ASTM D7858-2013(2018) 9375 Standard Test Method for Determination of Bisphenol A in Soil Sludge and Biosolids by Pressurized Fluid Extraction and Analyzed by Liquid Chromatography .pdf

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1、Designation: D7858 13 (Reapproved 2018)Standard Test Method forDetermination of Bisphenol A in Soil, Sludge, and Biosolidsby Pressurized Fluid Extraction and Analyzed by LiquidChromatography/Tandem Mass Spectrometry1This standard is issued under the fixed designation D7858; the number immediately fo

2、llowing the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This procedure

3、 covers the determination of BisphenolA(BPA) in soil, sludge, and biosolids. This test method is basedupon solvent extraction of a soil matrix by pressurized fluidextraction (PFE). The extract is filtered and analyzed by liquidchromatography/tandem mass spectrometry (LC/MS/MS).BPA is qualitatively a

4、nd quantitatively determined by this testmethod.1.2 UnitsThe values stated in SI units are to be regardedas standard. No other units of measurement are included in thisstandard.1.3 The method detection limit (MDL),2electrospray ion-ization (ESI) mode, and reporting range3for BPA are listed inTable 1

5、.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to us

6、e.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers

7、to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:4D653 Terminology Relating to Soil, Rock, and ContainedFluidsD1193 Specification for Reagent WaterD3694 Practices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3740 Practice for Minimum Requirements

8、 for AgenciesEngaged in Testing and/or Inspection of Soil and Rock asUsed in Engineering Design and ConstructionD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD5681 Terminology for Waste and Waste ManagementE2554 Practice for Estimating and Monitoring the Uncer-tainty

9、of Test Results of a Test Method Using ControlChart Techniques2.2 Other Documents:EPA SW-846 Test Methods for Evaluating Solid Waste,Physical/Chemical Methods540 CFR Part 136, Appendix B Definition and Procedure forthe Determination of the Method Detection Limit63. Terminology3.1 Definitions:3.1.1 B

10、isphenol A (BPA), n2,2-bis(4-hydroxyphenyl) pro-pane.3.1.2 Bisphenol A (propane-D6) (BPA-D6), ndeuteriumlabeled BisphenolAwhere the two methyl moieties contain all2H and is used as a surrogate in this method.1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is

11、the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Sept. 1, 2018. Published September 2018. Originallyapproved in 2013. Last previous edition approved in 2013 as D7858 13. DOI:10.1520/D7858-13R18.2The MDL is determined following the Code of Federal Regu

12、lations, 40 CFRPart 136, Appendix B utilizing solvent extraction of soil by PFE. A 10-g sample ofOttawa sand was utilized. A detailed process determining the MDL is explained inthe reference and is beyond the scope of this test method to be explained here.3Reporting range concentration is calculated

13、 from Table 4 concentrationsassuming a 25-L injection of the Level 1 calibration standard for BPA, and thehighest level calibration standard with a 5-mL final extract volume of a 10-g soilsample. Volume variations will change the reporting limit and ranges.4For referenced ASTM standards, visit the A

14、STM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.5Available from United States Environmental ProtectionAgency (EPA),WilliamJefferson Clinton Bldg., 1200

15、Pennsylvania Ave., NW, Washington, DC 20460,http:/www.epa.gov.6Available from U.S. Government Printing Office Superintendent of Documents,732 N. Capitol St., NW, Mail Stop: SDE, Washington, DC 20401, http:/www.access.gpo.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Cons

16、hohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Or

17、ganization Technical Barriers to Trade (TBT) Committee.13.1.3 filter unit, nin this test method, a filter that issupported with a housing that is inert to the solvents used asdescribed in 7.4 of this test method.3.1.4 filtration device, na device used to remove particlesfrom the extract that may clo

18、g the liquid chromatographysystem as described in 7.4 of this test method.3.1.5 glass fiber filter, na porous, glass fiber material ontowhich solid particles present in the extraction fluid, whichflows through it, are largely caught and retained, thus removingthem from the extract.3.1.6 hypodermic s

19、yringe, nin this test method, a Luer-lock-tipped glass syringe capable of holding a syringe-drivenfilter unit as described in 7.4 of this test method.3.1.7 pressurized fluid extraction, nthe process of trans-ferring the analytes of interest from the solid matrix, a soil, intothe extraction solvent u

20、sing pressure and elevated temperature.3.1.8 reporting range, nthe quantitative concentrationrange for an analyte in this test method.3.2 Abbreviations:3.2.1 BPAbisphenol A3.2.2 LCliquid chromatography3.2.3 LCS/LCSDlaboratory control spike/laboratory con-trol spike duplicate3.2.4 mMmillimolar,1103mo

21、les/L3.2.5 MRMmultiple reaction monitoring3.2.6 MSmatrix spike3.2.7 NAnot available3.2.8 NDnon-detect3.2.9 PFEpressurized fluid extraction3.2.10 PPBparts per billion3.2.11 QCquality control3.2.12 RLreporting limit3.2.13 SDstandard deviation3.2.14 SRMsingle reaction monitoring3.2.15 VOAvolatile organ

22、ic analysis4. Summary of Test Method4.1 For BPA analysis in soil, sludge, and biosolid, samplesare shipped to the lab between 0 C and 6 C. The samples areto be extracted and filtered within 14 days of collection, andanalyzed by LC/MS/MS within 14 days of extraction.4.2 BPA and the surrogate (BPA-D6)

23、 are identified byretention time and one SRM transition. The target analytes andsurrogates are quantitated using the SRM transitions utilizingan external calibration. The final report issued for each samplelists the concentration of BPA and surrogate recovery.5. Significance and Use5.1 This is a per

24、formance-based method, and modificationsare allowed to improve performance.5.1.1 Due to the rapid development of newer instrumenta-tion and column chemistries, changes to the analysis describedin this test method are allowed as long as better or equivalentperformance data result. Any modifications s

25、hall be docu-mented and performance data generated. The user of the datagenerated by this test method shall be made aware of thesechanges and given the performance data demonstrating betteror equivalent performance.5.2 The first reported synthesis of BPA was by the reactionof phenol with acetone by

26、Zincke.7BPA has become animportant high-volume industrial chemical used in the manu-facture of polycarbonate plastic and epoxy resins. Polycarbon-ate plastic and resins are used in numerous products, includingelectrical and electronic equipment, automobiles, sports andsafety equipment, reusable food

27、 and drink containers, electricallaminates for printed circuit boards, composites, paints,adhesives, dental sealants, protective coatings, and many otherproducts.85.3 The environmental source of BPA is predominantlyfrom the decomposition of polycarbonate plastics and resins.BPAis not classified as b

28、io-accumulative by the U.S. Environ-mental Protection Agency and will biodegrade. BPA has beenreported to have adverse effects in aquatic organisms and maybe released into environmental waters directly at trace levelsthrough landfill leachate and sewage treatment plant effluents.This method has been

29、 investigated for use with soil, sludge,and biosolids.5.4 The land application of biosolids has raised concernsover the fate of BPAin the environment, and a standard methodis needed to monitor concentrations. This method has beeninvestigated for use with various soils.6. Interferences6.1 Method inte

30、rferences may be caused by contaminants insolvents, reagents, glassware, and other apparatus producingdiscrete artifacts or elevated baselines. All of these materialsare demonstrated to be free from interferences by analyzinglaboratory reagent blanks under the same conditions assamples.6.2 All reage

31、nts and solvents shall be of pesticide residuepurity or higher to minimize interference problems.6.3 Matrix interferences may be caused by contaminantsthat are co-extracted from the sample. The extent of matrixinterferences can vary considerably from sample source de-pending on variations of the sam

32、ple matrix.7. Apparatus7.1 LC/MS/MS System:7Zincke, T., “Mittheilungen aus dem chemischen Laboratorium der UniversitatMarburg,” Justus Leibigs Annals Chemie, Vol 343, 1905, pp. 7579.8Additional information about BPA is available on the Internet at http:/www.bisphenol-a.org (2008).TABLE 1 Method Dete

33、ction Limit and Reporting RangeAnalyte ESI Mode MDL (PPB)Reporting Range(PPB)Bisphenol A Negative 2.8 10250D7858 13 (2018)27.1.1 Liquid Chromatography (LC) System9A completeLC system is required in order to analyze samples. An LCsystem that is capable of performing at the flows, pressures,controlled

34、 temperatures, sample volumes, and requirements ofthe standard shall be used.7.1.2 Analytical Column10A column that achieves ad-equate resolution shall be used. The retention times and orderof elution may change depending on the column used and needto be monitored. A reverse-phase analytical column

35、thatcombines the desirable characteristics of a reversed-phaseHPLC column with the ability to separate polar compoundswas used to develop this test method.7.1.3 Tandem Mass Spectrometer (MS/MS) System11AMS/MS system capable of multiple reaction monitoring(MRM) analysis, or any system that is capable

36、 of performing atthe requirements in this test method, shall be used.7.2 Pressurized Fluid Extraction Device (PFE):127.2.1 A PFE system was used for this test method withappropriately sized extraction cells. Cells are available that willaccommodate the 10-g sample sizes used in this test method.Cell

37、s shall be made of stainless steel or other material capableof withstanding the pressure requirements (2000 psi) neces-sary for this procedure. A pressurized fluid extraction deviceshall be used that can meet the necessary requirements in thistest method.7.2.2 Glass Fiber Filters.137.2.3 Amber VOA V

38、ials60 mL, for sample extracts forPFE.7.3 Organic Solvent Evaporation Device.147.4 Filtration Device:7.4.1 Hypodermic SyringeA Luer-lock tip glass syringecapable of holding a syringe-driven filter unit.7.4.1.1 A 10-mL lock-tip glass syringe size isrecommended, since a 3-mL sample extract results aft

39、erblow-down.7.4.2 Filter Unit15Filter units of polyvinylidene fluoride(PVDF) with a glass fiber prefilter were used to filter the PFEextracts.7.4.3 DiscussionA filter unit shall be used that meets therequirements of the test method.8. Reagents and Materials8.1 Purity of ReagentsHigh-performance liqu

40、id chroma-tography (HPLC) pesticide residue analysis andspectrophotometry-grade chemicals shall be used in all tests.Unless indicated otherwise, it is intended that all reagents shallconform to the Committee on Analytical Reagents of theAmerican Chemical Society.16Other reagent grades may beused, pr

41、ovided they are first determined to be of sufficientlyhigh purity to permit their use without affecting the accuracy ofthe measurements.8.2 Purity of WaterUnless otherwise indicated, referencesto water shall mean reagent water conforming to ASTM TypeI of Specification D1193. It must be demonstrated

42、that thiswater does not contain contaminants at concentrations suffi-cient to interfere with the analysis.8.3 GasesNitrogen (purity 97 %) and argon (purity99.999 %).8.4 Acetonitrile (CH3CN, CAS # 75-05-8).8.5 Ethyl acetate (CH3COOC2H5, CAS # 141-78-6).8.6 2-Propanol (C3H8O, CAS # 67-63-0).8.7 Methan

43、ol (CH3OH, CAS # 67-56-1).8.8 Ammonium acetate (CH3CO2NH4, CAS # 631-61-8).8.9 Bisphenol A (C15H16O2, 2,2-Bis(4-hydroxyphenyl)propane, CAS # 80-05-7).8.10 Bisphenol A (Propane-D6) represents deuterium la-beled Bisphenol A where the two methyl moieties contain all2H.8.10.1 DiscussionBPA-D6is used as

44、a surrogate in thistest method.8.11 Ottawa sand (CAS # 14808-60-7) or equivalent.8.12 Drying agent.178.13 Sodium sulfate (Na2SO4, CAS # 7757-82-6).9A Waters Acquity UPLC H-Class System was used to develop this testmethod and generate the precision and bias data presented in Section 16. WatersCorpora

45、tion, Milford, MA 01757. Instrumentation from other vendors may also beable to generate similar method performance.10A Waters-UPLC T3, 100 mm x 2.1 mm, 1.8-m particle size, was used todevelop this test method and generate the precision and bias data presented inSection 16. Waters Corporation, Milfor

46、d, MA 01757. Columns from other vendorsthat are able to generate similar method performance and that achieve adequateresolution may be used. A guard column was also used, VanGuard Pre-Column,2.1 5 mm, 1.8-m particle size.11AWaters Quattro microAPI mass spectrometer was used to develop this testmetho

47、d and generate the precision and bias data presented in Section 16. WatersCorporation, Milford, MA 01757. Instrumentation from other vendors may also beable to generate similar method performance.12A Dionex Accelerated Solvent Extraction (ASE 200) system with appropri-ately sized extraction cells wa

48、s used to develop this test method and generate theprecision and bias data presented in Section 16. Dionex Corporation, Sunnyvale, CA94088. Instrumentation from other vendors may also be able to generate similarmethod performance.13Whatman Glass Fiber Filters 19.8 mm, Dionex Corporation, Part # 0470

49、17specially designed for the PFE system11were used to develop this test method andgenerate the precision and bias data presented in Section 16. Filters from othervendors may also be able to generate similar method performance.14A TurboVap LV was used in this test method from Caliper Life Sciences,Hopkinton, MA01748 and an N-Evap 24-port nitrogen evaporation device was usedin this test method from Organomation Associates Inc., West Berlin, MA 01503.In-house built or devices from other vendors may also be able to generate simil