Analyzing Complex Phthalates: Standard Guide For

Designation: D7993 − 15
Standard Guide for

Analyzing Complex Phthalates1
This standard is issued under the fixed designation D7993; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope D7083 Practice for Determination of Monomeric Plasticiz-

1.1 This guide is established in response to regulatory ers in Poly (Vinyl Chloride) (PVC) by Gas Chromatogra-
requirements for the determination of complex branched phtha- phy
lates by CAS numbers. This guide is intended to provide D7823 Test Method for Determination of Low Level, Regu-
information on how to interpret and analyze data from a lated Phthalates in Poly (Vinyl Chloride) Plastics by
chromatographic analysis involving complex phthalates with Thermal Desorption—Gas Chromatography/Mass Spec-
defined CAS numbers. trometry
E355 Practice for Gas Chromatography Terms and Relation-
1.2 This guide provides a logical approach to determine ships
levels of complex branched phthalates meeting regulatory and E594 Practice for Testing Flame Ionization Detectors Used
CAS number requirements. in Gas or Supercritical Fluid Chromatography
1.3 The specific complex phthalates covered within this IEEE/ASTM SI-10 Practice for Use of the International
guide are DINP and DIDP. System of Units (SI), the Modernized Metric System
1.4 Limitations—This guide does not recommend any spe- 2.2 Spectral Library:
cific test method. In some cases, it is necessary to deduce the NIST/EPA/NIH Mass Spectral Library
quantity of substance present through the analysis and quanti- 2.3 SPI Association Publication:
fication of its components. Although this approach is routinely “Analytical Challenges in Detecting regulated Phthalates in
used some degree of uncertainty exists in the final result due to Flexible PVC products” SPI Flexible Vinyl Products
the reduced accuracy of the method. Division 23rd Annual Compounding Conference, July 17,
2012
1.5 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3. Terminology
standard.
3.1 Definitions—For definition of plastic terms used in this
1.6 This standard does not purport to address all of the test method, see Terminologies D883 and D1600.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.2 For units, symbols, and abbreviations used in this test
priate safety and health practices and determine the applica- method refer to Practices E355, E594, or IEEE/ASTM SI-10.
bility of regulatory limitations prior to use. 3.3 Acronyms:
3.3.1 CAS—Chemical Abstract Services
2. Referenced Documents
3.4 Compounds and Instrumentation:
2.1 ASTM Standards:2 3.4.1 (DINP) 1,2-Benzenedicarboxylicacid, di-C 8-10 -
D883 Terminology Relating to Plastics branched alkyl esters, C9-rich CAS #68515-48-0
D1600 Terminology for Abbreviated Terms Relating to Plas- 3.4.2 (DINP) 1,2-Benzenedicarboxylicacid, 1,2-diisononyl
tics CAS #28553-12-0
D3465 Test Method for Purity of Monomeric Plasticizers by 3.4.3 (DIDP) 1,2-Benzenedicarboxylicacid, di-C 9-11 -
Gas Chromatography branched alkyl esters, C10-rich CAS #68515-49-1
3.4.4 (DIDP) 1,2-Benzenedicarboxylicacid, 1,2-diisodecyl
1
CAS #26761-40-0
This guide is under the jurisdiction of ASTM Committee D20 on Plastics and
is the direct responsibility of Subcommittee D20.70 on Analytical Methods. 3.4.5 GC Gas Chromatography
Current edition approved April 1, 2015. Published April 2015. DOI: 10.1520/ 3.4.6 GC-MS Gas Chromatography-Mass Spectrometry
D7993-15
2
3.4.7 LC-MS Liquid Chromatography-Mass Spectrometry
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
3.4.8 PVC Poly(Vinyl Chloride)
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on 3.4.9 Complex branched phthalates are phthalate diesters/
the ASTM website. coesters based on alcohols with a variety of branched isomers.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
D7993 − 15
NOTE 1—DINP and DIDP, used in various PVC or formulations in other 5.3 This guide is intended to provide a method on how to
matrix are technical mixtures. When preparing the phthalate calibration interpret and determine data from an analysis involving com-
standard, technical grade material shall be used. Specific information on
examples of technical grade DINP and DIDP can be located on the internet
plex branched phthalates with defined CAS numbers. The test
search engine. procedure employed shall be used to provide speciation infor-
NOTE 2—Branched phthalates have ranges of degrees and positions in mation to assist use of the schematic flow diagram.
branching. Example: Branched C9 phthalates have ranges of Slightly
Branched (primarily monomethyl-1-octyl- and dimethyl-1-heptyl-), Mod- NOTE 3—A discussion on analytical challenges in complex branched
erately Branched (primarily dimethyl-1-heptyl), and Highly Branched phthalate analysis is found in: “Analytical Challenges in Detecting
(3,5,5-trimethyl-1-hexyl-).3 Regulated Phthalates in Flexible PVC Products,” SPI Flexible Vinyl
Products Division, 23rd Annual Compounding Conference, July 17, 2012.
4. Summary of Guide
6. Substance List
4.1 This guide provides a schematic flow diagram, illustrat-
6.1 Each of the four substances listed in Table 1 is a unique
ing how to identify and quantify either one or both DINP and
substance by manufacture defined by its CAS number. Its
DIDP, either in neat chemical form or as extract from a
unique chemical name defines its specific chemical composi-
polymer matrix.
tion as shown in Table 2. Since the same diesters and coesters
4.2 This guide provides identifier for each substance by can be found in each of the four substances, care must be taken
CAS number and the chemical name that defines that CAS to allocate the components to the correct CAS number.
number. Two CAS numbers and two associated chemical
6.2 The schematic flow diagram is designed to aid in the
names for DINP, and two CAS number and two associated
correct allocation as described in 6.1.
chemical names for DIDP are in Section 3.
4.3 This guide does not specify analytical method or proce- 7. Scheme Diagram
dure used for speciation. GC-MS and LC-MS are typically 7.1 Quantification of DINP (1) (2) and DIDP (1) (2) by CAS
used to identify chemical components in a substance. number shall include the entire distribution profile identified
following the flow diagram (see Fig. 1). Distribution profile of
5. Significance and Use
DINP (1) or DIDP (1) is sample specific and shall not be
5.1 The regulatory candidate list classifies substances by defined by controls, which are not from the same sample
CAS number. Complex branched phthalates, such as DINP or source.
DIDP, manufactured with a defined alcohol distribution and
NOTE 4—Commercially purchased control samples that are not repre-
registered by CAS number with a chemical description of the sentative of DINP (1), and DIDP (1) can introduce significant error in both
composition, shall be considered a single substance with that qualitative and quantitative analysis. Examples are shown in the publica-
composition as described. tion referenced in Note 3.
5.2 It is possible for the alcohols used in the manufacture of 7.2 Some other complex substances with different CAS
complex branched phthalates to vary in isomer composition. numbers, which share similar components as DINP and DIDP
Care must be used to ensure a representative standard is used must not be mistaken as containing DINP or DIDP. Care must
to the quantitation of the level of a complex branched phtha- be used to properly identify correctly. Some of such substances
late. are provided in the reference library list in Practice D7083.
7.3 A second set of scheme diagram is provided in Annex
3
Handbook of PVC Formulating. Edward Wickson, John Wiley & Sons, 1993. A1, using m/z mass ions in the flow cells as reference.
TABLE 1 DINP and DIDP Substances CAS Number and Their Corresponding Registered Chemical Names
Substance Name CAS Number Chemical Names
DINP (1) 68515-48-0 1,2-Benzenedicarboxylicacid, di-C8-10-branched alkyl esters, C9-rich
DINP (2) 28553-12-0 1,2-Benzenedicarboxylicacid, 1,2-diisononyl
DIDP (1) 68515-49-1 1,2-Benzenedicarboxylicacid, di-C9-11-branched alkyl esters, C10-rich
DIDP (2) 26761-40-0 1,2-Benzenedicarboxylicacid, 1,2-diisodecyl
TABLE 2 DINP and DIDP Substances CAS Number and Their Chemical Compositions
Substance Name CAS Number Cn/Cm- Chemical Composition of 1,2-Cn/Cm-phthalate (Cn and Cm are groups of branched isomers)
DINP (1) 68515-48-0 C8/C8 < C8/C9 < C9/C9 > C9/C10 > C10/C10 (plus C8/C10)
DINP (2) 28553-12-0 C9/C9
DIDP (1) 68515-49-1 C9/C9 < C9/C10 < C10/C10 > C10/C11 > C11/C11 (plus C9/C11)
DIDP (2) 26761-40-0 C10/C10
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FIG. 1 Scheme Diagram
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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FIG. 1 (continued)
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ANNEX
(Mandatory Information)
A1. SCHEME DIAGRAM USING m/z MASS IONS IN THE FLOW CELLS AS REFERENCE
A1.1 See Fig. A1.1.
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FIG. A1.1 Scheme Diagram
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FIG. A1.1 (continued)
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Designation: D7993 − 15

Standard Guide for

1. Scope D7083 Practice for Determination of Monomeric Plasticiz-

FIG. 1 Scheme Diagram

A1.1 See Fig. A1.1.

FIG. A1.1 Scheme Diagram

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

FIG. A1.1 (continued)

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