ISO 20163:2019 pdf download.Vulcanized rubber – Determination of free sulfur by gas chromatography (GC) and high performance liquid chromatography (HPLC)
1 Scope
This document specifies chromatographic methods for the determination of the inorganic free sulfur (Sx) not consumed during the vulcanization of the rubber. This method is used primarily to compare the free sulfur content in different samples.
NOTE 1 In this document, “free sulfur” is used instead of “inorganic free sulfur”.
NOTE2 The residual curing agent containing sulfur is not concerned by this measure.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.
ISO 1407:2011, Rubber一Determination of solvent extract
3 Terms and definitions
There are no term and definition in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
-ISO Online browsing platform: available at https://www.iso.org/obp
– IEC Electropedia: available at http://www.electropedia.org/
5.3.4 Data system, using an acquisition and a data processing software.
5.3.5 Apolar capillary column.
A column 5 % diphenyl-dimethylpolysiloxane of 30 m length, 0,25 mm diameter and 0,25 μum thickness film, is usually appropriate.
The use of an autosampler is recommended for a better precision.
5.4 Material for liquid chromatography (Method B).
5.4.1 Solvent pump, allowing the use of gradient.
5.4.2 Injector, allowing injection of variable volumes.
5.4.3 Ultraviolet (UV) detector.
5.4.4 Data system, using an acquisition and a data processing software.
5.4.5 Column, for example, a cartridge with C18 type silica-bound.
A column of 15 cm length, 4,6 mm diameter and 5 μm particle size, is usually appropriate.
6 Reagents and materials
6.1 Standard solutions
6.1.1 TPP, analytical grade.
6.1.2 TPPS, analytical grade.
6.1.3 Tetrahydrofuran (THF), HPLC grade.
6.2 Materials for preparation of samples
6.2.1 Single use polytetrafuoroethylene (PTFE) filters, 25 mm diameter, 0,45 μm porosity.
6.2.2 Solvent for extraction, according to ISO 1407:2011, Table A.1, or any suitable solvent (e.g.dichloromethane). ,
6.2.3 THF, HPLC grade.
6.3 Reagents used in GC
6.3.1 Helium, purity≥99,999 % or purity 2 99,999 9 % quality, as carrier gas (hydrogen can also be used).
6.3.2 Air and hydrogen, purity≥99,99 %.
6.3.3 Syringe rinsing solvent: cyclohexane of analytical grade [or other solvent for the sample dissolution]. .
ISO 20163:2019 pdf download
