title: A practical gas chromatography flame ionization detection method for the determination of octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane in silicone emulsions.
abstract: A gas chromatography with flame ionization detection (GC-FID) method for analysis of D4, D5, and D6 cyclic siloxanes in silicone emulsions is described. Sample preparation involves breaking the emulsion with methanol and hexanes, and then analyzing the hexanes phase after derivatization with hexamethyldisilazane (HMDS). Silylation is performed to reduce the potential for formation of cyclic siloxanes during the course of the GC analysis. The accuracy of the method was verified by performing analyses on samples spiked with known levels of D4, D5 and D6 and by comparison to a referee method using atmospheric pressure chemical ionization liquid chromatography with mass spectrometry detection (APCI-LC-MS). Absolute differences of the results obtained between the two techniques were 0.03 weight percent or less, and relative differences were 15% or less. The reproducibility and ruggedness of the method was demonstrated by performing a global round robin test at four different geographic sites on four different types of silicone emulsions. The %RSDs obtained were less than 10% for all analytes and all emulsions examined.
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA. Electronic address: h.brothers@dowcorning.com.
authors.forename: Herbert M
authors.initials: HM
authors.lastname: Brothers
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Eric
authors.initials: E
authors.lastname: Bovens
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Antonio
authors.initials: A
authors.lastname: Bruni
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Tanya M
authors.initials: TM
authors.lastname: Habitz
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Tadashi
authors.initials: T
authors.lastname: Hamachi
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Yuanhua
authors.initials: Y
authors.lastname: Han
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Zhouhua
authors.initials: Z
authors.lastname: Ji
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Joel J
authors.initials: JJ
authors.lastname: Kerbleski
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Claude
authors.initials: C
authors.lastname: Letouche
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Yi Dong
authors.initials: YD
authors.lastname: Lu
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Regis
authors.initials: R
authors.lastname: Nguyen
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Michelle L
authors.initials: ML
authors.lastname: Rivard
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Xiaoman
authors.initials: X
authors.lastname: Qi
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Miki
authors.initials: M
authors.lastname: Shoji
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Ken
authors.initials: K
authors.lastname: Tanaka
authors.affiliation: Dow Corning Corporation, Analytical Sciences Department, Mail # CO41C1, P.O. Box 994 Midland, MI 48686-0994, USA.
authors.forename: Ronald E
authors.initials: RE
authors.lastname: Tecklenburg
mesh_terms: D004655:Emulsions; D005410:Flame Ionization; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods; D015203:Reproducibility of Results; D012828:Silicones / Q000737:chemistry*; D012833:Siloxanes / Q000032:analysis*
chemical_list: D004655:Emulsions; D012828:Silicones; D012833:Siloxanes; C114768:decamethylcyclopentasiloxane; C024064:octamethylcyclotetrasiloxane; C542115:dodecamethylcyclohexasiloxane
keywords: Atmospheric pressure chemical ionization mass spectrometry; D4; D5; Gas chromatography flame ionization detection; Silicone emulsions; Siloxanes