1、Designation:D801815Standard Test Method forDetermination of(Tri-n-butyl)-n-tetradecylphosphoniumchloride(TTPC)in Soil by Multiple Reaction MonitoringLiquid Chromatography/Mass Spectrometry(LC/MS/MS)1This standard is issued under the fixed designation D8018;the number immediately following the design
2、ation 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 covers the determination
3、 of(Tri-n-butyl)-n-tetradecylphosphonium chloride(TTPC)in a soilmatrix by extraction with acetone,filtration,dilution withwater,and analysis by liquid chromatography/tandem massspectrometry.TTPC is a biocide that strongly adsorbs to soils.2The sample extracts are prepared in a solution of 75%acetone
4、and 25%water because TTPC has an affinity for surfaces andparticles.The reporting range for this method is from 250 to10 000 ng/kg.This analyte is qualitatively and quantitativelydetermine by this method.This method adheres to multiplereaction monitoring(MRM)mass spectrometry.1.2 The Method Detectio
5、n Limit(Note 1)(MDL)andReporting Range(Note 2)for the target analyte are listed inTable 1.NOTE1The MDL is determined following the Code of FederalRegulations,40 CFR Part 136,Appendix B,as a guide utilizing solventextraction of soil.Two-gram sample of Ottawa Sand was utilized.Adetailed process determ
6、ining the MDL is explained in the reference and isbeyond the scope of this standard to be explained here.NOTE2Reporting range concentration is calculated from Table 2concentrations assuming a 50 L injection of the Level 1 calibrationstandard for TTPC,and the highest level calibration standard with a
7、 20 mLfinal extract volume of a 2 g soil sample.Volume variations will changethe reporting limit and ranges.1.2.1 The reporting limit in this test method is the minimumvalue below which data are documented as non-detects.Ana-lyte detections between the method detection limit and thereporting limit a
8、re estimated concentrations and are not re-ported following this test method.The reporting limit iscalculated from the concentration of the Level 1 calibrationstandard as shown in Table 2 for TTPC after taking intoaccount a 2 g sample weight and a final extract volume of 20mL in 75%acetone/25%water.
9、The final extract volume is 20mL because a 15 mL volume of acetone is added to each soilsample and only the liquid layer after extraction is filteredleaving the solid behind followed by the addition of 5 mL ofwater to the acetone extract.1.3 UnitsThe values stated in SI units are to be regardedas st
10、andard.No other units of measurement are included in thisstandard.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 and health practices and determine the applic
11、a-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:3D1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD5681 Terminology for Waste and Waste ManagementD5847 Practice for
12、Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisE2554 Practice for Estimating and Monitoring the Uncer-tainty of Test Results of a Test Method Using ControlChart Techniques2.2 Other Documents:4EPA Publication SW-846 Test Methods for Evaluating SolidWaste,Physical/Ch
13、emical Methods40 CFR Part 136,Appendix B Definition and Procedure forthe Determination of the Method Detection Limit3.Terminology3.1 For determinations of terms used in this standard,referto Terminology D5681.1This test method is under the jurisdiction of ASTM Committee D34 on WasteManagement and is
14、 the direct responsibility of Subcommittee D34.01.06 onAnalytical Methods.Current edition approved Nov.1,2015.Published November 2015.DOI:10.1520/D8018-15.2More information on TTPC can be found at http:/ http:/iaspub.epa.gov/sor_internet/registry/substreg/searchandretrieve/advancedsearch/externalSea
15、rch.do?p_type=CASNO&p=81741-28-8(2014).3For referenced ASTM standards,visit the ASTM 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.4Available from National Te
16、chnical Information Service(NTIS),5301 ShawneeRd.,Alexandria,VA22312,http:/www.ntis.gov or at http:/www.epa.gov/epawaste/hazard/testmethods/index.htm.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.2 Definitions of Terms Specific to This Standard:3.2.1 batch QC,nall the quality control samples andstandards included in an analytical procedure.3.2.2 reporting limit check sample,RLCS,nthis sample isto verify that if the analyte was pre