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
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.
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.
General Information
Relations
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: D7858 − 13 (Reapproved 2018)
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
This standard is issued under the fixed designation D7858; 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 2. Referenced Documents
1.1 ThisprocedurecoversthedeterminationofBisphenolA 2.1 ASTM Standards:
D653Terminology Relating to Soil, Rock, and Contained
(BPA) in soil, sludge, and biosolids. This test method is based
Fluids
upon solvent extraction of a soil matrix by pressurized fluid
D1193Specification for Reagent Water
extraction (PFE).The extract is filtered and analyzed by liquid
D3694Practices for Preparation of Sample Containers and
chromatography/tandem mass spectrometry (LC/MS/MS).
for Preservation of Organic Constituents
BPAis qualitatively and quantitatively determined by this test
D3740Practice for Minimum Requirements for Agencies
method.
Engaged inTesting and/or Inspection of Soil and Rock as
1.2 Units—The values stated in SI units are to be regarded
Used in Engineering Design and Construction
asstandard.Nootherunitsofmeasurementareincludedinthis
D3856Guide for Management Systems in Laboratories
standard.
Engaged in Analysis of Water
D5681Terminology for Waste and Waste Management
1.3 The method detection limit (MDL), electrospray ion-
E2554Practice for Estimating and Monitoring the Uncer-
ization (ESI) mode, and reporting range for BPAare listed in
tainty of Test Results of a Test Method Using Control
Table 1.
Chart Techniques
1.4 This standard does not purport to address all of the
2.2 Other Documents:
safety concerns, if any, associated with its use. It is the
EPA SW-846Test Methods for Evaluating Solid Waste,
responsibility of the user of this standard to establish appro-
Physical/Chemical Methods
priate safety, health, and environmental practices and deter-
40 CFR Part 136,Appendix BDefinition and Procedure for
mine the applicability of regulatory limitations prior to use. 6
the Determination of the Method Detection Limit
1.5 This international standard was developed in accor-
dance with internationally recognized principles on standard-
3. Terminology
ization established in the Decision on Principles for the
3.1 Definitions:
Development of International Standards, Guides and Recom-
3.1.1 Bisphenol A (BPA), n—2,2-bis(4-hydroxyphenyl) pro-
mendations issued by the World Trade Organization Technical
pane.
Barriers to Trade (TBT) Committee.
3.1.2 Bisphenol A (propane-D ) (BPA-D ), n—deuterium
6 6
labeledBisphenolAwherethetwomethylmoietiescontainall
1 H and is used as a surrogate in this method.
This test method is under the jurisdiction ofASTM Committee D34 on Waste
Management and is the direct responsibility of Subcommittee D34.01.06 on
Analytical Methods.
Current edition approved Sept. 1, 2018. Published September 2018. Originally
approved in 2013. Last previous edition approved in 2013 as D7858–13. DOI: For referenced ASTM standards, visit the ASTM website, www.astm.org, or
10.1520/D7858-13R18. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
The MDL is determined following the Code of Federal Regulations, 40 CFR Standardsvolumeinformation,refertothestandard’sDocumentSummarypageon
Part 136,Appendix B utilizing solvent extraction of soil by PFE.A10-g sample of the ASTM website.
Ottawa sand was utilized.Adetailed process determining the MDL is explained in AvailablefromUnitedStatesEnvironmentalProtectionAgency(EPA),William
the reference and is beyond the scope of this test method to be explained here. Jefferson Clinton Bldg., 1200 Pennsylvania Ave., NW, Washington, DC 20460,
Reporting range concentration is calculated from Table 4 concentrations http://www.epa.gov.
assuming a 25-µL injection of the Level 1 calibration standard for BPA, and the AvailablefromU.S.GovernmentPrintingOfficeSuperintendentofDocuments,
highest level calibration standard with a 5-mL final extract volume of a 10-g soil 732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http://
sample. Volume variations will change the reporting limit and ranges. www.access.gpo.gov.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7858 − 13 (2018)
TABLE 1 Method Detection Limit and Reporting Range
5. Significance and Use
Reporting Range
Analyte ESI Mode MDL (PPB) 5.1 This is a performance-based method, and modifications
(PPB)
are allowed to improve performance.
Bisphenol A Negative 2.8 10–250
5.1.1 Due to the rapid development of newer instrumenta-
tionandcolumnchemistries,changestotheanalysisdescribed
in this test method are allowed as long as better or equivalent
performance data result. Any modifications shall be docu-
3.1.3 filter unit, n—in this test method, a filter that is
mented and performance data generated. The user of the data
supported with a housing that is inert to the solvents used as
generated by this test method shall be made aware of these
described in 7.4 of this test method.
changes and given the performance data demonstrating better
3.1.4 filtration device, n—a device used to remove particles
or equivalent performance.
from the extract that may clog the liquid chromatography
5.2 The first reported synthesis of BPAwas by the reaction
system as described in 7.4 of this test method.
of phenol with acetone by Zincke. BPA has become an
3.1.5 glass fiber filter, n—a porous, glass fiber material onto
important high-volume industrial chemical used in the manu-
which solid particles present in the extraction fluid, which
facture of polycarbonate plastic and epoxy resins. Polycarbon-
flowsthroughit,arelargelycaughtandretained,thusremoving
ateplasticandresinsareusedinnumerousproducts,including
them from the extract.
electrical and electronic equipment, automobiles, sports and
safetyequipment,reusablefoodanddrinkcontainers,electrical
3.1.6 hypodermic syringe, n—in this test method, a Luer-
lock-tipped glass syringe capable of holding a syringe-driven laminates for printed circuit boards, composites, paints,
adhesives, dental sealants, protective coatings, and many other
filter unit as described in 7.4 of this test method.
products.
3.1.7 pressurized fluid extraction, n—the process of trans-
ferringtheanalytesofinterestfromthesolidmatrix,asoil,into 5.3 The environmental source of BPA is predominantly
theextractionsolventusingpressureandelevatedtemperature.
from the decomposition of polycarbonate plastics and resins.
BPAisnotclassifiedasbio-accumulativebytheU.S.Environ-
3.1.8 reporting range, n—the quantitative concentration
mental Protection Agency and will biodegrade. BPA has been
range for an analyte in this test method.
reported to have adverse effects in aquatic organisms and may
3.2 Abbreviations:
be released into environmental waters directly at trace levels
3.2.1 BPA—bisphenol A
through landfill leachate and sewage treatment plant effluents.
3.2.2 LC—liquid chromatography
This method has been investigated for use with soil, sludge,
and biosolids.
3.2.3 LCS/LCSD—laboratory control spike/laboratory con-
trol spike duplicate
5.4 The land application of biosolids has raised concerns
–3
3.2.4 mM—millimolar,1×10 moles/L overthefateofBPAintheenvironment,andastandardmethod
is needed to monitor concentrations. This method has been
3.2.5 MRM—multiple reaction monitoring
investigated for use with various soils.
3.2.6 MS—matrix spike
3.2.7 NA—not available
6. Interferences
3.2.8 ND—non-detect
6.1 Methodinterferencesmaybecausedbycontaminantsin
3.2.9 PFE—pressurized fluid extraction solvents, reagents, glassware, and other apparatus producing
discrete artifacts or elevated baselines. All of these materials
3.2.10 PPB—parts per billion
are demonstrated to be free from interferences by analyzing
3.2.11 QC—quality control
laboratory reagent blanks under the same conditions as
3.2.12 RL—reporting limit
samples.
3.2.13 SD—standard deviation
6.2 All reagents and solvents shall be of pesticide residue
3.2.14 SRM—single reaction monitoring purity or higher to minimize interference problems.
3.2.15 VOA—volatile organic analysis
6.3 Matrix interferences may be caused by contaminants
that are co-extracted from the sample. The extent of matrix
4. Summary of Test Method
interferences can vary considerably from sample source de-
pending on variations of the sample matrix.
4.1 For BPA analysis in soil, sludge, and biosolid, samples
are shipped to the lab between 0°C and 6°C.The samples are
7. Apparatus
to be extracted and filtered within 14 days of collection, and
analyzed by LC/MS/MS within 14 days of extraction. 7.1 LC/MS/MS System:
4.2 BPA and the surrogate (BPA-D ) are identified by
retentiontimeandoneSRMtransition.Thetargetanalytesand
Zincke, T., “Mittheilungen aus dem chemischen Laboratorium der Universitat
surrogates are quantitated using the SRM transitions utilizing
Marburg,” Justus Leibigs Annals Chemie, Vol 343, 1905, pp. 75–79.
an external calibration.The final report issued for each sample
Additional information about BPA is available on the Internet at http://
lists the concentration of BPA and surrogate recovery. www.bisphenol-a.org (2008).
D7858 − 13 (2018)
7.1.1 Liquid Chromatography (LC) System —A complete 7.4.1.1 A 10-mL lock-tip glass syringe size is
LC system is required in order to analyze samples. An LC recommended, since a 3-mL sample extract results after
system that is capable of performing at the flows, pressures, blow-down.
controlled temperatures, sample volumes, and requirements of 7.4.2 Filter Unit —Filter units of polyvinylidene fluoride
the standard shall be used. (PVDF) with a glass fiber prefilter were used to filter the PFE
extracts.
7.1.2 Analytical Column —A column that achieves ad-
7.4.3 Discussion—A filter unit shall be used that meets the
equate resolution shall be used. The retention times and order
requirements of the test method.
ofelutionmaychangedependingonthecolumnusedandneed
to be monitored. A reverse-phase analytical column that
8. Reagents and Materials
combines the desirable characteristics of a reversed-phase
8.1 Purity of Reagents—High-performance liquid chroma-
HPLC column with the ability to separate polar compounds
was used to develop this test method. tography (HPLC) pesticide residue analysis and
spectrophotometry-grade chemicals shall be used in all tests.
7.1.3 Tandem Mass Spectrometer (MS/MS) System —A
Unlessindicatedotherwise,itisintendedthatallreagentsshall
MS/MS system capable of multiple reaction monitoring
conform to the Committee on Analytical Reagents of the
(MRM)analysis,oranysystemthatiscapableofperformingat
American Chemical Society. Other reagent grades may be
the requirements in this test method, shall be used.
used, provided they are first determined to be of sufficiently
7.2 Pressurized Fluid Extraction Device (PFE):
highpuritytopermittheirusewithoutaffectingtheaccuracyof
7.2.1 A PFE system was used for this test method with
the measurements.
appropriatelysizedextractioncells.Cellsareavailablethatwill
8.2 Purity of Water—Unless otherwise indicated, references
accommodate the 10-g sample sizes used in this test method.
to water shall mean reagent water conforming toASTM Type
Cells shall be made of stainless steel or other material capable
I of Specification D1193. It must be demonstrated that this
of withstanding the pressure requirements (≥2000 psi) neces-
water does not contain contaminants at concentrations suffi-
sary for this procedure. A pressurized fluid extraction device
cient to interfere with the analysis.
shall be used that can meet the necessary requirements in this
8.3 Gases—Nitrogen (purity ≥97 %) and argon (purity
test method.
≥99.999 %).
7.2.2 Glass Fiber Filters.
7.2.3 Amber VOA Vials—60 mL, for sample extracts for 8.4 Acetonitrile (CH CN, CAS # 75-05-8).
PFE.
8.5 Ethyl acetate (CH COOC H , CAS # 141-78-6).
3 2 5
7.3 Organic Solvent Evaporation Device.
8.6 2-Propanol (C H O, CAS # 67-63-0).
3 8
7.4 Filtration Device: 8.7 Methanol (CH OH, CAS # 67-56-1).
7.4.1 Hypodermic Syringe—A Luer-lock tip glass syringe
8.8 Ammonium acetate (CH CO NH , CAS # 631-61-8).
3 2 4
capable of holding a syringe-driven filter unit.
8.9 Bisphenol A (C H O , 2,2’-Bis(4-hydroxyphenyl)
15 16 2
propane, CAS # 80-05-7).
8.10 Bisphenol A (Propane-D ) represents deuterium la-
9 6
A Waters Acquity UPLC® H-Class System was used to develop this test
beled Bisphenol A where the two methyl moieties contain all
method and generate the precision and bias data presented in Section 16. Waters
H.
Corporation, Milford, MA01757. Instrumentation from other vendors may also be
able to generate similar method performance.
8.10.1 Discussion—BPA-D is used as a surrogate in this
A Waters-UPLC® T3, 100 mm x 2.1 mm, 1.8-µm particle size, was used to
test method.
develop this test method and generate the precision and bias data presented in
Section 16. Waters Corporation, Milford, MA01757. Columns from other vendors
8.11 Ottawa sand (CAS # 14808-60-7) or equivalent.
that are able to generate similar method performance and that achieve adequate
resolution may be used. A guard column was also used, VanGuard™ Pre-Column, 8.12 Drying agent.
2.1 × 5 mm, 1.8-µm particle size.
11 8.13 Sodium sulfate (Na SO , CAS # 7757-82-6).
AWatersQuattromicro™APImassspectrometerwasusedtodevelopthistest 2 4
method and generate the precision and bias data presented in Section 16. Waters
Corporation, Milford, MA01757. Instrumentation from other vendors may also be
able to generate similar method performance. Pall®-Acrodisc® Premium 25-mm Syringe Filter with GxF/0.2 µm PVDF
ADionexAccelerated Solvent Extraction (ASE® 200) system with appropri- Membrane (Pall Corporation, Catalog # AP-4793, were used to develop this test
ately sized extraction cells was used to develop this test method and generate the method and generate the precision and bias data presented in Section 16. Filters
precisionandbiasdatapresentedinSection16.DionexCorporation,Sunnyvale,CA from other vendors may also be able to generate similar method performance.
94088. Instrumentation from other vendors may also be able to generate similar Reagent Chemicals, American Chemical Society Specifications, American
method performanc
...
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