Report number PFA T. Authors: Stephen Summerfield. Date: 19 September 2012

Transcription

1 Reconsile Consortium: Substance Identification Profile for Silsesquioxanes, Ph (Reaction mass of the monomer, dimer and oligomers of phenyltris(trimethylsiloxy)silane) Report number PFA T Authors: Stephen Summerfield Date: 19 September 2012 Saxon House, John Roberts Business Park, Pean Hill, Nr Canterbury, Kent CT5 3BJ Tel: (+44)(0) Fax:(+44)(0) Mobile: (+44)(0) Web Site: Company Number (England and Wales) VAT Number: GB

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3 Contents Record of report finalisation... i Contents... ii 1. Substance Identification Profile Introduction and methods Analytical characterisation to confirm substance identity Reconsile substances: appropriate analytical information Information available for Silsesquioxanes, Ph Companies with an interest in the SIP Substance Identifiers Naming according to the REACH Guidance EC Name CAS Name Other Names EC Number CAS Number Other Identity Code Structural Information Structure and SMILES code Optical Activity Composition of the Substance % range of major constituents Nature of Impurities Percentage of Impurities Nature and Percentage of Any Additives Spectral Data Chromatographic Data Analytical Methods Confidential Annexes ii

4 Reconsile Consortium: Substance Identification Profile for Silsesquioxanes, Ph 1. Substance Identification Profile This is a multiconstituent substance. The naming according to the REACH Guidance on Substance Identity is: Reaction mass of the monomer, dimer and oligomers of phenyltris(trimethylsiloxy)silane. EC Name Silsesquioxanes, Ph EC CAS Name Phenyl Silsesquioxanes CAS , The substance identification profile applicable to the Reconsile Consortium at the date of this report is: Constituents Name Range Constituent 1 Phenyltris(trimethylsiloxy)silane 10-25% Constituent 2 1,3-diphenyl-1,1,3,3-tetra(trimethylsiloxy)disiloxane 30-45% Constituent 3 1,3,5-triphenyl-1,1,3,5,5-penta(trimethylsiloxy)trisiloxane 10-25% Structure Where n=1, 2 or 3 Deviations outside these purity ranges may be acceptable but should they occur a company should assess their statistical significance and submit new information if necessary. Siloxane and alkoxysilane impurities have been identified. No definite SVHC constituents are present. The basis of the profile is described in the sections following this summary. 3 Report number PFA T 19 September 2012

5 2. Introduction and methods The substance, Silsesquioxanes, Ph (EC , CAS ), may be registered by one or more members of the REACH Consortium known as Reconsile. This report concerns review of compositional data provided to Peter Fisk Associates for review, in order to establish the sameness (comparability) of samples from different suppliers (manufacturers or importers). It consists of a brief review of the information provided by each legal entity, in confidential annexes, and a generic non-confidential substance identification profile (SIP). Reconsile members having identified certain information entered in IUCLID 5 as confidential, such as impurity profiles, should inform PFA accordingly so that the confidentiality can be maintained in the SIP. This SIP assists with demonstration of Valid sharing of studies from different companies, as far as reasonably practicable pre-sief consortium arrangements and for the SIEF itself, inclusion of any non- Reconsile joiners. It may be of use in the Reach Registration process for individual registrants, but that is not its primary purpose. Should it be the case that during review, the authors of this report wished to exclude a substance from one or more suppliers on grounds of lack of sameness (despite use of the same EINECS number by the suppliers), then the authors will have discussed that with the suppliers, but no report of that has been included in this report. This report does not include the reports or spectra provided by the individual companies, but does reference the sources. 2.1 Analytical characterisation to confirm substance identity. (From the ECHA Guidance for identification and naming of substances under REACH). When a registration is required under REACH it shall include information on the identification of the substance as specified in item 2 of Annex VI (see table 1). This information shall be adequate to enable each substance to be identified sufficiently. A multi-constituent substance is a substance, defined by its quantitative composition, in which more than one main constituent is present in a concentration 10% (w/w) and < 80% (w/w). A multi-constituent substance is the result of a manufacturing process. REACH requires the registration of a substance as produced. If a multi-constituent substance is manufactured, the multi-constituent substance needs to be registered. It is a case by case decision to establish to what extent the different steps in producing the substance are covered by the definition manufacturing. All 4 Report number PFA T 19 September 2012

6 substances covered previously by EINECS (e.g. multiconstituent substances were covered if all individual constituents were listed on EINECS) would qualify as phase-in substances. There is no need to test the substance as such, if the hazard profile of the substance can be sufficiently described by the information of the individual constituents. A multi-constituent substance is named as a reaction mass of the main constituents of the substance as such i.e. not the starting materials needed to produce the substance.the generic format is: Reaction mass of [names of the main constituents]. It is recommended that the names of the constituents are presented in alphabetical order and they are separated by the conjunction and. Only main constituents typically 10% contribute to the name. In principle, the names should be given in English language according to the IUPAC nomenclature rules. Other internationally accepted designations can be given in addition. A multi-constituent substance is identified by the chemical name and identifiers of the substance as such, and the quantitative and qualitative chemical composition (chemical identity, including the molecular and structural formula) of the constituents, and is proven by analytical information. For multi-constituent substances, the chemical composition is known and more than one main constituent is relevant for the identification of the substance. Furthermore, the chemical composition of the substance is predictable, as typical values and ranges. The main constituents shall be specified completely by all relevant parameters. The sum of typical concentrations for main constituents ( 10%) and impurities (< 10%) shall be 100%. For correct application of the 10% and 80% rule, intentionally added substances, e.g. ph-regulators or colouring agents, shall not be included in the mass balance. If it is not technically possible, or if it does not appear scientifically necessary, to give information on one or more of the substance identification parameters, the reasons shall be clearly stated in the form of an expert statement. The analytical characterisation should on this basis confirm the identity of the substance, by defining its chemical composition. 5 Report number PFA T 19 September 2012

7 Table 1: Substance identification parameters in REACH Annex VI item 2: 2. IDENTIFICATION OF THE SUBSTANCE For each substance the information given shall be sufficient to enable each substance to be identified. If it is not technically possible or if it does not appear scientifically necessary to give information on one or more items below, the reason shall be clearly stated. 2.1 Name or other identifier of each substance Name(s) in the IUPAC nomenclature or other international chemical name(s) Other names (usual name, trade name, abbreviation) EINECS or ELINCS number (if available and appropriate) CAS name and CAS number (if available) Other identity code (if available) 2.2 Information related to molecular and structural formula of each substance Molecular and structural formula (including SMILES notation, if available) Information on optical activity and typical ratio of (stereo) isomer (if applicable and appropriate) Molecular weight or molecular weight range 2.3. Composition of each substance Degree of purity (%) Nature of impurities, including isomers and by-products Percentage of (significant) main impurities Nature and order of magnitude (...ppm,...%) of any additives (e.g. stabilising agents or inhibitors) Spectral data (ultra-violet, infra-red, nuclear magnetic resonance or mass spectrum) High performance liquid chromatogram, gas chromatogram Description of the analytical methods or the appropriate bibliographical references for the identification of the substance and, where appropriate, for the identification of impurities and additives. This information shall be sufficient to allow the methods to be reproduced. 2.2 Reconsile substances: appropriate analytical information Sufficient spectral data are needed to confirm the structure given for a monoconstituent substance or to confirm that a reaction mixture is not a preparation. Spectroscopic methods see below. Quantitative NMR is useful if quantification by chromatography is not analytically possible. It should be noted that 29 Si-NMR would only quantify silicon containing compounds. Chromatographic methods, such as Gas Chromatography (GC) or High- Performance Liquid Chromatography (HPLC) are needed to confirm the composition of the substance. An appropriate chromatogram will confirm the existence of impurities, additives and the constituents of a reaction mixture. If appropriate, also other valid constituent separation techniques may be used. Spectroscopic and analytical methods are subject to continuous change. Therefore, it is the responsibility of the registrant to present appropriate spectral and analytical data. REACH requires the registrant to describe the analytical methods and/or to provide the bibliographical references for the methods used for identification of the substance and, where appropriate, for the identification of impurities and additives. This information should be sufficient to allow the methods to be reproduced. 6 Report number PFA T 19 September 2012

8 The agreed application of these principles within the Reconsile Consortium: Qualitative NMR (at least one of 29 Si, 13 C, 1 H) would usually be useful GC-MS or GC-FID/GC-TCD and MS. FT-IR would usually be useful UV-Vis would most of the time not be needed for Si based materials due to the absence of chromophores (an expert statement may be required). In addition 1. GLP is not required for the analytical characterisation; 2. Impurities should be identified if 1% w/w; 3. svhc impurities should be identified if 0.1% w/w if there are grounds to believe based on expert review that they might be present, for example due to the manufacturing process. As general methodology, the lowest purity from a company causes a purity to be set in the SIP according to the following: Lowest Rounded down to 80-85% 80% w/w % 85% w/w % 90% w/w % 93% w/w % 95% w/w % 97% w/w % 98% w/w % 99% w/w % 99.5% w/w This gives some flexibility. In addition, it should be noted that suppliers were asked to analyse samples of their highest grade commercial products. When a company sells a product of lower purity than the SIP, then they have to ensure that they take any steps to ensure valid use of the shared data. 7 Report number PFA T 19 September 2012

9 3. Information available for Silsesquioxanes, Ph This section gives the basis of the substance identification profile. 3.0 Companies with an interest in the SIP Dow Corning Europe SA The exact legal entities with responsibility for the substance, as defined by the REACH Regulation, are the responsibility of these companies themselves. The SIP is based on the information available from the companies, described in section 2.3. The one company with an interest in the substance has provided data. 3.1 Substance Identifiers Naming according to the REACH Guidance Reaction mass of the monomer, dimer and oligomers of phenyltris(trimethylsiloxy)silane EC Name Silsesquioxanes, Ph CAS Name Phenyl Silsesquioxanes Other Names The relevant parts of the CAS Registry File entry (on 11 th February 2011) for the substance follow unamended: Display from REGISTRY ANSWER ACS on STN CAS Registry Number Deleted Registry Number , , , Chemical Name Silsesquioxanes, Ph (CA INDEX NAME) Silsesquioxanes, phenyl 217 Flake Belsil SPR 45VP CF Report number PFA T 19 September 2012

10 Dow Corning 217 Dow Corning 217 Flake Dow Corning 217 Flake Resin FT 8 Gelest SST 3P01 LP 103 Ph silsesquioxanes Phenylsilsesquioxanes PM 1270 Silane, chlorotrimethyl-, hydrolysis products with trimethoxyphenylsilane, polymeric SR 165 SR 21 SR 23 Molecular Formula See the individual constutents EC Number The EC number has been linked to CAS The EC number has been allocated to CAS CAS Number The substance was formerly referred to by CAS Other Identity Code None. 9 Report number PFA T 19 September 2012

11 3.2 Structural Information Structure and SMILES code Constituent 1 Phenyltris(trimethylsiloxy)silane Where n = 1, 2 or 3. Canonical SMILES O([Si](O[Si](C)(C)C)(O[Si](C)(C)C)c1ccccc1)[Si](C)(C)C Mol Wt: g/mol Constituent 2 1,3-diphenyl-1,1,3,3-tetra(trimethylsiloxy)disiloxane Structure Canonical SMILES O([Si](O[Si](C)(C)C)(O[Si](C)(C)C)c1ccccc1)[Si](O[Si](C)(C)C)(O[Si](C)(C)C)c1ccccc1 Mol Wt: g/mol 10 Report number PFA T 19 September 2012

12 Constituent 3 1,3,5-triphenyl-1,1,3,5,5-penta(trimethylsiloxy)trisiloxane Structure Canonical SMILES O([Si](O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)c1ccccc1)(O[Si](C)(C)C)c2ccccc2)[Si](O[Si](C) (C)C)(O[Si](C)(C)C)c3ccccc3 Mol Wt: g/mol Optical Activity The substance is not optically active. 11 Report number PFA T 19 September 2012

13 3.3 Composition of the Substance % range of major constituents Constituents Name Range Constituent 1 Phenyltris(trimethylsiloxy)silane 10-25% Constituent 2 1,3-diphenyl-1,1,3,3-tetra(trimethylsiloxy)disiloxane 30-45% Constituent 3 1,3,5-triphenyl-1,1,3,5,5-penta(trimethylsiloxy)trisiloxane 10-25% Nature of Impurities Listing of any impurities common to all suppliers Non-volatile oligomers and/or polymers 5-15% Description of the general structural types of other impurities Siloxane and alkoxysilane impurities have been identified Listing of possible SVHC impurities None Listing of other impurities that may contribute to the classification and labelling of the substance None of the impurities contribute to the classification and labelling of the substance. Specific details are given in the Confidential Annexes Percentage of Impurities Information on impurities >1% Non-volatile polymers 5-15% Information on SVHC >0.1% None Nature and Percentage of Any Additives None. 12 Report number PFA T 19 September 2012

14 3.3.5 Spectral Data NMR The one company with an interest in the SIP has provided 1 H NMR, 13 C NMR and 29 Si NMR spectra MS The one company with an interest in the SIP has provided MS data IR The one company with an interest in the SIP has provided an FT-IR spectrum UV The one company with an interest in the SIP has provided UV-Vis spectra Chromatographic Data GC The one company with an interest in the SIP has provided GC-FID data HPLC Not needed as purity has been established by GC Gel Permeation Chromatography The one company with an interest in the SIP has provided gel permeation chromatography data Analytical Methods This report is based on analytical data provided by the member companies and reviewed by PFA. Individual companies are responsible for providing their own analytical data and appropriate method descriptions as part of their registration submission. 13 Report number PFA T 19 September 2012

15 4. Confidential Annexes These are found in report PFA A. For each company with an interest in the SIP, the annex contains a brief statement of what analytical data has been provided, the purity of the substance and the name and percentage of identified impurities. The confidential annexes will be made available to authorised representatives of the Reconsile Consortium and to the authorities as may be required. 14 Report number PFA T 19 September 2012