents, paints, and other materials handled in significant quantities) in addition to those activities that propose to use the waste as a fuel.
SCOPE
1.1 This test method covers the determination of the approximate amount of insoluble, suspended solid material in organic liquid hazardous waste (OLHW).  
1.2 This test method is intended to be used in approximating the amount of insoluble, suspended solids in determining the material handling characteristics and fuel quality of OLHW. It is not intended to replace more sophisticated procedures for the determination of total solids.  
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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 This test method has been developed by the US EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 TTPC may be used in various industrial and commercial products for use as a biocide. Products containing TTPC have been approved for controlling algal, bacterial, and fungal slimes in industrial water systems.2 TTPC should not be persistent in water but may be deposited in sediments at concentrations of concern. Hence, there is a need for quick, easy, and robust method to determine TTPC concentration at trace levels in various soil matrices for understanding the sources and concentration levels in affected soils and sediments.  
5.3 This method has been used to determine TTPC in sand, a commercial top soil and four ASTM reference soils (Table 4).
SCOPE
1.1 This procedure covers the determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil matrix by extraction with acetone, filtration, dilution with water, and analysis by liquid chromatography/tandem mass spectrometry. TTPC is a biocide that strongly adsorbs to soils.2 The sample extracts are prepared in a solution of 75 % acetone and 25 % water because TTPC has an affinity for surfaces and particles. The reporting range for this method is from 250 to 10 000 ng/kg. This analyte is qualitatively and quantitatively determine by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry.  
1.2 The Method Detection Limit (Note 1) (MDL) and Reporting Range (Note 2) for the target analyte are listed in Table 1.  (A) Acronyms are defined in 3.3.  
Note 1: The MDL is determined following the Code of Federal Regulations, 40 CFR Part 136, Appendix B, as a guide utilizing solvent extraction of soil. Two-gram sample of Ottawa Sand was utilized. A detailed process determining the MDL is explained in the reference and is beyond the scope of this standard to be explained here.
Note 2: Reporting range concentration is calculated from Table 2 concentrations assuming a 50 μL injection of the Level 1 calibration standard for TTPC, and the highest level calibration standard with a 20 mL final extract volume of a 2 g soil sample. Volume variations will change the reporting limit and ranges.  
1.2.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. The reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for TTPC after taking into account a 2 g sample weight and a final extract volume of 20 mL in 75 % acetone/25 % water. The final extract volume is 20 mL because a 15 mL volume of acetone is added to each soil sample and only the liquid layer after extraction is filtered leaving the solid behind followed by the addition of 5 mL of water to the acetone extract.  
1.3 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
4.1 The U.S. Environmental Protection Agency Regulations, 40 CFR 266 , require that boilers, cement kilns, and other industrial furnaces utilizing waste-derived fuel adhere to specific guidelines in assessing potential metals emissions. A common approach for estimating potential emissions is performing total metals analysis on all feed stream materials. This practice describes a multi-stage microwave-assisted digestion procedure that solubilizes trace elements for spectroscopic analyses.
SCOPE
1.1 This practice describes the multi-stage microwave digestion of typical industrial furnace feed stream materials using nitric, hydrofluoric, hydrochloric, and boric acids for the subsequent determination of trace metals.  
1.2 This practice has been used successfully on samples of coal, coke, cement raw feed materials, and waste-derived fuels composed primarily of waste paint-related material in preparation for measuring the following trace elements: Ag, As, Ba, Be, Cd, Cr, Hg, Pb, Sb, and Tl. This practice may be applicable to elements not listed above.  
1.3 This practice is also effective for other waste materials (for example, flyash, foundry sand, alum process residue, cement kiln dust, etc.).  
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.

SIGNIFICANCE AND USE
4.1 The determination of total moisture is important for assessing the quality of fuels. Water content will affect the heating value of fuels directly and can contribute to instability in the operation of an industrial furnace. Additionally, high water contents can present material handling and storage problems during winter months or in cold environments.
SCOPE
1.1 This test method covers the determination by Karl Fischer (KF) titrimetry of total moisture in solid or liquid hazardous waste fuels used by industrial furnaces.  
1.2 This test method has been used successfully on numerous samples of hazardous waste fuel composed of solvents, spent oils, inks, paints, and pigments. The range of applicability for this test method is between 1.0 and 100 %; however, this evaluation was limited to samples containing approximately 5 to 50 % water.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
4.1 The analysis of trace elements is often a regulatory and process specific requirement for facilities utilizing LHWF. With proper instrument standardization, set-up, and quality control, this test method provides the user an accurate, rapid, nondestructive method for trace element determinations.
SCOPE
1.1 This test method applies to the determination of trace element concentrations by energy-dispersive X-ray fluorescence (EDXRF) spectrometry in typical liquid hazardous waste fuels (LHWF) used by industrial furnaces.  
1.2 This test method has been used successfully on numerous samples of LHWF that are mixtures of solvents, oils, paints, and pigments for the determination of the following elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.  
1.3 This test method also may be applicable to elements not listed above and to the analysis of trace metals in organic liquids other than those used as LHWF.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
The analysis of trace elements is often a regulatory and process specific requirement for facilities utilizing LHWF. With proper instrument standardization, set-up, and quality control, this test method provides the user an accurate, rapid, nondestructive method for trace element determinations.
SCOPE
1.1 This test method applies to the determination of trace element concentrations by energy-dispersive X-ray fluorescence (EDXRF) spectrometry in typical liquid hazardous waste fuels (LHWF) used by industrial furnaces.
1.2 This test method has been used successfully on numerous samples of LHWF that are mixtures of solvents, oils, paints, and pigments for the determination of the following elements: Ag, As, Ba, Cd, Cr, Hg, Ni, Pb, Sb, Se, and Tl.
1.3 This test method also may be applicable to elements not listed above and to the analysis of trace metals in organic liquids other than those used as LHWF.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.
WITHDRAWN RATIONALE
This test method applied to the determination of trace element concentrations by energy-dispersive X-ray fluorescence (EDXRF) spectrometry in typical liquid hazardous waste fuels (LHWF) used by industrial furnaces.
Formerly under the jurisdiction of Committee D34 on Waste Management, this test method was withdrawn in January 2015 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

SIGNIFICANCE AND USE
5.1 This test method has been developed by the US EPA Region 5 Chicago Regional Laboratory (CRL).  
5.2 PFCs are widely used in various industrial and commercial products; they are persistent, bio-accumulative, and ubiquitous in the environment. PFCs have been reported to exhibit developmental toxicity, hepatotoxicity, immunotoxicity, and hormone disturbance. A draft Toxicological Profile for Perfluoroalkyls from the U.S. Department of Health and Human Services is available.7 PFCs have been detected in soils, sludges, surface and drinking waters. Hence, there is a need for quick, easy, and robust method to determine these compounds at trace levels in various soil matrices for understanding of the sources and pathways of exposure.  
5.3 This method has been used to determine selected perfluorinated compounds in sand (Table 4) and four ASTM reference soils (Table 5).
SCOPE
1.1 This procedure covers the determination of selected perfluorinated compounds (PFCs) in a soil matrix using solvent extraction, filtration, followed by liquid chromatography (LC) and detection with tandem mass spectrometry (MS/MS). These analytes are qualitatively and quantitatively determined by this method. This method adheres to multiple reaction monitoring (MRM) mass spectrometry. This procedure utilizes a quick extraction and is not intended to generate an exhaustive accounting of the content of PFCs in difficult soil matrices. An exhaustive extraction procedure for polyfluoralkyl substances, such as published by Washington et al.2, for difficult matrices should be considered when analyzing PFCs.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The Method of Detection Limit3 and Reporting Range4 for the target analytes are listed in Table 1. (A) Abbreviations are defined in 3.2.    
1.3.1 The reporting limit in this test method is the minimum value below which data are documented as non-detects. Analyte detections between the method detection limit and the reporting limit are estimated concentrations and are not reported following this test method. In most cases, the reporting limit is calculated from the concentration of the Level 1 calibration standard as shown in Table 2 for the perfluorinated compounds after taking into account a 2 g sample weight and a final extract volume of 10 mL, 50 % water/50 % MeOH with 0.1 % acetic acid. The final extract volume is assumed to be 10 mL because 10 mL of 50 % water/50 % MeOH with 0.1 % acetic acid was added to each soil sample and only the liquid layer after extraction is filtered leaving the solid and any residual solvent behind. It is raised above the Level 1 calibration concentration for PFOS, PFHxA, FHEA, and FOEA, these compounds can be identified at the Level 1 concentration but the standard deviation among replicates at this lower spike level resulted in a higher reporting limit.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
4.1 This test method is useful in identifying the major 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.
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 designed 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-
trifluoroethane  
Methyl Ethyl Ketone
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 routinely seen in hazardous waste samples.  
1.2 The scope of this test method may be expanded to include other volatile and semivolatile organic constituents.  
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.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
5.1 This test method will identify waste materials that are potentially unstable when they come in contact with other materials at a waste treatment or disposal site.  
5.2 This test method will serve to determine the miscibility of waste materials with various media, including other wastes.  
5.3 This test method may not be applicable to all wastes. The appropriateness of these tests depends upon the proposed management of the waste.  
5.4 Since the initiation of some chemical reactions are slow to take place, the user may wish to establish reagent-to-waste contact times prior to observing the mixes for any reactions.
SCOPE
1.1 This test method is designed to determine whether a waste material reacts when it is mixed with air, water, strong acid, strong base, an oil/solvent mixture, other waste mixtures, or solid media such as a geological formation or solidification agents.  
1.2 The miscibility of the waste material with the above media can also be defined. Note 1—The following ASTM standards provide supplemental information: Test Methods D4978, D4979, D4980, D4981, D4982, D5049, D5057, and D5058.  
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 8.

SIGNIFICANCE AND USE
5.1 This is a performance based method, and modifications are allowed to improve performance.  
5.1.1 Due to the rapid development of newer instrumentation and column chemistries, changes to the analysis described in this test method are allowed as long as better or equivalent performance data result. Any modifications shall be documented and performance data generated. The user of the data generated by this test method shall be made aware of these changes and given the performance data demonstrating better or equivalent performance.  
5.2 The first reported synthesis of BPA was by the reaction of phenol with acetone by Zincke.7 BPA has become an important high volume industrial chemical used in the manufacture of polycarbonate plastic and epoxy resins. Polycarbonate plastic and resins are used in numerous products including electrical and electronic equipment, automobiles, sports and safety equipment, reusable food and drink containers, electrical laminates for printed circuit boards, composites, paints, adhesives, dental sealants, protective coatings and many other products.8  
5.3 The environmental source of BPA is predominantly from the decomposition of polycarbonate plastics and resins. BPA is not classified as bio-accumulative by the U.S. Environmental Protection Agency and will biodegrade. BPA has been reported to have adverse effects in aquatic organisms and may be released into environmental waters directly at trace levels through landfill leachate and sewage treatment plant effluents. This method has been investigated for use with soil, sludge, and biosolids.  
5.4 The land application of biosolids has raised concerns over the fate of BPA in the environment and a standard method is needed to monitor concentrations. This method has been investigated for use with various soils.
SCOPE
1.1 This procedure covers the determination of Bisphenol A (BPA) in soil, sludge, and biosolids. This test method is based upon solvent extraction of a soil matrix by pressurized fluid extraction (PFE). The extract is filtered and analyzed by liquid chromatography/tandem mass spectrometry (LC/MS/MS). BPA is qualitatively and quantitatively determined by this test method.  
1.2 Units—The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 The Method Detection Limit2 (MDL), electrospray ionization (ESI) mode, and Reporting Range3 for BPA are listed in Table 1.TABLE 1 Method Detection Limit and Reporting Range    
Analyte  
ESI Mode  
MDL (PPB)  
Reporting Range (PPB)  
Bisphenol A  
Negative  
2.8  
10-250
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method is intended for the evaluation of the wetting and drying resistance of monolithic, solid, solidified/stabilized wastes under the testing conditions of this test method.
This test method may be used for the comparison of wetting and drying resistance of wastes.
Data tabulated in Table 1, Table 2, and Table 3 may be used to observe irregularities caused by inhomogeneity of specimens and/or comparison of mass loss-cycle relations of different wastes, as well as to measure method-related mass losses such as matrix dissolution.
SCOPE
1.1 This test method covers procedures for determining material losses produced by repeated wetting and drying of solid waste specimens. It also covers the visual observation of the disintegration of solid specimens.
1.2 This test method intends that the material used in the procedure be physically, chemically, and biologically representative; hence it does not address problems as a result of the inhomogeneity of specimens.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
The U.S. Environmental Protection Agency Regulations, 40 CFR 266 , require that boilers, cement kilns, and other industrial furnaces utilizing waste-derived fuel adhere to specific guidelines in assessing potential metals emissions. A common approach for estimating potential emissions is performing total metals analysis on all feedstream materials. This practice describes a multi-stage microwave-assisted digestion procedure that solubilizes trace elements for spectroscopic analyses.
SCOPE
1.1 This practice describes the multi-stage microwave digestion of typical industrial furnace feedstream materials using nitric, hydrofluoric, hydrochloric, and boric acids for the subsequent determination of trace metals.
1.2 This practice has been used successfully on samples of coal, coke, cement raw feed materials, and waste-derived fuels composed primarily of waste paint-related material in preparation for measuring the following trace elements: Ag, As, Ba, Be, Cd, Cr, Hg, Pb, Sb, and Tl. This practice may be applicable to elements not previously listed.
1.3 This practice is also effective for other waste materials (for example, flyash, foundry sand, alum process residue, cement kiln dust, etc.).
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 7.

SIGNIFICANCE AND USE
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 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.
SCOPE
1.1 This practice describes the digestion of solid waste using nitric acid for the subsequent determination of inorganic constituents by plasma emission spectroscopy or atomic absorption spectroscopy.
1.2 The following elements may be solubilized by this practice:
  aluminummanganese  berylliummercury  cadmiumnickel  chromiumphosphorus  coppervanadium  ironzinc  lead
1.3 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 equivalent to total elements, depending on the element sought and 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-mercury are not solubilized by this practice.  
1.4 This practice has been divided into two methods, A and B, to account for the advent of digestion blocks. Method A utilizes an electric hot plate; Method B utilizes an electric digestion block.
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.6 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 7.

SIGNIFICANCE AND USE
The determination of total moisture is important for assessing the quality of fuels. Water content will affect the heating value of fuels directly and can contribute to instability in the operation of an industrial furnace. Additionally, high water contents can present material handling and storage problems during winter months or in cold environments.
SCOPE
1.1 This test method covers the determination by Karl Fischer (KF) titrimetry of total moisture in solid or liquid hazardous waste fuels used by industrial furnaces.
1.2 This test method has been used successfully on numerous samples of hazardous waste fuel composed of solvents, spent oils, paints, and pigments. The expected range of applicability for this test method is between 1.0 and 100 %; however, this evaluation was limited to samples containing approximately 5 to 50 % water.
1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
A high percentage of insoluble, suspended solid material can create pumping, filtering, or grinding difficulties in the off-loading of bulk shipments of OLHW and can contribute to excessive wear on processing equipment. High solids can also decrease the quality and consistency of commingled solutions by decreasing the effectiveness of agitation in storage tanks. These issues are of concern to the recycling industries (solvents, paints, and other materials handled in significant quantities) in addition to those activities that propose to use the waste as a fuel.
SCOPE
1.1 This test method covers the determination of the approximate amount of insoluble, suspended solid material in organic liquid hazardous waste (OLHW).
1.2 This test method is intended to be used in approximating the amount of insoluble, suspended solids in determining the material handling characteristics and fuel quality of OLHW. It is not intended to replace more sophisticated procedures for the determination of total solids.
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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
Waste composition information has widespread applications and can be used for activities such as solid waste planning, designing waste management facilities, and establishing a reference waste composition for use as a baseline standard in both facility contracts and acceptance test plans.
The method can be used to define and report the composition of MSW through the selection and manual sorting of waste samples. Where applicable, care should be taken to consider the source and seasonal variation of waste.
After performing a waste composition analysis, laboratory analyses may be performed on representative samples of waste components, or mixtures of waste components, for purposes related to the planning, management, design, testing, and operation of resource recovery facilities.
SCOPE
1.1 This test method describes procedures for measuring the composition of unprocessed municipal solid waste (MSW) by employing manual sorting. This test method applies to determination of the mean composition of MSW based on the collection and manual sorting of a number of samples of waste over a selected time period covering a minimum of one week.
1.2 This test method includes procedures for the collection of a representative sorting sample of unprocessed waste, manual sorting of the waste into individual waste components, data reduction, and reporting of the results.
1.3 This test method may be applied at landfill sites, waste processing and conversion facilities, and transfer stations.
1.4 The values stated in inch-pound units are to be regarded as the standard. The values given in parentheses are for information only.
1.5 This standard does not purport to address all of the safety problems, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 6.

SIGNIFICANCE AND USE
This test method will identify waste materials that are potentially unstable when they come in contact with other materials at a waste treatment or disposal site.
This test method will serve to determine the miscibility of waste materials with various media, including other wastes.
This test method may not be applicable to all wastes. The appropriateness of these tests depends upon the proposed management of the waste.
Since the initiation of some chemical reactions are slow to take place, the user may wish to establish reagent-to-waste contact times prior to observing the mixes for any reactions.
SCOPE
1.1 This test method is designed to determine whether a waste material reacts when it is mixed with air, water, strong acid, strong base, an oil/solvent mixture, other waste mixtures, or solid media such as a geological formation or solidification agents.
1.2 The miscibility of the waste material with the above media can also be defined.
Note 1—The following ASTM standards provide supplemental information: Test Methods D 4978, D 4979, D 4980, D 4981, D 4982, D 5049, D 5057, and D 5058.  
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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 7.

SIGNIFICANCE AND USE
The elemental analysis of liquid hazardous waste is often important for regulatory and process specific requirements. This test method provides the user an accurate, rapid method for trace and major element determinations.
SCOPE
1.1 This test method covers the determination of trace and major element concentrations by energy-dispersive X-ray fluorescence spectrometry (EDXRF) in liquid hazardous waste (LHW).
1.2 This test method has been used successfully on numerous samples of aqueous and organic-based LHW for the determination of the following elements: Ag, As, Ba, Br, Cd, Cl, Cr, Cu, Fe, Hg, I, K, Ni, P, Pb, S, Sb, Se, Sn, Tl, V, and Zn.
1.3 This test method is applicable for other elements (Si-U) not listed in 1.2.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
Extraction of organic pollutants from wastes can provide information on the susceptibility of compounds to leeching, water quality changes, or other site conditions.
Rapid heating, in combination with temperatures in excess of the atmospheric boiling point of organic solvents, reduces sample extraction times.
Small amounts of solvents (30 mL) are used resulting in reduced sample preparation cost and time.
SCOPE
1.1 This practice describes the closed vessel microwave extraction of soils, sediments, sludges, and wastes for subsequent determination of solvent extractable semivolatile and nonvolatile organic compounds by such techniques as gas chromatography and gas chromatography-mass spectrometry.
1.1.1 Compounds listed in Tables 1-5 can be extracted from the preceding materials.
1.2 This test method is applicable to samples that will pass through a 10-mesh (approximately 2-mm opening) screen.
1.3 The detection limit and linear concentration range for each compound is dependent on the gas chromatograph or gas chromatograph-mass spectrometer technique employed and may be found in the manual accompanying the instrument used.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. See Section for specific hazard statements.

SIGNIFICANCE AND USE
The TSEC provides a quantitative measure of the total solvent extractable organic content of the solid waste in question. Based upon the TSEC, the extract may be analyzed or further processed (that is, further cleanup or solvent concentration) in preparation for analysis. Thus, the TSEC provides a quantitative measure for optimizing the extractable organic concentration prior to chemical analysis.
The TSEC of soil or waste material may be used as a quantitative measure for the screening and selection of samples for chemical analysis.
The TSEC may be useful as a simple and relatively inexpensive quantitative indicator of changes occurring in the total extractable organic content of soil or waste materials.
The detection limit of the TSEC depends upon the specific procedures employed. Typical detection limits in solvent extracts (that is, without solvent pre-concentration) for Method A are more than 1000 μg/g. For Method B typical detection limits are 20 to 100 μg/g in the solvent extract. For Method C the typical detection limits are 3 to 20 μg/g for solutes in the solvent extract.
The sensitivity of the methods can be adjusted by varying the volume of solvent extract prior to gravimetric residue determination.
SCOPE
1.1 These test methods describe standard procedures for gravimetrically determining the total nonvolatile and semi-volatile organic content of solvent extracts from soils or solid wastes. The following methods are included: SectionMethod A-Micro-Determination of TSECMethod B-Evaporating Dish ProcedureMethod C-Boiling Flask Procedure
1.2 These methods are used after a solvent extract is obtained from a soil or solid waste. For these methods to be applicable, the extraction solvent must have a boiling point less than that of water at ambient pressure.
1.3 The total solvent extractable content (TSEC) of a soil, sediment, sludge, or solid waste depends upon the solvent and method used for the extraction procedure.

SIGNIFICANCE AND USE
This test method is useful in identifying the major 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.
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 designed for use as a screening method with a typical reporting level of 0.1 %.
1.1.1 This compound list is a compilation of hazardous solvents and other constituents that are routinely seen in hazardous waste samples.
1.2 The scope of this test method may be expanded to include other volatile and semivolatile organic constituents.
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.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method is intended for the evaluation of the wetting and drying resistance of monolithic, solid, solidified/stabilized wastes under the testing conditions of this test method.
This test method may be used for the comparison of wetting and drying resistance of wastes.
Data tabulated in Table 1, Table 2, and Table 3 may be used to observe irregularities caused by inhomogeneity of specimens and/or comparison of mass loss-cycle relations of different wastes, as well as to measure method-related mass losses such as matrix dissolution.
SCOPE
1.1 This test method covers procedures for determining material losses produced by repeated wetting and drying of solid waste specimens. It also covers the visual observation of the disintegration of solid specimens.
1.2 This test method intends that the material used in the procedure be physically, chemically, and biologically representative; hence it does not address problems as a result of the inhomogeneity of specimens.
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 and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
This test method is meant to allow for a rapid (24 h) index of a geomedia’sorption affinity for given chemicals or leachate constituents. A large number of samples may be run using this test method to determine a comparative ranking of those samples, based upon the amount of solute sorbed by the geomedia, or by various geomedia or leachate constituents. The 24-h time is used to make the test convenient and also to minimize microbial degradation which may be a problem in longer-timed procedures. While Kd values are directly applicable for screening and comparative ranking purposes, their use in predictive field applications generally requires the assumption that Kd be a fixed value.
While this test method may be useful in determining 24-h Kd values for nonvolatile organic constituents, interlaboratory testing has been carried out only for the nonvolatile inorganic species, arsenic and cadmium. However, the procedure has been tested for single laboratory precision with polychlorinated biphenyls (PCBs) and is believed to be useful for all stable and nonvolatile inorganic, and organic constituents. This test method is not considered appropriate for volatile constituents.
The 24-h time limit may be sufficient to reach a steady-state Kd. However, to report this determination as a steady-state Kd, this test method should be conducted for intermediate times (for example, 12, 18 and 22 h) to ensure that the soluble concentrations in the solution have reached a steady state by 24 h. Refer to Test Method D 4319 for an alternate procedure of longer duration.
SCOPE
1.1 This test method describes a procedure for determining the sorption affinity of waste solutes by unconsolidated geologic material in aqueous suspension. The waste solute may be derived from a variety of sources such as wells, underdrain systems, or laboratory solutions such as those produced by waste extraction tests like the Method D3987 shake extraction method.  
1.2 This test method is applicable in screening and providing relative rankings of a large number of geomedia samples for their sorption affinity in aqueous leachate/geomedia suspensions. This test method may not exactly simulate sorption characteristics that would occur in unperturbed geologic settings.  
1.3 While this procedure may be applicable to both organic and inorganic constituents, care must be taken with respect to the stability of the particular constituents and their possible losses from solution by such processes as degradation by microbes, light, or hydrolysis. This test method should not be used for volatile chemical constituents (see 6.1).  
1.4 This standard does not purport to address all of the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

SIGNIFICANCE AND USE
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 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. 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.
SCOPE
1.1 This practice describes the digestion of solid waste using nitric acid for the subsequent determination of inorganic constituents by argon plasma emission spectroscopy or atomic absorption spectroscopy.
1.2 The following elements may be solubilized by this practice: aluminummanganese berylliummercury cadmiumnickel chromiumphosphorus coppervanadium ironzinc lead
1.3 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 equivalent to total elements, depending on the element sought and 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 are not solubilized by this practice.
1.4 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 and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 7.