Determination of Octamethylcyclotetrasiloxane (D4) and Decamethylcyclopentasiloxane (D5) in Cosmetics - Gas Chromatography
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ICS 71.100.70
CCS Y 42
National Standard of the People’s Republic of China
GB/T 40955-2021
Determination of
Octamethylcyclotetrasiloxane (D4) and
Decamethylcyclopentasiloxane (D5) in
Cosmetics — Gas Chromatography
化妆品中八甲基环四硅氧烷（D4）和十甲基环五硅氧烷（D5）的测定
气相色谱法
(English translation)
Issue date: 2021-11-26 Implementation date: 2022-06-01
Issued by the State Administration for Market Regulation of the
People's Republic of China
the Standardization Administration of the People's Republic
of China
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Contents
Foreword .............................................................................................................................. II
1 Scope ............................................................................................................................. 1
2 Normative References ................................................................................................... 1
3 Terms and Definitions..................................................................................................... 1
4 Principle.......................................................................................................................... 1
5 Reagents and Materials ................................................................................................. 1
6 Apparatus ....................................................................................................................... 2
7 Procedures ..................................................................................................................... 2
8 Calculation of Results .................................................................................................... 4
9 Recovery Rate and Precision ........................................................................................ 4
10 Tolerance ...................................................................................................................... 5
Annex A (Informative) Information on Standard Substances .............................................. 6
Annex B (Informative) Gas Chromatograms of Standard Substances
Octmethylcyclotetrasiloxane (D4) and Decamethylcyclopentasiloxane (D5)...................... 7
Annex C (Informative) Confirmatory Test ............................................................................ 8
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Foreword
ChinaStandards.net is in charge of this English translation. In case of any doubt about
the English translation, the Chinese original shall be considered authoritative.
This document is developed in accordance with the rules given in GB/T 1.1-2020
Directives for Standardization — Part 1: Rules for the Structure and Drafting of
Standardizing Documents.
Attention is drawn to the possibility that some of the elements of this document may be the
subject of patent rights. The issuing body of this document shall not be held responsible
for identifying any or all such patent rights.
This document was proposed by and is under the jurisdiction of National Technical
Committee 374 on Products Test Methods of Standardization Administration of China
(SAC/TC 374).
II
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Determination of Octamethylcyclotetrasiloxane
(D4) and Decamethylcyclopentasiloxane (D5) in
Cosmetics — Gas Chromatography
1 Scope
This document specifies the principle, reagents and materials, apparatus, procedures,
calculation of results, recovery rate and precision, and tolerance for the determination of
octamethylcyclotetrasiloxane (D4) and decamethylcyclopentasiloxane (D5) in cosmetics
by gas chromatography.
This document is applicable to the determination of octamethylcyclotetrasiloxane (D4) and
decamethylcyclopentasiloxane (D5) in aqueous solution, emulsion and cream (except
waxy based cosmetics) in resident and rinsing cosmetics.
2 Normative References
No normative reference is listed in this document.
3 Terms and Definitions
No terms and definitions are listed in this document.
4 Principle
The sample can be dispersed by isopropanol and extracted by n-hexane, then determined
by gas chromatograph for qualitative retention time and quantitative by external standard
method, and confirmed by gas chromatography-mass spectrometry if necessary.
5 Reagents and Materials
Unless otherwise specified, only chromatographically pure reagents are used.
5.1 Isopropanol
5.2 n-Hexane.
5.3 Standard substance: purity ≥ 95%. Information on octmethylcyclotetrasiloxane (D4)
and decamethylcyclopentasiloxane (D5) is given in Annex A.
5.4 Standard stock solution, 1000 μg/mL: take a proper amount of (to the nearest 0.0001
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g) octmethylcyclotetrasiloxane (D4) and decamethylcyclopentasiloxane (D5) standard
substance (5.3) in a volumetric flask, and mix with n-hexane (5.2) in constant volume.
5.5 Mixed standard working solution: a proper amount of standard stock solution (5.4)
shall be transferred to a volumetric flask and diluted with n-hexane (5.2) step by step to a
mixed standard working solution with mass concentrations of 0.5 μg/mL, 1.0 μg/mL, 5.0
μg/mL, 20.0 μg/mL, 50.0 μg/mL and 100.0 μg/mL.
5.6 Organic filter membrane: with a pore diameter of 0.22 μm.
6 Apparatus
6.1 Gas chromatograph: equipped with flame ionization detector.
6.2 GC-MS: equipped with electron impact (EI).
6.3 Analytical balance: with sensibility of 0.001 g and 0.0001 g.
6.4 Vortex mixer.
6.5 Ultrasonic cleaner: power ≥ 250 W.
6.6 Centrifuger: rotation speed ≥ 5 5000 r/min.
7 Procedures
7.1 Preparation of sample
Weigh the sample about 0.5 g (to the nearest 0.001 g) in a 10 mL colorimetric tube (with
plug); add about 0.5 mL isopropyl alcohol (5.1), vortex dispersion; and then add n-hexane
(5.2) to near scale, vortex 30 s, ultrasonic 15 min, cool to room temperature; use n-hexane
(5.2) constant volume to scale. After vortex mixing, centrifuge at 5000 r/min for 5 min,
appropriate amount of supernatant shall be taken and filtered through organic filter
membrane (5.6), and the filtrate shall be used as the solution to be tested.
7.2 Conditions of determination
Because of the variety of laboratory apparatus, it is not possible to give a general
parameter for the analysis conditions. The following operating conditions have been
shown to be appropriate for the determination:
a) Chromatographic column: (14% cyanopropyl - phenyl) methyl polysiloxane silica
capillary column. 30 m × 0.25 mm (i.d.) × 0.25 μm, or equivalent;
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