1、Designation: D7993 15Standard Guide forAnalyzing Complex Phthalates1This standard is issued under the fixed designation D7993; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indic
2、ates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This guide is established in response to regulatoryrequirements for the determination of complex branched phtha-lates by CAS numbers. This guide is intended to pr
3、ovideinformation on how to interpret and analyze data from achromatographic analysis involving complex phthalates withdefined CAS numbers.1.2 This guide provides a logical approach to determinelevels of complex branched phthalates meeting regulatory andCAS number requirements.1.3 The specific comple
4、x phthalates covered within thisguide are DINP and DIDP.1.4 LimitationsThis guide does not recommend any spe-cific test method. In some cases, it is necessary to deduce thequantity of substance present through the analysis and quanti-fication of its components. Although this approach is routinelyuse
5、d some degree of uncertainty exists in the final result due tothe reduced accuracy of the method.1.5 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.6 This standard does not purport to address all of thesafety concerns, if any
6、, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminol
7、ogy forAbbreviated Terms Relating to Plas-ticsD3465 Test Method for Purity of Monomeric Plasticizers byGas ChromatographyD7083 Practice for Determination of Monomeric Plasticiz-ers in Poly (Vinyl Chloride) (PVC) by Gas Chromatogra-phyD7823 Test Method for Determination of Low Level, Regu-lated Phtha
8、lates in Poly (Vinyl Chloride) Plastics byThermal DesorptionGas Chromatography/Mass Spec-trometryE355 Practice for Gas Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyIEEE/ASTM SI-10 Practice for Use of the I
9、nternationalSystem of Units (SI), the Modernized Metric System2.2 Spectral Library:NIST/EPA/NIH Mass Spectral Library2.3 SPI Association Publication:“Analytical Challenges in Detecting regulated Phthalates inFlexible PVC products” SPI Flexible Vinyl ProductsDivision 23rd Annual Compounding Conferenc
10、e, July 17,20123. Terminology3.1 DefinitionsFor definition of plastic terms used in thistest method, see Terminologies D883 and D1600.3.2 For units, symbols, and abbreviations used in this testmethod refer to Practices E355, E594,orIEEE/ASTM SI-10.3.3 Acronyms:3.3.1 CASChemical Abstract Services3.4
11、Compounds and Instrumentation:3.4.1 (DINP) 1,2-Benzenedicarboxylicacid, di-C8-10-branched alkyl esters, C9-rich CAS #68515-48-03.4.2 (DINP) 1,2-Benzenedicarboxylicacid, 1,2-diisononylCAS #28553-12-03.4.3 (DIDP) 1,2-Benzenedicarboxylicacid, di-C9-11-branched alkyl esters, C10-rich CAS #68515-49-13.4.
12、4 (DIDP) 1,2-Benzenedicarboxylicacid, 1,2-diisodecylCAS #26761-40-03.4.5 GC Gas Chromatography3.4.6 GC-MS Gas Chromatography-Mass Spectrometry3.4.7 LC-MS Liquid Chromatography-Mass Spectrometry3.4.8 PVC Poly(Vinyl Chloride)3.4.9 Complex branched phthalates are phthalate diesters/coesters based on al
13、cohols with a variety of branched isomers.1This guide is under the jurisdiction of ASTM Committee D20 on Plastics andis the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved April 1, 2015. Published April 2015. DOI: 10.1520/D7993-152For referenced ASTM stand
14、ards, 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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA
15、 19428-2959. United States1NOTE 1DINP and DIDP, used in various PVC or formulations in othermatrix are technical mixtures. When preparing the phthalate calibrationstandard, technical grade material shall be used. Specific information onexamples of technical grade DINPand DIDPcan be located on the in
16、ternetsearch engine.NOTE 2Branched phthalates have ranges of degrees and positions inbranching. Example: Branched C9phthalates have ranges of SlightlyBranched (primarily monomethyl-1-octyl- and dimethyl-1-heptyl-), Mod-erately Branched (primarily dimethyl-1-heptyl), and Highly Branched(3,5,5-trimeth
17、yl-1-hexyl-).34. Summary of Guide4.1 This guide provides a schematic flow diagram, illustrat-ing how to identify and quantify either one or both DINP andDIDP, either in neat chemical form or as extract from apolymer matrix.4.2 This guide provides identifier for each substance byCAS number and the ch
18、emical name that defines that CASnumber. Two CAS numbers and two associated chemicalnames for DINP, and two CAS number and two associatedchemical names for DIDP are in Section 3.4.3 This guide does not specify analytical method or proce-dure used for speciation. GC-MS and LC-MS are typicallyused to
19、identify chemical components in a substance.5. Significance and Use5.1 The regulatory candidate list classifies substances byCAS number. Complex branched phthalates, such as DINP orDIDP, manufactured with a defined alcohol distribution andregistered by CAS number with a chemical description of theco
20、mposition, shall be considered a single substance with thatcomposition as described.5.2 It is possible for the alcohols used in the manufacture ofcomplex branched phthalates to vary in isomer composition.Care must be used to ensure a representative standard is usedto the quantitation of the level of
21、 a complex branched phtha-late.5.3 This guide is intended to provide a method on how tointerpret and determine data from an analysis involving com-plex branched phthalates with defined CAS numbers. The testprocedure employed shall be used to provide speciation infor-mation to assist use of the schem
22、atic flow diagram.NOTE 3A discussion on analytical challenges in complex branchedphthalate analysis is found in: “Analytical Challenges in DetectingRegulated Phthalates in Flexible PVC Products,” SPI Flexible VinylProducts Division, 23rd Annual Compounding Conference, July 17, 2012.6. Substance List
23、6.1 Each of the four substances listed in Table 1 is a uniquesubstance by manufacture defined by its CAS number. Itsunique chemical name defines its specific chemical composi-tion as shown in Table 2. Since the same diesters and coesterscan be found in each of the four substances, care must be taken
24、to allocate the components to the correct CAS number.6.2 The schematic flow diagram is designed to aid in thecorrect allocation as described in 6.1.7. Scheme Diagram7.1 Quantification of DINP (1) (2) and DIDP (1) (2) by CASnumber shall include the entire distribution profile identifiedfollowing the
25、flow diagram (see Fig. 1). Distribution profile ofDINP (1) or DIDP (1) is sample specific and shall not bedefined by controls, which are not from the same samplesource.NOTE 4Commercially purchased control samples that are not repre-sentative of DINP (1), and DIDP (1) can introduce significant error
26、in bothqualitative and quantitative analysis. Examples are shown in the publica-tion referenced in Note 3.7.2 Some other complex substances with different CASnumbers, which share similar components as DINP and DIDPmust not be mistaken as containing DINP or DIDP. Care mustbe used to properly identify
27、 correctly. Some of such substancesare provided in the reference library list in Practice D7083.7.3 A second set of scheme diagram is provided in AnnexA1, using m/z mass ions in the flow cells as reference.TABLE 1 DINP and DIDP Substances CAS Number and Their Corresponding Registered Chemical NamesS
28、ubstance Name CAS Number Chemical NamesDINP (1) 68515-48-0 1,2-Benzenedicarboxylicacid, di-C8-10-branched alkyl esters, C9-richDINP (2) 28553-12-0 1,2-Benzenedicarboxylicacid, 1,2-diisononylDIDP (1) 68515-49-1 1,2-Benzenedicarboxylicacid, di-C9-11-branched alkyl esters, C10-richDIDP (2) 26761-40-0 1
29、,2-Benzenedicarboxylicacid, 1,2-diisodecylTABLE 2 DINP and DIDP Substances CAS Number and Their Chemical CompositionsSubstance Name CAS Number Cn/Cm- Chemical Composition of 1,2-Cn/Cm-phthalate (Cnand Cmare groups of branched isomers)DINP (1) 68515-48-0 C8/C8C9/C10C10/C10(plus C8/C10)DINP (2) 28553-
30、12-0 C9/C9DIDP (1) 68515-49-1 C9/C9C10/C11C11/C11(plus C9/C11)DIDP (2) 26761-40-0 C10/C103Handbook of PVC Formulating. Edward Wickson, John Wiley 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:/ 1524
