1、Designation: D7485 16Standard Test Method forDetermination of Nonylphenol, p-tert-Octylphenol,Nonylphenol Monoethoxylate and Nonylphenol Diethoxylatein Environmental Waters by Liquid Chromatography/TandemMass Spectrometry1This standard is issued under the fixed designation D7485; the number immediat
2、ely following 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 tes
3、t method covers the determination of nonylphe-nol (NP), nonylphenol ethoxylate (NP1EO), nonylphenol di-ethoxylate (NP2EO), and octylphenol (OP), extracted fromwater utilizing solid phase extraction (SPE), separated usingliquid chromatography (LC) and detected with tandem massspectrometry (MS/MS). Th
4、ese compounds are qualitativelyand quantitatively determined by this method. This methodadheres to single reaction monitoring (SRM) mass spectrom-etry.1.2 The method detection limit (MDL) and reporting limit(RL) for NP, NP1EO, NP2EO, and OP are listed in Table 1.1.3 The values stated in SI units are
5、 to be regarded asstandard. 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
6、and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1129 Terminology Relating to WaterD1193 Specification for Reagent WaterD2777 Practice for Determination of Precision and Bias ofApplicable Test Methods of Committee D19 on WaterD3694 P
7、ractices for Preparation of Sample Containers andfor Preservation of Organic ConstituentsD3856 Guide for Management Systems in LaboratoriesEngaged in Analysis of WaterD5847 Practice for Writing Quality Control Specificationsfor Standard Test Methods for Water AnalysisD5905 Practice for the Preparati
8、on of Substitute Wastewater2.2 Other Documents:3The Code of Federal Regulations 40 CFR Part 136, Appen-dix B3. Terminology3.1 Definitions:3.1.1 For definitions of terms used in this standard refer toTerminology D1129.3.2 Definitions of Terms Specific to This Standard:3.2.1 environmental water, nshal
9、l refer to water testedusing this method. See Section 5.3.2.2 nonylphenol, NP, nis a mixture of branchedp-nonylphenol isomers. Commercial NP is produced by thereaction of phenol with commercial nonene. Commercialnonene is not simply a linear C9H18 alpha olefin; it is acomplex mixture of predominantl
10、y nine-carbon olefins, calledpropylene trimer, containing no linear isomers. This synthesisresults in a mixture of various branched nonylphenol isomersrather than a discrete chemical structure. The branched nonylgroup is positioned predominantly in the para position on thephenol ring.3.2.3 octylphen
11、ol, OP, ncommercial octylphenol is pro-duced by the reaction of phenol and diisobutylene to producepredominantly the 4-(1,1,3,3-tetramethylbutyl)phenol isomer.3.2.4 independent reference material, IRM, na material ofknown purity and concentration obtained either from theNational Institute of Standar
12、ds andTechnology (NIST) or otherreputable supplier. The IRM shall be obtained from a differentlot of material than is used for calibration.3.3 Acronyms:1This test method is under the jurisdiction of ASTM Committee D19 on Waterand is the direct responsibility of Subcommittee D19.06 on Methods forAnal
13、ysis forOrganic Substances in Water.Current edition approved Feb. 1, 2016. Published March 2016. Originallyapproved in 2009. Last previous edition approved in 2009 as D7485 09. DOI:10.1520/D7485-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service
14、at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available 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.
15、Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13.3.1 CCC, nContinuing Calibration Check3.3.2 IC, nInitial Calibration3.3.3 LC, nLiquid Chromatography3.3.4 LCS/LCSD, nLaboratory Control Sample/Laboratory Control Sample Duplicate3.3.5
16、MDL, nMethod Detection Limit3.3.6 MeOH, nMethanol3.3.7 mM, nmillimolar,110-3moles/L3.3.8 MRM, nMultiple Reaction Monitoring3.3.9 MS/MSD, nMatrix Spike/Matrix Spike Duplicate3.3.10 NA, adjNot Available3.3.11 ND, nnon-detect3.3.12 NP1EO, nrepresents branched nonylphenolmonoethoxylate.3.3.13 NP2EO, nre
17、presents branched nonylphenol di-ethoxylate.3.3.14 n-NP2EO, nrepresents normal straight chain non-ylphenol diethoxylate. n-NP2EO is used in this method as asurrogate. It is not produced commercially and is not expectedto be found in environmental waters.3.3.15 P liquid chromatography; monoethoxylate
18、;nonylphenol; octylphenol; solid phase extraction; tandem massspectrometry; waterTABLE 10 Single-Laboratory Recovery Data for Sequim Bay, WA SeawaterSampleYoudenPairTargetCompoundSpike (ppt)NPAMeasured(ppt)NPPercentRecoveryOPMeasured(ppt)OPPercentRecoveryUnspiked Seawater 1 30Unspiked Seawater 2 39S
19、ample 1 1 150 108 72 146 93Sample 2 180 135 75 173 92Sample 3 2 750 547 73 663 88Sample 4 900 595 66 678 75Sample 5 3 1500 1566 104 1718 114Sample 6 1800 1358 75 1508 83SampleYoudenPairTargetCompoundSpike (ppt)NP1EOMeasured(ppt)NP1EOPercentRecoveryNP2EOMeasured(ppt)NP2EOPercentRecoveryUnspiked Seawa
20、ter 1Unspiked Seawater 2Sample 1 1 150 135 90 134 90Sample 2 180 154 85 172 96Sample 3 2 750 588 78 624 83Sample 4 900 672 75 702 78Sample 5 3 1500 1534 102 1650 110Sample 6 1800 1276 71 1335 74ASubtracted 35 ppt from NP sample results to account for average NP concentration in Unspiked Seawater.TAB
21、LE 11 Single-Laboratory Recovery Data for Chicago River WaterSampleYoudenPairTargetCompoundSpike (ppt)NPAMeasured(ppt)NPPercentRecoveryOPMeasured(ppt)OPPercentRecoveryUnspiked River Water 1 65Unspiked River Water 2 57Sample 1 1 150 87 58 133 89Sample 2 180 156 87 174 96Sample 3 2 750 456 61 682 91Sa
22、mple 4 900 591 66 742 82Sample 5 3 1500 1051 70 1206 80Sample 6 1800 1239 69 1493 83SampleYoudenPairTargetCompoundSpike (ppt)NP1EOMeasured(ppt)NP1EOPercentRecoveryNP2EOMeasured(ppt)NP2EOPercentRecoveryUnspiked River Water 1Unspiked River Water 2Sample 1 1 150 120 80 118 79Sample 2 180 151 84 147 82S
23、ample 3 2 750 540 72 512 68Sample 4 900 681 76 642 71Sample 5 3 1500 1009 67 1006 67Sample 6 1800 1200 67 1206 67ASubtracted 61 ppt from NP sample results to account for average NP concentration in Unspiked River Water.D7485 1610ASTM International takes no position respecting the validity of any pat
24、ent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision
25、 at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comm
26、ents will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighte
27、d by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 1611
