ASTM D8310-20

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.  
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.

General Information

• Status: Published
• Publication Date: 31-Jan-2020
• ICS: 13.080.10 - Chemical characteristics of soils
• Technical Committee: D34 - Waste Management
• Drafting Committee: D34.01.06 - Analytical Methods

Standards Content (Sample)

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.
Designation: D8310 − 20
Standard Test Method for
Analysis of Target Phenols (TPs) in Soil by Multiple
Reaction Monitoring Liquid Chromatography/Mass
1
Spectrometry (LC/MS/MS)
This standard is issued under the fixed designation D8310; 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 D7858Test Method for Determination of Bisphenol A in
Soil, Sludge, and Biosolids by Pressurized Fluid Extrac-
1.1 This test method covers analysis of nonylphenol (NP),
tion and Analyzed by Liquid Chromatography/Tandem
nonylphenolmonoethoxylate(NP1EO),nonylphenoldiethoxy-
Mass Spectrometry
late (NP2EO), octylphenol (OP), and bisphenol A (BPA),
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2.2 Federal Standards:
referred to collectively as target phenols (TPs), in soil,
29CFRPart1910OccupationalSafetyandHealthStandards
sediments, and biosolids by extraction with acetone, filtration,
40 CFR Part 136,Appendix BDefinition and Procedure for
dilution with water, and analysis by liquid chromatography/
the Determination of the Method Detection Limit—
tandemmassspectrometry.Thesampleextractsarepreparedin
Revision 1.11
a solution of 75% acetone and 25% water because TPs have
anaffinityforsurfacesandparticlesthatismorepronouncedat
3. Terminology
lower concentrations. The range of applicability of the test
3.1 Definitions of Terms Specific to This Standard:
method is shown in Table 1. The method may be extended
3.1.1 batch quality control, n—all the quality control (QC)
outside of these ranges depending on additional performance
samples and standards included in an analytical procedure.
studies not undertaken here.
3.1.2 bisphenol A, BPA—defined in Test Method D7858.
1.2 Units—The values stated in SI units are to be regarded
3.1.3 bisphenol A (propane-D6), BPA-D —defined in Test
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as the standard. No other units of measurement are included in
Method D7858.
this standard.
3.1.4 2-bromo-4-(1,1,3,3-tetramethylbutyl)phenol, Br-OP,
1.3 This standard does not purport to address all of the
n—used in this test method as a surrogate.
safety concerns, if any, associated with its use. It is the
3.1.4.1 Discussion—2-bromo-4-(1,1,3,3-tetramethylbutyl)
responsibility of the user of this standard to establish appro-
phenol is not produced commercially and is not expected to be
priate safety, health, and environmental practices and deter-
found in the environment. It was reported that compounds in
mine the applicability of regulatory limitations prior to use.
highlychlorinated,bromide-richwastewaterscouldpotentially
1.4 This international standard was developed in accor-
interfere with the Br-OP surrogate. If this interference is
dance with internationally recognized principles on standard-
encountered, n-nonylphenol is suggested as an alternative
ization established in the Decision on Principles for the
surrogate.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical 3.1.5 nonylphenol, NP, n—mixture of branched
Barriers to Trade (TBT) Committee. p-nonylphenol isomers.
3.1.5.1 Discussion—Commercial NP is produced by the
2. Referenced Documents
reaction of phenol with commercial nonene. Commercial
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2.1 ASTM Standards: nonene is not simply a linear C H alpha olefin; it is a
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complex mixture of predominantly nine-carbon olefins, called
D1193Specification for Reagent Water
propylene trimer, containing no linear isomers. This synthesis
results in a mixture of various branched nonylphenol isomers
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This test method is under the jurisdiction ofASTM Committee D34 on Waste
rather than a discrete chemical structure. The branched nonyl
Management and is the direct responsibility of Subcommittee D34.01.06 on
Analytical Methods.
group is positioned predominantly in the para position on the
CurrenteditionapprovedFeb.1,2020.PublishedFebruary2020.DOI:10.1520/
phenol ring.
D8310-20.
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For referenced ASTM standards, visit the ASTM website, www.astm.org, or
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contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Available from U.S. Government Printing Office, Superintendent of
Standards volume information, refer to the standard’s Document Summary page on Documents, 732 N. Capitol St., NW, Washington, DC 20401-0001, http://
the ASTM website. www.access.gpo.gov.
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D8310 − 20
TABLE 1 Tested Method Paramet
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