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New Test Methods On-line

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The promulgation of the Methods Innovation Rule (MIR) (70 FR 34547, June 14, 2005) allows for the use of any appropriate method for RCRA applications. These new SW-846 methods are intended to be guidance methods which contain general information on how to perform an analytical procedure or technique which a laboratory can use as a basic starting point for generating its own detailed Standard Operating Procedure (SOP), either for its own general use or for a specific project application. Therefore these methods can be used for any RCRA applications for which their performance can be demonstrated to be appropriate, i.e. applications for which they can be demonstrated to work.

Method 8276 - Sep 2012
Method 9016 - Jun 2010
Method 4435 - Feb 2008
Method 4430 - Dec 2007
Method 8272 - Dec 2007
Method 8271 - Jul 2007
Method 8170 - Jul 2007
Method 3572 - Jul 2007
Method 3571 - Jul 2007
Method 6860 - Jan 2007

Method 6850 - Jan 2007
Method 8330B - Oct 2006
Method 8261A - Oct 2006
Method 8260C - Aug 2006
Method 3200 - Jul 2005
Method 3542A - May 2005
Method 9013A - Nov 2004
Method 9015 - Nov 2004
Method 5021A - Jun 2003
Method 8015D - Jun 2003

Method 5030C - May 2003
Method 8000C - Mar 2003
Method 8323 - Jan 2003
Method 3511 - Nov 2002
Method 3570 - Nov 2002
Method 4025 - Oct 2002
Method 5035A - Jul 2002
Method 8265 - Mar 2002

Method 8276 (PDF) (60 pp, 492K) [September 2012]
Toxaphene and Toxaphene Congeners by Gas Chromatography/Negative Ion Chemical Ionization Mass Spectrometry (GC-NICI/MS)

This determinative method is used to measure the concentrations of various toxaphene congeners and technical toxaphene (along with the possible addition of other toxaphene congeners and compounds from Method 8081) in extracts from solid and liquid matrices, using fused-silica, open-tubular capillary columns with negative ion chemical ionization mass spectrometry (NICI/MS). This approach emphasizes the analytical conditions recommended for technical toxaphene and for toxaphene congeners as compared to weathered toxaphene. Technical toxaphene can be definitively quantitated by NICI/MS while weathered toxaphene may only appear to be present based on the detection of ions found in toxaphene or the presence of known degradation products of toxaphene (e.g., Hx-Sed and Hp-Sed).

Analysis of toxaphene (a mixture of polychlorinated monoterpenes) involves monitoring a series of ions representing various congener groups found in the mixture and integrating all of these signals for a total toxaphene response. Individual toxaphene congeners are quantitated using the primary ion and confirmed by their secondary ions.

Method 9016 (PDF) (30 pp, 544K) [June 2010]
Free Cyanide in Water, Soils and Solid Wastes by Microdiffusion

This determinative method is used to measure free cyanide in wastewaters, ground waters, surface waters, drinking waters, soils and solid wastes. This test method reports the cyanide that dissociates from simple cyanides or weakly-bound metal cyanide complexes at room temperature, from a solution at pH 6-6.5.

This test method does not determine strongly-bound metal cyanide complexes that resist dissociation, such as the hexacyanoferrates and gold cyanide, nor does it determine thiocyanate and cyanohydrin.

Method 4435 (PDF) (58 pp, 386K) [February 2008]
Method For Toxic Equivalents (TEQS) Determinations For Dioxin-Like Chemical Activity with the CALUX® Bioassay

Method 4435 is a bio-analytical screening procedure for dioxin-like compounds in soils/sediments. This method is based on the ability of dioxin and related chemicals to activate the Ah receptor (AhR), a chemical-responsive DNA binding protein that is responsible for producing the toxic and biological effects of these chemicals. Measurement of the level of activation of AhR-dependent gene expression by a chemical or chemical extract provides a measure by which to estimate the relative potency and toxic potential of these chemicals and/or extracts with resulting values expressed as Toxic Equivalents (TEQs).

Method 4430 (PDF) (21 pp, 161K) [December 2007]
Screening For Polychlorinated Dibenzo-p-Dioxins And Furans (PCDD/Fs) By Aryl Hydrocarbon-Receptor PCR Assay

Method 4430 is a procedure for the screening of Polychlorinated dibenzo-p-dioxins and furans (PCDD/Fs) in soil and sediment. This method uses a commercially available Aryl hydrocarbon Receptor (AhR) based polymerase chain reaction (PCR) assay.. The AhR-PCR assay screens samples by their toxicity equivalent quotient (TEQ) by responding to individual PCDD/F congeners in approximate correlation to their toxicity equivalent factors (TEF). The TEQ measured by the AhR-PCR assay is the sum of the response from the individual congeners. There is a table which contains a detailed list of response factors for individual PCDD/F congeners. More information about the AhR-PCR assay can be found at the manufacturer’s website link in the method.

Method 8272 (PDF) (34 pp, 266K) [December 2007]
Parent and Alkyl Polycyclic Aromatics In Sediment Pore Water By Solid-Phase Microextraction And Gas Chromatography/Mass Spectrometry In Selected Ion Monitoring Mode

The EPA narcosis model for benthic organisms in sediments contaminated with polycyclic aromatic hydrocarbons (PAHs) is based on the concentrations of dissolved PAHs in the interstitial water or pore water in sediment. Method 8272 covers the separation of pore water from PAH-impacted sediment samples, the removal of colloids, and the subsequent measurement of dissolved concentrations of the 10-parent PAHs and two alkylated daughter PAHs in the pore water samples. This method directly determines the concentrations of dissolved PAHs in environmental sediment pore water, groundwater, and other water samples using solid-phase microextraction (SPME) for static sample collection followed by desorption into a gas chromatograph (GC) equipped with a mass spectrometric (MS) detector operated in the selected ion monitoring (SIM) mode for analyte identification and quantitation.

Method 8271 (PDF) (20 pp, 237K) [July 2007]
Assay of Chemical Agents in Solid and Aqueous Samples by Gas Chromatograph/Mass Spectrometry, Electron Impact (GC/MS/EI)

Method 8271 describes the analysis of chemical agents in aqueous and solid samples by gas chromatography/mass spectrometry (GC/MS). The method has been applied to concrete, charcoal, wood, water, brine, ash, coral, sand, and soil. It involves introduction of the sample into gas chromatograph with mass spectrometric detector. Samples can either be directly injected or desorbed from a solid sorbent. Potential extraction techniques include Methods 3571 and 3572. This determinative method may also be applicable to other chemically similar compounds and chemical agent degradation products.

Method 8170 (PDF) (18 pp, 205K) [July 2007]
Assay of Chemical Agents in Solid and Aqueous Samples by Gas Chromatography/Flame Photometric Detection (GC/FPD)

Method 8170 describes the analysis of chemical agents in aqueous and solid samples by gas chromatography/flame photometric detection (GCFPD). The method has been applied to concrete, charcoal, wood, water, brine, ash, coral, sand, and soil. It involves introduction of the sample into a gas chromatograph equipped with flame photometric detector. Samples can either be directly injected or thermally desorbed from a solid sorbent. Potential extraction techniques include Methods 3571 and 3572. This determinative method may also be applicable to other chemically similar compounds and chemical agent degradation products.

Method 3572 (PDF) (9 pp, 52K) [July 2007]
Extraction of Wipe Samples for Chemical Agents

Method 3572 describes the extraction of chemical agents from wipe samples using a microextraction technique. Potential determinative procedures include Methods 8170 and 8271. This extraction technique may also be applicable to other chemically similar compounds and chemical agent degradation products.

Method 3571 (PDF) (14 pp, 139K) [July 2007]
Extraction of Solid and Aqueous Samples for Chemical Agents

Method 3571 describes the extraction of chemical agents from aqueous and solid samples using a microextraction technique. The method has been applied to concrete, charcoal, wood, water, brine, ash, coral, sand, and soil. Potential determinative procedures include Methods 8170 and 8271. This extraction technique may also be applicable to other chemically similar compounds and chemical agent degradation products.

Method 6860 (PDF) (31 pp, 219K) [January 2007]
Perchlorate in Water, Soils and Solid Wastes Using Ion Chromatography/Electrospray Ionization/Mass Spectrometry

This test method uses ion chromatography (IC) coupled with electrospray ionization (ESI) mass spectrometry (MS) or tandem mass spectrometry (MS/MS) for the determination of perchlorate in surface water, groundwater, wastewater, salt water, and soil. Solids are first extracted prior to analysis using reagent water. Aqueous samples and extracts are filtered, and analyzed via IC/MS (with or without fragmentation) or IC/MS/MS. Perchlorate is detected and quantified using mass-to-charge (m/z) ratio 83 (or 99) for native perchlorate and internal standard calibration, based on the m/z ion 89 (or 107). Additional confirmation of perchlorate identification is provided by monitoring the abundance ratio of the isotopic ions, m/z 83 (or 99) and 85 (or 101). Method 6860 confirms perchlorate detection and overcomes many of the interference problems encountered when using IC/conductivity suppression analysis for perchlorate (Method 9058). The method allows analytical flexibility - a variety of chromatographic conditions and analysis options have been validated and are provided in the test method.

This method has not been fully validated for complex matrices, such as wastewater treatment sludges, using the recommended extraction procedure. Additional studies will be undertaken to confirm if alternative extraction approaches will provide more efficient perchlorate recoveries in such matrices.

Method 6850 (PDF) (27 pp, 143) [January 2007]
Perchlorate in Water, Soils and Solid Wastes Using High Performance Liquid Chromatography/Electrospray Ionization/Mass Spectrometry

This test method uses high performance liquid chromatography (HPLC) coupled with electrospray ionization (ESI) mass spectrometry (MS) or tandem mass spectrometry (MS/MS) for the determination of perchlorate in surface water, groundwater, wastewater, salt water, and soil. Solids are first extracted prior to analysis using reagent water. Aqueous samples and extracts are filtered, and analyzed via HPLC/MS (with or without fragmentation) or HPLC/MS/MS. Perchlorate is detected and quantified using mass-to-charge (m/z) ratio 83 (or 99) for native perchlorate and internal standard calibration, based on the m/z ion 89 (or 107). Additional confirmation of perchlorate identification is provided by monitoring the abundance ratio of the isotopic ions, m/z 83 (or 99) and 85 (or 101). Method 6850 confirms perchlorate detection and overcomes many of the interference problems encountered when using IC/conductivity suppression analysis for perchlorate (Method 9058). The method allows analytical flexibility - a variety of chromatographic conditions and analysis options have been validated and are provided in the test method.

This method has not been fully validated for complex matrices, such as wastewater treatment sludges, using the recommended extraction procedure. Additional studies will be undertaken to confirm if alternative extraction approaches will provide more efficient perchlorate recoveries in such matrices.

Method 8330B (PDF) (60 pp, 285K) [October 2006]
Nitroaromatics, Nitramines and Nitrate Esters by High Performance Liquid Chromatography (HPLC)

There are three major changes associated with this method update:

an update of information regarding use of up-to-date chromatographic columns and technology
integration of Method 8332 analytes by inclusion of dual wavelength detector; and,
addition of an appendix which addresses sampling issues for explosives and which contains many references.

This method is intended for the trace analysis of explosives and propellant residues by high performance liquid chromatography (HPLC) using a dual wavelength UV detector. This method provides a direct injection procedure for high level water samples, an extraction procedure for soils and sediments as well as a low level method for the extraction of water samples. The use of solid-phase extraction, Method 3535, has been shown to provide equal or superior results and is preferred for low level aqueous samples. All of these compounds are either used in the manufacture of explosives or propellants, are impurities in their manufacture, or they are the degradation products of compounds used for that purpose. Stock solutions for calibration are available through several commercial vendors.

Method 8261A (PDF) (99 pp, 487K) [October 2006]
Volatile Organic Compounds By Vacuum Distillation In Combination With Gas Chromatography/Mass Spectrometry (VD/GC/MS)

This is the version of this method that is recommended for use. It has been updated from the previous version to incorporate the latest available vacuum distillation equipment and has been made consistent with Method 8260C.

This method is based on a vacuum distillation and cryogenic trapping procedure (Method 5032) followed by gas chromatography/mass spectrometry (GC/MS). The method incorporates internal standard-based matrix correction, where the analysis of multiple internal standards is used to predict matrix effects. The normalization of matrix effects has the impact of making Method 8261 analyses matrix independent and allows multiple matrices to be analyzed within a sample batch. As a result, the calculations involved are specific to this method, and may not be used with data generated by another method. This method includes all of the necessary steps from sample preparation through instrumental analysis.

This method is used to determine the concentrations of volatile organic compounds, and some low-boiling semivolatile organic compounds, in a variety of liquid, solid, and oily waste matrices, as well as animal tissues. This method differs from the use of Method 5032/8260 in the use of internal standards to measure matrix effects and compensate analyte responses for matrix effects. This method is applicable to nearly all types of matrices, including water, soil, sediment, sludge, oil, and animal tissue. This method should be considered for samples where matrix effects are anticipated to severely impact analytical results.

This method can be used to quantitate most volatile organic compounds that have a boiling point below 245°C and a water-to-air partition coefficient below 15,000, which includes compounds that are miscible with water. Note that this range includes compounds not normally considered to be volatile analytes (e.g., nitrosamines, aniline, and pyridine).

Method 8260C (PDF) (92 pp, 324K) [August 2006]
Volatile Organic Compounds By Gas Chromatography/Mass Spectrometry(GC/MS)

Method 8260C is a GC/MS method that is used to determine volatile organic compounds in a variety of solid waste matrices. This method is applicable to nearly all types of samples, regardless of water content, including various air sampling trapping media, ground and surface water, aqueous sludges, caustic liquors, acid liquors, waste solvents, oily wastes, mousses, tars, fibrous wastes, polymeric emulsions, filter cakes, spent carbons, spent catalysts, soils, and sediments. The RCRA analytes that have been determined by this method are listed in the table in Sec. 1.1

There are various techniques by which these compounds may be removed from the original matrices and introduced into the GC/MS system. The more common techniques are listed in the table in Sec. 1.1. Purge-and-trap, by Methods 5030 (aqueous samples) and 5035 (solid and waste oil samples), is the most commonly used technique for volatile organic analytes. However, other techniques are also appropriate and necessary for some analytes. These include direct injection following dilution with hexadecane (Method 3585) for waste oil samples; automated static headspace by Method 5021 for solid samples; direct injection of an aqueous sample (concentration permitting) or injection of a sample concentrated by azeotropic distillation (Method 5031); and closed system vacuum distillation (Method 5032) for aqueous, solid, oil and tissue samples. For air samples, Method 5041 provides methodology for desorbing volatile organics from trapping media (Methods 0010, 0030, and 0031). In addition, direct analysis utilizing a sample loop is used for sub-sampling from polytetrafluoroethylene (PTFE) bags (Method 0040). Method 5000 provides more general information on the selection of the appropriate introduction method.

Method 3200 (PDF) (28 pp, 215K) [July 2005]
Mercury Species Fractionation and Quantification by Microwave-assisted Extraction, Selective Solvent Extraction and/or Solid Phase Extraction

This test method uses sequential extraction and separation procedures to differentiate mercury species that are present in soils and sediments into four distinct fractions: extractable organic mercury, extractable inorganic mercury, semi-mobile mercury and non-mobile mercury. Extraction is accomplished with the aid of either microwave irradiation or ultrasound. Quantification of mercury in the different fractions may be performed using any appropriate determinative method, (e.g. Method 7473, 1631, or Methods 7470 and 7471). The test method also contains provisions for separating and quantifying individual extractable mercury species using HPLC.

Method 3542A (PDF) (22 pp, 91K) [May 2005]
Extraction of Semivolatile Analytes Collected Using Method 0010 (Modified Method 5 Sampling Train)

Method 3542A describes the extraction of semivolatile organic compounds from samples collected by Method 0010. This method replaces the Sample Preparation section of Method 0010 (Modified Method 5 Sampling Train, also known as SemiVOST), which currently addresses preparation of Method 0010 train components for analysis with very little detail.

Method 9013A (PDF) (10 pp, 90K) [November 2004]
Cyanide Extraction Procedure for Solids and Oils

Method 9013A is a procedure for extracting soluble and insoluble cyanides from solids and oil wastes prior to analysis using aqueous-based determinative methods. The resulting extraction solutions may be distilled and analyzed for total cyanide and/or cyanides amenable to chlorination (Methods 9010, 9012 and 9014) as well as analyzed for metal cyanide complexes (Method 9015). The method is applicable to oil, solid, and multiphasic sample matrices.

Method 9015 (PDF) (51 pp, 396K) [November 2004]
Metal Cyanide Complexes by Anion Exchange Chromatography and UV Detection

This test method uses anion exchange chromatography and UV detection for the quantitative measurement of the individual anionic metal cyanide complexes of iron, cobalt, silver, gold, copper, and nickel in waters and solid waste extracts. There is no derivatization and little if any sample preparation. The analytes are measured directly in aqueous solution as the anionic cyanide complex species. Solid waste samples may also be analyzed through the use of a simple alkaline extraction procedure (Method 9013). Metal cyanide concentrations in the µg/L range are determined using on-line sample preconcentration.

Method 5021A (PDF) (25 pp, 132K) [June 2003]
Volatile Organic Compounds in Various Sample Matrices Using Equilibrium Headspace Analysis

Method 5021 is a general purpose method for the preparation of volatile organic compounds (VOCs) in soil/sediment, solid waste, aqueous and water-miscible liquid samples for determination by gas chromatography (GC) or gas chromatography/mass spectrometry (GC/MS). The method is applicable to a wide range of organic compounds that have sufficiently high volatility to be effectively removed from samples using an equilibrium headspace procedure. It is particularly useful as the sample preparation method for fuel oxygenates when both the ethers and alcohols are target analytes of concern.

Method 8015D (PDF) (37 pp, 202K) [June 2003]
Nonhalogenated Organics Using GC/FID

Method 8015D may be used to determine the concentrations of various nonhalogenated volatile organic compounds and semivolatile organic compounds, including fuel oxygenate compounds, by gas chromatography using a flame ionization detector (FID).

Method 5030C (PDF) (28 pp, 167K) [May 2003]
Purge-and-Trap for Aqueous Samples

Method 5030C describes a purge-and-trap procedure for the analysis of volatile organic compounds (VOCs) in aqueous samples and water miscible liquid samples. It also describes the analysis of high concentration soil and waste sample extracts prepared in Method 5035. The gas chromatographic determinative steps are found in Methods 8015 and 8021. The method is also applicable to GC/MS Method 8260.

Method 8000C (PDF) (66 pp, 250K) [March 2003]
Determinative Chromatographic Separations

Method 8000C is not a determinative method, but instead provides updated guidance on analytical chromatography and describes calibration and appropriate quality control procedures that are common to all SW-846 chromatographic methods. However, more specific quality control requirements that are provided in the applicable determinative method will supersede those noted in Method 8000C. Method 8000C should be applied in conjunction with all SW-846 determinative chromatographic methods.

Recently, it has been brought to our attention that there is an inconsistency in the recommended use of standards for the Initial Demonstration of Capability between Method 8000C and Methods 8260C and 8270D. This memorandum (2 pp, 36K) is intended to eliminate this inconsistency which is due to the much earlier publication date of Method 8000C than of the two GC/MS methods.

Method 8323 (PDF) (22 pp, 119K) [January 2003]
Determination of Organotins by Micro-Liquid Chromatography- Electrospray Ion Trap Mass Spectrometry

Method 8323 is the first product of an EPA project to develop a series of class-specific Electrospray HPLC/MS methods to replace the obsolete Thermospray interface currently used in Method 8321. When the project is complete, EPA will issue a single integrated Electrospray HPLC/MS method. Method 8323 covers the use of solid-phase extraction (SPE) discs, solvent extractions (for biological tissues) as sample preparation methods, and micro-liquid chromatography ( LC) coupled with Electrospray ion trap mass spectrometry (ES-ITMS) [this technique would also be applicable to ES-quadrupole mass spectrometry (ES-MS)] for the determination of organotins (as the cation) in waters and biological tissues.

Method 3511 (PDF) (10 pp, 83K) [November 2002]
Organic Compounds in Water by Microextraction

Method 3511 is a procedure for extracting selected volatile and semivolatile organic compounds from water using a microscale approach which minimizes sample size and solvent usage, thereby reducing the supply costs, health and safety issues, and waste generated.

Method 3570 (PDF) (9 pp, 74K) [November 2002]
Microscale Solvent Extraction (MSE)

Method 3570 is a procedure for extracting selected volatile, semivolatile, and nonvolatile organic compounds from solid matrices such as soils, sludges, and wastes using a microscale approach which minimizes sample size and solvent usage, thereby reducing the supply costs, health and safety issues, and waste generated.

Method 4025 (PDF) (20 pp, 64K) [October 2002]
Screening for Polychlorinated Dibenzodioxins and Polychlorinated Dibenzofurans (PCDD/Fs) by Immunoassay

This method is a procedure for the analysis of PolyChlorinated DibenzoDioxins and PolyChlorinated DibenzoFurans (PCDD/Fs) in soil at 500 ppt (pg/g). The procedure uses an Enzyme Immunoassay (EIA) commercially available test kit containing a polyclonal antibody specific for PCDD/Fs. The EIA kit is designed for the screening of samples according to their toxic equivalent concentration (TEQ) by responding to the toxic PCDD/F congeners in approximate correlation with their toxic equivalency factors (TEFs). The test is capable of multiple congener recognition and preferentially targets congeners with high TEF values; i.e., those with the highest toxicity relative to 2,3,7,8- TetraChloroDibenzo-p-Dioxin (2,3,7,8-TCDD). The final measured EIA response is the sum of the individual congener responses. This response correlates with TEQ because the immunoassay cross-reaction profile for PCDD/Fs correlates with TEF values.

Method 5035A (PDF) (69 pp, 200K) [July 2002]
Closed-System Purge-and-Trap and Extraction for Volatile Organics in Soil and Waste Samples

This method describes a closed-system purge-and-trap sample preparation process for the analysis of volatile organic compounds (VOCs) in solid materials (e.g., soils, sediments, and solid waste). While the method is designed for use on samples containing low levels of VOCs, procedures are also provided for collecting and preparing solid samples containing high concentrations of VOCs and for oily wastes. In addition, the method contains an appendix with pertinent information and appropriate references based on EPA's evaluation of currently available data and technology as applied to the most appropriate sample handling and preservation procedures in order to minimize the loss of VOCs during the collection and analysis of aqueous and solid materials, such as groundwater, wastewater, soils, solid waste, or sediments. These procedures are designed to minimize the losses of VOCs through the two most common mechanisms, volatilization and biodegradation.

Method 8265 (PDF) (64 pp, 231K) [March 2002]
Volatile Organic Compounds in Water, Soil, Soil Gas and Air by Direct Sampling Ion Trap Mass Spectrometry (DSITMS)

This method uses direct sampling ion trap mass spectrometry (DSITMS) for the rapid quantitative measurement, continuous real-time monitoring, and qualitative and quantitative preliminary screening of volatile organic compounds (VOCs) in water, soil, soil gas, and air. DSITMS introduces sample materials directly into an ion trap mass spectrometer by means of a simple interface (such as a capillary restrictor). There is little if any sample preparation and no chromatographic separation. The response of the instrument to analytes in a sample is nearly instantaneous. In addition, the instrument is field transportable, rugged, and relatively easy to operate and maintain.

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