ISO 22744-1-2020 pdf free.Textiles and textile products – Determination of organotin compounds – Part 1: Derivatisation method using gas chromatography.
This document specifies a test method for the qualification and quantification of organotin compounds. This test method is applicable to all types of materials of textile products.
NOTE CEN/TR 16741 defines which materials are applicable to this determination.
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 4787, Laboratory glassware — Volumetric instruments — Met hods for testing of capacity and for use
3 Terms and definitions
No terms and definitions are listed 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.orgJobp
— IEC Electropedia: available at
4 Principle
The organotin substances are extracted from the material of a textile product with a methanol-ethanol mixture using tropolone as a complexing agent.
The polar and high-boiling organotin is then converted to the corresponding volatile alkyl derivative, by reaction with sodium tetraethylborate, NaB(Et)4. Finally, it is detected and quantified by using a gas chromatograph fitted with a mass selective detector (GC-MS).
Table 1 indicates the list of target compounds which can be analysed with this document.
This document is also applicable for further organotin substances provided that the method is validated with the additional compounds.
5 Reagents
Unless otherwise specified, use only reagents of recognized analytical grade.
5.1 Water, grade 3 according to ISO 3696.
5.2 Ethanol, technical grade or industrial methylated spirit (IMS), CAS number: 64-17-5.
5.3 Glacial acetic acid, CAS number: 64-19-7.
5.4 Sodium tetraethylborate, CAS number: 15523-24-7.
5.5 Tetrahydrofuran (THF), stabilized, CAS number: 109-99-9.
5.6 n-Heptyltin trichloride, CAS number: 59344-47-7 (internal standard).
5.7 Di-n-heptyltin dichloride, CAS number: 74340- 12-8 (internal standard).
5.8 Tri-n-pentyltin chloride, CAS number: 3342-67-4 (internal standard).
5.9 Tetra-n-propyltln, CAS number: 2176-98-9 (internal standard).
lithe recovery rate of the internal standards (5, 5..Z and £.9) is low, alternative internal standards
may be used (for example deuterated compounds) (see also 9,J.).
5.10 Hexane,CAS number: 110-54-3.
5.11 Inert gas, e.g. nitrogen or argon.
5.12 Tropolone (2-hydroxy-2,4,6-cycloheptatrien- 1 -one), CAS number: 533-75-5.
5.13 Methanol, of analytical grade, CAS number: 67-56-1.
5.14 Sodium acetate, CAS number: 127-09-3.
5.15 Organotin compounds, listed in Table 1.
6 Apparatus and materials
The usual equipment and laboratory glassware, according to Iso 4787, shall be used, in addition to the following.
6.1 Gas chromatograph with a mass selective detector (GC-MS).
6.2 Analytical balance, with a resolution of 0,1 mg.
6.3 Glass vessel, with screw tops and a volume of, for example, 50 ml.
6.4 Micropipettes, 10 il to 500 il range, with disposable tips.
6.5 Pipettes, 1 ml to 10 ml capacity.
6.6 CalIbrated pH-meter. with a glass combination electrode and range of 0 to 14.
6.7 Ultrasonic bath, with adjustable temperature suitable for operation at about 60 °C.ISO 22744-1 pdf download.