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ASTM D8018-15

(Test Method)

Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

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.

General Information

Status
Historical
Publication Date
31-Oct-2015
ICS
13.080.10 - Chemical characteristics of soils
Technical Committee
D34 - Waste Management
Drafting Committee
D34.01.06 - Analytical Methods
Current Stage
Ref Project

Relations

Replaced By
ASTM D8018-15(2020) - Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
Effective Date
01-Feb-2020

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ASTM D8018-15 - Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)ASTM D8018-15 - Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
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ASTM D8018-15 - Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
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Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D8018 − 15
Standard Test Method for
Determination of (Tri-n-butyl)-n-tetradecylphosphonium
chloride (TTPC) in Soil by Multiple Reaction Monitoring
1
Liquid Chromatography/Mass Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D8018; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope mLin75%acetone/25%water.Thefinalextractvolumeis20
mL because a 15 mL volume of acetone is added to each soil
1.1 This procedure covers the determination of (Tri-n-
sample and only the liquid layer after extraction is filtered
butyl)-n-tetradecylphosphonium chloride (TTPC) in a soil
leaving the solid behind followed by the addition of 5 mL of
matrix by extraction with acetone, filtration, dilution with
water to the acetone extract.
water, and analysis by liquid chromatography/tandem mass
2
spectrometry.TTPCisabiocidethatstronglyadsorbstosoils. 1.3 Units—The values stated in SI units are to be regarded
Thesampleextractsarepreparedinasolutionof75%acetone asstandard.Nootherunitsofmeasurementareincludedinthis
and 25% water because TTPC has an affinity for surfaces and standard.
particles. The reporting range for this method is from 250 to
1.4 This standard does not purport to address all of the
10000 ng/kg. This analyte is qualitatively and quantitatively
safety concerns, if any, associated with its use. It is the
determine by this method. This method adheres to multiple
responsibility of the user of this standard to establish appro-
reaction monitoring (MRM) mass spectrometry.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.
1.2 The Method Detection Limit (Note 1) (MDL) and
Reporting Range (Note 2) for the target analyte are listed in
2. Referenced Documents
Table 1.
3
2.1 ASTM Standards:
NOTE 1—The MDL is determined following the Code of Federal
D1193Specification for Reagent Water
Regulations, 40 CFR Part 136, Appendix B, as a guide utilizing solvent
D2777Practice for Determination of Precision and Bias of
extraction of soil. Two-gram sample of Ottawa Sand was utilized. A
detailedprocessdeterminingtheMDLisexplainedinthereferenceandis Applicable Test Methods of Committee D19 on Water
beyond the scope of this standard to be explained here.
D5681Terminology for Waste and Waste Management
NOTE 2—Reporting range concentration is calculated from Table 2
D5847Practice for Writing Quality Control Specifications
concentrations assuming a 50 µL injection of the Level 1 calibration
for Standard Test Methods for Water Analysis
standardforTTPC,andthehighestlevelcalibrationstandardwitha20mL
E2554Practice for Estimating and Monitoring the Uncer-
final extract volume ofa2g soil sample. Volume variations will change
the reporting limit and ranges.
tainty of Test Results of a Test Method Using Control
Chart Techniques
1.2.1 Thereportinglimitinthistestmethodistheminimum
4
2.2 Other Documents:
value below which data are documented as non-detects. Ana-
EPAPublication SW-846Test Methods for Evaluating Solid
lyte detections between the method detection limit and the
Waste, Physical/Chemical Methods
reporting limit are estimated concentrations and are not re-
40 CFR Part 136,Appendix BDefinition and Procedure for
ported following this test method. The reporting limit is
the Determination of the Method Detection Limit
calculated from the concentration of the Level 1 calibration
standard as shown in Table 2 for TTPC after taking into
3. Terminology
accounta2g sample weight and a final extract volume of 20
3.1 For determinations of terms used in this standard, refer
to Terminology D5681.
1
This test method is under the jurisdiction ofASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.06 on
3
Analytical Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Nov. 1, 2015. Published November 2015. DOI: contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
10.1520/D8018-15. Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon
2
More information on TTPC can be found at http://www.buruenergy.com/wp- the ASTM website.
4
content/uploads/BE-Environmental-Properties-of-Proposed- Biocide-BE-91.pdf Available from NationalTechnical Information Service (NTIS), 5301 Shawnee
(2014) and http://iaspub.epa.gov/sor_internet/registry/substreg/searchandretrieve/ Rd.,Alexandria,VA22312,http://www.ntis.govorathttp://www.epa.gov/epawaste/
advancedsearch/externalSearch.do?p_type=CASNO&p=81741-28-8 (2014). hazard/testmethods/index.htm.
Copyright © ASTM
...

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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.  
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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.  
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ASTM E2787-21(Test Method)
Standard Test Method for Determination of Thiodiglycol in Soil Using Pressurized Fluid Extraction Followed by Single Reaction Monitoring Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

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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  
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ASTM D8018-15(2020)(Test Method)
Standard Test Method for Determination of (Tri-n-butyl)-n-tetradecylphosphonium chloride (TTPC) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

SIGNIFICANCE AND USE
5.1 This test method has been developed by the U.S. EPA Region 5 Chicago Regional Laboratory (CRL).  
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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.  
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Standard Test Method for Analysis of Target Phenols (TPs) in Soil by Multiple Reaction Monitoring Liquid Chromatography/Mass Spectrometry (LC/MS/MS)

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.  
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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.  
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ASTM D7858-13(2018)(Test Method)
Standard Test Method for Determination of Bisphenol A in Soil, Sludge, and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography/Tandem Mass Spectrometry

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.  
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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.  
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ASTM G51-23(Test Method)
Standard Test Method for Measuring pH of Soil for Use in Corrosion Evaluations

SIGNIFICANCE AND USE
4.1 Information on pH of soil is used as an aid in evaluating the corrosivity of a soil environment. Some metals are more sensitive to the pH of their environment than others, and information on the stability of a metal as a function of pH and potential is available in the literature.3
SCOPE
1.1 This test method covers a procedure for determining the pH of a soil in corrosion evaluations. The principle use of the test is to supplement soil resistivity measurements and thereby identify conditions under which the corrosion of metals in soil may be accentuated (see G57 – 78 (2012)).  
1.2 The values stated in SI units are to be regarded as 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.

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ASTM
ASTM D5831-23(Practice)
Standard Practice for Screening Fuels in Soils

SIGNIFICANCE AND USE
5.1 This practice is a screening procedure for determining the presence of fuels containing aromatic compounds in soils. If a sample of the contaminant fuel is available for use in calibration, the approximate concentration of the fuel in the soil can be calculated. If the fuel type is known but a sample of the contaminant fuel is not available for calibration, an estimate of the contaminant fuel concentration can be calculated using average response factors based on composition of the fuel in the soil. If the composition of the contaminant fuel is unknown, a contaminant concentration cannot be calculated, and this practice can only be used only to indicate the presence or absence of fuel contamination.  
5.2 Fuels containing aromatic compounds, such as diesel fuel and gasoline, as well as other aromatic-containing hydrocarbon materials, such as crude oil, coal oil, and motor oil, can be determined by this practice. The quantitation limit for diesel fuel is about 75 mg/kg. Approximate quantitation limits for other aromatic-containing hydrocarbon materials that can be determined by this screening practice are given in Table 1. Quantitation limits for highly aliphatic materials, such as aviation gasoline and synthetic motor oil, are much higher than those for more aromatic materials, such as coal oil and diesel fuel.  
Note 1: The quantitation limits listed in Table 1 are estimated values because in this practice, the quantitation limit can be influenced by the particular fuel type and soil background. For information on how the values given in Table 1 were determined, see Appendix X1. Data generated during the development of this screening practice and other information pertaining to this practice can be found in the referenced research reports (1, 2).3  
5.3 When applying this practice to sites contaminated by diesel fuel, care should be taken in selecting the appropriate response factor from the list given in Table 2, with consideration given to whether or not t...
SCOPE
1.1 This practice is a screening procedure for assessing the presence of fuels containing aromatic compounds in soils. If a sample of the contaminant fuel is available, the concentration of the fuel in the soil can be determined. If the contaminant fuel type is known but a sample of the contaminant fuel is not available, an estimate of the concentration of the fuel in the soil can be made using average response factors based on composition of the fuel in the soil. If the kind of contaminant fuel is unknown, this screening method can be used to identify the presence of contamination.  
1.2 The values stated in SI units are to be regarded as 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.

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ASTM
ASTM D7968-23(Test Method)
Standard Test Method for Determination of Polyfluorinated Compounds in Soil by Liquid Chromatography Tandem Mass Spectrometry (LC/MS/MS)

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.

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